description stringlengths 2.98k 3.35M | abstract stringlengths 94 10.6k | cpc int64 0 8 |
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CROSS-REFERENCE TO RELATED APLLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application Ser. No. 61/833,797 filed Jun. 11, 2013.
FIELD OF THE INVENTION
[0002] The invention generally relates to techniques for arbitrage and pricing power in a market. More specifically, it relates to methods that structure individual entities into a group to purchase in volume and economically gain through collective buying power while providing incentives and a manageable and predictable structure for counterparties.
BACKGROUND OF INVENTION
[0003] The general consensus in economic theory is that the structure of an efficient market is defined by the theory of perfect competition. However, markets may not always operate according to the conditions of perfect competition. Some criteria not fulfilled may include: perfect information, zero transaction costs, and non-increasing returns to scale. For instance, companies spend billions of dollars in advertisements to inform the public. It becomes necessary then to structure a market in such a way that limits these inefficiencies by applying technology and structuring the inefficiencies themselves.
[0004] With the advance of smartphones and computer technology, it becomes possible to address these issues. Today, people increasingly use smartphones to make purchases via ecommerce, access the Internet while in store to become better informed, and receive discounts through mobile coupons. In fact, the market for ecoupons is important as it is estimated that the number of mobile coupon users will increase from 12.3 million in 2010 to 53.2 million in 2014 (Mobile Spurs Digital Coupon User Growth, eMarketer, http://www.emarketer.com/Article/Mobile-Spurs-Digital-Coupon-User-Growth/1009639#VtDzxL6QcVIG76xo.99, Jan. 31, 2013). The connectivity of the smartphone, whether through social or some other form, has permitted this explosive growth and the growth of companies like Groupon© and LivingSocial©.
[0005] Coupons are a rather inefficient market mechanism for both the merchant whose goal it is to increase volume and consumer base and the consumer whose goal it is to decrease the price of an item or service. For the merchant, the coupons may only attract free riders whose goal it is to use the service once at the discounted price and never return. Additionally, time, money and organizational effort must be allocated to run and promote the program. For the consumer, the couponing scheme requires a large investment in the opportunity cost. The time to search, gather and organize the different coupons can be overwhelming. As a result, couponing scheme structures market participants into two segments: those who allocate their time to couponing or the ‘in’ crowd and those who do not or the ‘out’ crowd. The first group usually does it for the emotional benefit of “the deal.” The second group just pays a higher price. Moreover, coupons are usually limited in one manner or another with expiration dates and purchase limits. As a result, the structure itself is inefficient because it rewards people on a ‘know first’ basis and unsustainable because merchants cannot or do not allow an infinite amount of purchases at the prevailing coupon rate. More over, other couponing models may require a base number of people to join before the coupon is activated. This model introduces uncertainty on whether the coupon will ultimately be used. In many cases, it requires a significant amount of synchronous social communication and coordination to form a suitable collective buying group. Again, the opportunity cost in this couponing model is expensive.
BRIEF SUMMARY OF INVENTION
[0006] The two fundamental keys for the present invention are collective buying power and the contract. Collective buying power is the mechanism that will minimize costs for both the party receiving the good or service (participant) and the party providing the good or service (merchant). The contract is the mechanism that will structure the market to create the buying collective and the incentive to invite additional participant to join the collective. It will also provide all market participants the same price per unit at a discrete moment in time. Meaning that while prices of contracts may fluctuate, the fluctuation will return the best possible outcome for each user, both at a discrete moment and summed over the life of the contract.
[0007] There are a few outcomes of the present invention that decrease the inefficiencies of current markets and particularly couponing models. Market participants are provided a real monetary incentive to share and recruit additional market participants. New participants joining take advantage of the prevailing group's collective buying power. Merchants gain access to a large market of participants that is also a steady and defined stream. The model is also sustainable over an infinite period of time instead of a one-time offer. Moreover, the contract takes uncoordinated individual entities and structures them into a larger, coordinated collective.
DETAILED DESCRIPTION
[0008] A market is a system of multiple participants (parties) who engage in exchange based on a prevailing structure. A party is an entity that can enter into an agreement. In this present invention, a new structure will be defined that will increase the efficiencies of prevailing market structures and introduce a new market type.
[0009] The contract will be the mechanism that provides the de-facto structure for the market. A contract is a written or spoken agreement that is intended to be enforceable and has the minimum characteristics:
1.) The contract has a price, p. 2.) The contract is defined for a time of period x. 3.) x is further divided into y number of periods. 4.) y must be greater than 0. 5.) For each y period, the holder of the contract will receive an order, o, of z number of item(s) or service(s) on a particular datetime. 6.) z must be greater than 0. 7.) A symbol, typically a mathematical equation, which represents the collective buying power of a contract given z number of item(s) concurrently under contract given discrete references in time and a corresponding price. 8.) When the contract is fulfilled, the holder of the contract will have received y*z number of items or services. To adhere to the homogeneous condition for perfect competition, similar contracts within the market will have similar x, y and z conditions. Variable contractual duration may exist through secondary markets and their emergence cannot be ignored. However, the present invention limits the need as at any given moment in time, a participant receives the same volume discount at the same moment in time regardless of the date entered into the contract. Moreover, the type of discount provided, linear, quadratic or some other function, can vary. It is also worth noting that the participant could receive all the items at the beginning of the contract; however, an order fulfillment date based on the period must be necessarily generated to provide a change in volume over the life of the contract, reflecting the exiting of the contract from the market.
[0018] Parties become participants in the market by entering into and interacting with a contract. The market exchanges the above-mentioned contracts and produces desirable outcomes that permit stakeholders to collectively buy without coordination or concern for time, volume and price fluctuations, or the degree of collective buying power. To examine the benefits, equations will be presented to describe the market outcomes. The present invention does not make the case that these equations are the only mathematical representation of the market. Rather, they serve to demonstrate the value of and processes necessary to utilize the present invention.
[0019] In a market, a party must engage in an exchange. In the present invention, a market participant purchases the contract at an initial price, referred to hereafter as the prevailing price, and in return receives fulfillment of the contract as per the terms. The prevailing price is the price from the current date and time until the end of the contract at a future date and reflects the total volume of the collective from the current date to the end date. Volume at a current time can fluctuate as parties choose either to enter a new contract or exit by not renewing. Because collective buying power is necessary for the present invention, price and volume are in an inverse relationship. As a result, the price of the contract can increase or decrease.
[0020] Once a party enters the contract, the prevailing price quoted becomes a reference point, referred to hereafter as the prevailing contract price. Just like the prevailing price, a prevailing contract price is calculated from the collective volume; however, the volume quoted is from the start to the end of the contract. As a result, the volume of the contract can increase as other parties enter but cannot decrease because parties cannot exit as per the contract. With the contract providing structure and collective buying power forcing the price movements, the price of a participant's contract can only decrease or remain the same over time.
[0021] Examining the structure through equations, a standard prevailing price can be represented as:
[0000] pp=yz ( p−d )
[0000] where pp is the prevailing price, y is the number of periods in the contract, z is the total number of items per period, p is the price per item and d is the discount.
[0022] A standard discount due to the collective buying power can be represented as:
[0000] d x =√{square root over ( x )}
[0000] where d x is the instant discount for x the total number of items per order contracted and x greater than 1.
[0023] The total discount for x the total number of items is:
[0000]
td
x
=
∫
x
=
2
x
3
/
2
3
[0024] where td x is the total discount of a contract for x the total number of items per order contracted.
[0025] Equating the discount on all items equally yields:
[0000]
d
=
2
x
3
[0026] A standard prevailing price for x number of items can be represented as:
[0000]
pp
x
=
yzp
(
1
-
2
x
3
)
[0000] where pp x is the prevailing price for x total number of item for the entire number of participants, y is the number of periods in the contract, z is the total number of items per period, p is the price per item and d is the discount.
[0027] x, the total volume, can be represented as:
[0000]
x
=
z
∑
i
n
O
i
[0000] where x is the total volume, z is the total number of items per period, i is the initial datetime, n is the ending datetime, and o i is the number of orders at i.
[0028] The standard price for quoting a contract given time interval can be represented as:
[0000]
pp
in
=
yzp
(
1
-
2
z
∑
i
n
O
i
3
)
[0000] where pp in is the price for the datetime i to n, y is the number of periods in the contract, z is the total number of items per period, p is the price per item, z is the total number of items per period, i is the initial datetime, n is the ending datetime, and o i is the number of orders at i.
[0029] The present invention creates improved outcomes for market participants. First, at any given moment in time, the discount received reflects the best possible price for the collective at the given volume amount. This decreases uncertainty because a participant does not need to worry about waiting and buying at a lower price in the future. Moreover, the present invention limits the uncertainty of the future by calculating prices for the future and tying them to the present price of the contract. As is evident above, if the participant is in the contract, the added volume in the future is captured in the quoted discount. Buying for multiple periods will also prevent a whiplash of price increases. The only way to exit is by allowing the contract to lapse. In exiting, the volume of the collective will gradually decrease as one order after another is fulfilled and escapes the collective volume calculation. As a result, the volume of the collective at the current datetime will decrease slowly. The structure of the market also provides incentives for individuals to invite and market the contract. After all, increasing the collective buying power also increases the discount. If the discount increases for a contract, the participants will be credited the difference. This incentive also compensates for the limit of choices which participants face once in a contract. Moreover, neither does the invitee receive less not the inviter more of a discount because the calculated discount is the instance of the buying collective volume at that moment in time given the volume over the life of the contract. As a result, the interests of all participants overlap.
[0030] The market structure also provides benefits for the merchant and/or manufacturer. They have access to a steady stream of consumers, predictable over a longer run, which can only decline slowly over time. As a result, merchants can predict the future more accurately, providing the ability to allocate capital more efficiently with a better understanding of cash flow. | Method pertains to a system of entities that make purchases and interact either synchronously or asynchronously into a group that exercises collective buying power. It provides a process whereby individual entities can enter the group at a specified price and receive a rebate as new entities enter the group. The method is useful because of its transparency, sustainability, and ability to provide economic benefits equitably to all stakeholders and incentives to entities in the group to market the group and recruit individuals to join the group. Move over, the structure of the system improves upon the standard coupon scheme as well as the bid and offer system. | 6 |
TECHNICAL FIELD
[0001] The present invention relates to a centrifuge container.
BACKGROUND ART
[0002] There is a conventionally known centrifuge separator in which a centrifuge container accommodating a cell suspension in which fat-derived cells are isolated by breaking down fat tissues is rotated around an axis located away from the centrifuge container, thereby separating components contained in the cell suspension according to their specific gravities (see PTL 1).
[0003] The centrifuge container is formed into a substantially cylindrical shape one end of which is closed. When the centrifuge container is rotated with the closed end being directed radially outward, components with higher specific gravities are moved to the closed end and are separated in descending order of specific gravity from the closed end.
CITATION LIST
Patent Literature
[0000]
{PTL 1} PCT International Publication No. WO 05/012480 Pamphlet
SUMMARY OF INVENTION
Technical Problem
[0005] One problem, however, is that a cell group separated in a bottom portion of the centrifuge container when the cell suspension is centrifuged is formed into a centrifugally solidified pellet. Specifically, if the cell group is formed into a pellet, it is difficult to remove the centrifuged cell group from the centrifuge container by suction. Furthermore, there is a case where the cell group is formed into a pellet while unwanted components, such as proteolytic enzyme and fat, are incorporated in the cell group during the centrifugation, and, in that case, it is difficult to remove the unwanted components.
[0006] The present invention has been made in view of the above-described circumstances, and an object thereof is to provide a centrifuge container capable of recovering a cell suspension that contains a cell group from which unwanted components have been removed by efficiently washing the cell group.
Solution to Problem
[0007] In order to achieve the above-described object, the present invention provides the following solutions.
[0008] According to one aspect, the present invention provides a centrifuge container including: a cylindrical container main body that accommodates a cell suspension and is rotated with a bottom portion being directed radially outward; a supernatant suction tube that has a first opening at a position in the depth direction of the container main body and that suctions a supernatant obtained by centrifuging the cell suspension, from the first opening, in the radial direction of the container main body; and a washing-fluid discharge tube that has a second opening at a position in the depth direction of the container main body and that discharges a washing fluid from the second opening, in the axial direction toward the bottom portion of the container main body.
Advantageous Effects of Invention
[0009] According to the present invention, an advantage is afforded that it is possible to recover a cell suspension containing a cell group from which unwanted components have been removed by efficiently washing the cell group.
BRIEF DESCRIPTION OF DRAWINGS
[0010] FIG. 1 is a longitudinal sectional view showing a centrifuge container according to an embodiment of the present invention.
[0011] FIG. 2 is a longitudinal sectional view showing a state where a cell suspension is accommodated in the centrifuge container shown in FIG. 1 .
[0012] FIG. 3 is a longitudinal sectional view showing a state where the cell suspension accommodated in the centrifuge container shown in FIG. 1 is centrifuged.
[0013] FIG. 4 is a longitudinal sectional view for explaining a step of suctioning a supernatant from the cell suspension centrifuged in FIG. 3 .
[0014] FIG. 5 is a longitudinal sectional view showing a step of supplying a washing fluid in the state shown in FIG. 4 .
[0015] FIG. 6 is a longitudinal sectional view showing a step of suctioning and recovering the cell suspension resuspended in the centrifuge container shown in FIG. 1 .
[0016] FIG. 7 is a longitudinal sectional view showing a first modification of the centrifuge container shown in FIG. 1 .
[0017] FIG. 8A is a partially-enlarged longitudinal sectional view showing a step of supplying a cell suspension, using the centrifuge container shown in FIG. 7 .
[0018] FIG. 8B is a partially-enlarged longitudinal sectional view showing a step of suctioning a supernatant, using the centrifuge container shown in FIG. 7 .
[0019] FIG. 8C is a partially-enlarged longitudinal sectional view showing a step of supplying a washing fluid, using the centrifuge container shown in FIG. 7 .
[0020] FIG. 8D is a partially-enlarged longitudinal sectional view showing a step of suctioning and recovering a cell group, using the centrifuge container shown in FIG. 7 .
[0021] FIG. 9 is a longitudinal sectional view showing a second modification of the centrifuge container shown in FIG. 1 .
[0022] FIG. 10 is a longitudinal sectional view showing a third modification of the centrifuge container shown in FIG. 1 .
DESCRIPTION OF EMBODIMENTS
[0023] A centrifuge container 1 according to an embodiment of the present invention will be described below with reference to FIGS. 1 to 6 .
[0024] As shown in FIGS. 1 to 6 , the centrifuge container 1 according to this embodiment is provided with a cylindrical container main body 2 which is closed at one end forming a bottom portion 2 a , a fluid introduction tube (suspension supply tube, washing-fluid discharge tube) 3 that introduces a cell suspension A ( FIG. 2 ) and a washing fluid B ( FIG. 5 ) to the container main body 2 , a supernatant suction tube 4 that suctions a supernatant C ( FIG. 3 ) centrifuged in the container main body 2 , and a cell suction tube 5 that suctions a cell suspension A′ ( FIG. 6 ) that contains a cell group D ( FIG. 3 ) centrifuged in the container main body 2 .
[0025] The container main body 2 is formed into a substantially cylindrical shape and has an opening 2 b at one end and the bottom portion 2 a at the other end, which is closed. The bottom portion 2 a is formed into a tapered inner-surface shape, whose diameter is gradually reduced toward the tip.
[0026] The container main body 2 is sealed when the opening 2 b is closed by means of a lid member 6 .
[0027] The fluid introduction tube 3 , the supernatant suction tube 4 , and the cell suction tube 5 are fixed in the lid member 6 , the tubes passing through the center thereof and the tips of the tubes being disposed in the container main body 2 .
[0028] As shown in FIG. 3 , the fluid introduction tube 3 has a tip opening 3 a disposed at the supernatant C side with respect to an interfacial surface E between the cell group D and the supernatant C, which are centrifuged in the container main body 2 . The tip opening 3 a opens toward the bottom portion 2 a of the container main body 2 so as to discharge the supplied cell suspension A and washing fluid B toward the bottom portion 2 a of the container main body 2 .
[0029] The supernatant suction tube 4 has a tip opening 4 a that opens radially outward at substantially the same position as the tip opening 3 a of the fluid introduction tube 3 . Thus, when the supernatant C in the container main body 2 is suctioned from the tip opening 4 a , the supernatant C is radially suctioned from the tip opening 4 a , disposed at the supernatant C side with respect to the interfacial surface E between the cell group D and the supernatant C.
[0030] The cell suction tube 5 has a tip opening 5 a disposed at a position close to the bottom portion 2 a of the container main body 2 . Thus, all the cell suspension A′ containing the cell group D, accommodated in the container main body 2 , can be suctioned to the outside of the container main body 2 .
[0031] Pumps (not shown) are connected to the fluid introduction tube 3 , the supernatant suction tube 4 , and the cell suction tube 5 , which are connected to the container main body 2 , such that the fluids A, B, C, and A′ therein can be transferred.
[0032] The operation of the thus-configured centrifuge container 1 according to this embodiment will be described below.
[0033] In order to separately recover the desired cell group D from the cell suspension A by using the centrifuge container 1 of this embodiment, the centrifuge container 1 is set in a centrifuge separator (not shown), and, as shown in FIG. 2 , the cell suspension A is externally supplied to the container main body 2 through the fluid introduction tube 3 . In this state, the centrifuge separator is operated to rotate the centrifuge container 1 .
[0034] The centrifuge container 1 is rotated with the bottom portion 2 a of the container main body 2 being directed radially outward, thereby centrifugalizing the cell suspension A accommodated in the container main body 2 . Thus, various components contained in the cell suspension A are centrifuged according to the differences in their specific gravities, as shown in FIG. 3 .
[0035] Specifically, since the bottom portion 2 a of the container main body 2 is formed into the tapered inner-surface shape, the cell group D, with a higher specific gravity, contained in the cell suspension A is collected at the tip of the bottom portion 2 a along the tapered inner surface. Thus, the cell group D sinks to the tip of the bottom portion 2 a of the container main body 2 , thereby being separated from the rest of the supernatant C.
[0036] In this state, the centrifuge separator is stopped, and the centrifuge container 1 is disposed such that the bottom portion 2 a of the container main body 2 is directed vertically downward. Then, as shown in FIG. 4 , the supernatant C in the container main body 2 is suctioned through the supernatant suction tube 4 . Since the tip opening 4 a of the supernatant suction tube 4 is directed radially outward, the ambient supernatant C is suctioned radially inward. Thus, only the supernatant C can be suctioned while avoiding a disadvantage that the cell group D located in the bottom portion 2 a of the container main body 2 is suctioned.
[0037] Next, as shown in FIG. 5 , the washing fluid B is supplied to the container main body 2 through the fluid introduction tube 3 . Since the tip opening 3 a of the fluid introduction tube 3 is disposed at the supernatant C side with respect to the interfacial surface E between the supernatant C and the cell group D and is directed toward the bottom portion 2 a of the container main body 2 , the supplied washing fluid B is blown out toward the cell group D located in the bottom portion 2 a of the container main body 2 . Thus, even when the cell group D becomes solidified like a pellet, when the washing fluid B is blown out, the cell group D can be unsolidified and resuspended in the washing fluid B.
[0038] Specifically, during the centrifugation, some of unwanted components, such as proteolytic enzyme and fat, are incorporated into the cell group D, which is moved to the bottom portion 2 a side of the container main body 2 according to the specific gravity, thereby forming a pellet that is solidified together with the cell group D. However, when the washing fluid B is blown out to unsolidify the pellet-like cell group D, the incorporated unwanted components can be released.
[0039] The centrifuge container 1 in which the cell suspension A resuspended in this way is accommodated is rotated again through the operation of the centrifuge separator, to execute centrifugation. Thus, the cell group D in which the fraction of unwanted components has been reduced can be separated. Then, after the supernatant C is removed with suction similarly to the above-described manner, a small amount of washing fluid B is supplied to the container main body 2 through the fluid introduction tube 3 .
[0040] As a result, the washing fluid B is again blown out to the cell group D, thus forming a cell suspension A′ in which the pellet-like cell group D is unsolidified and resuspended. In this state, as shown in FIG. 6 , the cell suspension A′ accommodated in the container main body 2 is suctioned through the cell suction tube 5 . Since the tip opening 5 a of the cell suction tube 5 is disposed close to the bottom portion 2 a of the container main body 2 , all of the cell suspension A′ in the container main body 2 is recovered by suction.
[0041] In this way, according to the centrifuge container 1 of this embodiment, the washing fluid B can be discharged so as to be blown out to the cell group D, and, even when the cell group D separated through the centrifugation is solidified like a pellet, it is possible to unsolidify the cell group D to remove unwanted components and to easily perform suction for recovery.
[0042] Note that, in this embodiment, the supernatant suction tube 4 and the fluid introduction tube 3 are formed by separate piping; however, instead of this, as shown in FIG. 7 , they may be structured by a common path 7 in which a valve 8 is provided for switching between the suction of the supernatant C and the discharge of the fluids A and B.
[0043] In the example shown in FIG. 7 , a tip opening 7 a of the common path 7 , which is concentrically disposed radially outward from the cell suction tube 5 , is disposed at the supernatant C side with respect to the interfacial surface E between the centrifuged supernatant C and cell group D, and the valve 8 formed of a valving element made of an elastic member is disposed on the tip opening 7 a.
[0044] Tip openings 7 b used for suctioning the supernatant C are radially formed so as to pass through the outer wall of the common path 7 . Furthermore, the tip opening 7 a , used for discharging the cell suspension A and the washing fluid B, is formed at the end of the common path 7 in the direction of the axis and is a gap between the common path 7 and the cell suction tube 5 facing in the direction toward the bottom portion 2 a of the container main body 2 .
[0045] As shown in FIGS. 8A to 8D , the valve 8 is formed into a ring-plate shape, the outer-circumferential edge thereof is secured on the end surface of the common path 7 , and the inner-circumferential edge thereof can be displaced in the axial direction. Furthermore, a step portion 5 b against which the inner-circumferential edge of the valve 8 butts is provided on the outer-circumferential surface of the cell suction tube 5 .
[0046] With this structure, when the cell suspension A or the washing fluid B is supplied through the common path 7 , as shown in FIGS. 8A and 8C , the inner-circumferential edge of the valve 8 is displaced toward the bottom portion 2 a of the container main body 2 by the pressure of the supplied fluid, thus opening the valve 8 and discharging the cell suspension A or the washing fluid B toward the bottom portion 2 a of the container main body 2 . On the other hand, when the supernatant C is suctioned, as shown in FIG. 8B , the inner-circumferential edge of the valve 8 butts against the step portion 5 b , provided on the outer-circumferential surface of the cell suction tube 5 , thus closing the valve 8 and suctioning the supernatant C radially from the tip openings 7 b . Then, as shown in FIG. 8D , the cell suspension A′ containing the cell group D is recovered with suction through the cell suction tube 5 , located at the center.
[0047] By doing so, the structure can be simplified by sharing the path.
[0048] Furthermore, as shown in FIGS. 9 and 10 , the fluid introduction tube 3 and the cell suction tube 5 may be integrally formed. FIG. 9 illustrates a case where a common path representing a combination of the fluid introduction tube 3 with the cell suction tube 5 and the supernatant suction tube 4 are arranged in parallel. FIG. 10 illustrates a case where a common path representing a combination of the fluid introduction tube 3 with the cell suction tube 5 and the common path 7 (the supernatant suction tube 4 ) are concentrically arranged. The common path representing the fluid introduction tube 3 and the cell suction tube 5 can be selectively switched by a three-way valve or check valve (not shown) between the supply of the cell suspensions A and A′ and the washing fluid B, and recovery of the cell suspension A′ containing the cell group D by suction.
[0049] Since the cell suction tube 5 needs to recover almost all the cell suspension A′ existing in the container main body 2 by suction, the tip opening 5 a thereof needs to be disposed at a position close to the bottom portion 2 a . When the washing fluid B is supplied through the common path 7 , which is integrally formed with the cell suction tube 5 , it is possible to discharge the washing fluid directly to the pellet-like cell group D, formed through centrifugation, thus unsolidifying the cell group D more effectively.
REFERENCE SIGNS LIST
[0000]
A, A′ cell suspension
B washing fluid
C supernatant
D cell group
1 centrifuge container
2 container main body
2 a bottom portion
3 fluid introduction tube (washing-fluid discharge tube, suspension supply tube)
3 a , 7 a tip opening (second opening)
4 supernatant suction tube
4 a , 7 b tip opening (first opening)
5 cell suction tube
5 a tip opening
5 b step portion
6 lid member
7 common path
8 valve | A cell suspension that contains a cell group from which unwanted components have been removed by efficiently washing the cell group is recovered. A centrifuge container ( 1 ) includes a cylindrical container main body ( 2 ) that accommodates a cell suspension and is rotated with a bottom portion ( 2 a ) being directed radially outward; a supernatant suction tube ( 4 ) that has a first opening ( 4 a ) at a position in the depth direction of the container main body ( 2 ) and that suctions a supernatant obtained by centrifuging the cell suspension, in the radial direction of the container main body ( 2 ); and a washing-fluid discharge tube ( 3 ) that have a second opening ( 3 a ) at a position in the depth direction of the container main body ( 2 ) and that discharge a washing fluid in the axial direction toward the bottom portion ( 2 a ) of the container main body ( 2 ). | 1 |
FIELD OF THE INVENTION
The present invention relates to garments for animals, and particularly to a protective garment for a dog working in a cleanroom.
BACKGROUND OF THE INVENTION
Four-legged animals, particularly dogs, have long worn simple garments to protect them from cold or wet weather. Dogs have a wide assortment of sweaters, rain jackets, hats, and boots to keep them comfortable outdoors. Dogs that work often wear distinguishing uniforms, such as the colored capes or vests worn by assistance dogs. Dogs that work in law enforcement or the military may even wear armored apparel.
Dogs that have been groomed for a show may wear some sort of coverall suit to keep them clean, such as to keep them from accidentally rubbing against a dusty surface. Containment suits to keep insecticidal dust in contact with a dog's fur for a period of time are also known.
Both types of “cleanliness” garment for a dog are typically designed with air vents to keep the dog from overheating while wearing the coverall. Thus they prevent bulk transfer of dirt or insecticide between the inside and the outside of the suit, but do not totally prevent material, especially small particles and hairs, from entering or leaving the suit.
One very specialized job that dogs can perform is to identify and locate various harmful materials, such as bacteria, molds, and allergenic chemicals. Colonies of mold, yeast, or bacteria often create chemical products of their metabolism that have an odor that is diagnostic of the type of organism. Dogs can be trained to respond to these characteristic odors and to indicate the location of the strongest source of a detected odor.
For example, a dog trained to recognize characteristic odors from molds can locate infestations that are not visible, such as on the inner surface of wallpaper or underneath floor covering in houses. Dogs can also find colonies of harmful fungi and bacteria in restaurants, hospitals, and manufacturing areas such as semiconductor fabrication cleanrooms.
Bacterial types that can be identified by their odors include E. Coli, Salmonella , and Listeria . These genera include several pathogenic species that are health hazards to animals and humans. Bacteria and fungi can also cause various types of defects and yield loss in manufacturing.
It is desirable that dogs that perform jobs in restaurants, hospitals or other health care facilities, and manufacturing areas wear distinctive garments to indicate that they are service dogs and not unauthorized pets. Such garments are preferably also protective for the dogs and for the facility.
For example, dogs typically shed hairs, dander, and other materials when they move. These are allergenic to some people and are never seen as benign when found in a restaurant meal or on a semiconductor wafer. Thus, a garment for a dog working in a facility that prepares food, provides health care, or manufactures microscopic or sterile articles would preferably envelop the dog and keep hair and dander inside.
It is desirable that a work garment for a dog be constructed somewhat like “cleanroom” garb for humans: made of lintfree fabric that does not allow passage of small particles in either direction, composed of parts that overlap sufficiently that movement does not open a gap between parts or create a “bellows” effect to puff particles out between parts of the garment, and covering substantially all of the body.
However, human cleanroom garb typically either leaves the face bare or covers the face with a paper or fabric covering that air can penetrate. In the case of extremely “clean” applications, a human cleanroom suit may contain its own air source, such that the person may be totally enclosed in an impermeable unit.
A dog that is trained to detect certain odors uses a special type of breathing that maximizes the sensitivity of the sense of smell. The dog breathes more air in and out than is generally used for simple respiration and the air is preferably not filtered or obstructed. Filtration of the atmosphere through a permeable mask can add spurious odors and obscure the directionality of a scent. Thus, a cleanroom suit for a dog would have special requirements for the design of the face covering.
A dog trained to locate odors typically detects an odor then gradually approaches the strongest source of the odor. To signal the center of the odor, the dog may point to the source of odor with a paw, sit down directly in front of it, or stand close to it and wag the tail. Thus, an odor-detecting dog typically comes close to the source of an odor, which may be a pathogen or substance that may be harmful to the dog.
It would be desirable that a work suit for a dog protect the dog from hazards the dog encounters. Although the dog's nose must be relatively free to process air, it is desirable that the nose also be protected against accidental or careless contact with harmful substances. In fact, it would be desirable that the dog's entire body, including the pads of its paws, be protected from contact with pathogens or harmful chemicals.
There is a need for an identifying garment that a dog can wear while locating characteristic odors in restaurants, hospitals, laboratories, skilled nursing facilities, and cleanrooms. There is further a need for a garment that prevents particles from being shed by the dog while in the controlled facility. There is further a need for a garment that protects the dog from contact with dangerous materials. There is further a need for a protective garment for a dog that does not impede the dog's breathing or interfere with the dog's sense of smell.
SUMMARY OF THE INVENTION
The present invention is “clean” garb for a dog that uses the sense of smell to locate harmful bacteria or fungi in controlled environments such as hospitals and cleanroom manufacturing areas. The coverall covers nearly all of the dog's body and feet while providing a clear airway to the nostrils.
The garb generally includes a body covering suit with integral booties and a hood for covering the head. The body portion includes a back zipper for entry into the suit. Elongated portions enclose each leg separately for easy walking. An elastic band secures each leg portion above the foot to form a bootie, which may include a flexible sole for walking on.
Another elongate portion surrounds the tail. An elastic band holds the tail portion firmly near the base of the tail so that wagging or waving of the tail may be clearly seen by the dog's handler.
A hood for covering the head is donned after the body portion and overlaps it in the head and neck area. An elastic band secures the hood tightly against the base of the neck. The front of the hood is transparent plastic to allow the dog to see. The transparent portion surrounds the snout and extends slightly beyond it. The end of the transparent portion is open to allow free passage of air, but the extended end of the hood prevents the dog's nose from contacting any surface.
The invention will now be described in more particular detail with respect to the accompanying drawings in which like reference numerals refer to like parts throughout.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective, partly exploded view of the dog wearing work garb of the present invention.
FIG. 2 is a top view of the work garb alone.
FIG. 3 is a top view of the dog and work garb of FIG. 1 .
FIG. 4 is a side view of the dog and work garb of FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a dog 100 wearing the work garb 10 of the present invention. Work garb 10 includes two main parts: coverall 20 for covering the body and hood 50 for covering the head.
FIG. 2 shows the parts of work garb 10 in top view. FIG. 3 is a top view of the dog of FIG. 1 . FIG. 4 is a side view of the dog of FIG. 1 .
Coverall 20 covers the dog's entire body except for the front part of the head. Body portion 40 covers dog 100 's torso and includes a long zipper 43 that selectively opens up back 42 of coverall 20 for dog 100 to don coverall 20 . Neck/head portion 44 covers dog 100 's neck and the back part of the head. Preferably, neck/head portion 44 terminates near the ears and preferably, as shown, terminates between dog 100 's ears and eyes.
Neck/head portion 44 includes a cinching means, such as elastic band 45 , for holding the edge of neck/head portion 44 snugly against the dog's head.
Coverall 20 includes a leg covering 22 for each leg. Each leg covering 22 is an elongated sleeve with a closed end. The closed end of leg covering 22 forms an integral bootie 24 for the foot. Cinching means, such as an elastic band 25 , located just above the dog's foot, holds bootie 24 in place so that dog 100 may walk easily. Alternatively, elastic band 25 may be replaced with other cinching means for holding the bootie in place, such as a strap that is tied or otherwise secured above dog 100 's foot.
Coverall 20 preferably includes a tail pouch 30 for enclosing dog 100 's tail. Tail elastic 35 secures tail pouch 30 close to dog 100 's tail about an inch or two from the base of the tail. Tail elastic 35 ensures that the tail does not slip inside coverall 20 . Because some dogs 100 are trained to indicate the location of an odor by wagging the tail, it is necessary that the tail remains within tail pouch 30 so that wagging is easily seen.
Work garb 10 also includes a hood 50 for covering dog 100 's head without interfering with dog 100 's senses of vision or smell. Hood 50 generally comprises a bonnet portion 52 and a face shield 56 .
Bonnet portion 52 is for covering the rear part of dog 100 's head and overlapping neck/head portion 44 of coverall 20 . Bonnet portion 52 includes neck elastic 55 to hold bonnet portion 52 tightly overlapped over neck/head portion 44 .
Face shield 56 is attached to bonnet portion 52 and covers the front portion of dog 100 's head. Face shield 56 is generally in the shape of a truncated cone and constructed from transparent, flexible plastic. Face shield 56 is open at the end near dog 100 's nostrils to allow for unobstructed breathing and sampling of air for odors. Face shield 56 extends slightly beyond dog 100 's snout so that dog 100 cannot touch any surface with unprotected nose 101 , lips, or tongue.
Face shield 52 is preferably constructed of sheet material that is flexible enough to form into the general shape of a truncated cone that fits fairly snugly around the dog's snout. The preferred material is also sufficiently rigid when rolled into a conical shape that it extends past dog 100 's nose 101 in a sufficiently rigid manner that dog 100 will not be able to easily dislodge or mash opening 57 and be able to contact dangerous materials with nose 101 .
Face shield 56 may be permanently attached to bonnet portion 52 , such as by adhesive or by sewing. Alternatively, face shield 56 may be detachable so that it is easily replaced if scratched or contaminated. For example, face shield 56 may be attached with snaps (not shown) that are covered by a placket.
In an alternative embodiment, not illustrated, face shield 56 comprises a transparent portion of hood 50 sufficient for dog 100 to see through. In such case, opening 57 in the distal end of hood 50 is rigidified, such as by including a plastic armature around opening 57 .
Coverall 20 and bonnet portion 52 are constructed of suitable woven, knit, or non-woven sheet material that prevents passage of particles and microorganisms. Tyvek is an example of a non-woven material that is suitable for a single wearing. Suitable fabrics woven from synthetic fibers can be used to make work garb 10 that can be laundered and re-used many times. Zipper 43 must be of a type that does not generate free particles when operated. Alternative closure means include ties, snaps, hook and loop fastener, or similar.
Dog 100 must be appropriately prepared before donning work garb 10 . Dog 100 is thoroughly brushed and bathed. After drying, dog 100 is vacuumed to remove loose hairs and dander. The vacuuming is done before entering the “gowning area” that is typically adjacent to the clean work area.
The vacuumed dog 100 then enters the gowning area. The human handler with dog 100 dons gloves before helping dog 100 don work garb 10 . Zipper 43 is fully opened and coverall 20 is spread open for dog 100 to step into. Each of dog 100 's feet goes into an appropriate leg cover 22 and the handler ensures that the foot is fully engaged into bootie 24 , with elastic 25 disposed above the foot. Dog 100 's tail is similarly placed into tail pouch 30 . Then zipper 43 is closed and neck/head elastic 45 is smoothed in front of dog 100 's ears.
Hood 50 is then pulled over dog 100 's head from the front. Dog 100 's snout goes into conical face shield 52 and neck elastic 55 is overlapped over neck/head portion 44 of coverall 20 . The handler checks that dog 100 's nostrils and lips are protected by face shield 52 and cannot touch any external surface.
This garbing process is typically performed with dog 100 and handler standing on a tacky mat so that any lint or bacteria stirred up by the process is eventually collected by the tacky mat. The human handler typically replaces the gloves with fresh ones after assisting dog 100 don work garb 10 .
While work garb 10 has been described for use by a dog 100 , it may be seen that work garb 10 can be adapted for use by a similar animal, such as a pig, without loss of the benefits of the invention.
Although particular embodiments of the invention have been illustrated and described, various changes may be made in the form, composition, construction, and arrangement of the parts herein without sacrificing any of its advantages. Therefore, it is to be understood that all matter herein is to be interpreted as illustrative and not in any limiting sense, and it is intended to cover in the appended claims such modifications as come within the true spirit and scope of the invention | Protective suit for a dog allows a dog to work in a cleanroom or other controlled environment. Suit 10 includes particle-blocking coverall 20 and hood 50 . Hood 50 includes transparent face shield 52 to cover dog's eyes and snout. Face shield 52 is open at the end to allow air and odors to reach dog's nose unimpeded. Face shield 52 extends slightly beyond dog's nostrils to prevent dog from contacting hazardous chemicals or pathogens. Coverall 20 includes fitted sleeves 22 with integral boots 24 ; also a tail pouch 30 to keep tail separate and visible. | 0 |
This is a continuation of application Ser. No. 08/129,845 filed on Sep. 30, 1993 (now abandoned).
FIELD OF THE INVENTION
The present invention relates to apparatus for screening particulate material such as wood chips in general, and in particular to bar screen apparatus having a screening deck defining a screening area, wherein the deck is formed of a series of parallel bars with spaces therebetween.
BACKGROUND OF THE INVENTION
In a common process for the manufacture of pulp for producing paper, logs are reduced to chips by chipping mechanisms, and the chips are cooked with chemicals at elevated pressures and temperature to remove lignin. The chipping mechanisms produce chips which vary considerably in size and shape. For the cooking process, which is known as digesting, it is desirable that the chips supplied have a uniform thickness in order to achieve optimum yield and quality; that is, to obtain a pulp which contains a low percentage of undigested and/or over-treated fibers. Under preferred conditions of digesting, the pulping chemicals or liquor penetrate into chips uniformly. If chips are provided which have too great a thickness, the liquor may not adequately penetrate the chips and the digester will produce chips with a core of under-digested fibers. If chips are provided which are too thin, the digester will produce chips that are overcooked and of low quality. To insure proper delignification of the chips in the production of pulp, the supply should not contain chips having an excessive thickness which will give rise to lack of adequate penetration during the digestion process, nor chips which are overly thin and may be over-treated during the digestion process.
Two types of apparatus has been provided heretofore for screening chips to separate the over-thick and under-thick chips from those within the desired thickness range. One type of screening device is a disk screen. A disk screen has a plurality of generally circular disks mounted on parallel, rotating shafts. The disks are mounted coaxially on each shaft and spaced from each other, and the disks interleave with the disks of adjacent shafts to form screening gaps between the disks of one shaft and the disks of adjacent shafts. Through proper disk spacing, the screen can be used to separate either under-size or over-size chips from a stream of chips supplied to the screen.
A second type of screening apparatus for wood chips or the like which has substantially higher industrial capacity than a disk screen is a bar screen. A bar screen has a screening deck or bed which extends substantially horizontally, thus providing a large screening area. Chips are distributed across a receiving end of the screening deck, which is formed by a series of parallel bars having a particular top shape. Relative oscillatory motion is effected between sets of bars for effecting screening and moving the chips in a forward direction.
Bar screens have also been found to be useful for separating refuse and trash as an important step in recycling such materials.
Known bar screens separate a flow of material into two streams, an accept stream and a reject stream. In many circumstances, the reject stream will be further processed. Further processing of the reject stream would be greatly aided by an ability to divide the rejected stream into oversized and grossly oversized materials.
In processing municipal waste and the like, the spacing of the screen bars may need to be adjusted from one lot of material to another. On conventional bar screens, bar spacing can require the change-out of a bar positioning and retention member.
Yet another problem associated with known bar screens is the difficulty of aligning the interleaved sets of bars so that the space between bars is even and does not vary between the front and back of the bar screen.
What is needed is an improved mechanism for clamping bar screens to bar retention members which allows their ready replacement and adjustment Further, a bar screen which separates the rejected material into oversized and grossly oversized is needed. Still further, an adjustment mechanism is needed which allows one person to adjust the spacing between the interleaved bars of the two bar racks of a bar screen.
SUMMARY OF THE INVENTION
The bar screen apparatus of this invention employs one or more of four distinct improvements in the construction of a bar screen. The first improvement consists of extending the bars of one of two sets of interleaved screen bars beyond the interleaved portion of the screen bed, thus forming a region of the screen bed which has larger openings. Thus, a stream of wood chips or the like passing over the bar screen bed will be separated into three streams, one which will pass through the interleaved sets of oscillating interleaved bars, and an oversized stream which will pass through a single set of bars of one of the screens that extends beyond the interleaved portion of the bed. Finally, a grossly over-large stream of material will exit the end of the bar screen bed.
The second improvement involves the construction of a clamping member for holding legs which extend downwardly of individual screen bars. The clamping member holds a group of bars in parallel spaced relation, so forming a grid of screening bars. Two such grids of screening bars are interleaved to form the screen bed. The improved clamping member is a steel channel which has two vertical side walls with a steeply peaked roof. Flanges on either side of the channel are bolted to a beam which imparts an oscillatory motion to the clamping member and retained screen bars. The clamping member is transverse to the length-wise direction of the bars. The bar legs extend downwardly through slots in the peaked roof. The bar legs are retained in the clamping member by transverse retaining bolts which pass through the channel sidewalls and the legs, thus retaining and clamping the bars.
A third improvement is to mount a downwardly extending bracket to the clamping member which engages with a threaded rod connected to the oscillating member. The clamping member may thus be traversed by a screw and bolt arrangement laterally along oscillating member to adjust the spacing between the bars of the displaced rack and another interleaved rack. The clamping member is fixed to the oscillating beam by bolts which extend through over-sized slots in flanges which extend from the clamping member. The clamping member may be thus rapidly positioned without the need to actually remove the fasteners during positioning.
A fourth improvement which may be applied to a bar screen, particularly one used to separate municipal waste, is to form the clamping member as a single vertical plate with a horizontal slot therein which defines a keyway. The bar legs are formed with projecting keys which mate with the keyway formed in the clamping member plate. Two bolts pass through the projecting key on each bar leg and join a backing bar having two threaded holes to the keyed bar leg. Thus, the individual bars forming the screen may be conveniently laterally adjusted to readily adapt the bar screen to a particular type of material to be sorted.
It is an object of the present invention to provide a bar screen which separates material into three streams.
It is also an object of the present invention to provide a bar screen which may be readily aligned by a single person.
It is another object of the present invention to provide a bar screen in which the spacing between bars may be readily adjusted.
It is a further object of the present invention to provide a bar screen which prevents the build-up of material on the clamping member.
It is yet another object of the present invention to provide a bar screen having a clamping member which releasably engages and holds the bars forming the screen.
Further objects, features, and advantages of the invention will be apparent from the following detailed description when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a somewhat schematic, isometric view of the improved bar green of this invention.
FIG. 2 is a fragmentary, partly exploded isometric view of an alternative embodiment bar green of this invention.
FIG. 3 is a cross-sectional view of the clamping member of the apparatus of FIG. 2 taken along section line 3--3.
FIG. 4 is a cross-sectional view of another alternative embodiment clamping member and bar leg arrangement of FIG. 5 taken along section line 4--4.
FIG. 5 is a fragmentary, partly exploded isometric view of the apparatus of FIG. 4.
FIG. 6 is a cross-sectional view of an alternative embodiment green having green bar legs which are clamped between the walls of the clamping member channel.
FIG. 7 is a cross-sectional view of the apparatus of FIG. 6 taken along section line 7--7.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring more particularly to FIGS. 1--7, wherein like numbers refer to similar parts, a bar screen 20 is shown in FIG. 1. The bar screen 20 consists of a first rack 22 and a second rack 24. The first rack is made up out of a multiplicity of first screening bars 26. The second rack 24 is constructed of a multiplicity of second screening bars 28.
The first bars 26 of the first rack 22 have legs 27 which are held in spaced relation by two first clamping members 30. The bars 28 of the second rack 24 have legs 29 and are held in spaced parallel relation by two second clamping members 32. Each clamping member is connected to an oscillating beam 38. The first bars 26 and the second bars 28 are interleaved or interdigitated, and are so spaced that there are gaps 34 between the first bars 26 and the second bars 28. The gaps 34 form the openings for wood chips (not shown), municipal waste (not shown), or the like, of a predetermined size to pass through the screen bed 36. The screen bars 26, 28 are mounted by the depending legs 27, 29 to the clamping members 30,32.
The oscillating beams are rotatively mounted on shafts 40 which are eccentrically driven by eccentric shafts 42. The motion of the eccentric shafts 42 causes the oscillating beams 38 to move up and down, as well in the direction of chip flow. The beams 38 to which the first bars 26 of the first rack 22 are mounted are 180 degrees out of phase with the beams 38 to which the bars 28 of the second rack 24 are mounted.
The bar screen differs from an ordinary screen in that it can separate a granular material such as wood chips based on a single dimension, chip thickness. This is critical in the pulping of wood chips, as it is the smallest dimension, the thickness of the chips, which governs the rate of digestion of the chip by a pulping liquor which dissolves the lignin in order to release the wood fibers in the chips. This ability to separate based on a single dimension of a material has also been found to have great utility in separating municipal waste into different streams of material which are recycled by different processes.
The bar screen 20 separates material into two categories, that which passes through the bar screen, and that which progresses over the screen bed 36. If separation into more categories is needed, two or more bar screens can be used. However, in many circumstances, where the cost of another bar screen is not justified, it is still desirable to separate the rejected stream into materials which are grossly over-sized versus those which, while too big to pass the screen bed 36, are only slightly too large.
An example of this is in the paper making industry, wherein chips passing the screen bed 36 would be sent directly to a wood chip digester, and wherein grossly over-sized materials would be discarded. Middling chips, which are not grossly over-sized, can be further processed in a slicer or chip destructuring device which cracks the chips by passing them through the nip of two opposed rollers.
Referring to FIG. 2, a bar screen 45 is shown in which the first set of screen bars 26 have been extended with sloped extensions 43 which cream a short extension screen bed 44 with wider spacing between first bars 26, because they are not interleaved in the extension screen bed with the bars 28 of the second rack 24. The extensions 43 extend beyond the bars of the second rack at an angle of between ten degrees and thirty degrees with respect to the plane of the bars of the second rack.
Although the extension bed 44 is shown formed by the bars 26 of a single rack 22, the extension bed 44 could be formed by extending every other bar of both racks 22, 24, or every third bar, etc.
Alternatively, all the bars could be extended for a short distance with the extended portions formed to have a narrower width, such that the gaps 34 are increased in width.
As best shown in FIGS. 2 and 3, the clamping member 30 has a channel 46 having a cross-section shaped like a peaked roof house. The channel 46 has two vertical sidewalls 52, and a peak 48 formed at the meeting of two sloping roof sides 50 which extend upwardly from the sidewalls. The sidewalls 52 of the channel 46 are joined to an inside flange 54 and outside flange 56. Slots 58 are formed in the channel 46 which extend transversely across the roof sides 50 and the roof peak 48 between the side walls 52.
The screen bar support legs 27 extend downwardly into the slots 58 between the sidewalls 52 of the clamping member channel 46. The legs 27 are connected to the channel 46 by bolts 60 with end nuts 62 which pass through holes 64 in the legs 27.
The peaked-house cross-section channel 46 imparts two advantages over known clamping members which have shed-like cross-sections with a single pitch, more gently sloped roof. The first advantage is that the steeply sloped roof sides 50 and the peak 48 tend to readily shed wood chips or other screened materials, preventing a build-up of such materials on the clamping member 30. The other advantage is that the peaked roof cross-section 46, and particularly the roof peak 48, renders the sides 52 sufficiently hingedly connected so that they may be drawn together by the bolts 60 and nuts 62, thus clamping the screen bar legs 27 between the sides 52 of the clamping member 30. This clamping action prevents wear between the leg 27 and the bolt 60.
An alternative bar screen 104 is shown in FIGS. 6 and 7. The bar screen 104 has legs 106 which are not sufficiently thick for a bolt hole to be formed therein. Bolts 108 extend through bolt holes 110 in the channel 112 side walls 114 and positions intermediate between slots in the channel. The bolts 108 thus extend between adjacent legs 106 and clamp the two side walls 114 toward one another, clamping the leg 106 therebetween. The clamping action alone is relied on to hold the legs 108 (and thus their supported bars) in place on the clamping member 116.
The peaked channel 46 also facilitates the resilient mounting of the bar legs 27 inasmuch as the insides 66 of the sidewalls 52 could be lined with a resilient material such as rubber for gripping the legs 27 with damping effect.
As shown in FIG. 3, because the sides 52 may be moved inwardly relative to each other, the bolt holes 66 on the flange 56 are over-sized, to allow for this motion. The bolt holes 66 in the outside flange 56 and the bolt hole 68 in the inside flange 54 are also oblong, as shown in FIG. 2. The oblong bolt holes 66, 68 facilitate the positioning of the clamping member 30 by a lateral adjustment mechanism 70.
The lateral adjustment mechanism 70 has a positioning bracket 72 which is rigidly attached to the clamping member 30 at the outside flange 56. The positioning bracket 72 is formed of a downwardly sloping side plate 74 which is connected to two vertical end plates 76. The positioning bracket 72 and connected clamping member 30 rides on the top surface 77 of the oscillating beam 38. The top surface 77 is generally planar, and may be formed as a portion of an inverted U-channel welded integrally to the oscillating beam 38. Due to the oblong shape of the bolt holes 66, 68 in the clamping member channel 46, the clamping member may be repositioned with respect to the oscillating beam 38 by simply loosening the bolts 84 to allow play, but without the need to remove the bolts 84.
Two ears 78 extend outwardly from the oscillating beam 38 on either side of the positioning bracket 72. A threaded rod 80 extends through the ears 78 and the side plates 74 of the positioning bracket. Nuts 82 are threadedly mounted on the threaded rod 80 and positioned on either side of the ears 76 and the positioning bracket 72. The nuts 82 may be positioned to adjust the position of the sliding bracket 72 and the connected clamping member 30 with respect to the oscillating beam 38. The adjustment mechanism 70 allows one person with a wrench to position the clamping member 30 with respect to the oscillating beam 28. By employing a lateral adjustment mechanism 70 on each oscillating beam of a bar screen assembly, the bars of the first rack may be aligned with the bars of the second rack. The adjustment mechanism 70 may also be used to make sure that the bar gaps 34 on either side of the bars 26 are uniform, so that the bar screen will separate wood chips and the like of a uniform size.
Once the clamping member 30 has been positioned by the lateral adjustment mechanism 70, the clamping member bolts 84 may then be tightened to clamp the flanges 54, 56 of the clamping member 30 to the oscillating beam 38. In some circumstances, it may be desirable to replace the clamping bolts 84 in the inside flange 54 with simple pins.
In using a bar screen to separate wood chips, the desired screen spacing will only be infrequently changed, and this change can be accommodated by replacing the clamping member 30 with a clamping member with more narrowly or widely spaced slots However, in some applications, particularly in separating municipal waste, adjustments in the spacing between the bars of a bar screen may be required more frequently, either because the waste stream is changing in content, or because of the necessity of varying the bar spacing to find the optimal spacing for separating various components of municipal waste.
An alternative bar screen 85 with adjustable spacing between the bars within each rack is shown in FIGS. 4 and 5. The bar screen 85 has an adjustable bar leg clamping assembly 86 which facilitates spacing screening bars 88 in a readily adjustable manner. The screening bars 88 are connected such as by welding to upright adjustable legs 94. The clamping member is formed as single upright plate 90 with portions defining a transverse keyway 92. The keyway 92 is a horizontally extending slot with an upper slot surface 93 which faces a parallel lower slot surface 95. Each leg 94 extends perpendicularly to the attached bar 88 and is thus significantly wider than the bar. A projection or key 96 is formed on each leg 94 which extends into the keyway slot 92 and which has an upper surface 97 and a lower surface 99 which are spaced apart approximately the same distance as the slot upper surface 93 is paced from the slot lower surface 95. The key 96 thus mates within the slot 92, with appropriate clearance to permit free movement of the leg 94 within the slot, but such that possible tilting of the attached bars 88 is strictly limited by the engagement of the key upper and lower surfaces with the slot upper and lower surfaces. Two bolt holes 101 extend through the leg 94 midway through the projecting key 96. Two bolts 98 pass through the leg bolt holes 191 and engage with threaded holes 103 in a rectangular backing plate 100. The legs 94 may be positioned along the plate 90 by loosening the bolts 98 and sliding the leg, bolt, backing plate assembly along the keyway 92. When the leg 96 and its supported bar 88 are properly positioned, the bolts 98 may be tightened, clamping the bar 88 into position. The key 96 interfits with the keyway 92 and prevents lateral tipping of the bars 88 in response to side loads caused by wood chips or the like passing through the bars 88. The bars 88 are joined by welding into the upwardly extending slots 102 of the legs 94.
It should be understood that the leg clamping bar arrangement 86 allows the ready adjustment of the inter-bar spacing, as well as the addition of extra bars or the removal of bars, to accommodate a desired change in inter-bar spacing.
For typical wood chip screening, bar displacements of 2 inches to 3 inches are preferred, with the rotary drives to which the bars are eccentrically connected being driven at 200 to 250 r.p.m. Too slow operation and too shallow displacements result in chip matting due to insufficient agitation and insufficient chip tipping. Excessive speeds of the drive cause the chips, and particularly smaller acceptable chips, to become suspended above the screen, limiting engagement time for proper sizing.
It should be noted that one or more of the improved features described above may be utilized in a particular bar screen. For example, the peaked roofed clamping member channel may be employed as in the bar screen 20 FIG. 1 without employing the lateral adjusting mechanism 70.
It should be understood that at least one grid or set of bars may be provided with separate groups of bars having top surfaces disposed in at least two different planes. In such an arrangement, each grid of bars is provided with groups of bars having top surfaces in at least two different planes. That is, the top surfaces of the bars in any given grid do not form a single planar surface. The bars are so arranged that within a given grid or set of bars, adjacent bars are at a different height, and in the assembled bed adjacent bars are from different grids.
It should be understood that the invention is not confined to the particular construction and arrangement of parts herein illustrated and described, but embraces such modified forms thereof as some within the scope of the following claims. | The bars of one of two sets of interleaved screen bars is extended beyond the interleaved portion of the screen bed, thus forming a region of the screen bed which has screens particles of intermediate dimensions. A second improvement is a clamping member which holds the downwardly extending legs of individual bars of the screen. The clamping member is a steel channel which has a steeply peaked roof between legs which sheds particles. The bar legs fit into slots which penetrate the peaked roof transverse to the lengthwise direction of the channel. The legs are retained by transverse bolts which pass through the vertical sidewalls of the channel and the legs, retaining and clamping them. The third improvement mounts the clamping member to a flange which may be traversed by a screw and bolt arrangement such that the clamping member may be adjusted in its lateral position. A fourth improvement is a clamping member which extends longitudinally and which has a keyway formed therein. Bars with downwardly extending legs extend transversely to the direction of the clamping member. The legs have transverse keys which fit into the keyway formed in the clamping member. | 1 |
BACKGROUND OF THE INVENTION
I. Field of the Invention
The present invention relates generally to auxiliary or tag load supporting axles for wheeled vehicles of the utility, load-hauling type which can be selectively deployed into ground-engaging, load supporting disposition or retracted to an elevated or stowed position. The present invention is more specifically directed to an improved mounting and pivoting system for such auxiliary axle systems which is particularly adapted to be attached to the rear of a transit concrete mixing truck.
II. Related Art
Transit concrete mixing trucks typically include a cab for the operator and a rotatable drum behind the cab for containing and mixing of concrete ingredients. Such trucks further typically include a single set of forward steering wheels and a plurality of rear, load supporting drive axles carrying dual wheel arrangements all mounted on an elongated continuous chassis. For additional support, particularly in transit when the drum is substantially full, a mixing truck can benefit by having a pivotally mounted auxiliary axle able to operate between a raised position wherein it is carried by the truck and a lowered or deployed position wherein the auxiliary axle and its wheels share the truck's load with the permanent steering and drive wheel system.
Not only does the auxiliary or tag axle system assist in balancing the load carried by the transit cement truck when the drum is fully loaded, it may enable the cement truck to carry a higher total payload than would otherwise be permitted. This is because weight restrictions placed on vehicles traveling over highways by states and/or the federal government to prevent undue deterioration of highways and road surfaces are typically measured in terms of load per axle in combination with overall spacing between axles of a vehicle. By deploying an auxiliary or tag axle system, the number of axles as well as the spacing thereof can be temporarily increased when the truck is heavily loaded thereby enabling it to transport a higher total legal payload.
The related art is replete with numerous devices designed to achieve the foregoing end. Examples of such systems, particularly with regard to transit cement mixer vehicles, include U.S. Pat. No. 4,684,142 to Ronald E. Christenson, the inventor herein, and assigned to the same assignee as the present invention. That patent relates to a tag axle assembly and means for mounting it to a transit concrete mixing truck. The system is operable by a pair of pneumatic load springs extensible to pivot the assembly downward to operating position and a pair of pneumatic lift springs extensible to pivot the assembly upward to the raised or stowed position. The assembly includes a tag axle frame having a forward longitudinally extending stem and two rearward extending and diverging legs. The '142 system is particularly directed to improved tracking during turns and enabling adjustment to uneven terrain.
Another tag axle assembly for a work vehicle, particularly a transit cement mixing vehicle, is described in U.S. Pat. No. 4,848,783 to Ronald E. Christenson (the inventor herein) et al and assigned to the same assignee as the present invention. That invention is particularly concerned with a multi-hydraulic cylinder arrangement that enables the wheels to be raised a significantly greater distance above the ground than was previously the case. The '783 patent shows a cantilevered mounting system in FIG. 9. Because the pin is cantilever mounted, however, there is nothing to further stabilize the pin and it tends to wobble and cause undue wear of the mounting joint.
As illustrated by Brennan et al in U.S. Pat. No. 3,191,961, it is also known to mount bearing housings atop the chassis structural members or beneath the chassis structural members as shown generally in U.S. Pat. No. 3,112,100 to Prichard. These are mounted from the rear of transit concrete mixing vehicles. The spaced tag axle arms are carried by shafts or pivot pins journalled in these bearings.
Earlier devices have been satisfactory in many respects; however, one of the chronic shortcomings of many is related to the connection between the tag axle assembly and the rear of the vehicle. Many previous arrangements have experienced undue wear in connection with the pivoting points on which the tag axle assembly is mounted and about which it pivots for stowage and deployment.
It is therefore a principal object of the present invention to provide an improved articulating tag axle mounting assembly for a work vehicle.
Another object of the invention is to reduce wear in a tag axle assembly mounting system.
A further object of the invention is to provide a novel tag axle mounting assembly in which spaced sides of the assembly are pivoted each using a dual spherical bearing arrangement.
Still another object of the invention is to provide a novel tag axle mounting assembly in which the sides of the assembly are pivotally mounted each utilizing single spherical bearing arrangement in the mounting of the auxiliary axle to the truck frame.
Yet still another object of the invention is to provide a novel pivotal mounting assembly for a tag axle system wherein the tag axle system is pivotally mounted utilizing a pair of spaced elastomer filled journal bearing arrangements, one associated with each side of the system.
Still a further object of the invention is to provide a rugged, long-lasting deployable tag axle mounting assembly for a tag axle associated with a work vehicle such as a ready-mix concrete truck which either when stowed or fully extended is completely independent of and does not interfere with the chute used in unloading the vehicle.
A yet still further object of the invention is to provide an improved mounting assembly for a tag axle system for a transit concrete mixing vehicle that uses a stabilized bearing mount but does not diminish the interaxle distance.
These and other object and advantages of the invention will become apparent to those skilled in the art from the following detailed description of a plurality of embodiments, especially when considered in conjunction with the accompanying claims and drawings.
SUMMARY OF THE INVENTION
The foregoing and other objects of the invention are met by the provision of a novel auxiliary or tag axle system for a work vehicle of the class including transit cement mixer trucks which utilizes an improved pivotal mounting system that is more rugged and dependable than previous systems. It reduces associated pivot pin wear. In its preferred form, the tag axle system of the invention describes a generally rectangular shaped frame in which a pair of spaced parallel tag axle arms are connected by a pair of spaced transverse frame members which may be called an inner and an outer transverse frame member with respect to the distance from the pivot mount. The outer transverse frame member extends beyond the pair of spaced tag axle arms in both directions and carries a pair of spaced tag axle wheels mounted to the ends thereof using steerable king pin arrangements which are joined and aligned by a common tag axle steering linkage member. The spaced tag axle arms extend beyond the inner transverse frame member and are mounted on and journalled for rotation about a pair of spaced journal mounting assembles carried in openings in spaced longitudinal truck frame or chassis members. The tag axle assembly pivots about the pair of journal mounting assemblies during deployment and retraction or stowing and when the system is in the deployed truck supporting position, all the support forces and associated jars, and the like are transmitted through these pivotal joints.
The improved mounting joints of the invention may take any of several forms. In one embodiment, each of the spaced tag axle arms is provided with an end housing having a transverse opening. A pivot pin is mounted through the opening in the end housing of the arm and is journalled in a single spherical pivot bearing provided in a bearing housing carried in a mounting opening in each associated chassis structural member. Each pivot pin is further stabilized by being extended through and retained in an inner housing member or stabilizing member fixed to the inner transverse frame member spaced from and beyond the chassis member.
In an alternate embodiment, a dual pivot bearing arrangement is used to carry each of the spaced tag axle arms. Each arm is provided with an end bearing housing (outer) carrying an outer spherical bearing in which, at mounting, a tag axle pivot pin is journalled. An inner bearing housing or stabilizing member fixed to the inner transverse frame member is spaced inside each tag axle arm and carries a spherical bearing in which the inner end of the tag axle pivot pin is journalled. Each pivot pin extends through a pivot pin mounting housing welded to and traversing an opening in the main frame member which is located between the inner and outer bearing housings upon mounting. The central portion of the pivot pin is fixed to the mounting housing in the main chassis frame member as by a set screw, keying system or the like. Each arm of the tag axle system then is free to pivot vertically about a pair of spaced spherical bearings.
In still another embodiment, a journal bearing arrangement is associated with the mounting and pivoting of each of the spaced tag axle arms. In this embodiment, each tag axle arm is associated with a pivot pin mounted through an end housing in the axle arm, a truck frame or chassis longitudinal member and an inner housing member fixed to the inner transverse cross member beyond which it is retained. This portion of the arrangement is in the manner of the single spherical bearing arrangement. Instead of using a spherical bearing for a pivotal mounting between the truck frame or chassis member and the pivot pin, however, the bearing housing welded in the opening in the truck frame member is provided with a journal bearing system which employs concentric inner and outer tubular sleeves spaced by and fixed to a layer of an elastomer material therebetween in a sandwich construction. The pivot pin is mounted through the inner sleeve which acts as a journal or bushing type bearing which allows the tag axle pivot pin to rotate freely. A retainer bolt or cotter pin may be used to retain the tag axle pivot pin in the assembled state. Preferred elastomer materials include neoprene, polyurethane and polysiloxanes (silicon rubbers).
Any of the illustrated embodiments provide a sturdy mount for the tag axle system susceptible of a long life of trouble-free operation. The use of spherical bearings allows a certain degree of lateral pivotal adjustment in addition to straight vertical plane pivoting to further reduce wear on the system and particularly on the pivot pin. The steerable nature of the auxiliary tag wheels further alleviates stresses associated with sharp turns or in traversing rugged terrain. The open rectangular nature of the tag frame allows it to easily clear the concrete discharge chute when raised. Note that lower pivot point (through channel) mounting allows the tag axle to extend a greater distance beyond the rear of the truck thereby increasing axle span.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings, wherein like numerals are used to designate like parts throughout the same:
FIG. 1 is a side view of a transit concrete mixer vehicle with the tag axle system shown in the deployed or ground-engaging position;
FIG. 2 is an enlarged partial side view of the concrete mixer vehicle of FIG. 1 that focuses on the tag axle area;
FIG. 3 is a view from behind the tag axle of the invention with the axle in the raised or stowed position;
FIG. 4 is an enlarged fragmentary detail view of a single bearing embodiment of the mounting system of the invention;
FIG. 5 is an enlarged fragmentary detail view of an alternate embodiment using a dual pivot bearing system; and
FIG. 6 is an enlarged fragmentary detail view of another embodiment using an elastomer supported journal sleeve or bushing-type bearing.
DETAILED DESCRIPTION
The present invention contemplates an auxiliary or tag axle system that is especially useful to provide additional support to the aft section of the chassis or frame of a transit concrete mixing vehicle that provides additional balance and support for a fully loaded vehicle especially during over the road travel. The system of mounting the auxiliary axle contains the invention and several embodiments implementing the invention are shown and described. These are meant to be exemplary rather than limiting with respect to others that may occur to those skilled in the art.
FIG. 1 depicts a transit concrete mixing truck of the stretch variety 10 that includes a forward cab 12 and a rotatable mixing drum 14 mounted on a heavy truck chassis 16 and spaced behind the cab. The mixing drum is provided with a loading hopper 18 that facilitates the loading of cement, water and aggregate into the drum through an opening in the upper rear of the drum 14. mixed concrete is discharged through the rearward opening by reversing the rotation of the drum, the concrete placement being guided by a compound cylinder-operated chute system at 20. An access ladder 22 is provided to assist the operator in inspecting and cleaning the drum. The drum rotating mechanism is shown generally by 24 and an inspection hatch cover is depicted at 26.
The cab 12 and mixing drum 14 are supported by the chassis 16 which is, in turn, carried by a plurality of axle mounted wheels including a forward steering axle having a pair of wheels one of which is shown at 28 and a pair of load supporting axles 29 (FIG. 3) carrying sets of dual wheels as shown at 30 and 30a. The truck chassis or frame includes a pair of heavy spaced longitudinal structural members, normally channel shapes, such as depicted at 32 and 32a.
The tag axle of the invention is depicted generally by the reference numeral 34 and also with particular reference to FIGS. 2 and 3 includes spaced tag wheels 36 and 36a mounted on stub axles 38 and 38a which, in turn, are freely steerably connected by king pins 40 and 40a to a common tag axle outer transverse frame member 42. A common tie rod 44 of a tag axle steering linkage maintains alignment of the tag wheels 36 and 36a.
The frame of the tag axle system of the invention also includes a pair of spaced tag axle arms 46 and 46a, each connected at one end to the outer frame member 42 and spanned near the other end by an inner transverse frame member 48, normally a heavy tubular member. Pivotal mounting assemblies generally at 50 and 50a pivotally connect tag axle arms 46 and 46a to the longitudinal chassis members 32 and 32a as will be described.
The tag axle system is deployed and stowed using a tag axle cylinder mounting lever 52 fixed to the tubular member 48 and operated by a fluid cylinder which is partially shown at 53. The cylinder is attached by a tag axle cylinder pivot mount as at 54 (FIGS. 1 and 2). A tag axle fender is depicted at 56.
Of course, FIGS. 1 and 2 show the tag axle assembly in its deployed or ground-engaging position while FIG. 3 is a rear view of the system in a raised or stowed orientation. Although not specifically shown in the Figures, the open frame construction enables the tag axle system to be stowed over and substantially in front of the movable discharge chute 60 of the chute system 20. Locating the tag wheels at a relatively long span behind the dual wheels 30 enhances the support and interaxle distance provided.
Of particular significance with respect to the invention are the mounting assemblies 50, 50a. These assemblies must carry all of the truck supporting forces yet allow easy vertical pivoting of the tag axle system for deployment or return to a stowed location. As described above, one prior system included bearings journalled in the spaced rails or channels with the tag axle arms cantilever mounted on pivot pins extending through each frame channel. The tag axle system was pivoted and rode on the pivot pins. However, the cantilevered pins tended to wobble and wear and became loose in the mount.
The improved mounts of the invention add stability and strength to bearing assemblies in a manner that greatly reduces wear. These will be discussed in conjunction with FIGS. 4-6. Each of the FIGS. 4-6 depict one embodiment of an assembly as at 50 in FIG. 3 with respect to a tag axle arm 46, it being understood that an identical mounting is symmetrically located with respect to tag axle arm 46a in an entire system.
FIG. 4 depicts a mounting assembly that includes a single spherical pivot bearing 70 mounted in a housing 72 fixed to a like opening in the truck frame channel 32. The tag axle arm 46 is provided with an end housing 74 and an inner housing or stabilizing arm 76 spaced from the arm 46 is provided fixed to a transverse frame member or cross tube 48. A tag axle pivot pin 78 is inserted through a matching machined opening in the end housing 74 and extended through the spherical pivot bearing 70 and through aligned matching machined opening 82 in inner housing 76 where it is fixed in place as by retaining ring 84 with bolt holes as at 86 and a retainer bolt with nut 90 which nests in a hole 92 in the pivot pin 78. Pivot pin 78 is freely rotatable in spherical bearing 70 to allow free pivoting of the tag arm 46 and the system is stabilized by the spaced inner housing or stabilizing arm 76. The slight amount of lateral and angular motion allowed by the spherical bearing also acts to reduce stress in the working system.
FIG. 5 illustrates an embodiment that employs a pair of spaced aligned spherical pivot bearings including an outer spherical pivot bearing 100 and an inner spherical pivot bearing 102, respectively, carried by an outer bearing housing 104 mounted on the end of tag axle arm 46 and an inner bearing housing opening 105 provided in inner arm 106. A pivot pin mounting housing 107 is fixed, as by welding, in a matching opening in the truck frame channel member 32. A pivot pin 108 is inserted through the aligned bearings 100 and 102 and is fixed with respect to mounting housing 107 as by set screw 109. Each side of the tag axle system pivots freely about the stationary pivot pin 108 using the pair of spaced bearings.
A third embodiment is shown in FIG. 6 which uses an inner arm stabilizing elastomeric supported journal or bushing-type bearing system to replace the single spherical pivot bearing in the embodiment of FIG. 4. The journalled system consists of a sandwich construction on which an outer sleeve 110 is molded into a concentric inner tube or sleeve 112 using an intermediate layer 114 of an elastomeric material such as neoprene, polyurethane or polysiloxanes. The inner tube 112 has a lubricous fit over a pivot pin 116 and when lubricated acts as a bushing type bearing similar to a babbitt metal bearing or the like. The outer tube 110 is press fit into the pivot bearing housing 72. This combination also provides a freely pivoting mounting support for the tag axle system which allows a slight amount of lateral and angular motion.
This invention has been described herein in considerable detail in order to comply with the Patent Statutes and to provide those skilled in the art with the information needed to apply the novel principles and to construct and use embodiments of the example as required. However, it is to be understood that the invention can be carried out by specifically different devices and that various modifications can be accomplished without departing from the scope of the invention itself. | A dual attachment arm auxiliary or tag axle system for a work vehicle of the class including transit concrete mixer trucks utilizes an improved pivotal mounting system that is more rugged and dependable than previous systems and reduces associated pivot mount wear. The system uses a through-the-chassis member mounting which includes a spaced stabilizing arm to provide dual attachment for each arm and to prevent problems associated with a cantilevered arrangement. The improved mounting joints may take any of several forms. The through-the-chassis member configuration maximizes the distance behind the transit concrete mixing vehicle that the tag axle extends. | 1 |
FIELD OF INVENTION
This invention relates to the field of navigation route calculation and guidance, including hand-held navigation, in-vehicle navigation, server-based navigation, and cell-phone application-related navigation.
BACKGROUND OF INVENTION
Navigation systems contain certain required basics: input/output device(s); a processing unit, a navigation calculation core; geographic database usually including streets and Points of Interest (“POIs”); and a Global Positioning System chip-set to determine position; inter alia. For automotive systems, there is additionally a gyroscopic chip that provides heading and speed information. Significant disadvantages exist with current systems. Navigation systems built into vehicles by the OEMS require expensive hardware and software, which becomes obsolete far sooner than the car in which it is installed. Additionally, the on-board geographic database requires a storage medium, such as a hard-drive, which, relatively, are more prone to failure than other electronics components, and the database must be updated periodically.
Server-based navigation systems are those in which guidance algorithm is resident on a central processing unit or server. End users input navigation destinations using a variety of devices, including mobile phones, computers, portable navigation devices, embedded vehicle systems and mobile data terminals (“MDT”). The end user request is communicated to the server wirelessly, either via a mobile phone network, a satellite network, a Wi-Fi network, or mixed network containing both wireless and wired connections. The wireless link can be interrupted in a number of circumstances (e.g., tunnels, concrete canyons in the centers of major cities, in unpopulated areas, and at times of heavy wireless usage). Depending on how the system was configured, the amount of data that needs to be transmitted often overwhelms the wireless resource. Cellphone and personal navigation are similarly limited.
In any geographic region, there are a small number of sources for the navigation database information, itself. A navigation database will provide coordinates and names for streets, as well as defining a street-type for each road (e.g., residential, commercial, highway, interstate, etc.). Often, the navigation database will also include points of interest (“POIs”), which are local business, places of civic or historic significance, schools, churches, and other places frequented by the public. In the United States, the U.S. Census Bureau offers Topologically Integrated Geographic Encoding and Referencing system data (“TIGER data”). TIGER data does not contain a complete set of navigatable streets in the U.S., nor does it provide POIs. There are multiple commercial providers of navigation databases, who provide POIs and a substantially complete set of navigatable streets. The two largest, in the United States, are Navteq® and Tele Atlas®. Unless the text is specifically contrary, the use of POIs in this patent means the general idea of points of interests, rather than any specific, discrete collection of points of interests. In Korea and Japan, the navigation databases are government controlled. Other jurisdictions range from government-owned to private services providing the navigation databases. Additional navigation and navigation database competitors are rapidly entering the market, including Apple and Google. Additionally, the crowdsourcing revolution is impacting map databases. For example, MapBox is working on an open-source collaborative map database called OpenStreetMap. In general, at this point, almost all vehicular and mobile phone navigation relies on navigation software from one source, and a complimentary navigation database from another source. Almost always, a single entity bundles and sells the navigations components as a complete solution.
Despite its limitations, the last two decades have seen a proliferation of advanced electronics aimed at navigation. Two decades ago, most vehicles had very little electronic content, and cellphone or mobile phones were in their infancy. Today, the revolution in vehicle and wireless electronics has made global-positioning based navigation ubiquitous. However, the proliferation of options for consumers has not presented an optimized overall solution, yet. Most navigation solutions rely on computational cores which are more than a decade old.
All current navigation algorithms rely on one-dimensional optimization. All streets are represented by vectors of varying length and shape. Fundamentally there are two ways the current methods represent streets. In the first, all vectors are straight line vectors. Curves are decomposed into a number of straight line segments. In the second, curves and splines of one form or another are used to mimic the natural curvature of the roads.
In order to find a route, current algorithms piece-wise optimize in one dimension. Many individual algorithms exist to perform one-dimensional piece-wise navigation optimization, including, but not limited to, single-sided decision tree, double-sided decision tree, single-sided decision tree with gates, double-sided decision tree with gates, buckets, and leaky buckets. Multiple route segments are grown from either the origin or both the origin and the destination. The routes are compared with one another during the process, and a single or multiple rejection criteria are established to discard divergent solutions. Ultimately, a single route is grown between the origin and the destination, either meeting in the middle (in the case of piece-wise solutions growing from both the origin and the destination) or at the destination (in the case of piece-wise solutions growing only from the origin). Strangely enough, if the process was truly piece-wise optimizing a solution, it would be irrelevant for calculation purposes whether the algorithm started at the origin or the destination. In many algorithms, the calculation will pick different routes in a single-sided decision when the origin and destination are reversed. Some algorithms correct for this by calculating both routes and then presenting the more efficient or optimized route to the end user.
The process is facilitated by road weighting. Essentially, interstates and other highways are more highly weighted than major surface thoroughfares. Major surface roads are weighted more heavily than paved secondary roads, which, in turn, are weighted more heavily than residential streets. The weighting combines with the piece-wise, one-dimensional optimization to select a route between any origin and destination. Unfortunately, such weighting often ends up with “interstate bias.” Many users of navigation systems have noted that the systems tend to prefer interstate or highway routes, even when they are significantly detour from the straight line between the origin and destination.
The major characterization to take away about today's technology is that it creates routes using piece-wise optimization and weighting. It does not create explicit solutions, even in the relatively local area, even though modern processors and algorithms would easily allow explicit local solutions. Piece-wise optimization and weighting creates a bias towards interstate or highway travel. Such antiquated computational cores create legacy artifacts, which substantially affects the performance of today's navigation systems. These cores were written for slow processors, such as the first generation of RTOS processors. These cores assumed a much smaller volume of data than what can currently be handled (e.g., petabyte systems). These cores assumed that wireless data transfer, if any, would be at substantially slower speeds than what is currently capable.
This is not to say that companies have not been updating their software over the past twenty years. What it means is that, when a piece of core software is initially written, many limitations are inherently built-in, either through commission or omission, which makes it difficult to create an update which is truly up-to-date. Additionally, when re-envisioning their software, most software teams have unstated (often unconscious) pre-conceptions about what is possible, because they are starting from a knowledge-base that includes their legacy code.
The legacy artifacts caused by antiquated navigational cores include inaccurate estimated-time-of-arrival (“ETA”) calculations, lack of learning, inability to handle multi-vehicle/multi-destination problems with the same software that is used for normal navigation, inability to optimize the solution for multi-vehicle/multi-destination problems, the inability to reasonably assess when the user has substantially diverted from the calculated route, and the inability to pass navigation back-and-forth between devices (e.g., between an in-car unit and a cellphone).
Most navigation systems are capable of giving an ETA with a 10% error rate, or less, 80-90% of the time. Most consumers are satisfied with this because (1) they don't rely on the ETA information as their only estimate of their arrival time; (2) the ETA information is better information than what they have from other sources; and/or (3) end-users have normalized their expectations to the system performance level available. However, there are categories of users for whom the error rate is strictly unacceptable. For example, commercial vehicle drivers, commercial fleet operators, people on a tight deadline, and people living in congested areas (where current technology under-performs).
Poor ETAs are partially related to the inability of current navigation cores to learn in any meaningful sense. For example, most people know that on Monday morning (excluding holidays), Interstate 405 in Los Angeles is going to be congested at 8:00 a.m. Current navigation cores do not. Likewise, I-696 in metropolitan Detroit, I-90/94 in Chicago, I-95 in Boston, and many other major interstates in major cities are routinely congested. Travel speeds at rush hour on these roads can vary between 60 m.p.h. and 10 m.p.h., on average. Much of the variation is entirely predictable: particular times, days, and conditions are particularly bad, such as Friday afternoons and rain. Unfortunately, current navigation solutions are unable to assess this situation a priori.
Current systems attempt to mask this problem with “dynamic navigation.” Dynamic navigation usually entails using “real-time” traffic data, at an additional cost to the user, to re-route the user if there is congestion. Realistically speaking, there is nothing dynamic about dynamic navigation. Most “real-time” traffic reports have a latency of 20 minutes or more, and come from a single source. With little or no motivation to improve performance in a monopolized field, traffic data fed into dynamic navigation systems is atrophying. Moreover, routinely starting a route towards traffic congestion, only to be re-routed when the navigation system's weighting function finally calculates an actionable event from real-time traffic messaging system, creates a big issue, costs the end-user time, money, and tranquility.
Most people have learned preferred routes near their homes and businesses. These preferred routes offer the user a quicker and/or more convenient route. If a user continually traverses a preferred route, current navigation cores are incapable of incorporating the data in a meaningful way.
There are some solutions on the market that attempt to mask this inadequacy, by “learning” a preferred route. However, the way these systems work, the user has to travel between point A and point B. With repetition, the system will learn preferred sub-routes on which to guide the user between point A and point B. However, the systems are unable to generalize this information in a way which is useful to the end user. Most users would find dubious value in a system that will tell them the route they should take, after they have taken that route three or four times. What users desire is a way to take information, such as the avoidance of traffic control devices, particular ways into or out of business parks, shopping centers and residential sub-divisions, and generalize the information to all other route guidance performed by the unit.
The commercially available navigation software cores all have issues when it comes to reasonably re-routing people. In most systems, any divergence from the calculated route will cause the system to re-calculate a solution, which will essentially get the user back onto the originally calculated route. These re-calculations usually entail back-tracking, zigzagging, or returning the user, immediately, to the original route. There is no provision possible for small divergences from the proposed route, seamlessly re-introducing the user into the originally propose route at a reasonable distance.
Current navigation systems also lack interoperability. An end-user may have one system in their car, one on their laptop, and one on their cellphone. However, with few exceptions, little data can be passed from one to another. Additionally, it is impossible to start a navigation on a cellphone, enter into a vehicle, and have the vehicle's navigation system provide the navigation calculated on the cellphone.
SUMMARY OF THE INVENTION
Like most navigation systems, this one includes input/output devices with user interfaces, a method for geo-locating (e.g., a GPS antennae and chip-set), a server-based navigation database, end-user processor(s) and memory, server-based processor(s) and memory, a wireless method for communicating between the end-user and server, and a navigation software core.
Like many systems, the user will input a destination, using either POIs, an address, or memory. The origin is assumed to be the current location of the user, unless some other point is specified. The user may specify shortest time, shortest distance, user defined cost functions (such as least gas), or exclusions (e.g., no interstates or no toll roads). To get from the origin to the destination, the invention will calculate a navigation solution.
It is possible, on the surface of the Earth, or on any abstraction representing a portion of the surface of the Earth, to create bounded geographic regions (“BGRs”) in any localized area in which a user wants the assistance of a navigation device. Within each BGR there will be a plurality of streets and points of interest (“POIs”). On the periphery of the BGR, there will be nodes, representing the intersection of streets with the boundaries of the BGR.
When navigating within a BGR, there are only four possibilities: (1) the user enters the BGR at one node, and exits the BGR through another node; (2) the user originates a trip within the BGR and exits the BGR through a node; (3) the user enters the BGR through a node and the destination resides within the BGR; or (4) the origin and destination both reside within the BGR. In case 2, the origin will be treated as a node for calculation purposes. In case 3, the destination will be treated as a node for calculation purposes. In case 4, both the origin and destination will be treated as a node for calculation purposes. Therefore, in every BGR, it is possible to identify a finite number of Node Pairs, representing the total possible solution set for traversing the BGR. Additionally, BGRs are sized so that a quick, explicit solution is possible for every Node Pair.
This invention will optimize some user-defined dependent variable for the end user: (1) time; (2) distance; (3) fuel; (4) cost; or (5) other commercially-valuable, user-defined dependent variable. The invention will do this by creating an estimating function, which can be used to provide a value for each Node Pair. The estimating function will use weighting factors, based on the road-type from the navigation database, as well as historical data, to create the value for each Node Pair.
The navigation software core will identify a finite numbers of BGRs, which will be in reasonable geographic proximity between the origin and destination, in which to calculate solutions. By determining the value for each Node Pair for each BGR, it is possible to solve for the optimizing solution, explicitly. By creating BGRs which are small enough to that an explicit solution is possible, this system and method will allow a two-dimensional optimization for routing.
Once a solution is calculated for a Node Pair, the solution is saved in a Node Pair Look-Up Table (“NPLUT”). The NPLUT is sorted by BGR, so that at any given time, only the most local solutions are presented to the processing unit, improving speed and efficiency. The unit can compare actual performance to the calculated value for each Node Pair. Using an error function, the unit can adjust the stored solution for the Node Pair. Furthermore, the NPLUT can store both variable and attribute (digital event or flag) data, allowing for full-factorial ANOVA or MANOVA calculations, depending on the number of dependent variables of interest. The NPLUT can use factors, including, but not limited to, time of day, day of week, date, driver, driver age, location where driver learned to drive (Boston drivers always drive fast), special event occurrence (e.g., football game in proximity), construction, precipitation, temperature, etc.
Within the NPLUT, each BGR and Node Pair has a unique designator or name. Many numbering schemes are possible for both. BGRs can be ordered with an ordinal numbering scheme, a cardinal numbering scheme, an alphanumeric numbering scheme (with or without significance), or an identification scheme based on the BGR latitude and longitude. The internal numbering scheme should be focused at database and computational efficiency. The values used for the BGR ordering scheme do not need to be presented to the end user. In the event that it is advantageous to present BGR numbering or ordering to the end-user, a transform can be created to show the end-user BGRs with easy to reference designators (e.g., 1, 2, 3, etc.) This might be useful for certain fleet applications, such as vehicle for hire, where, currently, zones are used to distribute vehicles and orders.
For each node for each BGR, a unique designator needs to be assigned. A Node Pair designator would then be the unique designator for both nodes, as well as the designator for the associated BGR. To fully describe a Node Pair, one would need to identify both the BGR and the Node Pair. The node part of the Node Pair designator would be commutative to the system. In the real world, each node represents a point on a road as it passes through the boundary of a BGR. Therefore, a Node Pair designator will give two locations, either on the same road, or on different roads, which are both on the boundary of a particular BGR.
In the NPLUT, each Node Pair reference will have a value for each dependent variable (e.g., time, distance, fuel consumption, surface roads navigation, etc.). With each navigation traversing the Node Pair, the actual value will be measured or estimated. The actual value will then be stored in the NPLUT, along with independent variables related to the trip, such as age of driver, gender of driver, profession of driver, type of vehicle, age of vehicle, time of day, day of week, date, weather, etc. After each navigation, intermediate ANOVA and MANOVA values (i.e., sum, sum of squares, etc.) can be stored and associated with the Node Pair trip. In this way, when a particular user navigates, an adjusted value for each Node Pair can be presented.
The feedback used to adjust the values given for each Node Pair can be a simple least squared error calculation, an error function that more heavily favors recent events, or other commonly used control system error correction methods. Truly predictive traffic is no more than correctly identifying the dependent variable of interest, and capturing the independent variables of interest. If one does that the system will predict traffic with as much accuracy as the data and math allow.
The BGRs, Node Pairs, and independent variables can be used in ways not currently available, due to the navigation being server based. For example, if weather starts affecting traffic in Chicago, it will typically reach Detroit within a given amount of time. A simple auxiliary process can be appended to the system, which, based off of the independent variables, estimates the latency period between weather in Chicago, for example, and Detroit, and the time-dependent probability of the weather from Chicago becoming weather that affects traffic in Detroit. The system can then create ETAs for future trips based off of impending weather, or other predictable future events. The ETAs for future trips can then be periodically updated, as the correlation of the data becomes more certain.
BRIEF DESCRIPTION OF THE DRAWINGS
There are thirteen relevant drawings.
FIG. 1 is a system communication perspective drawing.
FIG. 2 is an alternative embodiment system communication perspective drawing.
FIG. 3 is an alternative embodiment system communication perspective drawing.
FIG. 4 is an alternative embodiment system communication perspective drawing.
FIG. 5 is an alternative embodiment system communication perspective drawing.
FIG. 6 is an alternative embodiment system communication perspective drawing.
FIG. 7 shows a flow chart for the high level software method embodied by the present novel system.
FIG. 8 shows a flow chart for creating BGRs through virtual tessellation in the resident server.
FIG. 9 shows an alternative method for creating BGRs in the resident server.
FIG. 10 shows a flow chart for fleet customer set-up on the resident server.
FIG. 11 shows is a flow chart of a server based navigation method using BGRs and Node Pairs.
FIG. 12 shows a flow chart for the hand-held or remote electronic device software process.
FIG. 13 shows the Earth inscribed in a tessellated cube.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following description represents the inventors' current preferred embodiment. The description is not meant to limit the invention, but rather to illustrate its general principles of operation. Examples are illustrated with the accompanying drawings.
FIG. 7 shows a high level flow chart for the software method associated with the system. Some operations are only performed on set-up of operation: 99 initial START, 26 loading map database; 62 create BGRs through sub-routine, and 56 system initialization. The map database 26 can be purchased from any map database vendor, or a crowd-sourced map database can be used. The system initialization includes such administrative routines as forming the NPLUT, populating the NPLUT with any available data, creating a user database, populating the user database with any available data, and similar tasks. Once the system has been initialized 56 and the BGRs have been created with the BGR sub 62 , the system is capable of taking navigation input 55 .
FIG. 13 shows the Earth 301 inscribed in a tessellated cube 302 . On a computer, the virtual Earth 301 can be rotated or tilted until a geographic land mass of interest is centered. Under almost all circumstances, even though the Earth 301 is an oblate spheroid, the geographic region of interest can be made to be almost parallel with a face of the inscribing cube 302 . By properly selecting the size of the tessellation on the cube 302 , one can influence the size of the BGR projected onto the Earth 301 . This method is called Virtual Tessellation, because the pattern on the Earth 301 is not technically a tessellation, because all of the BGRs will not be the same shape and size.
FIG. 8 shows a method of generating BGRs using Virtual Tessellation. First, the system inscribes the Earth in a cube 44 . The center of the cube face 45 is centered over the geographic region of interest. A starting tessellation size 46 for the face of the cube is selected. The Standard Surface Area (“SSA”) is the target surface area for the BGRs. A BGR SSA of approximately 1 sq. km seems ideal. Next, the variation limit for the SSA 64 is set. This number should be small (less than 10%). All BGRs should have a surface area very close to the SSA in order to minimize the potential for confounded data (non-orthogonal independent variables during an analysis of variance). If desired, the size of the tessellation squares 47 on the inscribing cube can be varied. Although this is computationally more difficult, it will minimize SSA variation (only the inner most piece is a square, with each proceeding layer being rectangles with higher and higher aspect ratios. The cube tessellation is projected onto the Earth 48 to create initial BGRs. The SSA of all BGRs is assessed 49 . If the SSA analysis is okay 50 , the BGRs are stored 53 , and the BGR generation process ends 59 . If the SSA analysis is not okay 50 , all the BGRs are erased 51 . Next, the system adjusts the starting tessellation size 52 , the outer layer tessellation ratio (how quickly the outer layers of the tessellated cube face become rectangles of higher and higher aspect ratio) is adjusted 63 , and adjust the SSA variation limit 64 . The whole process is then started again 47 .
FIG. 9 shows the flow chart for an alternative embodiment for generating BGRs. The process is started 58 by finding the centroid of the geographic region of interest 65 . A single BGR is created 66 with a surface area equal to the SSA and at least four sides. The SSA variation limit is set 64 . A layer of BGRs is created around the existing BGR(s), in which the new layer of BGRs has its perimeter minimized 67 . The SSA for the layer is analyzed 49 . As long as the SSA analysis is okay, additional layers of BGRs are added. If the SSA is not okay 50 , the SSA for just the last layer is analyzed 69 . If the last layer includes BGRs which overlap the border of the geographic region of interest 70 , and that is the sole cause of the unacceptable SSA, the BGRs are stored 71 . If it is not edge geography 70 , the last layer of BGRs is erased 51 . The allowable maximum perimeter will be increased by 10% from the previous iteration 68 , and a new layer of BGRs will be created 67 . The process continues until the entire geographic region of interest is covered with BGRs 72 .
In FIG. 7 , once the BGR routine 62 has occurred, Fleet Set-up 61 ( FIG. 10 ) can occur. In FIG. 10 , each customer or fleet is enrolled with a Fleet Set Up 80 . This includes populating a database with information about the Vehicles 81 , Drivers 86 , and Services Offered 91 . Data collected about Fleet Vehicles 81 includes number of vehicles 82 , types of vehicles (including fuel type) 83 , mileage of vehicles 84 , and other user defined vehicle data (independent variable or attribute data) 85 . Data collected about drivers includes name 87 , driver number or identifier 88 , employment type (employee, independent contractor, owner/operator, etc.) 89 , and other user defined driver data (independent variable or attribute data) 90 . Data collected about fleet services includes customer type 92 , service standards 93 , service area 94 , and other user defined service data (independent variable and attribute data) 95 . The database also allows user defined fueling stations 96 . Once all of the data has been defined, it is loaded into a database 97 , and the routine ends 98 .
From FIG. 7 , End User Nav Input Request 32 is received via a wireless means. FIG. 1 shows an embodiment of wireless communication and geo-location, which is necessary for navigation. The end user is in a vehicle 201 , which has a remote electronic device (“RED”), either built-in or mounted. The vehicle 201 geo-locates via a GPS chip-set, a gyro, and/or a satellite transceiver. A plurality of satellites 200 provides GPS signals to the vehicle's 201 GPS transceiver. The vehicle 201 is then able to communicate its location to a central server 203 , using a wireless network 202 . The wireless network 202 can be a cellular or mobile phone network, a radio-frequency network, or other wireless means. The transmission could also be made over a mixed means network, such as a wi-fi network that downloads and uploads requests to the server via a wired internet connection (not shown).
FIG. 2 shows an alternative embodiment for the communication and geo-location system. In FIG. 2 , the vehicle 201 has been replaced with a cellphone, MDT, or RED 204 . The cellphone, MDT, or RED 204 , geo-locates via the satellite network 200 . The cellphone, MDT, or RED 204 , communicates with the server 203 , via a wireless network 202 .
FIG. 3 shows an alternative embodiment for the communication and geo-location system in FIG. 2 . In this system, the wireless network 202 is used for both geo-location and communication with the server. The cellphone, MDT or RED 204 can use multiple cellphone towers or antennae to identify its current location. This data can be transmitted, along with a navigation request, to the remote server 203 .
FIG. 4 shows an alternative embodiment for the communication and geo-location system in FIG. 2 . In this system, satellites 200 are used for both geo-location and communication. Although GPS satellites are not currently multi-tasked for communication, it is conceivable, in the future, that both geo-location information and communication would happen with the same satellite 200 . However, this system is architected according to current satellite trends: one set of satellites 200 provides geo-location information, and another satellite 200 is used for communication to the remote server 203 .
FIG. 5 shows an alternative embodiment for the communication and geo-location system in FIG. 1 . In this system, the wireless network 202 is used for both geo-location and communication with the server. The vehicle 201 can use multiple cellphone towers or antennae to identify its current location. This data can be transmitted, along with a navigation request, to the remote server 203 .
FIG. 6 shows an alternative embodiment for the communication and geo-location system in FIG. 1 . In this system, satellites 200 are used for both geo-location and communication. One set of satellites 200 provides geo-location information, and another satellite 200 is used for communication to the remote server 203 .
In FIG. 7 , an end-user nav request 32 is communicated through one of the communication and geo-location systems in FIG. 1 through FIG. 6 . Whether a vehicle 201 or a cellphone, MDT, or RED 204 , the user interacts with the system through a user software method, generally referred to as a user application. In FIG. 12 , the User Application starts 101 by insuring that the user is registered 102 . If the user is registered 102 , destination input 128 occurs. The user can add multiple destinations 127 , 128 , either specifying the order or allowing the system to order the trip. Once input is complete 127 , the data is transmitted 129 to the remote server via the means shown in FIGS. 1-6 . At this point we will handle the remote server 203 as a black-box that produces a navigation route, given the destination input 128 . The remote server 203 transmits the route, where it is received 129 by the end user. At pre-determined intervals, the end user's application 101 will ping 130 the remote server 203 , by transmitting 126 its location. The remote server 203 will compare the user's progress versus what the remote server predicts the user's progress ought to be. If the progress towards the destination lies outside the acceptance criteria, the remote server 203 will transmit a re-route signal 125 to the user's application 101 . The end user's unit will notify the end user of the re-route, while the remote server 203 provides an alternative route. The new route will be received 126 by the end user's application 101 . Eventually, re-route or not, the end user will arrive at the destination 124 . After arriving at the destination, the end user's application 101 will transmit a final ping 123 to the remote server 203 , so that the remote server has a complete history of the trip.
When starting the end user application 101 , if the user is not registered, the unit can allow registration by opening an account 103 . After opening the account 103 , the user selects ping frequency 104 , navigation preferences 106 , and navigation exclusions 105 . The user then has to complete independent variables concerning him- or herself, and his or her vehicle. Driver information 107 includes years driving 108 , driving record 109 , miles driven per year 110 , age 111 , marital status 112 , home address 113 , where the user learned to drive 114 , the user's profession 115 , the user's gender 116 , and other company- or group-defined data 117 . The vehicle information 118 includes vehicle owner 119 , make and model 120 , model year 121 and miles on the vehicle 122 . The independent variable data should be of very high quality, because the user will be aware that their accuracy in answering the questions may directly relate to how well the system can navigate for them.
FIG. 7 shows that Guidance 60 occurs after End User Input 32 . In FIG. 11 , Guidance 60 begins by selecting nav optimizing factors 1 . Once the BGRs have been created, it is possible for the invention to create navigation solutions. FIG. 11 shows a single vehicle navigation solution. The user starts by selecting an optimizing factor 1 , or dependent variable: time, distance, fuel, cost, or an user defined dependent variable. Next, the user, if desired, excludes certain solutions from consideration 2 , such as interstates, tollways, bridges, or other potential routes. The user enters one or more destinations 3 using the input device. If inputting more than one destination, the user can select 6 an automatic 10 or manual 5 ordering of the destinations. When selecting a manual 5 ordering, the automatic destination ordering module 10 will defer to the manual entry. Once ordered, the origin and the next or only destination is identified 9 . If there is only a single destination input at the beginning 7 , the navigation core moves directly to identifying origin and destination 9 .
To calculate between an origin and destination, the invention will identify the BGRs that lie, linearly, between the origin and destination 8 , and designates them as Active. These BGRs are termed Gen 1. In the BGR containing the origin, the origin is designated the sole entry node 12 . In the BGR containing the current destination 9 , the current destination is designated as the sole exit node 13 . In all other BGRs, Node Pairs are created by selecting only those nodes which have a BGR on both sides 11 . The navigation core than creates a Node Pairs list for all Active BGRs 16 . In multi-processor systems, the navigation core will simultaneously create a temporary BGR array for all Node Pairs under consideration 20 , and survey the NPLUT 14 to see if solutions exist for any Node Pairs under consideration 17 . If the Node Pairs solution exists in the NPLUT, it is placed in the temporary BGR array 20 . If not, using weighting functions for each street classification, the invention makes dependent variable calculations for each Node Pair of each BGR 19 , capturing route information for each potential solution. The invention will delete any exclusions from the potential solution set 21 . Since only a limited set of BGRs are used for the initial calculation, not all nodes of each BGR is a potential entry and/or exit. The data generated from the nodes of interest can be stored in an array, in a temporary database format, or in any other data-handling format that allows quick access 20 . This temporary data can be stored in cache storage, on the hard-drive, or in any other type of suitable memory element. In a multi-core processor environment, such calculations are speedy, because each BGRs can be independently calculated.
The invention then creates an initial trial route by finding the initial minimum solution from the origin to the destination, travelling only through BGRs that lie, linearly, between the origin and destination 22 . As a boundary condition for the initial route calculation, the exit node of one BGR is the entry node of the adjoining BGR. By creating a matrix of possible solutions, the invention yields an explicit solution.
Once the initial trial route is identified, the solution engine adds all BGRs that were adjacent to Gen 1 BGRs 23 , 18 , and largely repeats the above process. The new BGRs are termed Gen 2. Gen 1 BGRs now use all nodes in the calculation. Gen 2 BGRs use a reduced set of nodes, because not all nodes have an adjoining BGR associated with them.
To calculate the Gen 2 trial route, the potential solutions calculated in the Gen 1 calculation are excluded, because they are found in the temporary array 20 . The invention, again, applies the boundary condition that the exit node of one BGR is the entry node of the adjoining BGR. By creating a matrix of possible unique solutions (excluding Gen 1 solutions), the invention yields an explicit solution, the Gen 2 trial route 22 .
The process is repeated for Gen 3, in much the same way as for Gen 2 23 , 18 . All BGRs adjoining Gen 2 BGRs are added to the calculation. All previously considered trial solutions are excluded from the potential solution set. An explicit solution for the Gen 3 trial route is calculated.
Call Gen A the optimum solution. The exit criteria is selected so that C generations are completed, where C=A+B, where C is the total number of generations, A is the optimum generation, and B is the number of desired divergent solutions calculated after the optimum solution. For example, if the Gen 1 trial route is preferable to the Gen 2 or Gen 3 trial route, and the calculations stop, presenting the Gen 1 trial route to the user as the preferred route, C=3, A=1, and B=2.
In practice, B is related to the distance between the origin and destination 23 . Additionally, selection of B can be optimized through a simple error feedback function, where the error is related to the distance. The upper limit of B is set by the maximum speed limit. In other words, the process ends when the vehicle would have to exceed the maximum allowable speed limit around the periphery in order to offer a more preferable solution to the dependent variable than the currently available solution. | A navigation system containing a software core, which uses bounded geographic regions (“BGRs”) and Node Pairs to explicitly optimize, in two dimensions, for user desired dependent variables, by analyzing variance due to standard and user-defined independent variables. The invention stores Node Pair data, and can use error function, feedback, and ANOVA/MANOVA to create a tightly convergent navigation solution. | 6 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application is a Continuation Application claiming benefit of PCT/EP2008/006657, filed on Aug. 13, 2008, which claims priority to German Application No. 102008030149.3, filed on Jun. 27, 2008, which applications are hereby incorporated by reference in their entirety.
TECHNICAL FIELD
The present disclosure relates to a boot with a first fastening region and to a system comprising such a boot and also a housing part.
BACKGROUND
Boots are used in particular for sealing joints, in particular in the automotive industry for sealing constant velocity sliding joints and fixed joints. However, other applications outside the automotive industry are also possible. Boots within the context of the present disclosure can take the form of rolling boots or folding boots.
Rolling boots of the aforementioned type are known from the prior art. For instance, FIG. 1 of the present application shows a section along a main axis 60 of a rolling boot according to the prior art having a first fastening region 12 intended for fastening to a joint housing and a second fastening region 14 intended for fastening to a shaft. Such a rolling boot, designated by the reference number 10 in FIG. 1 , is mounted on fixed joints, for example. The first fastening region 12 here has an outer part 34 and an inner part 36 , wherein an accumulation of material 38 in the form, for example of a peripheral annular bead is arranged in the inner part 36 so as to provide a seat in a peripheral groove on the outer lateral surface of a housing part. The first fastening region 12 is adjoined by a fold region 16 having a first fold peak region 20 with a first fold flank 22 close to the fastening region 12 and, opposite this first fold flank, a second fold flank 24 , the fold peak region 20 being adjoined by a fold trough 26 . The fold peak region 20 has a fold peak 21 with a maximum M. Furthermore, the rolling boot 10 according to the prior art shown in FIG. 1 is provided in its interior with reinforcing ribs 40 which are arranged in the fold region 16 .
FIG. 4 of the present application shows a boot 10 according to FIG. 1 mounted on a housing part 54 of a fixed joint. The housing part 54 has an outer lateral circumferential surface 70 and also an end surface 68 , between which surfaces a peripheral edge 55 is arranged. The boot 10 is mounted on the joint housing part 54 by a first fastening element 58 , and on a shaft 56 in a second fastening region 14 using a second fastening element 62 . The first fastening element 58 and also the first fastening region 12 of the boot 10 are in this case completely assigned to the outer lateral circumferential surface 70 of the joint housing part 54 , or to the joint housing part 54 itself, and the first fastening region 12 is directly followed by a fold region 16 having exactly one fold in the example shown in FIG. 1 and FIG. 4 .
A particular disadvantage with the known prior art as shown in FIGS. 1 and 4 is that, because of the complete overlapping of the outer lateral surface of the joint housing by the first fastening element and the first fastening region, the fold region displays large deformations during operation of the boot, for example when used in a fixed joint. Given the forces which act, particularly at high rotational speeds, and the associated high mechanical loading, it may occur that boots will possibly even burst during operation.
Therefore a boot and also a system comprising such a boot is needed in which the deformations acting in particular on the fold region, in particular those in the first fold of the fold region that is near the first fastening region, are reduced.
SUMMARY
A boot is disclosed herein, the boot having a first fastening region, wherein the first fastening region is displaced axially, as viewed in the direction of a main axis of the boot, and with respect to a housing part, such as, for example, a housing part of a constant velocity sliding joint or fixed joint. It is understood that the boot may be used with any other housing part, and may be used on a joint on which the boot can be mounted, in such a way that the first fastening region at least partially projects beyond an edge of the housing part. In one exemplary configuration, the first fastening region is provided with a base surface which makes available a seat for a first fastening element and which at least partially projects beyond the edge of the housing part, with respect to the main axis of the boot.
By virtue of the projecting length made available according to the disclosure by the first fastening region, there finally occurs an only partial overlapping of the outer lateral circumferential surface by the first fastening region or the first fastening element arranged on the base surface thereof. The fastening element then has, in addition to the known sealing function, a supporting function by virtue of the possibility made available by the first fastening element to make available, in the region of the projecting length, a support for the fold region, and here in particular the first fold of the fold region that is near the first fastening region. As a result, the deformation of the boot during operation is reduced overall and an increased rotational speed stability is thereby achieved. This has a particularly advantageous effect when the boot according to the disclosure is designed as a rolling boot, it also being possible within the context of the present disclosure for the boot to be designed as a folding boot having a plurality of folds in the fold region. However, a double-folding boot design is also possible, for example.
As already discussed above, the boot according to the disclosure may be used in fixed joints or else constant velocity sliding joints. However, it can also be arranged on any other type of joints, for example on ball joints, or else in pushrods, for sealing tube ends or other housing parts, in order to provide a sufficient degree of sealing and an additional supporting function. The present disclosure is thus not restricted in terms of the type of housing parts on which the boot can be mounted. Examples of applicable housing parts here are also tube ends of any type, including, for example, push rods, shafts or the like, but also joints and their outer joint housing.
The projecting length of the base surface of the first fastening region of the boot according to an exemplary configuration of the disclosure is advantageously situated in a range from approximately 20% to approximately 45%, preferably approximately 24% to approximately 35%, of a width of the first fastening element. With such a projecting length ratio, there is made available, on the one hand, a sufficient sealing function of the folding boot but also, on the other hand, a sufficient supporting function, provided by the first fastening element. If the projecting length were smaller, that is to say below 20%, a sufficient supporting function would not be provided under certain circumstances; on the other hand, if the projecting length were too large, the sealing function of the boot could be diminished. The use of the word “approximately” in the present connection makes it clear to the person skilled in the art who is being addressed that embodiments somewhat outside the stated range are hereby readily also covered by the scope of protection of the present disclosure. In particular, deviations of approximately plus/minus 10%, preferably approximately plus/minus 5%, of the respective upper and lower limits do not, within the context of the present disclosure, go outside the scope of protection thereof since a sufficient sealing and protective function can still be provided within these ranges.
In one exemplary configuration, the base surface of the first fastening region at least partially overlaps a transition region, as viewed in the direction of the main axis of the boot. The transition region adjoins the first fastening region in the direction of a second fastening region in the direction of the main axis of the boot, wherein the second fastening region often has a smaller inside and outside diameter than the first fastening region. Subsequently arranged after the transition region is a fold region which comprises at least one fold. If the fold region has exactly one fold, the boot according to the disclosure can be designed, for example, as a rolling boot. If it has two folds, it may be designed, for example, as a double-folding boot, or alternatively, if it has a plurality of folds, it is designed as a multi-folding boot. The transition region between the first fastening region and fold region can here be configured, for example, in such a way that it is thereby possible for the transition region to bear by way of its inner surface or an arrangement thereof closely against a peripheral end surface of a housing part. However, it is also possible to provide in the transition region for example a joint region which entails advantageous properties in the case of certain embodiments of folding boots in particular. Furthermore, additional retaining or orienting elements can also be arranged in the transition region, these elements facilitating a fastening of a first fastening element in the first fastening region. The first transition region is preferably configured in such a way that its inner surface is arranged opposite a peripheral end surface of a housing part, and with further preference is in contact therewith, i.e. bears against this surface. Then, by virtue of the overlapping of this transition region by the base surface of the first fastening region which makes available the binder seat, and after mounting the first fastening element, there is advantageously achieved a situation whereby the forces exerted by the mounting of the fastening element are transmitted into the first transition region, making it possible to further reduce a more pronounced deformation of the boot according to an embodiment of the disclosure. A complete overlapping here means that the base surface overlaps the entire material thickness of the transition region, and in this region makes available a binder seat for the first fastening element. Preferably, as viewed in the direction of the main axis of the boot, the projecting length is arranged axially displaced in the direction of the fold region of the boot and at least partially outside the transition region.
In a further exemplary configuration, at least two outer ribs bridge the first fastening region and the transition region at least in parts, with respect to a direction perpendicular to the main axis of the boot. The outer set of ribs advantageously achieves a situation whereby the boot according to the disclosure can be designed to be even more compact, and in particular can have a smaller inside volume. The displacement of the first fastening region already advantageously achieves a reduction in the overall height of the boot according to the disclosure, this reduction being further supported by the provision of an outer set of ribs. An outer set of ribs here is particularly advantageous in the case of rolling boots since they provide a sufficient degree of stability during deformation, and, on the other hand, the inside diameter of these boots is reduced, with the result finally that a reduction in the grease pressure is also achieved and higher service lives and a lower susceptibility to wear can be achieved.
In a further exemplary configuration of the present disclosure, a plurality of ribs are arranged with a uniform distribution on an outer circumferential surface of the boot. Provision may be made for the respective ribs to be arranged oppositely in pairs on the outer circumferential surface of the boot. For example, four, six, seven, eight, nine, ten or more such pairs can be arranged on the outer circumferential surface of the boot, depending on the requirements which are known to the person skilled in the art who is being addressed. Preference is given here to arranging the respective pairs with a uniform spacing from one another.
In yet another exemplary configuration, at least one of the ribs protrudes beyond the base surface of the first fastening region to form a positioning and/or bearing surface. The first fastening region constitutes a binder seat surface for a fastening element, for example a clamping strap, a clamp or a compression ring. However, other fastening elements known to a person skilled in the art can also be used within the context of the present disclosure. The specific design of at least one of the outer ribs, preferably at least half the number of outer ribs, more preferably all the outer ribs, serves to facilitate the positioning of this fastening element in the first fastening region, it additionally being the case that the fastening element can also bear by way of its peripheral side edge at least partially against the bearing surface formed by the at least one outer rib, i.e. is in direct contact with this bearing surface. Here, contact does not have to be made by the entire side face of the fastening element with respect to the overall height or thickness of the fastening element. Rather, the positioning and/or bearing surface can also only be at most approximately 90 percent, more preferably at most approximately 60 percent, of the overall height of the fastening element. The fastening element will in this case protrude beyond the positioning and/or bearing surface. In an exemplary arrangement, the positioning and/or bearing surface is designed to be substantially perpendicular in relation to the main axis of the boot, and is part of an offset which is arranged between that end of the first outer edge of the outer rib facing the first fastening region and the positioning and/or bearing surface. Here, this offset preferably has a second outer edge for the at least one outer rib, which edge is preferably oriented substantially parallel to the main axis of the rolling boot, and is part of the rib in question. However, provision can also be made here for this second outer edge for the at least one outer rib to have a slightly angled design, with respect to the main axis of the rolling boot, the angle between the second outer edge and the main axis of the rolling boot being smaller than that angle which is defined between the first outer edge of the at least one outer rib and the main axis of the rolling boot.
In one exemplary configuration, the outer rib preferably has a first outer edge which is directed away from the outer circumferential surface of the rolling boot. In one exemplary configuration, the first outer edge of the outer rib here starts approximately in the fold peak region of the first fold, more preferably exactly at the fold peak, i.e. the maximum of the first fold, and moreover preferably extends linearly and at an angle to the main axis of the rolling boot. However, provision can also be made for the first outer edge to have another design, for example to be curved.
Furthermore, the present disclosure also relates to a system consisting of a housing part, which may be part of a joint, such as part of a fixed joint, and even a joint itself, and of a boot as defined above. More specifically, an exemplary system according to the disclosure comprises at least a first fastening element, but may also include at least a second fastening element for fastening the rolling boot in a second fastening region, in particular on a shaft. The first fastening element bears at least by way of a portion of a side face against the positioning and/or bearing surface of at least one rib. In one exemplary configuration, the side face of the fastening element protrudes beyond the positioning and/or bearing surface of the rib. The base surface of the first fastening region, which base surface makes available a seat surface for the fastening element, is displaced axially with respect to the housing part and displaced with respect to the main axis of the boot in such a way that the base surface at least partially projects beyond an edge of the housing part, for example of a joint housing. The projecting length of the base surface here is preferably situated in a range from approximately 20 percent to approximately 45 percent, more preferably in a range from approximately 25 percent to approximately 35 percent, of a width of the first fastening element.
BRIEF DESCRIPTION OF THE DRAWINGS
These and further advantages of the present disclosure will be explained in more detail below with reference to the following figures, in which:
FIG. 1 shows a cross section along a main axis of a rolling boot according to the prior art;
FIG. 2 shows a cross section on a line B-B in FIG. 3 along a main axis of a rolling boot according to an exemplary embodiment of the disclosure;
FIG. 3 shows an outer view of the rolling boot according to the disclosure as shown in FIG. 2 ;
FIG. 4 shows a sectional view through a system according to the prior art comprising a housing part of a fixed joint, a rolling boot in accordance with FIG. 1 , a shaft and first and second fastening elements; and
FIG. 5 shows a cross section on a line A-A in FIG. 3 through a system according to an exemplary embodiment of the disclosure comprising a joint housing, a folding boot according to FIGS. 2 and 3 and a first fastening elements for fastening the folding boot to the housing part.
DETAILED DESCRIPTION
It should be stated first of all that the features shown in the figures are not restricted to the individual embodiments. Rather, the features in each case shown and indicated in the description, including the description of the figures, can be combined with one another for development purposes, identical features, including those from the prior art, are designated here by the same references. In particular, the subject of the present disclosure is not restricted to the embodiment, shown in the figures, of the system according to the disclosure for a fixed joint with a rolling boot. Rather, the present disclosure can be applied to boots of any type which are mounted on whatever parts for sealing purposes. In particular, it is also neither envisioned nor intended to restrict the disclosure to fixed joints in automobiles; rather, the boots according to the disclosure can be used in a large number of application areas, in particular in constant velocity sliding joints. Finally, it is also possible, in particular, to design the fold region in such a way that, if appropriate, second or other further folds can be provided.
FIG. 1 shows the folding boot according to the prior art already described in the background, this boot having in its interior a plurality of inner ribs 40 arranged in the fold region 16 in order to achieve a sufficient degree of rigidity. It is clearly evident from FIG. 1 that the folding boot 10 according to the prior art shown therein is relatively bulky.
FIG. 4 shows the folding boot 10 according to the prior art as shown in FIG. 1 mounted on a fixed joint housing having a housing part 54 with an outer lateral circumferential surface 70 and a shelf 56 , the folding boot 10 being mounted in the first fastening region 12 on the housing part 54 using a first fastening element 58 and in the second fastening region 14 on the shelf 60 housing a second fastening element 62 . This forms an overall system 74 . The first fastening region 12 receives over its full surface the first fastening element 58 , which comes to lie between a first retaining element 30 and a second retaining element 32 . The first and second retaining elements 30 or 32 in this embodiment of a boot 10 according to the prior art can here be embodied as peripheral webs, but also as interrupted webs, for example also in the form of “ear webs”, which have a rounded outer contour as viewed in a direction perpendicular to the main axis 60 of the boot 10 . In the embodiment of the system 74 as shown in FIG. 4 , in this case the base surface 28 of the first fastening region of the boot 10 is identical to the binder seat surface.
It is clearly evident from FIG. 4 that the first fastening region, and hence also the base surface 28 thereof, does not project beyond a housing edge 55 which is arranged in the transition from the outer lateral circumferential surface 70 to a peripheral end surface 68 of the housing part 54 .
FIG. 2 now shows a folding boot 10 according to an exemplary embodiment of the present disclosure with a first fastening region 12 and a second fastening region 14 , wherein an interior 36 of the boot 10 is assigned, in the first fastening region 12 , an accumulation of material 38 , formed as a peripheral annular bead, which can engage in a corresponding peripheral annular groove on a housing part (see FIG. 5 in this respect). The first fastening region 12 makes available a base surface 28 which has a greater width than the width of a fastening element 58 , as can be seen from FIG. 5 . The first fastening region is adjoined by a transition region 50 with an outer base surface 52 and an inner base surface 53 . In the example shown here, this transition region is designed in such a way that it extends substantially perpendicularly to a main axis 60 of the boot 10 , and moreover bears against the outer peripheral end surface 68 of the housing part 54 or is arranged close to it, as can also be seen from FIG. 5 . Following the transition region 50 is provided a fold region 16 which has a first fold 18 with a first fold flank 22 near the first fastening region 12 and, opposite this first fold flank, a second fold flank 24 . The first fold 18 here has a fold peak region 20 with a fold peak 21 and a maximum M. The first fold 18 is followed by a fold trough 26 which is directly adjoined by the second fastening region 14 .
Furthermore, the boot according to one exemplary configuration of the disclosure as shown in FIG. 2 has an outer rib 42 with a first outer edge 44 , which starts at the maximum M of the fold peak region, i.e. at the fold peak 21 , and a second outer edge 43 which extends substantially parallel to the main axis 60 of the boot 10 . The outer rib 44 here makes available a bearing and/or positioning surface 48 for the fastening element 58 (see FIG. 5 ). For this purpose, the outer rib 42 protrudes somewhat beyond the base surface 28 of the first fastening region 12 , with the result that the second outer edge 43 also protrudes beyond the base surface 28 and in so doing is formed substantially parallel to this surface.
An angle α, which is approximately 110°, is formed between the outer base surface 52 and an outer side 23 of the first fold flank 22 of the fold 18 . In principle, the angle a within the context of the present invention is measured between an outer base surface 52 of the transition region 50 and an outer side 23 of a first fold flank 22 of the first fold 18 . In one exemplary configuration, the angle α is preferably situated in a range from approximately 90° to approximately 140°, with further preference in a range from approximately 100° to approximately 130°.
It is also evident from FIG. 2 how a height H of the first fold 18 within the context of the present disclosure is determined. This involves measuring the region between a tangent extending through the maximum M or the fold peak 21 of the first fold 18 , this tangent being oriented perpendicularly to the main axis 60 of the boot 10 , and an inner base surface 53 of the transition region 10 . Since this base surface in the exemplary embodiment is likewise oriented perpendicularly to the main axis 60 of the boot 10 , the tangent extending through the fold peak 21 of the maximum M of the first fold 18 extends parallel to this inner base surface 53 of the transition region 50 . However, provision can also be made for the inner base surface 53 of the transition region 50 to be arranged at an angle in relation to the main axis 60 of the rolling boot 10 .
In the context of the present disclosure, the depth T of the fold trough 26 is determined by measuring the region between a tangent extending on an inner base surface 27 , i.e. the minimum of the fold trough 26 directed toward the interior of the boot 10 , and perpendicularly to the main axis 60 of the boot 10 , and that tangent which extends through the fold peak 21 or the maximum M of the first fold 18 and perpendicularly to the main axis 60 of the boot 10 . Since both tangents thus extend parallel and perpendicularly to the main axis 60 of the boot 10 , the depth T can be determined simply.
As can be seen from FIG. 2 , the depth T is approximately 42 percent of the height H.
FIG. 3 shows the line B-B along which was taken the section of the boot 10 which can be seen in FIG. 2 . Furthermore, FIG. 3 shows particularly clearly that plurality of outer ribs 42 , more precisely a total of 10 rib pairs 42 , that is to say a total of twenty outer ribs 42 , are arranged on an outer circumferential surface 11 of the boot 10 . It can also be clearly seen that the outer ribs 42 fractionally protrude beyond the base surface 28 of the first fastening region 12 so as to form a bearing and positioning surface 48 , the outer edge 43 for this purpose being indicated in FIG. 3 to make this clear.
FIG. 5 now shows a system 74 according to an exemplary embodiment of the disclosure, comprising a boot 10 as shown in one of FIGS. 2 and 3 and also a housing part 54 , here a fixed joint, together with a first fastening element 58 . FIG. 5 also shows a shaft 56 . The housing part 54 has an outer lateral circumferential surface 70 and an outer end surface 68 , between which surfaces is arranged a housing edge 55 . The fastening element 58 has a first side face 59 . 1 and a second side face 59 . 2 , in one embodiment of the fastening element 58 , for example as a compression ring, are to be regarded as peripheral side faces. Not shown in FIG. 5 is a second fastening element 62 which serves to fasten the boot 10 on the shaft 56 in the second fastening region 14 . In the second fastening region can be clearly seen an offset 64 at which the fold trough 26 merges into the second fastening region 14 . The offset 64 here is designed to be peripheral so as to produce a bearing and/or positioning surface for a second fastening element 16 , not shown in FIG. 5 . Moreover, the section through the system 74 , with respect to the boot 10 , was taken along a line A-A in FIG. 3 .
In the system 74 according to the exemplary configuration of the disclosure shown in FIG. 5 , the fastening element 58 projects beyond the housing edge 55 by a projecting length 46 . This projecting length 46 is determined by the outer end surface 68 of the housing part 54 on the one hand and, on the other hand, by the bearing and/or positioning surface 48 , made available by the outer rib 42 . This projecting length 46 is a portion of the base surface 28 , but also of the binder seat surface, of the first fastening region 12 . FIG. 5 also shows the width 8 of the fastening element 58 determined by the two outer side faces 59 . 1 and 59 . 2 thereof. The projecting length 46 here is somewhat more than 25 percent of the width of the first fastening means 58 . | A boot which has reduced deformations during operation is disclosed. The boot includes a first fastening region, wherein the first fastening region is displaced axially, with respect to the direction of a main axis of the boot, and with respect to a housing part on which the boot can be mounted, in such a way that the first fastening region at least partially projects beyond an edge of the housing part. | 5 |
TECHNICAL FIELD
[0001] The present invention relates to a mixing instrument (apparatus) for mixing a first component in a solid phase or a liquid phase and a second component in a liquid phase with each other. The present invention also relates to a piercing method for a double-ended needle.
BACKGROUND ART
[0002] Heretofore, in a medical organization or the like, when a patient is to be given an intravenous drip injection (for transfusion), an adhesion preventive, or a living tissue adhesive or the like, it often is customary to prepare a drug solution by diluting or dissolving a drug within a liquid, and then to draw the drug solution into a syringe. To produce such a drug solution, a device with a double-ended needle is used. More specifically, a plug (rubber plug) on a drug container which contains a drug in a solid phase or a liquid phase, and which has a negative pressure developed therein, is pierced with one end of the double-ended needle to connect the drug container to the double-ended needle, and a plug on a liquid container, which contains a liquid such as distilled water or the like, is pierced with the other end of the double-ended needle to connect the liquid container to the double-ended needle, thereby bringing the drug container and the liquid container into fluid communication with each other through the double-ended needle. Since a negative pressure is developed in the drug container, the liquid in the liquid container is attracted to and flows into the drug container via the double-ended needle. Thereafter, the drug container is shaken several times. The drug in the drug container becomes diluted and is dissolved by the liquid that has flowed into the drug container.
[0003] Background art, which is concerned with a device for mixing a drug and a liquid using a double-ended needle, is disclosed in Japanese Laid-Open Patent Publication No. 2008-523851 (PCT) and Japanese Laid-Open Patent Publication No. 2001-333961, for example.
SUMMARY OF INVENTION
[0004] When the double-ended needle is connected to the drug container and the liquid container, if the piercing point of the double-ended needle for the drug container is inserted through the plug on the drug container before the piercing point of the double-ended needle for the liquid container is inserted through the plug on the liquid container, then the negative pressure in the drug container is eliminated, making it impossible to attract the liquid from the liquid container. Conversely, if the piercing point of the double-ended needle for the liquid container is inserted through the plug on the liquid container before the piercing point of the double-ended needle for the drug container is inserted through the plug on the drug container, then the liquid tends to unduly leak from the liquid container. Consequently, the amount of liquid that flows into the drug container tends to change, and a proper amount of liquid to be mixed with the drug cannot be made available.
[0005] Therefore, the mixing instruments according to the background art are liable to cause a handling error by eliminating the negative pressure in the drug container or by allowing liquid to leak from the liquid container, unless the timing at which the piercing point of the double-ended needle for the drug container is inserted through the plug on the drug container is the same as the timing at which the piercing point of the double-ended needle for the liquid container is inserted through the plug on the liquid container. The above two timings may be brought into conformity with each other by increasing the speed at which the double-ended needle is inserted into the drug container and the liquid container. However, such an approach is difficult to apply if the double-ended needle is handled by persons who are not sufficiently skilled or physically strong enough.
[0006] The present invention has been made in view of the above problems. It is an object of the present invention to provide a mixing instrument, which can be handled easily without causing handling errors, by maintaining a negative pressure in a drug container and preventing liquid from leaking from a liquid container, even if the timing at which a puncture needle for the drug container of a double-ended needle penetrates a plug on the drug container differs from the timing at which a puncture needle for the liquid container of the double-ended needle penetrates a plug on the liquid container. Another object of the present invention is to provide a piercing method for a double-ended needle.
[0007] To achieve the above objects, there is provided in accordance with the present invention a mixing instrument for mixing a first component and a second component with each other, comprising a first container for storing the first component, the first container having a mouth sealed by a first plug made of an elastic material and having a negative pressure developed therein, a second container for storing the second component, the second container having a mouth sealed by a second plug made of an elastic material, and a double-ended needle having a first puncture needle for piercing the first plug and a second puncture needle for piercing the second plug, wherein the double-ended needle brings the first container and the second container into fluid communication with each other when the first puncture needle pierces the first plug and the second puncture needle pierces the second plug, wherein the first puncture needle and the second puncture needle include respective increased penetration resistance members disposed at positions closer to proximal end portions than distal-end tubes thereof including cutting faces, and having a greater penetration resistance to the first plug and the second plug than the distal-end tubes, and wherein the cutting faces of the distal-end tubes have respective heights in an axial direction which are smaller than thicknesses of the first plug and the second plug.
[0008] With the above arrangement of the present invention, the first puncture needle and the second puncture needle have respective distal-end tubes with openings formed in the cutting faces on distal ends thereof, and the respective increased penetration resistance members, which are disposed at positions closer to the proximal end portions than the distal-end tubes thereof, and having a greater penetration resistance to the first plug and the second plugs than the distal-end tubes. When the double-ended needle is connected to the first container and the second container, the distal-end tubes, including needle points with a relatively small penetration resistance, are initially inserted into the rubber plugs, and then, the increased penetration resistance members with a relatively large penetration resistance are inserted into the rubber plugs. After the openings in the needle points of the first puncture needle and the second puncture needle have been closed respectively by the first plug and the second plug, the first puncture needle and the second puncture needle penetrate the first plug and the second plug, respectively. Consequently, the negative pressure in the drug container is maintained and liquid is prevented from leaking out, even if the timing at which the first puncture needle penetrates the first plug differs from the timing at which the second puncture needle penetrates the second plug. More specifically, even if the first puncture needle penetrates the first plug before the second puncture needle penetrates the second plug, since the opening in the distal end of the second puncture needle is closed by the second plug, the negative pressure in the drug container is maintained. Further, even if the second puncture needle penetrates the second plug before the first puncture needle penetrates the first plug, since the opening in the distal end of the first puncture needle is closed by the first plug, liquid is prevented from leaking out. According to the present invention, since the negative pressure in the first container is maintained and liquid is prevented from leaking out, even if the timing at which the first puncture needle penetrates the first plug differs from the timing at which the second puncture needle penetrates the second plug, a mixing instrument is provided which can be handled easily without causing handling errors.
[0009] In the above mixing instrument, the increased penetration resistance members comprise increased diameter members having outside diameters greater than the outside diameters of the distal-end tubes.
[0010] With the above arrangement, since the increased penetration resistance members comprise the increased diameter members, respectively, having an outside diameter greater than the outside diameter of the distal-end tubes, the penetration resistance is increased with a simple arrangement by a step provided by the different outside diameters of the distal-end tubes and the increased diameter members.
[0011] In the above mixing instrument, the first puncture needle and the second puncture needle have respective inner tubes made of metal and including the distal-end tubes and respective outer tubes surrounding the inner tubes that serve as the increased penetration resistance members.
[0012] With the above arrangement, since the distal-end tubes including the cutting edges are made of metal, the cutting edges can easily be formed as sharp edges. The cutting edges, which are formed as sharp edges, reduce the penetration resistance of the distal-end tubes with respect to the first plug and the second plug, thereby reducing the forces required to cause the distal-end tubes to pierce the first plug and the second plug. The mixing instrument can thus be handled more easily.
[0013] The above mixing instrument further comprises a first holder shaped as a hollow tube having a first opening formed in an end thereof, the first container being mounted in the first holder, a second holder shaped as a hollow tube having a second opening formed in an end thereof, the second container being mounted in the second holder, and a connector, the double-ended needle being mounted on the connector, the connector being slidable in an axial direction of the double-ended needle into fitting engagement with the end of the first holder with the first container insertion opening formed therein, and being slidable in an axial direction of the double-ended needle into fitting engagement with the end of the second holder with the second container insertion opening formed therein.
[0014] With the above arrangement, the first holder with the first container mounted therein and with the first plug positioned near the first opening, and the connector with the first puncture needle oriented toward the first plug are slid axially into fitting engagement with each other. Further, the second holder with the second container mounted therein and with the second plug positioned near the second opening, and the connector with the second puncture needle oriented toward the second plug are slid axially into fitting engagement with each other. The first puncture needle thus pierces the first plug, while the second puncture needle pierces the second plug. When the first holder, the connector, and the second holder are fitted together, they slide against each other and are guided in relative axial movement. Therefore, the first puncture needle and the second puncture needle can pierce the first plug and the second plug, respectively, accurately and simply in the axial direction, whereby the mixing instrument can be handled more easily.
[0015] The above mixing instrument further comprises a lock mechanism for releasably locking the first holder, the connector, and the second holder inseparably together when the first holder, the connector, and the second holder are fitted together in a relative positional relation, such that the first puncture needle pierces the first plug and the second puncture needle pierces the second plug.
[0016] With the above arrangement, when the first holder, the connector, and the second holder are coupled together, they are locked by the lock mechanism so that they can be handled in their entirety as an integrated mixing instrument. Consequently, it is easy to perform the process of shaking the mixing instrument in order to accelerate mixing of the first component and the second component.
[0017] In the above mixing instrument, the first container, the second container, and the double-ended needle each are provided in two sets, two first containers are mounted in the first holder, two second containers are mounted in the second holder, paired double-ended needles are mounted on the connector and spaced from each other in directions perpendicular to the axial direction, and one of the double-ended needles and the other double-ended needle have respective cutting faces facing away from each other in directions in which the double-ended needles are spaced from each other.
[0018] With the above arrangement, when the paired double-ended needles pierce the first plug and the second plug, respectively, forces acting horizontally on the double-ended needles cancel each other out. Therefore, the sliding resistance between the first holder, the connector, and the second holder is prevented from increasing when such elements are fitted together. Since resistive forces are prevented from unduly increasing at the time that the first holder, the connector, and the second holder are coupled together, the mixing instrument can be handled with greater ease.
[0019] According to the present invention, there also is provided a piercing method for causing a double-ended needle, having a first puncture needle on one end and a second puncture needle on another end thereof, to pierce a first plug made of an elastic material and sealing a mouth of a first container and a second plug made of an elastic material and sealing a mouth of a second container having a negative pressure developed therein, thereby bringing the first container and the second container into fluid communication with each other, comprising the steps of preparing the double-ended needle having the first puncture needle and the second puncture needle which include respective increased penetration resistance members disposed at positions closer to proximal end portions than distal-end tubes thereof including cutting faces, and having a greater penetration resistance to the first plug and the second plug than the distal-end tubes, sealing both ends by pressing a distal end of the first puncture needle into the first plug to close a first opening formed in the distal end of the first puncture needle with the first plug while temporarily preventing a distance by which the first puncture needle is inserted into the first plug from increasing with the increased penetration resistance member of the first puncture needle, and pressing a distal end of the second puncture needle into the second plug to close a second opening formed in the distal end of the second puncture needle while temporarily preventing a distance by which the second puncture needle is inserted into the second plug from increasing with the increased penetration resistance member of the second puncture needle, and after sealing both ends, piercing the first plug with the first puncture needle and piercing the second plug with the second puncture needle to thereby bring the first container and the second container into fluid communication with each other.
[0020] With the above piercing method for the double-ended needle according to the present invention, the negative pressure in the drug container is maintained and the liquid is prevented from leaking out, even if the timing at which the first puncture needle penetrates the first plug differs from the timing at which the second puncture needle penetrates the second plug. More specifically, even if the first puncture needle penetrates the first plug before the second puncture needle penetrates the second plug, since the opening in the distal end of the second puncture needle is closed by the second plug, negative pressure in the drug container is maintained. Further, even if the second puncture needle penetrates the second plug before the first puncture needle penetrates the first plug, since the opening in the distal end of the first puncture needle is closed by the first plug, liquid is prevented from leaking out. According to the present invention, therefore, the plugs can be pierced by the double-ended needle simply without handling errors, by maintaining the negative pressure in the first container and preventing liquid from leaking out, even if the timing at which the first puncture needle penetrates the first plug differs from the timing at which the second puncture needle penetrates the second plug.
[0021] According to the present invention, there also is provided a mixing instrument for mixing a first component and a second component with each other, comprising a first container for storing the first component, the first container being sealed by a first plug made of an elastic material and having a negative pressure developed therein, a second container for storing the second component, the second container having a mouth sealed by a second plug made of an elastic material, and a double-ended needle having a first puncture needle for piercing the first plug and a second puncture needle for piercing the second plug, wherein the double-ended needle brings the first container and the second container into fluid communication with each other when the first puncture needle pierces the first plug and the second puncture needle pierces the second plug, wherein respective needle point angles of the first puncture needle and the second puncture needle and respective elastic characteristics of the first plug and the second plug are established, such that when the first puncture needle is pressed by the first plug and the second puncture needle is pressed by the second plug, openings formed in opposite ends of a lumen of the double-ended needle are sealed by the first plug and the second plug, respectively, and wherein the first puncture needle and the second puncture needle have respective cutting faces having respective heights in an axial direction which are smaller than thicknesses of the first plug and the second plug.
[0022] With the above arrangement according to the present invention, since the needle point angles of the first puncture needle and the second puncture needle and the elastic characteristics of the first plug and the second plug are established in the foregoing manner, when the double-ended needle pierces the first plug and the second plug, the first plug pressed by the first puncture needle and the second plug pressed by the second puncture needle are initially elastically deformed, and openings in opposite ends of the lumen are simultaneously sealed before the first puncture needle and the second puncture needle penetrate through the first plug and the second plug, respectively. Therefore, even if the timing at which the first puncture needle penetrates the first plug differs from the timing at which the second puncture needle penetrates the second plug, negative pressure in the drug container is maintained and liquid is prevented from leaking out. More specifically, even if the first puncture needle penetrates the first plug before the second puncture needle penetrates the second plug, since the opening of the lumen of the second puncture needle is sealed by the second plug, negative pressure in the drug container is maintained. Further, even if the second puncture needle penetrates the second plug before the first puncture needle penetrates the first plug, since the opening of the lumen of the first puncture needle is sealed by the first plug, liquid is prevented from leaking out. According to the present invention, therefore, even if the timing at which the first puncture needle penetrates the first plug of the drug container differs from the timing at which the second puncture needle penetrates the second plug of the liquid container, negative pressure in the drug container is maintained and liquid is prevented from leaking out. Accordingly, a mixing instrument is provided, which can be handled easily without causing handling errors.
[0023] In the above mixing instrument, the cutting faces of the first puncture needle and the second puncture needle are shaped as concave surfaces, which are curved as viewed in vertical cross section, and a point of intersection between a line segment that extends between a proximal end portion of each of the cutting faces and a distal end portion thereof, and a line normal to the line segment that extends from a deepest point on the concave surface is positioned closer to the proximal end portion of the cutting face than the midpoint of the line segment, and a center of the lumen is closer to the proximal end portion of the cutting face than a central line of each puncture needle.
[0024] With the above arrangement, the proximal end areas of the cutting faces, which are formed as concave surfaces, of the first puncture needle and the second puncture needle function as chins. Since such chins increase the penetration resistance by which the first plug and the second plug are penetrated, when the distal ends of the first puncture needle and the second puncture needle bite into the first plug and the second plug, the chins temporarily bear the first plug and the second plug. Since the openings of the lumen are positioned closer to the proximal end portions (the chins) of the cutting faces than the central line of the needle, while the chins bear the first plug and the second plug, the openings in opposite ends of the lumen are simultaneously sealed by the first plug and the second plug.
[0025] The above mixing instrument further comprises a first holder shaped as a hollow tube having a first opening formed in one end thereof, the first container being mounted in the first holder, a second holder shaped as a hollow tube having a second opening formed in one end thereof, the second container being mounted in the second holder, and a connector, the double-ended needle being mounted on the connector, the connector being slidable in an axial direction of the double-ended needle into fitting engagement with the end of the first holder with the first container insertion opening formed therein, and being slidable in an axial direction of the double-ended needle into fitting engagement with the end of the second holder with the second container insertion opening formed therein.
[0026] With the above arrangement, the first holder with the first container mounted therein and with the first plug positioned near the first opening, and the connector with the first puncture needle oriented toward the first plug are slid axially into fitting engagement with each other. Also, the second holder with the second container mounted therein and with the second plug positioned near the second opening, and the connector with the second puncture needle oriented toward the second plug are slid axially into fitting engagement with each other. Therefore, the first puncture needle pierces the first plug and the second puncture needle pierces the second plug. When the first holder, the connector, and the second holder are fitted together, such elements slide against each other and are guided for relative axial movement. Therefore, the first puncture needle and the second puncture needle can pierce the first plug and the second plug, respectively, accurately and simply in the axial direction. Consequently, the mixing instrument can be handled more easily.
[0027] The above mixing instrument further comprises a lock mechanism for releasably locking the first holder, the connector, and the second holder inseparably together when the first holder, the connector, and the second holder are fitted together in a relative positional relation, such that the first puncture needle pierces the first plug and the second puncture needle pierces the second plug.
[0028] With the above arrangement, when the first holder, the connector, and the second holder are coupled together, the components are locked by the lock mechanism so that they can be handled in their entirety as an integrated mixing instrument. Consequently, it is easy to perform the process of shaking the mixing instrument to accelerate mixing of the first component and the second component.
[0029] In the above mixing instrument, the first container, the second container, and the double-ended needle each are provided in two sets, such that two first containers are mounted in the first holder, two second containers are mounted in the second holder, the paired puncture needles are mounted on the connector and spaced from each other in directions perpendicular to the axial direction, and one of the double-ended needles and the other double-ended needle have respective cutting faces facing away from each other in directions in which the double-ended needles are spaced from each other.
[0030] With the above arrangement, when the paired double-ended needles pierce the first plug and the second plug, respectively, horizontal forces acting on the double-ended needles cancel each other out. Therefore, sliding resistance between the first holder, the connector, and the second holder is prevented from increasing when the components are fitted together. Since resistive forces are prevented from unduly increasing at the time that the first holder, the connector, and the second holder are coupled together, the mixing instrument can be handled with greater ease.
[0031] According to the present invention, there is further provided a piercing method for causing a double-ended needle, having a first puncture needle on one end and a second puncture needle on another end thereof, to pierce a first plug made of an elastic material and sealing a mouth of a first container, and a second plug made of an elastic material and sealing a mouth of a second container having a negative pressure developed therein, thereby bringing the first container and the second container into fluid communication with each other. The method comprises the steps of preparing the double-ended needle, the first plug, and the second plug, wherein respective needle point angles of the first puncture needle and the second puncture needle and respective elastic characteristics of the first plug and the second plug are established, such that when the first puncture needle is pressed by the first plug and the second puncture needle is pressed by the second plug, openings formed in opposite ends of a lumen of the double-ended needle are sealed by the first plug and the second plug, respectively, sealing both ends by pressing a distal end of the first puncture needle into the first plug to elastically deform the first plug and to close a first opening formed in the distal end of the first puncture needle with the first plug, and pressing a distal end of the second puncture needle into the second plug to elastically deform the second plug and to close a second opening formed in the distal end of the second puncture needle with the second plug, and after sealing both ends, piercing the first plug with the first puncture needle and piercing the second plug with the second puncture needle to thereby bring the first container and the second container into fluid communication with each other.
[0032] With the above piercing method for a double-ended needle according to the present invention, the negative pressure in the drug container is maintained and the liquid is prevented from leaking out, even if the timing at which the first puncture needle penetrates the first plug differs from the timing at which the second puncture needle penetrates the second plug. More specifically, even if the first puncture needle penetrates the first plug before the second puncture needle penetrates the second plug, since the opening in the distal end of the second puncture needle is closed by the second plug, negative pressure in the drug container is maintained. Further, even if the second puncture needle penetrates the second plug before the first puncture needle penetrates the first plug, since the opening in the distal end of the first puncture needle is closed by the first plug, liquid is prevented from leaking out. According to the present invention, therefore, the plugs can be pierced by the double-ended needle simply and without handling errors by maintaining the negative pressure in the first container and preventing the liquid from leaking out, even if the timing at which the first puncture needle penetrates the first plug differs from the timing at which the second puncture needle penetrates the second plug.
[0033] According to the present invention, the mixing instrument can be handled easily without causing handling errors by maintaining the negative pressure in the drug container and by preventing liquid from leaking out, even if the timing at which the puncture needle for the drug container of the double-ended needle penetrates the plug on the drug container differs from the timing at which the puncture needle for the liquid container of the double-ended needle penetrates the plug on the liquid container.
[0034] According to the present invention, the piercing method for the double-ended needle allows the double-ended needle to pierce the plugs simply without causing handling errors.
BRIEF DESCRIPTION OF DRAWINGS
[0035] FIG. 1 is a cross-sectional view of a mixing instrument according to a first embodiment of the present invention;
[0036] FIG. 2A is an enlarged cross-sectional view, partially omitted from illustration, showing a lock mechanism in a first state;
[0037] FIG. 2B is an enlarged cross-sectional view, partially omitted from illustration, showing the lock mechanism in a second state;
[0038] FIG. 3 is an enlarged cross-sectional view, partially omitted from illustration, showing a double-ended needle and nearby parts of the mixing instrument according to the first embodiment of the present invention;
[0039] FIG. 4 is an enlarged cross-sectional view, partially omitted from illustration, illustrative of dimensions of a distal end portion of the double-ended needle of the mixing instrument according to the first embodiment of the present invention;
[0040] FIG. 5 is a cross-sectional view showing the manner in which the double-ended needle of the mixing instrument according to the first embodiment of the present invention has distal-end tubes thereof inserted into a first plug and a second plug;
[0041] FIG. 6 is an enlarged cross-sectional view, partially omitted from illustration, showing the manner in which the double-ended needle of the mixing instrument according to the first embodiment of the present invention has one of the distal-end tubes thereof inserted into the first plug;
[0042] FIG. 7 is a cross-sectional view showing the manner in which the double-ended needle of the mixing instrument according to the first embodiment of the present invention extends through the first plug and the second plug, thereby bringing a first container and a second container into fluid communication with each other;
[0043] FIG. 8A is an enlarged cross-sectional view, partially omitted from illustration, showing a first modification of the double-ended needle of the mixing instrument according to the first embodiment of the present invention;
[0044] FIG. 8B is an enlarged cross-sectional view, partially omitted from illustration, showing a second modification of the double-ended needle of the mixing instrument according to the first embodiment of the present invention;
[0045] FIG. 9 is an exploded perspective view of a mixing instrument according to a second embodiment of the present invention;
[0046] FIG. 10 is a cross-sectional view of the mixing instrument according to the second embodiment of the present invention;
[0047] FIG. 11 is a cross-sectional view showing the manner in which double-ended needles of the mixing instrument according to the second embodiment of the present invention have distal-end tubes thereof inserted into first plugs and second plugs;
[0048] FIG. 12 is a cross-sectional view showing the manner in which the double-ended needles of the mixing instrument according to the second embodiment of the present invention extend through the first plugs and the second plugs, thereby bringing first containers and second containers into fluid communication with each other;
[0049] FIG. 13 is a cross-sectional view of a mixing instrument according to a third embodiment of the present invention;
[0050] FIG. 14 is an enlarged cross-sectional view, partially omitted from illustration, showing a double-ended needle and nearby parts of the mixing instrument according to the third embodiment of the present invention;
[0051] FIG. 15 is an enlarged cross-sectional view, partially omitted from illustration, showing a first puncture needle and nearby parts of the mixing instrument according to the third embodiment of the present invention;
[0052] FIG. 16 is a cross-sectional view showing the manner in which the double-ended needle of the mixing instrument according to the third embodiment of the present invention pierces a first plug and a second plug;
[0053] FIG. 17 is an enlarged cross-sectional view, partially omitted from illustration, showing the manner in which a lumen of the first puncture needle of the mixing instrument according to the third embodiment of the present invention is sealed by the first plug;
[0054] FIG. 18 is a cross-sectional view showing the manner in which the double-ended needle of the mixing instrument according to the third embodiment of the present invention extends through the first plug and the second plug, thereby bringing a first container and a second container into fluid communication with each other;
[0055] FIG. 19 is an exploded perspective view of a mixing instrument according to a fourth embodiment of the present invention;
[0056] FIG. 20 is a cross-sectional view of the mixing instrument according to the fourth embodiment of the present invention;
[0057] FIG. 21 is an enlarged cross-sectional view, partially omitted from illustration, showing a pair of double-ended needles and nearby parts of the mixing instrument according to the fourth embodiment of the present invention;
[0058] FIG. 22 is a cross-sectional view showing the manner in which the double-ended needles of the mixing instrument according to the fourth embodiment of the present invention pierce first plugs and second plugs; and
[0059] FIG. 23 is a cross-sectional view showing the manner in which the double-ended needles of the mixing instrument according to the fourth embodiment of the present invention extend through the first plugs and the second plugs, thereby bringing first containers and second containers into fluid communication with each other.
DESCRIPTION OF EMBODIMENTS
[0060] Embodiments of the present invention will hereinafter be described below with reference to the drawings. For illustrative purposes, the upper side, the lower side, the left side, and the right side in FIGS. 1 to 12 will be referred to as “upper,” “lower,” “left,” and “right” sides respectively.
First Embodiment
[0061] FIG. 1 is a cross-sectional view of a mixing instrument 10 according to a first embodiment of the present invention. The mixing instrument 10 serves to mix a first component in a solid phase or a liquid phase, and a second component in a liquid phase. Although the first component is illustrated as being in a solid phase or a liquid phase, whereas the second component is illustrated as being in a liquid phase, the components are not limited to such states. The first component may be in a gel state or a gaseous state. Similarly, the second component may be in a gel state or a gaseous state.
[0062] As shown in FIG. 1 , the mixing instrument 10 includes a drug container (first container) 12 for storing the first component therein, a drug holder (first holder) 14 for mounting the drug container 12 thereon, a liquid container (second container) 16 for storing the second component therein, a liquid holder (second holder) 18 for mounting the liquid container 16 thereon, a double-ended needle 20 for bringing the drug container 12 and the liquid container 16 into fluid communication with each other, and a connector 22 to which the double-ended needle 20 is fixed.
[0063] The drug container 12 and the liquid container 16 are not limited to any particular type of container, but may be vials or the like.
[0064] The drug container 12 stores a drug as the first component. The drug is not limited to any particular form, but may be a solid (tablets, granules, etc.), a powder (powder medicine, etc.), or a liquid (liquid medicine, etc.). If a living tissue adhesive is to be prepared, then the drug may be thrombin or fibrinogen. If an adhesion preventive is to be prepared, then the drug may be carboxymethyl dextrin produced by modifying a drug with a succinimidyl group, for example, or a mixture of sodium hydrogen carbonate and sodium carbonate. The drug container 12 has a negative pressure developed therein.
[0065] The liquid container 16 stores a liquid as the second component. The second component is a liquid such as distilled water or the like, for example, which dilutes or dissolve the drug that makes up the second component.
[0066] As shown in FIG. 1 , the drug container 12 includes a hard container body 24 and a first plug 26 made of an elastic material, which hermetically seals the mouth of the container body 24 . The liquid container 16 includes a hard container body 28 and a second plug 30 made of an elastic material, which hermetically seals the mouth of the container body 28 .
[0067] The container bodies 24 , 28 are made of a material, which is not limited to any particular material, but which may be any of various glasses or various resins, such as polyvinyl chloride, polyethylene, polypropylene, cyclic polyolefin, polystyrene, poly-(4-methylpentene-1), polycarbonate, acrylic resin, an acrylonitrile-butadiene-styrene copolymer, a polyester such as polyethylene terephthalate, polyethylene naphthalate, or the like, a butadiene-styrene copolymer, and polyamide (e.g., nylon 6, nylon 6·6, nylon 6·10, or nylon 12). Resins are preferable to glasses. If the container bodies 24 , 28 are made of a resin, then the container bodies 24 , 28 can be discarded by burning and hence the process of discarding the container bodies 24 , 28 can be minimized. The container bodies 24 , 28 should preferably be permeable to light (virtually transparent or translucent) for keeping the interior thereof visible.
[0068] The first plug 26 and the second plug 30 can be pierced by a first puncture needle 42 and a second puncture needle 44 , to be described later. The first plug 26 and the second plug 30 are made of a material, which is not limited to any particular material, but which may be any of various rubber materials, such as natural rubber, butyl rubber, isoprene rubber, butadiene rubber, styrene-butadiene rubber, and silicone rubber, various thermoplastic elastomers such as a polyurethane thermoplastic elastomer, a polyester thermoplastic elastomer, a polyamide thermoplastic elastomer, an olefin thermoplastic elastomer, and a styrene thermoplastic elastomer, and elastic materials including mixtures of the aforementioned materials. If the first plug 26 and the second plug 30 are made of butyl rubber, then the rubber hardness thereof should preferably have a Shore A hardness in the range from 39 to 53°, and more preferably, in the range from 45 to 47°.
[0069] Portions of the first plug 26 and the second plug 30 , which are pierced by the double-ended needle 20 , have a thickness t (see FIG. 5 ), which preferably is in the range from 1 to 4 mm, and more preferably, in the range from 2.0 to 2.5 mm.
[0070] The drug holder 14 is a bottomed tubular component for storing the drug container 12 therein. The drug holder 14 is made of any of various resins, such as polyvinyl chloride, polyethylene, polypropylene, cyclic polyolefin, polystyrene, poly-(4-methylpentene-1), polycarbonate, acrylic resin, an acrylonitrile-butadiene-styrene copolymer, polyester such as polyethylene terephthalate, polyethylene naphthalate, or the like, a butadiene-styrene copolymer, and polyamide (e.g., nylon 6, nylon 6·6, nylon 6·10, or nylon 12).
[0071] The drug holder 14 has a first opening 14 a formed in one end thereof. The drug container 12 is inserted into the drug holder 14 through the first opening 14 a.
[0072] The drug holder 14 also has ledges 32 , 34 that project horizontally outwardly from left and right sides of the upper end of the drug holder 14 . The ledges 32 , 34 have respective holes 32 a , 34 a formed vertically therethrough.
[0073] The drug holder 14 houses therein a restraint member 36 for restraining the drug container 12 with respect to the drug holder 14 . The restraint member 36 has a tubular shape, which is open at upper and lower ends thereof. The restraint member 36 has protrusions (not shown) on the outer circumferential surface thereof, which engage in either recesses (not shown) formed in an inner circumferential surface of the drug holder 14 , or holes (not shown) formed in a side wall of the drug holder 14 , for thereby securing the drug container 12 at a predetermined position with respect to the drug holder 14 .
[0074] The restraint member 36 may be made of materials, which are the same as the aforementioned materials of the drug holder 14 .
[0075] The liquid holder 18 is a bottomed tubular component for storing the liquid container 16 . As shown in FIG. 1 , the liquid holder 18 has a side wall with a height large enough to fully house the liquid container 16 in the liquid holder 18 .
[0076] The liquid holder 18 has a plurality of support guides 19 spaced circumferentially on an inner circumferential surface thereof for supporting the liquid container 16 , and limiting projections 21 on the inner circumferential surface thereof for limiting the depth to which the liquid container 16 can be inserted.
[0077] The liquid holder 18 has a second opening 18 a formed in an end thereof. The liquid container 16 is inserted into the liquid holder 18 through the second opening 18 a.
[0078] The liquid holder 18 also includes a pair of lock members 38 , 40 extending downwardly from left and right sides of an outer circumferential surface thereof. The lock members 38 , 40 include respective arms 38 a , 40 a , first engaging portions 38 b , 40 b disposed on respective distal ends of the arms 38 a , 40 a , and second engaging portions 38 c , 40 c disposed on the arms 38 a , 40 a more closely to proximal ends thereof than the first engaging portions 38 b , 40 b . The arms 38 a , 40 a have a plurality of vertically spaced projections 38 d , 40 d , respectively, on outer side surfaces thereof.
[0079] As shown in FIG. 1 , the double-ended needle 20 includes a first puncture needle 42 for piercing the first plug 26 , and a second puncture needle 44 for piercing the second plug 30 . The double-ended needle 20 is formed integrally with the connector 22 .
[0080] The connector 22 has a partition 46 extending horizontally, a lower side wall 48 extending downwardly from the partition 46 , and an upper side wall 50 extending upwardly from the partition 46 . The first puncture needle 42 is mounted on the lower surface of the partition 46 , and the second puncture needle 44 is mounted on the upper surface of the partition 46 . The connector 22 may be made of materials, which are the same as the aforementioned materials of the drug holder 14 .
[0081] The lower side wall 48 surrounds the first puncture needle 42 . The lower side wall 48 has a height (vertical dimension) greater than the height of the first puncture needle 42 , so that the distal end (cutting face) of the first puncture needle 42 does not project downwardly from the lower side wall 48 .
[0082] The upper side wall 50 surrounds the second puncture needle 44 and has a shape and size such that the upper side wall 50 can be inserted into the drug container 12 . The upper side wall 50 has a height greater than the height of the second puncture needle 44 , so that the distal end (cutting face) of the second puncture needle 44 does not project upwardly from the upper side wall 50 . The upper side wall 50 has ledges 52 , 54 projecting horizontally outwardly from left and right sides of an upper end thereof. The ledges 52 , 54 have respective holes 52 a , 54 a formed vertically therethrough.
[0083] The connector 22 can be inserted into the drug holder 14 with the outer circumferential surface of the upper side wall 50 serving as a sliding surface. More specifically, the connector 22 is capable of sliding longitudinally (vertically) along the double-ended needle 20 into fitting engagement with the drug holder 14 .
[0084] The liquid holder 18 can be inserted into the connector 22 such that the outer circumferential surface of the lower end portion thereof serves as a sliding surface. More specifically, the liquid holder 18 can slide longitudinally along the double-ended needle 20 into fitting engagement with the connector 22 .
[0085] According to the first embodiment, the lock members 38 , 40 , the ledges 32 , 34 , and the ledges 52 , 54 jointly make up a lock mechanism 37 . The lock mechanism 37 serves to releasably lock the drug holder 14 , the connector 22 , and the liquid holder 18 inseparably together when the drug holder 14 , the connector 22 , and the liquid holder 18 are fitted together in a relative positional relation, such that the first puncture needle 42 pierces the first plug 26 and the second puncture needle 44 pierces the second plug 30 .
[0086] The lock mechanism 37 can selectively be placed in a first state, as shown in FIG. 2A , and a second state, as shown in FIG. 2B . In the first state, the liquid holder 18 engages the connector 22 and the drug holder 14 as a whole. In the second state, the liquid holder 18 engages the connector 22 , but is disengaged from the drug holder 14 .
[0087] Since the ledges 32 , 34 of the drug holder 14 are identical in constitution, the right ledge 34 will typically be described below. Similarly, since the lock members 38 , 40 and the ledges 52 , 54 of the connector 22 are identical in constitution, the right lock member 40 and the right ledge 54 will typically be described below. Since the ledge 34 , the lock member 40 , and the ledge 54 are provided in respective pairs, the first state and the second state can be reliably achieved.
[0088] As shown in FIGS. 1 , 2 A and 2 B, the lock member 40 includes a plate-like arm 40 a projecting from the outer circumferential surface of the side wall of the liquid holder 18 , a first engaging portion 40 b projecting from one surface 401 of the arm 40 a , and a second engaging portion 40 c projecting from another surface 402 of the arm 40 a.
[0089] The other surface 402 of the arm 40 a faces toward the side wall of the liquid holder 18 . The arm 40 a has one end (an upper end as shown) supported on and fixed to the side wall of the liquid holder 18 . Thus, the arm 40 a is supported in a cantilevered fashion and can be elastically deformed when the arm 40 a is pressed at a certain location on a floating portion thereof toward the side wall of the liquid holder 18 . The arm 40 a is of a crank shape as viewed in side elevation, or more specifically, the arm 40 a is spaced from the side wall of the liquid holder 18 by a distance that increases stepwise toward the other end thereof (a lower end as shown).
[0090] As shown in FIGS. 2A and 2B , the first engaging portion 40 b is constituted as a prong, which projects from the distal end of the arm 40 a . The first engaging portion 40 b has a slanted surface 403 inclined with respect to the vertical direction, and a horizontal engaging surface 404 opposite to the slanted surface 403 .
[0091] The second engaging portion 40 c is constituted as a prong, which projects from the arm 40 a at a position above the first engaging portion 40 b . The second engaging portion 40 c has a slanted surface 405 inclined with respect to the vertical direction, and a horizontal engaging surface 406 opposite to the slanted surface 405 .
[0092] As shown in FIG. 2A , the ledge 34 of the drug holder 14 can engage with the first engaging portion 40 b . In an assembled state, the arm 40 a can be inserted into the hole 34 a in the ledge 34 . When the liquid holder 18 is connected, i.e., is inserted into, the drug holder 14 , the arm 40 a is inserted into the hole 34 a in the ledge 34 . At this time, the slanted surface 403 of the first engaging portion 40 b of the arm 40 a presses against and then moves over and beyond the inner circumferential surface of the hole 34 a . When the slanted surface 403 of the first engaging portion 40 b moves over and beyond the inner circumferential surface of the hole 34 a , the arm 40 a snaps back under its own resilient force, thereby causing the engaging surface 404 to engage with the lower surface of the ledge 34 , as shown in FIG. 2A . In this state, the liquid holder 18 and the drug holder 14 engage with each other. In the state shown in FIG. 2A , a clearance 410 is formed between the other surface 402 of the arm 40 a and the inner circumferential surface of the hole 34 a in the ledge 34 . The engaging surface 404 of the first engaging portion 40 b has a horizontal length slightly smaller than the distance provided by the clearance 410 .
[0093] The arm 40 a can be elastically deformed from the state shown in FIG. 2A by being pressed toward the side wall of the liquid holder 18 over the distance provided by the clearance 410 . When the arm 40 a is elastically deformed in this manner, the engaging surface 404 of the first engaging portion 40 b is spaced from the lower surface of the ledge 34 (see FIG. 2B ). The first engaging portion 40 b and the ledge 34 , i.e., the liquid holder 18 and the drug holder 14 , do not become disengaged from each other.
[0094] As shown in FIGS. 2A and 2B , the ledge 54 of the connector 22 engages with the second engaging portion 40 c . In an assembled state, the arm 40 a can be inserted into the hole 54 a in the ledge 54 . When the liquid holder 18 is connected, i.e., is inserted into, the drug holder 14 , the arm 40 a is inserted into the hole 54 a in the ledge 54 . At this time, the slanted surface 405 of the second engaging portion 40 c of the arm 40 a presses against and then moves over and beyond the inner circumferential surface of the hole 54 a . When the slanted surface 405 of the second engaging portion 40 c moves over and beyond the inner circumferential surface of the hole 54 a , the arm 40 a snaps back under its own resilient force, thereby causing the engaging surface 406 to engage with the ledge 54 , as shown in FIG. 2A . In this state, the liquid holder 18 and the connector 22 engage with each other.
[0095] In the state shown in FIG. 2A , a clearance 412 is formed between the other surface 402 of the arm 40 a and the inner circumferential surface of the hole 54 a . The engaging surface 406 of the second engaging portion 40 c has a horizontal length, which is sufficiently smaller than the distance provided by the clearance 412 . Therefore, even in the presence of the clearance 412 , the second engaging portion 40 c can engage with the ledge 54 sufficiently and reliably.
[0096] Unlike the first engaging portion 40 b , the second engaging portion 40 c has the engaging surface 406 , which remains in engagement with the ledge 54 even when the arm 40 a is elastically deformed from the state shown in FIG. 2A as a result of being pressed toward the side wall of the liquid holder 18 (regardless of whether the arm 40 a is pressed or released) (see FIG. 2B ).
[0097] When the first engaging portions 38 b , 40 b of the lock members 38 , 40 engage with the ledges 32 , 34 , respectively, of the drug holder 14 , and the second engaging portions 38 c , 40 c of the lock members 38 , 40 engage with the ledges 52 , 54 , respectively, of the connector 22 , the lock mechanism 37 is placed in the first state, in which the liquid holder 18 engages the connector 22 and the drug holder 14 as a whole. When the arms 38 a , 40 a are pressed from the first state, the first engaging portions 38 b , 40 b of the lock members 38 , 40 disengage from the ledges 32 , 34 , respectively, of the drug holder 14 , while the second engaging portions 38 c , 40 c of the lock members 38 , 40 remain in engagement with the ledges 52 , 54 , respectively, of the connector 22 . In this condition, the lock mechanism 37 is placed in the second state, in which the liquid holder 18 remains in engagement with the connector 22 , but is disengaged from the drug holder 14 .
[0098] According to a modification of the lock mechanism 37 shown in FIG. 1 , the drug holder 14 may include lock members similar to the lock members 38 , 40 , and the liquid holder 18 may include ledges similar to the ledges 32 , 34 for engaging with the lock members.
[0099] FIG. 3 is an enlarged cross-sectional view, partially omitted from illustration, showing the double-ended needle 20 integral with the connector 22 and nearby parts. As shown in FIG. 3 , the first puncture needle 42 and the second puncture needle 44 include increased penetration resistance members 64 , 66 , respectively, disposed at positions closer to proximal end portions thereof (at the partition 46 ) than distal-end tubes 60 , 62 including cutting faces 56 , 58 , and having a greater penetration resistance to the first plug 26 and the second plug 30 than the distal-end tubes 60 , 62 .
[0100] In the first embodiment, according to one configuration, the increased penetration resistance members 64 , 66 comprise increased diameter members 64 A, 66 A, respectively, having an outside diameter greater than the outside diameter of the distal-end tubes 60 , 62 . According to another configuration (modification), the increased penetration resistance members 64 , 66 may have a zigzag shape (sawtooth shape) provided by a vertical array of alternate peaks and valleys on the outer circumferential surfaces of the first puncture needle 42 and the second puncture needle 44 .
[0101] According to the first embodiment, as shown in FIG. 3 , the first puncture needle 42 and the second puncture needle 44 include an inner tube 68 of metal, which has a relatively small diameter (thin diameter), including the distal-end tubes 60 , 62 and outer tubes 70 , 72 , which have a large diameter, and which surround the inner tube 68 so as to provide the increased penetration resistance members 64 , 66 . The distal ends of the inner tube 68 , which project from the distal ends of the outer tubes 70 , 72 , serve as the distal-end tubes 60 , 62 .
[0102] The inner tube 68 may be made of stainless steel, an aluminum alloy, a copper-based alloy, or the like.
[0103] According to the first embodiment, the inner tube 68 comprises a single member shared by the first puncture needle 42 and the second puncture needle 44 . However, the inner tube 68 may comprise separate members, each of which is associated respectively with the first puncture needle 42 and the second puncture needle 44 .
[0104] The outer tubes 70 , 72 may be made of materials, which are the same as the aforementioned materials of the drug container 12 .
[0105] The outer tubes 70 , 72 and the partition 46 may be formed integrally, or alternatively, may be separate members, which are secured together by adhesive bonding, welding, or the like.
[0106] According to the first embodiment, as shown in FIG. 3 , the cutting face 56 of the first puncture needle 42 and the cutting face 58 of the second puncture needle 44 are inclined substantially at the same angle in one direction with respect to the axial direction (vertical direction in FIG. 3 ) of the double-ended needle 20 . According to a modification of the first embodiment, however, the cutting face 56 of the first puncture needle 42 and the cutting face 58 of the second puncture needle 44 may be inclined in opposite directions with respect to the axial direction.
[0107] FIG. 4 is an enlarged cross-sectional view, partially omitted from illustration, illustrative of dimensions of a distal end portion of the double-ended needle 20 of the mixing instrument 10 . Since the first puncture needle 42 and the second puncture needle 44 basically have the same constitution, the dimensions of the distal end portion of the first puncture needle 42 of the double-ended needle 20 will typically be described below.
[0108] As shown in FIG. 4 , the outside diameter of the inner tube 68 (distal-end tube 60 ) is represented by P, the outside diameter of the outer tube 70 (increased diameter member 64 A) is represented by Q, the distance in the axial direction from the distal end face of the outer tube 70 to the proximal end of the opening of the inner tube 68 is represented by L 1 , the distance in the axial direction from the distal end face of the outer tube 70 to the distal end of the opening of the inner tube 68 is represented by L 2 , and the angle formed between the axial direction of the inner tube 68 and the cutting face 56 is represented by θ.
[0109] P may be set to a value in a range from 1.20 mm to 1.30 mm (preferably 1.25 mm), for example. Q may be set to a value in a range from 2.25 mm to 2.35 mm (preferably 2.3 mm), for example. L 1 may be set to a value in a range from 0.7 mm to 0.9 mm (preferably 0.8 mm), for example. L 2 may be set to a value in a range from 1.5 mm to 1.7 mm (preferably 1.6 mm), for example. θ may be set to a value in a range from 55° to 60° (preferably 57°). The difference Q−P is preferably in a range from 0.95 to 1.15 mm.
[0110] In the illustrated mixing instrument 10 , P is set to 1.25, Q is set to 2.3 mm, L 1 is set to 0.8 mm, L 1 is set to 1.6 mm, and θ is set to 57°. The thickness of the plug 26 is set to 3 mm.
[0111] The mixing instrument 10 according to the first embodiment is basically constituted as described above. Operations and advantages of the mixing instrument 10 will be described below.
[0112] As shown in FIG. 1 , the drug container 12 is stored in the drug holder 14 and is secured to the drug holder 14 by the restraint member 36 . The liquid container 16 is mounted in the liquid holder 18 and is held by the liquid holder 18 .
[0113] Then, the connector 22 , with the double-ended needle 20 installed therein, is inserted into the drug holder 14 , such that the first puncture needle 42 is oriented toward the drug container 12 . The liquid holder 18 , with the liquid container 16 mounted therein, is inserted into the connector 22 , such that the second plug 30 is oriented toward the second puncture needle 44 .
[0114] During the insertion process, as shown in FIGS. 5 and 6 , the distal-end tubes 60 , 62 (the portions of the inner tube 68 that project from the outer tubes 70 , 72 ) of the first puncture needle 42 and the second puncture needle 44 pierce (are inserted into) the first plug 26 and the second plug 30 . Also, distal ends of the outer tubes 70 , 72 , which provide the increased diameter members 64 A, 66 A that function as the increased penetration resistance members 64 , 66 , abut against the first plug 26 and the second plug 30 , respectively, thereby temporarily preventing the distance that the first puncture needle 42 penetrates into the first plug 26 from increasing, and also temporarily preventing the distance that the second puncture needle 44 penetrates into the second plug 30 from increasing.
[0115] Such a state occurs because the increased diameter members 64 A, 66 A are larger in diameter than the distal-end tubes 60 , 62 , and hence the increased diameter members 64 A, 66 A exert an increased penetration resistance, such that the increased diameter members 64 A, 66 A cannot be inserted into the first plug 26 and the second plug 30 until after the distal-end tubes 60 , 62 on the opposite ends have been inserted fully into the first plug 26 and the second plug 30 .
[0116] As shown in FIG. 6 , since the height h in the axial direction of the cutting face 56 ( 58 ) of the distal-end tube 60 ( 62 ) is smaller than the thickness t of the portion of the first plug 26 (the second plug 30 ), which is pierced by the first puncture needle 42 (the second puncture needle 44 ), when the distal end of the first puncture needle 42 is pushed into the first plug 26 , the opening at the distal end of the first puncture needle 42 is closed by the first plug 26 , and when the distal end of the second puncture needle 44 is pushed into the second plug 30 , the opening at the distal end of the second puncture needle 44 is closed by the second plug 30 . In other words, both the opening of the first puncture needle 42 and the opening of the second puncture needle 44 become closed. As shown in FIG. 6 , the reverse side of the portion of the first plug 26 , which is pierced by the first puncture needle 42 , has a recess 26 a formed therein, thereby allowing that portion of the first plug 26 to be pierced easily. The reverse side of the portion of the second plug 30 , which is pierced by the second puncture needle 44 , has a similar recess formed therein.
[0117] When the liquid holder 18 is pushed further toward the drug holder 14 from the state shown in FIG. 5 , the mixing instrument 10 is assembled as shown in FIG. 7 . The lock mechanism 37 is easily brought into the first state, as described above. More specifically, the first engaging portions 38 b , 40 b of the arms 38 a , 40 a engage with the ledges 32 , 34 , respectively, of the drug holder 14 , whereas the second engaging portions 38 c , 40 c of the arms 38 a , 40 a engage with the ledges 52 , 54 , respectively, of the connector 22 . In this manner, the lock mechanism 37 operates to limit the mutual positional relation between the drug container 12 and the liquid container 16 , i.e., to prevent the containers 12 , 16 from unduly moving, thereby reliably keeping the drug container 12 and the liquid container 16 in fluid communication with each other.
[0118] At this time, as shown in FIG. 7 , the increased diameter members 64 A, 66 A of the first puncture needle 42 and the second puncture needle 44 pierce and penetrate the first plug 26 and the second plug 30 . Therefore, the needle points (i.e., the cutting faces) of the first puncture needle 42 and the second puncture needle 44 move respectively into the drug container 12 and the liquid container 16 . Thus, the drug container 12 and the liquid container 16 are brought into fluid communication with each other through the double-ended needle 20 .
[0119] Inasmuch as a negative pressure is developed in the drug container 12 , the liquid in the liquid container 16 is attracted to and flows into the drug container 12 through the double-ended needle 20 . Thereafter, in order to mix the drug and the liquid in the drug container 12 , the mixing instrument 10 is shaken several times. At this time, the drug in the drug container 12 becomes diluted and dissolved by the liquid, which has flowed into the drug container 12 .
[0120] After mixing of the first component and the second component is completed, the arms 38 a , 40 a of the lock members 38 , 40 on the liquid holder 18 are pressed inwardly toward the liquid holder 18 . The first engaging portions 38 b , 40 b of the arms 38 a , 40 a disengage from the ledges 32 , 34 of the drug holder 14 , whereas the second engaging portions 38 c , 40 c of the arms 38 a , 40 a remain in engagement with the ledges 52 , 54 of the connector 22 . In other words, the lock mechanism 37 is brought into the second state.
[0121] Then, the liquid holder 18 is pulled upwardly. The liquid holder 18 , in which the liquid container 16 is held, can now be released (removed) from the drug holder 14 together with the connector 22 . Since the projections 38 d , 40 d are disposed on the outer circumferential surfaces of the arms 38 a , 40 a , the user finds it easy to pull the liquid holder 18 , because the projections 38 d , 40 d function as a slip stop when the user presses the arms 38 a , 40 a laterally inward.
[0122] Then, the drug holder 14 , from which the connector 22 has been removed, is vertically inverted. Then, the left and right side walls of the drug holder 14 are pressed inwardly to release the restraint member 36 out of engagement with the drug holder 14 . The drug container 12 is released (drops) from the drug holder 14 together with the restraint member 36 .
[0123] According to the first embodiment, as described above, the cutting face 56 of the first puncture needle 42 and the cutting face 58 of the second puncture needle 44 are inclined in one direction with respect to the axial direction. With this arrangement, when the first puncture needle 42 and the second puncture needle 44 pierce the first plug 26 and the second plug 30 , respectively, forces acting horizontally on the first puncture needle 42 and the second puncture needle 44 cancel each other out. Therefore, the connector 22 is prevented from being pressed against the inner circumferential surface of the drug holder 14 , with the result that sliding resistance between the connector 22 and the drug holder 14 is prevented from increasing when the connector 22 is inserted into the drug holder 14 .
[0124] According to the first embodiment, as described above, the first puncture needle 42 and the second puncture needle 44 have respective distal-end tubes 60 , 62 with openings formed in the cutting faces on the distal ends thereof. The increased penetration resistance members 64 , 66 (the increased diameter members 64 A, 66 A) are disposed at positions closer to the proximal end portions than the distal-end tubes 60 , 62 , and have a greater penetration resistance to the first plug 26 and the second plug 30 than the distal-end tubes 60 , 62 . Therefore, when the double-ended needle 20 is connected to the drug container 12 and the liquid container 16 , the distal-end tubes 60 , 62 , including the needle points with relatively small penetration resistance, initially are inserted into the first plug 26 and the second plug 30 . Thereafter, the increased penetration resistance members 64 , 66 , with relatively large penetration resistance, are inserted into the first plug 26 and the second plug 30 .
[0125] After the openings in the needle points of the first puncture needle 42 and the second puncture needle 44 have been closed respectively by the first plug 26 and the second plug 30 , the first puncture needle 42 and the second puncture needle 44 penetrate the first plug 26 and the second plug 30 , respectively. Consequently, negative pressure in the drug container 12 is maintained, and liquid is prevented from leaking out, even if the timing at which the first puncture needle 42 penetrates the first plug 26 differs from the timing at which the second puncture needle 44 penetrates the second plug 30 .
[0126] More specifically, even if the first puncture needle 42 penetrates the first plug 26 before the second puncture needle 44 has penetrated the second plug 30 , since the opening in the distal end of the second puncture needle 44 is closed by the second plug 30 , negative pressure in the drug container 12 is maintained. Even if the second puncture needle 44 penetrates the second plug 30 before the first puncture needle 42 has penetrated the first plug 26 , since the opening in the distal end of the first puncture needle 42 is closed by the first plug 26 , liquid is prevented from leaking out. Accordingly, a mixing instrument 10 is provided, which can be handled easily without causing handling errors, and a piercing method is provided, which allows a double-ended needle 20 to pierce plugs simply without handling errors.
[0127] According to the first embodiment, since the increased penetration resistance members 64 , 66 comprise the increased diameter members 64 A, 66 A, respectively, each having an outside diameter greater than the outside diameter of the distal-end tubes 60 , 62 , penetration resistance is increased with a simple arrangement, i.e., by a step, which is provided by the different outside diameters of the distal-end tubes 60 , 62 and the increased diameter members 64 A, 66 A.
[0128] According to the first embodiment, since the distal-end tubes 60 , 62 including the cutting edges are made of metal, the cutting edges can easily be formed as sharp edges. The cutting edges, which are formed as sharp edges, reduce the penetration resistance of the distal-end tubes 60 , 62 with respect to the first plug 26 and the second plug 30 , thereby reducing forces required to cause the distal-end tubes 60 , 62 to pierce the first plug 26 and the second plug 30 . The mixing instrument 10 can thus be handled more easily.
[0129] According to the first embodiment, when the drug holder 14 , the connector 22 , and the liquid holder 18 are fitted together, the components slide against each other and are guided for relative axial movement. Therefore, the first puncture needle 42 and the second puncture needle 44 can pierce the first plug 26 and the second plug 30 , respectively, accurately and simply in the axial direction. Therefore, the mixing instrument 10 can be handled more easily.
[0130] According to the first embodiment, when the drug holder 14 , the connector 22 , and the liquid holder 18 are coupled together, the components are locked by the lock mechanism 37 , so that the drug holder 14 , the connector 22 , and the liquid holder 18 can be handled in their entirety as an integrated mixing instrument 10 . Consequently, it is easy to perform the process of shaking the mixing instrument 10 in order to accelerate mixing of the first component and the second component.
[0131] FIG. 8A is an enlarged cross-sectional view, partially omitted from illustration, showing a first modification of the double-ended needle 20 , which is of the basic form according to the first embodiment of the present invention. With the basic form according to the first embodiment, the inner tube 68 provides the small-diameter distal-end tubes 60 , 62 , and the outer tubes 70 , 72 provide the large-diameter increased diameter members 64 A, 66 A. According to the first modification shown in FIG. 8A , a double-ended needle 71 may comprise a first puncture needle 73 and a second puncture needle 74 , including distal-end tubes 76 , 78 and increased diameter members 80 , 82 , which are integral with each other. The first puncture needle 73 and the second puncture needle 74 may be made of materials, which are the same as the aforementioned materials of the drug holder 14 .
[0132] FIG. 8B is an enlarged cross-sectional view, partially omitted from illustration, showing a second modification of the double-ended needle 20 , which is of the basic form according to the first embodiment of the present invention. According to the second modification shown in FIG. 8B , a double-ended needle 90 may include increased penetration resistance members 96 , 98 in the form of projections 64 B, 66 B, which are integral therewith, near distal end portions of a first puncture needle 92 and a second puncture needle 94 , respectively. The projections 64 B, 66 B may be annular protrusions that extend fully around the outer circumferential surfaces of the first puncture needle 92 and the second puncture needle 94 , or protrusions that extend less than fully around the outer circumferential surfaces of the first puncture needle 92 and the second puncture needle 94 . The projections 64 B, 66 B may be a plurality of protrusions, which are spaced longitudinally (axially) along the first puncture needle 92 and the second puncture needle 94 .
Second Embodiment
[0133] FIG. 9 is an exploded perspective view of a mixing instrument 100 according to a second embodiment of the present invention. FIG. 10 is a cross-sectional view of the mixing instrument 100 according to the second embodiment of the present invention.
[0134] As shown in FIGS. 9 and 10 , the mixing instrument 10 includes two drug containers (first containers) 112 A, 112 B for storing a first component therein in a solid phase or a liquid phase, a drug holder (first holder) 114 in which the two drug containers 112 A, 112 B are mounted, two liquid containers (second containers) 116 A, 116 B for storing a second component in a liquid phase, a liquid holder (second holder) 118 in which two liquid containers 116 A, 116 B are mounted, two double-ended needles 120 A, 120 B, which are capable of bringing the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B into fluid communication with each other, and a connector 122 to which the double-ended needles 120 A, 120 B are fixed. According to the first embodiment, the drug container 12 , the liquid container 16 , and the double-ended needle 20 each are provided as a single part. However, according to the second embodiment, such components are provided as two parts each.
[0135] The drug containers 112 A, 112 B are basically of the same constitution as the drug container 12 . The two drug containers 112 A, 112 B have substantially the same constitution, except that the drug containers 112 A, 112 B differ in size and shape from each other. A negative pressure is developed in each of the drug containers 112 A, 112 B.
[0136] The liquid containers 116 A, 116 B are basically of the same constitution as the liquid container 16 . The two liquid containers 116 A, 116 B are substantially of the same constitution, except that they differ in size and shape from each other.
[0137] The first component stored in the drug containers 112 A, 112 B may be the same drug as the first component stored in the above-described drug container 12 .
[0138] The second component stored in the liquid containers 116 A, 116 B may be the same liquid as the second component stored in the above-described liquid container 16 .
[0139] The drug holder 114 is a bottomed tubular component, which stores the two drug containers 112 A, 112 B therein. The drug holder 114 is made of materials, which are the same as the aforementioned materials of the drug holder 14 .
[0140] The drug holder 114 has a first opening 114 a formed in one end thereof. The drug containers 112 A, 112 B are inserted into the drug holder 114 through the first opening 114 a.
[0141] The drug holder 114 also has ledges 132 , 134 , which project horizontally outwardly from left and right sides of the upper end thereof. The ledges 132 , 134 have respective holes 132 a , 134 a formed vertically therethrough.
[0142] The drug holder 114 houses therein a restraint member 136 for restraining the two drug containers 112 A, 112 B with respect to the drug holder 114 . The restraint member 136 includes a pair of tubular members 137 A, 137 B, which are open at upper and lower ends thereof, and a joint 139 that interconnects the tubular members 137 A, 137 B.
[0143] The restraint member 136 also has an engaging protrusion 141 disposed between the tubular members 137 A, 137 B. When the engaging protrusion 141 engages in an engaging recess 143 , which is formed in an inner surface of the drug holder 114 , the drug containers 112 A, 112 B become fixed in position with respect to the drug holder 114 . Instead of the engaging recess 143 , the drug holder 114 may have a hole formed in a side wall thereof, and the engaging protrusion 141 may engage in the hole.
[0144] The restraint member 136 may be made of materials, which are the same as the aforementioned materials of the drug holder 14 .
[0145] The liquid holder 118 is a bottomed tubular component for storing the two liquid containers 116 A, 116 B. As shown in FIG. 10 , the liquid holder 118 has a plurality of support guides 119 A, 119 B provided on the inner circumferential surface thereof for supporting the two liquid containers 116 A, 116 B, and a plurality of limiting projections 121 A, 121 B provided on the inner circumferential surface thereof for limiting the depth at which the liquid containers 116 A, 116 B can be inserted.
[0146] The liquid holder 118 includes a second opening 118 a formed in one end thereof. The liquid containers 116 A, 116 B are inserted into the liquid holder 118 through the second opening 118 a.
[0147] The liquid holder 118 also includes a pair of lock members 138 , 140 extending downwardly from left and right sides of the outer circumferential surface thereof. The lock members 38 , 40 include respective arms 138 a , 140 a , first engaging portions 138 b , 140 b , which are disposed on respective distal ends of the arms 138 a , 140 a , and second engaging portions 138 c , 140 c , which are disposed on the arms 138 a , 140 a more closely to the proximal ends (i.e., the upper ends thereof, as illustrated) than the first engaging portions 138 b , 140 b . The arms 138 a , 140 a have a plurality of vertically spaced projections 138 d , 140 d provided respectively on outer side surfaces thereof.
[0148] According to the second embodiment, the lock members 138 , 140 , the ledges 132 , 134 , and the ledges 152 , 154 jointly make up a lock mechanism 137 . The lock mechanism 137 serves to releasably lock the drug holder 114 , the connector 122 , and the liquid holder 118 inseparably when the drug holder 114 , the connector 122 , and the liquid holder 118 are fitted together in a relative positional relation, such that the first puncture needles 142 A, 142 B pierce the first plugs 126 A, 126 B and the second puncture needles 144 A, 144 B pierce the second plugs 130 A, 130 B.
[0149] The lock mechanism 137 can selectively be placed in a first state, in which the liquid holder 118 engages the connector 122 and the drug holder 114 as a whole, and a second state, in which the liquid holder 118 engages the connector 122 but is disengaged from the drug holder 114 . The constitution and functions of the lock mechanism 137 are the same as those of the lock mechanism 37 according to the first embodiment, and such features will not be described in detail below.
[0150] According to a modification of the lock mechanism 137 , lock members, which are similar to the lock members 138 , 140 , may be provided on the drug holder 114 , and ledges, which are similar to the ledges 132 , 134 , may be provided on the liquid holder 118 for engaging with the lock members.
[0151] As shown in FIGS. 9 and 10 , the two double-ended needles 120 A, 120 B have respective first puncture needles 142 A, 142 B that pierce the first plugs 126 A, 126 B, respectively, and respective second puncture needles 144 A, 144 B that pierce the second plugs 130 A, 130 B, respectively. The two double-ended needles 120 A, 120 B are joined to each other integrally by the connector 122 .
[0152] The two first puncture needles 142 A, 142 B and the two second puncture needles 144 A, 144 B have increased penetration resistance members 164 , 165 , 166 , 167 , respectively, disposed at positions closer to proximal end portions thereof (i.e., on the partition 146 ) than the distal-end tubes 160 A, 160 B, 162 A, 162 B including cutting faces, and having a greater penetration resistance with respect to the first plugs 126 A, 126 B and the second plugs 130 A, 130 B than the distal-end tubes 160 A, 160 B, 162 A, 162 B.
[0153] In the second embodiment, according to one configuration, the increased penetration resistance members 164 , 165 , 166 , 167 comprise increased diameter members 164 A, 165 A, 166 A, 167 B, respectively, having an outside diameter greater than the outside diameter of the distal-end tubes 160 A, 160 B, 162 A, 162 B. According to another configuration (modification), the increased penetration resistance members 164 , 165 , 166 , 167 may have a zigzag shape (sawtooth shape) provided by a vertical array of alternate peaks and valleys on outer circumferential surfaces of the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B.
[0154] According to the second embodiment, the two first puncture needles 142 A, 142 B and the two second puncture needles 144 A, 144 B include inner tubes 168 A, 168 B made of metal, which are relatively small (thin) in diameter, including the distal-end tubes 160 A, 160 B, 162 A, 162 B, together with outer tubes 170 A, 170 B, 172 A, 172 B, which are relatively large in diameter, and which surround the inner tubes 168 A, 168 B and serve to provide the increased penetration resistance members 164 , 165 , 166 , 167 . The distal ends of the inner tubes 168 A, 168 B, which project from the distal ends of the outer tubes 170 A, 170 B, 172 A, 172 B, serve as the distal-end tubes 160 A, 160 B, 162 A, 162 B.
[0155] The inner tubes 168 A, 168 B may be made of materials, which are the same as the aforementioned materials of the inner tube 68 according to the first embodiment. The outer tubes 170 A, 170 B, 172 A, 172 B may be made of materials, which are the same as the aforementioned materials of the outer tubes 70 , 72 according to the first embodiment.
[0156] According to the second embodiment, one of the inner tubes 168 A comprises a single member, which is shared by the first puncture needle 142 A and the second puncture needle 144 A. However, the inner tube 168 A may comprise separate members associated respectively with the first puncture needle 142 A and the second puncture needle 144 A. The same holds true for the other inner tube 168 B.
[0157] The outer tubes 170 A, 170 B, 172 A, 172 B may be made of materials, which are the same as the aforementioned materials of the drug containers 112 A, 112 B.
[0158] The outer tubes 170 A, 170 B, 172 A, 172 B and the partition 146 may be formed integrally with each other, or alternatively, the outer tubes 170 A, 170 B, 172 A, 172 B may be separate members secured together by adhesive bonding, welding, or the like.
[0159] According to the second embodiment, the cutting faces of the first puncture needles 142 A, 142 B and the cutting faces of the second puncture needles 144 A, 144 B are inclined in opposite directions with respect to the axial direction of the double-ended needles 120 A, 120 B, at substantially the same absolute angle. The angle is set such that the gradients of one of the first puncture needles 142 A and the other first puncture needle 142 B are mirror images of each other (in point symmetry) with respect to a vertical line that extends between the double-ended needles 120 A, 120 B. Similarly, the angle is set such that the gradients of one of the second puncture needles 144 A and the other second puncture needle 144 B are mirror images of each other (in point symmetry) with respect to a vertical line that extends between the double-ended needles 120 A, 120 B.
[0160] According to a modification of the second embodiment, however, the cutting faces of the first puncture needles 142 A, 142 B and the cutting faces of the second puncture needles 144 A, 144 B may be inclined in one direction with respect to the axial direction, as is the case with the double-ended needle 20 according to the first embodiment shown in FIG. 2 .
[0161] The connector 122 has a partition 146 extending horizontally, a lower side wall 148 extending downwardly from the partition 146 , and an upper side wall 150 extending upwardly from the partition 146 . The two first puncture needles 142 A, 142 B are mounted on the lower surface of the partition 146 , whereas the two second puncture needles 144 A, 144 B are mounted on the upper surface of the partition 146 . The connector 122 may be made of materials, which are the same as the aforementioned materials of the drug holder 14 .
[0162] The lower side wall 148 surrounds the two first puncture needles 142 A, 142 B as a whole. The lower side wall 148 has a height (vertical dimension), which is greater than the height of the two first puncture needles 142 A, 142 B, so that the distal ends (cutting faces) of the two first puncture needles 142 A, 142 B do not project downwardly from the lower end of the lower side wall 148 .
[0163] The upper side wall 150 surrounds the two second puncture needles 144 A, 144 B in their entirety. The upper side wall 150 has a height greater than the height of the two second puncture needles 144 A, 144 B, so that the distal ends (cutting faces) of the two second puncture needles 144 A, 144 B do not project upwardly from the upper side wall 150 . The upper side wall 150 has ledges 152 , 154 projecting horizontally outwardly from the left and right sides of the upper end thereof. The ledges 152 , 154 have respective holes 152 a , 154 a formed vertically therethrough.
[0164] The connector 122 can be inserted into the drug holder 114 , with the outer circumferential surface of the upper side wall 150 thereof serving as a sliding surface. More specifically, the connector 122 can move longitudinally (vertically) along the double-ended needles 120 A, 120 B with respect to the drug holder 114 .
[0165] The liquid holder 118 can be inserted into the connector 122 with the outer circumferential surface of the lower end portion thereof serving as a sliding surface. More specifically, the liquid holder 118 is capable of moving longitudinally along the double-ended needles 120 A, 120 B with respect to the connector 122 .
[0166] The dimensions and angles of the distal end portions of the two double-ended needles 120 A, 120 B may be set in the same manner as the dimensions P, Q, L 1 , L 2 and the angle θ (see FIG. 4 ) of the aforementioned corresponding portions according to the first embodiment.
[0167] The mixing instrument 100 according to the second embodiment is basically constituted as described above. Operations and advantages of the mixing instrument 100 will be described below.
[0168] As shown in FIG. 10 , the drug containers 112 A, 112 B are stored in the drug holder 114 , and are secured to the drug holder 114 by the restraint member 136 . The liquid containers 116 A, 116 B are mounted in the liquid holder 118 and are held by the liquid holder 118 .
[0169] Then, the connector 122 , with the two double-ended needles 120 A, 120 B installed therein, is inserted into the drug holder 114 such that the two first puncture needles 142 A, 142 B are oriented toward the drug containers 112 A, 112 B. Further, the liquid holder 118 , with the two liquid containers 116 A, 116 B mounted therein, is inserted into the connector 122 such that the second plugs 130 A, 130 B are oriented toward the second puncture needles 144 A, 144 B.
[0170] During the insertion process, as shown in FIG. 11 , the distal-end tubes 160 A, 160 B, 162 A, 162 B (i.e., the portions of the inner tubes 168 A, 168 B that project from the outer tubes 170 A, 170 B, 172 A, 172 B) of the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B pierce (are inserted into) the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, and the distal ends of the outer tubes 170 A, 170 B, 172 A, 172 B, which provide the increased diameter members 164 A, 165 A, 166 A, 167 A that function as the increased penetration resistance members 164 , 165 , 166 , 167 , abut against the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively, thereby temporarily preventing the distance by which the first puncture needles 142 A, 142 B are inserted into the first plugs 126 A, 126 B from increasing, as well as temporarily preventing the distance by which the second puncture needles 144 A, 144 B are inserted into the second plugs 130 A, 130 B from increasing.
[0171] Such a condition occurs because the increased diameter members 164 A, 165 A, 166 A, 167 A are larger in diameter than the distal-end tubes 160 A, 160 B, 162 A, 162 B, and hence the increased diameter members 164 A, 165 A, 166 A, 167 A exert an increased penetration resistance, such that the increased diameter members 164 A, 165 A, 166 A, 167 A cannot be inserted into the first plugs 126 A, 126 B and the second plugs 130 A, 130 B until after the distal-end tubes 160 A, 160 B, 162 A, 162 B on the opposite ends thereof have been inserted fully into the first plugs 126 A, 126 B and the second plugs 130 A, 130 B.
[0172] Since the height in the axial direction of the cutting faces of the distal-end tubes 160 A, 160 B, 162 A, 162 B is smaller than the thickness of the portions of the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, which are pierced by the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B, the openings at the distal ends of the first puncture needles 142 A, 142 B are closed by the first plugs 126 A, 126 B, and the openings at the distal ends of the second puncture needles 144 A, 144 B are closed by the second plugs 130 A, 130 B. In other words, both openings of the first puncture needles 142 A, 142 B and both openings of the second puncture needles 144 A, 144 B are closed.
[0173] When the liquid holder 118 is further pushed toward the drug holders 114 from the state shown in FIG. 11 , the mixing instrument 100 is assembled together, as shown in FIG. 12 . The lock mechanism 137 is easily brought into the first state, as described above. More specifically, the first engaging portions 138 b , 140 b of the arms 138 a , 140 a engage with the respective ledges 132 , 134 of the drug holder 114 , and the second engaging portions 138 c , 140 c of the arms 138 a , 140 a engage the respective ledges 152 , 154 of the connector 122 . The lock mechanism 137 thus operates to limit the mutual positional relation between the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B, i.e., to prevent the containers 112 A, 112 B, 116 A, 116 B from unduly moving, thereby reliably maintaining the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B in fluid communication with each other.
[0174] At this time, as shown in FIG. 12 , the increased diameter members 164 A, 165 A, 166 A, 167 A of the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B pierce the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively, and the needle points (the cutting faces) of the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B move respectively into the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B. At this time, the two drug containers 112 A, 112 B and the two liquid containers 116 A, 116 B are brought into fluid communication with each other by the corresponding double-ended needles 120 A, 120 B.
[0175] Inasmuch as a negative pressure is developed in the two drug containers 112 A, 112 B, liquid in the liquid containers 116 A, 116 B is attracted to and flows into the drug containers 112 A, 112 B through the two double-ended needles 120 A, 120 B. Thereafter, the mixing instrument 100 is shaken several times. At this time, the drugs in the drug containers 112 A, 112 B become diluted and are dissolved by the liquids that flow into the drug containers 112 A, 112 B.
[0176] After mixing of the drug and the liquid is completed, the arms 138 a , 140 a of the lock members 138 , 140 on the liquid holder 118 are pressed inwardly toward the liquid holder 118 . The first engaging portions 138 b , 140 b of the arms 138 a , 140 a disengage from the ledges 132 , 134 of the drug holder 114 , whereas the second engaging portions 138 e , 140 e of the arms 138 a , 140 a remain in engagement with the ledges 152 , 154 of the connector 122 . In other words, the lock mechanism 137 is brought into the second state.
[0177] Then, the liquid holder 118 is pulled upwardly. The liquid holder 118 , which holds the liquid containers 116 A, 116 B therein, can now be released (removed) from the drug holder 114 together with the connector 122 . Since the projections 138 d , 140 d are disposed on the arms 138 a , 140 a , the user finds it easy to pull the liquid holder 118 , because the projections 138 d , 140 d function as a slip stop.
[0178] Then, the drug holder 114 , from which the connector 122 has been removed, is vertically inverted. Then, the left and right side walls of the drug holder 114 are pressed inwardly to cause the engaging protrusion 141 of the restraint member 136 to disengage from the engaging recess 143 of the drug holder 114 . The drug containers 112 A, 112 B are released (drop) from the drug holder 114 together with the restraint member 136 .
[0179] According to the second embodiment, as described above, the cutting faces of the first puncture needles 142 A, 142 B and the cutting faces of the second puncture needles 144 A, 144 B are inclined in opposite directions with respect to the axial direction, and one of the double-ended needles 120 A and the other double-ended needle 120 B are mirror images of each other. With this arrangement, when the two double-ended needles 120 A, 120 B pierce into the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively, forces acting horizontally on the two double-ended needles 120 A, 120 B cancel each other out. Therefore, sliding resistance between the connector 122 and the drug holder 114 is prevented from increasing when the connector 122 is inserted into the drug holder 114 .
[0180] According to the second embodiment, as described above, the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B have respective distal-end tubes 160 A, 160 B, 162 A, 162 B with openings formed in the cutting faces on distal ends thereof, and the increased penetration resistance members 164 , 165 , 166 , 167 (increased diameter members 164 A, 165 A, 166 A, 167 A), which are disposed at positions closer to proximal end portions thereof than the distal-end tubes 160 A, 160 B, 162 A, 162 B, and having a greater penetration resistance to the first plugs 126 A, 126 B and the second plugs 130 A, 130 B than the distal-end tubes 160 A, 160 B, 162 A, 162 B. Therefore, when the double-ended needles 120 A, 120 B are connected to the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B, the distal-end tubes 160 A, 160 B, 162 A, 162 B, which include the needle points with a relatively small penetration resistance, are inserted initially into the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, and then the increased penetration resistance members 164 , 165 , 166 , 167 , which have a relatively large penetration resistance, are inserted into the first plugs 126 A, 126 B and the second plugs 130 A, 130 B.
[0181] After the openings in the needle points of the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B have been closed respectively by the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B penetrate the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively. Consequently, negative pressure in the drug containers 112 A, 112 B is maintained and liquids are prevented from leaking out, even if the timing at which the first puncture needles 142 A, 142 B penetrate the first plugs 126 A, 126 B differs from the timing at which the second puncture needles 144 A, 144 B penetrate the second plugs 130 A, 130 B.
[0182] More specifically, even if the first puncture needles 142 A, 142 B penetrate the first plugs 126 A, 126 B before the second puncture needles 144 A, 144 B penetrate the second plugs 130 A, 130 B, since the openings in the distal ends of the second puncture needles 144 A, 144 B are closed by the second plugs 130 A, 130 B, negative pressure in the drug containers 112 A, 112 B is maintained. Further, even if the second puncture needles 144 A, 144 B penetrate the second plugs 130 A, 130 B before the first puncture needles 142 A, 142 B penetrate the first plugs 126 A, 126 B, since the openings in the distal ends of the first puncture needles 142 A, 142 B are closed by the first plugs 126 A, 126 B, liquids are prevented from leaking out. Accordingly, a mixing instrument 100 is provided, which can be handled easily without causing handling errors, while in addition, a piercing method is provided for allowing double-ended needles 120 A, 120 B to pierce plugs simply without handling errors, by maintaining negative pressure in the drug containers 112 A, 112 B and preventing liquids from leaking out, even if the timing at which the first puncture needles 142 A, 142 B penetrate the first plugs 126 A, 126 B differs from the timing at which the second puncture needles 144 A, 144 B penetrate the second plugs 130 A, 130 B.
[0183] According to the second embodiment, since the increased penetration resistance members 164 , 165 , 166 , 167 comprise the increased diameter members 164 A, 165 A, 166 A, 167 A, respectively, which have an outside diameter greater than the outside diameter of the distal-end tubes 160 A, 160 B, 162 A, 162 B, penetration resistance is increased with a simple arrangement, due to the step, which is formed by the different outside diameters of the distal-end tubes 160 A, 160 B, 162 A, 162 B and the increased diameter members 164 A, 165 A, 166 A, 167 A.
[0184] According to the second embodiment, since the distal-end tubes 160 A, 160 B, 162 A, 162 B including the cutting edges are made of metal, the cutting edges can easily be formed as sharp edges. The cutting edges, which are formed as sharp edges, reduce the penetration resistance of the distal-end tubes 160 A, 160 B, 162 A, 162 B with respect to the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, thereby reducing the forces required to cause the distal-end tubes 160 A, 160 B, 162 A, 162 B to pierce the first plugs 126 A, 126 B and the second plugs 130 A, 130 B. Thus, the mixing instrument 100 can be handled more easily.
[0185] According to the second embodiment, when the drug holder 114 , the connector 122 , and the liquid holder 118 are fitted together, the drug holder 114 , the connector 122 , and the liquid holder 118 slide against each other and are guided for relative axial movement. Therefore, the first puncture needles 142 A, 142 B and the second puncture needles 144 A, 144 B are capable of piercing the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively, accurately and simply in the axial direction. Therefore, the mixing instrument 100 can be handled more easily.
[0186] According to the second embodiment, when the drug holder 114 , the connector 122 , and the liquid holder 118 are coupled together, the drug holder 114 , the connector 122 , and the liquid holder 118 are locked by the lock mechanism 137 , so that the drug holder 114 , the connector 122 , and the liquid holder 118 can be handled in their entirety as an integrated mixing instrument 100 . Consequently, it is easy to perform the process of shaking the mixing instrument 100 in order to accelerate mixing of the first component and the second component.
[0187] One or both of the two double-ended needles 120 A, 120 B may be constituted in the same manner as the double-ended needle 71 shown in FIG. 8A , or may be constituted in the same manner as the double-ended needle 90 shown in FIG. 8B .
Third Embodiment
[0188] FIG. 13 is a cross-sectional view of a mixing instrument 200 according to a third embodiment of the present invention. Components of the mixing instrument 200 according to the third embodiment, which have identical or similar functions and advantages to those of the mixing instrument 10 according to the first embodiment, are denoted by identical reference characters, and such features will not be described in detail below.
[0189] The mixing instrument 200 includes a connector 202 that is used in place of, and differs in constitution from the connector 22 of the mixing instrument according to the first embodiment. The connector 202 has a double-ended needle 204 that brings the drug container 12 and the liquid container 16 into fluid communication with each other. The double-ended needle 204 includes a first puncture needle 206 for piercing the first plug 26 and a second puncture needle 208 for piercing the second plug 30 . The double-ended needle 204 is formed integrally with the connector 202 .
[0190] Other constitutive details of the connector 202 are the same as those of the connector 22 of the mixing instrument according to the first embodiment. More specifically, the connector 202 has a partition 46 extending horizontally, a lower side wall 48 extending downwardly from the partition 46 , and an upper side wall 50 extending upwardly from the partition 46 . The first puncture needle 206 is mounted on the lower surface of the partition 46 , whereas the second puncture needle 208 is mounted on the upper surface of the partition 46 .
[0191] The lower side wall 48 surrounds the first puncture needle 206 . The lower side wall 48 has a height (vertical dimension), which is greater than the height of the first puncture needle 206 , so that the distal end (cutting face) of the first puncture needle 206 does not project downwardly from the lower end of the lower side wall 48 .
[0192] The upper side wall 50 surrounds the second puncture needle 208 . The upper side wall 50 has a height, which is greater than the height of the second puncture needle 208 , so that the distal end (cutting face) of the second puncture needle 208 does not project upwardly from the upper side wall 50 .
[0193] The connector 202 can be inserted into the drug holder 14 such that the outer circumferential surface of the upper side wall 50 serves as a sliding surface. More specifically, the connector 202 can slide longitudinally (vertically) along the double-ended needle 204 into fitting engagement with the drug holder 14 .
[0194] The mixing instrument 200 includes a lock mechanism 37 , which is identical in constitution to the lock mechanism 37 of the mixing instrument 10 . The lock mechanism 37 serves to releasably lock the drug holder 14 , the connector 202 , and the liquid holder 18 inseparably together, when the drug holder 14 , the connector 202 , and the liquid holder 18 are fitted together in a relative positional relation, such that the first puncture needle 206 pierces the first plug 26 and the second puncture needle 208 pierces the second plug 30 .
[0195] According to a modification of the lock mechanism 37 shown in FIG. 13 , the drug holder 14 may have lock members similar to the lock members 38 , 40 , and the liquid holder 18 may have ledges similar to the ledges 32 , 34 for engaging with the lock members.
[0196] FIG. 14 is an enlarged cross-sectional view, partially omitted from illustration, showing the double-ended needle 204 , which is formed integrally with the connector 202 , and nearby parts. As shown in FIG. 14 , the double-ended needle 204 has a lumen 210 (bore) extending longitudinally (axially), and which is open at opposite ends thereof. One of the openings of the lumen 210 opens at a cutting face 212 of the first puncture needle 206 , and the other opening of the lumen 210 opens at a cutting face 214 of the second puncture needle 208 .
[0197] Respective needle point angles θ 1 , θ 2 of the first puncture needle 206 and the second puncture needle 208 , and respective elastic characteristics of the first plug 26 and the second plug 30 are established, such that when the first plug 26 is pressed by the first puncture needle 206 and the second plug 30 is pressed by the second puncture needle 208 , the openings at the opposite ends of the lumen 210 of the double-ended needle 204 are sealed by the first plug 26 and the second plug 30 , respectively.
[0198] The first puncture needle 206 and the second puncture needle 208 may be made of materials, which are the same as the aforementioned materials of the drug holder 14 .
[0199] The first puncture needle 206 and the partition 46 may be formed integrally with each other, or alternatively, may be formed as separate members, which are secured together by adhesive bonding, welding, or the like. Likewise, the second puncture needle 208 and the partition 46 may be formed integrally with each other, or alternatively, may be formed as separate members, which are secured together by adhesive bonding, welding, or the like. For example, the first puncture needle 206 and the second puncture needle 208 may be made of metal, preferably SUS, whereas the connector 202 itself may be integrally molded from a resin material.
[0200] According to the third embodiment, as shown in FIG. 14 , the first puncture needle 206 and the second puncture needle 208 have respective cutting faces 212 , 214 , which are shaped as concave surfaces and are curved as viewed in vertical cross section. Typically, with respect to the first puncture needle 206 , the gradient of the cutting face 212 with respect to the axial direction increases progressively from a proximal end portion 216 toward a distal end portion 218 thereof.
[0201] The cutting face 212 of the first puncture needle 206 and the cutting face 214 of the second puncture needle 208 are oriented in one direction with respect to directions (horizontal directions in FIG. 14 ) perpendicular to the axial direction.
[0202] As shown in FIG. 14 , the height h 1 in the axial direction of the cutting face 212 of the first puncture needle 206 is smaller than the thickness t 1 (see FIG. 13 ) of the portion of the first plug 26 that is pierced by the first puncture needle 206 . Similarly, the height h 2 in the axial direction of the cutting face 214 of the second puncture needle 208 is smaller than the thickness t 2 (see FIG. 13 ) of the portion of the second plug 30 that is pierced by the second puncture needle 208 . The thicknesses t 1 , t 2 of such portions of the first plug 26 and the second plug 30 are preferably in the range from 1 to 4 mm, and more preferably, in the range from 2.0 to 2.5 mm.
[0203] FIG. 15 is an enlarged cross-sectional view, partially omitted from illustration, showing the first puncture needle 206 and nearby parts of the double-ended needle 204 of the mixing instrument 200 . Since the constitution of the first puncture needle 206 and the second puncture needle 208 are basically the same, the shape of the first puncture needle 206 of the double-ended needle 204 will typically be described below.
[0204] According to the third embodiment, as shown in FIG. 15 , a line segment A extends between the distal end portion 218 and the proximal end portion 216 of the cutting face 212 , and a line B normal to the line segment A extends from a deepest point on the concave surface (the cutting face 212 ). The point of intersection between the line segment A and the line B is positioned closer to the proximal end portion 216 of the cutting face 212 than the midpoint of the line segment A. The distance between the point of intersection and the distal end portion 218 of the cutting face 212 is set to a value, which is in the range of ⅗ to ⅘ the length of the line segment A. In other words, the cutting face (the concave surface) 212 has a curved shape, the concavity of which is formed more deeply near the proximal end portion 216 than near the distal end portion 218 . The center C 2 of the lumen 210 is closer to the proximal end portion 216 of the cutting face 212 than the central line C 1 of the first puncture needle 206 .
[0205] The angle θ 1 a formed between a line tangential to the distal end portion 218 of the cutting face 212 and the central line C 1 is preferably of a value in the range from 5° to 40°, and more preferably, in the range from 10° to 30°. If the angle θ 1 a is smaller than 5°, then the mechanical strength of the cutting edge is reduced to such an extent that when the cutting edge attempts to pierce the first plug 26 , the distal end tends to become bent, and it is difficult to pierce the first plug 26 . If the angle θ 1 a is in excess of 40°, then the cutting edge has an obtuse angle, thus presenting a large penetration resistance when the cutting edge attempts to pierce the first plug 26 , and making the first puncture needle 206 poor in operability.
[0206] The angle θ 1 b formed between a line tangential to the proximal end portion 216 of the cutting face 212 and the central line C 1 is preferably of a value in the range from 90° to 150°, and more preferably, in the range from 100° to 130°. If the angle θ 1 b is smaller than 90°, then the lumen 210 extends to the proximal end of the first puncture needle 206 , and the sealing capability at the time that the first puncture needle 206 contacts the first plug 26 is lost. Further, the extending portion of the lumen 210 tends to hollow out the first plug 26 , resulting in coring. If the angle θ 1 b is in excess of 150°, then when the first puncture needle 206 pierces the first plug 26 , the cutting face 212 does not come into full contact with the first plug 26 , resulting in poor sealing capability.
[0207] In the illustrated mixing instrument 200 , θ 1 a is set to 30° and θ 1 b is set to 110°.
[0208] The mixing instrument 200 according to the third embodiment is basically constituted as described above. Operations and advantages of the mixing instrument 200 will be described below.
[0209] As shown in FIG. 16 , the drug container 12 is held by the drug holder 14 , and is secured in the drug holder 14 by the restraint member 36 . The liquid container 16 also is mounted in the liquid holder 18 and is held by the liquid holder 18 .
[0210] Then, the connector 202 , with the double-ended needle 204 installed therein, is inserted into the drug holder 14 with the first puncture needle 206 being oriented toward the drug container 12 . The liquid holder 18 , with the liquid container 16 mounted therein, is inserted into the connector 202 with the second plug 30 being oriented toward the second puncture needle 208 .
[0211] During the insertion process, as shown in FIG. 16 , the first puncture needle 206 is pressed against the first plug 26 , and the second puncture needle 208 is pressed against the second plug 30 , whereby the first plug 26 and the second plug 30 are elastically deformed. FIG. 17 is an enlarged cross-sectional view, partially omitted from illustration, showing the first puncture needle 206 , the first plug 26 , and nearby parts at this time.
[0212] As described above, the respective needle point angles θ 1 , θ 2 of the first puncture needle 206 and the second puncture needle 208 , and the elastic characteristics of the first plug 26 and the second plug 30 are established, such that when the first puncture needle 206 is pressed by the first plug 26 and the second puncture needle 208 is pressed by the second plug 30 , openings in opposite ends of the lumen 210 of the double-ended needle 204 are sealed by the first plug 26 and the second plug 30 , respectively. When the double-ended needle 204 pierces the first plug 26 and the second plug 30 , the first plug 26 , which is pressed by the first puncture needle 206 , and the second plug 30 , which is pressed by the second puncture needle 208 , are elastically deformed, so that the first plug 26 is held in close contact with the cutting face 212 of the first puncture needle 206 and the second plug 30 is held in close contact with the cutting face 214 of the second puncture needle 208 . As a result, openings in opposite ends of the lumen 210 are sealed respectively by the first plug 26 and the second plug 30 .
[0213] According to the double-ended needles of the background art, the needle point angles are relatively small, so as to reduce the resistance that the double-ended needles undergo when the double-ended needles penetrate the plugs. Therefore, the double-ended needles penetrate the plugs easily. According to the double-ended needles of the background art, consequently, the openings in the opposite ends of the lumen cannot be sealed simultaneously by the plugs.
[0214] According to the third embodiment of the present invention, the needle point angles of the first puncture needle 206 and the second puncture needle 208 are greater than in the double-ended needles of the background art, thereby intentionally lowering the forces with which the first puncture needle 206 and the second puncture needle 208 penetrate (pierce) the first plug 26 and the second plug 30 . Therefore, the first plug 26 and the second plug 30 are elastically deformed significantly, so as to seal the openings in the opposite ends of the lumen 210 .
[0215] Whether or not the openings in the opposite ends of the lumen 210 can be sealed by the first plug 26 and the second plug 30 is determined by the forces applied by the first puncture needle 206 and the second puncture needle 208 to penetrate the first plug 26 and the second plug 30 (i.e., the sharpness of the needle points), together with the elastic characteristics, such as hardness and elongation characteristics, of the first plug 26 and the second plug 30 . Therefore, the needle point angles θ 1 , θ 2 of the first puncture needle 206 and the second puncture needle 208 are established in view of the elastic characteristics of the first plug 26 and the second plug 30 .
[0216] According to the third embodiment, the proximal end areas of the cutting faces 212 , 214 , which are formed as concave surfaces of the first puncture needle 206 and the second puncture needle 208 , function as chins. Since such chins increase the penetration resistance with which the first plug 26 and the second plug 30 are penetrated, when the distal ends of the first puncture needle 206 and the second puncture needle 208 bite into the first plug 26 and the second plug 30 , the chins temporarily bear the first plug 26 and the second plug 30 . Since the openings of the lumen 210 are positioned closer to the proximal end portions (the chins) of the cutting faces 212 , 214 than the needle central line C 1 , while the chins bear the first plug 26 and the second plug 30 , the openings in the opposite ends of the lumen 210 are sealed simultaneously by the first plug 26 and the second plug 30 .
[0217] When the liquid holder 18 is further pushed toward the drug holder 14 from the state shown in FIG. 16 , the mixing instrument 200 becomes assembled, as shown in FIG. 18 . The lock mechanism 37 is easily brought into the aforementioned first state. More specifically, the first engaging portions 38 b , 40 b of the arms 38 a , 40 a engage with the ledges 32 , 34 , respectively, of the drug holder 14 , and the second engaging portions 38 c , 40 c of the arms 38 a , 40 a engage with the ledges 52 , 54 , respectively, of the connector 22 . In this manner, the lock mechanism 37 operates to limit the mutual positional relation between the drug container 12 and the liquid container 16 , i.e., to prevent the containers 12 , 16 from unduly moving, thereby reliably maintaining the drug container 12 and the liquid container 16 in fluid communication with each other.
[0218] When the liquid holder 18 is further pushed toward the drug holder 14 from the state shown in FIG. 18 , and the distance that the first puncture needle 206 bites into the first plug 26 increases to a certain extent, the first plug 26 is no longer capable of withstanding the pressure from the first puncture needle 206 , and the first puncture needle 206 then pierces the first plug 26 . Similarly, when the distance that the second puncture needle 208 bites into the second plug 30 increases to a certain extent, the second plug 30 is no longer capable of withstanding the pressure from the second puncture needle 208 , and the second puncture needle 208 then pierces the second plug 30 . The cutting faces 212 , 58 of the first puncture needle 206 and the second puncture needle 208 move into the drug container 12 and the liquid container 16 , respectively, whereby the drug container 12 and the liquid container 16 are brought into fluid communication with each other by the double-ended needle 204 .
[0219] Inasmuch as a negative pressure is developed in the drug container 12 , the liquid in the liquid container 16 is attracted to and flows into the drug container 12 through the double-ended needle 204 . Thereafter, in order to mix the drug and the liquid in the drug container 12 , the mixing instrument 200 is shaken several times. The drug in the drug container 12 becomes diluted and dissolved by the liquid that has flowed into the drug container 12 .
[0220] After mixing of the first component and the second component is completed, the arms 38 a , 40 a of the lock members 38 , 40 on the liquid holder 18 are pressed inwardly toward the liquid holder 18 . The first engaging portions 38 b , 40 b of the arms 38 a , 40 a disengage from the ledges 32 , 34 of the drug holder 14 , whereas the second engaging portions 38 c , 40 c of the arms 38 a , 40 a remain in engagement with the ledges 52 , 54 of the connector 202 . In other words, the lock mechanism 37 is brought into the second state.
[0221] Then, the liquid holder 18 is pulled upwardly. The liquid holder 18 , which holds the liquid container 16 therein, can now be released (removed) from the drug holder 14 together with the connector 22 . Since the projections 38 d , 40 d are disposed on outer circumferential surfaces of the arms 38 a , 40 a , the user finds it easy to pull the liquid holder 18 , because the projections 38 d , 40 d function as a slip stop when the arms 38 a , 40 a are pressed laterally inward.
[0222] Then, the drug holder 14 , from which the connector 202 has been removed, is vertically inverted. The left and right side walls of the drug holder 14 are pressed inwardly to release the restraint member 36 out of engagement with the drug holder 14 . The drug container 12 is released (drops) from the drug holder 14 together with the restraint member 36 .
[0223] According to the third embodiment, as described above, the needle point angles of the first puncture needle 206 and the second puncture needle 208 , and the elastic characteristics of the first plug 26 and the second plug 30 are established, such that when the first plug 26 is pressed by the first puncture needle 206 and the second plug 30 is pressed by the second puncture needle 208 , the opening of the lumen 210 in the first puncture needle 206 is sealed by the first plug 26 , and the opening in the lumen 210 of the second puncture needle 208 is sealed by the second plug 30 . When the double-ended needle 204 pierces the first plug 26 and the second plug 30 , the first plug 26 , which is pressed by the first puncture needle 206 , and the second plug 30 , which is pressed by the second puncture needle 208 , are initially elastically deformed, so that the openings of the lumens 210 of the first puncture needle 206 and the second puncture needle 208 become sealed by the first plug 26 and the second plug 30 . Thereafter, the first puncture needle 206 and the second puncture needle 208 penetrate the first plug 26 and the second plug 30 , respectively.
[0224] Since the needle point angles of the first puncture needle 206 and the second puncture needle 208 , and the elastic characteristics of the first plug 26 and the second plug 30 are established as described above, openings in opposite ends of the lumen 210 are simultaneously sealed before the first puncture needle 206 and the second puncture needle 208 actually penetrate the first plug 26 and the second plug 30 , respectively.
[0225] Therefore, even if the timing at which the first puncture needle 206 penetrates the first plug 26 differs from the timing at which the second puncture needle 208 penetrates the second plug 30 , negative pressure in the drug container 12 is maintained and liquid is prevented from leaking out. More specifically, even if the first puncture needle 206 penetrates the first plug 26 before the second puncture needle 208 penetrates the second plug 30 , since the opening of the lumen 210 of the second puncture needle 208 is sealed by the second plug 30 , negative pressure in the drug container 12 is maintained. Further, even if the second puncture needle 208 penetrates the second plug 30 before the first puncture needle 206 penetrates the first plug 26 , since the opening of the lumen 210 of the first puncture needle 206 is sealed by the first plug 26 , liquid is prevented from leaking out.
[0226] According to the present invention, therefore, even if the timing at which the first puncture needle 206 penetrates the first plug 26 of the drug container 12 differs from the timing at which the second puncture needle 208 penetrates the second plug 30 of the liquid container 16 , negative pressure in the drug container 12 is maintained and liquid is prevented from leaking out. Accordingly, a mixing instrument 200 is provided, which can be handled easily without causing handling errors.
[0227] According to the third embodiment, each of the respective cutting faces 212 , 214 of the first puncture needle 206 and the second puncture needle 208 is formed as a curved concave surface, and the point of intersection between a line segment, which extends between the proximal end portion and the distal end portion of each of the cutting faces 212 , 214 , and the line normal to the line segment, which extends from the deepest point on the concave surface, is positioned closer to the proximal end portion of the cutting face than the midpoint of the line segment. Also, the center of the lumen 210 is closer to the proximal end portion of the cutting face than the central line of each puncture needle. With this arrangement, when the distal ends of the first puncture needle 206 and the second puncture needle 208 bite into the first plug 26 and the second plug 30 , the areas (chins) of the cutting faces 212 , 214 near the proximal end portions thereof temporarily bear the first plug 26 and the second plug 30 . Since the openings of the lumen 210 are positioned closer to the chins, the openings in the opposite ends of the lumen 210 are reliably and simultaneously sealed.
[0228] According to the third embodiment, when the drug holder 14 , the connector 202 , and the liquid holder 18 are fitted together, the drug holder 14 , the connector 202 , and the liquid holder 18 slide against each other and are guided for relative axial movement. Therefore, the first puncture needle 206 and the second puncture needle 208 can pierce the first plug 26 and the second plug 30 , respectively, accurately and simply in the axial direction. Therefore, the mixing instrument 200 can be handled more easily.
[0229] According to the third embodiment, when the drug holder 14 , the connector 202 , and the liquid holder 18 are coupled together, they are locked by the lock mechanism 37 so that they can be handled in their entirety as the integrated mixing instrument 10 . Consequently, it is easy to perform the process of shaking the mixing instrument 200 to accelerate mixing of the first component and the second component.
Fourth Embodiment
[0230] FIG. 19 is an exploded perspective view of a mixing instrument 300 according to a fourth embodiment of the present invention. FIG. 20 is a cross-sectional view of the mixing instrument 300 according to the fourth embodiment of the present invention. Components of the mixing instrument 300 according to the fourth embodiment, which have identical or similar functions and advantages to those of the mixing instrument 100 according to the second embodiment, are denoted by identical reference characters, and such features will not be described in detail below.
[0231] The mixing instrument 300 includes a connector 302 , which is used in place of and differs in constitution from the connector 122 of the mixing instrument according to the second embodiment. The connector 302 has two integral double-ended needles 304 A, 304 B, which serve to bring the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B into fluid communication with each other.
[0232] The mixing instrument 300 includes a lock mechanism 137 , which is constitutively identical to the lock mechanism 137 of the mixing instrument 100 . The lock mechanism 137 serves to releasably lock the drug holder 114 , the connector 302 , and the liquid holder 118 inseparably together when the drug holder 114 , the connector 302 , and the liquid holder 118 are fitted together in a relative positional relation, such that the first puncture needles 306 A, 306 B pierce the first plugs 126 A, 126 B and the second puncture needles 308 A, 308 B pierce the second plugs 130 A, 130 B.
[0233] According to a modification of the lock mechanism 137 shown in FIG. 19 , lock members, which are similar to the lock members 138 , 140 , may be provided on the drug holder 114 , and ledges, which are similar to the ledges 132 , 134 for engaging the lock members, may be provided on the liquid holder 118 .
[0234] As shown in FIGS. 19 and 20 , the two double-ended needles 304 A, 304 B have respective first puncture needles 306 A, 306 B for piercing the first plugs 126 A, 126 B, respectively, and respective second puncture needles 308 A, 308 B for piercing the second plugs 130 A, 130 B, respectively. The two double-ended needles 304 A, 304 B are joined together integrally through the connector 302 .
[0235] FIG. 21 is an enlarged cross-sectional view, partially omitted from illustration, showing the pair of double-ended needles 304 A, 304 B and nearby parts. The double-ended needles 304 A, 304 B have respective lumens (bores) 310 A, 310 B extending longitudinally (axially) therethrough, and which are open at opposite ends thereof. One of the openings of the lumens 310 A, 310 B opens into the cutting faces 312 A, 312 B of the first puncture needles 306 A, 306 B, whereas the other opening opens into the cutting faces 314 A, 314 B of the second puncture needles 308 A, 308 B.
[0236] Respective needle point angles θ 1 A, θ 1 B, θ 2 A, θ 2 B of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B, and respective elastic characteristics of the first plugs 126 A, 126 B and the second plugs 130 A, 130 B are established, such that when the first plugs 126 A, 126 B are pressed by the first puncture needles 306 A, 306 B and the second plugs 130 A, 130 B are pressed by the second puncture needles 308 A, 308 B, the openings in opposite ends of the lumens 310 A, 310 B of the double-ended needles 304 A, 304 B are sealed by the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively.
[0237] The first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B may be made of materials, which are the same as the aforementioned materials of the drug containers 112 A, 112 B.
[0238] The first puncture needles 306 A, 306 B and the partition 146 may be formed integrally with each other, or alternatively, may be separate members, which are secured together by adhesive bonding, welding, or the like. Similarly, the second puncture needles 308 A, 308 B and the partition 146 may be formed integrally with each other, or alternatively, may be separate members, which are secured together by adhesive bonding, welding, or the like. For example, the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B may be made of metal, preferably SUS, whereas the connector 302 itself may be integrally molded from a resin material.
[0239] According to the third embodiment, as shown in FIG. 21 , the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B have respective cutting faces 312 A, 312 B, 314 A, 314 B, which are shaped as concave surfaces and are curved as viewed in vertical cross section.
[0240] In one of the double-ended needles 304 A, the cutting face 312 A of the first puncture needle 306 A and the cutting face 314 A of the second puncture needle 308 A face in the same direction (i.e., the leftward direction shown in FIG. 20 ), in a direction perpendicular to the axial direction. In the other double-ended needle 304 B, the cutting face 312 B of the first puncture needle 306 B and the cutting face 314 B of the second puncture needle 308 B face in the same direction (i.e., the rightward direction shown in FIG. 21 ), in a direction perpendicular to the axial direction. The double-ended needle 304 A and the double-ended needle 304 B face away from each other in respective directions in which the double-ended needle 304 A and the double-ended needle 304 B are spaced from each other (i.e., in leftward and rightward directions as shown in FIG. 20 ).
[0241] According to a modification of the fourth embodiment, the double-ended needles 304 A, 304 B shown in FIG. 21 may be inverted 180° about central axes thereof. More specifically, the cutting face 312 A of the first puncture needle 306 A and the cutting face 312 B of the first puncture needle 306 B may face toward each other, and the cutting face 314 A of the second puncture needle 308 A and the cutting face 314 B of the second puncture needle 308 B may face toward each other.
[0242] As shown in FIG. 21 , in the double-ended needle 304 A, the height h 1 A in the axial direction of the cutting face 312 A of the first puncture needle 306 A is smaller than the thickness t 1 A (see FIG. 20 ) of the portion of the first plug 126 A that is pierced by the first puncture needle 306 A. Further, the height h 12 in the axial direction of the cutting face 314 A of the second puncture needle 308 A is smaller than the thickness t 2 A (see FIG. 20 ) of the portion of the second plug 130 A that is pierced by the second puncture needle 308 A. The thicknesses t 1 A, t 2 A of the first plug 126 A and the second plug 130 A should preferably be in the range from 1 to 4 mm, and more preferably, in the range from 2.0 to 2.5 mm.
[0243] In the other double-ended needle 304 B, the relationship between the height in the axial direction of the cutting face 312 B of the first puncture needle 306 B and the thickness of the portion of the first plug 126 B that is pierced by the first puncture needle 306 B, and the relationship between the height in the axial direction of the cutting face 314 B of the second puncture needle 308 B and the thickness of the portion of the second plug 130 B that is pierced by the second puncture needle 308 B are the same as in the double-ended needle 304 A.
[0244] According to the fourth embodiment, as with the third embodiment (see FIG. 4 ), the point of intersection between the line segment that extends between the distal end portion 318 of the cutting face 312 A and the proximal end portion 316 thereof, and the line normal to the line segment, which extends from the deepest point on the concave surface (cutting face), is positioned closer to the proximal end portion of the cutting face than the midpoint of the line segment. Also, the center of the lumen 310 A is closer to the proximal end portion 316 of the cutting face 312 A than the central line of the puncture needle. In other words, the cutting face (concave surface) 312 A is more deeply concave near the proximal end portion 316 of the cutting face 312 A than near the distal end portion 318 thereof. The first puncture needle 306 B and the second puncture needle 308 B of the double-ended needle 304 B are similar in shape to the first puncture needle 306 A of the double-ended needle 304 A.
[0245] The connector 302 has a partition 146 extending horizontally, a lower side wall 148 extending downwardly from the partition 146 , and an upper side wall 150 extending upwardly from the partition 146 . The two first puncture needles 306 A, 306 B are mounted on the lower surface of the partition 146 , whereas the two second puncture needles 308 A, 308 B are mounted on the upper surface of the partition 146 . The connector 302 may be made of materials, which are the same as the aforementioned materials of the drug holder 114 .
[0246] The lower side wall 148 surrounds the first puncture needles 306 A, 306 B in their entirety. The lower side wall 148 has a height (vertical dimension), which is greater than the height of the first puncture needles 306 A, 306 B, so that the distal ends (cutting faces) of the two first puncture needles 306 A, 306 B do not project downwardly from the lower end of the lower side wall 148 .
[0247] The upper side wall 150 surrounds the second puncture needles 308 A, 308 B in their entirety. The upper side wall 150 has a height (vertical dimension), which is greater than the height of the second puncture needles 308 A, 308 B, so that the distal ends (cutting faces) of the two second puncture needles 308 A, 308 B do not project upwardly from the upper side wall 150 . The upper side wall 150 has ledges 152 , 154 projecting horizontally outwardly from the left and right sides of the upper end thereof. The ledges 152 , 154 have respective holes 152 a , 154 a formed vertically therethrough.
[0248] The connector 302 can be inserted into the drug holder 114 , with the outer circumferential surface of the upper side wall 150 thereof serving as a sliding surface. More specifically, the connector 302 can move longitudinally (vertically) along the double-ended needles 304 A, 304 B with respect to the drug holder 114 .
[0249] The liquid holder 118 can be inserted into the inside of the upper side wall 150 of the connector 302 , with the outer circumferential surface of the lower end portion thereof serving as a sliding surface. More specifically, the liquid holder 118 can move longitudinally along the double-ended needles 304 A, 304 B with respect to the connector 302 .
[0250] The mixing instrument 300 according to the fourth embodiment is basically constituted as described above. Operations and advantages of the mixing instrument 300 will be described below.
[0251] As shown in FIG. 20 , the drug containers 112 A, 112 B are stored in the drug holder 114 and secured to the drug holder 114 by the restraint member 136 . The liquid containers 116 A, 116 B are mounted in the liquid holder 118 and held by the liquid holder 118 .
[0252] Then, the connector 302 , with the two double-ended needles 304 A, 304 B installed therein, is inserted into the drug holder 114 , such that the two first puncture needles 306 A, 306 B are oriented toward the drug containers 112 A, 112 B. Further, the liquid holder 118 , with the two liquid containers 116 A, 116 B mounted therein, is inserted into the connector 302 , such that the second plugs 130 A, 130 B are oriented toward the second puncture needles 308 A, 308 B.
[0253] During the insertion process, as shown in FIG. 22 , the first puncture needles 306 A, 306 B are pressed against the first plugs 126 A, 126 B, and the second puncture needles 308 A, 308 B are pressed against the second plugs 130 A, 130 B. Thus, the first plugs 126 A, 126 B and the second plugs 130 A, 130 B are elastically deformed. At this time, the first plugs 126 A, 126 B and the second plugs 130 A, 130 B are elastically deformed significantly, as with the first plug 26 (see FIG. 17 ) according to the third embodiment.
[0254] As described above, respective needle point angles θ 1 A, θ 2 A, θ 3 A, θ 4 A of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B, and respective elastic characteristics of the first plugs 126 A, 126 B and the second plugs 130 A, 130 B are established, such that when the first puncture needles 306 A, 306 B are pressed against the first plugs 126 A, 126 B and the second puncture needles 308 A, 308 B are pressed against the second plugs 130 A, 130 B, openings in opposite ends of the lumens 310 A, 310 B of the double-ended needles 304 A, 304 B are sealed by the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively. In the illustrated embodiment, θ 1 A to θ 4 A are set to 30°, and θ 1 B to θ 4 B are set to 130°.
[0255] When the pair of double-ended needles 304 A, 304 B pierce the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, the first plugs 126 A, 126 B, which are pressed by the first puncture needles 306 A, 306 B, and the second plugs 130 A, 130 B, which are pressed by the second puncture needles 308 A, 308 B, are elastically deformed initially, so that the first plugs 126 A, 126 B are held in close contact with the cutting faces 312 A, 312 B of the first puncture needles 306 A, 306 B, and the second plugs 130 A, 130 B are held in close contact with the cutting faces 314 A, 314 B of the second puncture needles 308 A, 308 B. As a result, openings in opposite ends of the lumens 310 A, 310 B are sealed respectively by the first plugs 126 A, 126 B and the second plugs 130 A, 130 B.
[0256] With the double-ended needles of the background art, the needle point angles are relatively small in order to reduce the resistance that the double-ended needles undergo when they penetrate the plugs. Therefore, the double-ended needles can penetrate the plugs easily. According to the double-ended needles of the background art, consequently, openings in opposite ends of the lumen cannot be simultaneously sealed by the plugs.
[0257] According to the fourth embodiment of the present invention, the needle point angles of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B are greater than those in the double-ended needles of the background art, thereby intentionally lowering the forces with which the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B penetrate (pierce) the first plugs 126 A, 126 B and the second plugs 130 A, 130 B. Therefore, the first plugs 126 A, 126 B and the second plugs 130 A, 130 B are elastically deformed significantly, so as to seal the openings in the opposite ends of the lumens.
[0258] Whether or not the openings in the opposite ends of the lumens 310 A, 310 B can be sealed by the first plugs 126 A, 126 B and the second plugs 130 A, 130 B is determined by the forces applied by the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B to penetrate the first plugs 126 A, 126 B and the second plugs 130 A, 130 B (i.e., the sharpness of the needle points), together with elastic characteristics, such as hardness and elongation characteristics, of the first plugs 126 A, 126 B and the second plugs 130 A, 130 B. Therefore, the needle point angles of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B are established in view of the elastic characteristics of the first plugs 126 A, 126 B and the second plugs 130 A, 130 B.
[0259] According to the fourth embodiment, the proximal end areas of the cutting faces 312 A, 312 B, 314 A, 314 B, which are formed as concave surfaces, of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B function as chins. Since such chins increase the penetration resistance with which the first plugs 126 A, 126 B and the second plugs 130 A, 130 B are penetrated when the distal ends of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B bite into the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, the chins temporarily bear the first plugs 126 A, 126 B and the second plugs 130 A, 130 B. Since the openings of the lumens 310 A, 310 B are positioned closer to the proximal end portions (the chins) of the cutting faces than the central lines of the double-ended needles 304 A, 304 B, while the chins bear the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, the openings in the opposite ends of the lumens are simultaneously sealed by the first plugs 126 A, 126 B and the second plugs 130 A, 130 B.
[0260] When the liquid holder 118 is further pushed toward the drug holders 114 from the state shown in FIG. 22 , the mixing instrument 300 is assembled together, as shown in FIG. 23 . The lock mechanism 137 is easily brought into the first state, as described above. More specifically, the first engaging portions 138 b , 140 b of the arms 138 a , 140 a engage with the respective ledges 132 , 134 of the drug holder 114 , and the second engaging portions 138 c , 140 c of the arms 138 a , 140 a engage the respective ledges 152 , 154 of the connector 302 . The lock mechanism 137 thus operates to limit the mutual positional relation between the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B, i.e., to prevent the containers 112 A, 112 B, 116 A, 116 B from unduly moving, thereby reliably maintaining the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B in fluid communication with each other.
[0261] When the liquid holder 118 is further pushed toward the drug holder 114 from the state shown in FIG. 22 , the distance at which the first puncture needles 306 A, 306 B bite into the first plugs 126 A, 126 B increases to a certain extent, and the first plugs 126 A, 126 B are no longer capable of withstanding the pressure from the first puncture needles 306 A, 306 B, which then pierce the first plugs 126 A, 126 B. Similarly, when the distance at which the second puncture needles 308 A, 308 B bite into the second plugs 130 A, 130 B increases to a certain extent, the second plugs 130 A, 130 B are no longer capable of withstanding the pressure from the second puncture needles 308 A, 308 B, which then pierce the second plugs 130 A, 130 B. The cutting faces of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B move respectively into the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B. At this time, the drug containers 112 A, 112 B and the liquid containers 116 A, 116 B are brought into fluid communication with each other through the double-ended needles 304 A, 304 B.
[0262] Inasmuch as a negative pressure is developed in the two drug containers 112 A, 112 B, the liquid in the liquid containers 116 A, 116 B is attracted to and flows into the drug containers 112 A, 112 B through the two double-ended needles 304 A, 304 B. Thereafter, the mixing instrument 300 is shaken several times. At this time, the drugs in the drug containers 112 A, 112 B become diluted and dissolved by the liquids, which have flowed into the drug containers 112 A, 112 B.
[0263] After mixing of the drugs and the liquids is completed, the arms 138 a , 140 a of the lock members 138 , 140 on the liquid holder 118 are pressed inwardly toward the liquid holder 118 . The first engaging portions 138 b , 140 b of the arms 138 a , 140 a disengage from the ledges 132 , 134 of the drug holder 114 , whereas the second engaging portions 138 c , 140 c of the arms 138 a , 140 a remain in engagement with the ledges 152 , 154 of the connector 122 . In other words, the lock mechanism 137 is brought into the second state.
[0264] Then, the liquid holder 118 is pulled upwardly. The liquid holder 118 , which holds the liquid containers 116 A, 116 B therein, can be released (removed) from the drug holder 114 together with the connector 302 . Since the projections 138 d , 140 d are disposed on the arms 138 a , 140 a , the user finds it easy to pull the liquid holder 118 due to the fact that the projections 138 d , 140 d function as a slip stop.
[0265] Then, the drug holder 114 , from which the connector 302 has been removed, is vertically inverted. The left and right side walls of the drug holder 114 are pressed inwardly to cause the engaging protrusion 141 of the restraint member 136 to become disengaged from the engaging recess 143 of the drug holder 114 . At this time, the drug containers 112 A, 112 B are released (drop) from the drug holder 114 together with the restraint member 136 .
[0266] According to the fourth embodiment, as described above, the double-ended needle 304 A and the double-ended needle 304 B face away from each other in respective directions in which the double-ended needle 304 A and the double-ended needle 304 B are spaced from each other. Consequently, when the double-ended needles 304 A, 304 B pierce the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively, forces acting horizontally on the double-ended needles 304 A, 304 B cancel each other out. Therefore, sliding resistance between the connector 302 and the drug holder 114 is prevented from increasing at the time that the connector 302 is inserted into the drug holder 114 .
[0267] Further, according to the fourth embodiment, as described above, the needle point angles of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B, and elastic characteristics of the first plugs 126 A, 126 B and the second plugs 130 A, 130 B are established, such that when the first plugs 126 A, 126 B are pressed against the first puncture needles 306 A, 306 B, and the second plugs 130 A, 130 B are pressed against the second puncture needles 308 A, 308 B, the openings of the lumens 310 A, 310 B of the first puncture needles 306 A, 306 B are sealed by the first plugs 126 A, 126 B, respectively, and the openings of the lumens 310 A, 310 B of the second puncture needles 308 A, 308 B are sealed by the second plugs 130 A, 130 B, respectively. When the double-ended needles 304 A, 304 B pierce the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, the first plugs 126 A, 126 B, which are pressed by the first puncture needles 306 A, 306 B, and the second plugs 130 A, 130 B, which are pressed by the second puncture needles 308 A, 308 B, are elastically deformed initially, so that the openings of the lumens 310 A, 310 B of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B are sealed respectively by the first plugs 126 A, 126 B and the second plugs 130 A, 130 B. Thereafter, the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B pierce the first plug 26 and the second plugs 130 A, 130 B, respectively. In other words, the openings at opposite ends of the lumens 310 A, 310 B are simultaneously sealed before the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B penetrate through the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively.
[0268] Consequently, even if the first puncture needles 306 A, 306 B penetrate the first plugs 126 A, 126 B before the second puncture needles 308 A, 308 B have penetrated the second plugs 130 A, 130 B, since the openings of the lumens of the second puncture needles 308 A, 308 B are sealed by the second plugs 130 A, 130 B, negative pressure in the drug containers 112 A, 112 B can be maintained. Further, even if the second puncture needles 308 A, 308 B penetrate the second plugs 130 A, 130 B before the first puncture needles 306 A, 306 B have penetrated the first plugs 126 A, 126 B, since the openings of the lumens of the first puncture needles 306 A, 306 B are sealed by the first plugs 126 A, 126 B, liquids are prevented from leaking out.
[0269] Consequently, negative pressure in the drug containers 112 A, 112 B is maintained, and the first components are prevented from leaking out, even if the timing at which the first puncture needles 306 A, 306 B penetrate the first plugs 126 A, 126 B differs from the timing at which the second puncture needles 308 A, 308 B penetrate the second plugs 130 A, 130 B. Accordingly, a mixing instrument 300 is provided, which can be handled easily without causing handling errors.
[0270] According to the fourth embodiment, the cutting faces of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B are formed as concave surfaces, and the point of intersection between a line segment that extends between the proximal end portion of each of the cutting faces and the distal end portion thereof, and the line normal to the line segment, which extends from the deepest point on the concave surface, is positioned closer to the proximal end portion of the cutting face than the midpoint of the line segment. Also, the center of the lumen is closer to the proximal end portion of the cutting face than the central line of each puncture needle. With this arrangement, when the distal ends of the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B bite into the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, the proximal end areas (i.e., chins) of the cutting faces temporarily bear the first plugs 126 A, 126 B and the second plugs 130 A, 130 B. Since the openings at the opposite ends of the lumens 310 A, 310 B are positioned closer to the chins, the openings at the opposite ends of the lumens 310 A, 310 B are reliably and simultaneously sealed.
[0271] According to the fourth embodiment, when the drug holder 114 , the connector 302 , and the liquid holder 118 are fitted together, the components slide against each other and are guided for relative axial movement. Therefore, the first puncture needles 306 A, 306 B and the second puncture needles 308 A, 308 B are capable of piercing the first plugs 126 A, 126 B and the second plugs 130 A, 130 B, respectively, accurately and simply in the axial direction. Therefore, the mixing instrument 300 can be handled more easily.
[0272] According to the fourth embodiment, when the drug holder 114 , the connector 302 , and the liquid holder 118 are coupled together, the drug holder 114 , the connector 302 , and the liquid holder 118 become locked by the lock mechanism 37 , so that they can be handled in their entirety as an integrated mixing instrument 300 . Consequently, it is easy to perform the process of shaking the mixing instrument 300 in order to accelerate mixing of the first component and the second component.
[0273] The present invention is not limited to the above arrangements, but various other arrangements may be adopted based on the content of the present description. | A mixing apparatus for mixing a first component and a second component comprises: a first vessel which has a negative internal pressure and houses the first component; a second vessel which houses the second component; and a double-ended needle which allows communication between the first vessel and the second vessel when a first stopper element and a second stopper element have been pierced through by the needle. Penetration-resistance increasing parts which have a greater penetration resistance with respect to the first stopper element and the second stopper element than tip end tubes are respectively provided on a first puncture needle and a second puncture needle of the double-ended needle at positions further towards the base end than the tip end tubes. The axial heights of the edge faces of the tip end tubes are both less than the thicknesses of the first stopper element and of the second stopper element. | 0 |
BACKGROUND OF THE INVENTION
[0001] The present invention relates to a method for determining the functional relation of several pumps in an installation, which may be controlled in their rotational speed.
[0002] Particularly in heating installations of larger buildings or of a more complex construction type, a multitude of pumps, i.e. centrifugal pumps, with an electric motor driving these, are installed, in order to reliably supply the individual installation parts with fluid or heat. Modern pumps of this type are typically controlled by frequency converter, so that with regard to power, they may supply over a wide range and may be operated in a different manner depending on requirement. If a multitude of such pumps cooperate in an installation, be it by way of parallel connection, series connection or a combination of this, then a complex hydraulic network results, which from the start must be known with regard to its structure, i.e. with regard to its functional relationship, in order to be able to energetically optimize the operation of the entirety of the pumps. Particularly with older installations it may be the case that the hydraulic connection plan is no longer available. Even this may no longer be unambiguously determined with a sufficient accuracy by way of the existing pipework. It is then necessary to determine the functional relationship of the pumps.
BRIEF SUMMARY OF THE INVENTION
[0003] Against this background, it is an object of the present invention to provide a method for determining the functional relationship of several pumps in an installation, which may be controlled in their rotational speed, with which this functional relationship, thus quasi the hydraulic circuit of the installation, may be determined in an unambiguous manner.
[0004] According to the present invention, the above object is achieved by the features specified in the independent claim(s). Advantageous designs of the present invention are specified in the dependent claims, the subsequent description and the drawing.
[0005] According to the present invention, the functional relationship of several pumps in an installation which are controllable in their rotational speed, is determined by way of changing the rotational speed with regard to at least one pump, and determining at least one functional relationship of the installation from the hydraulic reaction resulting therefrom. Depending on the scope of the functional relationship to be determined, one may activate one or also more pumps with a changed rotational speed, in order to determine this relationship. Thus, for example, for ascertaining whether two pumps are connected in parallel or in series, it is sufficient to activate one of the pumps with an increased rotational speed, in order then, by way of the pressure measurement or throughput measurement compared to the initial condition, to determine in which way these pumps are connected.
[0006] According to one advantageous further formation of the present invention, the method is applied in three basic method steps:
[0007] a) In a first method step, all pumps built into the installation are preferably activated with a constant rotational speed, and a hydraulic variable is detected for each pump or for each consumer assigned to the pumps or for each consumer group if several consumers are assigned to a pump. Typically, the pumps thereby are activated with a constant average rotation speed, and specifically until quasi stationary values set in. These values are detected either with regard to the pump or to the consumer, and thereby it is optionally the case of the pressure or the volume flow, wherein these do not necessarily need to be detected in a direct manner, but may also be indirectly determined in a manner known per se by way of other variables, e.g. electrical variables of the drive of the pumps manner;
[0008] b) Then one after the other, in each case one of the pumps or several pumps are activated with a changed rotational speed, and the change of the hydraulic variable which results in each case is detected. Thus, each individual pump is typically activated with a rotational speed, which is increased compared to step a), and then the changes of the hydraulic variables, which result either on the consumer side or the pump side, are detected, wherein on the part of the pump, the hydraulic variables of the pump activated with the changed rotational speed as well as those of the other pumps are detected. Basically thereby, it is of no significance as to whether the changed rotational speed is one which is increased or decreased compared to the rotational speed according to step a, but as a rule a rotation speed which is greater in comparison is advantageously selected. It is to be understood that in the same manner, one after the other, all pumps must be operated either with a rotational speed which is increased or reduced compared to the rotation speed in step a, in order to detect the hydraulic changes of the hydraulic variables which thereby result.
[0009] c) In a third method step, then after the changes of the hydraulic variables are detected, the assignment of the pumps or pump group to the consumers or consumer groups is determined by way of these detected hydraulic variable changes.
[0010] The method according to a preferred embodiment of the present invention, with the advantageous application of pumps controlled by a frequency converter, may be implemented into the digital frequency converter electronics, wherein then a data connection of the pumps amongst one another should be formed, be it wireless per radio or for example via a network cable, in order to suitably coordinate the pumps with regard to the method and furthermore to determine the hydraulic variables at the pumps or at the consumers. However, this method may also be implemented in a separate control, which is data-connected to the pumps and, as the case may be, to the consumers or their sensors in a wireless or wired manner.
[0011] The method according to a preferred embodiment of the present invention offers the huge advantage that it may be carried out with equipment which is present in the heating installation in any case, i.e. with the exception of the control and the data connection, one does not need to provide any additional measures with regard to the installation. The control and data connection may however be integrated into the pumps with only low additional costs, given a suitable design of these pumps.
[0012] The evaluation of the thus determined hydraulic variables and variable changes may be effected in a simple manner. Thereby, the methods differ essentially as to whether the hydraulic variables or their changes are detected on the part of the pump or on the part of the consumer.
[0013] If the variables are detected on the part of the consumer (on the consumer side), i.e. at a consumer or a consumer group if several consumers are assigned to a pump, then according to a further formation of the method of the present invention, at the pumps which on activation with a changed rotational speed produce the same consumer-side hydraulic variable changes, one ascertains that these are assigned to a pump group. A pump group consists of two or more pumps which are connected directly in parallel and/or series. With the consumer side variable detection, the first assignment step thus lies in determining whether the pumps are hydraulically connected as individual pumps or in groups, in the installation.
[0014] According to a further advantageous design of the method of the present invention, when, with a change in rotational speed of one or consecutively also of several pumps, only one consumer or a consumer group is influenced in an increasing or reducing manner according to the change in rotational speed, one ascertains that then the pump or the pumps are directly assigned to the respectively influenced consumer or to the respectively influenced consumer group, i.e. no further pumps are located in the conduit path between the previously mentioned pump/previously mentioned pumps, and the consumer or the consumer group.
[0015] In order to determine the functional relationship within a pump group, according to a further formation of the method according to the present invention, one envisages activating all pumps of the pump group with a constant rotational speed, thus for example according to method step a), wherein then the pressure difference produced by the respective pumps is detected at the respective pump by a differential pressure sensor. Then, one after the other, in each case one of the pumps is activated with a changed, preferably increased pressure and the differential pressure change or rotational speed changes of the other pumps which result thereby is detected, whereupon then the assignment of the pumps within the pump group is determined by way of the detected variable changes, as results by way of the hydraulic laws with the parallel connection and series connection of the pumps. In order to be able to ascertain the functional relationship within the pump group, either the pumps of a pump group are activated subsequently with a changed, preferably increased rotational speed and the throughput quantity through the respective pump is detected, or however the pumps are activated one after the other in each case for producing an increased differential pressure, wherein then the pressure levels, which sets in, of these and of the other pumps, is detected, and the assignment of the pumps within the pump group is ascertained by way of the changes which result as the case may be.
[0016] According to one advantageous further formation of the method according to the present invention, the pump or the pumps, which with their rotational speed change influence two or more consumers or consumer groups in a increasing or reducing manner according to the rotational speed change, is or are assigned according to the number of influenced consumers or consumer groups. Thus one may determine which pumps affect which consumers and thus the assignment of the pumps amongst one another may be determined.
[0017] It is particularly advantageous if, with the method according to the present invention, it is not the absolute values of the hydraulic variables or variable changes which are detected, but merely the direction, since then on the one hand one may apply a very simple sensor means which is not calibrated, and on the other hand the evaluation only requires a low computational effort as well as reduced memory requirement. Thus for carrying out the method according to the present invention, it is sufficient to detect whether the respectively detected hydraulic variable increases, reduces or remains the same, given a change in the rotational speed or pressure of a determined pump. Thus, it is merely a question of a simplified direction detection, which is adequately accurate when it may be categorized into three groups, specifically larger (+1), smaller (−1) and equal (0).
[0018] If the method according to the present invention is to be carried out by way of detecting the hydraulic variables of the pumps, thus for example the pressure or the volume flow, which as a rule, is more favorable with regard to the installation, since heating circulation pumps controlled by a frequency converter are nowadays usually equipped with differential pressure sensors, then it is useful firstly once to determine with the method as to whether the hydraulic installation is a hydraulic network or whether it consists of two or more installation parts which are independent of one another. With installation parts which are independent of one another, a rotational-speed-changed or pressure-increased activation of the pump has no influence on the other part, so that in this manner, with the method, one may firstly be able to determine the installation parts which are hydraulically connected to one another.
[0019] The method with hydraulic variables of the pump, typically pressure or differential pressure or volume flow are detected for determining the functional relationship, in turn differ fundamentally from one another.
[0020] If, as is envisaged according to a further formation of the present invention, the volume flows and thus volume flow changes as hydraulic changes are detected at all pumps, then the functional relationship of the pumps may be determined as follows, wherein hereinafter the changes on activating a pump with an increasing rotational speed are noted. However, one must emphasize that the changes may also be used in an analogous manner if the activation is effected with a reduced rotational speed:
[0021] A matrix is formed, in which the hydraulic changes of at least one hydraulically independent installation part are detected, wherein advantageously here too, the direction changes are detected, thus the matrix is formed with the values 0 for remaining the same, +1 for increasing and −1 for reducing. Thereby, for each pump, the changes of the hydraulic variables at this pump as well as at the other pumps, which result with its activation with a changed rotational speed, are specified in rows. Moreover, a column is assigned to each pump, whereby the rows within the matrix are sorted, and specifically increasing from the top to the bottom according to their number of increasing changes (+1), and the columns increasing from the left to the right according to their number of increasing changes (+1). Thus the changes of the pump which produces the fewest increasing changes in the entirety of the pumps are detected in the uppermost row of the matrix, and the associated column of this pump connects at the same location at the top left of the matrix. The pump with the most increasing changes is in the last, thus lowermost row, wherein then also the last column, thus the column at the far right, is assigned to this pump. It is to be understood that the matrix may also be arranged exactly in the reverse manner, since it is compellingly mirror-symmetrical with regard to its diagonals.
[0022] The matrix is divided by a diagonal, which runs from the one to the other matrix axis, which quasi intersects or erases the fields of the matrix in which an increasing variable change, thus typically a 1 is located. These are the fields with which the pump assignment of the column and row corresponds. By way of observing the number of increasing changes of the hydraulic variables in each column below the previously mentioned diagonal or in each row above the previously mentioned diagonal, one may determine which pumps are connected hydraulically in parallel and which ones hydraulically in series.
[0023] With the pumps with which an equal number of increasing changes (+1) of the hydraulic variables in the columns below the diagonal or in the rows above the diagonal of the matrix is given, it is the case of pumps connected in parallel, thus of those pumps which deliver from the same conduit and from the same pressure level.
[0024] According to a further formation of the method according to the present invention, pumps which are assigned directly to a consumer or to a consumer group are determined, i.e. which deliver into such a consumer or a consumer group without intermediate connection of further pumps. Hereby, it is the case of pumps with which no increasing change of the hydraulic variables in a row below the diagonal or in a column above the diagonal of the matrix is present. The first pump of the matrix may belong to this as the case may be, which is assigned to the first row and the first column and lies on the diagonal. This results from the row sorting or the column sorting.
[0025] According to a further formation of the method according to the present invention, by way of evaluating the matrix, one determines how many pumps are hydraulically connected in series upstream of the respectively considered pump. For this, the number of increasing changes of the hydraulic variables in the columns below the diagonals or in the rows above the diagonals of the matrix, are detected. This number corresponds to the number of the pumps which are connected in series upstream of the respective pump, wherein no information is given with regard to the hydraulic connection of the pumps connected in series upstream.
[0026] According to one method variant of the present invention, with which the matrix is formed in the same manner as previously described, one may determine which pumps are connected hydraulically in parallel and which ones hydraulically in series, by way of the number of increasing changes of the hydraulic variables in each row below or in each column above a diagonal dividing the matrix and running from one to the other matrix axis. Thereby, according to a further formation of the method according to the present invention, the number of increasing changes of the hydraulic variables in the rows below the diagonal or in the columns above the diagonal of the matrix may be used for determining the number of pumps which are hydraulically connected in series downstream of the respective pump, and thus the number may be assigned.
[0027] The method according to the present invention, if the hydraulic variables of the pump are evaluated, may either be carried out by way of detecting the volume flow of the pumps or however alternatively the pressure or differential pressure of the pumps. If the determining is to be effected via the pressure changes, then according to the present invention, a matrix is formed in the same manner as previously described, in which the hydraulic changes of at least one hydraulically independent installation part are detected, wherein here too in rows for each pump, the changes of the hydraulic variable which results with its activation for delivering with a changed pressure, is specified at this pump and the other pumps, and wherein a column is assigned to each pump. Thereby, the rows are sorted increasing from the top to bottom according to their number of reducing changes (−1) and the columns are sorted from the left to the right according to their number of reducing changes, wherein then one determines which pumps are hydraulically connected in parallel and which are connected hydraulically in series by way of the number of reducing changes of the hydraulic variable in each column below, or in each row above a diagonal which divides the matrix and which runs from the one to the other matrix axis. Here too, the diagonal forms a symmetrical partition of the matrix and runs through the fields which have been indicated as always increasing and which in the row and column concern the same pump in each case. These fields are not co-counted with the subsequent evaluation, just as with the previously described one.
[0028] Thereby, an equal number of reducing changes of the hydraulic variables in the columns below the diagonal or in the row above the diagonal of the matrix indicates a connection of the respective pumps in parallel.
[0029] A different number of decreasing changes of the hydraulic variables in columns below the diagonal or in rows above the diagonal indicates the connection of the respective pumps in series.
[0030] If a row below the diagonal or a column above the diagonal of the matrix has no reducing change of the hydraulic variables, then this determines the direct assignment of the respective pump to a consumer or to a consumer group.
[0031] The number of reducing changes of the hydraulic variables in the columns below the diagonal or in the rows above the diagonal of the matrix according to a further formation of the method according to the invention indicates the number of pumps which are hydraulically connected upstream in series of the respective pump.
[0032] According to a further formation of the method according to the present invention, one alternatively determines which pumps are connected hydraulically in parallel and which ones are connected hydraulically in series, by way of the number of reducing changes of the hydraulic variables in each column below, or in each row above a diagonal dividing the matrix and running from one to the other matrix axis. Thereby, the pumps which have the same number of reducing changes of the hydraulic variable in the column below, or in the row above the diagonal of the matrix, are connected hydraulically in parallel, and those with a different number are connected hydraulically in series.
[0033] According to a further formation of the method according to the present invention, the number of the reducing changes of the hydraulic variables in the rows below the diagonal or in the columns above the diagonal of the matrix indicates the number of the pumps which are hydraulically connected in series downstream of the respective pump.
[0034] Thus it becomes clear that the previously described matrix unambiguously determines the functional relationship of the pumps when the hydraulic variable change is detected at each pump. On detecting hydraulic changes at the consumer or consumer group, as the case may be, it may be necessary as initially described, to differentiate additional pump groups as to whether they are connected in parallel or series by way of changing a hydraulic variable of the pump.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0035] The foregoing summary, as well as the following detailed description of the invention, will be better understood when read in conjunction with the appended drawings. For the purpose of illustrating the invention, there are shown in the drawings embodiments which are presently preferred. It should be understood, however, that the invention is not limited to the precise arrangements and instrumentalities shown. In the drawings:
[0036] FIG. 1 a is a hydraulic circuit diagram of an installation with several pumps and consumers according to a preferred embodiment of the present invention;
[0037] FIG. 1 b is a matrix with regard to the installation according to FIG. 1 a;
[0038] FIG. 2 a is a circuit diagram of four pumps arranged in parallel in accordance with a preferred embodiment of the present invention;
[0039] FIG. 2 b shows the temporal behavior of the pumps with a pressure increase;
[0040] FIG. 3 a is a circuit diagram of a pump group of pumps arranged in parallel and in series;
[0041] FIG. 3 b shows the behavior of the pumps with an activation with a changed rotational speed;
[0042] FIG. 4 a is a circuit diagram of three pumps arranged in parallel;
[0043] FIG. 4 b shows the behavior of the pumps with a change in rotational speed;
[0044] FIG. 5 a is a circuit diagram of three pumps arranged in series;
[0045] FIG. 5 b shows the behavior of the pumps with activation with a change in rotational speed;
[0046] FIG. 6 is a hydraulic circuit diagram of a hydraulic installation according to FIG. 1 , but with a pump-side sensor arrangement;
[0047] FIG. 7 is a first matrix with regard to the installation according to FIG. 6 ; and
[0048] FIG. 8 is a second matrix with regard to the installation according to FIG. 6 .
DETAILED DESCRIPTION OF THE INVENTION
[0049] The hydraulic installation represented by way of FIG. 1 and FIG. 6 is a heating installation which here is not to be explained in detail because such an explanation is not necessary to a full and complete understanding of the present invention. The hydraulic installation is equipped as a whole with 11 pumps PU 1 -PU 11 . These in total eleven (11) pumps supply six (6) consumers V 1 -V 6 . These consumers may be individual consumers, but are typically consumer groups such as, for example, a network of heat exchangers connected in parallel, as is normal in the construction of apartments for room heating, which as the case may be, may also be connected in groups in parallel and/or in series. A sensor S 1 , S 3 , S 6 , S 7 , S 10 , S 11 is assigned to each consumer and detects the pressure dropping at the consumer.
[0050] The installation preferably consists of two installation parts which are hydraulically independent of one another, specifically of the installation part represented at the bottom right in FIG. 1 a consisting of the pump PU 11 and the consumer V 6 , as well as the remaining installation part. In the remaining installation part, in the lowermost plane, a pump PU 10 supplies a consumer V 5 , parallel to this, two pumps PU 8 and PU 9 connected in parallel feed the consumer V 3 via a pump PU 6 connected in series downstream, as well as parallel to this, the consumer V 4 via a pump PU 7 connected in series downstream. The pumps PU 1 , PU 2 and PU 3 are supplied via the pumps PU 5 and PU 4 connected in series and for their part however connected in parallel supply the consumer V 1 and the consumer V 2 respectively. This arrangement is preferably selected at random and exclusively serves for illustrating the method according to the invention.
[0051] For carrying out the method, now firstly, all pumps PU 1 to PU 11 are preferably activated with a constant rotational speed, typically of a medium rotational speed which is selected such that the installation is operated according to directed use, but reserves are present so that the pumps, as the case may be, may be activated with a rotational speed which is increased with respect to this. With regard to the pumps, it is typically the case of heating circulation pumps, which are controlled by frequency converter, as are normal in the market.
[0052] All pumps are operated at a constant rotational speed and this rotational speed should be constant with respect to the respective pump, but of course the rotational speeds may differ amongst one another. If one of the pumps during the method must be activated with a changed rotation speed on account of a requirement on the part of the installation, then this may be effected when the correspondingly changed rotational speed is taken numerically into account. Pressures are detected at the sensors S 1 , S 3 , S 6 , S 7 , S 10 , S 11 during this activation with constant rotational speed. Now a first pump, e.g. the pump PU 1 is activated with a changed rotational speed, for example with an increased rotational speed and the changes which set in as the case may be or also the non-changes, are detected by way of the sensors S 1 , S 3 , S 6 , S 7 , S 10 , S 11 .
[0053] A matrix is usefully set up for this, as is represented in FIG. 1 b . In the matrix, the pumps PU 1 -PU 11 are listed on the one axis, which here is vertical, and the sensors S 1 -S 11 on the other, here horizontal axis, in order then in the fields which results with this, to detect whether and, as the case may be, which hydraulic changes result on activating a pump with an increased rotational speed. Thereby a categorization in 0, −1 and 1 is effected, wherein 0 indicates no change, 1 an increasing hydraulic variable and −1 a reducing hydraulic variable.
[0054] On activating the pump PU 1 with an increased rotational speed, thus according to FIG. 1 b , an increasing pressure difference results at the sensor S 1 , a reducing pressure difference at the sensor S 3 , a reducing pressure difference at the sensor S 6 , a reducing pressure difference at the sensor S 7 and likewise a reducing pressure difference at the sensor S 10 , compared to a prior activation of this pump PU 1 at a reduced rotational speed. The sensor S 11 detects no change since it relates to an installation part which is not hydraulically connected to the pump PU 1 . If these changes are detected, the pump PU 1 is moved down again to the previously activated constant first rotational speed, whereupon now the pump PU 2 is activated with an increased rotational speed and the changes resulting at the sensors S 1 -S 11 are plotted in the matrix. This is effected hereinafter with all pumps until the matrix is set up completely as in FIG. 1 b.
[0055] The matrix representation here is set up only for a simplified numbered representation, but is basically not necessary for evaluation. By means of the activation it may now be ascertained for starters that the pumps PU 1 -PU 10 have no influence on the sensor S 11 whatsoever and thus on the consumer V 6 . Vice versa the pump PU 11 has no influence at all on the consumers V 1 -V 5 from which it results that it hereby must be the case of two installation parts which are independent of one another, wherein pump PU 11 evidently only supplies the consumer V 6 .
[0056] With the remaining installation part, which comprises the pumps PU 1 -PU 10 , firstly one examines which pumps are arranged in pump groups, i.e. which pumps are connected into a group in parallel or series. The pumps which on the consumer side cause the same hydraulic changes with a change of their rotational speed, are connected into groups. This, as is to be deduced from the matrix according to FIG. 1 b , is the case for the pumps PU 8 and PU 9 , for the pumps PU 1 and PU 2 as well as for the pumps PU 4 and PU 5 . These pumps are thus identified as groups and one thus should yet determine whether these in each case are connected in series or in parallel, which is described further below.
[0057] One then determines which pumps, with a change of rotational speed, influence only one consumer or only one consumer group according to the rotation speed change, i.e. with an increase in rotational speed influence in a pressure increasing manner and with a rotational speed reduction in a pressure-reducing manner. Since, with the embodiment example which is represented by way of FIG. 1 , one has assumed that the pumps in method step b are activated with an increased rotational speed compared to the previous lower constant rotational speed, it results that they only have one positive 1 in the row. It is the pumps PU 1 , PU 2 , PU 3 , PU 6 , PU 7 , PU 10 and of course PU 11 which belong to the other installation part. These pumps are directly assigned to a consumer, i.e. they supply the consumer without intermediate connection of further pumps.
[0058] However, one may not only ascertain by way of these assignments as to which pumps are directly assigned to a consumer, but moreover which consumers are supplied by which pumps at all. Thus, it is evident that the pump PU 10 only affects the consumer V 5 and this in a direct manner. With regard to the pump group PU 8 and PU 9 , one may recognize that these influence the sensors S 1 , S 3 , S 6 , S 7 in the same direction, i.e. that with an activation of the pump with an increased rotational speed, a higher pressure drops at these sensors, i.e. an increasing pressure change is given. This says that the pumps PU 8 and PU 9 feed the consumers V 1 -V 4 but only indirectly, i.e. that yet other pumps need to be intermediately connected. With regard to the pumps PU 4 and PU 5 , one may ascertain in the same manner that they supply the consumers S 1 and S 3 , but however likewise only in an indirect manner, since the consumers V 3 and V 4 are directly supplied by the pumps PU 6 and PU 7 respectively, and since the pumps PU 4 and PU 5 as a pump group however do not influence these consumers in the same direction, it results that the pump group PU 4 and PU 5 as well as the pump PU 6 and the pump PU 7 are connected in parallel, wherein the pumps PU 6 and PU 7 in each case are assigned to the associated consumers V 3 and V 4 , whereas the pump group PU 4 and PU 5 affect the consumers V 1 and V 2 , but likewise not in a direct manner.
[0059] Inasmuch as this is concerned, one merely yet needs to determine how the pump groups are connected. These three groups of pumps PU 8 and PU 9 , PU 4 and PU 5 as well as PU 1 and PU 2 therefore need to be examined further as far as this is concerned. However further sensors are required for this, which detect the differential pressure of the respective pumps of the pump group or the throughput. With the embodiments according to FIGS. 2 and 3 , the differential pressure sensors are applied parallel to the pump, whereas with the embodiments according to the FIGS. 4 and 5 , volume flow sensors, namely so-called throughput meters, are assigned to the pumps. Irrespective of which sensors are applied, again the previously described method is applied for determining the arrangement of the pumps in a pump group, i.e. the pumps are firstly represented as by way of FIGS. 4 and 5 , operated with a constant rotational speed, whereupon a pump, here the pump PU 1 , is activated with an increased rotational speed. By way of the changing volume flow of this and of the other pumps, one may now determine whether the pumps arranged into a pump group are connected in series or in parallel. With a parallel connection according to FIG. 4 a , with an activation of a pump, here pump the PU 1 with an increased rotational speed ω 1 of this pump, an increased throughput q 1 results, whereas the other two pumps PU 2 and PU 3 continue to run with the previous constant rotational speed, but have a reduced flow volume rate q 2 and q 3 respectively. It directly results from this, that the pumps must be connected in parallel, since otherwise the delivery rates would have to increase as is illustrated by way of FIG. 5 , where three pumps PU 1 -PU 3 are connected in series. If here the pump PU 1 is activated with an increased rotational speed ω 1 , an increased throughput quantity q 1 , q 2 and q 3 of all three pumps thus results despite a constant rotational speed of the pumps PU 2 and PU 3 .
[0060] If the arrangement of the pumps is to be determined by way of pressure sensors thus differential pressure sensors parallel to the pump, then one of the pumps of a pump group after all have been activated for producing a constant pressure, activates one of the pumps for producing this increased pressure. This is effected with the examples according to FIG. 2 and FIG. 3 in each case with the pump PU 1 . On may deduce from FIG. 2 b as to the temporal course of the change of the hydraulic variables. After the pressure jump of the pump PU 1 , the pressure at the pumps PU 2 , PU 3 and PU 4 remains practically unchanged, wherein the rotational speeds of the pumps PU 2 and PU 3 reduce with a slightly increasing pressure, which may be deduced as a parallel connection, whereas the rotational speed of the pump PU 4 with a constant pressure increases, which indicates that this pump does not belong to the pumps connected in parallel. Analogously, with the series connection of the pumps PU 1 , PU 2 and PU 3 into a group, a pressure change only at the pump PU 1 and with all other pumps merely a rotation speed change and specifically in an increasing manner, results.
[0061] As the above explanations illustrate, thus the circuit diagram according to FIG. 1 a may be completely determined. Since with the previously described method, only one sensor is assigned to only each consumer or each consumer group, the separate sensor means must be applied on the part of the pump in the pump groups for determining the arrangement of the pumps.
[0062] Inasmuch as this is concerned, it is often more favorable to design the method according to the present invention exclusively with pump-side pressure sensors, differential pressure sensors and throughput sensors, as this is represented by way of the FIGS. 6-8 . This method takes its course in the same manner, i.e. firstly in a first method step, all pumps are activated with a constant rotation speed and then in a second method step subsequently all pumps are activated individually and one after the other with a rotational speed which is changed with respect to this, typically an increased rotational speed. The resulting changes are recorded in a matrix, as is represented by way of FIG. 7 for the throughput measurement of the pumps and by way of FIG. 8 for the differential pressure measurement at the pumps. Thereby, the matrix is formed in the same manner as that described by way of FIG. 1 b , i.e. 0 stands for no change of the hydraulic variable of the respective sensor on activating the respective pump with an increased rotational speed, 1 for an increasing change and −1 for a reducing change.
[0063] For the evaluation of the matrix according to FIG. 7 , it is however necessary to previously sort this according to rows. With the detection of the volume flow changes as are drawn in FIG. 7 , the sorting of the rows is effected according to the number of increasing changes from the top to bottom. Thus the uppermost row concerning pump PU 7 has one 1, specifically at q 11 . The row PU 10 arranged therebelow also has only one 1, specifically at q 10 . The rows PU 7 and PU 6 in each case have three increasing changes, the rows PU 1 , PU 2 and PU 3 in each case 5 increasing changes, the rows PU 4 and PU 5 7 increasing changes and the rows PU 8 and PU 9 8 increasing changes. The rows are sorted in an increasing manner from the top to bottom according to this sequence. Thereby, a pump is assigned to each row and the sensor assigned to the pump in each case is assigned to each column. The columns are sorted in an increasing manner in the same manner as the pumps, but from the left to the right, so that a mirror-symmetry of the matrix with respect to a diagonal D, which is formed by the fields which relate to the same pumps, results. This diagonal extends from the top left to the bottom right in the matrix beginning from the field PU 11 , q 11 to the field PU 9 , q 9 .
[0064] The functional relationship, i.e. the construction of the installation may be directly evaluated by way of this matrix. Thus, firstly in the same manner as with the first embodiment example, by way of the zeros in the first column below the diagonal or in the first row above the diagonal, one may ascertain that the pumps PU 1 -PU 10 belong to a different installation part than the pump PU 11 , since this pump only influences its own sensor q 11 .
[0065] By way of the number of increasing changes, thus the numbers 1 of the throughput in each gap below the diagonal D or in each row above the diagonal D which divides the matrix, it results as to which pumps are hydraulically connected in parallel and which are hydraulically connected in series. An equal number as occurs for example in the columns q 7 and q 6 and q 5 in FIG. 7 below the diagonal D, indicates that these pumps are arranged in parallel, whereas a number differing with respect to this, such as for example at q 4 —here it is three—indicates that this pump PU 5 does not lie in parallel but in series with one of the previously mentioned pumps. As to how the arrangement is given, results from the number of increasing changes. Thereby, the number of increasing changes of the hydraulic variables in the columns below the diagonals or, since it is mirror-symmetrical, in the rows above the diagonal, indicates the number of the pumps which are hydraulically connected in series upstream of the respective pump. Thus, for example, the pump PU 1 to which the sensor q 1 is assigned, is characterized by four ones in the column q 1 below the diagonal, i.e. four increasing changes of the hydraulic variables, which means that four pumps are connected in series upstream of the pump PU 1 . This may thus be determined for each of the pumps.
[0066] Moreover, one may ascertain which of the pumps are directly assigned to a consumer or to a consumer group, and here it is specifically the case of the pumps with which no increasing change of the hydraulic variables in a row below the diagonal or a column above the diagonal of the matrix is plotted. This for example applies to the pump PU 7 , in whose associated rows in FIG. 7 below the diagonal there are only the numerals 0 and −1, in the same manner for PU 6 there are the numerals 0, −1, −1, etc. Thus, one may ascertain by way of these details as to how many pumps are connected in series upstream of the respective pump and which pumps connect directly to a consumer or consumer group. Thus, the circuit arrangement according to FIG. 6 is unambiguously defined.
[0067] Moreover, in FIG. 7 , one may determine which pumps are connected hydraulically in parallel and which in series by way of the number of increasing changes of the hydraulic variable in each row below, or in each column above, the diagonal of the matrix. The number of increasing changes (+1) thereby indicates the number of pumps which are hydraulically connected in series downstream of this pump. Thus, in FIG. 7 , the pump PU 8 in row 7 has ones below the diagonal D, which means seven pumps are connected in series downstream of this pump. Thereby, it is the case of the pumps PU 1 -PU 7 . If in FIG. 7 , below PU 4 , one reads the row below the diagonal D, then three ones result, i.e. three pumps are connected in series downstream. Thereby, it is the case of the pumps PU 1 -PU 3 as the circuit diagram according to FIG. 6 illustrates.
[0068] In an analogous manner, the evaluation of the matrix according to FIG. 8 , with which instead of throughput changes q, the pressure changes s are specified. However, here it is not the increasing changes 1 , but the reducing changes −1 which are used for evaluation, but otherwise the evaluation is effected the same manner as described by way of FIG. 7 .
[0069] It will be appreciated by those skilled in the art that changes could be made to the embodiments described above without departing from the broad inventive concept thereof. It is understood, therefore, that this invention is not limited to the particular embodiments disclosed, but it is intended to cover modifications within the spirit and scope of the present invention as defined by the appended claims. | A method for determining the functional relationship of several pumps which are controllable in their rotational speed, in a hydraulic installation. At least one pump is activated with a changed rotational speed, and at least one functional relationship of the installation is determined from the hydraulic reactions. With a suitable selection of the control and detection of the hydraulic changes, one may determine the functional relationship of the complete installation. | 5 |
BACKGROUND OF THE INVENTION
The present invention relates to a device for holding screws securely in contact with a driving bit during positioning and driving of the screw. The device is mounted upon a screw driver bit, particularly a bit intended for use in a motor powered driver and more particularly, for surgical procedures involving driving screws into bone.
The device is capable of undergoing repeated steam sterilization without impairment of function, may be quickly disassembled without the need for tools for rapid change of screw driver bit size or style, and is capable of accommodating screws of a variety of sizes and head shapes. The device provides positive, locking screw holding engagement yet permits angular screw displacement of about 10° from axial direction. The device contributes little toward operator fatigue because of its compact size, light weight and use of counter-balanced spring bias forces.
Devices previously used for surgical procedures, primarily bone fixation, although of similar size, operated on a totally different principle. These devices utilized a plurality of spring-like gripping elements each having a forward groove for gripping the screw head. They usually had no, or poor, screw locking means, were prone to malfunction, were subject to frequent premature release of the screw, and provided for little or no angular displacement of the screw from axial alignment so that a screw which was misdirected into a pilot hole could cause cracking or splintering of the bone.
Screw holding devices intended for use by craftsman or in the trades were much more dependable than those used by the surgical profession but were bulky, clumsy and complicated and hence, poorly qualified for adaptation to this highly specialized use. Also, for devices used by a craftsman, equipment cost is a primary concern with little worry directed to possible damage to the screw threads and heads. The damage to screw threads and screw heads caused by these devices is of slight importance in, e.g., sheet metal work but would be of extreme concern in a delicate surgical procedure.
Many of the craft directed prior art devices utilized ball members as well as concentric sleeves, springs, etc. for their gripping action.
Thus, Schmitt U.S. Pat. 2,840,126, although seemingly incorporating many features which are roughly comparable to those of the present invention, differs markedly. Schmitt uses the bit to back up the screw while the balls are forced backward along the screw with possible damage to the screw threads in the process. Further, the device is necessarily fastened onto the motor rather than to the bit because of its large size and weight due partly to the unique screw loading mechanism. Such a mechanism would not only render the device exceedingly clumsy for use in surgical procedures but would also be difficult to clean, disassemble, and sterilize. Schmitt's device appears to have been primarily designed for attachment to a stationary screw-press machine. The device could easily cause scoring or marring of screw heads during engagement, an unacceptable condition for surgical usage. The device also causes positive locking of the screw when loaded, a feature which does not allow any angular movement of the screw to permit compensation for an angularly displaced pilot hole without stressing the substrate. Another disadvantage is that Schmitt's device can only accommodate a given length of screw unless the bit is changed, which necessitates an extensive operation involving the use of tools. Finally, it is doubted whether the device could be used to extract a screw since a screw cannot be engaged by the bit from the front.
Luber, U.S. Pat. No. 2,845,968, is an even more primitive device in that the screw is loosely held by forcing the device forward against the substrate whereby the end of the device, containing balls backed by resilient material, is forced back relative to the bit and screw causing the balls to center the screw. This device would be entirely impractical for exacting surgical work since at no point can the screw be seen for exact positioning. This device would cause damage to both the head and threads of the screw, would be clumsy to use and could hardly be used to extract a screw. The device also would require the use of excessive pressure against a patient causing fatigue to the surgeon.
Taylor, U.S. Pat. No. 3,181,580, is one variation of the many available spring-clip type screw holders. Among the main disadvantages of spring-clip holders are:
(1) They allow for no angular misalignment of the screw from the axial direction.
(2) They are prone to accidental premature release of the screw.
(3) They are usually intolerant of slight screw size changes.
(4) They are prone to fatigue of one or more of the spring elements, a malfunction which is difficult to repair.
(5) They do not have a positive locking mechanism.
McKenzie, U.S. Pat. No. 3,244,208, is another variation of the spring-clip screw holder. This type suffers the further disadvantage that while it can hold flat-head screws such as the sheet metal screws for which it was designed, it has very poor holding power for a screw such as a surgical screw which is designed to fit into a countersunk hole.
Morifuji, U.S. Pat. No. 3,298,410, discloses a simple low cost device for use with a manually operated screwdriver. It does not appear that the resilient holding means can provide the secure locking required for surgical usage with a powered driver.
Eby, U.S. Pat. No. 3,901,298, another spring-clip holder with the disadvantages previously listed, also has the further disadvantage of requiring manual release of the screw as contrasted with the automatic release of the present invention.
Belgium Pat. No. 500,711 relates to a device which requires too much manual dexterity for use in surgical procedures.
Lesner, U.S. Pat. No. 3,967,664, suffers from the disadvantage, common with many of the other prior art patents, that the operator must exert considerable pressure upon the device while driving screws to overcome the spring bias built into the device. For example, the first embodiment described by Lesner requires a driving force counter to the combined action of three heavy springs. This not only causes undue fatigue to the operator but in the case of surgical procedures, would cause entirely unacceptable stress and strain upon the surgical repair site. By contrast, the device of the present invention uses counteracting springs to lessen the overall bias. During the majority of the screw travel there is no spring bias to overcome. During the final screw tightening, there is a very low spring reaction which is almost unnoticeable. Lesner's balls are restricted from penetrating more than a minor amount inwardly toward the screw, restricting gripping power, angular displacement of the screw and the ability of the device to handle screws of various head sizes and shapes. Lesner's device attaches to the driver housing, restricting interchangeability, cleaning and sterilization. The device undergoes very sensitive transition changes within the locking mechanism between loading and driving which would appear to inevitably result in malfunction, particularly if the springs are not proportioned correctly or if the screw is started into an angularly misaligned pilot hole. In the second embodiment, the screw is entirely unlocked from gripping contact during the entire driving operation.
SUMMARY OF THE INVENTION
The device of the present invention is particularly suited for use in surgical procedures involving the driving of screws into bone. The device provides positive locking screw-holding engagement in contact with a driving bit during positioning and driving of the screw. The device is mounted upon a screw driver bit, particularly a bit intended for use with a motor powered driver. As noted, the device of the present invention holds screws securely in contact with a driving bit, yet, due to the unique design of the screw-holding mechanism, the screw is permitted to be displaced about 10° from the axial direction. Thus, if a screw were started in a pilot hole at an angle displaced from normal, the screw-holding and restraining mechanism would permit angular displacement of the screw from the normal axis of the device until realignment of the screw can be accomplished so that the screw can be driven into the hole without causing undue stresses upon the fragile bony substrate, thus avoiding splitting or shattering of the fragile bony substrate. The device is compact in size and light weight, and can be quickly disassembled without tools for rapid change of screw driver bit sizes or styles, and is capable of accommodating screws over a variety of sizes and head shapes.
BRIEF DESCRIPTION OF THE DRAWINGS
In the accompanying drawings which illustrate the invention:
FIG. 1 is an enlarged sectional view of a device of the invention loaded with a screw and ready for operation;
FIG. 2 shows the device in its unlocked form prior to being loaded with a screw;
FIG. 3 shows the device approximately midway in the screw loading process;
FIG. 4 shows the relationship of the components shortly after the forward edge of the collet has contacted the substrate surface as the screw is driven into place;
FIG. 5 shows the relationship of the components with the screw driven further into the substrate;
FIG. 6 illustrates the device with the screw fully driven into the substrate;
FIG. 7 illustrates another embodiment of the invention; and
FIG. 8 shows a still further embodiment of a device according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now more particularly to the drawings, device 10 is fastened to a screw-driver bit 11. The bit 11 is shown as a cruciate slotted bit although it should be realized that any type of bit may be used depending, of course, upon the screw type to be driven. A variety of bits would normally be furnished and each of these could carry a screw retaining device 10, as shown, or the bits could be rapidly interchanged to one screw retaining device as will be described later. For simplicity, the bit 11 is shown as having one diameter change throughout its length although it will be understood that the bit can have various changes of diameter throughout its length. Bits for surgical usage will be constructed of stainless steel or other suitable rust-resistant alloy which can take a good finish, maintain a hardened driving edge and withstand repeated steam sterilization. Although the device is described as being fastened to the bit, this terminology is not entirely accurate in that all parts of the device are movable with respect to the bit, the degree of movement being restricted only by the bit retainer 12 and the various locking and biasing means. Again, the bit retainer 12 has been over-simplified for purposes of explanation and will be described more fully later.
The retainer nut 13 is used to fasten the bit 11 to the device. When it becomes necessary to change bits so that different types of screws may be used, the retainer nut 13 may be easily and quickly unscrewed, usually without the need for tools, and after the threaded portions are disengaged, the bit 11 removed from the device, the bit retainer 12 pulling the retainer nut 13 with it. The retainer nut 13 can then be slipped onto a different bit and the bit slipped into the device and the retainer nut quickly tightened. while this method of bit replacement is preferred, it should be understood that the retainer nut may be more or less permanently fastened to the device particularly if the need to change bits is of no concern.
Collet 19 is shown serving both as a bushing for the bit 11, and shoulder 14 thereon acts as the backing restraint for bias spring 15, which bears against the plunger 16, which thereby presses against the head of a screw 17 holding said screw head firmly against balls 18, which in turn are held in place within openings of the collet 19. It is, of course, contemplated that the screw driving bit 11, slightly modified, can be spring biased to bear against the head of screw 17, thus eliminating the need for the separate plunger 16.
In the preferred form of the invention, four balls 18 are used. A lesser or greater number may be used but four seems to provide the best compromise between holding power and angular freedom. With most of the prior art devices, the screw was locked rigidly in axial position so that it tended to be directed wholly by the operator even though such direction might be at an angle displaced from that of the drilled pilot hole, thereby causing undue stresses upon the substrate into which it was being driven. In the case of fragile bone substrates, such misdirection could cause disastrous splitting of the bone. With the present device, the balls 18 hold the head of the screw 17 firmly and in non-releasable security against the pressure of the plunger 16 while still allowing about 10° of angular displacement from the axis of the device.
While restraining means other than balls may be used, spherical balls provide the best restraint for screw heads and provide a certain latitude for restraint of various size screws while also contributing to the smoothness of operation of the device.
It will be seen that the plunger spring 15 acts against the shoulder 14 of collet 19 to bias the plunger 16 which in turn forces the screw head 17 against the balls 18, which are always retained axially within the openings in the collet 19. It will be appreciated that a separate spring retainer 14 could be incorporated as a loose insert held in place against the collet 19. This method of assembly would have the advantage that the device could be easily disassembled into individual components for cleaning and/or sterilization, a particular advantage for surgical tools and instruments. The separate spring retainer 14 should have a fixed relationship to the collet 19 and this fixed relationship can be provided by press fitting them together or through the use of other retaining means such as screw threads, retaining ring, etc.
The exterior of the device is made up of a spring retainer 20, a collet sleeve spring 21 and a collet sleeve 22. The spring retainer 20 can be a loose insert held in place by the retainer nut 13 so that it can be removed when the retainer nut 13 is removed, thereby allowing easy disassembly of the components for cleaning and/or sterilization. As shown, spring retainer 20 is press-fitted to the collet 19 or can be assembled thereto as by screw threads, socket-head screw, retainer ring, or the like.
The spring retainer 20 acts as a stop or backup for the collet sleeve spring 21 which biases the collet sleeve 22 forward against the balls 18. The collet sleeve 22 holds the balls 18 inwardly radially against the screw head and/or screw shank and is restrained from further forward movement in the unlocked position by the action of its inner shoulder 23, against these same balls 18. As can be clearly seen in FIGS. 7 and 8, collet sleeve 22 is provided with a shallow circumferential recess 34 adjacent inner shoulder 23 for the purpose of limiting the forward movement of the collet sleeve 22 in the loaded condition (FIGS. 1 and 4) through the action of balls 18 against said recess 34.
Although the device 10 is free to move axially to some extent relative to the bit 11, there is an interaction between these movements which can best be seen in FIGS. 1 through 6.
In the unlocked position shown in FIG. 2, the plunger 16 is in full forward position due to the bias action of the extended plunger spring 15. The plunger 16 is restrained from further forward motion by the action of its outer forward shoulder 24 against the balls 18. Complementarily, this shoulder 24 presses the balls outward of their openings in the collet 19 where they act to retain the collet sleeve 22 in its rearward position against the compressed collet sleeve spring 21.
The bit 11 is also shown in full forward position although it could also be retracted rearwardly, unless biased forward by an additional spring 30 as can be seen in the drawings.
In FIG. 3, the device 10 is held in one hand, the head of the screw 17 engaged with the bit and the screw then pushed back forcing the plunger 16 and bit 11 backward against spring 15. The plunger 16 is shown in this view depressed almost to the point where the balls 18 can move radially inwardly toward the screw 17.
In the loaded position shown in FIG. 1, the screw has been pushed rearwardly forcing the plunger 16 back and compressing plunger spring 15. As the plunger 16 is pushed back past its position in FIG. 3, the balls 18 are forced inward against the screw 17 by the camming action of the collet sleeve 22 as it is forced forward by the collet sleeve spring 21. The balls 18 act to prevent the collet sleeve 22 from going any further forward than the position shown.
The device as shown in FIG. 1 would be used to start driving the screw. The entire device 10 would rotate with the bit 11 and screw 17. This relationship would be maintained until the forward end of the collet sleeve made contact with the substrate surface as shown in FIG. 4, which schematically illustrates the situation in the majority of surgical procedures where bone is held together with screws. A metal plate 35 is placed along and against the fractured bone 36 and surgical screws 17 are then driven into predrilled countersunk holes in the plate and into the bone. It is, of course, understood that in those procedures where a metal plate is not used, the bone would be the substrate against which the collet sleeve would make contact. The collet sleeve 22 has been partially forced back against the biasing action of the collet sleeve spring 21 due to its having been forced against the substrate surface. At this point, collet sleeve 22 is still holding the balls 18 against the screw 17.
FIG. 5 shows the action as the screw is driven further into the substrate. The collet sleeve 22 has now been forced back fully in relationship to the collet 19 and has allowed the balls 18 to migrate outward radially due to the camming action of the screw head. With the balls 18 thus retracted, the screw head and plunger 16 are allowed to pass the balls 18. The screw 17 is no longer secured between the balls 18 and the plunger 16 but since the screw is almost completely driven in place, such holding action is no longer necessary. The bit 11 is still in contact with the screw head and plunger 16 follows screw 17 because of its spring bias and maintains concentricity of the bit 11 within the slots of the screw head.
FIG. 6 shows the situation at the time that the screw 17 is fully driven into place. Under pressure from the operator, the bit 11 has continued to follow the screw. Under pressure from the plunger spring 15, the plunger 16 has also followed the screw and in the process has locked balls 18 into retracted position radially against the collet sleeve 22. The device 10 and bit 11 can now be removed from contact with the screw. The device is locked into unload relationship and is ready to be loaded with another screw as the device is now in the same position as that shown in FIG. 2.
Since during the final driving stages, shown in FIGS. 4, 5 and 6, it is difficult to visualize the exact position of the screw, the bit 11 could be marked to indicate the amount of screw still remaining above the substrate surface. The amount of forward travel of the bit 11 can also be varied by positioning the bit retainer 12 so that the screw can be fully driven as shown or so that the screw could be left protruding a small amount. The final tightening of the screw would then be done manually without the use of the device. The arrangement shown is preferred since it reduces the possibility of marring the screw head during premature disengagement of the bit from the screw head while the bit is still powered.
The spring loading arrangement for bit retainer 12 can be seen in any of FIGS. 1 to 6. Forward split retainer ring 27 and rear split retainer ring 26 keep the spring assembly and the retainer nut 13 in place during disassembly of the device 10. If it should be necessary to remove the retainer nut 13 from the bit 11, it can be firmly pulled rearwardly depressing split retainer ring 26 further into its groove allowing retaining nut 13 to pass over it. Spring retainer bushings 28 and 29 maintain the spring position, transmit forces to the spring, and can similarly be passed over the split retainer ring 26 with firm axial pressure. In use, the spring 30 maintains forward bias on the bit relative to the retainer nut 13 and hence relative to the device 10 so that the bit 11 always remains in contact with the screw head slots, particularly during screw loading thereby eliminating marring of the screw head during the start of driving.
While a screw 17 is being driven, the device 10 will rotate with the bit 11. The rotational speed is slow enough so as not to cause any safety hazard and in fact the frictional drag between bit 11 and device 10 is so low that the device 10 can easily be held and prevented from rotating. Nevertheless, even slow, low torque rotation can be undesirable in some instances, even possibly causing slight scratching of the substrate from contact with the rotating collet sleeve 22. To further reduce this possibility. FIG. 7 shows an alternative construction having a further outer sleeve 31 which can be mounted over the collet sleeve 22 by means of bearings such as the ball bearings 32.
The embodiment shown in FIG. 8 utilizes a "Teflon" extension 33, for the collet sleeve 22. The sleeve 33 can be snapped into place over the collet sleeve 22 as shown and will not only present a low friction mar-proof contact surface but can also rotate relative to the collet sleeve 22 due to its inherent low-friction surface. | The present disclosure relates to a device designed for use in surgical procedures requiring the driving of screws into bone. The device provides positive locking screw holding engagement yet permits angular movement of the screw of up to 10° from the axial direction. | 0 |
CROSS-REFERENCE TO RELATED APPLICATION
The present patent application is a continuation-in-part patent application of U.S. patent application Ser. No. 10/908,469, filed May 12, 2005, entitled “Recreational Structure Using a Sleeve Joint Coupling,” invented by Craig Adams, which is a continuation-in-part (CIP) patent application of U.S. patent application Ser. No. 10/905,105, filed Dec. 15, 2004, entitled “Recreational Structure Using A Sleeve-Joint Coupling,” invented by Craig Adams, both of which are incorporated by reference herein.
BACKGROUND
The subject matter disclosed herein relates to recreational structures. More particularly, the subject matter disclosed herein relates to a frame arrangement for a recreational structure, such as a trampoline, that uses a coupling member.
DESCRIPTION OF THE RELATED ART
Recreational structures having frames, such as trampolines, are well-known. For example, a trampoline has a horizontal frame to which a rebounding surface is attached and a plurality of vertical frame members, or legs, that support the horizontal frame and rebounding surface above the ground. While the horizontal and vertical frame portions of a trampoline could be fabricated to be one unitary structure, such a unitary structure is cumbersome when the trampoline frame is transported to a place where the trampoline is used. Accordingly, trampoline frames are typically formed from a plurality of pieces that are fastened together at the time a trampoline is assembled.
A desirable characteristic for all trampoline frames formed from a plurality of pieces is that the various pieces are attached or joined to each other using a technique that is simple, quick to assemble and is reliable.
BRIEF SUMMARY
The subject matter disclosed herein provides a technique for joining structural components of a recreational structure, such as a trampoline, that is simple, quick to assemble and is reliable.
The subject matter disclosed herein provides a recreational structure frame system that includes a plurality of horizontal frame members, at least one vertical frame member, at least one vertical pole member, and at least one sleeve-joint coupling. Each horizontal frame member has two ends. Similarly, each vertical frame member has two ends, and each vertical pole member has two ends. In one exemplary embodiment, at least one coupling member has first, second and third arm members arranged to substantially form a T configuration. The first arm member and the second arm member are disposed in an opposite relationship with each other. The third arm member includes flange members that receive one end of a vertical frame member and one end of a vertical pole member. The second and third arm members each receive one end of a horizontal frame member.
The vertical pole member can be part of, for example, a safety enclosure, in which case the safety enclosure can include a plurality of vertical pole members, such that each vertical pole member is received by the flange members of the coupling member. A plurality of horizontal support members can be coupled to two adjacent vertical pole members, thereby forming the safety enclosure. In one exemplary embodiment, the vertical pole member is configured to substantially form an arch.
BRIEF DESCRIPTION OF THE DRAWINGS
The subject mater disclosed herein is illustrated by way of example and not by limitation in the accompanying figures in which like reference numerals indicate similar elements and in which:
FIG. 1 depicts a perspective view of an exemplary trampoline having an exemplary safety enclosure;
FIGS. 2A-2C respectively show a side view, a top view and an end view of the first exemplary embodiment of a sleeve joint coupling for a trampoline frame according to the subject matter disclosed herein;
FIG. 2D shows a perspective view of the first exemplary embodiment of a sleeve joint coupling according to the present invention;
FIG. 3 shows details of a first exemplary embodiment of sleeve-joint coupling according to the subject matter disclosed herein;
FIGS. 4A-4C respectively show a side view, a top view and an end view of a second exemplary embodiment of a sleeve-joint coupling for a trampoline frame according to the subject matter disclosed herein;
FIGS. 5A-5C respectively show a side view, a top view and an end view of a third exemplary embodiment of a sleeve-joint coupling for a trampoline frame according to the subject matter disclosed herein;
FIGS. 6A-6C respectively show a side view, a top view and an end view of a fourth exemplary embodiment of a sleeve-joint coupling for a trampoline frame according to the subject matter disclosed herein;
FIGS. 7A and 7B respectively show a side view and a top view of a fifth exemplary embodiment of a sleeve-joint coupling for a trampoline frame according to the subject matter disclosed herein;
FIGS. 8A-8C respectively show a side view, a top view and an end view of a sixth exemplary embodiment of a sleeve-joint coupling for a trampoline frame according to the subject matter disclosed herein;
FIG. 9 depicts a top cutaway view of the first exemplary embodiment of a sleeve joint coupling according to the present invention;
FIG. 10 shows a cut-away view of an exemplary embodiment of a vertical pole member for a safety enclosure, a sleeve-joint coupling, and a vertical frame member according to the present invention; and
FIG. 11 depicts a perspective view of an exemplary trampoline having an exemplary alternative embodiment of a safety enclosure.
DETAILED DESCRIPTION
It should be understood that the word “exemplary” is used herein to mean “serving as an example, instance, or illustration.” Any embodiment described herein as “exemplary” is not necessarily to be construed as preferred or advantageous over other embodiments.
FIG. 1 depicts a perspective view of an exemplary trampoline 100 having an exemplary safety enclosure 101 . Trampoline 100 includes a rebounding surface 102 and a frame structure having vertical frame members 103 and a circular frame that can be formed from a plurality of circular frame members 104 . Vertical frame members 103 and circular frame members 104 are typically made from hollow metal tubing having sufficient strength to bear the stresses and loads that are associated with trampolines. Safety enclosure 101 includes a frame structure having vertical pole members 105 and horizontal support members 106 . A horizontal support member 106 is connected between adjacent vertical pole members in a substantially inflexible manner. A structural member that is suitable for both vertical pole members 105 and horizontal support members 106 is disclosed by U.S. Pat. No. 6,450,187 B1 to Lin et al., which is incorporated by reference herein.
Complete details of trampoline 100 and safety enclosure 101 are not shown in FIG. 1 for simplicity. For example, safety enclosure includes a mesh- or netting-type of material that extends between adjacent vertical pole members 105 and between horizontal frame members 106 and circular frame member 104 that together with circular frame 104 , vertical pole members 105 and horizontal support members 106 operate as a fence around rebounding surface 102 in order to keep a user on trampoline 100 and reduce the risk of injury to the user.
According to the subject matter disclosed herein, vertical pole members 105 of safety enclosure 101 attach to the frame structure of trampoline 100 using a plurality of sleeve-joint couplings, of which one is indicated at A in FIG. 1 . FIGS. 2A-2D and FIG. 3 show details of a first exemplary embodiment of a sleeve-joint coupling according to the subject matter disclosed herein. In particular, FIGS. 2A-2C respectively show a side view, a top view and an end view of the first exemplary embodiment of a sleeve-joint coupling 200 for a trampoline frame according to the subject matter disclosed herein. FIG. 2D shows a perspective view of sleeve-joint coupling 200 . Sleeve joint coupling 200 is generally shaped as a “T” and includes three arm members 201 - 203 , each having a generally square cross-sectional shape. Each arm member 201 - 203 receives a trampoline frame member (not shown in FIGS. 2A-2C ) of similar cross-sectional shape into an opening 204 ( FIGS. 2C and 2D ). Sleeve joint coupling 200 includes an opening 205 , shown in FIG. 2B , that receives a safety enclosure vertical pole member (not shown in FIGS. 2A-2C ) having a generally square cross-sectional member.
FIG. 3 depicts View A, shown in FIG. 1 , in greater detail. In FIG. 3 , sleeve-joint coupling 200 couples circular frame member 104 A to circular frame member 104 B and to vertical frame member 103 . Circular frame members 104 A and 104 B are secured to sleeve-joint coupling 200 using, for example, pins 301 and cotter rings 302 (not shown in FIGS. 2A-2D ). Alternatively, circular frame members 104 A and 104 B can be secured to sleeve-joint coupling 200 using sheet metal screws, and/or bolts and nuts. As yet another alternative, the inner surface of each arm member of sleeve-joint coupling can be threaded to engage complementary threading on each end of a circular frame member 104 and on one end of a vertical frame member 103 . Additionally, a threaded connection between sleeve-joint coupling 200 and a frame member can be secured using a pin and cotter ring arrangement, a sheet metal screw and/or a bolt and nut.
Vertical pole member 105 of safety enclosure 101 is inserted into opening 205 ( FIGS. 3B and 3D ) and extends through sleeve-joint coupling 200 into vertical frame member 103 a distance that is sufficient to distribute any shearing and/or torquing forces that may be imparted to vertical pole member 105 along the inside of vertical frame member 103 so that vertical frame member 103 does not fail. Vertical pole member 105 can be secured in vertical frame member 103 using, for example, a pin 301 and a cotter ring (not shown). Alternatively, vertical pole member 105 is secured in vertical frame member 103 using a sheet metal screw and/or a bolt and nut.
FIGS. 4A-4C respectively show a side view, a top view and an end view of a second exemplary embodiment of a sleeve-joint coupling 400 for a trampoline frame according to the subject matter disclosed herein. Sleeve-joint coupling 400 is generally shaped as a “T” and includes three arm members 401 - 403 , each having a generally round cross-sectional shape. Each arm member 401 - 403 receives a trampoline frame member (not shown in FIGS. 4A-4C ) of similar cross-sectional shape into an opening 404 ( FIG. 4C ). Sleeve-joint coupling 400 includes an opening 405 , shown in FIG. 4B , that receives a safety enclosure vertical pole member (not shown in FIGS. 4A-4C ) having a generally round cross-sectional member.
FIGS. 5A-5C respectively show a side view, a top view and an end view of a third exemplary embodiment of a sleeve-joint coupling 500 for a trampoline frame according to the subject matter disclosed herein. Sleeve-joint coupling 500 is generally shaped as a “T” and includes three arm members 501 - 503 , each having a generally oval cross-sectional shape. Each arm member 501 - 503 receives a trampoline frame member (not shown in FIGS. 5A-5C ) of similar cross-sectional shape into an opening 504 ( FIG. 5C ). Sleeve-joint coupling 500 includes an opening 505 , shown in FIG. 5B , that receives a safety enclosure vertical pole member (not shown in FIGS. 5A-5C ) having a generally oval cross-sectional member.
FIGS. 6A-6C respectively show a side view, a top view and an end view of a fourth exemplary embodiment of a sleeve-joint coupling 600 for a trampoline frame according to the subject matter disclosed herein. Sleeve-joint coupling 600 is generally shaped as a “T” and includes three arm members 601 - 603 , each having a generally triangular cross-sectional shape. Each arm member 601 - 603 receives a trampoline frame member (not shown in FIGS. 6A-6C ) of similar cross-sectional shape into an opening 604 ( FIG. 6C ). Sleeve-joint coupling 600 includes an opening 605 , shown in FIG. 6B , that receives a safety enclosure vertical pole member (not shown in FIGS. 6A-6C ) having a generally triangular cross-sectional member.
FIGS. 7A and 7B respectively show a side view and a top view of a fifth exemplary embodiment of a sleeve-joint coupling 700 for a trampoline frame according to the subject matter disclosed herein. Sleeve-joint coupling 700 is generally shaped as an “X” or a “+” and includes four arm members 701 - 704 , each having a generally square cross-sectional shape. Each arm member 701 - 704 receives a trampoline frame member (not shown in FIGS. 7A and 7B ) of similar cross-sectional shape into an opening 705 , of which only one opening 705 is shown ( FIG. 7B ). Each opening 705 receives a safety enclosure vertical frame member 103 , a circular frame member 104 or a vertical pole member 105 (none of which are shown in FIGS. 7A and 7B ) having a generally square cross-sectional member. It should be understood that sleeve-joint coupling 700 can have an alternative cross-sectional shape, such as any of the exemplary cross-sectional shapes described herein, and a mating vertical frame member, circular frame member and vertical pole member would have a corresponding cross-sectional shape.
FIGS. 8A-8C respectively show a side view, a top view and an end view of a sixth exemplary embodiment of a sleeve-joint coupling 800 for a trampoline frame according to the subject matter disclosed herein. Sleeve-joint coupling 800 is generally shaped as a “T” and includes three arm members 801 - 803 , each having a generally round cross-sectional shape. Sleeve-joint coupling 800 also includes a side sleeve member 804 having an aperture 805 , configured as a blind hole, that receives a safety enclosure vertical pole member (not shown in FIGS. 8A-8C ) having a generally round cross-sectional member. Side sleeve member 804 has sufficient length and strength to allow a safety enclosure vertical pole to extend into side sleeve member 804 so that the vertical pole would not come out during use. Each arm member 801 - 803 receives a trampoline frame member (also not shown in FIGS. 8A-8C ) of similar cross-sectional shape into an opening 806 ( FIG. 8C ). In an alternative embodiment, aperture 805 could be configured to allow a safety enclosure vertical pole to extend through the length of the side sleeve member 804 to the ground or to another device that fastens the vertical pole to the corresponding vertical frame member 103 .
FIGS. 9A-9C respectively show side, top and end views of an exemplary embodiment of a coupling member 900 for a trampoline frame according to the subject matter disclosed herein. Coupling member 900 is generally shaped as a “T” and includes three arm members 901 - 903 , each having a cross-sectional shape having a portion that is generally round. Each arm member 901 and 902 receives a corresponding circular frame member 104 . Arm member 903 receives a corresponding vertical frame member 103 . Alternatively, each arm member 901 - 903 has a cross-sectional shape that matches the cross-sectional shape of the corresponding circular frame member and vertical frame member. Arm 903 of coupling member 900 is also configured with flange members 903 a and 903 b that receive a vertical pole member 105 of a safety enclosure. Vertical pole member 105 is held in place between flange members 903 a and 903 b with fasteners 904 a and 904 b , such as a bolt 904 a and nut 904 b , that extend through holes (not shown) in vertical pole member 105 . Flange members 903 a and 903 b have sufficient length and strength, and fasteners 904 a and 904 b have sufficient strength so that vertical pole member 105 remains in place during use. In an alternative embodiment, vertical pole member 105 could extend past flange member 903 a and 903 b to the ground or to another device that fastens vertical pole member 105 to the corresponding vertical frame member 103 .
FIG. 10 depicts a top cutaway view of the first exemplary embodiment of a sleeve-joint coupling 200 according to the subject matter disclosed herein. Two circular frame members 104 A and 104 B are shown in FIG. 10 respectively engaging arm members 201 and 202 of sleeve-joint coupling 200 . A vertical pole member 105 of a safety enclosure is also shown. A frame tension member 1001 , such as a strap of webbing, a wire or a cable, is shown threaded through circular frame members 104 A and 104 B and sleeve-joint coupling 200 , in addition the other circular frame members and sleeve-joint coupling forming a trampoline frame. Frame tension member 1001 is fastened in a well-known manner to a hook assembly 1002 that engages a loop 1003 of a buckle assembly 1004 that is accessible through a hole (not shown) in circular frame member 104 B. Buckle assembly 1004 has two positions; an open position that allows hook assembly 1002 and loop 1003 to be conveniently engaged, and a closed assembly that places frame tension member 1001 under tension. When frame tension member 1001 is under tension, each sleeve-joint coupling 200 that frame tension member 1001 passes through is urged toward the center of the trampoline frame structure, thereby making the joints of frame structure even more reliable. Alternatively, a plurality of frame tension members can be used to form a line of continuous tension around a trampoline frame instead of a single frame tension member, as depicted in FIG. 10 . As yet another alternative, frame tension member 1001 could be attached to the outside of sleeve-joint coupling 200 , such as through a loop fastened to the outside of sleeve-joint coupling 200 . Still another alternative provides that a turn-buckle arrangement is used for placing tension on frame tension member 1001 .
While exemplary trampoline 100 shown in FIG. 1 is depicted as being round, it should be understood that the subject matter disclosed herein could be used with a trampoline and safety enclosure having a different shape, such as square, rectangular or oval. Additionally, the sleeve-joint coupling of the subject matter disclosed herein can be made from any suitable material that has sufficient strength to bear the loads and stresses that are associated with trampolines, such as metals and plastics. Further, while the sleeve-joint coupling of the subject matter disclosed herein has been described in terms of vertical frame members and circular frame members fitting into the sleeve-joint coupling, it should be understood that the sleeve-joint coupling of the subject matter disclosed herein can be configured so that one or all of the arm members of the sleeve-joint coupling fit into vertical frame members and circular frame members of the trampoline frame. Further still, while the sleeve-joint coupling of the subject matter disclosed herein has been described as having several exemplary cross-sectional shapes, it should be understood that a sleeve-joint coupling according to the subject matter disclosed herein could have any cross-sectional shape or have arm members having different cross-sectional shapes. As yet another alternative, the sleeve-joint coupling of the subject matter disclosed herein could be formed to be part of a vertical frame member. As still another alternative, the sleeve-joint coupling of the subject matter disclosed herein could be configured to substantially form a “T”.
While the vertical pole members 105 of safety enclosure 101 has been described as extending into vertical frame members 103 , it should be understood that at least one or more vertical pole member 105 of safety enclosure 101 could extend to the ground along the outside of a vertical frame member 103 , in which case such a vertical pole member would be attached to the corresponding vertical frame member at a minimum of two places, such as by using a sleeve-joint coupling similar to that shown in FIGS. 8A-8C and, for example, a tie-wrap device near the bottom of a vertical frame member 103 .
As yet another alternative embodiment, a safety enclosure vertical pole member 105 could be configured to form an arch ( 105 a of trampoline 100 a in FIG. 11 ), or an arc shape, between two frame members 103 . The two frame members 103 could be adjacent or could be separated by one or more other frame members 103 . A horizontal support member would then be connected between adjacent peaks of an arch in a substantially inflexible manner.
Although the foregoing subject matter has been described in some detail for purposes of clarity of understanding, it will be apparent that certain changes and modifications may be practiced that are within the scope of the appended claims. Accordingly, the present embodiments are to be considered as exemplary and not restrictive, and the subject matter disclosed herein is not to be limited to the details given herein, but may be modified within the scope and equivalents of the appended claims. | A recreational structure, such as a trampoline frame, can be quickly and reliably assembled using a coupling member generally having a “T” configuration. A first arm member and a second arm member are disposed in an opposite relationship with each other. The first and second arm members each receive one end of a horizontal frame member of the recreational structure. The third arm member includes flange members that receive one end of a vertical frame member of the recreational structure and one end of a vertical pole member of, for example, a safety enclosure. | 0 |
This application is a Continuation-In-Part of U.S. patent application Ser. No. 09/688,946 filed Oct. 16, 2000, now U.S. Pat. No. 6,733,744 and expressly incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
This invention relates to novel optical probes for use in physiological function monitoring, particularly indole and benzoindole compounds.
BACKGROUND OF THE INVENTION
Dynamic monitoring of physiological functions of patients at the bedside is highly desirable in order to minimize the risk of acute renal failure brought about by various clinical, physiological, and pathological conditions (C. A. Ravito, L. S. T. Fang, and A. C. Waltman, Renal function in patients at risk with contrast material-induced acute renal failure: Noninvasive real-time monitoring Radiology 1993,186, 851-854; N. L. Tilney, and J. M. Lazarus, Acute renal failure in surgical patients: Causes, clinical patterns, and care, Surgical Clinics of North America, 1983, 63, 357-377; B. E. VanZee, W. E. Hoy, and J. R. Jaenike, Renal injury associated with intravenous pyelography in non-diabetic and diabetic patients, Annals of Internal Medicine, 1978, 89, 51- 54; S. Lundqvist, G. Edbom, S. Groth, U. Stendahl, and S.-O. Hietala, Iohexol clearance for renal function measurement in gynecologic cancer patients, Acta Radiologica, 1996, 37, 582-586; P. Guesry, L. Kaufman, S. Orlof, J. A. Nelson, S. Swann, and M. Holliday, Measurement of glomerular filtration rate by fluorescent excitation of non-radioactive meglumine iothalamate, Clinical Nephrology, 1975, 3, 134-138). This monitoring is particularly important in the case of critically ill or injured patients because a large percentage of these patients face the risk of multiple organ failure (MOF), resulting in death (C. C. Baker et al., Epidemiology of Trauma Deaths, American Journal of Surgery, 1980, 144-150; G. Regel et al., Treatment Results of Patients with Multiple Trauma: An Analysis of 3406 Cases Treated Between 1972 and 1991 at a German Level I Trauma Center, Journal of Trauma, 1995, 38, 70-77). MOF is a sequential failure of lung, liver, and kidneys, and is incited by one or more severe causes such as acute lung injury (ALI), adult respiratory distress syndrome (ARDS), hypermetabolism, hypotension, persistent inflammatory focus, or sepsis syndrome. The common histological features of hypotension and shock leading to MOF include tissue necrosis, vascular congestion, interstitial and cellular edema, hemorrhage, and microthrombi. These changes affect the lung, liver, kidneys, intestine, adrenal glands, brain, and pancreas, in descending order of frequency (J. Coalson, Pathology of Sepsis, Septic Shock, and Multiple Organ Failure. In New Horizons: Multiple Organ Failure, D. J. Bihari and F. B. Cerra (Eds). Society of Critical Care Medicine , Fullerton, Calif., 1986, pp. 27-59). The transition from early stages of trauma to clinical MOF is marked by the extent of liver and renal failure and a change in mortality risk from about 30% to about 50% (F. B. Cerra, Multiple Organ Failure Syndrome. In New Horizons: Multiple Organ Failure, D. J. Bihari and F. B. Cerra (Eds). Society of Critical Care Medicine , Fullerton, Calif., 1989, pp. 1-24).
Serum creatinine measured at frequent intervals by clinical laboratories is currently the most common way of assessing renal function and following the dynamic changes in renal function which occur in critically ill patients (P. D. Doolan, E. L. Alpen, and G. B. Theil, A clinical appraisal of the plasma concentration and endogenous clearance of creatinine, American Journal of Medicine, 1962, 32, 65-79; J. B. Henry (Ed). Clinical Diagnosis and Management by Laboratory Methods, 17th Edition, W. B. Saunders, Philadelphia, Pa., 1984); C. E. Speicher, The right test: A physician's guide to laboratory medicine, W. B. Saunders, Philadelphia, Pa., 1989). These values are frequently misleading, since age, state of hydration, renal perfusion, muscle mass, dietary intake, and many other clinical and anthropometric variables affect the value. In addition, a single value returned several hours after sampling is difficult to correlate with other important physiologic events such as blood pressure, cardiac output, state of hydration and other specific clinical events (e.g., hemorrhage, bacteremia, ventilator settings and others). An approximation of glomerular filtration rate can be made via a 24-hour urine collection, but this requires 24 hours to collect the sample, several more hours to analyze the sample, and a meticulous bedside collection technique. New or repeat data are equally cumbersome to obtain. Occasionally, changes in serum creatinine must be further adjusted based on the values for urinary electrolytes, osmolality, and derived calculations such as the “renal failure index” or the “fractional excretion of sodium”. These require additional samples of serum collected contemporaneously with urine samples and, after a delay, precise calculations. Frequently, dosing of medication is adjusted for renal function and thus can be equally as inaccurate, equally delayed, and as difficult to reassess as the values upon which they are based. Finally, clinical decisions in the critically ill population are often as important in their timing as they are in their accuracy.
Exogenous markers such as inulin, iohexol, 51 Cr-EDTA, Gd-DTPA, or 99m Tc-DTPA have been reported to measure the glomerular filtration rate (GFR) (P. L. Choyke, H. A. Austin, and J. A. Frank, Hydrated clearance of gadolinium -DTPA as a measurement of glomerular filtration rate, Kidney International, 1992, 41, 1595-1598; M. F. Tweedle, X. Zhang, M. Fernandez, P. Wedeking, A. D. Nunn, and H. W. Strauss, A noninvasive method for monitoring renal status at bedside, Invest. Radiol., 1997, 32, 802-805; N. Lewis, R. Kerr, and C. Van Buren, Comparative evaluation of urographic contrast media, inulin, and 99m Tc -DTPA clearance methods for determination of glomerular filtration rate in clinical transplantation, Transplantation, 1989, 48, 790-796). Other markers such as 123 I and 125 I labeled o-iodohippurate or 99m Tc-MAG 3 are used to assess tubular secretion processes (W. N. Tauxe, Tubular Function, in Nuclear Medicine in Clinical Urology and Nephrology , W. N. Tauxe and E. V. Dubovsky, Editors, pp. 77-105, Appleton Century Crofts, East Norwalk, 1985; R. Muller-Suur, and C. Muller-Suur, Glomerular filtration and tubular secretion of MAG 3 in rat kidney, Journal of Nuclear Medicine, 1989, 30,1986-1991). However, these markers have several undesirable properties such as the use of radioactivity or ex-vivo handling of blood and urine samples. Thus, in order to assess the status and to follow the progress of renal disease, there is a considerable interest in developing a simple, safe, accurate, and continuous method for determining renal function, preferably by non-radioactive procedures. Other organs and physiological functions that would benefit from real-time monitoring include the heart, the liver, and blood perfusion, especially in organ transplant patients.
Hydrophilic, anionic substances are generally recognized to be excreted by the kidneys (F. Roch-Ramel, K. Besseghir, and H. Murer, Renal excretion and tubular transport of organic anions and cations, Handbook of Physiology, Section 8 , Neurological Physiology , Vol. II, E. E. Windhager, Editor, pp. 2189-2262, Oxford University Press, New York, 1992; D. L. Nosco, and J. A. Beaty-Nosco, Chemistry of technetium radiopharmaceuticals 1: Chemistry behind the development of technetium-99m compounds to determine kidney function, Coordination Chemistry Reviews, 1999, 184, 91-123). It is further recognized that drugs bearing sulfonate residues exhibit improved clearance through the kidneys (J. Baldas, J. Bonnyman, Preparation, HPLC studies and biological behavior of technetium-99m and 99mTcN0-radiopharmaceuticals based on quinoline type ligands, Nucl. Med. Biol., 1999, 19, 491-496; L Hansen, A. Taylor, L., L. G. Marzilli, Synthesis of the sulfonate and phosphonate derivatives of mercaptoacetyltriglycine. X-ray crystal structure of Na 2 [ReO(mercaptoacetylglycylglycylaminomethane-sulfonate)]3H 2 0 , Met.-Based Drugs, 1994, 1, 31-39).
Assessment of renal function by continuously monitoring the blood clearance of exogenous optical markers, viz., fluorescein bioconjugates derived from anionic polypeptides, has been developed by us and by others (R. B. Dorshow, J. E. Bugaj, B. D. Burleigh, J. R. Duncan, M. A. Johnson, and W. B. Jones, Noninvasive fluorescence detection of hepatic and renal function, Journal of Biomedical Optics, 1998, 3, 340-345; M. Sohtell et al., FITC-Inulin as a Kidney Tubule Marker in the Rat, Acta. Physiol. Scand., 1983, 119, 313-316, each of which is expressly incorporated herein by reference). The main drawback of high molecular weight polypeptides is that they are immunogenic. In addition, large polymers with narrow molecular weight distribution are difficult to prepare, especially in large quantities. Thus, there is a need in the art to develop low molecular weight compounds that absorb and/or emit light that can be used for assessing renal, hepatic, cardiac and other organ functions.
SUMMARY OF THE INVENTION
The present invention overcomes these difficulties by incorporating hydrophilic anionic or polyhydroxy residues in the form of sulfates, sulfonates, sulfamates and strategically positioned hydroxyl groups. Thus, the present invention is related to novel dyes containing multiple hydrophilic moieties and their use as diagnostic agents for assessing organ function.
The novel compounds of the present invention comprise dyes of Formulas 1 to 6 which are hydrophilic and absorb light in the visible and near infrared regions of the electromagnetic spectrum. The blood clearance rate can be modified by formulating the dyes in liposomes, micelles, or other microparticles. This enhances their use for physiological monitoring of many organs. Compounds with longer blood persistence are useful for angiography and organ perfusion analysis, which is particularly useful in organ transplant and critical ill patients. Predominant kidney clearance of the dyes enables their use for dynamic renal function monitoring, and rapid liver uptake of the dyes from blood serves as a useful index for the evaluation of hepatic function.
As illustrated in FIGS. 1-7 , these dyes are designed to inhibit aggregation in solution by preventing intramolecular and intermolecular induced hydrophobic interactions.
The present invention relates particularly to the novel compounds comprising indoles of the general Formula 1
wherein R 3 , R 4 , R 5 , R 6 , and R 7 , and Y 1 are independently selected from the group consisting of —H, C1-C10 alkoxyl, C1-C10 polyalkoxyalkyl, C1-C20 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, glucose derivatives of R groups, saccharides, amino, C1-C10 aminoalkyl, cyano, nitro, halogen, hydrophilic peptides, arylpolysulfonates, C1-C10 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —(CH 2 ) a CONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCO(CH 2 ) b SO 3 T, —(CH 2 ) a NHCONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCSNH(CH 2 ) b SO 3 T, —(CH 2 ) a OCONH(CH 2 ) b SO 3 T, —(CH 2 ) a PO 3 HT, —(CH 2 ) a PO 3 T 2 , —(CH 2 ) a OPO 3 HT, —(CH 2 ) a OPO 3 T 2 , —(CH 2 ) a NHPO 3 HT, —(CH 2 ) a NHPO 3 T 2 , —(CH 2 ) a CO 2 (CH 2 ) b PO 3 HT, —(CH 2 ) a CO 2 (CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCO(CH 2 ) b PO 3 HT, —(CH 2 ) a OCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a CONH(CH 2 ) b PO 3 HT, —(CH 2 ) a CONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCO(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCONH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCONH(CH 2 ) b PO 3 HT, and —(CH 2 ) a OCONH(CH 2 ) b PO 3 T 2 , —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 1 is selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; a, b, d, f, h, i, and j independently vary from 1-10; c, e, g, and k independently vary from 1-100; R a , R b , R c , and R d are defined in the same manner as Y 1 ; T is either H or a negative charge.
The present invention also relates to the novel compounds comprising benzoindoles of general Formula 2
wherein R 8 , R 9 , R 10 , R 11 , R 12 , R 13 , R 14 , and Y 2 are independently selected from the group consisting of —H, C1-C10 alkoxyl, C1-C10 polyalkoxyalkyl, C1-C20 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, glucose derivatives of R groups, saccharides, amino, C1-C10 aminoalkyl, cyano, nitro, halogen, hydrophilic peptides, arylpolysulfonates, C1-C10 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —(CH 2 ) a CONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCO(CH 2 ) b SO 3 T, —(CH 2 ) a NHCONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCSNH(CH 2 ) b SO 3 T, —(CH 2 ) a OCONH(CH 2 ) b SO 3 T, —(CH 2 ) a PO 3 HT, —(CH 2 ) a PO 3 T 2 , —(CH 2 ) a OPO 3 HT, —(CH 2 ) a OPO 3 T 2 , —(CH 2 ) a NHPO 3 HT, —(CH 2 ) a NHPO 3 T 2 , —(CH 2 ) a CO 2 (CH 2 ) b PO 3 HT, —(CH 2 ) a CO 2 (CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCO(CH 2 ) b PO 3 HT, —(CH 2 ) a OCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a CONH(CH 2 ) b PO 3 HT, —(CH 2 ) a CONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCO(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCONH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCONH(CH 2 ) b PO 3 HT, and —(CH 2 ) a OCONH(CH 2 ) b PO 3 T 2 , —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 2 is selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; a, b, d, f, h, i, and j independently vary from 1-10; c, e, g, and k independently vary from 1-100; R a , R b , R c , and R d are defined in the same manner as Y 2 ; T is either H or a negative charge.
The present invention also relates to the novel compounds comprising cyanine dyes of general Formula 3
wherein R 15 , R 16 , R 17 , R 18 , R 19 , R 20 , R 21 , R 22 , R 23 , Y 3 , and Z 3 are independently selected from the group consisting of —H, C1-C10 alkoxyl, C1-C10 polyalkoxyalkyl, C1-C20 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, glucose derivatives of R groups, saccharides, amino, C1-C10 aminoalkyl, cyano, nitro, halogen, hydrophilic peptides, arylpolysulfonates, C1-C10 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —(CH 2 ) a CONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCO(CH 2 ) b SO 3 T, —(CH 2 ) a NHCONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCSNH(CH 2 ) b SO 3 T, —(CH 2 ) a OCONH(CH 2 ) b SO 3 T, —(CH 2 ) a PO 3 HT, —(CH 2 ) a PO 3 T 2 , —(CH 2 ) a OPO 3 HT, —(CH 2 ) a OPO 3 T 2 , —(CH 2 ) a NHPO 3 HT, —(CH 2 ) a NHPO 3 T 2 , —(CH 2 ) a CO 2 (CH 2 ) b PO 3 HT, —(CH 2 ) a CO 2 (CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCO(CH 2 ) b PO 3 HT, —(CH 2 ) a OCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a CONH(CH 2 ) b PO 3 HT, —(CH 2 ) a CONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCO(CH 2 ) b PO 3 HT, —CH 2 ) a NHCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCONH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCONH(CH 2 ) b PO 3 HT, and —(CH 2 ) a OCONH(CH 2 ) b PO 3 T 2 , —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 3 and X 3 are selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; V 3 is a single bond or is selected from the group consisting of —O—, —S—, —Se—, and —NR a ; a, b, d, f, h, i, and j independently vary from 1-10; c, e, g, and k independently vary from 1-100; a 3 and b 3 vary from 0 to 5; R a , R b , R c , and R d are defined in the same manner as Y 3 ; T is either H or a negative charge.
The present invention further relates to the novel compounds comprising cyanine dyes of general Formula 4
wherein R 24 , R 25 , R 26 , R 27 , R 28 , R 29 , R 30 , R 31 , R 32 , R 33 , R 34 , R 35 , R 36 , Y 4 , and Z 4 are independently selected from the group consisting of —H, C1-C10 alkoxyl, C1-C10 polyalkoxyalkyl, C1-C20 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, saccharides, glucose derivatives of R groups, amino, C1-C10 aminoalkyl, cyano, nitro, halogen, hydrophilic peptides, arylpolysulfonates, C1-C10 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —(CH 2 ) a CONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCO(CH 2 ) b SO 3 T, —(CH 2 ) a NHCONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCSNH(CH 2 ) b SO 3 T, —(CH 2 ) a OCONH(CH 2 ) b SO 3 T, —(CH 2 ) a PO 3 HT, —(CH 2 ) a PO 3 T 2 , —(CH 2 ) a OPO 3 HT, —(CH 2 ) a OPO 3 T 2 , —(CH 2 ) a NHPO 3 HT, —(CH 2 ) a NHPO 3 T 2 , —(CH 2 ) a CO 2 (CH 2 ) b PO 3 HT, —(CH 2 ) a CO 2 (CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCO(CH 2 ) b PO 3 HT, —(CH 2 ) a OCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a CONH(CH 2 ) b PO 3 HT, —CH 2 ) a CONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCO(CH 2 ) b PO 3 HT, —CH 2 ) a NHCO(CH 2 ) b PO 3 T 2 , —CH 2 ) a NHCONH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCONH(CH 2 ) b PO 3 HT, and —(CH 2 ) a OCONH(CH 2 ) b PO 3 T 2 , —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 4 and X 4 are selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; V 4 is a single bond or is selected from the group consisting of —O—, —S—, —Se—, and —NR a ; a 4 and b 4 vary from 0 to 5; a, b, d, f, h, i, and j independently vary from 1-10; c, e, g, and k independently vary from 1-100; R a , R b , R c , and R d are defined in the same manner as Y 4 ; T is either H or a negative charge.
The present invention also relates to the novel compounds comprising cyanine dyes of general Formula 5
wherein R 37 , R 38 , R 39 , R 40 , R 41 , R 42 , R 43 , R 44 , R 45 , Y 5 , and Z 5 are independently selected from the group consisting of —H, C1-C10 alkoxyl, C1-C10 polyalkoxyalkyl, C1-C20 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, glucose derivatives of R groups, saccharides, amino, C1-C10 aminoalkyl, cyano, nitro, halogen, hydrophilic peptides, arylpolysulfonates, C1-C10 alkyl, C1-C10 aryl-C5C20 aryl-, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —(CH 2 ) a CONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCO(CH 2 ) b SO 3 T, —(CH 2 ) a NHCONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCSNH(CH 2 ) b SO 3 T, —(CH 2 ) a OCONH(CH 2 ) b SO 3 T, —(CH 2 ) a PO 3 HT, —(CH 2 ) a PO 3 T 2 , —(CH 2 ) a OPO 3 HT, —(CH 2 ) a OPO 3 T 2 , —(CH 2 ) a NHPO 3 HT, —(CH 2 ) a NHPO 3 T 2 , —(CH 2 ) a CO 2 (CH 2 ) b PO 3 HT, —(CH 2 ) a CO 2 (CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCO(CH 2 ) b PO 3 HT, —(CH 2 ) a OCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a CONH(CH 2 ) b PO 3 HT, —(CH 2 ) a CONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCO(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCONH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCONH(CH 2 ) b PO 3 HT, and —(CH 2 ) a OCONH(CH 2 ) b PO 3 T 2 , —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 5 and X 5 are selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; V 5 is a single bond or is selected from the group consisting of —O—, —S—, —Se—, and —NR a ; D 5 is a single or a double bond; A 5 , B 5 and E 5 may be the same or different and are selected from the group consisting of —O—, —S—, —Se—, —P—, —NR a , —CR c R d , CR c , alkyl, and —C═O; A 5 , B 5 , D 5 , and E 5 may together form a 6 or 7 membered carbocyclic ring or a 6 or 7 membered heterocyclic ring optionally containing one or more oxygen, nitrogen, or a sulfur atom; a, b, d, f, h, i, and j independently vary from 1-10; c, e, g, and k independently vary from 1-100; a 5 and b 5 vary from 0 to 5; R a , R b , R c , and R d are defined in the same manner as Y 5 ; T is either H or a negative charge.
The present invention also relates to the novel compounds comprising cyanine dyes of general Formula 6
wherein R 46 , R 47 , R 48 , R 49 , R 50 , R 51 , R 52 , R 53 , R 54 , R 55 , R 56 , R 57 and R 58 , Y 6 , and Z 6 are independently selected from the group consisting of —H, C1-C10 alkoxyl, C1-C10 polyalkoxyalkyl, C1-C20 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, saccharides, glucose derivatives of R groups, amino, C1-C10 aminoalkyl, cyano, nitro, halogen, hydrophilic peptides, arylpolysulfonates, C1-C10 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH,—(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —(CH 2 ) a CONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCO(CH 2 ) b SO 3 T, —(CH 2 ) a NHCONH(CH 2 ) b SO 3 T, —(CH 2 ) a NHCSNH(CH 2 ) b SO 3 T, —(CH 2 ) a OCONH(CH 2 ) b SO 3 T, —(CH 2 ) a PO 3 HT, —(CH 2 ) a PO 3 T 2 , —(CH 2 ) a OPO 3 HT, —(CH 2 ) a OPO 3 T 2 , —(CH 2 ) a NHPO 3 HT, —(CH 2 ) a NHPO 3 T 2 , —(CH 2 ) a CO 2 (CH 2 ) b PO 3 HT, —(CH 2 ) a CO 2 (CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCO(CH 2 ) b PO 3 HT, —(CH 2 ) a OCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a CONH(CH 2 ) b PO 3 HT, —(CH 2 ) a CONH(CH 2 ) b PO 3 T 2 , —CH 2 ) a NHCO(CH 2 ) b PO 3 HT, —CH 2 ) a NHCO(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCONH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCONH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 HT, —(CH 2 ) a NHCSNH(CH 2 ) b PO 3 T 2 , —(CH 2 ) a OCONH(CH 2 ) b PO 3 HT, and —(CH 2 ) a OCONH(CH 2 ) b PO 3 T 2 , —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 6 and X 6 are selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; V 6 is a single bond or is selected from the group consisting of —O—, —S—, —Se—, and —NR a ; D6 is a single or a double bond; A 6 , B 6 and E 6 may be the same or different and are selected from the group consisting of —O—, —S—, —Se—, —P—, —NR a , —CR c R d , CR c , alkyl, and —C═O; A 6 , B 6 , D 6 , and E 6 may together form a 6 or 7 membered carbocyclic ring or a 6 or 7 membered heterocyclic ring optionally containing one or more oxygen, nitrogen, or sulfur atom; a, b, d, f, h, i, and j independently vary from 1-10; c, e, g, and k independently vary from 1-100; a 6 and b 6 vary from 0 to 5; R a , R b , R c , and R d are defined in the same manner as Y 6 ; T is either H or a negative charge.
A chelate such as ethylenediaminetetraacetic acid (EDTA), diethylenetriaminepentaacetic acid (DPTA), 1,4,7,10-tetraazacyclododecanetetraacetic acid (DOTA), or their derivatives, can be attached to the compounds of Formulas 1-6 as one or more R groups. These structures are expected to be highly water soluble.
The inventive compounds, compositions and methods advantageously provide a real-time, accurate, repeatable measure of renal excretion rate using exogenous markers under specific yet changing circumstances. This represents a substantial improvement over any currently available or widely practiced method, since no reliable, continuous, repeatable bedside method for the assessment of specific renal function by optical methods exists. Moreover, because the inventive method depends solely on the renal elimination of the exogenous chemical entity, the measurement is absolute and requires no subjective interpretation based on age, muscle mass, blood pressure, etc. In fact it represents the nature of renal function in a particular patient, under particular circumstances, at a precise moment in time.
The inventive compounds, compositions and methods provide simple, efficient, and effective monitoring of organ function. The compound is administered and a sensor, either external or internal, is used to detect absorption and/or emission to determine the rate at which the compound is cleared from the blood. By altering the R groups, the compounds may be rendered more organ specific.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 : Reaction pathway for the preparation of indole derivatives.
FIG. 2 : Reaction pathway for the preparation of benzoindole derivatives.
FIG. 3 : Reaction pathway for the preparation of indocarbocyanine derivatives.
FIG. 4 : Reaction pathway for the preparation of benzoindocarbocyanine derivatives.
FIG. 5 : Reaction pathway for the preparation of robust indocarbocyanine derivatives.
FIG. 6 : Reaction pathway for the preparation of robust benzoindocarbocyanine derivatives.
FIG. 7 : Reaction pathway for the preparation of long-wavelength absorbing indocarbocyanine derivatives.
FIG. 8 a : Absorption spectrum of indoledisulfonate in water.
FIG. 8 b : Emission spectrum of indoledisulfonate in water.
FIG. 9 a : Absorption spectrum of indocarbocyaninetetrasulfonate in water.
FIG. 9 b : Emission spectrum of indocarbocyaninetetrasulfonate in water.
FIG. 10 a : Absorption spectrum of chloroindocarbocyanine in acetonitrile.
FIG. 10 b : Emission spectrum of chloroindocarbocyanine in acetonitrile.
FIG. 11 : Blood clearance profile of carbocyanine-polyaspartic (10 kDa) acid conjugate in a rat.
FIG. 12 : Blood clearance profile of carbocyanine-polyaspartic (30 kDa) acid conjugate in a rat.
FIG. 13 : Blood clearance profile of indoledisulfonate in a rat.
FIG. 14 : Blood clearance profile of carbocyaninetetrasulfonates in a rat.
DETAILED DESCRIPTION
In one embodiment, the dyes of the invention serve as probes for continuous monitoring of renal function, especially for critically ill patients and kidney transplant patients.
In another embodiment, the dyes of the invention are useful for dynamic hepatic function monitoring, especially for critically ill patients and liver transplant patients.
In yet another embodiment, the dyes of the invention are useful for real-time determination of cardiac function, especially in patients with cardiac diseases.
In still another embodiment, the dyes of the invention are useful for monitoring organ perfusion, especially for critically ill, cancer, and organ transplant patients.
The novel dyes of the present invention are prepared according to methods well known in the art, as illustrated in general in FIGS. 1-7 and described for specific compounds in Examples 1-11.
In one embodiment, the novel compounds, also called tracers, have the Formula 1, wherein R 3 , R 4 , R 5 , R 6 and R 7 , and Y 1 are independently selected from the group consisting of —H, C1-C5 alkoxyl, C1-C5 polyalkoxyalkyl, C1-C10 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, mono- and disaccharides, nitro, hydrophilic peptides, arylpolysulfonates, C1-C5 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 1 is selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; a, b, d, f, h, I, and j independently vary from 1-5; c, e, g, and k independently vary from 1-20; R a , R b , R c , and R d are defined in the same manner as Y 1 ; T is a negative charge.
In another embodiment, the novel compounds have the general Formula 2, wherein R 8 , R 9 , R 10 , R 11 , R 12 , R 13 , R 14 , and Y 2 are independently selected from the group consisting of —H, C1-C5 alkoxyl, C1-C5 polyalkoxyalkyl, C1-C10 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, mono- and disaccharides, nitro, hydrophilic peptides, arylpolysulfonates, C1-C5 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 (CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 (CH 2 —O—CH 2 ) g —CH 2 NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 -(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 2 is selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; a, b, d, f, h, i, and j independently vary from 1-5; c, e, g, and k independently vary from 1-20; R a , R b , R c , and R d are defined in the same manner as Y 2 ; T is a negative charge.
In another embodiment, the novel compounds have the general Formula 3, wherein R 15 , R 16 , R 17 , R 18 , R 1 g, R 20 , R 21 , R 22 , R 23 , Y 3 , and Z 3 are independently selected from the group consisting of —H, C1-C5 alkoxyl, C1-C5 polyalkoxyalkyl, C1-C10 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, mono- and disaccharides, nitro, hydrophilic peptides, arylpolysulfonates, C1-C5 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 3 and X 3 are selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; V 3 is a single bond or is selected from the group consisting of —O—, —S—, —Se—, and —NR a ; a, b, d, f, h, i, and j independently vary from 1-5; c, e, g, and k independently vary from 1-50; a 3 and b 3 vary from 0 to 5; R a , R b , R c , and R d are defined in the same manner as Y 3 ; T is either H or a negative charge.
In another embodiment, the novel compounds have the general Formula 4, wherein R 24 , R 25 , R 26 , R 27 , R 28 , R 29 , R 30 , R 31 , R 32 , R 33 , R 34 , R 35 , R 36 , Y 4 , and Z 4 are independently selected from the group consisting of —H, C1-C5 alkoxyl, C1-C5 polyalkoxyalkyl, C1-C10 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, mono- and disaccharides, nitro, hydrophilic peptides, arylpolysulfonates, C1-C5 alkyl, C1-C10 aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 CO 2 T; W 4 and X 4 are selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; V 4 is a single bond or is selected from the group consisting of —O—, —S—, —Se—, and —NR a ; a 4 and b 4 vary from 0 to 5; a, b, d, f, h, i, and j independently vary from 1-5; c, e, g, and k independently vary from 1-50; R a , R b , R c , and R d are defined in the same manner as Y 4 ; T is either H or a negative charge.
In another embodiment, the novel compounds have the general Formula 5, wherein R 37 , R 38 , R 39 , R 40 , R 41 , R 42 , R 43 , R 44 , R 45 , Y 5 , and Z 5 are independently selected from the group consisting of —H, C1-C5 alkoxyl, C1-C5 polyalkoxyalkyl, C1-C10 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, mono- and disaccharides, nitro, hydrophilic peptides, arylpolysulfonates, C1-C5 alkyl, C1-C10 aryl-C5-C20 aryl-, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) 2 SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 CO 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O—CH 2 ) k —CH 2 —CO 2 T; W 5 and X 5 are selected from the group consisting of —CR c CR d , —O—, —NR c , —S—, and —Se; V 5 is a single bond or is selected from the group consisting of —O—, —S—, —Se—, and NR a ; D 5 is a single or a double bond; A 5 , B 5 and E 5 may be the same or different and are selected from the group consisting of —O—, —S—, —NR a , —CR c R d , CR c , and alkyl; A 5 , B 5 , D 5 , and E 5 may together form a 6 or 7 membered carbocyclic ring or a 6 or 7 membered heterocyclic ring optionally containing one or more oxygen, nitrogen, or sulfur atom; a, b, d, f, h, i, and j independently vary from 1-5; c, e, g, and k independently vary from 1-50; a5 and b 5 vary from 0 to 5; R a , R b , R c , and R d are defined in the same manner as Y 5 ; T is either H or a negative charge.
In yet another embodiment, the novel compounds have the general Formula 6, wherein R 46 , R 47 , R 48 , R 49 , R 50 , R 51 , R 52 , R 53 , R 54 , R 55 , R 56 , R 57 , R 58 , Y 6 , and Z 6 are independently selected from the group consisting of —H, C1-C5 alkoxyl, C1-C5 polyalkoxyalkyl, C1-C10 polyhydroxyalkyl, C5-C20 polyhydroxyaryl, mono- and disaccharides, nitro, hydrophilic peptides, arylpolysulfonates, C1-C5 alkyl, C1-C10aryl, —SO 3 T, —CO 2 T, —OH, —(CH 2 ) a SO 3 T, —(CH 2 ) a OSO 3 T, —(CH 2 ) a NHSO 3 T, —(CH 2 ) a CO 2 (CH 2 ) b SO 3 T, —(CH 2 ) a OCO(CH 2 ) b SO 3 T, —CH 2 (CH 2 —O—CH 2 ) c —CH 2 —OH, —(CH 2 ) d —CO 2 T, —CH 2 —(CH 2 —O—CH 2 ) e —CH 2 —CO 2 T, —(CH 2 ) f —NH 2 , —CH 2 —(CH 2 —O—CH 2 ) g —CH 2 —NH 2 , —(CH 2 ) h —N(R a )—(CH 2 ) i —CO 2 T, and —(CH 2 ) j —N(R b )—CH 2 —(CH 2 —O——CH 2 ) k —CH 2 —CO 2 T; W 6 and X 6 are selected from the group consisting of —CR c R d , —O—, —NR c , —S—, and —Se; V 6 is a single bond or is selected from the group consisting of —O—, —S—, —Se—, and —NR a ; D 6 is a single or a double bond; A 6 , B 6 and E 6 may be the same or different and are selected from the group consisting of —O—, —S—, —NR a , —CR c R d , CR c , and alkyl; A 6 , B 6 , D 6 , and E 6 may together form a 6 or 7 membered carbocyclic ring or a 6 or 7 membered heterocyclic ring optionally containing one or more oxygen, nitrogen, or sulfur atom; a, b, d, f, h, i, and j independently vary from 1-5; c, e, g, and k independently vary from 1-50; a 5 and b 5 vary from 0 to 5; R a , R b , R c , and R d are defined in the same manner as Y 6 ; T is either H or a negative charge.
The compounds of the invention can be formulated into diagnostic and therapeutic compositions for enteral or parenteral administration. These compositions contain an effective amount of the dye along with conventional pharmaceutical carriers and excipients appropriate for the type of administration contemplated. For example, parenteral formulations advantageously contain the inventive agent in a sterile aqueous solution or suspension. Parenteral compositions may be injected directly or mixed with a large volume parenteral composition for systemic administration. Such solutions also may contain pharmaceutically acceptable buffers and, optionally, electrolytes such as sodium chloride.
Formulations for enteral administration may vary widely, as is well known in the art. In general, such formulations are liquids, which include an effective amount of the inventive agent in aqueous solution or suspension. Such enteral compositions may optionally include buffers, surfactants, thixotropic agents, and the like. Compositions for oral administration may also contain flavoring agents and other ingredients for enhancing their organoleptic qualities.
The compositions are administered in doses effective to achieve the desired enhancement. The dosage of the tracers may vary according to the clinical procedure contemplated and generally ranges from 1 picomolar to 100 millimolar. The compositions may be administered to a patient, typically a warm-blooded animal either systemically or locally to the organ or tissue to be imaged, and the patient then subject to the imaging procedure. The tracers may be administered to the patient by any suitable method, including intravenous, intraperitoneal, or subcutaneous injection or infusion, oral administration, transdermal absorption through the skin, aerosols, or by inhalation. The detection of the tracers is achieved by optical fluorescence, absorbance, or light scattering methods known in the art (Muller et al. Eds, Medical Optical Tomography , SPIE Volume IS11, 1993, which is expressly incorporated herein by reference) using invasive or non-invasive probes such as endoscopes, catheters, ear clips, hand bands, surface coils, finger probes, and the like. Physiological function is correlated with the clearance profiles and rates of these agents from body fluids (R. B. Dorshow et al., Non -Invasive Fluorescence Detection of Hepatic and Renal Function, Bull. Am. Phys. Soc. 1997, 42, 681, which is expressly incorporated by reference herein).
The inventive composition may be administered for imaging by more than one modality. As one example, the composition may be used for imaging by optical imaging alone, by nuclear imaging alone, or by both optical and nuclear imaging modalities when a radioactive isotope is included in the chemical formula, such as replacing a halogen atom with a radioactive halogen, and/or including a radioactive metal ion such as Tc 99 , In 111 . As another example, the composition may be used for imaging by optical imaging alone, by magnetic resonance (MR) alone, or by both optical and MR modalities when a paramagnetic metal ion such as gadolinium or manganese is included in the chemical formula.
It will also be appreciated that the inventive compositions may be administered with other contrast agents or media used to enhance an image from a non-optical modality. These include agents for enhancing an image obtained by modalities including but not limited to MR, ultrasound (US), x-ray, positron emission tomography (PET), computed tomography (CT), single photon emission computed tomography (SPECT), etc. Both optical and non-optical agents may be formulated as a single composition (that is, one composition containing one, two or more components, for example, an optical agent and a MR agent), or may be formulated as separate compositions. The inventive optical imaging contrast agent and the non-optical contrast agent are administered in doses effective to achieve the desired enhancement, diagnosis, therapy, etc., as known to one skilled in the art. The inventive compositions, either alone or combined with a contrast agent, may be administered to a patient, typically a warm-blooded animal, systemically or locally to the organ or tissue to be imaged. The patient is then imaged by optical imaging and/or by another modality. As one example of this embodiment, the inventive compounds may be added to contrast media compositions. As another example, the inventive compositions may be co-administered with contrast media, either simultaneously or within the same diagnostic and/or therapeutic procedure (for example, administering the inventive composition and administering a contrast agent then performing optical imaging followed by another imaging modality, or administering the inventive composition and administering a contrast agent then performing another imaging modality followed by optical imaging, or administering the inventive composition and optical imaging, then administering a contrast agent and MR, US, CT, etc. imaging, or administering a contrast agent and imaging by MR, US, CT, etc., then administering the inventive composition and optical imaging, or administering the inventive composition and a contrast agent, and simultaneously imaging by an optical modality and MR, US, CT, etc.). As another example, an optical imaging agent may be added as an additive or excipient for a non-optical imaging modality. In this embodiment, the optically active component, such as the dyes disclosed herein, could be added as a buffering agent to control pH or as a chelate to improve formulation stability, etc. in MR contrast media, CT contrast media, x-ray contrast media, US contrast media, etc. The MR, CT, x-ray, US contrast media would then also function as an optical imaging agent. The information obtained from the modality using the non-optical contrast agent is useful in combination with the image obtained using the optical contrast agent.
In one embodiment, the agents may be formulated as micelles, liposomes, microcapsules, or other microparticles. These formulations may enhance delivery, localization, target specificity, administration, etc. Preparation and loading of these are well known in the art.
As one example, liposomes may be prepared from dipalmitoyl phosphatidylcholine (DPPC) or egg phosphatidylcholine (PC) because this lipid has a low heat transition. Liposomes are made using standard procedures as known to one skilled in the art (e.g., Braun-Falco et al., (Eds.), Griesbach Conference, Liposome Dermatics, Springer-Verlag, Berlin (1992)). Polycaprolactone, poly(glycolic) acid, poly(lactic) acid, polyanhydride or lipids may be formulated as microspheres. As an illustrative example, the optical agent may be mixed with polyvinyl alcohol (PVA), the mixture then dried and coated with ethylene vinyl acetate, then cooled again with PVA. In a liposome, the optical agent may be within one or both lipid bilayers, in the aqueous between the bilayers, or with the center or core. Liposomes may be modified with other molecules and lipids to form a cationic liposome. Liposomes may also be modified with lipids to render their surface more hydrophilic which increases their circulation time in the bloodstream. The thus-modified liposome has been termed a “stealth” liposome, or a long-lived liposome, as described in U.S. Pat. No. 6,258,378 which is expressly incorporated by reference herein in its entirety, and in Stealth Liposomes, Lasic and Martin (Eds.) 1995, CRC Press, London. Encapsulation methods include detergent dialysis, freeze drying, film forming, injection, as known to one skilled in the art and disclosed in, for example, U.S. Pat. No. 6,406,713 which is expressly incorporated by reference herein in its entirety.
The agent formulated in liposomes, microcapsules, etc. may be administered by any of the routes previously described. In a formulation applied topically, the optical agent is slowly released over time. In an injectable formulation, the liposome capsule circulates in the bloodstream and is delivered to a desired site.
Organ function can be assessed either by the differences in the manner in which the normal and impaired cells remove the tracer from the bloodstream, by measuring the rate or accumulation of these tracers in the organs or tissues, or by obtaining tomographic images of the organs or tissues. Blood pool clearance may be measured non-invasively from convenient surface capillaries such as those found in an ear lobe or a finger, for example, using an ear clip or finger clip sensor, or may be measured invasively using an endovascular catheter. Accumulation of the tracer within the cells of interest can be assessed in a similar fashion. The clearance of the tracer dyes may be determined by selecting excitation wavelengths and filters for the emitted photons. The concentration-time curves may be analyzed in real time by a microprocessor. In order to demonstrate feasibility of the inventive compounds to monitor organ function, a non-invasive absorbance or fluorescence detection system to monitor the signal emanating from the vasculature infused with the compounds is used. Indole derivatives, such as those of Formulas 1-6, fluoresce at a wavelength between 350 nm and 1300 nm when excited at the appropriate wavelength as is known to, or readily determined by, one skilled in the art.
In addition to the noninvasive techniques, a modified pulmonary artery catheter can be used to make the necessary measurements (R. B. Dorshow, J. E. Bugaj, S. A. Achilefu, R. Rajagopalan, and A. H. Combs, Monitoring Physiological Function by Detection of Exogenous Fluorescent Contrast Agents, in Optical Diagnostics of Biological Fluids IV , A. Priezzhev and T. Asakura, Editors, Proceedings of SPIE 1999, 3599, 2-8, which is expressly incorporated by reference herein). Currently, pulmonary artery catheters measure only intravascular pressures, cardiac output and other derived measures of blood flow. Critically ill patients are managed using these parameters, but rely on intermittent blood sampling and testing for assessment of renal function. These laboratory parameters represent discontinuous data and are frequently misleading in many patient populations. Yet, importantly, they are relied upon heavily for patient assessment, treatment decisions, and drug dosing.
The modified pulmonary artery catheter incorporates an optical sensor into the tip of a standard pulmonary artery catheter. This wavelength specific optical sensor can monitor the renal function specific elimination of an optically detectable chemical entity. Thus, by a method analogous to a dye dilution curve, real-time renal function can be monitored by the disappearance of the optically detected compound. Modification of a standard pulmonary artery catheter only requires making the fiber optic sensor wavelength specific, as is known to one skilled in this art. Catheters that incorporate fiber optic technology for measuring mixed venous oxygen saturation currently exist.
The present invention may be used for rapid bedside evaluation of renal function and also to monitor the efficiency of hemodialysis. The invention is further demonstrated by the following examples. Many modifications, variations, and changes in detail may be made to the described embodiments, and it is intended that all matter in the foregoing description and shown in the accompanying drawings be interpreted as illustrative and not in a limiting sense.
EXAMPLE 1
Synthesis of indole disulfonate (FIG. 1 , Compound 5, Y 7 ═SO 3 − ; X 7 ═H; n=1)
A mixture of 3-methyl-2-butanone (25.2 mL), and p-hydrazinobenzenesulfonic acid (15 g) in acetic acid (45 mL) was heated at 110° C. for 3 hours. After reaction, the mixture was allowed to cool to room temperature and ethyl acetate (100 mL) was added to precipitate the product, which was filtered and washed with ethyl acetate (100 mL). The intermediate compound, 2,3,3-trimethylindolenium-5-sulfonate ( FIG. 1 , compound 3 ) was obtained as a pink powder in 80% yield. A portion of compound 3 (9.2 g) in methanol (115 mL) was carefully added to a solution of KOH in isopropanol (100 mL). A yellow potassium salt of the sulfonate was obtained in 85% yield after vacuum-drying for 12 hours. A portion of the 2,3,3-trimethylindolenium-5-sulfonate potassium salt (4 g) and 1,3-propanesultone (2.1 g) was heated in dichlorobenzene (40 mL) at 110° C. for 12 hours. The mixture was allowed to cool to room temperature and the resulting precipitate was filtered and washed with isopropanol. The resulting pink powder was dried under vacuum to give 97% of the desired compound.
Other compounds prepared by a similar method described above include polyhydroxyl indoles such as
EXAMPLE 2
Synthesis of indole disulfonate (FIG. 1 , Compound 5, Y 7 ═SO 3 − ; X 7 ═H; n=2)
This compound was prepared by the same procedure described in Example 1, except that 1,4-butanesultone was used in place of 1,3-propanesultone.
EXAMPLE 3
Synthesis of benzoindole disulfonate (FIG. 2 , Compound 8, Y 7 Y 8 ═SO 3 − ; X 7 ═H; n=2)
This compound was prepared by the same procedure described in Example 1, except that hydrazinonaphthalenedisulfonic acid was used in place of hydrazinobenzenesulfonic acid.
Other compounds prepared by a similar method include polyhydroxyindoles such as:
EXAMPLE 4
Synthesis of benzoindole disulfonate (FIG. 2 , Compound 8, Y 7 , Y 8 ═SO 3 − ; X 7 ═OH; n=4)
This compound was prepared by the same procedure described in Example 1, except that 3-hydroxymethyl-4-hydroxyl-2-butanone was used in place of 3-methyl-2-butanone.
EXAMPLE 5
Synthesis of Bis(ethylcarboxymethyl)indocyanine Dye
A mixture of 1,1,2-trimethyl-[1H]-benz[e]indole (9.1 g, 43.58 mmoles) and 3-bromopropanoic acid (10.0 g, 65.37 mmoles) in 1,2-dichlorobenzene (40 mL) was heated at 110□ C for 12 hours. The solution was cooled to room temperature and the red residue obtained was filtered and washed with acetonitrile:diethyl ether (1:1) mixture. The solid obtained was dried under vacuum to give 10 g (64%) of light brown powder. A portion of this solid (6.0 g; 16.56 mmoles), glutaconaldehyde dianil monohydrochloride (2.36 g, 8.28 mmoles) and sodium acetate trihydrate (2.93 g, 21.53 mmoles) in ethanol (150 mL) were refluxed for 90 minutes. After evaporating the solvent, 40 mL of 2 N aqueous HCl was added to the residue and the mixture was centrifuged and the supernatant was decanted. This procedure was repeated until the supernatant became nearly colorless. About 5 mL of water:acetonitrile (3:2) mixture was added to the solid residue and lyophilized to obtain 2 g of dark green flakes. The purity of the compound was established with 1 H-NMR and liquid chromatography/mass spectrometry (LC/MS).
EXAMPLE 6
Synthesis of Bis(pentylcarboxymethyl)indocyanine Dye
A mixture of 2,2,3-trimethyl-[1H]-benz[e]indole (20 g, 95.6 mmoles) and 6-bromohexanoic acid (28.1 g, 144.1 mmoles) in 1,2-dichlorobenzene (250 mL) was heated at 110° C. for 12 hours. The green solution was cooled to room temperature and the brown solid precipitate formed was collected by filtration. After washing the solid with 1,2dichlorobenzene and diethyl ether, the brown powder obtained (24 g, 64%) was dried under vacuum at room temperature. A portion of this solid (4.0 g; 9.8 mmoles), glutaconaldehyde dianil monohydrochloride (1.4 g, 5 mmoles) and sodium acetate trihydrate (1.8 g, 12.9 mmoles) in ethanol (80 mL) were refluxed for 1 hour. After evaporating the solvent, 20 mL of a 2 N aqueous HCl was added to the residue and the mixture was centrifuged and the supernatant was decanted. This procedure was repeated until the supernatant became nearly colorless. About 5 mL of water:acetonitrile (3:2) mixture was added to the solid residue and lyophilized to obtain about 2 g of dark green flakes. The purity of the compound was established with 1 H-NMR, HPLC, and LC-MS.
EXAMPLE 7
Synthesis of polyhydroxyindole sulfonate
( FIG. 3 , Compound 13, Y 7 , Y 8 ═SO 3 − ; 13, Y 7 , Y 8 ═SO 3 − ; X 7 ═OH; n=2)
Phosphorus oxychloride (37 ml, C.4 mole) was added dropwise with stirring to a cooled (−2° C.) mixture of dimethylformamide (DMF, C.5 mole, 40 mL) and dichloromethane (DCM, 40 mL), followed by the addition of acetone (5.8 g, 0.1 mole). The ice bath was removed and the solution refluxed for 3 hours. After cooling to room temperature, the product was either partitioned in water/DCM, separated and dried, or was purified by fractional distillation. Nuclear magnetic resonance and mass spectral analyses showed that the desired intermediate, 10 , was obtained. Reaction of the intermediate with 2 equivalents of 2,2,3-trimethyl-[H]-benz[e]indolesulfonate-N-propanoic acid and 2 equivalents of sodium acetate trihydrate in ethanol gave a blue-green solution after 1.5 hours at reflux. Further functionalization of the dye with bis(isopropylidene)acetal protected monosaccharide is effected by the method described in the literature (J. H. Flanagan, C. V. Owens, S. E. Romero, et al., Near infrared heavy-atom-modified fluorescent dyes for base-calling in DNA-sequencing application using temporal discrimination. Anal. Chem., 1998, 70(13), 2676-2684).
EXAMPLE 8
Synthesis of polyhydroxyindole sulfonate (FIG. 4 , Compound 16, Y 7 , Y 8 ═SO 3 − ; X 7 ═H; n=1)
Preparation of this compound was readily accomplished by the same procedure described in Example 6 using p-hydroxybenzenesulfonic acid in the place of the monosaccharide, and benzoindole instead of indole derivatives.
EXAMPLE 9
Synthesis of polyhydroxyindole sulfonate (FIG. 5 , Compound 20, Y 7 , Y 8 ═H; X 7 ═OH; n=1)
The hydroxyindole compound was readily prepared by a literature method (P. L. Southwick, J. G. Cairns, L. A. Ernst, and A. S. Waggoner, One pot Fischer synthesis of (2,3,3-trimethyl-3-H-indol-5-yl)-acetic acid derivatives as intermediates for fluorescent biolabels. Org. Prep. Proced. Int. Briefs, 1988, 20(3), 279-284). Reaction of p-carboxymethylphenylhydrazine hydrochloride (30 mmol, 1 equiv.) and 1,1-bis(hydroxymethyl)propanone (45 mmol, 1.5 equiv.) in acetic acid (50 mL) at room temperature for 30 minutes and at reflux for 1 hour gave (3,3-dihydroxymethyl2-methyl-3-H-indol-5-yl)-acetic acid as a solid residue.
The intermediate 2-chloro-1-formyl-3-hydroxymethylenecyclo-hexane was prepared as described in the literature (G. A. Reynolds and K. H. Drexhage, Stable heptamethine pyrylium dyes that absorb in the infrared. J. Org. Chem., 1977, 42(5), 885-888). Equal volumes (40 mL each) of dimethylformamide (DMF) and dichloromethane were mixed and the solution was cooled to −10° C. in acetone-dry ice bath. Under argon atmosphere, phosphorus oxychloride (40 mL) in dichloromethane was added dropwise to the cool DMF solution, followed by the addition of 10 g of cyclohexanone. The resulting solution was allowed to warm up to room temperature and heated at reflux for 6 hours. After cooling to room temperature, the mixture was poured into ice-cold water and stored at 4° C. for 12 hours. A yellow powder was obtained. Condensation of a portion of this cyclic dialdehyde (1 equivalent) with the indole intermediate (2 equivalents) was carried out as described in Example 5. Further, the functionalization of the dye with bis (isopropylidene)acetal protected monosaccharide was effected by the method described in the literature (J. H. Flanagan, C. V. Owens, S. E. Romero, et al., Near infrared heavy-atom-modified fluorescent dyes for base-calling in DNA-sequencing application using temporal discrimination. Anal. Chem., 1998, 70(13), 2676-2684).
EXAMPLE 10
Synthesis of polyhydroxylbenzoindole sulfonate (FIG. 6 , Compound 22, Y 7 , Y 8 ═H; X 7 ═OH; n=1)
A similar method described in Example 8 was used to prepare this compound by replacing the indole with benzoindole derivatives.
EXAMPLE 11
Synthesis of Rigid heteroatomic indole sulfonate (FIG. 7 , Compound 27, Y 7 , Y 8 , Y 7 ═H; n=1)
Starting with 3-oxo-4-cyclohexenone, this heteroatomic hydrophilic dye was readily prepared as described in Example 8.
EXAMPLE 12
Minimally Invasive Monitoring of the Blood Clearance Profile of the Dyes
A laser of appropriate wavelength for excitation of the dye chromophore was directed into one end of a fiber optic bundle and the other end was positioned a few millimeters from the ear of a rat. A second fiber optic bundle was also positioned near the same ear to detect the emitted fluorescent light, and the other end was directed into the optics and electronics for data collection. An interference filter (IF) in the collection optics train was used to select emitted fluorescent light of the appropriate wavelength for the dye chromophore.
Sprague-Dawley or Fischer 344 rats were anesthetized with urethane administered via intraperitoneal injection at a dose of 1.35 g/kg body weight. After the animals had achieved the desired plane of anesthesia, a 21 gauge butterfly with 12″ tubing was placed in the lateral tail vein of each animal and flushed with heparinized saline. The animals were placed onto a heating pad and kept warm throughout the entire study. The lobe of the left ear was affixed to a glass microscope slide to reduce movement and vibration.
Incident laser light delivered from the fiber optic was centered on the affixed ear. Data acquisition was then initiated, and a background reading of fluorescence was obtained prior to administration of the test agent. The compound was administered to the animal through a bolus injection in the lateral tail vein. The dose was typically 0.05 to 20 μmole/kg of body weight. The fluorescence signal rapidly increased to a peak value, then decayed as a function of time as the conjugate cleared from the bloodstream.
This procedure was repeated with several dye-peptide conjugates in normal and tumored rats. Representative profiles are shown in FIGS. 6-10 .
While the invention has been disclosed by reference to the details of preferred embodiments of the invention, it is to be understood that the disclosure is intended in an illustrative rather than in a limiting sense, as it is contemplated that modifications will readily occur to those skilled in the art, within the spirit of the invention and the scope of the appended claims. | Highly hydrophilic indole and benzoindole derivatives that absorb and fluoresce in the visible region of light are disclosed. These compounds are useful for physiological and organ function monitoring. Particularly, the molecules of the invention are useful for optical diagnosis of renal and cardiac diseases and for estimation of blood volume in vivo. | 2 |
BACKGROUND OF THE INVENTION
This invention relates to a furnace of the type having a combustion chamber for ignition of a fuel and air mixture and, in particular, to the means for controlling the discharge of the condensate and flue gas by-products of combustion.
Gas furnaces typically include a heat exchanger having a combustion chamber for combustion of a fuel and air mixture. The heat exchanger is designed to permit the passage of air over the combustion chamber. Often the heat exchanger includes a secondary heat exchanger to enhance the transfer of heat to a medium which is then directed to an enclosure for heating thereof.
Concomitantly with transfer of heat from the combustion products, the combustion products are cooled and liquid condensate will form during the heat extraction process particularly in the secondary heat exchanger. The condensate is typically collected and directed through a conduit from the heat exchanger to a drain. However, because the condensate may constitute an acid solution, it is common to direct the condensate products through an acid neutralizing media before it is passed into a drain.
Devices of this nature are disclosed particularly in Tomlinson et al, U.S. Pat. No. 4,543,892 entitled "Condensate Handling Means for Condensing Furnace". In Tomlinson et al, flue gas and condensate flow into a vertical tube. The flue gas products discharge upwardly through the vertical tube and the condensate products flow downwardly through the tube, through a trap at the bottom of the tube and then through a neutralizing media. In known embodiments of the device depicted in the Tomlinson et al patent, a styrofoam float is additionally provided within the vertical collection tube to block the flow of flue gas in the event the trap becomes somehow blocked. The float is buoyed by the condensate in such a circumstance to close the flue gas passage.
Other patents disclose similar furnaces and teach various ways to neutralize the collected condensate collected from the combustion products including Ketterer in U.S. Pat. No. 4,309,947 entitled "Mounting Arrangement for Condensate Neutralizer in a Furnace" and Tomlinson in U.S. Pat. No. 4,289,730 entitled "Furnace with Flue Gas Condensate Neutralizer". The concept of collecting condensate from a heat exchanger is also taught in Herbert U.S. Pat. No. 3,212,288 entitled "Heat Exchanger with Condensate Collector".
The various referenced prior art patents disclose highly useful and efficient means for collecting condensate and discharging flue gas from a hot air furnace and, in particular, a gas hot air furnace. However, there has remained a need to provide an improved trap assembly associated with such furnaces. That need inspired the development of the present invention.
SUMMARY OF THE INVENTION
Briefly the present invention comprises an improvement in a furnace of the type including a heat exchanger with a combustion chamber for ignition of a fuel and air mixture, means for introducing a fuel and air mixture to that chamber, means for igniting the fuel and air mixture, a combustion product plenum connected to the chamber for directing combustion products from the chamber to a flue gas exhaust passage, and a fluid drain conduit for draining combustion products (i.e. condensate) from the combustion chamber and the plenum. Specifically, the improvement is a trap assembly for the drain conduit which includes means cooperative with the exhaust passage to collect and pass the condensate to a drain while simultaneously being capable of terminating furnace operation if the condensate flow from the trap assembly becomes somehow blocked causing excessive condensate to accumulate.
The trap assembly includes a condensate inlet positioned near the bottom of a vertical tube closed at its lower end. Immediately above the condensate inlet is a condensate outlet which typically connects through a neutralization media to a drain. Positioned further above the condensate outlet is a flue gas inlet through the side of the tube. Finally, the tube extends vertically upward to define a flue gas outlet.
A float is positioned within the vertical tube and includes a specially constructed cap for forming a seal with the flue gas outlet when the float is raised a sufficient height to simultaneously block the flue gas inlet. The float rides upon the condensate collected within the tube and will only operate to terminate flue gas flow whenever the condensate outlet is blocked. Thus, only when condensate collects in a sufficient amount within the vertical tube will the flue gas inlet and outlet be blocked.
Sensing means within the plenum connected to the flue gas inlet is designed to detect a pressure change within the plenum when the flue gas inlet is blocked. When that pressure change is sensed, switch means operates to terminate the flow of the fuel and air mixture to the combustion chamber of the furnace.
Thus, it is an object of the present invention to provide an improved trap assembly for the combustion products from a furnace of the type which combusts a fuel and air mixture and releases a combination of condensate and flue gas products.
Yet a further object of the present invention is to provide an economical, easy to use, and efficient combustion product trap assembly for a fossil fuel furnace.
Yet a further object of the present invention is to provide an improved trap assembly for collecting and neutralizing condensate that passes through a first set of connected passages and for directing flow of flue gas through a second set of passages, all the passages being interconnected to control the flow of condensate as well as the flow of flue gas through the furnace.
Yet another object of the invention is to provide an improved a safe way for the collection of condensate from a heat exchanger.
Yet a further object is to provide a single, low cost trap assembly for a high efficiency furnace to collect the condensate and flue gas products in compliance with appropriate industry and government standards.
One further object of the invention is to provide a single assembly accomplishing the aforesaid objectives which is not dependent upon expensive electrical sensing devices and which is low cost, easy to maintain, easy to construct, and rugged.
These and other objects, advantages and features of the invention will be set forth in the detailed description which follows.
BRIEF DESCRIPTION OF THE DRAWING
In the detailed description which follows, reference will be made to the drawing comprised of the following figures:
FIG. 1 is a typical prior art device;
FIG. 2 is a perspective view of a typical high efficiency, forced air, gas furnace incorporating the improved trap assembly of the present invention;
FIG. 3 is a perspective view of the component part of the trap assembly incorporated in FIG. 2;
FIG. 4 is a cutaway perspective view of the trap assembly of FIG. 3 wherein the float, which rides on the condensate within the trap assembly, is in its lower or first position; and
FIG. 5 is a cutaway perspective view similar to FIG. 4 wherein the float has been transported to its second or flue gas blocking position in response to the rise of condensate within the vertical tube portion of the trap assembly.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, there is illustrated a prior art, high efficiency, condensing furnace generally depicted at 10. Flue gas and condensate flow from the furnace 10 through a discharge passage 12. Condensate, which is typically water mixed with various acid components, will then flow downward to the lower portion of a collection tube 14. Gas products, namely flue gas products, flow upwardly through an exhaust outlet 16 from the tube 14.
An outlet line 18 extends from the bottom of the tube 14 upwardly through an outlet connector 42 through the side of the tube 14 and down through a conduit 22. Condensate which flows through the outlet line 18 and conduit 22 flows through a neutralizing media 24 retained within a neutralizing device 26 and thence through an outlet tube 28 to a drain 30. In the event of condensate overflow through the tube 22, due to the fact that the device 26 is blocked, condensate will flow upwardly through a line 32 and through a T connection 34 to a bypass tube 36 which also connects to the drain 30. A vapor vent 38 connects to the T connection 34 to prevent blockage due to vapor or gas formation.
Within the prior art trap assembly as depicted in FIG. 1, a styrofoam float 40 may be positioned above the elbow 42 associated with the line 18. When condensate fills the tube 14, float 40 rises thereby partially blocking off the flue gas flow through the passages 12 and 16. However, condensate continues to flow from passage 12 over the float 40 filling the tube 14. So it is important to avoid totally blocking of the passage 12. The float 40 when serves to partially block off passage 12 may cause a back pressure which is sensed within the furnace 10 thereby operating a switching mechanism (not shown) to terminate operation of the furnace. Line 32 continues to act as a condensate bypass, though line 32 may be excluded since the device is supposed to terminate operation of the furnace.
However, the prior art device does not contemplate full termination of flue gas flow through the exhaust passage 12 or termination of condensate flow through the condensate passages of the device. As a result, the furnace may continue to operate, though undesirably.
FIGS. 2-5 disclose the trap assembly of the present invention which is designed to totally terminate flue gas flow and the operation of a furnace in the situation where a condensate neutralizer package or device becomes blocked. Thus, referring to FIG. 2, a high efficiency hot air furnace 50 includes a forced air fan 52 which delivers air to a heat exchanger assembly 54 for heating. The heated air then passes upward through the furnace 50, then through an outlet 56 from the furnace 50 to the enclosure being heated.
Within the heat exchanger 54, shown schematically in FIG. 2, a gas and air mixture is delivered by a gas burner tube assembly 58 for combustion within the heat exchanger 54. Controls 59, as known to those skilled in the art, provide the appropriate gas and air mixture to burner 58. The design and operation of the heat exchanger 54 as well as a secondary heat exchanger, in order to increase the efficiency of the furnace 50, is known to those skilled in the art.
For purposes of the invention, the combustion products from the burning of the fuel and air mixture are collected in a plenum 60. The flue gas portion of the combustion products passes from the plenum 60 through a flue gas tube or pipe 62. Liquid condensate collects at the bottom of the plenum 60 and passes through a conduit tube 64 or drain tube 64 to the improved trap assembly of the present invention; namely, the trap assembly 66. A pressure sensing tube 68 is connected to the flue gas passage 62 at one end and is connected at its opposite end to a pressure switch 70 that controls the input of ignitable materials to the burner 58. When the back pressure through the sensing tube 68 increases above a permissible limit, the pressure switch 70 senses this increased pressure thereby terminating the flow of combustible fuel to the furnace 50 and terminating operation of the furnace 50.
The trap assembly 66 is constructed so as to provide for initiation of the appropriate pressure sequence through the sensing tube 68 in the event the drain tube 64 or the condensate flow from the plenum 60 have become somehow blocked. Specifically, therefore, the remainder of the description will be directed to the construction of the trap assembly 66 and its component parts. Thus, as shown in FIGS. 2-5, the trap assembly 66 includes a vertical, generally cylindrical, hollow tube 72. The tube 72 is sealed at its lower end 73 by a cap construction 74.
The drain tube 64 leads through an inlet 76 into the lower end of the tube 72. A drain outlet 78 extends from the inside of the tube 72 and discharges vertically below the level of the inlet 76. Thus, condensate flow into the tube 72 will collect within the bottom of the tube 72 and, upon reaching an appropriate level, will flow outwardly through the outlet 78.
As shown in FIG. 2, the flow from the outlet 78 passes through discharge tubing 80, then through a neutralizing device 82 of a type known to those of skill in the art. A final drain tube 84 connects from the neutralizing device 82 into a drain 86.
The vertical tube 72 includes a right angle, uniform diameter, flue gas inlet 88 which connects from the passage 62 directly into the tube 72. The flue gas inlet 88 is positioned above the condensate outlet 78 approximately 12 inches in the circumstance where the diameter of the tube is approximately 2 inches. The distance of the flue gas inlet 88 above the condensate outlet 78 may be varied according to desire and need depending upon the internal diameter of the tube 72, the rate at which condensate is collected and flows through the trap, and the neutralizing device 82, as well as other empirical factors that will be developed upon building of such a trap assembly for a particular model furnace.
A flue gas outlet tube 90 constitutes a vertical upward extension of the tube 72 and normally connects with the flue gas inlet 88. During normal operation of the furnace, flue gas flows through the inlet 88 and directly through the outlet tube 90, thence to a chimney or other exhaust associated with the furnace 50. Simultaneously condensate flows through the drain tube 64 into the trap inlet 76 at the bottom of the tube 72 and through the outlet 78 to the neutralizing device 82.
A float 92 comprising an elongate cylindrical member is positioned to slidably move within the tube 72. The float 92 includes a cap member 94 having an external diameter slightly greater than the internal diameter of the tube 90 defining the outlet. In this manner (since tube 90 slips or fits within tube 72 and has a lesser diameter than tube 90) the cap 94 can form a seal against the bottom of tube 90. Thus, cap 94 has a generally cylindrical shape coincident with the internal shape of the tube 72 with a diameter slightly less than the diameter of tube 72.
Float 92 and cap 94 have a density less than that of the condensate. The float 92 is thus buoyed by the condensate which flows into the tube 72. When the condensate level increases sufficiently, the float 92 will move upwardly causing the generally cylindrical cap 94 to cooperate with the lower cylindrical flange or edge 91 of outlet tube 90 and block not only a part of the inlet passage 88, but seal the outlet tube 90. That is, the float or cap 94 has a generally cylindrical planar surface which forms as a seal against the lower face of the tubing defining the flue gas outlet 90.
The length of the skirt 96 of the cap 94 is such that when the cap 94 is in the fully raised position as it floats upwardly due to the level of condensate, there remains some clearance for passage of flue gas about the float 92. This will tend to pressurize the position of the cap 94 against the outlet 90 by acting on the lower surface or rim of skirt 96 thereby maintaining the seal of the cap 94 against tube 90. This also causes pressure within the line or passage 62 to increase dramatically and quickly thereby effectively and quickly causing a pressure signal to pass to the sensing tube 68 to be detected by the pressure switch 70. The mechanism provides a simple, yet quick and effective way for causing pressure to terminate flow of flue gas and to initiate the sequence of switching to terminate operation of the furnace.
The skirt 96 is also shaped to conform generally to the internal shape of the tube 72. This promotes vertical alignment of the float 92 in tube 72 as the float 92 is transported on the condensate.
It is possible, of course, to vary the shape and configuration of the cap 94 as well as the float 92 and the internal construction and cross section of the tube 72. Importantly, the relative position flue gas inlet 88, outlet tube 90 and the cooperative relationship between the cap 94 and outlet tube 90 are all very important to the invention. Note, for example, that relative to the prior art, gas venting or discharge from the condensate occurs in tube 72 rather than externally. Also, note the unique cooperative relationship and sizing of the cap 94 relative to the tube 72 and outlet tube 90. Also, the relationship of inlet 76 and outlet 78 can be reversed without rendering the invention ineffective. The device will operate in either configuration. The invention is therefore to be limited only by the following claims and their equivalents. | An improved trap assembly for a high efficiency fossil fuel furnace includes a vertical tube closed at its lower end with a condensate inlet immediately above the lower end and a condensate outlet above the inlet. A flue gas inlet is provided at the top end of the tube with a flue gas outlet immediately adjacent thereto. A float with a sealing cap is positioned within the tube and rises in response to the level of condensate to block the flue gas outlet. | 8 |
BACKGROUND OF THE INVENTION
This invention relates generally to the measurement of fluid flow. More particularly, the present invention is directed towards an in-line parallel proportionally partitioned by-pass metering device and method of measuring fluid flow within a closed conduit system.
Fluid flow measurement is widely practiced and fulfills an array of purposes including energy distribution, custody transfer, regulation, control and research. The measuring unit, i.e. "flowmeter", typically consists of a primary and a secondary device. The primary device is acted upon by the fluid directly, and the secondary device converts the primary device's response to the fluid into an observable quantity. Flowmeters are generally classified into those which measure quantity of fluid flow and those which measure rate.
Because of the wide practice of fluid flow measurement, engineers have a greater choice when specifying a flowmeter than for perhaps any other process measuring, monitoring device. Currently, there are over one hundred types of flowmeters available, and expenditures on flowmeters exceed one billion dollars per year. Thus in choosing a flowmeter, an engineer will typically evaluate: (1) the degree of accuracy and/or precision required, (2) the suitability of the flowmeter to the particular application and conditions, and (3) the cost of the various alternative flowmeters and other limitations such as space requirements, and the like.
The selection of a flowmeter requires an understanding of the flow behavior of fluids. First, a fluid is any matter which undergoes continuous deformation upon being subjected to shearing forces. Viscosity is that property of a fluid by which it offers resistance to deformation or shear. The response of a fluid subjected to shearing forces is "flow". The type of flow, whether laminar, turbulent, cavitational, or some combination, depends upon the fluid viscosity and other parameters of the fluid flow system. Second, a fluid in motion, i.e., flowing, possesses energy. This energy may be displacement or pressure energy, velocity or kinetic energy, potential energy, thermal or internal energy, or some combination of these forms of energy. Flowmeters utilize the energy of a fluid in motion to monitor fluid flow. Therefore, an engineer must also consider the type of flow and the energy of the fluid flow when selecting a flowmeter.
Flowmeters which measure quantity repeatedly measure a fixed volume of fluid. These flowmeters are generally of the reciprocating or rotating piston, nutating disk, or rotary vane type. A limited number of flowmeters are available to measure volume or quantity of fluid flow. There is more selection when choosing a flowmeter to measure rate of fluid flow. These flowmeters generally measure differential pressure, area, velocity, heat area, thermal, or other characteristics of the fluid flow from which the rate of flow may be determined. Examples of types of flowmeters which measure differential pressures include orifice, venturi, flow nozzle, and pitot tube devices. Flowmeters which measure velocity include cup, propeller and turbine type devices. Each of these devices are more or less suitable for a particular application based on conduit size, type of fluid, and required accuracy.
Traditionally, flowmeters have been of the "full bore" design; that is, the flowmeter is of the same size as the conduit in which the fluid is flowing. While this is economical for small conduit sizes, flowmeters for large conduit sizes, e.g., in excess of four inches in diameter, may cost thousands of dollars. Furthermore, the "full bore" flowmeter is typically situated directly in the main conduit line. Thus, when the meter requires service or other maintenance the fluid flow in the main conduit must be stopped which causes operational losses. Still further, "full bore" flowmeters, particularly those in large diameter conduit systems, are exposed to high stresses generated by the fluid flow and potential corrosion or erosion due to fluid exposure. Thus, these meters are typically constructed of heavy duty materials such as cast iron, aluminum, bronze or other similar metals. However, these materials may potentially leach harmful elements, such as lead from bronze, into the fluid flow. This undesirable effect is of particular concern in applications which monitor fluid flow for human or livestock consumption.
In response to the high cost and maintenance of large flowmeters, a class of flowmeters known as "insertion type" flowmeters have become commercially available. Insertion type flowmeters, suitable for applications involving the measurement of flow rate, infer an overall flow rate based on the measurement of fluid velocity at particular locations within the conduit. These types of meters are typically utilized in conjunction with larger conduit sizes (i.e., greater than six inches) and where repeatability, not accuracy, is the prime requirement. The accuracy of insertion type flowmeters is limited by a number of factors including accuracy of the primary and secondary meter elements, the position of the primary meter element when inserted into the fluid stream, the velocity profile of the fluid stream, and variation or uncertainty of the inside diameter of the conduit. A further source of inaccuracy with some types of insertion flowmeters is that they sample the fluid stream at a right angle to the fluid path thus causing an abrupt change in the fluid direction. This abrupt change in fluid direction can cause distortions of the fluid flow which further reduces accuracy. At best, a typical insertion type flowmeter will have an accuracy less than 95%. This compares adversely to a full bore type flowmeter which can have an accuracy exceeding 99%. Such a difference in accuracy can be quite significant. In an exemplary application where fluid flow averages 100 gallons per minute, at the end of one year the potential error in quantity of fluid measured by an insertion type flowmeter compared to a full bore type flowmeter may be over 2 million gallons.
An example of an insertion type flowmeter is described in U.S. Pat. Nos. 3,581,565 and 3,803,921 to Dieterich. The Dieterich device is a multi-port slidable flow measuring device of the differential pressure class. Specifically, it is a modified pitot tube device incorporating an interpolating tube for averaging fluid samples. In this arrangement the sampling tube is inserted across the fluid path thus sampling the fluid stream at a right angle. As discussed, sampling of the fluid at right angles to the fluid flow is undesirable as this causes an abrupt change in the fluid flow direction thereby causing distortions (such as eddy currents) of the fluid flow and reducing accuracy. The Dieterich device has been used for low flow gas measurements in stacks and flues where the sample is caused to route through a bypass prior to reentering the fluid stream. This bypass, as suggested, contains a costly auxiliary measuring sensor such as a hot wire anemometer device to monitor the gas flow.
The Dieterich device hence is distinguishable from the present invention in that it incorporates a multi-port tube inserted vertically across the fluid path, uses an auxiliary measuring device, is movable within the fluid path, and is adaptable mainly to conduit sizes in excess of three inches. Such a device further requires relatively high mechanical dexterity and know-how to install and operate and, as described, has an undesirably high cost associated with the flow measuring sensor.
It is another object of the present invention to provide an apparatus for measuring total fluid flow within a closed conduit system by a reduced size flowmeter. Accordingly, it is an object of the present invention to provide an apparatus for measuring total fluid flow within a closed conduit system with at least the same accuracy and reproducibility as a full bore flowmeter yet without the cost attendant therewith.
It is still another object of the present invention to provide a method of accurately measuring the rate or quantity of fluid flow within a closed conduit system by measuring the flow of a proportional amount of the fluid flow.
It is a further object of the present invention to provide an apparatus suitable for use with flowmeters constructed of alternative materials such as plastics, ceramics, and metal alloys.
It is still another object of the present invention to provide a fluid flow measuring device readily adaptable for use with most commercially available flowmeters.
SUMMARY OF THE INVENTION
The present invention provides a low cost, highly accurate apparatus incorporating a reduced sized flowmeter to measure the rate or quantity of a proportional amount of fluid flow within a closed conduit system in order to provide measurement of total fluid flow with essentially equivalent accuracy and reproducibility as full bore type flowmeters. In contrast to the Dieterich and other known devices, the present invention has a single port tube horizontally situated and essentially parallel to the fluid path, uses a fixed in-line flow measuring device, is permanent, and is adaptable to all conduit sizes. Once installed it requires no mechanical dexterity to operate and is very economical.
These and other advantages, objects and features of the present invention will become apparent to those skilled in the art by referring to the following written description and figures. The objects and advantages of the invention may be realized and attained by means of the instrumentalities and methods particularly pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic elevational drawing of an exemplary in-line parallel proportionally partitioned by-pass metering device of the present invention;
FIG. 2 is a side view of the metering device of schematic FIG. 1;
FIG. 3 is a schematic representation of an exemplary fluid flow profile within a conduit; and
FIG. 4 is a perspective view of a physical embodiment of the metering device of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention is directed to a device or apparatus for accurately and economically measuring the flow of fluid within a closed conduit. Shown in FIGS. 1 and 4 is a schematic diagram and physical representation of a metering device 10 of the present invention. The metering device 10 consists of a first inlet tube 12 of diameter D 2 having a first end 14 and a second end 16. First end 14 of inlet tube 12 is disposed within main conduit line 11 having diameter D 1 to extract in a non-disruptive manner a portion of the fluid flowing within main conduit 11. As shown in the Figures, the diameter D 2 of inlet tube 12 is substantially smaller than the diameter D 1 of main conduit 11. In order to remove the fluid sample from main conduit 11, inlet tube 12 passes through an aperture 32 formed in the wall of main conduit 11 and is suitably fixed and sealed to main conduit 11 by welding, brazing or other known techniques.
Metering device 10 further includes a reduced size flow meter 28 having an inlet connection 34 and an outlet connection 36. Second end 16 of inlet tube 12 is suitably connected to inlet connection 34 of reduced size flow meter 28 to deliver the extracted portion of fluid to the flowmeter. Reduced size flowmeter 28 is a "full bore" flow meter with a primary device sized to measure the proportional amount of fluid flowing through inlet tube 12 and a secondary device calibrated to display total fluid flow. In this configuration, reduced size flowmeter 28 will measure the proportional amount of fluid flow conducted through inlet tube 12 and display the total amount of fluid flowing through main conduit 11. In accordance with the teachings of the present invention, it is apparent that reduced size flowmeter 28 may be of the quantity or rate measuring type or any commercially available flowmeter.
As further shown in FIG. 1, metering device 10 includes an outlet tube 20 having a first end 24 and a second end 22. First end 24 of outlet tube 20 is suitably connected to the outlet connection 36 of reduced size flowmeter 28 to conduct the extracted fluid from reduced size flowmeter 28 after measurement and to return the extracted fluid to the main conduit line 11. Similar to inlet tube 12, outlet tube 20 passes through an aperture 38 formed in main conduit 11 downstream of aperture 32 and is suitably fixed and sealed to main conduit 11 at aperture 38. Second end 22 of outlet tube 20 is thereby disposed within main conduit 11 to discharge the extracted fluid flow back into the main fluid flow in a non-disruptive manner.
With continued reference to FIG. 1, diameter D 2 of inlet tube 12 is proportional to the diameter of main conduit diameter D 1 . In a preferred embodiment, the ratio of D 1 to D 2 is in a range of approximately two-to-one to fifty-to-one. In this way under normal flow conditions, a proportional flow of fluid will be extracted by inlet tube 12 and measured by reduced size flowmeter 28. In the present invention this proportional amount of fluid flow is defined by the ratio (K pat ). In an exemplary embodiment, a theoretical K pat may be calculated as the ratio of the cross-sectional area of the main conduit 11 having a diameter D 1 , to the cross-sectional area of the inlet tube 14 having a diameter D 2 . Therefore, the theoretical proportional flow parameter is defined by the following formula: ##EQU1## The total theoretical amount of fluid flow through main conduit 10 may be calculated as the measured amount of fluid flow through the reduced size flow meter 28 multiplied by theoretical K pat , the ratio of the area of main conduit 11 to the area of inlet tube 12.
It should be understood, however, that the definition of the theoretical proportional flow parameter K pat is dependant on the fluid flow characteristics and the inter-relationship of D 2 and the inlet aperture of the reduced size flowmeter. If the diameter of the inlet aperture of the reduced size flowmeter is less than D 2 , then its geometry will control in the theoretical K pat calculation and not D 2 . With reference to FIG. 3, there is shown a typical fluid flow profile within a pipe 42. The length of the flow lines 40, represent schematically the proportional amount of fluid flowing at any particular cross-sectional area of pipe 42. As shown in FIG. 3, the flow lines are longer at the center of pipe 42 and shorter near the walls which indicates that more fluid is flowing in the center of pipe 42 than at the outer walls. This is typical of flow within a pipe where friction along the pipe walls hinders fluid flow. If, as illustrated in FIG. 2, the central axis of inlet pipe 12 is co-linear with the central axis of main conduit 11, the proportional amount of fluid intercepted by inlet pipe 12 would not be equal to the ratio of the areas of the main conduit 11 to the inlet tube 12. In such an example, the theoretical K pat calculation would have to be adjusted accordingly as it is necessarily based on the particular flow characteristics of the fluid being measured.
Thus, the location of the inlet tube 12 within the main conduit 11 will affect the proportional amount of fluid extracted from main conduit 11. Accordingly, it may be advantageous to locate the inlet tube 12 within the main conduit 11 at various positions based on the distribution of fluid flow. In the case of non-uniform flow distributions, for example, the inlet pipe 12 may be located where the flow distribution is equal to the average flow for the entire main conduit 11. In such an example, the original definition of theoretical K pat as the ratio of main conduit area to inlet tube area is valid for calculating total fluid flow. Where the distribution of the fluid flow is unknown, general understanding of fluid flow dynamics suggests an inlet tube location in the lower portion of the conduit halfway between the center of the main conduit and the outer wall.
It should be understood from the foregoing discussion that in practice the actual K pat of the metering device will most likely be something different than the theoretical K pat of the metering device. It will therefore be necessary to calibrate the metering device to determine the actual K pat . This calibration should be made in accordance with standard practices for calibrating flowmeters (see e.g., American Water Works Association Standard ANSI/AWWA C700-90). It should be further understood that in practice, the secondary device for converting the primary device's response into an observable quantity would also be calibrated to display actual flow through the main conduit.
For example, with a metering device of the present invention wherein the main conduit diameter D 1 is 2 inches, the inlet metering tube diameter D 2 is 1/2 inch, and the bypass flow promotion barrier diameter D 3 is 11/2 inches (the purpose of the bypass flow promotion barrier to be discussed below), the foregoing formula suggests a theoretical K pat of 16 to 1. The results of actual experimentation with a metering device of the present invention having such dimensional parameters, however, suggests an observed K pat of approximately 12. The experimentation further demonstrated that the observed K pat varied less than 2% over flow ranges from 22 gallons per minute to over 150 gallons per minute, thus reiterating the accuracy of the metering device over a wide range of flow rates. In another series of actual trial runs of the metering device 10, the repeatability of the metering device was shown to vary less than 1/2 of 1% over repeated samples at the same flow rate. Such trial runs wherein the metering device was constructed of laboratory materials and no consideration was made for streamlining the fluid flow either through the main conduit or through the inlet tube suggests that production versions of the metering device will have even significantly higher accuracies.
As discussed above, one of the advantages of the metering device 10 of the present invention is in the proportionally smaller amount of fluid measured by the reduced size flowmeter compared to the total volume of fluid that flows through the main conduit 11. Previously, use of polymeric, ceramic or metal alloys in construction of flowmeters has been limited because of the inability of such flowmeters to survive the stresses and forces of the piping system. By measuring only a proportional amount of the flow, the stresses on the flowmeter components are greatly reduced thus making it possible to construct flowmeters from alternative materials. Further, since smaller flowmeters typically have longer service lives than larger flowmeters, metering device 10 will have a longer expected life, approximately equal to that of reduced size flowmeter 28, than the comparable full bore flowmeter that would conventionally be utilized for main conduit 11.
Referring again to FIG. 1, inlet tube 12 is shown to have an inlet section 15 which is substantially parallel to main conduit 11. Inlet section 15 is provided to ensure that the fluid flow distribution is not disturbed as fluid is extracted by inlet tube 12. In the preferred embodiment, inlet tube 12 is further designed to avoid abrupt disruptions of the flow within main conduit 11 as it moves around inlet tube 12 and as the extracted portion of fluid flowing within inlet tube 12 is conducted to the reduced size flowmeter 28. Similarly, outlet tube 20 is similarly designed with an outlet section that is substantially parallel to main conduit 11 to provide for non-disrupted fluid flow.
With reference to FIGS. 1 and 2, there is further shown a flow promotion barrier 30. Selective use of a flow promotion barrier reduces the sensitivity of the metering device 10 to air locks, pressure losses and other inherent resistance to flow present within all flow present all flowmeters and thus encourages the flow of the proportionally partitioned amount of fluid through the reduced sized flowmeter 28. Flow promotion barrier 30 is shown as a necked down or venturi section of the main conduit 11 having a beginning diameter approximately equal to the diameter D 1 of the main conduit 11. The diameter of the necked down section gradually decreases until it reaches a reduced diameter D 3 approximately mid-way through the necked down portion. In the preferred embodiment of metering device 10, the ratio of main conduit diameter D 1 to reduced diameter D 3 is in a range of approximately one-to-one (i.e. no reduction in diameter) to less than two-to-one.
Flow promotion barrier 30 is positioned between the first end 14 of inlet tube 12 and the second end 22 of outlet tube 20 and may be secured to the main conduit by welding, brazing, or other suitable fastening techniques, or may simply be formed as part of the main conduit structure. It will be appreciated by those skilled in the art, that the flow promotion barrier 30 should be suitably streamlined to avoid the causation of disruptions in the fluid flow. While the longitudinal length and "height" (i.e., ##EQU2## as shown in FIG. 1) of the flow promotion barrier 30 can vary, it is believed that the relationship between the two is optimized when the length is approximately 3 to 5 times the height. In this manner disruption in flow through main conduit 11 is minimized, which is a primary consideration in metering device 10. Furthermore, it is to be appreciated that multiple flow promotion barriers 30 may be utilized depending on the flow characteristics of the particular fluid being measured, space restrictions, and the like.
As shown in FIG. 1, metering device 10 still further includes an inlet shut-off valve 18 and an outlet shut-off valve 26. Optional shut-off valves 18 and 26 provide means for isolating reduced size flowmeter 28 from the main conduit fluid flow. Thus, reduced size flowmeter 28 may be serviced or replaced without stopping the fluid flow in main conduit 10.
The foregoing description of the invention has been provided for the purposes of illustration only, and it should be appreciated by those skilled in the art that modifications can be made without departing from the true spirit or fair scope of the present invention. The present invention will therefore be understood as susceptible to modification, alternation, and variation by those skilled in the art without deviating from the scope of the invention as defined by the following claims. | An apparatus and method are disclosed for accurately and economically measuring fluid flow within a closed conduit system. The apparatus includes a means for extracting a proportional amount of the fluid flow, a flowmeter reduced in size from the main conduit system for measuring the flow of the extracted proportional amount of fluid, and a means for returning the extracted portion of fluid to the fluid flow. The fluid flow is extracted and returned without disrupting the fluid flow. A means for promoting the extraction of the proportional amount of fluid flow is provided within said conduit between the means for extracting and returning the fluid flow. | 6 |
FIELD OF THE INVENTION
[0001] The invention relates to the use of yeast cells to incorporate biologically available phosphorus in a culture medium into their own biomass. These yeasts are useful in waste treatment, and can be obtained by growth in electromagnetic fields with specific frequencies and field strengths.
BACKGROUND OF THE INVENTION
[0002] Environmental pollution by urban sewage and industrial waste water has posed a serious health threat to living organisms in the world. Currently, the most common methods for large-scale waste treatment, such as water treatment, include the activated sludge technology and the biomembrane technology. These technologies rely on the innate abilities of myriad natural microorganisms, such as fungi, bacteria and protozoa, to degrade pollutants. However, the compositions of these natural microbial components are difficult to control, affecting the reproducibility and quality of water treatment. Moreover, pathogenic microbes existing in these activated sludge or biomembranes cannot be selectively inhibited, and such microbes usually enter the environment with the treated water, causing “secondary pollution.”
[0003] Further, most of the current technologies cannot degrade harmful chemicals such as pesticides, insecticides, and chemical fertilizers. These technologies also cannot alleviate eutrophication, another serious environmental problem around the world. Eutrophication is usually caused by sewage, industrial waste water, fertilizers and the like. It refers to waters (e.g., a lake or pond) rich in minerals and organic nutrients that promote a proliferation of plant life, especially algae, which reduces the dissolved oxygen content or otherwise deteriorates water quality. Eutrophication often results in the extinction of other organisms.
SUMMARY OF THE INVENTION
[0004] This invention is based on the discovery that certain yeast cells can be activated by electromagnetic fields of specific frequencies and field strengths to convert biologically available phosphorus, a major environmental pollutant, to intracellular phosphorus (i.e., incorporating biologically available phosphorus in their environs into their own biomass). Compositions comprising these activated yeast cells can therefore be used for waste treatment, for example, treatment of sewage, industrial waste water, surface water, drinking water, sediment, soil, garbage, and manure, to reduce the content of available phosphorus in the waste. Waste treatment methods using these compositions are more effective, efficient, and economical in preventing eutrophication than the conventional methods.
[0005] This invention embraces a composition comprising a plurality of yeast cells that have been cultured in an alternating electric field having a frequency in the range of about 80 MHz to 440 MHz (e.g., 86-120 or 410-430 MHz) and a field strength in the range of about 0.5 to 350 mV (e.g., 60-260 mV/cm). The yeast cells are cultured for a period of time sufficient to substantially increase the capability of said plurality of yeast cells to convert biologically available phosphorus in a culture medium into intracellular phosphorus. In one embodiment, the frequency and/or the field strength of the alternating electric field can be altered within the aforementioned ranges during said period of time. In other words, the yeast cells can be exposed to a series of electromagnetic fields. An exemplary period of time is about 12-400 hours, e.g., 228-368 hours.
[0006] Yeast cells that can be included in this composition are available from the China General Microbiological Culture Collection Center (“CGMCC”), a depository recognized under the Budapest Treaty (China Committee for Culture Collection of Microorganisms, Institute of Microbiology, Chinese Academy of Sciences, Haidian, P.O. Box 2714, Beijing, 100080, China). Useful yeast species include, but are not limited to, Saccharomyces cerevisiae and Saccharomyces carlsbergensis. For instance, the yeast cells can be of the strain Saccharomyces cerevisiae AS2.346, AS2.423, AS2.430, AS2.451, AS2.558, AS2.620, AS2.628, or IFFI1203; or Saccharomyces carlsbergensis AS2.189.
[0007] This invention further embraces a composition comprising a plurality of yeast cells, wherein said plurality of yeast cells have been activated such that they have a substantially increased capability to convert biologically available phosphorus in a culture medium into intracellular phosphorus as compared to unactivated yeast cells. Included in this invention are also methods of making these compositions.
[0008] As used herein, “biologically available” or “assimilable” phosphorus refers to phosphorus that is readily available, useable, or assimilable by living organisms for survival and/or growth. Exemplary biologically available or assimilable phosphorus includes, but is not limited to, PO 4 3+ , H 3 PO 4 , HPO 4 2+ , H 2 PO 4 + , other water-soluble inorganic phosphorus-containing compounds, and organic phosphorus-containing compounds.
[0009] A “substantial increase” means an increase of more than 10 (e.g., 10 2 , 10 3 , 10 4 , 10 5 , or 10 6 ) fold.
[0010] A “culture medium” refers to a medium used in a laboratory for selecting and growing a given yeast strain, or to liquid or solid waste in need of treatment.
[0011] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Exemplary methods and materials are described below, although methods and materials similar or equivalent to those described herein can also be used in the practice or testing of the present invention. All publications and other references mentioned herein are incorporated by reference in their entirety. In case of conflict, the present specification, including definitions, will control. The materials, methods, and examples are illustrative only and not intended to be limiting.
[0012] Other features and advantages of the invention will be apparent from he following detailed description, and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] [0013]FIG. 1 is a schematic diagram showing an exemplary apparatus for activating yeast cells using electromagnetic fields. 1 : yeast culture; 2 : container; 3 : power supply.
DETAILED DESCRIPTION OF THE INVENTION
[0014] This invention is based on the discovery that certain yeast strains can be activated by electromagnetic fields (“EMF”) having specific frequencies and field strengths to become highly efficient in converting biologically available phosphorus to intracellular phosphorus. Yeast cells having this function are defined herein as belonging to the same “functional group.” Compositions containing the activated yeast cells are useful in waste treatment.
[0015] Without being bound by any theory or mechanism, the inventor believes that EMFs activate or enhance the expression of a gene or a set of genes in yeast cells such that the yeast cells become active or more efficient in performing certain metabolic activities which lead to the desired phosphorus conversion result.
I. Yeast Strains Useful in the Invention
[0016] The types of yeasts useful in this invention include, but are not limited to, yeasts of the genera of Saccharomyces, Schizosaccharomyces, Sporobolomyces, Torulopsis, Trichosporon, Wickerhamia, Ashbya, Blastomyces, Candida, Citeromyces, Crebrothecium, Cryptococcus, Debaryomyces, Endomycopsis, Eremothecium, Geotrichum, Hansenula, Kloeckera, Lipomyces, Pichia, Rhodosporidium, and Rhodotorula.
[0017] Exemplary species within the above-listed genera include, but are not limited to, Saccharomyces cerevisiae, Saccharomyces bailii, Saccharomyces carlsbergensis, Saccharomyces chevalieri, Saccharomyces delbrueckli, Saccharomyces exiguus, Saccharomyces fermentati, Saccharomyces logos, Saccharomyces mellis, Saccharomyces microellipsoides, Saccharomyces oviformis, Saccharomyces rosei, Saccharomyces rouxii, Saccharomyces sake, Saccharomyces uvarum, Saccharomyces willianus, Saccharomyces sp., Saccharomyces ludwigii, Saccharomyces sinenses, Saccharomyces bailii, Saccharomyces carisbergensis, Schizosaccharomyces octosporus, Schizosaccharomyces pombe, Sporobolomyces roseus, Sporobolomyces salmonicolor, Torulopsis candida, Torulopsisfamta, Torulopsis globosa, Torulopsis inconspicua, Trichosporon behrendoo, Trichosporon capitatum, Trichosporon cutaneum, Wickerhamiafluoresens, Ashbya gossypii, Blastomyces dermatitidis, Candida albicans, Candida arborea, Candida guilliermondii, Candida krusei, Candida lambica, Candida lipolytica, Candida parakrusei, Candida parapsilosis, Candida pseudotropicalis, Candida pulcherrima, Candida robusta, Candida rugousa, Candida tropicalis, Candida utilis, Citeromyces matritensis, Crebrothecium ashbyii, Cryptococcus laurentii, Cryptococcus neoformans, Debaryomyces hansenii, Debaryomyces kloeckeri, Debaryomyces sp., Endomycopsis fibuligera, Eremothecium ashbyii, Geotrichum candidum, Geotrichum ludwigii, Geotrichum robustum, Geotrichum suaveolens, Hansenula anomala, Hansenula arabitolgens, Hansenula jadinii, Hansenula saturnus, Hansenula schneggii, Hansenula subpelliculosa, Kloeckera apiculata, Lipomyces starkeyi, Pichia farinosa, Pichia membranaefaciens, Rhodosporidium toruloides, Rhodotorula aurantiaca, Rhodotorula glutinis, Rhodotorula minuta, Rhodotorula rubar, and Rhodotorula sinesis.
[0018] Yeast strains useful for this invention can be obtained from laboratory cultures, or from publically accessible culture depositories, such as CGMCC and the American Type Culture Collection, 10801 University Boulevard, Manassas, Va. 20110-2209. Non-limiting examples of useful strains (with accession numbers of CGMCC) are Saccharomyces cerevisiae Hansen AS2.346, AS2.423, AS2.430, AS2.451, AS2.558, AS2.620, AS2.628, and IFFI1203; and Saccharomyces carlsbergensis AS2.189.
[0019] Although it is preferred, the preparation of the yeast compositions of this invention is not limited to starting with a pure strain of yeast. A yeast composition of the invention may be produced by culturing a mixture of yeast cells of different species or strains that have the same function, for example, converting biologically available phosphorus to intracellular phosphorus. The ability of any species or strain of yeast to perform this function can be readily tested by methods known in the art.
[0020] Certain yeast species that can be activated according to the present invention are known to be pathogenic to human and/or other living organisms. These yeast species include, for example, Ashbya gossypii, Blastomyces dermatitidis, Candida albicans, Candida parakrusei, Candida tropicalis, Citeromyces matritensis, Crebrothecium ashbyii, Cryptococcus laurentii, Cryptococcus neoformans, Debaryomyces hansenii, Debaryomyces kloeckeri, Debaryomyces sp., and Endomycopsis fibuligera. Under certain circumstances, it may be less preferable to use such pathogenic yeasts in this invention. If use of these species is necessary, caution should be exercised to minimize the leak of the yeast cells into the final treatment product that enters the environment.
II. Application of Electromagnetic Fields
[0021] An electromagnetic field useful in this invention can be generated and applied by various means well known in the art. For instance, the EMF can be generated by applying an alternating electric field or an oscillating magnetic field.
[0022] Alternating electric fields can be applied to cell cultures through electrodes in direct contact with the culture medium, or through electromagnetic induction. See, e.g., FIG. 1. Relatively high electric fields in the medium can be generated using a method in which the electrodes are in contact with the medium. Care must be taken to prevent electrolysis at the electrodes from introducing undesired ions into the culture and to prevent contact resistance, bubbles, or other features of electrolysis from dropping the field level below that intended. Electrodes should be matched to their environment, for example, using Ag—AgCl electrodes in solutions rich in chloride ions, and run at as low a voltage as possible. For general review, see Goodman et al., Effects of EMF on Molecules and Cells, International Review of Cytology, A Survey of Cell Biology, Vol. 158, Academic Press, 1995.
[0023] The EMFs useful in this invention can also be generated by applying an oscillating magnetic field. An oscillating magnetic field can be generated by oscillating electric currents going through Helmholtz coils. Such a magnetic field in turn induces an electric field.
[0024] The frequencies of EMFs useful in this invention range from about 5 to 5000 MHz, e.g., from 80 to 440 MHz (e.g., 86-120 MHz or 410-430 MHz). Exemplary frequencies are 86, 88, 90, 92, 94, 96, 98, 100, 102, 104, 106, 108, 110, 112, 114, 116, 118, 120, 410, 411, 412, 413, 414, 415, 416, 417, 418, 419, 420, 421, 422, 423, 424, 425, 426, 427, 428, 429, and 430 MHz. The field strength of the electric field useful in this invention ranges from about 0.5 to 350 mV/cm, e.g., from about 60 to 260 mV/cm. Exemplary field strengths are 68 and 240 mV/cm.
[0025] When a series of EMFs are applied to a yeast culture, the yeast culture can remain in the same container while the same set of EMF generator and emitters is used to change the frequency and/or field strength. The EMFs in the series can each have a different frequency or a different field strength; or a different frequency and a different field strength. Such frequencies and field strengths are preferably within the above-described ranges. In one embodiment, an EMF at the beginning of the series has a field strength identical to or lower than that of a subsequent EMF, such that the yeast cell culture is exposed to EMFs of progressively increasing field strength. Although any practical number of EMFs can be used in a series, it may be preferred that the yeast culture be exposed to a total of 2, 3, 4, 5, 6, 7, 8, 9 or 10 EMFs in a series.
[0026] By way of example, the yeast cells can be cultured in a first series of alternating electric fields each having a frequency in the range of 86 to 120 MHz and a field strength in the range of 60 to 260 mV/cm. The yeast cells are exposed to each EMF for about 24 hours. After culturing in the first series of EMFs, the resultant yeast cells are further incubated in a second series of alternating electric fields for a total of 24 to 132 hours. It may be preferred that the frequencies in the second series of alternating electric fields are identical to those of the first series in sequence and the field strengths in the second series are increased to a higher level within the range of 60 to 260 mV/cm.
[0027] Although the yeast cells can be activated after even a few hours of culturing in the presence of an EMF, it may be preferred that the activated yeast cells be allowed to multiply and grow in the presence of the EMF(s) for a total of 228-368 hours.
[0028] [0028]FIG. 1 illustrates an exemplary apparatus for generating alternating electric fields. An electric field of a desired frequency and intensity is generated by an AC source ( 3 ) capable of generating an alternating electric field, preferably in a sinusoidal wave form, in the frequency range of 5 to 5000 MHz. Signal generators capable of generating signals with a narrower frequency range can also be used. If desirable, a signal amplifier can also be used to increase the output. The alternating electric field can be applied to the culture by a variety of means including placing the yeast culture in close proximity to the signal emitters. In one embodiment, the electric field is applied by electrodes submerged in the culture ( 1 ). In this embodiment, one of the electrodes can be a metal plate placed on the bottom of the container ( 2 ), and the other electrode can comprise a plurality of electrode wires evenly distributed in the culture ( 1 ) so as to achieve even distribution of the electric field energy. The number of electrode wires used depends on the volume of the culture as well as the diameter of the wires. In a preferred embodiment, for a culture having a volume up to 5000 ml, one electrode wire having a diameter of 0.1 to 1.2 mm can be used for each 100 ml of culture. For a culture having a volume greater than 1000 L, one electrode wire having a diameter of 3 to 30 mm can be used for each 1000 L of culture.
III. Culture Media
[0029] Culture media useful in this invention contain sources of nutrients assimilable by yeast cells. In this invention, a culture medium refers to a laboratory culture medium, or liquid or solid waste in need of treatment. Complex carbon-containing substances in a suitable form, such as carbohydrates (e.g., sucrose, glucose, fructose, dextrose, maltose, xylose, cellulose, starches, etc.) and coal, can be the carbon sources for yeast cells. The exact quantity of the carbon sources utilized in the medium can be adjusted in accordance with the other ingredients of the medium. In general, the amount of carbohydrates varies between about 0.1% and 5% by weight of the medium and preferably between about 0.1% and 2%, and most preferably about 1%. These carbon sources can be used individually or in combination. Among the inorganic salts which can be added to the culture medium are the customary salts capable of yielding sodium, potassium, calcium, phosphate, sulfate, carbonate, and like ions. Non-limiting examples of nutrient inorganic salts are (NH 4 ) 2 HPO 4 , KH 2 PO 4 , CaCO 3 , MgSO 4 , NaCl, KNO 3 , and CaSO 4 .
IV. Electromagnetic Activation of Yeast Cells
[0030] Yeasts of this invention convert biologically available or assimilable phosphorus in a culture medium, such as waste water, into their own biomass, i.e., intracellular phosphorus. Biologically available phosphorus convertible by these yeasts includes, but is not limited to, PO 4 3+ , H 3 PO 4 , HPO 4 2+ , H 2 PO 4 + , other water-soluble inorganic phosphorus-containing compounds, and organic phosphorus-containing compounds. Biologically available phosphorus in waste water causes undesired eutrophication of water bodies in the world.
[0031] To activate the innate ability of yeast cells to convert biologically available phosphorus into intracellular phosphorus, these cells can be cultured in an appropriate medium under sterile conditions at 25° C.-30° C., e.g., 28° C., for a sufficient amount of time, e.g., 12-400 hours (for example, 228-368 hours) in an alternating electric field or a series of alternating electric fields as described above. An exemplary culture medium contains in per 1000 ml of sterile water: 10 g of sucrose, 3 g of (NH 4 )H 2 PO 4 (or other biologically available phosphorus), 1.2 g of NaCl, 0.2 g of MgSO 4 •7H 2 O, 3 g of CaCO 3 •5H 2 O, 0.3 g of CaSO 4 •2H 2 O, 0.3 g of KNO 3 , and 0.5 g of yeast extract. The culturing process may preferably be conducted under conditions in which the concentration of dissolved oxygen is between 0.025 to 0.8 mol/m 3 , preferably 0.4 mol/m 3 . The oxygen level can be controlled by, for example, stirring and/or bubbling.
[0032] Subsequently, the yeast cells can be measured for their ability to convert biologically available phosphorus to intracellular phosphorus using standard methods, such as using ultraviolet spectrophotometry or the chemical oxygen demand (“COD”) method. In an exemplary method, waste water from a phosphorus fertilizer manufacturer containing high levels of HPO 4 2+ , H 2 PO 4 + , and/or H 3 PO 4 is mixed with distilled water to achieve the following COD concentrations: (1) 100-1,000 mg/L; (2) 1,000-5,000 mg/L; (3) 5,000-10,000 mg/L; and (4) 10,000-50,000 mg/L. The solutions are then inoculated with a dry yeast cell preparation at a concentration of 0.2-0.6 g/L, and cultured for 24-48 hours at 10-40° C. The COD levels of the solutions are then measured using standard techniques. The difference between the COD levels before and after 24-48 hours indicates the phosphorus converting activity of the yeast cells. Another method for determining the phosphorus-converting abilities of the activated cells is described in the working example, infra.
[0033] Essentially the same protocol as described above can be used to grow activated yeast cells. To initiate the process, each 100 ml of culture medium is inoculated with yeast cells of the same functional group at a density of 10 2 -10 5 cells/ml, preferably 3×10 2 -10 4 cells/ml. The culturing process is carried out at about 20-40° C., preferably at about 25-28° C., for 48-96 hours. The process can be scaled up or down according to needs. For an industrial scale of production, seventy-five liters of a sterile culture medium are inoculated with the yeast cells. This culture medium consists of 10 L of the culture medium described above for this particular yeast functional group, 30 kg of starch, and 65 L of distilled water. At the end of the culturing process, the yeast cells may preferably reach a concentration of 2×10 10 cells/ml. The cells are recovered from the culture by various methods known in the art, and stored at about 15-20° C. The yeast should be dried within 24 hours and stored in powder form.
V. Acclimatization of Yeast Cells To Waste Environment
[0034] In yet another embodiment of the invention, the yeast cells may also be cultured under certain conditions so as to acclimatize the cells to a particular type of waste. This acclimatization process results in better growth and survival of the yeasts in a particular waste environment.
[0035] To achieve this, the yeast cells of a given functional group can be mixed with waste material from a particular source at 10 6 to 10 8 cells (e.g., 10 7 cells) per 1000 ml. The yeast cells are then exposed to an alternating electric field as described above. The strength of the electric field can be about 100 to 400 mV/cm (e.g., 120-250 mV/cm). The culture is incubated at temperatures that cycle between about 5° C. to about 45° C. at a 5° C. increment. For example, in a typical cycle, the temperature of the culture may start at 5° C. and be kept at this temperature for about 1-2 hours, then adjusted up to 10° C. and kept at this temperature for 1-2 hours, then adjusted to 15° C. and kept at this temperature for about 1-2 hours, and so on and so forth, until the temperature reaches 45° C. Then the temperature is brought down to 40° C. and kept at this temperature for about 1-2 hours, and then to 35° C. and kept at this temperature for about 1-2 hours, and so on and so forth, until the temperature returns to 5° C. The cycles are repeated for about 48-96 hours. The resulting yeast cells are then dried and stored at 0-4° C.
VI. Manufacture of the Waste Treatment Compositions
[0036] The yeast cells of this invention can be mixed with an appropriate filler, such as rock powder and coal ash at the following ratio: 600 L of yeast cell culture at 2×10 10 cells/ml and 760 kg of filler materials. The mixture is quickly dried at a temperature below 65° C. for 10 minutes in a dryer, and then further dried at a temperature below 70° C. for no more than 30 minutes so that the water content is less than 7%. The dried composition is then cooled to room temperature for packaging.
[0037] These dried yeast compositions may be used to treat polluted surface water, sewage, or any other type of waste water. To treat polluted surface water, a yeast solution may be prepared by adding 1 kg of the dried yeast composition to 30 L of clean water. The yeast solution is then sprayed onto the polluted surface water at about 1-3 L of the solution per square meter of the polluted surface water. To treat sewage or any other type of waste water, a yeast solution may be prepared by adding about 1 kg of the dried yeast composition to 10-30 L of clean water. The yeast solution is incubated at 10-35° C. for 24-48 hours. The resultant yeast solution is then added to the waste water at about 3-20 L of the solution per liter of waste water.
[0038] In order that this invention be more fully understood, the following example is set forth. This example is for the purpose of illustration only and is not to be construed as limiting the scope of the invention in any way.
VII. Example: Conversion of PO 4 3+ , HPO 4 2+ , H 2 PO 4 + , and/or H 3 PO 4 in a Culture Medium Into Intracellular Phosphorus
[0039] [0039] Saccharomyces cerevisiae Hansen AS2.620 cells were cultured in the presence of a series of alternating electric fields in the following sequence: the yeast cells were exposed to (1) an alternating electric field having a frequency of 98 MHz and a field strength of 68 mV/cm for 24 hours; (2) then to an alternating electric field having a frequency of 112 MHz and a field strength of 68 mV/cm for 24 hours; (3) then to an alternating electric field having a frequency of 108 MHz and a field strength of 68 mV/cm for 24 hours; (4) then to an alternating electric field having a frequency of 118 MHz and a field strength of 68 mV/cm for 24 hours; (5) then to an alternating electric field having a frequency of 98 MHz and a field strength of 240 mV/cm for 24 hours; (6) then to an alternating electric field having a frequency of 112 MHz and a field strength of 240 mV/cm for 24 hours; (7) then to an alternating electric field having a frequency of 108 MHz and a field strength of 240 mV/cm for 42 hours; and (8) finally to an alternating electric field having a frequency of 118 MHz and a field strength of 240 mV/cm for 42 hours.
[0040] To test the ability of the EMF-treated AS2.620 cells to convert biologically available phosphorus to intracellular phosphorus, waste water or filtrate from animal manure or garbage was supplemented with Na 3 PO 4 to reconstitute a solution containing Na 3 PO 4 at 200 mg/L. 0.1 ml of the EMF-treated AS2.620 cells at a concentration higher than 10 8 cells/ml was added to 100 L of the Na 3 PO 4 solution and cultured at 28° C. for 48 hours (solution A). One hundred liters of the Na 3 PO 4 solution containing the same number of non-treated yeast cells (solution B) or containing no yeast cells (solution C) were used as controls. After 48 hours of incubation, the solutions were examined using ultraviolet spectrophotometry. The results showed that after 48 hours of incubation, the Na 3 PO 4 concentration in solution A decreased more than 23% relative to solution C. In contrast, the Na 3 PO 4 concentration in solution B had no significant change relative to solution C.
[0041] While a number of embodiments of this invention have been set forth, it is apparent that the basic constructions may be altered to provide other embodiments which utilize the compositions and methods of this invention. | Compositions comprising a plurality of yeast cells, wherein said plurality of yeast cells have been cultured in the presence of an alternating electric field having a specific frequency and a specific field strength for a period of time sufficient to substantially increase the capability of said plurality of yeast cells to convert biologically available phosphorus in a culture medium into their own biomass. Also included are methods of making such compositions. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to cotton gins and in particular to an improved cotton gin roller bar.
2. Description of the Prior Art
The conventional cotton gin includes a series of circular saws arranged at relatively close spacings along a rotatable shaft, the saws operating between a series of gin bars spaced to provided minimum clearance for the saws and to permit passage of cotton fibers impaled on the saw teeth, and rejecting the seed as the lint fiber is detached therefrom. A limiting factor in the use of the gin bar and rotary saw blade combination is the excessive wear on the gin bar at the ginning point caused by the abrasive action of particulated material such as grit which clings to the cotton fibers. The resulting damage to the gin bar affects the quality of the cotton fibers by reducing their length.
Gin bar improvements are known wherein a freely rotatable roller disc is attached to the gin bar at the ginning point where fibers are pulled between adjacent gin bars by a rotary saw blade. The roller disc modification has greatly increased the output of the gin stand, while also improving the quality of the cotton by reducing fiber breakage and increasing the staple length.
The beneficial effect of the rotatable gin bar disc is provided by the rotational movement of the roller disc relative to the saw blade. The rolling action of the disc presents an ever-changing shear surface on which the seed and fiber can be pulled apart. The rolling movement of the disc also reduces the tensile forces acting on the cotton fibers, thereby reducing fiber breakage. It is important, therefore, that the roller disc turn freely as the cotton fiber is pulled by the rotatable saw.
The roller discs are press fitted into a sealed ball bearing assembly mounted on the gin bar. A factor which limits usage of the roller disc assembly is that grit, lint and other particulate material tends to accumulate between the inside face of the rotary disc and the stationary structure of the gin bar and the outer race of the annular roller bearing. The build-up of grit, lint and other particulate material restrains the free movement of the roller disc relative to the gin bar, thereby diminishing the beneficial effect of the roller disc. Further build-up of particulate material in the region between the roller disc and the gin bar will arrest movement of the roller disc and may cause seizure of the roller bearings.
OBJECTS OF THE INVENTION
It is, therefore, the principal object of the present invention to provide an improved gin bar having a rotatable seal interposed between the gin bar and a roller disc for preventing the build-up of grit and other particulate material in the interface region between the fixed gin bar and the rotatable roller disc.
A related object of the invention is to provide a rotatable grit seal for a cotton gin roller bar, operative parts of which can be interchangably incorporated into the gin bar and roller disc.
Yet another object of the invention is to provide an improved cotton gin roller bar for use in a conventional gin stand to insure maximum efficiency of a roller disc as it removes cotton fibers from seed while preventing the accumulation of particulate materials in critical regions between the roller disc and gin bar thereby assuring free rotation of the roller disc and providing for the efficient separation of fiber from the seed.
SUMMARY OF THE INVENTION
A cotton gin bar including a roller assembly comprising a pair of discs rotatably arranged on the upper portion of the bar at the ginning point, the discs being operative on opposing sides of the bar for detaching lint from the seed is disclosed. Each roller disc is provided with an annular rib and the gin bar is provided with an annular groove in which the rib is received, thereby defining a rotatable seal. The rotatable seal restricts the passage of small particles such as grit and lint which interfere with operation of the annular bearing on which the roller disc is mounted.
According to a preferred embodiment, the rotatable seal is enhanced by an annular bushing disposed in the interface region between the gin bar and the roller disc. The annular bushing is preferably constructed of a durable, pliant material such as nylon, and may be mounted either on the gin bar or on the roller disc. In the preferred arrangement, the annular bushing is disposed within the annular groove and is bonded onto the gin bar by an epoxy adhesive. The annular bushing is yieldable with respect to rotation of the roller disc, and serves as an effective barrier to the migration of particulate material into the critical interface region between the gin bar and the roller disc.
The novel features which characterize the invention are defined by the appended claims. The foregoing and other objects, advantages and features of the invention will hereinafter appear, and for purposes of illustration of the invention, but not of limitation, an exemplary embodiment of the invention is shown in the appended drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevation view showing the relative positions of a gin bar, rotary saw and doffing brush as utilized in a gin stand;
FIG. 2 is a sectional view of the gin bar and rotary saw taken to the lines II--II of FIG. 1;
FIG. 3 is an enlarged fragmentary view of the upper portion of the gin bar shown in FIG. 1;
FIG. 4A is a sectional view of a preferred embodiment of the gin bar and roller disc combination shown in FIG. 3, taken along the lines IV--IV;
FIG. 4B is a sectional view similar to FIG. 4A which illustrates an alternate embodiment;
FIG. 4C is an enlarged, partial sectional view taken along the lines IV--IV of FIG. 3;
FIG. 4D is an enlarged partial sectional view similar to FIG. 4C;
FIG. 5 is a perspective view of the roller discs shown in FIG. 2;
FIG. 6 is a sectional view of a roller disc;
FIG. 7 is a partial perspective view of a gin bar which reveals the annular roller bearing; and,
FIG. 8 is a view similar to FIG. 7 which includes roller discs rotatably mounted onto the gin bar.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the description which follows, like parts are marked throughout the specification and drawings with the same reference numerals, respectively. The drawings are not necessarily to scale and in some instances proportions have been exaggerated in order to more clearly depict certain features of the invention.
Referring now to FIG. 1, the invention is embodied in a gin roller bar assembly 10 which is mounted adjacent a rotary saw blade 12. The saw blade 12 is secured to a rotatable shaft 14 in a gin stand (not shown). The gin roller bar assembly 10 includes an elongated, curved gin bar 16, at each end of which are attaching pads 18, 20 for securing the gin bar to supporting members in the gin stand. In the gin stand, an array of the gin roller bar assemblies 10 are installed in side-by-side spaced relation, in interleaved relationship with the rotary saw blade 12, as illustrated in FIG. 2.
The ginning point, or the point in which the teeth of the saw 12 pass between adjacent gin bars, occurs near the upper end of gin bar at its outer face. Cotton fibers impaled upon the teeth of the saw 12 are separated from the seed at this point, and are drawn between the gin bars 16 and are wiped from the saw teeth by a doffing brush 22. The doffing brush 22 is mounted for rotation on a shaft 24 within the gin stand. The cotton fiber is thereafter dispatched by suitable means to a bailing press (not shown).
The body of the gin bar 16 is generally uniform in thickness, having a reduced thickness towards its lower end, as shown in FIG. 2, and has an enlarged width portion 22 near its upper end, the opposing faces of which are undercut, narrowing the thickness of the gin bar 16 outwardly toward its upper end, and defining a circular recess 24 on each side of the gin bar, as shown in FIGS. 1 and 7, to accomodate roller discs 26, 28 which are rotatably seated in each recess, respectively. Each recess 24 opens to the outer face of the gin bar to expose a portion of the periphery of the associated disc.
Referring now to FIGS. 5 and 7, each disc has an annular rib 30 concentrically formed on one face thereof. The face 32 of the recess 24 on the enlarged gin bar portion 22 is intersected by an annular groove 34 in which the annular rib 30 is received. The annular rib 30 is rotatable within the annular groove 34 thereby defining a rotary seal. The purpose of the rotary seal is to prevent particulate material such as grit from being accumulated in the interface region 36 (FIGS. 4A, 4B) between the fixed gin bar 16 and the rotatable discs 26, 28.
The roller discs 26, 28 are rotatably coupled to the gin bar 16 by an annular roller bearing assembly 38. The roller bearing assembly 38 includes an inner race 40, an outer race 42 and roller ball bearings 44 movably carried in the raceway defined by the inner and outer races. The enlarged portion 22 of the gin bar 16 is provided with a central bore 46 in which the annular bearing assembly 38 is secured by a press fit. The roller discs 26, 28 are likewise secured in a press fit against the inside bore of the inner race 40.
The roller discs 26, 28 are secured together within the inner race 40 by a threaded fastener 48. Each roller disc 26, 28 is provided with a press fit ring in the form of an annular boss 50 and annular boss 52, respectively, which are inserted into and received in binding engagement with the inner race 40. Each disc is provided with a small annular shoulder 51, 53, respectively, which bears against the opposite faces of the inner race 40 so that when they are brought together as shown in FIG. 4A and FIG. 4B, the interface clearance region 36 is established to permit the roller disc to rotate freely with respect to the gin bar 16.
The presence of the rotatable rib 30 within the annular groove 34 serves as a shield to prevent the migration of particulate material such as grit into the interface region 36.
According to one aspect of the invention, an improved rotary seal is provided by beveling the outer sidewall 54 of the annular rib 30 as illustrated in FIGS. 4A and 6. The beveled sidewall surface 54 in combination with the sidewall of the annular groove 34 defines a small annular chamber 56 which serves as a lint trap. It has been discovered during gin stand testing that an annular body of cotton fiber will accumulate in the lint trap chamber 56. This annular body of cotton lint serves as a yieldable barrier which prevents the migration of grit and other particulate material into the critical interface region 36.
Referring now to FIG. 4B, the relative positions of the annular rib 30 and annular groove 34 are reversible, with the annular rib 30 being formed on opposite faces of the stationary gin bar 16, and the annular groove 34 being formed on the rotatable discs 26, 28. The embodiment shown in FIG. 4B provides the same rotary sealing effect as the structure shown in FIG. 4A. In each configuration, the annular ribs and annular grooves are coaxially aligned with the axis 58 of the roller bearing assembly.
Referring now to FIGS. 4C and 4D, the rotatable seal is enhanced by an annular bushing 57 disposed in the interface region between the gin bar 16 and the roller discs 26, 28. The annular bushing 57 is preferably constructed of a durable, pliant material such as nylon, and is preferably embodied in a fibrous weave. The annular bushing 57 may be mounted either on the gin bar 16 or on the roller discs 26, 28. In the preferred embodiment, the annular bushing 57 is disposed within the annular groove 34 and is bonded onto the gin bar by an epoxy adhesive 59. The annular bushing is yieldable with respect to rotation of the roller disc, and serves as an effective barrier to the migration of particulate material into the critical interface region between the gin bar and the roller disc.
While the annular bushing 57 is bonded to a sidewall surface of the annular groove 34 as illustrated in FIGS. 4C and 4D, good service can be achieved with the bushing bonded onto a side surface of the annular rib 30 (not illustrated). The structure to which the bushing 57 is bonded is machined to the appropriate depth for receiving the bushing and bonding material and so that there will be positive, non-binding engagement between the annular rib 30 and the bushing 57.
Two preferred constructions for the roller discs 30 are illustrated in FIGS. 5 and 8. In FIG. 5, the roller discs 26, 28 are characterized by a circular, planar face 60 (FIG. 1) and a smooth edge in the form of a cylindrical sidewall 62 as can best be seen in FIGS. 5 and 6.
An alternate embodiment for the roller discs 26, 28 is illustrated in FIG. 8. In this embodiment, each roller disc 26, 28 is characterized by a circular, planar face 60 and a smooth, cylindrical sidewall edge 62, with the exterior face 60 of each disc being intersected by radially extending serrations 64 thereby defining alternating lands and grooves 64A, 64B which in combination form an undulating outer periphery on the disc face 60. This undulating border on the disc face 60 substantially reduces the degree of friction which occurs at the ginning point, thereby eliminating much of the wear on the roller disc which would ordinarily result when the lint is pulled between the ribs.
In operation, seed cotton is impaled on the teeth of the saw 12 from a roller box (not shown) and is carried upwardly, the fibers being detached from the seed at the point at which the teeth enter between the saw blade and the roller discs. As the cotton fiber is pulled across the roller disc 24, much of the particulate material including grit is separated from the lint and is dropped out of the path of the gin fibers. Entry of cotton lint, grit and other particulate material into the critical interface region 36 is limited by operation of the rotary seal provided by the annular rib 30 and annular groove 34.
Although preferred embodiments of the invention have been described in detail, it should be understood that various changes, substitutions and alterations can be made therein without departing from the spirit and scope of the invention as defined by the appended claims. | A cotton gin bar including a roller assembly comprising a pair of discs rotatably arranged on the upper portion of the bar at the ginning point, the discs being operative on opposing sides of the bar for detaching lint from the seed. Each roller disc is provided with an annular rib and the gin bar is provided with an annular groove in which the rib is received, thereby defining a rotatable seal. The rotatable seal restricts the passage of small particles such as grit and lint which interfere with operation of the annular bearing on which the roller disc is mounted. | 3 |
FIELD OF THE INVENTION
A durable pivot mechanism with bearing surface is described that provides for smooth planar travel perpendicular to the pivot axis. The absence of ball bearings, sealed joints, or the need for lubrication makes the pivot mechanism of the invention well suited for outdoor applications in inaccessible locations. The pivot mechanism of the invention is particularly well suited for use on utility poles.
BACKGROUND OF THE INVENTION
In certain situations, there is a need for a durable pivot connection that is able to withstand cyclic weather extremes with little or no maintenance yet provide a reliable pivot action after extended inaction. Additionally, the pivot connection must be able to move smoothly in a plane despite significant twisting and other nonplanar forces.
SUMMARY OF THE INVENTION
It is an object of the invention to provide a pivoting connection that is durable with little need for maintenance.
It is another object of the invention to provide a pivot mechanism that will move smoothly in a plane and will resist torsional and other forces outside the plane of travel.
In accordance with these and other objects of the invention that will become apparent from the description herein, a pivoting connection according to the invention includes:
a. a first connector member extending in a first plane and having a first end with a first pin opening transverse to said first plane and a second end with a first pair of projections spaced from a second pair of projections in substantially an H shape,
b. a second connector member having a first end with transverse pin openings for mating with the pin openings of the first connector member to receive a pin therethrough and pivotably secure said first connector member and said second connector member, and a second end for connection to a movable member that can displace in a second planar direction, and
c. a base member having first and second coplanar ends with an offset section therebetween, said offset section having an X-shaped opening therein made of two diagonal lengths and a second support surface therebetween for receiving one pair of said projection of the H-shaped end of said first connector member when inserted along a nonvertical position and retain said first connector member in a vertical position.
The pivoting connection of the invention provides a simple, durable pivoting connection for guidance in a plane of motion with little maintenance and high reliability. One leg of the H-shaped end of the connector member fits through the X-shaped opening in the base member along one leg of the X shape and is twisted to a vertical position to secure the H-shaped end within the base member. The first support surface of the H-shaped end of the connector member rests directly on and is supported by the second support surface of the base member in a low friction, metal point-to-point bearing relationship that is essentially immune to the adverse effects of weathering or rusting.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a top view of a pivoting connector secured to a support pole.
FIGS. 2A-4 show alternate embodiments of a pivoting connection to a movable control rod.
FIGS. 5-7 illustrate ranges of angular motion and lateral displacement for the pivoting connector of the invention as well as additional embodiments for connection to a movable control arm.
FIGS. 8-12 depict the connector member as formed with integral lateral walls and then as bent to final shape with various views thereof. shaped opening therein.
FIGS. 13-15 show details of the base member that can be mounted to a support structure with an X-shaped opening to receive and hold the H-shaped end of the connector member illustrated in FIGS. 8-10 and 12 .
DETAILED DESCRIPTION
The pivoting connection 1 of the invention is made with a first connector member 2 having an H-shaped end 3 dimensioned to fit into an X-shaped opening 4 in a base member 5 at a nonvertical insertion angle 6 and be secured therein at a vertical angle 7 , and a second connector member 8 pivotably connected to the other end of the first connector member 2 . The second connector member 8 is attached to a movable member 9 , such as a control linkage for operating a high voltage overhead power switch, that requires intermittent lateral movement without twisting outside the plane of motion. The base member 5 is secured to a support 11 , such as a utility pole 10 .
Alternate configurations for second connector member 8 are shown in FIGS. 2A-4, 6 and 7 . FIG. 3 shows the use of a pipe 30 with pin 20 passing through the entire diameter of pipe 30 to provide a rigid connection between pipes 33 , 34 . FIGS. 2A, 2 B, 2 C and 4 illustrate offset arms 31 , 32 secured within each end of pipes 33 , 34 with pin 20 passing through the opposite mated openings in each for a pivoting connection of pipes 33 , 34 that will allow angular movement within a common plane as well as lateral planar displacement. This offset arrangement can be used in connection with an external connection shown in side view in FIG. 6 . In this figure, each of the offset arms 31 , 32 is laterally displaced from the longitudinal displacement axis of control rods 33 , 34 but is secured to their respective rods by an external frictional or mechanical fit around each of rods 33 , 34 .
The first connector member 2 has one end pivotally supported by the base member 5 and the other end pivotally connected to a movable member 9 . The pivot axes of these ends are parallel and allow the first connector member 2 to move around each axis within a range of motion 12 in the displacement plane 13 of the movable member 9 . Such a motion is useful in many applications but particularly so in connection with high voltage interrupter switch assemblies of the type described in copending application Ser. No. 09/457,593, the disclosure of which is herein incorporated by reference. The distance 14 traversed by movable member 9 from a first position 15 to a second position 16 is intended to be adequate to open or close an electrical connection associated with the position of moveable arm member 17 .
The first connector member 2 extends longitudinally in a first plane and has a first end 18 with a transverse first pin opening 19 for establishing a pivotal connection with a second connector member 8 that is preferably secured to a moveable arm member 17 . Second connector member 8 allows movement within a plane but stabilizes moveable arm member 17 against transplanar motion.
If desired and the structure of the moveable arm member 17 permits, the first pin opening 19 of the first connector member 2 can be pivotally secured directly to the moveable arm member 17 by a pin 20 inserted through the first pin opening 19 and a transverse opening through the moveable arm member 17 . In such a direct connection embodiment, the moveable arm member 17 is equivalent in function to the second connector member 8 .
The H-shaped end 3 of the first connector member 2 is roughly in the form of the capital letter “H” with leading projections 37 and trailing projections 36 extending transverse to the longitudinal axis 22 of the first connector member 2 . Each pair of projections 36 , 37 is longitudinally separated by a flat distance 23 that will act as a pivotal support surface when first connector member 2 is inserted into an appropriately sized opening within base member 5 .
First connector member 2 and base member 5 may be made by molding, forging, and stamping and forming techniques of durable, weather resistant, workable material. As shown in FIGS. 11 and 12, first connector member is stamped as a blank unit 24 from formable material. Blank 24 is symmetrical about longitudinal axis with trailing projections 36 separated by a distance from leading projections 37 to form an “H”-shaped end. Along each side of blank 24 is an extended midsection 25 and a terminal end 26 with first pin opening 19 . Blank 24 is formed into first connector 2 by bending midsection 25 and terminal end 26 along parallel axes 27 , 28 into first connector 2 (FIG. 12 ).
The bending operations on blank 24 can occur by way of any forming technique. Examples include the use of a punch, die, or some combination of these so that midsection 25 and terminal end 26 are rotated roughly 90° relative to planar surface 29 . Preferably, the bottom 30 of planar surface 29 forms a plane 31 that passes through the center of first pin opening 19 . This orientation maximizes the leverage forces of and minimizes the shearing forces on first connector member 2 when pin 20 is connected to a movable arm member.
Base member 5 is shown in more details in FIGS. 13 and 14. As illustrated, base member 5 has first and second coplanar ends 40 , 41 with an intermediate support section 42 therebetween having an X-shaped opening 43 in support section 42 . Preferably, the coplanar ends 40 , 41 are used to secure the base member to the outer surface of a support member, such as a utility pole or wall, with bolts passing through bolt holes 44 , 45 . Angled edges 46 can rise from coplanar ends 40 , 41 at an obtuse angle 47 that is adequate to apply continuous force on any bolts used to secure base member 5 to a support. Angled edges 46 are also intended to pierce into the mounting surface to maintain stability against twisting as well as dimensional shrinkage in the support surface.
Generally, support surface 42 is elevated relative to coplanar ends 40 , 41 to provide clearance for the lead pair of projections 37 on first connector 2 . If the support surface is cut or shaped to provide clearance under the base member 5 beneath the X-shaped opening 43 , the support section 42 may lie on the same or substantially the same plane as the coplanar ends 40 , 41 of the base member 5 .
The X-shaped opening 43 is shaped and dimensioned to allow insertion of the lead projections 37 when inserted along angle 47 but retain the first connector member when twisted to a vertical position 48 . Preferably, angle 47 is within the range from about 5° to about 180° relative to vertical position 48 . The length 52 of opening 43 along angle 47 will correspond to the length 53 of lead projections 37 .
Flat bearing support surfaces 49 , 50 are formed into opening 43 along the top and bottom between each leg of the X-shape. The vertical height 51 between bearing surfaces 49 , 50 corresponds to the vertical height 54 of the flat space between lead projection 37 and trailing projections 36 on the first connector member 2 . | A pivoting connection is described that uses an H-shaped connector secured within the X-shaped opening of a base. One end of the H shaped connector can be inserted into the X-shaped opening at an angle corresponding to one leg of the X but is secured in the opening when twisted to a vertical position. This pivoting connection provides a reliable connection that is durable, weather resistant, and does not readily seize. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method and device for forming reinforcement elements composed of resistant fibers distributed along three dimensions. It also relates to the composite pieces obtained from said reinforcement elements after impregnation thereof with a hardenable binder, such as a synthetic resin.
2. Description of the Prior Art
From the American patents U.S. Pat. No. 2,283,802 and U.S. Pat. No. 3,322,868 a method is already known for example for forming composite elements from fibers distributed along three dimensions. In these known techniques, a substrate is formed from such fibers crossed in at least two directions, then the fibers of said substrate are bound together by stitching, by introducing a continuous fiber in said substrate using a needle driven with a reciprocal movement, whereas a relative movement of said needle with respect to said substrate occurs, so that said continuous fiber forms a zig-zag stitching line inside said substrate.
The use of such techniques raises no difficulty, when the two faces of the substrate are free, for then said needle may penetrate into said substrate by one of the faces and leave through the opposite face. On the other hand, when said substrate rest on a support, it is necessary to treat said support with special care.
For example, in the American patent U.S. Pat. No. 4,080,915 in which said support is rigid, openings are formed therein for allowing the end of the needle to penetrate therein without breaking. It will be noted that such a solution greatly limits the possibilities of stitching, since the number of openings formed in the support is necessarily limited and that it is imperative, for each stitch, for said needle to be opposite such an opening. Thus, in this prior patent, the openings are formed of elongate slits and the stitching lines are rectilinear, in correspondence with said slits. It can then be seen that not only the density of the stitches on the substrate must necessarily be low, but in addition, the form of the stitching lines and the distribution of the stitches are imposed once and for all by said openings.
On the other hand, in the American patent U.S. Pat. No. 4,863,660, the support is formed from a foam material or similar, allowing penetration of the point of a needle. In this case, there is no longer a limit imposed on the density of the stitches or the form of the stitching lines, but it is necessary to make the support from an easily destructible material, so as to be able to release the substrate from said support.
SUMMARY OF THE INVENTION
The object of the present invention is to overcome these drawbacks and make it possible to stitch a fiber substrate resting on a suppport without limiting the density of the stitches or the form of the stitching lines and without particular treatment of said support.
To this end, in accordance with the invention, the method for forming reinforcement elements form resistant fibers distributed along three dimensions, wherein, in a substrate resting on a support formed of such fibers crossed in at least two directions, a continuous fiber is introduced by stitching, from the free face of said substrate opposite said support by means of a needle driven with a reciprocal movement, a relative movement being in addition generated between said support and said needle so that said continuous fiber is formed inside said substrate of a succession of consecutive segments forming a zig-zag stitching line, is remarkable in that said needle is curved and imposes on each segment of said continuous fiber a similar curved form and in that the reciprocal movement of said curved needle occurs while rotating about an axis perpendicular to the plane of said needle and disposed on the concave side thereof. Preferably, said curved needle has a circular shape and said axis of rotation is coaxial with said needle.
Thus, with the invention, it is possible to cause said curved needle during its reciprocal movement, at the maximum, to come tangential to said support on which said substrate rests. Said curved needle does not then have to penetrate into said support to perform its stitching operation so that said support does not have to be specially treated for this purpose. The result is then in addition, that said needle may follow any desired path, as well as executing any desired density and distribution of stitches.
For example, during its reciprocal movement, said curved needle may come tangential to the face of said support on which said substrate rests. On the other hand, said curved needles may remain away from said support on which said substrate rests.
In addition, at the end of the outgoing stroke and at the beginning of the return stroke of said curved needle, the point thereof may project with respect to said free face of said substrate or else this point may be pricked inside said substrate.
Furthermore, the relative movement between said support and said needle may be rectilinear or curved. This relative movement between said support and said needle may be parallel to the plane of said needle. It may also be perpendicular to the plane of said needle.
In addition, the relative movement between said support and said needle may be inclined by an angle different from 90° with respect to the plane of said needle.
Generally, the relative movement between said support and said needle takes place so that the axis of rotatioin of said needle remains at a constant distance from said support. However, during the relative movement between said support and said needle, the axis of rotation of said needle may move away from or towards said support, for example to extract from said needle the amount of fiber required for forming a stitch.
The present invention also relates to a device for implementing the method.
For this, the device for forming reinforcement elements formed of resistant fibers distributed along three dimensions, which device comprises:
a support on which a substrate rests formed of such fibers crossed in at least two directions;
a needle capable of introducing a continuous fiber into said substrate, from the free face thereof opposite said support;
means for driving said needle with a reciprocal movement; and
means for generating a relative movement of said support with respect to said needle, is remarkable in that:
said needle is curved and guides said continuous fiber inside said substrate; and
means are provided so that the needle is driven in reciprocal rotation about an axis perpendicular to the plane of said needle and disposed on a concave side thereof.
Said curved needle may comprise, for guiding said fiber, an internal channel opening, in the vicinity of the point of said needle, through a lateral eye. Preferably, said lateral eye is located in the concavity of said needle.
In a variant, said curved needle may comprise a thread guide groove along its convexity and a lateral eye in its concavity close to its point, said eye being in communication with said groove via a passage.
Said curved needle may also comprise, close to its point, a hook turned towards its concavity and which may be closed by a latch. Said latch may be controlled by a device or be controlled automatically by said fiber and by said substrate.
Advantageously, said needle is mounted in a needle-holder which is articulated, about said axis of rotation of the needle, on an arm which is moveable with respect to said support. Preferably, a controllable thread clamp is mounted on said needle holder and said arm carries a reserve of fiber for said needle.
If necessary, said arm has in addition a mechanism for drawing the fiber when the needle exits between each stitch. Said arm may also carry a mechanism to form a loop when the point of said needle, after penetrating into said substrate, leaves again through the free side thereof.
Preferably, said arm is fixed to a machine capable of moving it with respect to the support. Such a support may be fixed; on the contrary, it may be formed by a rotary mandrel.
Thus, with the invention, a reinforcement element is obtained formed of resistant fibers distributed in three dimensions, said reinforcement element comprising a substrate formed of such fibers crossed in at least two directions and being remarkable in that it comprises curved fiber segments disposed in the thickness of said substrate.
From this reinforcement element, a composite piece may be produced by impregnating said element with a hardenable binder. The part thus obtained may as required be machined, at least on the surface, so as to obtain a final part.
BRIEF DESCRIPTION OF THE DRAWINGS
The figures of the accompanying drawings will better show how the invention may be put into practice. In these figures, identical references designate similar elements.
FIG. 1 is a schematic and partial perspective view illustrating the stitching method and device according to the invention, using a curved hollow needle through which the stitching fiber passes.
FIG. 2 is a section, through its median plane, of the hollow needle of FIG. 1.
FIGS. 3a1, 3b1, 3c1 and 3d1 are diagrams illustrating different ways of implementing the method of the present invention.
FIGS. 3a2, 3b2, 3c2 and 3d2 are diagrams illustrating other ways of implementing the method according to the invention
FIG. 4 shows, in a view similar to that of FIG. 1, a variant of the needle used in the method according to the invention.
FIG. 5 is a section, through its median plane, of the needle of FIG. 4.
FIG. 6 is a cross section of the needle of FIG. 4. through line VI--VI of FIG. 5.
FIGS. 7 and 8 show, in views similar to FIGS. 1 and 4, other variants of the needle used in the method according to the invention.
FIG. 9 shows, in a schematic and partial view, one embodiment of the device according to the invention.
FIGS. 10 and 11 illustrate two ways of implementing the method according to the invention.
FIGS. 12a to 12f illustrate several steps of another way of implementing the method according to the invention.
FIG. 13 and 14 show, in elevation, in two perpendicular directions and in partial section, a device according to the invention in the form of a stitching head.
FIG. 15 shows in perspective a stitching machine incorporating the head of FIGS. 13 and 14.
FIG. 16 illustrates the formation of a final composite part, by machining an undressed piece obtained by impregnating a reinforcement element formed in accordance with the invention with a hardenable binder.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In FIG. 1, a support 1 has been shown on which rests a substrate 2 formed of resistant fibers, as well as a stitching needle 3.1 for introducing a fiber 4 inside said substrate 2.
Support 1 may be made from any desirable material, such as metal and may possible be covered with a coating (not shown) for example of polytetrafluoroethylene. It may however also be made from a foam material, as is known in the techinque. Depending on the form of the reinforcement element to be obtained, it may be formed by a simple plate (which is shown is FIG. 1) or else by a mandrel hving a form of revolution and intended to be driven in rotation during the stitching operation (FIG. 15).
The resistant fiber substrate 2 may be of the two dimensional type, formed of fibers crossed in at least two directions. In this case, fiber 4 is intended to form the third dimension of this substrate. However, substrate 2 may also be of the three dimensional type and then fiber 4 is intended to form a reinforcement of the third dimension. Substrate 2 may be formed on support 1 or be formed elsewhere and brought to said support for there undergoing the curved stitching operations.
The resistant fibers forming substrate 2 and fiber 4 may be of different known kinds, such as glass, carbon boron, KEVLAR (registered trademark), etc. . .
As can also be seen in FIG. 2, needle 3.1 has a circular shape with center 5. It is hollow and has therethrough an internal channel 6 opening through a lateral eye 7, adjacent the point 8 of said needle and disposed in the concavity thereof. On the side opposite point 8, the internal channel 6 opens through an orifice 9. The fiber 4 is intended to pass through the internal channel 6, entering through orifice 9 and leaving through the lateral eye 7. In order to prevent damage and possibly breakage of the fiber 4 by rubbing against the walls of orifice 9 and the lateral eye 7, the internal channel 6 comprises a rounded widened portion 10 at said orifice 9, whereas an internal rounded bead 11 is provided on the edge of eye 7, opposite point 8.
The end of needle 3.1, opposite point 8, is fixed in a needle-holder 12, capable of being driven (see the double arrow F) with a reciprocal rotational movement about an axis 13--13 passing through the center 5 of needle 3.1 and at least substantially perpendicular to the plane thereof. Furthermore, a relative movement is generated between the support 1 and substrate 2 assembly, on the one hand, and needle 3.1, on the other.
If, as is shown in FIG. 1, this relative movement takes place in a direction f1 parallel to axis 13--13, it can be readily understood (possibly with the help of the complementary information given hereafter) that, on each outgoing stroke of needle 3.1 (clockwise rotation in FIG. 1), this needle introduces into substrate 2 a curved segment 4a of fiber 4 and that, at each of its return strokes (anti-clockwise rotation in FIG. 1), said needle 3.1 introduces into substrate 2 a curved segment 4b of said fiber 4, the segment 4b of a pair of segments 4a, 4b being connected to segment 4a of the following pair of segments 4a4b by a bridge 4c, parallel to axis 13--13, which is formed during the relative movement f1, whereas, on the side opposite bridges 4c, the two segments 4a and 4b of the same pair are joined together by a loop 4d.
In addition, depending on the radius of curvature of needle 3.1, and the height H of axis 13--13 above substrate 2 and on the thickness E of said substrate, numerous stitching configurations may be obtained. Some of them have been shown in FIGS. 3a1, 3b1 and 3c1, which correspond to schematic views along line III--III of FIG. 1 and on which, for the sake of clarity, the segments 4a and 4b have been showwn offset in the direction of the thickness of substrate 2.
For example, in FIG. 3a1, a stitching configuration has been shown in which the segments 4a and 4b are tangential to the face 1a of support 1 on which substrate 2 rests and loops 4d appear externally of the free face 2a of said substrate, through which needle 3.1 penetrates. Such a stitching configuration is advantageous when a support 1 is used in which needle 3.1 could not penetrate (metal support for example) and when it is desirable for segments 4a and 4b to form a reinforcement over the whole thickness of said substrate 2.
It goes however without saying that if support 1 were made from a material easily penetrated by needle 3.1, segments 4a and 4b could pass through at least the surface layer of said support. This is particularly advantageous when support 1 is made from a material which, in addition, is destructible after the reinforcement element has been produced.
In the example of FIG. 3b, loops 4d are also outside substrate 2, on the same side as the free face 2a thereof, but segments 4a and 4b do not penetrate into said substrate 2 as far as the face 1a of support 1. In this case, segments 4a and 4b may form a surface reinforcement of substrate 2.
On the other hand, in the example of 3c1, loops 4d are formed inside substrate 2, for example at the level of the free face 1a of support 1, and are held in position by the pressure and friction exerted by the material of substrate 2. In FIG. 3d1, a first stitching operation is assumed to have taken place, similar to that of FIG. 3c1, then a second similar operation, symmetrical with the first one with respect to the plane passing through the axis 13--13 and orthogonal to support 1.
Instead of providing between support 1 and needle 3.1, as described above, a relative movement f1 parallel to axis 13--13, in FIGS. 3a2 to 3d2, a rectilinear movement has been illustrated parallel to a direction f2 perpendicular to said axis 13--13. This stitching method will moreover be described in detail, by way of example, with reference to FIGS. 10, 11 and 12a to 12f.
To each of the FIGS. 3a2 to 3d2 there correspond FIGS. 3a1 to 3d1, with identical index a, b, c, d. In this case, the bridges 4c, instead of being perpendicular to the plane of the drawinges as in FIGS. 3a1 to 3d1 (the pairs of adjacent segments 4a and 4b being thus superimposed), are on the contrary parallel to the plane of FIGS. 3a2 to 3d2, so that they are visible thereon and several pairs of consecutive segments 4a and 4b are also visible.
Of course, the relative movement of needle 3.1 with respect to support 1 does not necessarily take place in one of the directions f1 or f2. Such a relative movement could take place in any other direction, for example at 45° with respect to f1 and f2. In addition, it will be understood that this relative movement is not necessarily linear and that it may follow a curved path, such as circular, helical, spiralled, etc. . . or else a combination of such paths.
In FIGS. 4, 5 and 6 a first variant 3.2 of needle 3.1 has been shown. Needle 3.2 is also circular, with center 5. However, instead of being hollow it is solid and comprises a thread guide groove 14 along its convexity. On the same side as its point 8 it has an eye 15 turned towards its concavity and in comunication through a passage 16 with said groove 14. It will be readily understood that needle 3.2 operates in a similar way to needle 3.1, fiber 4 being guided by groove 14 and through eye 15 (see FIG. 4) instead of being guided by the internal channel 6.
The second variant 3.3 of needle 3.1 shown in FIG. 7 is circular with center 5. On the same side as its point 8, it comprises a hook 17 turned towards its concavity and closable by a latch formed by the end of a circular rod 18 which may slide inside a channel 19 provided in said needle, under the action of a translation control device 20. Needle 3.3 operates in a way somewhat different from that of needle 3.1 and needle 3.2. With the latch of needle 3.3 closed, said needle is caused to pass through substrate 2 during its outgoing movement, and to leave again through the free face thereof. The latch opens and hook 17 grips the fiber 4, brought by an auxiliary device 21, after which said latch closes again and needle 3.3 pulls fiber 4 through said substrate during its return movement, thus forming simultaneously the segments 4a and 4b of a pair of segments, said fiber being gripped by hook 17 at the level of a loop 4d. When leaving surface 2a, needle 3.3 causes said loop 4d to project, after which a new cycle may begin again. Thus, a loop being formed is passed through the previously formed loop, so that loops 4d are joined together by a chain stitch. It will be noted that needle 3.3 requires the free face 2a of substrate 2 to be traversed at the end of the outgoing movement of said needle, so that it cannot provide stitching configurations as illustrated in FIGS. 3c1, 3d1, 3c2 and 3d2.
In the third variant 3.4 of needle 3.1, shown in FIG. 8, we have a latch needle operating similarly to needle 3.3. However, in this case, latch 22 is rotary and automatic, opening in the outgoing movements of the needle under the thrust of loop 4d which has just been formed, and being partially housed in housing 23 provided in the concavity of said needle. On the return stroke, the latch is swung into a closed position of hook 17 under the pressure of the material of substrate 2.
In FIG. 9, the device of FIG. 1 has been shown in a front view, completing it. In this FIG. 9, an arm 30 has been shown which is fixed to displacement means not shown of a machine so as to be able to move with respect to support 1 and which has, at its end directed opposite said support 1, the needle-holder 12 mounted for pivoting about an axis 13--13 by an ariculation 31. In addition, a thread clamp 32 is mounted on the needle-holder 12, on the same side as orifice 9 of needle 3.1, opposite point 8. For example, this thread clamp has a fixed part 32a and a movable part 32b, which is controllable away from or towards said part 32a, i.e. the fiber 4 which passes between the fixed and movable parts 32a and 32b may be free to pass therebetween or on the contrary be nipped therebeteen.
FIG. 10 illustrates one operating mode of the device of FIG. 9, mainly used for substrates 2 of small thickness. In this operation mode, at the end of the preceding stitch, with the thread clamp 32 open, needle 3.1 undergoes a return rotation about axis 13--13 of an amplitude A sufficient for the length 33 of fiber 4 leaving the needle and situated between eye 7 and substrate 2 to correspond to the sum of the lengths of bridge 4c, the curved segment 4a and loop 4d. After closing the thread clamp 32, bridge 4c and the curved segment 4a may then be formed by causing needle 3.1 to rotate about its axis 13--13, from this return position, in the direction of substrate 2. When needle 3.1 has arrived at the end of its stitching stroke, the thread clamp 32 is opened before the needles begins its return travel. Thus, during the return travel of needle 3.1, the curved segment 4b is formed, for example because of the friction which substrate 2 exerts on fiber 4. As will be seen herefter, it would of course be possible, in the case where such friction is not sufficient, to use a member for retaining loop 4d.
In the operating mode variant illustrated in FIG. 11, arm 30 is moved orthogonally to support 1. Axis 13--13 may be brought from a first position 13.1 close to support 1 to a position 13.2 away from support 1 then to a second close up position 13.3. Thus, in this movement of axis 13--13 towards and away from substrate 2, associated with the return stroke of needle 3.1 about said axis 13--13, it is possible to obtain an amplitude of movement B sufficient to release from said needle, with the thread clamp 32 open, a length 34 of fiber 4 corresponding to the sum of the lengths of bridge 4c, segment 4a and loop 4d. This fiber length 34 is stitched into substrate 2, when the axis 13--13 occupies its close up position 13.3.
FIGS. 12a to 12f illustrate yet another operating mode. In FIG. 12a, needle 21 has just been moved by a step p, corresponding to bridge 4c, and an adequate length 35 of fiber 4 is available at the output of needle 3.1. In addition, the thread clamp 32 is closed. The stitching operation begins by rotating needle 3.1 (FIG. 12b) and continues until, after insertion of segment 4a, loop 4d appears on the face 2a (FIG. 12c). A retention member 36 grips loop 4d. The thread clamp 32 opens and needle 3.1 travels over its return stroke while rotating and forms segement 4b (FIG. 12d). At the end of the return stroke (FIG. 12e), a member 37 grips fiber 4 at the output of needle 3.1 so as to form the length 35. The thread clamp 32 closes again and members 36 and 37 are retracted and the device (see FIG. 12f) is ready to move by step p so as to take up the position illustrated in FIG. 12a. Another stitching cycle may begin.
FIGS. 13 and 14 illustrate one embodiment of a stitching head 40 according to the invention. Arm 30 supports a reserve 41 of fiber 4 which is brought to needle 3 through a guide 42. Arm 30 carries in addition a motor 43 for actuating needle 3 in rotation about axis 13--13, a member 44 for actuating the loop retention member 36 and a member 46 for actuating the fiber gripping member 37. The various members and motor 43 to 46 are connected to control devices (not shown) by a connnector 47. In addition, the stitching head 40 comprises a collar 48 for fixing to a stitching machine such as shown in FIG. 15.
The machine 50, shown in FIG. 15, comprises an arm 51 which may be moved along three dimensions X, Y and Z with respect to a frame 52. For this, arm 51 may be moved vertically along Z, with respect to a carriage 53, by means of a motor 54, whereas carriage 53 is mounted for movement along Y on a beam 55 by means of a motor 56 and said beam 55 is itself movable along X, with respect to frame 52, by means of a motor 57. The stitching head 40 is mounted at the lower end of arm 51 so as to be rotatable about each of axes X, Y and Z. In addition support 1, illustrated in FIG. 15 in the form of a rotary mandrel, carries substrate 2. From control station 58 the movement of head 40 with with respect to substrate 2 and the different stitching operations of needle 3 in the substrate can be controlled.
It can thus be seen that with the invention reinforcement elements can be obtained comprising curved fibrous segments. Of course, support 1 may have any desired form and the direction of the stitching lines, not only with respect to support 1 but also with respect to the plane of needle 3 may be chosen depending on the result to be obtained. The same goes for the depth of stitching in substrate 2. Moreover, the stitching lines may be rectilinear, curved, circular, helical etc . . . .
After obtaining such a reinforcement element, it is impregnated as is known with a hardenable binder so as to obtain a part 60 (see FIG. 16). If required, this part 60 is then machined, at least on the surface, so as to obtain the final part 61. | A method and device are disclosed for forming reinforcement elements from resistant fibers distributed along three dimensions, in which method, a continuous fiber is introduced in a substrate resting on a support formed of such fibers crossed in at least two directions, by stitching, from the free face of said substrate opposite said support by means of a needle driven with a reciprocal movement, a relative movement being in addition generated between said support and said needle so that said continuous fiber is formed inside said substrate of a succession of consecutive segments forming a zig-zag line.
The invention is remarkable in that:
said needle is curved and imposes on each segment of said continuous fiber a similar curved form; and
the reciprocal movement of said curved needle occurs while rotating about an axis perpendicular to the plane of said needle and disposed on the concave side thereof. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 12/008,772 filed Sep. 21, 2010, now U.S. Pat. No. 7,799,221, which is herein incorporated by reference in its entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to liquid pumps and more particularly it relates to structure of a rotary axial piston pumping unit, that can serve as the primary system pump pressurizing a system destination, such as an RO (reverse osmosis) chamber, the pumping unit incorporating a pressure exchanger for reducing the operating cost by recovering energy from a secondary flow that may be an unwanted byproduct from the process, for example brine discharged at high pressure from an RO seawater desalination system.
2. Background of the Invention
The functional block diagram of FIG. 1 shows a basic form of an RO (reverse osmosis) filtering system of known art without energy recovery, e.g., a small system for an individual home or small business. A pressurized RO enclosure 10 receives a water supply at its input node “a” at elevated pressure, either from municipal water mains or, as shown pressurized by a pressure pump 12 driven by a motor 14 , typically electric. Pump 12 draws water from a relatively low pressure source such as a well, river or lake optionally via preconditioning and filtration apparatus, and develops high pressure at node “b”, the intake port of the main chamber IDA of RO container 10 , where the pressurized liquid is forced against an RO membrane 10 B, typically polyamide thin-film composite that will not pass sodium or chloride ions. In RO seawater desalination, about 40% of the intake liquid traverses membrane 10 B to compartment 10 C as desalinated water, available to be drawn off as required at outlet “c”. The remaining 60% of the input liquid including extracted residue leaves chamber 10 A as a secondary flow of more concentrated unwanted components, such as the salt in brine, from the RO outlet port “d” where it passes through a back-pressure regulating valve 17 to discharge port “d” where the secondary flow is discharged to a drainage system as wastewater, typically returned directly or indirectly to the sea.
It has long been recognized that there is a substantial amount of energy Ed available in the secondary liquid flow at RO brine exit port “d”, where, compared to 100% pressure Pb and flow rate Rb of the primary flow at intake port “b”, the pressure Pd is typically 99% and the flow rate Rd is 60%.
The energy at the RO brine exit port “d” can be calculated from the product of pressure and flow rate (Ed=Pd*Rd): for the foregoing conditions, Ed is found to be 59.4% of Eb. Since the ultimate discharge from node “e” is typically at relatively low pressure, most of the waste energy is dissipated as heat at valve 17 and its environment. Efficient recovery of this energy can provide substantial savings in operating cost.
The energy available at the outlet valve 17 can be estimated from the reduction in pressure at the rated discharge flow; if this energy could be totally exchanged for a reduction in the electrical energy consumed by the motor driving the primary pump 12 , the net energy recovery of 59.4% would reduce the operating energy cost to 40.6% of the operating energy cost of the basic non-recovery system of FIG. 1 . However, practical systems can only approach this limit due to unavoidable machine losses such as friction of bearings, and pistons, and leakage of seals, pistons and valves, turbulence, etc. Thus the design of more efficient systems of this kind remains a challenge with potential that has not yet been fulfilled by known art.
FIG. 2 illustrates a system as in FIG. 1 modified to include energy recovery by the addition of an energy exchanger 18 , connected into the RO brine discharge flow path between nodes “d” and “e” in place of valve 17 . Energy recaptured from pressure drop in this flow is fed back to the primary liquid flow side between nodes “a” and “b” as indicated by the arrow.
Many different approaches have been suggested and tried for implementing this energy feedback. The flow/pressure drop energy recaptured in a liquid motor such a turbine from which torque can be applied to shaft 16 of the primary RO pressurizing pump 12 . Alternatively or additionally, the recovered energy torque can drive an auxiliary pump or equivalent introduced in series and/or parallel with the existing primary pump 12 to reduce its pressure/flow rate loading, and thus reduce the electric power consumption of drive motor 14 . The efficiency of this energy exchange system is critically important since it directly affects the actual amount of operating cost savings realized. Electric motor efficiency is about 90-95% and pump efficiency ranges from 50 to 90%, typically 80%, so these machines are generally selected for high efficiency.
Energy and pressure exchange systems have been the subject of much design research, development and refinement to reduce capital costs and operating costs; with increasing concern about world wide consumer water availability, there are increasing efforts to develop machines that recapture energy from RO brine discharge even more efficiently to accomplish more cost-effective desalination.
DISCUSSION OF KNOWN ART
Several different approaches have been disclosed in patents for apparatus performing the function of energy/pressure exchange, e.g., in the role of energy exchanger 18 in FIG. 2 , for energy recovery in RO desalination systems.
FIG. 3 is a simplified functional block diagram illustrating a basic energy exchanger approach, as exemplified in U.S. Pat. No. 6,804,962 to Prueitt for a “Solar Energy Desalination System”, wherein a hydraulic motor 20 , driven by the flow of brine discharge from exit port d, has its shaft 21 coupled to the shaft 16 of the main motor 16 which also drives the main pump 12 .
Hydraulic motor 20 , typically a turbine, converts P*F hydraulic energy to mechanical energy, i.e., torque applied via shaft 22 to shaft 16 , that acts to reduce the load on main motor 14 and thus reduces the electrical power consumption and the overall operating costs accordingly.
To estimate the efficiency of such a system, it is assumed that the system is designed and regulated so as to hold the RO input pressure and flow, thus the RO input energy Eb, constant. Assuming a typical high quality commercially available level of 90% efficiency (10% loss) for both the main pump 12 and for the hydraulic energy exchange motor 20 , their combined efficiency will be 81% (19% loss); thus the net energy recovery of 48.1% would reduce the operating energy cost to 51.9% of that of the basic non-recovery system of FIG. 1 , whereas the theoretical limits are 59.4% (recovery) and 40.6% (cost).
To avoid the compounding of energy loss by both the pump 12 and the hydraulic motor 20 , various “pressure” and “energy” exchangers have been developed to exchange energy in a more direct and efficient manner, usually in cylinders with programmed valves and moving piston barriers between the output and input liquid flow paths, exchanging reduction of pressure in the outflow for contribution to RO input pressure and/or flow rate, thus reducing the work load on the main pump 12 and motor 14 for lower operating cost.
FIG. 4 shows a known AP (axial piston) pressure exchange system utilizing a pair of fixed dual-chamber cylinders 22 and 24 mounted between end block valve enclosures 26 and 27 under control of a timing system that causes free-moving pistons 28 and 30 to reciprocate in a manner to exchange pressure. Because pistons 28 and 30 are equal in diameter on both sides, the primary side acting as pump provides about 60% of the total primary flow, with pump 12 providing only the remaining 40%. However due to pipe and exchanger losses, a small pressure booster pump 32 and motor 34 must be added in the primary side. This approach is exemplified by U.S. Pat. No. 5,306,428 to Tonner for “Method of Recovering Energy From Reverse Osmosis Waste Streams” and U.S. patent application publication No. 2005/0166978 A1 to Brueckmann et al for “Pressure Exchanger System”.
FIG. 5 shows a related AP approach: two dual-chamber cylinders 36 and 38 are disposed co-linearly in a common cylinder sleeve between end block valve assemblies 40 and 42 . A free-moving pair of double-sided asymmetrical pistons 44 and 46 , separating the two quasi-complementary chambers in cylinders 36 and 38 respectively, are coupled by a central rod 48 which traverses central partition 49 through a sliding seal. Rod 48 is specially dimensioned to reduce the effective piston area on one side of each piston, proportional to respective flow rates, thus eliminating the need for a booster pump and motor as in FIG. 4 . This approach is exemplified in U.S. Pat. No. 4,637,783 to Andeen for “Fluid Motor-Pumping Apparatus and Method for Energy Recovery” and U.S. Pat. No. 5,462,414 to Permar for “Liquid Treatment Apparatus for Providing a Flow of Pressurized Liquid”. In a similar arrangement disclosed in U.S. Pat. No. 6,017,200 to Childs et al for “Integrated Pumping and/or Energy Recovery System”, the shaft-linked piston pair is driven by a pump to reciprocate axially.
While in each of the foregoing patents the two cylinders are shown equal in diameter, U.S. Pat. No. 3,293,881 to Walker for “Means for Transferring Fluids in an Absorption Refrigeration System” shows the two co-linear cylinders (and their respective free-moving central-shaft coupled pistons) made substantially different in diameter (see FIG. 2 ) to provide different flow rates which are proportional to piston area for a given stroke length.
It should be understood that the above descriptions of fixed cylinder type energy/pressure exchangers are greatly simplified for ease of understanding, while in real implementation they become extremely complex due to critical requirements of an elaborate control system for motor speed, flow rate, timing, synchronizing and sequencing the control valves and regulators with the reciprocating travel of driven or free-moving pistons as required to realize acceptable operating efficiency.
In a special category of pressure/energy exchangers similar to those described above with free-moving pistons, even these pistons are eliminated to avoid their friction losses and maintenance problems; the seawater and brine are allowed to interface directly at a virtual piston region, and the control system and/or operating staff must monitor and regulate flows, pressures, valve timings, rotational speeds, synchronization, etc., very diligently and precisely to minimize the unwanted effects of intermixing.
Whether through sophisticated computer automation or the diligence of skilled human operating staff, high operating efficiency for economical operation is extremely difficult and challenging to accomplish and maintain since it has to take into account many short term and long term side effects and variables such as temperature of liquids and machines, variation in demand and removal of desalinated product, power line voltage variations, membrane condition, leakage, wear degradation of machinery, seals, valves, etc.
Fluctuation in the cost of electric power is an important factor as evidenced by U.S. Pat. No. 6,998,053 B2 to Awerbuch for “Water Desalination Process Using Ion Selective Membranes” “ . . . at a variable pressure as a function of the cost of electricity . . . . ” Similarly, interest rates have been cited as influencing decisions involving capital costs versus operating costs in overall design tradeoffs, particularly for large scale projects.
Patent publication US 2007/0128056 A1 to Haudenschild for a “Highly Efficient Durable Fluid Pump and Method” discloses a piston, in a cylinder defining first and second volumes, driven reciprocally by an attached rod. Two ports of the stationary cylinder block are fitted with check valves 38 and 40 and two other ports are fitted with ball-type rotary valve units 42 and 44 , driven from an external motor by a pair of rotating shafts 58 and 60 .
FIG. 6 is a cross-sectional representation of an energy exchanger of the rotor-drum AP (axial piston) category in the field of endeavor addressed by the present invention. This AP rotor-drum category is exemplified in U.S. Pat. No. 3,431,747 to Hashemi et al for “Engine For Exchanging Energy Between High And Low Pressure Systems”. Two cylinders 50 and 52 (or more) are formed as bores through a metal cylindrical rotor-drum 54 , mounted to rotate between sliding end valve enclosures 56 and 58 and driven rotationally, typically from the shaft of a motor. A free-moving symmetrical double-sided piston is formed in each cylinder by lightweight spheres 60 and 62 . A rotor-drum with free-moving pistons is also disclosed in European Patent Application EP 1,508,361 A1 by Olsen for “A Pressure Exchanger”. Other AP rotor-drum type pressure exchangers are disclosed in U.S. Pat. No. 4,887,942 to Hauge for “Pressure Exchanger for Liquid” and U.S. Pat. No. 6,659,731 B1 to Hauge for “Pressure Exchanger”.
In recognition of the desirability of combining the main input pump with a pressure exchanger for energy recovery in a single self-contained unit, a combined primary pressure pump and energy/pressure exchanger utilizing swash-plate driven axial cylinder/piston arrays in rotor drums has been disclosed by the present inventor in U.S. patent application Ser. No. 11/523,937, filed Sep. 21, 2006.
In a special category of AP rotor-drum hydraulic pumps and motors addressed by the present invention, the axial pistons in a setoff cylinders arrayed radially in the rotor-drum are reciprocated by an angled swash-plate, sometimes referred to as a wobble-plate or cam-plate. This swash-plate AP rotor-drum category has been highly developed and used widely in hydraulic motors and/or pumps for refrigeration and industrial hydraulic machinery, as exemplified in U.S. Pat. No. 5,778,757 to Kristensen et al and U.S. Pat. No. 6,000,316 to Møller et al., both assigned to Danfoss A/S, Nordborg, Denmark under the title “Hydraulic Axial Piston Machine”.
Swash-plate AP type units can be designed to function either as a pump or as a hydraulic motor, And, as such, they have been applied in oil hydraulic systems for decades, but only recently have there been good technological advancements in the field of water hydraulics where water is used as both the lubricating and hydraulic fluid instead of oil. As a result, water hydraulic AP pumps are now available made from materials suitable for seawater desalination and find use in salt water RO systems today. A water hydraulic pump is available from Danfoss Pump.
However, the concept of combining the hydraulic AP (axial piston) pump and hydraulic PX (pressure exchanger) motor in a single integral unit for use with non-oily liquids such as seawater remains a challenge unfulfilled by known art, subject to the discovery and development of new configurations with novel deployment of recently developed materials.
In principle, energy could be recovered in an RO process as in FIG. 3 utilizing a hydraulic swash-plate type motor driven from the output brine stream, shaft-coupled to assist the input pump which could also be of the hydraulic swash-plate type, subject to capability of handling seawater; however such an approach would require two hydraulic machines of special custom design and manufacture to operate with water and would still be subject to the compounding of transducer losses in both machines with the resultant limitation on efficiency as described above in connection with FIG. 3 . The cylinders/pistons are arranged in two arrays, primary and secondary, each in a corresponding rotor-drum with typically nine cylinders a radial array, the two rotor-drums flanking a stationary swash-plate assembly that drives the pistons axially when the rotor-drums are driven rotationally from an external motor, typically electric. The pistons are arranged in collinear pairs, each pair coupled by a mechanical link that traverses a central opening in the swash-plate. The pistons in the primary array and their corresponding cylinders are made to have an effective diameter that is different than, typically larger than, that in the secondary array, as dictated by the physical liquid dynamics of the required pressure exchange.
The above-described disclosure represents a step of accomplishment in the advancement and ongoing development in the field of endeavor of primary liquid flow pumps of the AP swash-plate rotor-drum type incorporating pressure exchanger energy recovery, particularly as directed to seawater desalination.
OBJECTS OF THE INVENTION
It is a primary object of the present invention to provide further refinements beyond the art described above for enhancements in efficiency, reliability and cost effectiveness in the evolution of this field of endeavor, including simplification with fewer moving parts for long term reliability and low maintenance, thus accomplishing lower capital costs and lower operating costs.
It is a primary object to provide an improved hydraulic pump mechanism suitable to serve as the primary input pump of an RO system, incorporating structure that includes a pressure exchanger that recovers energy from the brine output flow of the RO system through direct pressure exchange without intervening energy conversions.
It is a further object to implement the combination pump utilizing proven aspects of rotor-drum rotational sliding valve port technology for both the APP (axial piston pump) function and the PX (pressure exchanger) function in novel combination that provides optimal benefit of recovered energy, particularly as applied to an RO desalination system.
It is a further object to minimize the number of moving parts in the combination pump and pressure exchanger.
It is a still further object that the implementation of the combination machine allows the pistons to rotate freely within the cylinders as practiced in known swash-plate type hydraulic motors and pumps, since this practice is considered beneficial with regard to long term reliability through even distribution of wear throughout the cylinder walls and pistons.
It is a still further object that the rotor be allowed to float freely axially between the two flat valve planes of the end blocks so that the liquid lubricant is allowed to form balanced seals at the interfacing surfaces at each end.
SUMMARY OF THE INVENTION
The above mentioned and other objects and advantages have been realized in a rotor-drum type APP (axial piston pump), for primary liquid flow pressuring, that incorporates a PX (pressure exchange) hydraulic motor function for energy recovery from a secondary liquid flow such as the brine discharge from an RO seawater desalination system. A single rotor-drum contains a set of dual function cylinders each containing a dual function axial piston. The system can be optimized for efficient deployment in an RO system to provide benefits including unusual simplicity, compact machine size and low capital and operating costs. Long term reliability is enhanced by the pistons being made free to rotate in place within the cylinders for uniform distribution of frictional wear. Special materials, tolerances and configurations such as lubrication ducts directed to the swash-plate sliders enable liquid such as seawater to act as lubricant.
BRIEF DESCRIPTION OF THE DRAWINGS
The above stated and further objects, features and advantages of the present invention will be more fully understood from the following description taken with the accompanying drawings in which:
FIG. 1 is a functional block diagram of a basic RO system without energy recovery as described above in connection with background of the invention.
FIG. 2 is a functional block diagram of a basic RO system as in FIG. 1 with the addition of energy recovery from the brine discharge as described above in connection with background of the invention.
FIG. 3 depicts an implementation of FIG. 2 with energy recovery utilizing a hydraulic motor shaft-coupled to the primary pump as described above in the discussion of known art.
FIG. 4 is a functional block diagram of a known RO system with energy recovery utilizing a pressure exchanger with a free-floating piston in each of two cylinders as described above.
FIG. 5 is a functional block diagram of a known RO system with energy recovery utilizing a pressure exchanger with a coupled pair of pistons free-floating two co-linear cylinders as described above.
FIG. 6 is a functional block diagram of a known rotor-drum type pressure exchanger with two cylinders each containing a free-floating spherical piston as described above.
FIG. 7 is a functional block diagram showing a single machine combining a pressure pump and a pressure exchanger according to the present invention deployed as the primary pump in a reverse osmosis desalination system.
FIG. 8 is a three-dimensional view of the exterior of the machine of FIG. 7 in a primary embodiment of the present invention.
FIG. 9 is a quasi-cross-sectional representation showing the interior configuration of the machine of FIG. 8 .
FIG. 10 depicts the primary stator sliding valve plate of the machine of FIG. 9 .
FIG. 11 depicts the secondary stator sliding valve plate of the machine of FIG. 9 .
FIGS. 12-15 show four sequential operating conditions of the pistons and valves of the machine of FIGS. 8 and 9 within a revolution of rotation of the rotor-drum.
FIG. 16 is a quasi-cross-sectional representation of an alternate version of the secondary portion of the pumping machine of FIGS. 8-11 .
FIG. 17 is a quasi-cross-sectional representation of an alternative embodiment of the pumping machine of the present invention with all valves and ports located in the primary end block at the primary end of the rotor-drum.
FIG. 18 depicts the single dual-function stator sliding valve plate of the machine of FIG. 17 .
FIG. 19 is a table showing nominal values of pressure P, flow rate F, and energy (P*F) at five system nodes of a reverse osmosis system as shown in FIG. 7
DETAILED DESCRIPTION
FIGS. 1 and 2 have been described above in connection with the discussion of background of the invention. FIGS. 3-6 have been described above in connection with the discussion of known art.
FIG. 7 is a functional block diagram showing a single machine 64 combining a pump and a pressure exchanger in accordance with the present invention, deployed as the primary pump in a reverse osmosis desalination system. The machine 64 is a self-contained unit that includes the main primary flow pressure pump and a secondary (brine) flow actuated energy exchanger PX assisting the pump AP.
Machine 64 is connected to RO unit 12 seawater intake flow path (ports/nodes a and b) which receives seawater at low pressure from pre-conditioning apparatus, and the brine output flow path (ports/nodes d and e) in the simple and direct manner shown: all that is needed additionally to operate the RO unit 12 is the electric motor 14 driving shaft 16 , seawater acquisition and preconditioning apparatus, and the interconnecting pipelines, with minimal requirements for associated control and monitoring apparatus, primarily to regulate motor speed for RO input pressure and flow rate.
FIG. 8 is a three-dimensional view of the exterior of a combined axial piston type pump and energy-recovery pressure-exchanger 64 in a preferred embodiment of the present invention with liquid flow indicated by the four arrows.
At the left hand end, inlet port “a” and outlet port “b” are in the primary flow path. At the right hand end inlet port “d”, shown at the top, and associated outlet port “e” at the bottom but not visible in this view, are in the secondary flow path. Drive shaft 16 , at the right hand end, is provided for connection to a drive motor, typically electric, to rotate an internal rotor-drum.
FIG. 9 is a quasi-cross-sectional representation of machine 64 of the present invention as in FIGS. 7 and 8 . A pair of end blocks 66 (AP) and 68 (APX) interface opposite ends of a rotatable rotor-drum assembly 70 wherein a rotor-drum 72 driven by shaft 16 is configured with a set of cylinder bores arranged axially in a polar array and extending uniformly to open ends at the left hand primary end. Each cylinder contains a closely fitted piston as exemplified by pistons 74 and 76 shown this view.
The number of cylinders in a rotor-drum is a matter of design choice, subject to appropriate valve design; it could even function with a single cylinder (subject to balancing difficulties); however for clarity and ease of understanding, in FIGS. 9 and 12 - 15 two cylinders are shown as being located diametrically opposite each other, i.e., 180 degrees apart, as they would be in a rotor-drum having an even number of cylinders. Since the cylinders function in uniform sequence, the present descriptions are valid for any number of cylinders, e.g., five as in the preferred embodiment.
At the left hand APP primary end, the inner face of primary end block 66 is configured as a manifold with a pair of cavity compartments, one for the primary intake port “a” and one for primary outlet port “b” (refer to FIGS. 7 and 8 ); these are shaped to function as primary valve ports. Attached on the flat inner surface of end block 66 is a primary stator plate 88 which is made of special liquid-lubricated material and which forms a sealed sliding valve interface that interfaces the flat primary end of rotor-drum 72 forming valve ports directly at the open ends of the primary cylinders and provides rotary valve commutation for the primary pump function.
At the right hand secondary end, a set of passageways, e.g., passageways 78 and 80 , are configured in a peripheral extended secondary region of rotor-drum 72 each leading outwardly from a side location of a corresponding secondary cylinder to a corresponding valve port in the flat annular secondary end region of rotor-drum 72 , interfacing a secondary stator plate 90 , attached to or made part of secondary end block 68 , which is configured as a manifold with a pair of compartments in communication with secondary inlet port d and secondary outlet port e, thus providing rotary valve commutation for the secondary pressure exchanger function.
A swash-plate 82 , at the inward side of the secondary end block 68 , presents a liquid-lubricated angled flat surface that serves to reciprocate the pistons, e.g., 74 and 76 , via slide pads 84 and 86 attached to the spherical ends of the piston drive rods in a swivel manner, as the rotor-drum assembly 70 is rotated by a motor coupled to shaft 16 . Piston 74 is shown at the left hand end of its stroke while piston 76 is shown at the right hand end of its stroke, in accordance with their locations on the swash-plate 82 at the particular point of time/rotation. Swash-plate 82 shown as a separate part with a wedge shape, thicker at the top, attached to end block 68 , could be made as an integral part of end block 68 in a single piece, or alternatively the swash-plate could be made uniform in thickness and attached to a wedge-shaped support part configured specially in end block 68 .
In the secondary cylinder chambers, the coaxial piston drive-rods each extend through a corresponding sealed circular slide-bearing opening in a bulkhead region of rotor-drum 72 , thus forming a working secondary cylinder chamber at the secondary end of each piston. In this secondary cylinder region, the effective area of each piston is reduced by the presence of the drive rod by an amount equal to the cross-sectional area of the drive rod. In overall design, these rods are dimensioned particularly to make the ratio of effective secondary/primary piston area equal to the ratio of secondary/primary liquid flow rate, the piston stroke length being the same for both the primary and secondary cylinder regions. A tubular outer shell 92 extends between the end blocks 66 and 68 .
FIG. 10 depicts the primary stator sliding valve plate 88 , of the machine of FIG. 9 , which serves as reversing/commutating liquid-lubricated sliding valve commutating the fluid communication between the open ends of the primary cylinder chambers, e.g., end 96 aligned circularly with arcuate kidney-shaped pair of slots 94 , forming valve ports, and two manifold chambers configured as a manifold in primary end block 66 ( FIG. 9 ) that includes primary intake/outlet ports a and b respectively. These valve ports remain open to those cylinders whose piston is moving throughout a half-revolution stroke, but can be allowed to close for each cylinder at stroke-end locations for reversal transition, as the liquid flow ceases momentarily.
FIG. 11 depicts the secondary stator valve plate 90 of the machine of FIG. 9 . A symmetrical pair of arcuate kidney-shaped valve apertures 98 are aligned with the circular rotational path of the set of five arcuate valve ports 100 , shown in broken lines, formed at the ends of the passageways, e.g., 78 and 80 in rotor-drum 72 ( FIG. 9 ), providing sliding valve commutation of fluid communication through the passageways to the corresponding secondary cylinder chambers. The secondary valve stator plate apertures 98 are made narrower than the primary valve stator plate apertures 94 , but their operation is similar. These apertures are carefully sized in design to balance the thrust on the rotor-drum sliding valve surfaces.
FIG. 12 is the first of four sequential functional quasi-cross-sectional representations, FIGS. 12-16 , depicting piston and valve operating conditions in a single revolution of the rotor-drum assembly of any embodiment of the present invention, as exemplified in FIGS. 7-11 . At the starting point of rotor-drum revolution shown in FIG. 12 , piston 74 is shown having traveled axially to the left hand limit of its travel range, while piston 76 is shown having traveled axially to its right hand travel limit.
Pistons 72 and 74 at opposite limits of their respective axial travel range as dictated by the swash-plate-driven stroke; at this instant there is virtually no liquid flow in or out while the sliding valve ports are typically closed in a brief transition interruption in their role of sequentially diverting cylinder liquid flow path alternately between the intake and the outflow ports in synchronism with rotor-drum rotation.
FIG. 13 shows pistons 72 and 74 moving in the directions indicated by the arrows, the rotor-drum having rotated about a quarter revolution and shifted the pistons to a mid-stroke region of the travel range as driven by the swash-plate. Piston 76 is moving axially to the left as indicated by the arrow, driven by the stationary swash-plate as the rotor-drum rotates; piston 76 also receives a portion of its driving force from the high pressure of secondary liquid entering via the arcuate slot of secondary stator valve plate 90 ( FIG. 11 ) from intake port “d”, acting on the of piston 74 in the secondary (right hand end) cylinder chamber. The left hand end of piston 74 , in the primary cylinder chamber, is acting in a pump pressure stroke, performing the work of moving primary liquid under pressure to its destination through primary stator valve plate 88 ( FIG. 10 ) and port b. Simultaneously, piston 74 , moving to the right in an output stroke as indicated, is expelling secondary liquid from the secondary chamber through stator valve plate 90 and port “e” while the left end of piston 74 , in an intake stroke, is drawing primary liquid into the primary chamber through valve plate 88 and port “a”.
Throughout a major portion of each half-revolution stroke, the ports in the rotor-drum and the stator valve plates are made and arranged to align and co-operate as sliding valves to provide the required liquid flow path between each primary and secondary cylinder chamber and the corresponding one of the four intake/output ports: “a”, “b”, “d” and “e”.
FIG. 14 shows the rotor-drum having rotated about a quarter revolution further to end of the half revolution stroke with pistons 74 and 76 having reached the end of their axial travel range opposite to their locations in FIG. 12 : at this point, pistons 74 and 76 have become interchanged in both their axial and radial locations, and again as in the FIG. 12 , there is no primary or secondary liquid flow, as the valves are in a state of transition.
FIG. 15 shows the rotor-drum having further rotated about a quarter revolution to the three quarter revolution mid-stroke region where the actions and liquid flow are identical to those shown and described in connection with FIG. 13 except that now the roles of the two pistons 74 and 75 have become interchanged, and they will continue to travel in the directions indicated during the fourth quarter of revolution of rotation until once again the rotor-drum returns to the initial condition shown in FIG. 12 , after which the same cycle repeats for each revolution of the rotor-drum.
Continuous repetition of these two-stroke cycles at a suitable regulated motor speed produces the desired destination pressure and energy-recovery-assisted flow rate at port b of the machine, which in an RO system is the main node, i.e., the main intake port of the RO chamber (node “b”, FIG. 7 ), at a required energy level, i.e., product of pressure and flow rate. A substantial portion of this energy may be recovered from the waste brine flow by highly efficient performance of the pressure exchanger in reducing the loading on the pumping action of the primary cylinder assembly and thus substantially reducing the electric power consumed by the pump drive motor and reducing the operating cost accordingly.
As an alternative to the valve/port configuration shown in FIGS. 9-11 , the pumping machine of this invention could be implemented with manifold cavities in primary end block 66 that would locate ports a and b on the top and bottom of end block 66 facing radially instead of axially as shown. Similarly the manifold cavities and passageways 78 and 80 in secondary end block 68 could be configured differently so as to locate ports d and e on the end surface of end block 68 facing axially instead of radially as shown.
FIG. 16 is a quasi-cross-sectional representation of an alternative version of the primary embodiment of the pumping machine of the present invention as shown in FIG. 9 , wherein the secondary stator sliding valve plate 90 A has been relocated inwardly to a plane that defines a flat secondary end of rotor-drum 72 A. The APX end block 68 A is configured with passageways 78 A and 78 B as part of the dual manifold cavities communicating with ports d and e. The stator sliding valve plate 90 A is similar to the counterpart in the previous version ( FIG. 9 ).
FIG. 17 is a quasi-cross-sectional representation of a second embodiment of the pumping machine of the present invention as an alternative to the primary embodiment, e.g., as shown in FIG. 9 . The main difference is that a set of passageways, e.g., passageways 78 B and 80 B, configured in rotor-drum 72 B, are directed inwardly from each secondary cylinder end and thence to the primary end thus enabling all valves and ports a, b, d and e to be located at the primary end with manifolds configured in primary end block 66 A where a single dual-function stator sliding valve plate 88 A slidingly interfaces the primary end of the rotor-drum 72 B as shown.
Pistons 74 and 76 , sliders 84 and 86 , swash-plate 82 , shaft 16 and tubular outer shell 92 may be essentially the same as in the primary embodiment ( FIG. 9 ).
A simple end plate 68 B serves as the secondary end block, requiring no manifold cavities or ports. This embodiment enables the pumping machine to be made smaller and simpler than the primary embodiment, however it will require design attention to pressure effects at the valve interface since it does not receive benefit of the primary embodiment's inherent degree of interface pressure balance between the two valve units due to their location at opposite ends of the rotor-drum.
FIG. 18 depicts the single dual-function stator sliding valve plate 88 A of the machine of FIG. 17 with arcuate kidney-shaped primary valve ports 94 interacting with open cylinder ends 96 , essentially the same as in the primary embodiment ( FIG. 10 ), and the secondary arcuate kidney-shaped valve ports 98 A interacting with open passageway ends, e.g., passageway 78 B.
FIG. 19 is a table showing nominal values of pressure P, flow rate F, and energy (P*F) at five system nodes of a reverse osmosis system as shown in FIG. 7 operating from the combination machine of the present invention; four of the five system nodes correspond to the machine's primary and secondary intake/output ports.
In any of the embodiments, all of the interfacing sliding-valve surfaces and the swash-plate/slider surfaces are preferably precision-machined, polished or otherwise configured for water-lubricated sliding action and kept lubricated, e.g., by liquid from the primary and/or secondary liquid flow.
Ideally the slide pad surfaces are specially configured with a combination of super-flat surfaces and strategic cavities that enable them to hydroplane against the swash-plate on a film of liquid lubricant.
As described above in connection with the illustrative embodiment, the five dual-function cylinders located on a common polar array with the five associated dual-function pistons makes the rotor-drum assembly simple and straightforward with only about half the moving components required for an equivalent APP/PX machine having two rotor-drums, i.e., one primary and one secondary, straddling the swash-plate. Furthermore there are performance advantages of inherent rotor balance, smoothness of rotation, freedom from binding effects, and reliability due to the minimum number of moving parts. Thus it is believed that this integrated primary/secondary cylinder/piston arrangement accomplishes an unusually simplified, elegant, cost effective and reliable machine of this category. The illustrative embodiment represents a special case of convergence of judicious choice, amongst numerous possible variations, that yields an optimal manner in which the invention may be practiced.
There are some alternatives and matters of design choice with which the invention could be practiced with comparable if not totally equivalent benefit, and there are many more alternatives that would function generally but that could introduce tradeoffs of various degrees of degradation such as added complexity, production difficulty, increased cost, and potential loss of reliability.
As a matter of design choice, the quantity of cylinders/pistons in the rotor-drum assembly is not particularly critical, e.g., six or seven or more could function as well as five. Technically the invention could be practiced with as few as two, and possibly with one, but would risk inherent unbalance and vibration, and could require a more complex reversing valve and control system.
In any embodiment of the invention, as an alternative to implementing the stator valve plates (e.g., 88 and 90 , FIG. 9 ) as separate plates affixed to the end blocks 66 and 68 , either or both could be made as an integral part of the associated end block, subject to proper material selection for liquid-lubricated sliding valve surfaces.
Shaft 16 could be extended from the primary end of the machine instead of the secondary end as shown, or it could be made to extend from both ends.
The swash-plate being also known and described in literature as a cam-plate, and even sometimes regarded as a subdivision under the heading of cam mechanisms, suggests that there are other forms of cam mechanisms or modifications of swash-plate mechanisms capable of converting shaft rotation efficiently into reciprocation for pistons in cylinders, with which the present invention could be practiced as design choice alternatives to the embodiment shown.
There are viable alternatives in implementing the rotor-drum assembly. The cylinders may formed as simple bores traversing an otherwise solid drum, or the cylinders walls could be made individual and replaceable by utilizing tubular cylinder liner inserts. The drum may made in the form of a framework instead of solid for material savings, or the cylinders may be formed as individual stand-alone sleeves cantilevered from a base at one end or supported at both ends by circular end disks.
End-block reversing-valve systems have been utilized in hydraulic machines, typically along with swash-plate reciprocation in conjunction with axial cylinder rotor-drums, providing advantages of elegant simplicity. However with evolving technology there is increasing potential of alternatively performing the valve reversal function under more sophisticated electronic system control that may enable practice of the invention with equivalent results.
While shown as directed to reverse osmosis seawater desalination, the principles of the energy-recovering pump-motor combination of the present invention are not limited thereto and may be beneficially applied to any two liquid flow streams and/or to liquids other than water and/or to other liquid flow energy exchange requirements, e.g., regular filtration and purification of drinking or other fresh water supplies.
While it is not essential for all the cylinders in one assembly to be the same size or to be uniformly spaced in a single circular polar pattern as shown, a uniform array pattern is generally preferable for providing inherent rotor-drum balance and thus minimizing vibration. However, subject to risk of vibration and increased cost and complexity regarding suitable reversing valve arrangements, virtually any pattern of multiple identical or different-sized cylinders could be made to function as long as their total piston area meets the necessary designated primary and secondary flow requirements. The ratio between the total piston areas in the primary and in the secondary cylinder assemblies is a key parameter that must be observed since it is inherently equal to the ratio between the primary flow rate and the secondary flow rate, for a given stroke length.
The swash-plate principle for developing reciprocation is based on relative rotation between two portions, shown herein as a rotor portion including the cylinders and pistons and a stator portion including the swash-plate and the end block valve system. The same functions could be performed with the present stator components being rotated and the present rotor components made stationary, with appropriate and possibly more complex modification of the reversing valve system. Alternatively the functions could be performed with both portions rotating at different rates and/or directions, but probably at the expense of further complication and increased cost.
The invention may be embodied and practiced in other specific forms without departing from the spirit and 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 by the foregoing description; and all variations, substitutions and changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. | A pumping machine, that can serve a system as the sole main pump for pressurizing a primary liquid flow, incorporates, in a single machine, a rotor-drum type AP (axial piston) pump and a PX (pressure exchanger) that recovers energy from a secondary liquid flow such as the brine discharge from an RO seawater desalination system, with benefits including fewer moving parts and small machine size along with lower capital and operating costs. A single rotor-drum containing the cylinders and pistons is located between two end blocks, one or both configured with manifold passageways, ports and sliding valves. A swash-plate at one end reciprocates the pistons axially when the rotor-drum is rotated. Two working chambers, primary and secondary, are formed at opposite ends of a single piston in each cylinder, thus enabling the single rotor-drum to function as a primary liquid-pressurizing axial pump (AP) with sliding valves at the primary end enabling primary liquid pumping, and as a secondary outflow-driven pressure exchanger (PX) recovering energy from pressure drop in the secondary liquid flow and thus contributing work to primary pumping, saving energy and reducing operating costs. | 8 |
RELATED APPLICATION INFORMATION
[0001] This application claims the benefit of and priority to U.S. Provisional Application Ser. No. 62/032,757, filed Aug. 4, 2014, the disclosure of which is hereby incorporated by reference herein in its entirety.
FIELD
[0002] The present invention relates to stereochemically defined polypropionates and methods for preparing and using the same. The stereochemically defined polypropionates may be useful in the synthesis of natural products and/or natural product-like libraries.
BACKGROUND
[0003] Biologically active natural products have played a key role in the elucidation of cellular processes and biological mechanisms, and have been fruitful sources of therapeutic agents for many decades. Nearly half of the new chemical entities introduced in drug discovery between 1981 and 2002 were natural products or semi-synthetic analogs of natural products. (Vasilevich, N. I., et al., J. Med. Chem. 2012, 55, 7003-7009.) Polypropionate tetrads and pentads comprise a core structural element of many biologically active natural products.
SUMMARY
[0004] The present invention provides stereochemically defined polypropionates, including stereochemically defined pentads and tetrads, and methods for preparing and using the same.
[0005] In some embodiments provided is a compound of Formula II′, III′, IV′, V′, VI′, and/or VII′ having the following structure:
[0000]
[0006] wherein:
[0007] Ph is phenyl; and
[0008] R 3 is each independently a hydrogen or an oxygen protecting group;
[0009] or a salt thereof.
[0010] In some embodiments, a compound of Formula II′, III′, IV′, V′, VI′, and/or VII′ can be used in a method of preparing a therapeutic.
[0011] In some embodiments, provided is a compound of Formula II, III, IV, V, VI, and/or VII having the following structure:
[0000]
[0012] In some embodiments, the invention provides methods for preparing stereochemically defined polypropionate pentads, such as compounds of Formulas II′, II, III′, III, V′, V, VI′, and VI, and stereochemically defined polypropionate tetrads, such as compounds of Formulas IV′, IV, VII′, and VII, from a compound of Formula I having the following structure:
[0000]
[0013] In certain embodiments, a compound of Formula II′, II, III′, III, IV′, and/or IV is prepared from an enantiomerically pure compound of Formula Ia having the following structure:
[0000]
[0014] In some embodiments, a compound of Formula V′, V, VI′, VI, VII′, and/or VII is prepared from an enantiomerically pure compound of Formula Ib having the following structure:
[0000]
[0015] In some embodiments, methods for preparing compounds of Formulas Ia and Ib are provided. In some embodiments, compounds of Formulas Ia and Ib are prepared in optically active form.
[0000]
[0016] In some embodiments, compounds of Formulas Ia and/or Ib are prepared by oxidizing a compound of Formula 1 having the following structure:
[0000]
[0017] In certain embodiments, a compound of Formula Ia or Ib is prepared by oxidizing an optically active compound of Formula 1A or 1B, respectively, having the following structure:
[0000]
[0018] In some embodiments, compounds of Formulas 1A and/or 1B can be obtained by resolving a mixture of compounds of Formulas 1A and 1B. In some embodiments, the resolution compounds of Formulas 1A and 1B can be achieved by selective crystallization and/or selective precipitation of a mixture of diastereomeric salts of Formulas 1A and 1B. In some embodiments, the mixture of diastereomeric salts of Formulas 1A and 1B can be obtained by forming a mixture of esters of Formulas 1A and 1B having free carboxylate groups, and then treating the mixture of esters of Formulas 1A and 1B having free carboxylate groups with a chiral amine-containing compound. In some embodiments, the mixture of esters of Formulas 1A and 1B having free carboxylate groups is obtained by treating a mixture of Formulas 1A and 1B with phthalic anhydride, to form a mixture of phthalates of Formulas 2A and 2B.
[0000]
[0019] In some embodiments, the mixture of phthalates of Formulas 2A and 2B is reacted with a chiral amine-containing compound to produce a mixture of diastereomeric salts. In some embodiments, the chiral amine is an enantiomer of α-methylbenzylamine. In some embodiments, the mixture of Formulas 2A and 2B is reacted with (R)-α-methylbenzylamine. In some embodiments, the mixture of Formulas 2A and 2B is reacted with (S)-α-methylbenzylamine.
[0020] In some embodiments, the mixture of diastereomeric salts is resolved by selective crystallization, or selective crystallization followed by recrystallization. In some embodiments, the mixture of Formulas 2A and 2B is treated with (S)-α-methylbenzylamine, and one of the diastereomeric salts is removed by filtration after it precipitates.
[0021] In some embodiments, a process for resolving enantiomers of a compound of Formula 1, is provided, the method comprising the steps of:
[0022] reacting the racemic compound of Formula 1 with phthalic anhydride to form a racemic mixture of phthalates of Formulas 2A and 2B having the structure:
[0000]
[0023] reacting the racemic mixture of phthalates of Formulas 2A and 2B with a first chiral amine in a solvent to form a pair of diastereomeric salts thereof in a solution;
[0024] precipitating a first diastereomeric salt of the pair of diastereomeric salts from the solution to provide an isolated first diasteriomeric salt and an second diastereomeric salt; and
[0025] forming the enantiomers of the compound of Formula 1 from the isolated first diastereomeric salt and the second diastereomeric salt, thereby resolving the enantiomers of the compound of Formula 1.
[0026] In some embodiments, provided is a compound of Formula 1′:
[0000]
[0027] wherein:
[0028] R is hydrogen or —C(O)R 1 , and
[0000] R 1 is selected from the group consisting of C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl, and heteroaryl, R 1 may be unsubstituted or substituted from 1 to 3 times with independently selected C 1 -C 6 alkyl, hydroxy, hydroxyC 1 -C 6 alkyl, methoxy, methoxyC 1 -C 6 alkyl, halo, haloC 1 -C 6 alkyl, —C(O)NH 2 , —NHCOOC 1 -C 6 alkyl, or —COOH group(s);
[0029] or a salt thereof.
[0030] In certain embodiments, provided is a compound of Formula 1 having the following structure:
[0000]
[0031] In some embodiments, a process for preparing a compound of Formula 1 is provided, the method comprising the steps of:
[0032] reacting 6,8-dimethyl-3,9-dioxatricyclo[3.3.1.0 2,4 ]nonan-7-one with a reducing agent to form an intermediate having the following structure:
[0000]
[0000] and
[0033] reacting the intermediate with an acid to form the compound of Formula 1.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] FIG. 1 shows exemplary natural products and illustrates portions corresponding to a compound of Formula II or IV.
DETAILED DESCRIPTION
[0035] Compounds of this invention include those described generally herein, and are further illustrated by the embodiments, sub-embodiments, and species disclosed herein. As used herein, the following definitions shall apply unless otherwise indicated.
[0036] As described herein, compounds of the invention may optionally be substituted with one or more substituents, such as those illustrated generally herein, or as exemplified by particular classes, subclasses, and species of the invention. In general, the term “substituted” refers to the replacement of a hydrogen atom in a given structure with a specified substituent. Unless otherwise indicated, a substituted group may have a substituent at each substitutable position of the group, and when more than one position in any given structure may be substituted with more than one substituent selected from a specified group, the substituent may be either the same or different at every position. Combinations of substituents envisioned by this invention are preferably those that result in the formation of stable or chemically feasible compounds.
[0037] “Isomers” refer to compounds having the same number and kind of atoms and hence the same molecular weight, but differing with respect to the arrangement or configuration of the atoms.
[0038] “Stereoisomers” refer to isomers that differ only in the arrangement of the atoms in space.
[0039] “Diastereoisomers” or “diastereomers” and grammatical variants thereof, as used herein, refer to stereoisomers that are not mirror images of each other.
[0040] “Enantiomers” and grammatical variants thereof, as used herein, refer to stereoisomers that are non-superimposable mirror images of one another.
[0041] Enantiomers include “enantiomerically pure” isomers that comprise substantially a single enantiomer, for example, greater than or equal to 90%, 92%, 95%, 98%, or 99%, or equal to 100% of a single enantiomer.
[0042] “Enantiomerically pure” as used herein refers a compound that comprises substantially a single enantiomer, for example, greater than or equal to 90%, 92%, 95%, 98%, or 99%, or equal to 100% of a single enantiomer. In some embodiments, a composition may comprise a compound that is enantiomerically pure.
[0043] “Stereomerically pure” as used herein means a compound or composition thereof that comprises one stereoisomer of a compound and is substantially free of other stereoisomers of that compound. For example, a stereomerically pure composition of a compound having one chiral center will be substantially free of the opposite enantiomer of the compound. A stereomerically pure composition of a compound having two chiral centers will be substantially free of diastereomers, and substantially free of the enantiomer, of the compound. A typical stereomerically pure compound comprises greater than about 80% by weight of one stereoisomer of the compound and less than about 20% by weight of other stereoisomers of the compound, more preferably greater than about 90% by weight of one stereoisomer of the compound and less than about 10% by weight of the other stereoisomers of the compound, even more preferably greater than about 95% by weight of one stereoisomer of the compound and less than about 5% by weight of the other stereoisomers of the compound, and most preferably greater than about 97% by weight of one stereoisomer of the compound and less than about 3% by weight of the other stereoisomers of the compound. See, e.g., U.S. Pat. No. 7,189,715.
[0044] “R” and “S” as terms describing isomers are descriptors of the stereochemical configuration at an asymmetrically substituted carbon atom. The designation of an asymmetrically substituted carbon atom as “R” or “S” is done by application of the Cahn-Ingold-Prelog priority rules, as are well known to those skilled in the art, and described in the International Union of Pure and Applied Chemistry (IUPAC) Rules for the Nomenclature of Organic Chemistry. Section E, Stereochemistry.
[0045] “Enantiomeric excess” (ee) of an enantiomer is [(the mole fraction of the major enantiomer) minus (the mole fraction of the minor enantiomer)]×100.
[0046] “Stable”, as used herein, refers to compounds that are not substantially altered when subjected to conditions to allow for their production, detection, and preferably their recovery, purification, and use for one or more of the purposes disclosed herein. In some embodiments, a stable compound or chemically feasible compound is one that is not substantially altered when kept at a temperature of 40° C. or less, in the absence of moisture or other chemically reactive conditions, for at least a week.
[0047] “Refluxing” as used herein refers to a technique in which vapors from a boiling liquid are condensed and returned to the mixture from which it came, typically by boiling the liquid in a vessel attached to a condenser.
[0048] “Powdered iron” or “iron powder” is iron having an average particle size of less than 0.1, 0.5, 1, 5, 10, 20, 50, 250, 500 or 1000 μm. Particle size can be measured using methods known in the art, e.g., mesh sizing, laser diffraction, etc.
[0049] “Zinc dust” is zinc having an average particle size of less than 0.001, 0.05, 0.1, 0.5, 1, 5, 10, 15 or 20 μm. “Zinc powder” is zinc having an average particle size of less than 200, 175, 150, 125, or 100 μm. Particle size can be measured using methods known in the art, e.g., mesh sizing, laser diffraction, etc.
[0050] An “organic” compound as used herein is a compound that contains carbon. Similarly, an “organic solvent” is a compound containing carbon that is useful as a solvent. An “inorganic” compound is a compound not containing carbon.
[0051] “Mineral acid” as used herein is the acid of an inorganic compound. Examples include, but are not limited to, hydrochloric acid (HCl), nitric acid (HNO 3 ), phosphoric acid (H 3 PO 4 ), sulfuric acid (H 2 SO 4 ), boric acid (B(OH) 3 ), hydrofluoric acid (HF), hydrobromic acid (HBr), perchoric acid (HClO 4 ), etc.
[0052] A “hydrocarbon” is an organic compound consisting of carbon and hydrogen atoms. Examples of hydrocarbons useful as “hydrocarbon solvents” include, but are not limited to, an “aromatic hydrocarbon solvent” such as benzene, toluene, xylenes, etc., and an “aliphatic hydrocarbon solvent” such as pentane, hexane, heptane, etc.
[0053] An “amine” or “amine base” as used herein refers to an organic compound having a basic nitrogen atom (R—NR′R″), and may be a primary (R—NH 2 ), secondary (R—NHR′) or tertiary (R—NR′R″) amine.
[0054] A “strong base” as used herein is a compound that is capable of deprotonating very weak acids. Examples of strong bases include, but are not limited to, hydroxides, alkoxides, and ammonia.
[0055] A “hydroxide” is the commonly known diatomic anion OH − , or a salt thereof (typically an alkali metal or alkaline earth metal salt thereof). Examples of hydroxides include, but are not limited to, sodium hydroxide (NaCl), potassium hydroxide (KOH), lithium hydroxide (LiOH), and calcium hydroxide (CaOH).
[0056] An “alkoxide” is RO − , the conjugate base of an alcohol. Examples include, but are not limited to, methoxide, ethoxide, and propoxide.
[0057] “Ar” or “aryl” refer to an aromatic carbocyclic moiety having one or more closed rings. Examples include, without limitation, phenyl, naphthyl, anthracenyl, phenanthracenyl, biphenyl, and pyrenyl.
[0058] “Heteroaryl” refers to a cyclic moiety having one or more closed rings, with one or more heteroatoms (for example, oxygen, nitrogen or sulfur) in at least one of the rings, wherein at least one of the rings is aromatic, and wherein the ring or rings may independently be fused, and/or bridged. Examples include, without limitation phenyl, thiophenyl, triazolyl, pyridinyl, pyrimidinyl, pyridazinyl, pyrazinyl, quinolinyl, isoquinolinyl, indolyl, furyl, thienyl, pyrazolyl, quinoxalinyl, pyrrolyl, indazolyl, thieno[2,3-c]pyrazolyl, benzofuryl, pyrazolo[1,5-a]pyridyl, thiophenylpyrazolyl, benzothienyl, benzothiazolyl, thiazolyl, 2-phenylthiazolyl, and isoxazolyl.
[0059] “Alkyl” or “alkyl group,” as used herein, means a straight-chain (i.e., unbranched), branched, or cyclic hydrocarbon chain that is completely saturated. In some embodiments, alkyl groups contain 1, 2, or 3, to 4, 5, 6, 7, or 8 carbon atoms (e.g., C 1-4 , C 2-4 , C 3-4 , C 1-5 , C 2-5 , C 3-5 , C 1-6 , C 2-6 , C 3-6 , C 2-7 , C 1- , C 4-8 , etc.). In some embodiments, alkyl groups contain 1-8 carbon atoms. In certain embodiments, alkyl groups contain 1-6 carbon atoms. In still other embodiments, alkyl groups contain 2-3 carbon atoms, and in yet other embodiments alkyl groups contain 1-4 carbon atoms. In certain embodiments, the term “alkyl” or “alkyl group” refers to a cycloalkyl group, also known as carbocycle. Non-limiting examples of exemplary alkyl groups include methyl, ethyl, propyl, isopropyl, butyl, cyclopropyl and cyclohexyl.
[0060] “Alkenyl” or “alkenyl group,” as used herein, refers to a straight-chain (i.e., unbranched), branched, or cyclic hydrocarbon chain that has one or more double bonds. In certain embodiments, alkenyl groups contain 1-8 carbon atoms. In certain embodiments, alkenyl groups contain 1-6 carbon atoms. In still other embodiments, alkenyl groups contain 1-4 carbon atoms, and in yet other embodiments alkenyl groups contain 2-3 carbon atoms. According to another aspect, the term alkenyl refers to a straight chain hydrocarbon having two double bonds, also referred to as “diene.” In other embodiments, the term “alkenyl” or “alkenyl group” refers to a cycloalkenyl group. Non-limiting examples of exemplary alkenyl groups include —CH═CH 2 , —CH 2 CH═CH 2 (also referred to as allyl), —CH═CH 3 , —CH 2 CH═CH═CH 2 , —CH 2 CH═CHCH 3 , —CH═CH 2 CH 2 CH 3 , —CH═CH 2 CH═CH 2 , and cyclobutenyl.
[0061] “Alkoxy”, or “alkylthio”, as used herein, refers to an alkyl group, as previously defined, attached to the principal carbon chain through an oxygen (“alkoxy”) or sulfur (“alkylthio”) atom.
[0062] “Methylene”, “ethylene”, and “propylene” as used herein refer to the bivalent moieties —CH 2 —, —CH 2 CH 2 —, and —CH 2 CH 2 CH 2 —, respectively.
[0063] “Ethenylene”, “propenylene”, and “butenylene” as used herein refer to the bivalent moieties —CH═CH—, —CH═CHCH 2 —, —CH 2 CH═CH—, —CH═CHCH 2 CH 2 —, —CH 2 CH═CH 2 CH 2 —, and —CH 2 CH 2 CH═CH—, where each ethenylene, propenylene, and butenylene group can be in the cis or trans configuration. In certain embodiments, an ethenylene, propenylene, or butenylene group can be in the trans configuration.
[0064] “Alkylidene” refers to a bivalent hydrocarbon group formed by mono or dialkyl substitution of methylene. In certain embodiments, an alkylidene group has 1-6 carbon atoms. In other embodiments, an alkylidene group has 2-6, 1-5, 2-4, or 1-3 carbon atoms. Such groups include propylidene (CH 3 CH 2 CH═), ethylidene (CH 3 CH═), and isopropylidene (CH 3 (CH 3 )CH═), and the like.
[0065] “Alkenylidene” refers to a bivalent hydrocarbon group having one or more double bonds formed by mono or dialkenyl substitution of methylene. In certain embodiments, an alkenylidene group has 2-6 carbon atoms. In other embodiments, an alkenylidene group has 2-6, 2-5, 2-4, or 2-3 carbon atoms. According to one aspect, an alkenylidene has two double bonds. Exemplary alkenylidene groups include CH 3 CH═C═, CH 2 ═CHCH═, CH 2 ═CHCH 2 CH═, and CH 2 ═CHCH 2 CH═CHCH═.
[0066] “C 1-6 alkyl ester or amide” refers to a C 1-6 alkyl ester or a C 1-6 alkyl amide where each C 1-6 alkyl group is as defined above. Such C 1-6 alkyl ester groups are of the formula (C 1-6 alkyl)OC(═O)— or (C 1-6 alkyl)C(═O)O—. Such C 1-6 alkyl amide groups are of the formula (C 1-6 alkyl)NHC(═O)— or (C 1-6 alkyl)C(═O)NH—.
[0067] “C 2-6 alkenyl ester or amide” refers to a C 2-6 alkenyl ester or a C 2-6 alkenyl amide where each C 2-6 alkenyl group is as defined above. Such C 2-6 alkenyl ester groups are of the formula (C 2-6 alkenyl)OC(═O)— or (C 2-6 alkenyl)C(═O)O—. Such C 2-6 alkenyl amide groups are of the formula (C 2-6 alkenyl)NHC(═O)— or (C 2-6 alkenyl)C(═O)NH—.
[0068] “Halo” refers to fluoro, chloro, bromo or iodo.
[0069] “Haloalkyl” refers to an alkyl group substituted with one or more halo atoms (e.g., fluoro, chloro, bromo, and/or iodo atoms). For example, “fluoromethyl” refers to a methyl group substituted with one or more fluoro atoms (e.g., monofluoromethyl, difluoromethyl, and trifluoromethyl).
[0070] “Hydroxyalkyl” refers to an alkyl group substituted with a hydroxyl group (—OH).
[0071] “Fluoromethoxy” as used herein, refers to a fluoromethyl group, as previously defined, attached to the principal carbon chain through an oxygen atom.
[0072] “Protecting group” as used herein, is meant that a particular functional moiety, e.g., O, S, or N, is temporarily blocked so that a reaction can be carried out selectively at another reactive site in a multifunctional compound. For example, in certain embodiments, as detailed herein, certain exemplary oxygen protecting groups are utilized. Oxygen protecting groups include, but are not limited to, groups bonded to the oxygen to form an ether, such as methyl, substituted methyl (e.g., Trt (triphenylmethyl), MOM (methoxymethyl), MTM (methylthiomethyl), BOM (benzyloxymethyl), PMBM or MPM (p-methoxybenzyloxymethyl)), substituted ethyl (e.g., 2-(trimethylsilyl)ethyl), benzyl, substituted benzyl (e.g., para-methoxybenzyl), silyl (e.g., TMS (trimethylsilyl), TES (triethylsilyl), TIPS (triisopropylsilyl), TBDMS (t-butyldimethylsilyl), tribenzylsilyl, TBDPS (t-butyldiphenyl silyl), 2-trimethylsilylprop-2-enyl, t-butyl, tetrahydropyranyl, allyl, etc.
[0073] In some embodiments, a compound of the present invention may be provided as a salt, such as a pharmaceutically acceptable salt. Pharmaceutically acceptable salts are salts that retain the desired biological activity of the parent compound and do not impart undesired toxicological effects. Specific examples of pharmaceutically acceptable salts include inorganic acid salts (such as sulfates, nitrates, perchlorates, phosphates, carbonates, bicarbonates, hydrofluorides, hydrochlorides, hydrobromides and hydroiodides), organic carboxylates (such as acetates, oxalates, maleates, tartrates, fumarates and citrates), organic sulfonates (such as methanesulfonates, trifluoromethanesulfonates, ethanesulfonates, benzenesulfonates, toluenesulfonates and camphorsulfonates), amino acid salts (such as aspartates and glutamates), quaternary amine salts, alkali metal salts (such as sodium salts and potassium salts) and alkali earth metal salts (such as magnesium salts and calcium salts).
[0074] Unless indicated otherwise, nomenclature used to describe chemical groups or moieties as used herein follow the convention where, reading the name from left to right, the point of attachment to the rest of the molecule is at the right-hand side of the name. For example, the group “(C 1-3 alkoxy)C 1-3 alkyl,” is attached to the rest of the molecule at the alkyl end. Further examples include methoxyethyl, where the point of attachment is at the ethyl end, and methylamino, where the point of attachment is at the amine end.
[0075] Unless indicated otherwise, where a mono or bivalent group is described by its chemical formula, including one or two terminal bond moieties indicated by “-,” it will be understood that the attachment is read from left to right.
[0076] Unless otherwise stated, structures depicted herein are meant to include all enantiomeric, diastereomeric, and geometric (or conformational) forms of the structure; for example, the R and S configurations for each asymmetric center, (Z) and (E) double bond isomers, and (Z) and (E) conformational isomers. Therefore, single stereochemical isomers as well as enantiomeric, diastereomeric, and geometric (or conformational) mixtures of the present compounds are within the scope of the invention. Unless otherwise stated, all tautomeric forms of the compounds of the invention are within the scope of the invention.
[0077] Additionally, unless otherwise stated, structures depicted herein are also meant to include compounds that differ only in the presence of one or more isotopically enriched atoms. For example, compounds having the present structures except for the replacement of hydrogen by deuterium or tritium, or the replacement of a carbon by a 3 C- or 14 C-enriched carbon are within the scope of this invention. Such compounds are useful, for example, as analytical tools or probes in biological assays.
[0078] Provided herein according to some embodiments is a compound of Formula 1′:
[0000]
[0000] wherein:
[0079] R is hydrogen or —C(O)R 1 , and
[0080] R 1 is selected from the group consisting of C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl, and heteroaryl, R 1 may be unsubstituted or substituted from 1 to 3 times with independently selected C 1 -C 6 alkyl, hydroxy, hydroxyC 1 -C 6 alkyl, methoxy, methoxyC 1 -C 6 alkyl, halo, haloC 1 -C 6 alkyl, —C(O)NH 2 , —NHCOOC 1 -C 6 alkyl, or —COOH group(s);
[0081] or a salt thereof.
[0082] In some embodiments, a compound of Formula 1′ has the stereochemistry of Formula 1A′:
[0000]
[0083] In some embodiments, a compound of Formula I has the stereochemistry of Formula IB:
[0000]
[0084] According to some embodiments, R in a compound of Formula 1′ is a hydrogen and the compound has a structure of Formula 1:
[0000]
[0085] or a salt thereof.
[0086] In some embodiments, a compound of Formula 1 has the stereochemistry of Formula 1A:
[0000]
[0087] In some embodiments, a compound of Formula 1 has the stereochemistry of Formula 1B:
[0000]
[0088] According to some embodiments, R in a compound of Formula 1′ is —C(O)R 1 or a salt thereof. In certain embodiments, in a compound of Formula 1′, R is —C(O)R 1 and R 1 is substituted with —COOH, or a salt thereof.
[0089] Provided according to further embodiments of the present invention is a compound of Formula 2:
[0000]
[0000] or a salt thereof.
[0090] In some embodiments, a compound of Formula 2 has the stereochemistry of Formula 2A:
[0000]
[0091] In some embodiments, a compound of Formula 2 has the stereochemistry of Formula 2B:
[0000]
[0092] In some embodiments, a process for preparing a compound of Formula 1 is provided. The process may comprise reacting 6,8-dimethyl-3,9-dioxatricyclo[3.3.1.0 2,4 ]nonan-7-one with a reducing agent to form an intermediate having the following structure:
[0000]
[0000] reacting the intermediate with an acid to form the compound of Formula 1.
[0093] Exemplary reducing agents that may be used in preparing a compound of Formula 1 include, but are not limited to, hydrides, such as sodium borohydride, potassium borohydride, lithium borohydride, lithium aluminum hydride, and sodium cyanoborohydride. In some embodiments, the reducing agent may be sodium borohydride.
[0094] Exemplary acids that may be used in preparing a compound of Formula 1 include, but are not limited to, hydrochloric acid, hydrofluoric acid, hydrobromic acid, hydroiodic acid, sulfuric acid, nitric acid, citric acid, glycolic acid, formic acid, oxalic acid, boric acid, and/or acetic acid. In some embodiments, the acid may be hydrochloric acid.
[0095] According to some embodiments, a process for resolving enantiomers of the compound of Formula 1 is provided. The process may be a process for resolving a mixture of compounds of Formulas 1A and 1B. In some embodiments, the resolution compounds of Formulas 1A and 1B may be achieved by selective crystallization and/or selective precipitation of a mixture of diastereomeric salts of Formulas 1A and 1B. In some embodiments, the mixture of diastereomeric salts of Formulas 1A and 1B may be obtained by forming a mixture of esters of Formulas 1A and 1B having free carboxylate groups, and then by treating the mixture of esters of Formulas 1A and 1B having free carboxylate groups with a chiral amine-containing compound (i.e., a chiral amine), such as, for example, α-methylbenzylamine.
[0096] In some embodiments, a process for resolving enantiomers of the compound of Formula I may comprise reacting the racemic compound of Formula 1:
[0000]
[0000] with phthalic anhydride to form a racemic mixture of phthalates of Formulas 2A and 2A:
[0000]
[0000] The racemic mixture of phthalates of Formula 2 may be reacted with a first chiral amine in a solvent to form a pair of diastereomeric salts thereof in a solution, and a first diastereomeric salt of the pair of diastereomeric salts may be precipitated from the solution to provide an isolated first diastereomeric salt and an second diastereomeric salt. Enantiomers of the compound of Formula 1 may then be formed from the isolated first diastereomeric salt and the second diastereomeric salt, thereby resolving the enantiomers of the compound of Formula 1.
[0097] In some embodiments, prior to reacting the racemic mixture of phthalates of Formula 2 with the first chiral amine in the solvent to form the pair of diastereomeric salts thereof in the solution, the racemic mixture of phthalates of Formula 2 may be dissolved in the solvent. In some embodiments, the racemic mixture of phthalates of Formula 2 may be dissolved in the solvent at a volume ratio in a range of about 1:12 to about 1:20 (phthalates:solvent), such as, but not limited to, at a volume ratio of about 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, or 1:20. In some embodiments, the volume ratio may be about 1:15. In some embodiments, the solvent may be acetone.
[0098] In some embodiments, the first chiral amine is (S)-α-methylbenzylamine. Reacting (S)-α-methylbenzylamine with the racemic mixture of phthalates of Formula 2 in a solvent may precipitate the first diastereomeric salt of the pair of diastereomeric salts from the solution, thereby providing the isolated first diastereomeric salt. In some embodiments, the isolated first diastereomeric salt may have the following structure of Formula 2B′:
[0000]
[0099] In some embodiments, a process for resolving enantiomers of the compound of Formula 1 may comprise treating the isolated first diastereomeric salt with a base to form a first enantiomeric compound of Formula 1. Exemplary bases include, but are not limited to, sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide, cesium hydroxide, and/or alkoxides, such as, for example sodium, potassium, and/or lithium methoxide, ethoxide, propoxide, and/or n-butoxide. In some embodiments, the isolated first diastereomeric salt may be a compound of Formula 2B′ and the first enantiomeric compound of Formula 1 may be a compound of Formula 1B having the following structure:
[0000]
[0000] or a salt thereof. The first diastereomeric salt may be in crystalline form. Accordingly, the process may comprise one or more crystallization steps (e.g., crystallizing and/or recrystallizing steps).
[0100] In some embodiments, a process for resolving enantiomers of the compound of Formula 1 may comprise separating the first diastereomeric salt from the solution to separately provide the isolated first diastereomeric salt and the second diastereomeric salt. Exemplary methods of separating will be known to those of skill in the art and include, but are not limited to, filtering the solution to separately provide the isolated first diastereomeric salt and the second diastereomeric salt.
[0101] A process for resolving enantiomers of the compound of Formula 1 may comprise acidifying the second diastereomeric salt to form a free phthalate. The second diastereomeric salt may have the following structure of Formula 2A′:
[0000]
[0000] The free phthalate may be reacted with a second chiral amine to reform the second diastereomeric salt in a solution. In some embodiments, the second chiral amine is (R)-α-methylbenzylamine. The second diastereomeric salt may be precipitated from the solution to form an isolated second diastereomeric salt. In some embodiments, the isolated second diastereomeric salt may be a compound of Formula 2A′. A second enantiomeric compound of Formula 1 may be from the isolated second diastereomeric salt.
[0102] In some embodiments, prior to reacting the free phthalate with the second chiral amine to reform the second diastereomeric salt in the solution, the free phthalate may be dissolved in a solvent. In some embodiments, the free phthalate may be dissolved in the solvent at a volume ratio in a range of about 1:12 to about 1:20 (phthalate:solvent), such as, but not limited to, at a volume ratio of about 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, or 1:20. In some embodiments, the volume ratio may be about 1:15. In some embodiments, the solvent may be acetone.
[0103] In some embodiments, a process for resolving enantiomers of the compound of Formula 1 may comprise treating the isolated second diastereomeric salt with a base to form a second enantiomeric compound of Formula 1. Exemplary bases include, but are not limited to, sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide, cesium hydroxide, and/or alkoxides, such as, for example sodium, potassium, and/or lithium methoxide, ethoxide, propoxide, and/or n-butoxide. In some embodiments, the isolated second diastereomeric salt may be a compound of Formula 2A′ and the second enantiomeric compound of Formula 1 may be a compound of Formula 1A having the following structure:
[0000]
[0104] In some embodiments, the second diastereomeric salt may be in crystalline form. Accordingly, the process may comprise one or more crystallization steps (e.g., crystallizing and/or recrystallizing steps).
[0105] Provided according to further embodiments of the present invention is a compound of Formula I having the structure:
[0000]
[0106] In some embodiments, a compound of Formula I may have the stereochemistry of a compound of Formula Ia:
[0000]
[0107] In some embodiments, a compound of Formula I may have the stereochemistry of a compound of Formula Ib:
[0000]
[0108] According to some embodiments, a process for preparing a compound of Formula I may be provided. The process may comprise treating a compound of Formula 1:
[0000]
[0000] with an oxidizing agent to form the compound of Formula I. Exemplary oxidizing agents include, but are not limited to, peracetic acid, perbenzoic acid, m-chloroperbenzoic acid, perphthalic acid, performic acid, trifluoroperacetic acid, sulfur trioxide pyridine complex, hydrogen peroxide, pyridinium dichromate (PDC), and/or pyridinium chlorochromate (PCC). In some embodiments, the oxidizing agent may be m-chloroperbenzoic acid. In some embodiments, the oxidizing agent may be a sulfur trioxide pyridine complex.
[0109] A catalyst may optionally be present during the treatment of a compound of Formula 1 with an oxidizing agent to form a compound of Formula I. Exemplary catalysts include, but are not limited to, 2,2,6,6-tetramethyl-1-piperidinyloxy, 4-hydroxy-2,2,6,6-tetramethyl-1-piperidinyloxy, 4-(2-chloroacetamido)-2,2,6,6-tetramethyl-1-piperidinyloxy, and/or 4-(acetylamino)-2,2,6,6-tetramethyl-piperidinyloxy. In some embodiments, the catalyst may be 2,2,6,6-tetramethyl-1-piperidinyloxy. In certain embodiments, the catalyst may be 2,2,6,6-tetramethyl-1-piperidinyloxy and the oxidizing agent may be m-chloroperbenzoic acid.
[0110] In some embodiments, a process for preparing a compound of Formula I may form an intermediate ketone having the following structure of Formula Ia″:
[0000]
[0111] In some embodiments, a process for preparing a compound of Formula I may form an intermediate ketone having the following structure of Formula Ib″:
[0000]
[0112] In some embodiments, a compound of Formula 1 may be reacted with an oxidizing agent, such as, for example, a sulfur trioxide pyridine complex, to form the intermediate ketone of Formula Ia″ and/or Formula Ib″. The intermediate ketone of Formula Ia″ and/or Formula Ib″ may be then reacted with an oxidizing agent, such as, for example, m-chloroperbenzoic acid, optionally in the presence of a catalyst.
[0113] In some embodiments, a process for preparing a compound of Formula I may comprise treating a compound of Formula 1a:
[0000]
[0000] with an oxidizing agent, optionally in the presence of a catalyst, to form a compound of Formula Ia:
[0000]
[0114] In some embodiments, a process for preparing a compound of Formula I may comprise treating a compound of Formula 1b:
[0000]
[0000] with an oxidizing agent, optionally in the presence of a catalyst, to form a compound of Formula Ib:
[0000]
[0115] According to some embodiments, provided is a compound of Formula II′, III′, IV′, V′, VI′, and/or VII′ having the following structure:
[0000]
[0116] wherein:
[0117] Ph is phenyl; and
[0118] R 3 is each independently a hydrogen or an oxygen protecting group;
[0119] or a salt thereof.
[0120] In some embodiments, at least one R 3 is hydrogen in a compound of Formula II, III′, IV′, V′, VI′, or VII′. In some embodiments, at least one R 3 is an oxygen protecting group in a compound of Formula II′, III′, IV′, V′, VI′, or VII′. In some embodiments, at least one R 3 is hydrogen and at least one R 3 is an oxygen protecting group in a compound of Formula II′, III′, IV′, V′, VI′, or VII′. In some embodiments, two or more R 3 are hydrogen in a compound of Formula II′, III′, IV′, V′, VI′, or VII′. In some embodiments, two or more R 3 are an oxygen protecting group that may be the same as or different than another R 3 in a compound of Formula II′, III′, IV′, V′, VI′, or VII′. In certain embodiments, all R 3 are hydrogen in a compound of Formula II′, III′, IV′, V′, VI′, or VII′. In certain embodiments, all R 3 are an oxygen protecting group that may be the same as or different than another R 3 in a compound of Formula II, III′, IV′, V′, VI′, or VII′.
[0121] Exemplary oxygen protecting groups include, but are not limited to, those described herein, such as Trt (triphenylmethyl), MOM (methoxymethyl), MTM (methylthiomethyl), BOM (benzyloxymethyl), PMBM or MPM (p-methoxybenzyloxymethyl)), substituted ethyl (e.g., 2-(trimethylsilyl)ethyl), benzyl, substituted benzyl (e.g., para-methoxybenzyl), silyl (e.g., TMS (trimethylsilyl), TES (triethylsilyl), TIPS (triisopropylsilyl), TBDMS (t-butyldimethylsilyl), tribenzylsilyl, TBDPS (t-butyldiphenyl silyl), 2-trimethylsilylprop-2-enyl, t-butyl, tetrahydropyranyl, and/or allyl. In some embodiments, the oxygen protecting group is triethylsilyl (TES).
[0122] In some embodiments, provided is a compound of Formula II, III, IV, V, VI, and/or VII having the following structure:
[0000]
[0123] Provided in some embodiments is a method for preparing a compound of Formula II′, II, III′, III, IV′, IV, V′, V, VI′, VI, VII′, and/or VII. Described below are exemplary processes for preparing a compound of Formula II, III, IV, V, VI, and VII. As those skilled in the art will readily appreciate the exemplary processes may be modified, such as by not removing the oxygen protecting group to prepare a compound of Formula II′, III′, IV′, V′, VI′, or VII′. Exemplary reducing agents and oxygen protecting that may be used in a method for preparing a compound of Formula II′, II, III′, III, IV′, IV, V′, V, VI′, VI, VII′, and/or VII include those described herein.
[0124] In some embodiments, a process for preparing a compound of Formula IV is provided. A process for preparing a compound of Formula IV may comprise providing a mixture of a dialkyl((arylsulfonyl)methyl)phosphonate and a compound of Formula I having the stereochemistry of a compound of Formula Ia:
[0000]
[0125] reacting the mixture with an alkoxide in a polar protic solvent to form a compound of Formula AAAA having the structure:
[0000]
[0126] reducing the compound of Formula AAAA in the presence of a catalyst to form a compound of Formula BBBB having the structure:
[0000]
[0127] reacting the compound of Formula BBBB with an oxygen protecting group to form a protected ester;
[0128] reacting the protected ester with a reducing agent to form a protected alcohol;
[0129] reacting the protected alcohol with a halogen to form a halogenated compound;
[0130] dehalogenating the halogenated compound to form a compound of Formula KKKK having the structure:
[0000]
[0131] wherein:
[0132] Ph is a phenyl group; and
[0133] R 2 is an oxygen protecting group; and
[0134] removing the oxygen protecting group of the compound of Formula KKKK to form the compound of Formula IV.
[0135] In some embodiments, a process for preparing a compound of Formula III may be provided. A process for preparing a compound of Formula III may comprise providing a mixture of a dialkyl((arylsulfonyl)methyl)phosphonate and a compound of Formula I having the stereochemistry of a compound of Formula Ia:
[0000]
[0136] reacting the mixture with an alkoxide in a polar protic solvent to form a compound of Formula AAAA having the structure:
[0000]
[0137] reacting the compound of Formula AAAA with an oxygen protecting group to form a protected ester;
[0138] reacting the protected ester with a reducing agent to form a protected alcohol;
[0139] reacting the protected alcohol with a halogen to form a halogenated compound;
[0140] dehalogenating the halogenated compound to form a compound of Formula LLLL having the structure:
[0000]
[0141] wherein:
[0142] Ph is a phenyl group; and
[0143] R 2 is an oxygen protecting group; and
[0144] reacting the compound of Formula LLLL with a methyllithium-lithium bromide complex to form the compound of Formula III.
[0145] In some embodiments, a process for preparing a compound of Formula II may be provided. A process for preparing a compound of Formula II may comprise providing a mixture of a dialkyl((arylsulfonyl)methyl)phosphonate and a compound of Formula I having the stereochemistry of a compound of Formula Ia:
[0000]
[0146] reacting the mixture with an alkoxide in a polar protic solvent to form a compound of Formula AAAA having the structure:
[0000]
[0147] reacting the compound of Formula AAAA with an oxygen protecting group to form a protected ester;
[0148] reacting the protected ester with a reducing agent to form a protected alcohol;
[0149] reacting the protected alcohol with a halogen to form a halogenated compound;
[0150] dehalogenating the halogenated compound to form a compound of Formula LLLL having the structure:
[0000]
[0151] wherein:
[0152] Ph is a phenyl group; and
[0153] R 2 is an oxygen protecting group; and
[0154] reacting the compound of Formula LLLL with methyllithium in the presence of copper to form the compound of Formula II.
[0155] In some embodiments, a process for preparing a compound of Formula VII may be provided. A process for preparing a compound of Formula VII may comprise providing a mixture of a dialkyl((arylsulfonyl)methyl)phosphonate and a compound of Formula I having the stereochemistry of a compound of Formula Ib:
[0000]
[0156] reacting the mixture with an alkoxide in a polar protic solvent to form a compound of Formula MMMM having the structure:
[0000]
[0157] reducing the compound of Formula MMMM in the presence of a catalyst to form a compound of Formula NNNN having the structure:
[0000]
[0158] reacting the compound of Formula NNNN with an oxygen protecting group to form a protected ester;
[0159] reacting the protected ester with a reducing agent to form a protected alcohol;
[0160] reacting the protected alcohol with a halogen to form a halogenated compound;
[0161] dehalogenating the halogenated compound to form a compound of Formula OOOO having the structure:
[0000]
[0162] wherein:
[0163] Ph is a phenyl group; and
[0164] R 2 is an oxygen protecting group; and
[0165] removing the oxygen protecting group of the compound of Formula OOOO to form the compound of Formula VII.
[0166] In some embodiments, a process for preparing a compound of Formula VI may be provided. A process for preparing a compound of Formula VI may comprise providing a mixture of a dialkyl((arylsulfonyl)methyl)phosphonate and a compound of Formula I having the stereochemistry of a compound of Formula Ib:
[0000]
[0167] reacting the mixture with an alkoxide in a polar protic solvent to form a compound of Formula MMMM having the structure:
[0000]
[0168] reacting the compound of Formula MMMM with an oxygen protecting group to form a protected ester;
[0169] reacting the protected ester with a reducing agent to form a protected alcohol;
[0170] reacting the protected alcohol with a halogen to form a halogenated compound;
[0171] dehalogenating the halogenated compound to form a compound of Formula PPPP having the structure:
[0000]
[0172] wherein:
[0173] Ph is a phenyl group; and
[0174] R 2 is an oxygen protecting group; and
[0175] reacting the compound of Formula PPPP with a methyllithium-lithium bromide complex to form the compound of Formula VI.
[0176] In some embodiments, a process for preparing a compound of Formula V may be provided. A process for preparing a compound of Formula V may comprise providing a mixture of a dialkyl((arylsulfonyl)methyl)phosphonate and a compound of Formula I having the stereochemistry of a compound of Formula Ib:
[0000]
[0177] reacting the mixture with an alkoxide in a polar protic solvent to form a compound of Formula MMMM having the structure:
[0000]
[0178] reacting the compound of Formula MMMM with an oxygen protecting group to form a protected ester;
[0179] reacting the protected ester with a reducing agent to form a protected alcohol;
[0180] reacting the protected alcohol with a halogen to form a halogenated compound;
[0181] dehalogenating the halogenated compound to form a compound of Formula PPPP having the structure:
[0000]
[0182] wherein:
[0183] Ph is a phenyl group; and
[0184] R 2 is an oxygen protecting group; and
[0185] reacting the compound of Formula PPPP with methyllithium in the presence of copper to form the compound of Formula V.
[0186] Any suitable dialkyl((arylsulfonyl)methyl)phosphonate may be used in a process for preparing a compound of Formula II, III, IV, V, VI, or VII. In some embodiments, in a process for preparing a compound of Formula II, III, IV, V, VI, or VII, the dialkyl((arylsulfonyl)methyl)phosphonate may be dimethyl((phenylsulfonyl)methylphosphonate.
[0187] In some embodiments, in a process for preparing a compound of Formula II, III, IV, V, VI, or VII, the alkoxide may be present in an excess of about 2 to about 3 equivalents, such as, for example, in an excess of about 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, or 3 equivalents. Any suitable alkoxide may be used in a process for preparing a compound of Formula II, III, IV, V, VI, or VII. In some embodiments, the alkoxide is a sodium alkoxide, such as, but not limited to, sodium methoxide and sodium ethoxide.
[0188] Any suitable polar protic solvent may be used in a process for preparing a compound of Formula II, III, IV, V, VI, or VII. In some embodiments, in a process for preparing a compound of Formula II, III, IV, V, VI, or VII, the polar protic solvent is an alcohol, such as, but not limited to, methanol and ethanol. Any suitable alcohol may be used in a process for preparing a compound of Formula II, III, IV, V, VI, or VII. In some embodiments, the polar protic solvent and alkoxide used in a process for preparing a compound of Formula II, III, IV, V, VI, or VII may be compatible. For example, in some embodiments, the alkoxide may be sodium methoxide and the polar protic solvent may be methanol.
[0189] According to some embodiments of the present invention, a method of using a compound of Formula II′, III′, IV′, V′, VI′, and/or VII′ is provided. In some embodiments, a method of using a compound of Formula II, I, IV, V, VI, and/or VII is provided.
[0190] In some embodiments, a compound of Formula II′, III′, IV′, V′, VI′, and/or VII′ may be used to prepare a natural product or an intermediate thereof. In some embodiments, a compound of Formula II, III, IV, V, VI, and/or VII may be used to prepare a natural product or an intermediate thereof. Exemplary natural products include, but are not limited to, spirangien A, spirangien B, dolabriferol, scytophycin C, zincophorin, stigmatellin, rifamycin SV, tirandamycin A, aplyronine A, aplyronine E, reidispongioloide, misakinolide, and/or mycarolide. FIG. 1 illustrates exemplary natural products and indicates areas (i.e., the boxed areas) that are consistent with a compound of Formula II or IV and/or in which a compound of Formula II or IV may be used to prepare that portion of the natural product Thus, a compound of Formula II or IV may be used to prepare the shown natural products or intermediates thereof.
[0191] In some embodiments, a compound described herein, or a salt thereof, may be useful in a method of synthesizing a fused aminodihydrothiazine derivative. In some embodiments, the compound may be a compound of Formula II′, II, III′, III, IV′, IV, V′, V, VI, VI, VII′, and/or VII.
[0192] In some embodiments, a compound described herein, or salt thereof, may be used to prepare a combinatorial library. In some embodiments, a compound of Formula II′, III′, IV′, V′, VI′, and/or VII′ may be used to prepare a combinatorial library. In some embodiments, a compound of Formula II, III, IV, V, VI, and/or VII may be used to prepare a combinatorial library.
[0193] In order that the invention described herein may be more fully understood, the following examples are set forth. It should be understood that these examples are for illustrative purposes only and are not to be construed as limiting this invention in any manner.
Examples
[0194] General:
[0195] Column chromatography was carried out using Biotage SP4. Solvent removal was carried out using either a Btlchii rotary evaporator or a Genevac centrifugal evaporator. Preparative LC/MS was conducted using a Waters autopurifier and 19×100 mm XTerra 5 micron MS C18 column under acidic mobile phase condition. NMR spectra were recorded using Varian 400 MHz spectrometer.
[0196] When the term “inerted” is used to describe a reactor (e.g., a reaction vessel, flask, glass reactor, and the like) it is meant that the air in the reactor has been replaced with an essentially moisture-free or dry, inert gas (such as nitrogen, argon, and the like). The term “equivalent” (abbreviation: eq) as used herein describes the stoichiometry (molar ratio) of a reagent or a reacting compound by comparison to a pre-established starting material. The term “weight” (abbreviation: wt) as used herein corresponds to the ratio of the mass of a substance or a group of substances by comparison to the mass of a particular chemical component of a reaction or purification specifically referenced in the examples below. The ratio is calculated as: g/g, or Kg/Kg. The term “volume” (abbreviation: vol) as used herein corresponds to the ratio of the volume of a given substance or a group of substances to the mass or volume of a pre-established chemical component of a reaction or purification. The units used in the equation involve matching orders of magnitude. For example, a ratio is calculated as: mL/mL, mL/g, L/L or L/Kg.
[0197] General methods and experimentals for preparing compounds of the present invention are set forth below. In certain cases, a particular compound is described by way of example. However, it will be appreciated that in each case a series of compounds of the present invention were prepared in accordance with the schemes and experimentals described below.
[0198] The following abbreviations are used herein:
[0000]
Abbreviation
Definition
TMS
Trimethylsilyl
TBAF
Tetrabutylammonium fluoride
NaOH
Sodium hydroxide
Bu 4 N HSO 4
Tetrabutylammonium hydrogen sulfate
THF
Tetrahydrofuran
rt
Room temperature
h
Hour(s)
NaCl
Sodium chloride
HCOOH
Formic acid
V
Volumes
wt
Weights
CDI
1,1′-Carbonyldiimidazole
DCM
Dichloromethane
Aq
Aqueous
Sat.
Saturated
HCl
Hydrochloric acid
HRMS
High Resolution Mass Spectrometry
nBuLi
n-butyl lithium
NH 4 Cl
Ammonium chloride
MeOH
Methanol
EtOAc
Ethyl acetate
NaHCO 3
Sodium bicarbonate
M
Molar (moles/liter)
T
Temperature
MTBE
Methyl tert-butyl ether
TLC
Thin layer chromatography
N
Normal (equivalents per liter)
iPrMgBr
Isopropyl magnesium bromide
LiCl
Lithium chloride
NaOAc
Sodium acetate
NH 4 OH
Ammonium hydroxide
HPLC
High performance liquid chromatography
ee
Enantiomeric excess
DMI
1,3-Dimethyl-2-imidazolidinone
UV
Ultraviolet
RRT
Relative retention time
OROT
Optical rotation
Bz
Benzoyl
T3P ® (Archimica)
n-propyl phosphonic acid anhydride
Ph
Phenyl
TES
Triethylsilyl
[0199] A. Preparation of Compounds of Formula 1
[0200] Compounds of Formulas 1a and 1b were prepared as shown in Scheme 1.
[0000]
[0201] Synthesis and Resolution of Alcohols of Formulas 1a and 1b.
[0000]
(1R,2S,4R,5S)-2,4-Dimethyl-8-oxabicyclo[3.2.1]oct-6-en-3-one
[0202] To a 22 L reactor under nitrogen were charged acetonitrile (6.2 L) and sodium iodide (4420 g) at room temperature. While vigorously stirring, the suspension was treated with copper (969 g) and freshly distilled furan (1.47 L). Then, a solution of 2,4-dibromo-3-pentanone (1247 g) in acetonitrile (1.2 L) was added maintaining the internal temperature below 55° C. The resulting mixture was stirred at 45-50° C. for 4 h. After cooling to 20° C., the reaction was quenched with water (4 L) and MTBE (4 L), and the resulting mixture was stirred at 0° C. overnight. The resulting precipitate was filtered through celite 545 (2.4 kg) and sequentially washed with MTBE (1 L) and methylene chloride (4 L). The organic layer was separated from the filtrate, diluted with MTBE (1 L), and sequentially washed with 28% ammonium hydroxide (3.5 L) and a mixture of 28% ammonium hydroxide (3 L) and water (1 L). The organic layer was further diluted with MTBE (6.5 L), and sequentially washed with water (2 L, containing sodium chloride (25 g)), a mixture of 28% ammonium hydroxide (1.5 L) and water (1 L), and water (4 L). The first aqueous layer was back-extracted twice with a mixture of MTBE (3 L) and methylene chloride (3 L). The organic layers were combined, washed twice with a mixture of 28% ammonium hydroxide (2.5 L), water (1 L) and sodium chloride (25 g), and then washed with water (4 L). The yellow organic layer was concentrated under reduced pressure, and azeotroped with n-heptane (4 L). The residue was treated with n-heptane (4 L), concentrated down to ˜3 L, and stirred at −20° C. overnight. The resulting faint yellow solid was collected by vacuum filtration, washed with cold heptane (500 mL), and dried under vacuum overnight at room temperature to give the title compound (549 g, 71%). 1 H NMR (CDCl 3 , 400 MHz): δ 6.35 (s, 2H), 4.85 (d, 2H), 2.8 (m, 2H), 0.95 (d, 6H).
[0000]
(1R,2R,4S,5S,6S,8R)-6,8-dimethyl-3,9-dioxatricyclo[3.3.1.02,4]nonan-7-one
[0203] To a stirred solution of (1R,2S,4R,5S)-2,4-dimethyl-8-oxabicyclo[3.2.1]oct-6-en-3-one (1.06 kg) in 1,2-dichloroethane (10 L) at room temperature was added m-chloroperbenzoic acid (1.80 kg) in one portion. The resulting suspension was stirred under reflux (at 70-75° C.) for 5 h. More m-chloroperbenzoic acid (180 g) was added and stirring was continued for additional 3 h. The mixture was cooled to 0° C. and stirred at 0° C. overnight. The resulting precipitate was filtered and washed with methylene chloride (4 L). The filtrate was sequentially washed with 10 M sodium carbonate in water (7 L) and water (4 L). The organic layer was concentrated in vacuo and chased twice with n-heptane (2 L). The resulting pale yellow solid was dissolved in MTBE (2.5 L) by heating to 55° C., treated with n-heptane (0.8 L), and stood at −20° C. for 3 days. The precipitate was collected by vacuum filtration and washed with a 3:2 mixture of MTBE and n-heptane (750 mL) to give the title compound (1050 g, 90%) as a white solid. 1 H NMR (CDCl 3 , 400 MHz): δ 4.40 (t, 2H), 3.55 (t, 2H), 2.80 (m, 2H), 1.05 (d, 6H).
[0000]
Synthesis of rac-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-ol
[0204] To a cold (−15° C.) suspension of sodium borohydride (337 g) in methanol (4 L) in a 22 L reactor under nitrogen was carefully charged a solution of (1R,2R,4S,5S,6S,8R)-6,8-dimethyl-3,9-dioxatricyclo[3.3.1.02,4]nonan-7-one (1 kg) in a mixture of methanol (2 L) and methylene chloride (4 L) over 1.5 h maintaining the internal temperature below 0° C. The resulting mixture was stirred at −5-0° C. for 2 h. After quenching the reaction with water (160 mL), the mixture was concentrated under vacuum and chased with methylene chloride (2 L). The resulting solid was dissolved in methylene chloride (8 L) and washed with water (4 L). The aqueous layer was back-extracted with methylene chloride (4 L). The organic layers were combined, dried over anhydrous sodium sulfate and stood at 0° C. overnight. The sodium sulfate was removed by vacuum filtration and rinsed with methylene chloride (1 L).
[0205] The filtrate was treated with 5.5 M HCl in isopropyl alcohol (3 L) at 5° C. and stirred at 20-30° C. for 1 h. The reaction mixture was concentrated under vacuum at 30° C. and chased twice with toluene (2 L) to give the title compound (975 g, 96%) as a pale yellow solid. 1 H NMR (C 6 D 6 , 400 MHz): 4.30 (t, 1H), 4.10 (t, 1H), 4.00 (t, 1H), 3.75 (t, 1H), 3.15 (t, 1H), 2.45 (s, 1H), 1.85 (m, 1H), 1.45 (m, 1H), 0.60 (d, 3H), 0.55 (d, 3H).
[0000]
[0206] Synthesis of the Corresponding Phthalate of the Racemic Alcohol
[0207] rac-6,7-Dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-ol (970 g) was dissolved in a mixture of triethylamine (1.99 L) and toluene (2.1 L), treated with phthalic anhydride (925 g), and stirred at 70° C. for 2 h. The mixture was cooled to 10° C. and treated with 3 M hydrogen chloride in water (7 L) maintaining the temperature below 30° C. White solids began falling out of solution. The mixture was stirred at rt for an additional 20 min. The white solid product was then collected by vacuum filtration, washed with water (2 L), and dried under vacuum. The crude product was chased with toluene (4 L) and then heated in toluene (5.6 L) to 70° C. to obtain a clear solution. The solution was allowed to cool to 65° C. where solids began falling out of solution, and slowly cooled to rt overnight. The white solid product was collected by vacuum filtration, washed with toluene (1 L), and dried under vacuum. The product was recrystallized again in toluene (5.6 L) by heating to 75°, cooling to rt at a rate of 10° C. per hour, and stirring at rt overnight. Solids began falling out of solution at 65° C. The resulting precipitate was collected by vacuum filtration, washed with toluene (1 L), and dried under vacuum at 40° C. to give the title compound (1.65 kg, 91%) as a white solid. 1 H NMR analysis showed that there was 4% of the suspected equatorial by-product and approximately 4% of triethylamine salt present. 1 H NMR (CDCl 3 , 400 MHz): 7.80 (d, 1H), 7.65 (d, 1H), 7.55 (m, 2H), 5.50 (s, 1H), 4.80 (t, 1H), 4.50 (t, 1H), 4.35 (t, 1H), 3.75 (t, 1H), 3.10 (m, 1H), 2.00 (m, 1H), 1.05 (d, 3H), 0.85 (d, 3H).
[0000]
[0208] Resolution of the Phthalate with α-methylbenzylamine:
[0209] A phthalate of rac-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-ol (800 g) was dissolved in acetone (12 L) with slight heating to 50° C. The resulting clear solution was treated with (S)-methylbenzylamine (324 mL) and stirred at 50° C. for 10 min. The mixture was stirred at 45° C. for 1 h, at 40° C. for 1 h, and at 35° C. for 1 h before cooling to 18-22° C. over 2 h. The mixture was then allowed to stir at 18-22° C. for 17 h. The solid precipitate was collected by vacuum filtration, washed with acetone (1 L), and dried under vacuum at 30° C. to give (S)-1-phenylethanaminium 2-((((2R,3R,3aR,5S,6R,6aS,7S)-6,7-dimethyl hexahydro-2,5-methanofuro[3,2-b]furan-3-yl)oxy)carbonyl)benzoate (372 g, 36.6%, dr=98.4:1.6 by chiral HPLC) as a white solid. 1 H NMR (CDCl 3 , 400 MHz): δ 8.1 (bs, 3H), 7.60 (d, 1H), 7.55 (d, 1H), 7.30-7.40 (m, 4H), 7.20 (m, 3H), 5.30 (s, 1H), 4.60 (t, 1H), 4.30 (t, 1H), 4.25 (t, 1H), 3.95 (t, 1H), 3.65 (t, 1H), 2.10 (m, 1H), 1.85 (m, 1H), 1.70 (d, 3H), 0.95 (d, 3H), 0.75 (d, 3H).
[0210] The filtrate was concentrated under vacuum and then dissolved in MTBE (4 L). The solution was then washed with 1.0 M aqueous HCl (3 L) and the aqueous layer was back extracted with MTBE (2 L). The organic layers were combined, washed with water (2 L), and concentrated under vacuum at 30° C. to give a red-brown foam. The foam was chase with MTBE (2 L) and then with acetone (2 L). The brown foam (520 g) was dissolved in acetone (7.8 L) at 50° C. and treated with (R)-α-methylbenzylamine (210 mL). The mixture was stirred at 50° C. for 10 min, at 45° C. for 1 h, at 40° C. for 1 h, and at 35 for 1 h before cooling to 18-22° C. over 2 h. The mixture was then allowed to stir at 18-22° C. over 17 h. The precipitate was collected by vacuum filtration, washed with acetone (0.5 L), and dried under vacuum at 35° C. to give (R)-1-phenylethanaminium 2-((((2S,3S3aS,5R,6S,6aR,7R)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-yl)oxy)carbonyl)benzoate (402 g, 40%, dr=96.7:3.3 by chiral HPLC) as a white solid. 1 H NMR (CDCl 3 , 400 MHz): δ 8.1 (bs, 3H), 7.60 (d, 1H), 7.55 (d, 1H), 7.30-7.40 (m, 4H), 7.20 (m, 3H), 5.30 (s, 1H), 4.60 (t, 1H), 4.30 (t, 1H), 4.25 (t, 1H), 3.95 (t, 1H), 3.65 (t, 1H), 2.10 (m, 1H), 1.85 (m, 1H), 1.70 (d, 3H), 0.95 (d, 3H), 0.75 (d, 3H).
[0000]
(2R,3R,3aS,5R,6R,6aS,7S)-6,7-dimethylhexahydro-2,5-methanoforo[3,2-b]furan-3-ol
[0211] (S)-1-phenylethanaminium 2-((((2R,3R,3aR,5S,6R,6aS,7S)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-yl)oxy)carbonyl)benzoate (362 g) was dissolved in 1.0 M aqueous HCl (1.7 L) and MTBE (2 L). The organic layer was separated and the aqueous layer was extracted with MTBE (1 L). The organic layers were combined, washed with 1.0 M aqueous HCl (0.4 L), and treated with a solution of sodium hydroxide (99 g) in water (1 L). After stirring at rt for 1 h, the organic layer was separated and the aqueous layer was extracted with MTBE (1 L×2) and ethyl acetate (0.5 L). The combined organic layers were concentrated under vacuum to give the title compound (127 g, 91%) as a white solid. 1 H NMR (CDCl 3 , 400 MHz): δ 4.50 (t, 1H), 4.40 (t, 1H), 4.20 (t, 1H), 4.00 (t, 1H), 3.70 (s, 1H), 2.30 (m, 1H), 2.20 (m, 1H), 2.00 (m, 1H), 1.00 (d, 3H), 0.90 (d, 3H).
[0000]
(2S,3S,3aR,5S,6S,6aR,7R)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-ol
[0212] (R)-t-phenylethanaminium 2-((((2S,3S,3aS,5R,6S,6aR,7R)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-yl)oxy)carbonyl)benzoate (397 g) was dissolved in a mixture of 1.0 M aqueous HCl (1.9 L) and MTBE (2 L). The organic layer was separated and the aqueous layer was extracted with MTBE (1 L). The organic layers were combined, washed with 1.0 M aqueous HCl (0.5 L), and then treated with a solution of sodium hydroxide (108 g) in water (l L). After stirring at rt for 1 h, the organic layer was separated and the aqueous layer was extracted with MTBE (1 L×2) and ethyl acetate (0.5 L). The combined organic layers were concentrated under vacuum to give the title compound (135.8 g, 88%) as a white solid. 1 H NMR (CDCl 3 , 400 MHz): δ 4.40 (t, 1H), 4.30 (t, 1H), 4.20 (t, 1H), 4.00 (t, 1H), 3.70 (s, 1H), 2.30 (m, 2H), 2.00 (m, 1H), 1.00 (d, 3H), 0.90 (d, 3H).
[0213] B. Stereochemistry Determination for Compounds of Formula 1.
[0214] The stereochemistry of compounds of Formula 1 was determined using Mosher ester reacations as described below.
[0000]
Mosher ester of (2R,3R,3aS,5R,6R,6aS,7S)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-ol
[0215] (S)-1-1-phenylethanaminium 2-((((2R,3R,3aR,5S,6R,6aS,7S)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-yl)oxy)carbonyl)benzoate (105 mg, 0.24 mmol) was suspended in MTBE (6 mL) and washed twice with 1 N aqueous HCl (1 mL). The organic layer was treated with 3 N NaOH (1 mL) and stirred at rt for 1 h. The organic layer was separated, dried over MgSO 4 and concentrated in vacuo to give a crude alcohol.
[0216] Ca. 5 mg of the crude alcohol was dissolved in CH 2 Cl 2 (0.3 mL) and treated with triethylamine (30 uL), (S)-methoxy-trifluoromethylphenylacetyl chloride (18 mg) and a catalytic amount of DMAP. After stirring at rt for 30 min, the mixture was diluted with water (5 mL) and MTBE (5 mL). The organic layer was separated, filtered through silica gel pad, and concentrated in vacuo to give a crude Mosher ester, which was analyzed by NMR. 1 H NMR (CDCl 3 , 400 MHz): δ 7.58 (m, 2H, Ph), 7.42 (m, 3H, Ph), 5.37 (s, 1H, C3-H), 4.72 (m, 1H, C3a-H), 4.42 (m, 1H, C6a-H), 4.30 (m, 1H, C2-H), 3.80 (s, lit, C5-H), 3.55 (s, 3H, OMe), 2.35 (q, 1H, C6-H), 2.07 (m, 1H, C7-H), 1.12 (d, 3H, Me), 0.89 (d, 3H, Me).
[0000]
[0217] Mosher Ester of a Racemic Alcohol:
[0218] The phthalate of racemic alcohol (77 mg) prepared by above procedure was dissolved in MTBE (6 mL) and treated with 3 N NaOH (1 mL). After stirring at rt for 1 h, the organic layer was separated, dried over MgSO4 and concentrated in vacuo.
[0219] Ca. 5 mg of the crude alcohol was dissolved in CH 2 Cl 2 (0.3 mL) and treated with triethylamine (30 uL), (S)-methoxy-trifluoromethylphenylacetyl chloride (18 mg) and a catalytic amount of DMAP. After stirring at rt for 30 min, the mixture was diluted with water (5 mL) and MTBE (5 mL). The organic layer was separated, filtered through silica gel pad, and concentrated in vacuo to give a crude Mosher ester, which was analyzed by NMR. Peaks corresponding to the compound A and B was assigned based on literature (Rieser, M. J. et al., J. Am. Chem. Soc. 1992, 114, 10203). 1 H NMR (CDCl 3 , 400 MHz): δ 7.58 (m, 4H, Ph), 7.42 (m, 6H, Ph), 5.37 (s, 2H, C3-H for A and B), 4.72 (m, 1H, C3a-H for A), 4.62 (m, 1H, C3a-H for B), 4.42 (m, 2H, C5a-H for A and B), 4.38 (m, 1H, C2-H for B), 4.30 (m, 1H, C2-H for A), 3.80 (s, 2H, C5-H for A and B), 3.60 (s, 3H, OMe for B), 3.55 (s, 3H, OMe for A), 2.35 (m, 2H, C6-H for A and B), 2.07 (m, 2H, C.7-H for A and B), 1.12 (d, 3H), 1.10 (d, 3H), 0.89 (2d, 6H).
[0220] C. Oxidation of Alcohols of Formulas 1a and 1b to Lactones of Formulas Ia and Ib, Respectively.
[0221] Compounds of Formulas Ia and Ib were prepared as shown in Scheme 2 and described below.
[0000]
(2S,3aS,5R,6S,6aR,7R)-6,7-dimethyltetrahydro-2,5-methanofuro[3,2-b]furan-3(2H)-one
[0222] Sulfur trioxide-pyridine complex (118 g, 741 mmol) was dissolved in DMSO (400 mL) and stirred at ambient temperature for 20 min. After cooling to 0° C., the mixture was treated with a mixture of (2S,3S,3aR,5S,6S,6aR,7R)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-ol (42.2 g, 248 mmol) and triethylamine (207 mL, 1.49 mol) in methylene chloride (400 mL) over 1 h maintaining the internal temperature below 10° C. After stirring at ambient temperature for 4 h, the reaction was quenched with water (400 mL). The organic layer was separated and the aqueous layer was extracted with MTBE (500 mL). The organic layers were combined, washed twice with water (200 mL) and then with brine (150 mL), and concentrated in vacuo.
[0223] The residue was dissolved in MTBE (50 mL) and treated with n-heptane (200 mL). The resulting turbid solution was stirred at ambient temperature for 18 h. The precipitate was filtered, washed with n-heptane (20 mL), and dried under nitrogen purge to give the title compound (1 st crop, 5.4 g, 13%). The filtrate was concentrated in vacuo and dissolved in a mixture of MTBE (2 mL) and n-heptane (55 mL) with heating. The resulting clear solution was stirred at ambient temperature for 1 h and at 0° C. for 3 h. The precipitate was filtered and washed with n-heptane to give the 2 nd crop (13.8 g, 33%). 1 H NMR (CDCl 3 , 400 MHz): δ 4.68 (m, 1H), 4.29 (m, 1H), 3.96 (s, 1H), 3.90 (m, 1H), 2.48 (q, 1H), 2.36 (m, 1H), 1.10 (d, 3H), 0.93 d, 3H).
[0000]
(2S,4aR,6R,7S,7aR,8R)-7,8-dimethyltetrahydro-2,6-methanofuro[2,3-b][1,4]dioxin-3(2H)-one
[0224] (2S,3aS,5R,6S,6aR,7R)-6,7-dimethyltetrahydro-2,5-methanofuro[3,2-b]furan-3(2H)-one (7.07 g, 45.8 mmol) was dissolved in methylene chloride (120 mL) and treated with m-chloroperbenzoic acid (14.1 g, 81.7 mmol). After stirring at rt for 18 h, the mixture was diluted with MTBE (150 mL) and washed with 1 N aqueous NaOH solution (50 mL) and brine (30 mL). The organic layer was separated, dried over MgSO 4 and concentrated in vacuo. The residue was further purified by crystallization with MTBE and n-heptane to give the title compound (total 5.9 g, 62.7%). 1 H NMR (CDCl 3 , 400 MHz): δ 5.95 (t, 1H), 4.35 (t, 1H), 4.20 (t, 1H), 3.95 (t, 1H), 2.40 (m, 1H), 2.10 (m, 1H), 1.00 (d, 3H), 0.95 (d, 3H).
[0000]
(2S,4aR,6R,7S,7aR,8R)-7,8-dimethyltetrahydro-2,6-methanofuro[2,3-b][1,4]dioxin-3(2H)-one
[0225] (2S,3S,3aR,5S,6S,6aR,7R)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-ol (20 g) was dissolved in a mixture of methylene chloride (300 mL) and saturated aqueous NaHCO 3 (230 mL). After cooling to 0° C., the mixture was treated with 2,2,6,6-tetramethyl-1-piperidinyloxy, free radical (370 mg) and m-chloroperbenzoic acid (105 g). The mixture was stirred at 0° C. for 10 min and at rt for 16 h. After dilution with MTBE (400 mL), the organic layer was separated, and sequentially washed with a solution of sodium bisulfite (37 g) in water (100 mL), saturated aqueous NaHCO 3 (150 mL×3), and water (100 mL). The organic layer was concentrated under vacuum at 30° C. and chased with MTBE (100 mL) to furnish a yellow-white solid. The crude product was recrystallized from isopropyl alcohol (65 mL) by heating to 55° C., slowly cooling to rt over 4 h, and stirring at 0° C. for 1 h. The precipitate was collected by vacuum filtration, washed with isopropyl alcohol (15 mL), and dried under vacuum to give the title compound (16.5 g, 76%) as a white solid. [α] D 20 =+269.7° (c 0.51, MeOH); 1 H NMR (CDCl 3 , 400 MHz): δ 5.95 (t, 1H), 4.35 (t, 1H), 4.20 (t, 1H), 3.95 (t, 1H), 2.40 (m, 1H), 2.10 (m, 1H), 1.00 (d, 3H), 0.95 (d, 3H).
[0000]
(2R,4aS,6S,7R,7aS,8S)-7,8-dimethyltetrahydro-2,6-methanofuro[2,3-b][1,4]dioxin-3(2H)-one
[0226] (2R,3R,3aS,5R,6R,6aS,7S)-6,7-dimethylhexahydro-2,5-methanofuro[3,2-b]furan-3-ol (100 g) was dissolved in a mixture of methylene chloride (1.5 L) and saturated aqueous NaHCO 3 (1.15 L). After cooling to 10° C., the mixture was treated with 2,2,6,6-tetramethyl-1-piperidinyloxy, free radical (1.8 g) and m-chloroperbenzoic acid (530 g). The mixture was stirred at 10° C. for 30 min and at rt overnight. After dilution with MTBE (2 L), the organic layer was separated, and sequentially washed with a solution of sodium bisulfite (167 g) in water (1 L), saturated aqueous NaHCO 3 (1 L×3), and water (500 mL). The organic solution was then concentrated under vacuum and chased with toluene (1 L). The resulting solid was suspended in toluene (350 mL), heated to 45° C. and then allowed to cool to rt overnight. The white solid precipitate (mCPBA residue) was collected by vacuum filtration and washed with toluene (50 mL). The filtrate was concentrated under vacuum and recrystallized from isopropyl alcohol (300 mL) by dissolving at 55° C., slowly cooling to 22° C. over 1.5 h, and stirring at 0-5° C. for 1 h. The precipitate was collected by vacuum filtration, washed with isopropyl alcohol (75 mL), and dried under vacuum at 35° C. to give the title compound (85.5 g, 79%) as a white solid. [α] D =−248.6° (c 0.52, MeOH); 1 H NMR (CDCl 3 , 400 MHz): δ 5.95 (t, 1H), 4.40 (t, 1H), 4.20 (t, 1H), 4.00 (t, 1H), 2.40 (m, 1H), 2.20 (m, 1H), 1.05 (d, 3H), 1.00 (d, 3H).
[0227] D. Elaboration of Lactone of Formula a to Protected Tetrad 3
[0228] A compound of Formula Ia was elaborated as shown in Scheme 3 and described below.
[0000]
Methyl 6 (1,3-dithiolan-2-yl)-4-hydroxy-3,5-dimethyltetrahydro-2H-pyran-2-carboxylate
[0229] 7,8-dimethyltetrahydro-2,6-methanofuro[2,3-b][1,4]dioxin-3(2H)-one (20 mg, 0.11 mmol) was dissolved in 4 M hydrogen chloride in 1,4-dioxane (0.5 mL, 18 equiv) and treated with methanol (0.044 mL) and 1,2-ethanedithiol (0.020 mL, 2 equiv). After stirring at rt for 3 days, the reaction was quenched with sat. NaHCO3. The mixture was extracted with MTBE. The organic layer was washed with brine and concentrated in vacuo. The crude product was purified by column chromatography (ethyl acetate/n-heptane=1/10 to 1/3) to give the title compound (3 mg, 9%) as a white solid. 1 H NMR (CDCl 3 , 400 MHz): δ 4.70 (d, 1H), 4.16 (dd, 1H), 4.04 (t, 1H), 3.82 (s, 3H), 3.33 (dd, 1H), 3.20-3.28 (m, 4H), 2.26 (m, 2H), 1.06 (d, 3H), 0.96 (d, 3H).
[0000]
(2S,3R,4R,5S,6S)-methyl 4-hydroxy-6-((E)-3-methoxy-3-oxoprop-1-en-1-yl)-3,5-dimethyltetrahydro-2H-pyran-2-carboxylate
[0230] (2S,4aR,6R,7S,7aR,8R)-7,8-dimethyltetrahydro-2,6-methanofuro[2,3-b][1,4]dioxin-3(2H)-one (114 mg, 0.62 mmol) was dissolved in a mixture of methanol (1 mL) and tetrahydrofuran (0.2 mL), cooled to 0° C. and treated with trimethyl phosphonoacetate (0.15 mL, 1.5 equiv). Sodium methoxide (25% in methanol, 0.169 mL, 3.0 equiv) was added over 5 min and the resulting mixture was stirred at 0° C. for 40 min. The mixture was diluted with 2-methoxy-2-methylpropane (10 mL), and washed twice with water (5 mL) and then with sat. NH4Cl (5 mL) and brine (5 mL). The organic layer was concentrated in vacuo to give the title compound (117 mg, 70%) as a white solid. 1 H NMR (CDCl 3 , 400 MHz): δ 6.90 (dd, 1H), 6.38 (dd, 1H), 4.19 (m, 2H), 4.12 (m, 1H), 3.82 (s, 31H), 3.78 (s, 3H), 2.40 (m, 1H), 2.12 (m, 1H), 1.76 (bd, 1H), 0.98 (d, 3H), 0.98 (d, 3H).
[0000]
(2S,3R,4R,5S,6R)-methyl 4-hydroxy-3,5-dimethyl-6-((E)-2-(phenysulfonyl) vinyl)tetrahydro-2H-pyran-2-carboxylate
[0231] A mixture of (2S,4aR,6R,7S,7aR,8R)-7,8-dimethyltetrahydro-2,6-methanofuro[2,3-b][1,4]dioxin-3(2H)-one (5.25 g, 28.5 mmol) and dimethyl ((phenylsulfonyl)methyl)phosphonate (8.75 g, 30.0 mmol, 1.05 equiv) was dissolved in a mixture of methanol (54.6 mL) and tetrahydrofuran (27.3 mL). After cooling to 0° C., the mixture was treated with sodium methoxide (25% solution in methanol, 5.97 mL, 2.3 equiv) and stirred at 0° C. for 1 h.
[0232] The mixture was diluted with 2-methoxy-2-methylpropane (100 mL) and sequentially washed with water (50 mL) and saturated aqueous NaHCO3 (50 mL). The aqueous layers were combined and back-extracted with 2-methoxy-2-methylpropane (50 mL). The organic layers were combined, dried over MgSO4 and concentrated in vacuo to give the title compound (10.3 g, 97%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.92 (m, 2H), 7.62 (m, 1H), 7.58 (m, 2H), 6.90 (dd, 1H), 6.82 (dd, 1H), 4.22 (m, 1H), 4.19 (m, 1H), 4.13 (d, 1H), 4.10 (t, 1H), 3.78 (s, 3H), 2.36 (m, 1H), 2.15 (m, 1H), 0.91 (d, 3H), 0.88 (d, 3H).
[0000]
(2S,3R,4R,5S,6S)-methyl 4-hydroxy-3,5-dimethyl-6-(2-(phenylsulfonyl)ethyl)tetrahydro-2H-pyran-2-carboxylate
[0233] (2S,3R,4R,5S,6R)-methyl 4-hydroxy-3,5-dimethyl-6-((E)-2-(phenylsulfonyl) vinyl)tetrahydro-2H-pyran-2-carboxylate (9.1 g, 25.7 mmol) was dissolved in a mixture of ethyl acetate (100 mL) and methanol (20 mL), and treated with 10% Pd/C (50% wet, Degussa type E101 NE/W, 550 mg). The mixture was stirred under hydrogen atmosphere (balloon) for 15 h. The catalyst was filtered off using celite pad and washed with ethyl acetate. The filtrate was concentrated in vacuo to give the title compound (11.23 g), which was used for the next step without further purification. 1 H NMR (CDCl 3 , 400 MHz): δ 7.96 (m, 2H), 7.65 (m, 1H), 7.61 (m, 2H), 4.20 (m, 1H), 4.00 (m, 1H), 3.78 (s, 3H), 3.52 (m, 1H), 3.38 (m, 1H), 3.22 (m, 1H), 2.22 (m, 1H), 2.18 (m, 1H), 1.92 (m, 2H), 0.94 (d, 3H), 0.90 (d, 3H).
[0000]
(2S,3S,4R,5R,6S)-methyl 3,5-dimethyl-6-(2-(phenylsulfonyl)ethyl)-4-((triethylsilyl) oxy)tetrahydro-2H-pyran-2-carboxylate
[0234] A solution of (2S,3R,4R,5S,6S)-methyl 4-hydroxy-3,5-dimethyl-6-(2-(phenylsulfonyl)ethyl)tetrahydro-2H-pyran-2-carboxylate (9.15 g, 25.7 mmol) in methylene chloride (100 mL) was cooled to 0° C. and treated with imidazole (3.5 g, 2.0 equiv) and chlorotriethylsilane (4.74 mL, 1.1 equiv). The mixture was stirred at rt for 21 h. The resulting mixture was diluted with 2-methoxy-2-methylpropane (150 mL), sequentially washed with water (70 mL) and brine (30 mL), and concentrated in vacuo. The resulting crude product was purified by column chromatography (ethyl acetate/n-heptane=1/10 to 1/3) to give the title compound (10.75 g, 94% for two steps). 1 H NMR (CDCl 3 , 400 MHz): δ 7.96 (m, 2H), 7.65 (m, 1H), 7.61 (m, 2H), 3.98 (m, 1H), 3.90 (t, 1H), 3.78 (s, 3H), 3.49 (m, 1H), 3.38 (m, 1H), 3.21 (m, 1H), 2.16 (m, 2H), 1.92 (m, 1H), 1.78 (m, 1H), 1.00 (t, 9H), 0.92 (d, 3H), 0.88 (d, 3H), 0.62 (q, 6H).
[0000]
((2S,3S,4R,5R,6S)-3,5-dimethyl-6-(2-(phenylsulfonyl)ethyl)-4-((triethylsilyl)oxy)tetrahydro-2H-pyran-2-yl)methanol
[0235] (2S,3S,4R,5R,6S)-methyl 3,5-dimethyl-6-(2-(phenylsulfonyl)ethyl)-4-((triethylsilyl)oxy)tetrahydro-2H-pyran-2-carboxylate (1.0 g, 2.1 mmol) was dissolved in tetrahydrofuran (13 mL) and cooled to 0° C. 2 M Lithium tetrahydroborate in tetrahydrofuran (2.46 mL, 2.3 equiv) was added and the resulting mixture was stirred at rt for 22 h. After cooing to 0° C., the mixture was diluted with 2-methoxy-2-methylpropane (20 mL) and treated with 20 wt % citric acid (3.87 mL) maintaining the internal temperature below 10° C. The mixture was vigorously stirred for 10 min. The organic layer was separated and the aqueous layer was extracted with 2-methoxy-2-methylpropane (20 mL). The organic layers were combined, washed twice with sat. NaHCO3 and then concentrated under vacuum to give the title compound (0.90 g, 95%) as a clear oil. 1 H NMR (CDCl 3 , 400 MHz): δ 7.95 (m, 2H), 7.65 (m, 1H), 7.60 (m, 2H), 3.83 (m, 1H), 3.72 (m, 1H), 3.40-3.52 (m, 3H), 3.32 (m, 1H), 3.19 (m, 1H), 2.10 (m, 1H), 1.70-1.90 (m, 3H), 0.80-1.00 (m, 15H), 0.60 (q, 6H).
[0000]
Triethyl(((2S,3S,4R,5R,6S)-2-(iodomethyl)-3,5-dimethyl-6-(2-(phenylsulfonyl)ethyl)tetrahydro-2H-pyran-4-yl)oxy)silane
[0236] ((2S,3S,4R,5R,6S)-3,5-dimethyl-6-(2-(phenyl sulfonyl)ethyl)-4-((triethylsilyl)oxy)tetrahydro-2H-pyran-2-yl)methanol (0.18 g, 0.40 mmol) was dissolved in tetrahydrofuran (3 mL) and treated with triphenylphosphine (0.21 g, 2.0 equiv) and imidazole (82 mg, 3.0 equiv). After cooling to 0° C., the mixture was treated with iodine (0.15 g, 2.0 equiv) and stirred at rt for 5 h. More triphenylphosphine (0.21 g, 2.0 equiv), imidazole (82 mg, 3.0 equiv) and iodine (0.15 g, 2.0 equiv) were added, and stirring was continued at rt for 15 h and at 40° C. for 5 h. After cooling to rt, the reaction was quenched with 10% aqueous sodium thiosulfate solution (5 mL) and extracted with MTBE. After concentration, the crude product was purified by column chromatography (MTBE/n-heptane=1/10 to 1/3) to give the title compound (172 mg, 77%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.95 (m, 2H), 7.65 (m, 1H), 7.60 (m, 2H), 3.80 (m, 1H), 3.42-3.58 (m, 2H), 3.40 (m, 1H), 3.24 (m, 1H), 3.22 (m, 1H), 2.10 (m, 1H), 1.98 (m, 1H), 1.82 (m, 1H), 1.68 (m, 1H), 0.98 (t, 9H), 0.86 (d, 3H), 0.82 (d, 3H), 0.60 (q, 6H).
[0000]
(3S,4R,5S,6S)-4,6-dimethyl-1-(phenylsulfonyl)-5-((triethylsilyl)oxy)oct-7-en-3-ol
[0237] To a cooled (0° C.) mixture of zinc (0.101 g, 5 equiv) and acetic acid (0.035 mL, 2.0 equiv) in water (0.3 mL) was added a solution of triethyl(((2S,3S,4R,5R,6S)-2-(iodomethyl)-3,5-dimethyl-6-(2-(phenylsulfonyl)ethyl)tetrahydro-2H-pyran-4-yl)oxy)silane (0.17 g, 1.3 mmol) in tetrahydrofuran (1 mL). After stirring at 0° C. for 2 h, the mixture was diluted with 2-methoxy-2-methylpropane (20 mL). The mixture was sequentially washed with water (5 mL) and saturated aqueous NaHCO3 (5 mL), concentrated in vacuo and purified by column chromatography (MTBE/n-heptane=1/10 to 1/2) to give the title compound (104 mg, 79%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.93 (m, 2H), 7.63 (m, 1H), 7.58 (m, 2H), 5.74 (m, 1H), 5.02 (m, 2H), 4.01 (m, 1H), 3.55 (dd, 1H), 3.50 (s, 1H), 3.34 (m, 1H), 3.08 (m, 1H), 2.39 (m, 1H), 1.88 (m, 1H), 1.60-1.76 (m, 2H), 0.86-0.96 (m, 15H), 0.60 (m, 6H).
[0000]
(5S,6R,7S)-5-((S)-but-3-en-2-yl)-3,3,9,9-tetraethyl-6-methyl-7-(2-(phenylsulfonyl)ethyl)-4,8-dioxa-3,9-disilaundecane
[0238] A solution of (3S,4R,5S,6S)-4,6-dimethyl-1-(phenylsulfonyl)-5-((triethylsilyl)oxy)oct-7-en-3-ol (0.36 g, 0.84 mmol) in methylene chloride (4.5 mL) was cooled to 0° C., treated with imidazole (0.172 g, 3.0 equiv) and chlorotriethylsilane (0.212 mL, 0.15 equiv), and stirred at rt for 7 h. More imidazole (30 mg, 0.52 equiv) and chlorotriethylsilane (20 □L, 0.14 equiv) were added and stirring was continued at rt for additional 16 h. After quenching the reaction with water (10 mL), the mixture was extracted with 2-methoxy-2-methylpropane (10 mL). The separated organic layer was washed with brine and concentrated in vacuo. The crude product was purified by column chromatography (MTBE/n-heptane=l/20 to 1/5) to give the title compound (342 mg, 75%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.95 (m, 2H), 7.66 (m, 1H), 7.61 (m, 2H), 5.87 (m, 1H), 4.95 (m, 2H), 3.82 (m, 1H), 3.49 (dd, 1H), 3.20 (m, 1H), 3.06 (m, 1H), 2.26 (m, 1H), 1.8-2.0 (m, 2H), 1.50 (m, 1H), 0.86-1.00 (min, 21H), 0.82 (d, 3H), 0.50-0.66 (m, 12H).
[0239] E. Synthesis of Protected Pentads 4 and 5
[0240] Protected pentads of Formulas 4 and 5 were synthesized from a compound of Formula Ia as shown in Scheme 4 and described below.
[0000]
(2S,3S,4R,5R,6R)-methyl 3,5-dimethyl-6-((E)-2-(phenylsulfonyl)vinyl)-4-((triethyl silyl)oxy)tetrahydro-2H-pyran-2-carboxylate
[0241] A solution of (2S,3R,4R,5S,6R)-methyl 4-hydroxy-3,5-dimethyl-6-((E)-2-(phenylsulfonyl)vinyl)tetrahydro-2H-pyran-2-carboxylate (1.0 g, 2.8 mmol) in methylene chloride was cooled to 0° C. and treated with imidazole (0.406 g, 2.1 equiv) and chlorotriethylsilane (0.521 mL, 1.1 equiv). After stirring at rt for 4 h, the mixture was diluted with 2-methoxy-2-methylpropane (20 mL) and washed with water (10 mL) and brine (10 mL). After concentration, the crude product was purified by column chromatography (MTBE/n-heptane=1/10 to 1/2) to give the title compound (1.11 g, 88%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.92 (m, 2H), 7.65 (m, 1H), 7.58 (m, 2H), 6.90 (dd, 1H), 6.80 (dd, 1H), 4.20 (m, 1H), 4.12 (m, 1H), 4.02 (t, 1H), 3.78 (s, 3H), 2.22 (m, 1H), 2.02 (m, 1H), 1.01 (t, 9H), 0.89 (d, 3H), 0.87 (d, 3H), 0.64 (q, 6H).
[0000]
((2S,3S,4R,5R,6R)-3,5-dimethyl-6-((E)-2-(phenylsulfonyl)vinyl)-4-((triethylsilyl)oxy)tetrahydro-2H-pyran-2-yl)methanol
[0242] To a cooled (−70° C.) solution of (2S3S,4R,5R,6R)-methyl 3,5-dimethyl-6-((E)-2-(phenylsulfonyl)vinyl)-4-((triethylsilyl)oxy)tetrahydro-2H-pyran-2-carboxylate (7.91 g, 16.9 mmol) in methylene chloride (80 mL) was added 1 M diisobutylaluminum hydride in toluene (37.1 mL, 2.2 equiv). After stirring at −65° C. for 1 h, additional 1 M diisobutylaluminum hydride in toluene (5.1 mL, 0.3 equiv) was added and stirring was continued at −65° C. for additional 0.5 h. After quenching the reaction with methanol (3.3 mL), the mixture was stirred at −65° C. for 5 min, poured into saturated aqueous sodium potassium tartrate (180 mL), and vigorously stirred at rt for 1 h. Then, the mixture was extracted twice with 2-methoxy-2-methylpropane (100 mL). The organic layers were combined and concentrated in vacuo.
[0243] The residue was dissolved in methanol (66 mL), cooled to 0° C., and treated with sodium tetrahydroborate (0.19 g, 0.3 equiv). After stirring for 1 h at 0° C., the reaction was quenched with 0.1 M hydrogen chloride in water (66 mL) and the mixture was extracted twice with 2-methoxy-2-methylpropane (60 mL). The organic layers were combined, sequentially washed with sat. NaHCO3 (30 mL) and brine (30 mL), and concentrated in vacuo. The crude product was purified by column chromatography (ethyl acetate/n-heptane=1/10 to 1/2) to give the title compound (4.76 g, 95%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.93 (m, 2H), 7.66 (m, 1H), 7.57 (m, 2H), 6.90 (dd, 1H), 6.64 (dd, 1H), 4.22 (m, 1H), 3.95 (t, 1H), 3.78 (m, 1H), 3.58 (m, 1H), 3.52 (m, 1H), 2.00 (m, 1H), 1.82 (m, 1H), 1.79 (m, 1H), 0.98 (t, 9H), 0.86 (d, 3H), 0.82 (d, 3H), 0.62 (q, 6H).
[0000]
triethyl((2S,3S,4R,5R,6R)-2-(iodomethyl)-3,5-dimethyl-6-((E)-2-(phenylsulfonyl) vinyl)tetrahydro-2H-pyran-4-yl)oxy)silane
[0244] ((2S,3S,4R,5R,6R)-3,5-dimethyl-6-((E)-2-(phenylsulfonyl)vinyl)-4-((triethylsilyl)oxy)tetrahydro-2H-pyran-2-yl)methanol (4.54 g, 10.3 mmol) was dissolved in tetrahydrofuran (85 mL) and treated with triphenylphosphine (9.47 g, 3.5 equiv) and imidazole (4.21 g, 6 equiv). After addition of iodine (7.85 g, 3 equiv), the mixture was stirred at rt for 1 h and at 40° C. for 22 h. The mixture was cooled to rt and diluted with n-heptane (50 mL). The resulting precipitate was filtered and washed with 2-methoxy-2-methylpropane (100 mL). The filtrate was sequentially washed with 10% aqueous sodium thiosulfate solution (80 mL) and brine (30 mL), and concentrated in vacuo. The crude product was purified by column chromatography (MTBE/heptane=1/10 to 1/5) to give the title compound (4.72 g, 83%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.93 (m, 2H), 7.66 (m, 1H), 7.57 (m, 2H), 6.87 (dd, 1H), 6.71 (dd, 1H), 4.19 (m, 1H), 3.93 (t, 1H), 3.63 (m, 1H), 3.28 (dd, 1H), 3.10 (dd, 1H), 2.10 (m, 1H), 1.94 (m, 1H), 1.00 (t, 9H), 0.86 (d, 3H), 0.81 (d, 3H), 0.64 (q, 6H).
[0000]
(3R,4R,5S,6S,E)-4,6-dimethyl-1-(phenylsulfonyl)-5-((triethylsilyl)oxy)octa-1,7-dien-3-ol
[0245] To a cooled (0° C.) mixture of zinc (100 mesh, 2.8 g, 5.0 equiv), lead dichloride (0.24 g) and acetic acid (0.975 mL, 2 equiv) in water (8.4 mL) was added a solution of triethyl(((2S,3S,4R,5R,6R)-2-(iodomethyl)-3,5-dimethyl-6-((E)-2-(phenylsulfonyl)vinyl)tetrahydro-2H-pyran-4-yl)oxy)silane (4.72 g, 8.6 mmol) in tetrahydrofuran (43.7 mL). After stirring at 0° C. for 2 h, additional zinc (1 g, 1.8 equiv) was added and stirring was continued at 0° C. for 3 h and at rt for 12 h. Additional zinc (powder, 1.4 g, 2.5 equiv) and acetic acid (0.15 mL, 0.3 equiv) were added and stirring was continued at rt for another 7 h. After removal of unreacted zinc by filtration, the filtrate was washed with saturated aqueous NaHCO3 (17 mL), and the aqueous layer was back-extracted with 2-methoxy-2-methylpropane (50 mL). The organic layers were combined, washed with brine, and concentrated in vacuo. The crude product was purified by column chromatography (MTBE/n-heptane=1/10 to 1/2) to give the title compound (2.6 g, 71%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.92 (m, 2H), 7.63 (m, 1H), 7.55 (m, 2H), 6.90 (dd, ii), 6.68 (dd, 1H), 5.80 (m, 1H), 5.10 (m, 2H), 4.88 (4.19 (m, 1H), 3.80 (s, 1H), 3.70 (m, 1H), 2.50 (m, 1H), 1.92 (m, 1H), 1.08 (d, 3H), 0.98 (t, 9H), 0.91 (d, 3H), 0.66 (q, 6H).
[0000]
(2S,3R,4R,5S,6S)-2,4,6-trimethyl-1-(phenylsulfonyl)oct-7-ene-3,5-diol
[0246] (3R,4R,5S,6S,E)-4,6-dimethyl-1-(phenylsulfonyl)-5-((triethylsilyl)oxy)octa-1,7-dien-3-ol (51 mg, 0.12 mmol) in tetrahydrofuran (2 mL) was cooled to −78° C. and treated with 1.5 M methyllithium-lithium bromide complex in ether (0.24 mL, 3.0 equiv). After stirring at −78 C˜−60° C. for 1 h, the mixture was treated with chlorotrimethylsilane (46 μL, 3.0 equiv) and stirred at −60° C. for additional 20 min. After cooling back to −78° C., the mixture was treated with 1.5 M methyllithium-lithium bromide complex in ether (0.24 mL, 3.0 equiv) and warmed up to −40° C. over 3 h. The reaction was quenched with sat.NH4Cl and extracted with MTBE. The organic layer was dried over MgSO4 and concentrated in vacuo.
[0247] The residue was dissolved in tetrahydrofuran (2 mL), treated with 1 M tetra-n-butylammonium fluoride in tetrahydrofuran (0.36 mL), and stirred at rt for 1 h. After dilution with MTBE, the mixture was washed with water and dried over MgSO4. The crude product was purified by column chromatography (ethyl acetate/n-heptane=1/10 to 2/1) to give the title compound (7 mg, 20%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.95 (m, 2H), 7.70 (m, 1H), 7.61 (m, 2H), 5.70 (m, 1H), 5.20 (m, 2H), 3.83 (dd, 1H), 3.32 (m, 1H), 3.28 (dd, 1H), 3.23 (ds, 1H), 2.93 (dd, 1H), 2.40 (m, 1H), 2.26 (m, 1H), 2.20 (bs, 1H), 1.70 (m, 1H), 1.19 (d, 3H), 1.02 (d, 3H), 0.94 (d, 3H).
[0000]
(2R,3R,4R,5S,6S)-2,4,6-trimethyl-1-(phenylsulfonyl)oct-7-ene-3,5-diol
[0248] To a cold (0° C.) suspension of copper(I) iodide (0.45 g, 5 equiv) in tetrahydrofuran (10 mL) was added 1.6 M methyllithium in ether (4.42 mL, 15 equiv). After stirring at 0° C. for 30 min, the mixture was treated with a solution of (3R,4R,5S,6S,E)-4,6-dimethyl-1-(phenylsulfonyl)-5-((triethylsilyl)oxy)octa-1,7-dien-3-ol (0.2 g, 0.47 mmol) in tetrahydrofuran (2 mL and 1 mL for rinse). The mixture was stirred at 0° C. for 1 h and at rt for 1 h. The reaction was quenched with a mixture of 28% ammonium hydroxide (4 mL) and saturated NH4Cl (40 mL), and the resulting mixture was extracted with MTBE. The organic layer was washed with brine and concentrated in vacuo. The crude product was purified by column chromatography (ethyl acetate/n-heptane=1/10 to 1/2) to give the title compound (95 mg, 62%). 1 H NMR (CDCl 3 , 400 MHz): δ 7.95 (m, 2H), 7.66 (m, 1H), 7.60 (m, 2H), 5.70 (m, 1H), 5.20 (m, 2H), 3.50-3.70 (m, 2H), 3.37 (m, 1H), 2.90 (dd, 1H), 2.40 (m, 1H), 2.28 (m, 1H), 1.90 (m, 1H), 1.15 (d, 3H), 1.01 (2d, 6H).
[0249] F. Exemplary Elaboration of Protected Tetrad of Formula 3
[0250] The protected tetrad of Formula 3 was used to prepare intermediates of aplyronine as described below.
[0000]
(2S,3R,6S,7S,8R,9S,E)-2-((2R,3R,5S)-5-methoxy-3-methyltetrahydrofuran-2-yl)-6,8-dimethyl-11-(phenylsulfonyl)-7,9-bis((triethylsilyl)oxy)undec-4-en-3-ol
[0251] A mixture of (5S,6R,7S)-5-((S)-but-3-en-2-yl)-3,3,9,9-tetraethyl-6-methyl-7-(2-(phenylsulfonyl)ethyl)-4,8-dioxa-3,9-disilaundecane (84 mg, 0.16 mmol) and (3R,4S)-4-((2R,3R,5S)-5-methoxy-3-methyltetrahydrofuran-2-yl)pent-1-en-3-ol (21 mg, 0.11 mmol) was dissolved in a degassed 1,2-dichloroethane (3 mL) and heated to 45° C. After stirring at 45° C. for 5 min, the mixture was treated with Grubbs 2 nd generation catalyst (6 mg, 7 μmol) and stirred at 45° C. for 21 h and at 60° C. for 2 h. The mixture was cooled to rt and concentrated in vacuo. The residue was purified by column chromatography (ethyl acetate/n-heptane=1/10 to 2/1) to give the title compound (8 mg, 10%) along with 67% of recovered starting material. 1 H NMR (CDCl 3 , 400 MHz): δ 7.95 (m, 2H), 7.70 (m, 1H), 7.61 (m, 2H), 5.76 (dd, 1H), 5.49 (dd, 1H), 4.98 (d, 1H), 4.31 (M, 1H), 3.83 (bq, 1H), 3.59 (dd, 1H), 3.52 (dd, 1H), 3.38 (s, 3H), 3.16 (m, 1H), 3.13 (d, 1H), 3.05 (m, 1H), 2.32 (m, 2H), 2.13 (m, 1H), 1.90 (m, 2H), 1.83 (m, 1H), 1.65 (m, 1H), 1.49 (m, 1H), 1.12 (d, 3H), 0.9-1.4 (m, 24H), 0.81 (d, 3H), 0.62 (q, 6H), 0.56 (q, 6H).
[0000]
(2S,3R,6S,7S,8R,9S)-2-((2R,3R,5S)-5-methoxy-3-methyltetrahydrofuran-2-yl)-6,8-dimethyl-11-(phenylsulfonyl)-7,9-bis((triethylsilyl)oxy)undecan-3-ol
[0252] (2S,3R,6S,7S,8R,9S,E)-2-((2R,3R,5S)-5-methoxy-3-methyltetrahydrofuran-2-yl)-6,8-dimethyl-11-(phenylsulfonyl)-7,9-bis((triethylsilyl)oxy)undec-4-en-3-ol (8 mg, 11 μmol) was dissolved in ethyl acetate (3 mL) and treated with 10% Pd on C (5 mg). The mixture was stirred at rt under hydrogen atmosphere (balloon) for 1 h. The catalyst was filtered off and rinsed with ethyl acetate. The filtrate was concentrated in vacuo to give the title compound in quantatative yield. 1 H NMR (CDCl 3 , 400 MHz): δ 7.95 (m, 2H), 7.69 (m, 1H), 7.61 (m, 2H), 4.95 (d, 1H), 3.84 (m, 2H), 3.60 (dd, 1H), 3.45 (m, 1H), 3.37 (s, 3H), 3.35 (d, 1H), 3.03-3.22 (m, 2H), 2.31 (m, 1H), 2.14 (m, 1H), 1.91 (m, 2H), 1.59-1.75 (m, 3H), 1.45-1.55 (m, 4H), 1.35 (m, 1H), 1.09 (d, 3H), 0.85-1.00 (m, 24H), 0.81 (d, 3H), 0.50-0.63 (m, 12H). | The present invention relates to stereochemically defined polypropionates and methods for preparing and using the same. The stereochemically defined polypropionates may be useful in the synthesis of natural products and/or natural product-like libraries. | 2 |
[0001] This is a divisional application of pending U.S. patent application Ser. No. 09/747,642 filed Dec. 22, 2000.
BACKGROUND OF THE INVENTION
[0002] The present invention is directed to manufacturing, testing, and operating a control platform based on communicating sensors and control devices.
[0003] The processes involved in building a chiller range from obtaining the required parts, correctly installing and assembling the parts, and verifying that the chiller was assembled correctly and functions in accordance with the customer's specified requirements. To support these processes, communication connections are needed to component supplier development systems, to sales order entry, to manufacturing method sheets and to manufacturing performance specifications. The information from each of these areas is used throughout the assembly process. Accessibility to this information in a timely manner, and keeping this information up-to-date are crucial to running and maintaining smooth assembly processes.
[0004] Presently the process of verifying the assembly process and the final product functionality are very much manual. Paper is used as the primary method to determine the testing functionality and the performance criteria. Mistakes in data entry may go unchecked and remain undiscovered until the product is delivered to the customer site. To correct the problem with the product at the customer site is not only expensive, but it hurts the manufacturer's reputation to deliver a quality product.
[0005] Also, today's manual systems do not support coordination between the various “build” stations in the assembly process. What is more, critical components are provided by different suppliers. Without good coordination between the stations and the suppliers, there may be errors, deficiencies or omissions in the functionality of the product. Additionally, without good coordination, a process manufacturing organization structure is difficult to support.
[0006] The process becomes more complex if the product includes a communications system including digital controls interconnected by a bus or the equivalent.
[0007] Products with digital controls are more expensive and difficult than they need to be. This is because, in the case of specialized equipment, off-the-shelf controllers are not available to meet that product's needs. As a result, a particular company uses its own controllers with custom hardware and fixed configurations of input and output points. This means that for a particular product line selling only 1,000 to 3,000 units a year, the cost of a controller for that product line may provide disproportionately high overhead costs since a controller generally costs between $500,000.00 and a $1,000,000.00 per board to develop. Additionally, development of control circuit boards is slow and costly, inhibiting the development of new or special control features. Moreover, the design life of a particular controller is five to seven years. When any single chip used in such a controller becomes obsolete, the entire controller and the control system may often need redesign. This increases costs for both production controllers as well as costs for supporting service parts.
[0008] Furthermore, complex products are sold and configured on a job-by-job basis. As a result, there are many possible system and control configurations. For a single controller to fit all needs, designers are forced to populate controllers with the maximum anticipated capacity to control all potential control points. Thus, most equipment ships with many more control points than the product actually needs.
[0009] Moreover, previous control designs consisted of five to ten communicating devices. Although the number of network devices was small, many problems were incurred in factories when the communications network did not function properly. Usually, the factory did not have good tools in which to troubleshoot the network problem, and the assembly line operators would resort to trial and error replacement of electronic modules one at a time until the problem was corrected. Not only is this trial and error approach very time consuming, it often did not correct the root cause of the problem and the customer would therefore receive a product which was marginally working since the root cause was not corrected. Additionally, since good tools did not exist to analyze the communications network, the factory's emphasis was to get the devices communicating. There was no assessment of actual communication signal levels just the result. Although the communications levels were judged adequate at the factory to allow communications, typically when the product was started at the job site, the marginal communications would fail since the signal was lost in the normal electrical noise characteristics of the particular job site. This normal electrical noise need not have been excessive to interfere with a communications system that had no margin for error. A good communication system has a large amount of design margin built in to allow it to operate in a wide variety of environments. Without this margin, the communication systems are susceptible to intermittent performance or total failure. Intermittent performance and total failure problems are difficult and time consuming to troubleshoot in the field, and job sites with these problems received a lot of attention since a product or process was usually inoperable as a result of the intermittent performance or total failure. Also, without good tools in the factory, problems were often not discovered until the final assembly functional test.
[0010] In addressing all of these problems, sensors such as temperature, pressure and level sensors and control devices such as valves and actuators have been each packaged with an electronic controller into a new unitary device. For purposes of this application, such a unitary device is referred to as a low level intelligent device or LLID. The low level intelligent devices are installed throughout an industrial product such as an air conditioning chiller system and are interconnected with a four-wire communications bus cable that provides each low level intelligent device with the necessary power and with communication to a main processor for the product.
[0011] Each low level intelligent device must be provided with an identity which the low level intelligent device will thereafter use to identify itself when communicating on the communications bus and will use in recognizing communications on a communications bus which are directed to that particular component. Additionally, the electronic control portion of each low level intelligent device must be provided with its appropriate operating parameters. Furthermore, each low level intelligent device on a particular communications bus, the communications bus itself, and the connections of the LLID to the communications bus as well as the identity and operating parameters for each low level intelligent device must be verified and tested to avoid errors in manufacture and operation of the product.
[0012] It is also desirable that products include a control platform that does not rely upon large, complex and multi-chip controller boards. It is desirable that the control platform consist of communicating “mini-boards” having only one or two control points and functioning as low level intelligent devices. These low level intelligent devices are building blocks that allow the control system to be configured exactly as required for the product, per the customer's order. The low level intelligent devices are infinitely configurable for new applications, thereby providing a hardware design that need only be designed a single time. Additionally, since the same low level intelligent devices are applied in many different types of units, there can be significantly higher volumes for low level intelligent device than traditional controller boards. These higher volumes allow mass production and lower costs. Since the desired control platform is readily configurable, products can be shipped with only the controls needed for the product's particular application and since the controller is also configurable, the redesign in addition of control points is relatively simple and fast and by breaking the system into “granules”, the controllers become less susceptible to obsolence caused by a phase out of any particular component.
[0013] What is needed is a versatile tool that, with minimal operator input, will verify proper installation of low level intelligent devices during the manufacturing process by monitoring the electrical integrity of each low level intelligent device and the comm bus as a whole. The tool will also configure each low level intelligent device per customer order and verify the functionality of the low level intelligent device. Monitoring each individual low level intelligent device as it's attached to the comm bus will avoid difficulty when installing subsequent low level intelligent devices or confirming the operation of a communications bus and its components as a whole.
SUMMARY OF THE INVENTION
[0014] It is an object, feature and advantage of the present invention to solve the problems with the prior art.
[0015] It is an object, feature and advantage of the present invention to avoid potential errors in low level intelligent device installation that would cause subsequent communication and operational problems.
[0016] It is an object, feature and advantage of the present invention to provide a system for manufacturing a product with a communications bus and low level intelligent devices. It is a further object, feature and advantage of the present invention to verify proper installation of each low level intelligent device at the time the device is installed. It is a further object, feature and advantage of the present invention to verify proper installation at the time of installation so as to avoid future difficulties when installing subsequent low level intelligent devices or confirming the operation of the communications bus and its components.
[0017] It is an object, feature and advantage of the present invention to provide a single application that confirms that the proper connection and configuration of low level intelligent device occurs at the time of its installation. It is a further object, feature and advantage of the present invention to verify wirings, identity and operating parameters for each low level intelligent device.
[0018] It is an object, feature and advantage of the present invention to monitor the integrity of a communications system and the installation of a low level intelligent device communicating by means of a bus. It is a further object, feature and advantage of the present invention to notify an installer immediately upon the introduction of any wiring or device error.
[0019] It is an object, feature and advantage of the present invention to improve the efficiency and manufacture of control platforms. It is a further object, feature and advantage of the present invention to avoid a plurality of separately dedicated steps for each installed device. It is a still further object, feature and advantage of the present invention to combine all necessary steps into a two-part process comprising a first step of routing a primary bus cable throughout the product, and a second step of connecting individual low level intelligent devices to the bus cable. It is a still further object, feature and advantage of the present invention to provide a single application which sequences, configures and verifies each low level intelligent devices connection to the bus cable.
[0020] It is an object, feature and advantage of the present invention to build a communications system for a product operably controlled by same using a master database to obtain all build and test information. It is a further object, feature and advantage of the present invention to use this master database to provide installation sequence and instructions to a factory technician. It is a still further object, feature and advantage of the present invention to support demand flow manufacturing including factory on-line sequence of event sheets and method sheets. It is yet a further object, feature and advantage of the present invention to accommodate graphics showing details such as the installation area for a particular low level intelligent device. It is a still further object, feature and advantage of the present invention to provide informative alarm messages to aid the factory technician in troubleshooting. It is another object, feature and advantage of the present invention to allow an advanced user to interrogate integrity and power supply integrity using a PC based scope analyzer and voltage magnitude measurement card. It is yet another object, feature and advantage of the present invention to check for failure mode scenarios and provide the factory technician with corrective steps. It is yet another object, feature and advantage of the present invention to allow communications from the factory technician to an installation sequence controller using a remote hand held selector. This remote hand held selector preferably includes a push button allowing the user to advance screens while working on the product at the location of the low level intelligent devices installation. It is yet another object, feature and advantage of the present invention to record failures in a log file for tracking and future quality management.
[0021] It is an object, feature and advantage of the present invention to confirm the wiring, identification and operating parameters for each individual low level intelligent device occur properly at the time of installation.
[0022] It is an object, feature and advantage of the present invention to automatically download sales order information to a central database to be accessible by all of the various testers, whether inside of or outside of the manufacturer's facilities, thereby ensuring that the correct information is available at the point of use during assembly, manufacture and testing.
[0023] It is an object, feature and advantage of the present invention to allow the testers in a manufacturing process to access the central database to obtain any late sales order changes and to incorporate them into the normal assembly process.
[0024] It is an object, feature and advantage of the present invention to read part number information stored in the low level intelligence device (hardware and software numbers) and compare the numbers read to numbers stored in a controlled database. Any discrepancy between numbers read from low level intelligence device and numbers stored in database results in enunciation of alarm to user.
[0025] It is an object, feature and advantage of the present invention to allow the testers in the manufacturing process to obtain the latest configuration data for the product being assembled, so that the product is setup and assembled exactly in accordance with the customer's ordering instructions.
[0026] It is a further object, feature and advantage of the present invention to include options and operating parameters in this configuration data to minimize any setup and commissioning by the customer prior to using, starting or operating the product.
[0027] It is an object, feature and advantage of the present invention to provide the exact information needed to assemble a product at the assembly point when the product is there for assembly.
[0028] It is a further object, feature and advantage of the present invention to provide a simple identification system to the floor assembler to immediately make available the information needed to build the product.
[0029] It is an object, feature and advantage of the present invention to allow for uploads and retention of a particular test during assembly to a centralized database.
[0030] It is a further object, feature and advantage of the present invention to maintain a file automatically for each product with the requirements for its assembly and the results of the testing for each step of the assembly.
[0031] It is a further object, feature and advantage of the present invention that information and results from one test or one station to be accessed by other test stations to minimize the probability of a particular item being missed or skipped since all testers know or can view the other tester's work.
[0032] It is another object, feature and advantage of the present invention to allow the automatic upload of test results into the centralized database to allow a manufacturing engineer to analyze the process and take actions to optimize that process.
[0033] It is a further object, feature and advantage of the present invention that the manufacturing engineer have available and be able to analyze the items that failed during the build and test process as well as assembly and testing and subsequently in the field.
[0034] It is an object, feature and advantage of the present invention to change the process of manufacturing a communications system from a process where a human controls the process sequence to a process where a computer controls and the process sequence.
[0035] It is an object, feature and advantage of the present invention to provide a way to look at communication signals on a communications network and verify that proper signals exist. It is a further object, feature and advantage of the present invention to examine these communication signals and accurately identify any part of the signal that does not meet specification. It is a further object, feature and advantage of the present invention to generate an alarm when a problem is detected and suggest corrective actions to resolve the problem.
[0036] It is an object, feature and advantage of the present invention to allow signal analysis of a communications network to be undertaken at various stages of assembly as well as at the final functional tester. It is a further object, feature and advantage of the present invention to minimize the time troubleshooting on an assembly line and therefore keep TAKT times low.
[0037] It is an object, feature and advantage of the present invention to eliminate trial and error troubleshooting of communication devices.
[0038] It is an object, feature and advantage of the present invention to provide a high level of confidence that a control network is operating with the desired margins when the product is shipped.
[0039] It is an object, feature and advantage of the present invention to provide an approach to a localized problem to the testing device itself, a control network master device, any of the control network responding devices, or any of the interconnecting communications media.
[0040] It is an object, feature and advantage of the present invention to verify acceptable fanout of each communicating device in a communication system.
[0041] It is an object, feature and advantage of the present invention to identify the exact time and exact problem that is introduced into the product being assembled. It is a further object, feature and advantage of the present invention to do this with specificity in a distributed control platform.
[0042] The present invention provides a method of doing business. The method comprises generating a sales order representative of a product; developing build and test instructions from the sales order; developing an installation sequence from the build and test instructions; and building the product using the build and test instructions in the sequence laid out by the installation sequence.
[0043] The present invention also provides a method of manufacturing a control system for an industrial or a process unit. The method comprises providing a plurality of components, each component including a control portion and a functional portion with an operational link therebetween; installing a communications bus on the unit; verifying the operability of the communications bus by means of a tester device; initiating, under the direction of the tester device, a request that one of the plurality of components be attached to the bus; receiving a signal from the connected component by means of the communications bus; analyzing the communications bus and the newly connected component for operability; and responding to the newly connected component by means of the communications bus with instructions providing an identity and operating parameters to the component.
[0044] The present invention further provides a device with an analog or digital input or output. The device comprises a control portion and a functional portion operably connected and controlled by the control portion. The functional portion is operably capable of providing an analog or digital input or output. The control portion includes an external communications port operably connected to a control bus, an actuator responsive to a non-invasive signal, and a controller operably connected to the external communications port and capable of sending and receiving communications through that port. The controller is operably connected to the actuator and receives a signal from the actuator. The controller transmits a signal to the external port upon receipt of an actuator signal.
[0045] The present invention additionally provides a method of guiding a technician in manufacturing a communication system having a bus, a main controller, a plurality of components, and a subcontroller associated with each component. The method comprises the steps of: attaching a tester controller to the bus; providing a path from the tester controller to the technician; instructing, on the path, the technician to attach a specific one of the plurality of components to the bus; signaling, with a first signal from the technician to the tester controller, upon completion of the component attachment; signaling, with a second signal from the tester controller to the technician, to confirm receipt of the first signal; causing the subcontroller to signal the main controller; and configuring the subcontroller by transmitting configuration instructions from the main controller to the subcontroller over the bus.
[0046] The present invention still further provides a method of integrating the manufacture of a product by a plurality of businesses. The method comprises generating a sales order in an electronic form; converting the sales order to an electronic build document; transferring the electronic build document to a first company for the construction of a first subassembly for the product; testing the subassembly of the first company; attaching the test results to the electronic build document; forwarding the electronic build document to a second company for main assembly; attaching a communications bus to the product; testing the operability of the bus; adding the bus operability test results to the electronic build document; attaching the first subassembly to the bus; testing the operability of the first subassembly and the bus; attaching the subassembly and bus operability test results to the electronic build document; and shipping the product.
[0047] The present invention yet further provides a method of manufacturing a distributed control system for a product having a plurality of components, each component including a functional portion and a controller portion. The method comprises the steps of: attaching a communications bus to the product; attaching the functional portion of a component to the product and attaching the controller portion of a component to the bus; causing the controller portion to send a self-identifying signal on the bus; receiving the self-identifying signal in a configuring controller; transmitting from the configuring controller to the controller portion a signal including an identifier and operating parameters; receiving the identifier and the operating parameters in the controller portion; and configuring the controller portion in accordance with the identifier and the operating parameters.
[0048] The present invention additionally provides a method of building a product. The method comprises the steps of: creating an electronic build document cataloging the features and requirements for the product; forwarding the electronic build document to at least one component manufacturer, each component manufacturer building one or more components, testing the operability of said one or more components, and attaching the test results to the electronic build document to create a modified electronic build document; forwarding the modified electronic build document to a final assembly location wherein the one or more components and other materials are assembled into the product; testing the assembled product; and attaching the test results for the assembled product to the modified electronic build file to create a final electronic build file.
[0049] The present invention also provides a method of doing business. The method comprises the steps of: electronically creating a customer order which includes the requirements and components for a product desired by the customer; developing a bill of materials from the electronic order detailing the parts and materials required to build the product; developing an electronic specification from the customer order detailing the components, subassemblies and product required by the customer; sequentially transmitting the specification to the manufacturer of each component, assembly and final assembly, each manufacturer building the requisite component, subassembly or assembly, each manufacturer testing the requisite component, subassembly or assembly, and each manufacturer attaching the test results to the electronic specification; and periodically checking the electronic bill of materials versus the electronic specification to verify the compatibility and accuracy thereof.
[0050] The present invention moreover provides a bus analyzer system. The system comprises a communications bus; and an integral analyzer device operably connected to the bus and configured to receive signals thereon. The analyzing device includes a scope instrument and a voltage meter instrument configured to receive those signals. The system also comprises a computer operably connected to the scope and voltage meter instruments such that the scope and voltage meter instruments and the computer collectively analyze the bus and determine corrective actions as needed. The present invention yet further provides that the scope and voltage meter instruments include the capability to analyze 24 VDC signals and ground signals for DC voltage magnitude and AC components and that the scope and voltage meter instruments include the capabilities to analyze communications plus and minus lines for magnitude and to determine an RS485 differential signal to verify signals to be within design limits. The invention also provides that the scope and voltage meter instruments include the capability to test for common mode characteristics such as magnitude with respect to ground and differential and common mode signal aspects for logic 1 and logic 0 signals.
[0051] The present invention moreover provides a method of verifying the integrity of a communications bus having a power line and a communications line. The method comprises the steps of: analyzing a signal in the power line to determine a quality thereof; analyzing a signal on a communications line to determine a quality thereof; generating a power analysis result signal as a function of the power line signal analysis; generating a communications line analysis result signal as a function of the communications line signal analysis; receiving the power line and communications line result signals in a controller; evaluating the received signals; and providing a comprehensive analysis of the power line, the communications line, the power line signal, the communications line signal, communications bus, and any components attached thereto.
[0052] The present invention yet further provides a monitor for a communications bus having a power line and a communications line. The monitor comprises a power line analyzer, a communications line analyzer and a controller. The power line analyzer is operably connected to a source of power and has circuitry and programs to analyze the transmissions on the power line and to generate a first signal with the analysis results. The communications line analyzer is operably connected to the communications line and has circuitry and programs to analyze communication signals on the communications line and to generate a second signal with the analysis results. The controller is operably connected to the power line analyzer and the data line analyzer for receiving the first and second signals and is operably capable of evaluating the content of the first and second signals and providing an analysis of the signals, the power line, the communications line and the communications bus as well as any attached components.
BRIEF DESCRIPTION OF THE DRAWINGS
[0053] FIG. 1 is a diagram of a product equipped with a communications bus and components in accordance with the present invention.
[0054] FIG. 2 is a diagram of a bus and its components in accordance with the present invention.
[0055] FIG. 3 is a diagram of the product sale to manufacture of a product in accordance with the present invention.
[0056] FIG. 4 is a flow chart of a method of doing business in accordance with the present invention.
[0057] FIG. 5 is a diagram of the manufacture and test of the bus and components in accordance with the present invention.
[0058] FIG. 6 is a flow chart of a method of manufacture of a product in accordance with the present invention.
[0059] FIG. 7 shows a magnetically actuatable component in accordance with the bus of FIG. 5 .
[0060] FIG. 8 shows a communications bus, components and bus signal analyzer in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0061] The present invention is directed to the manufacture, testing and operation of a communications and control system for a industrial or process product. In the preferred embodiment, such a product is embodied by a chiller system cooling an air conditioning fluid like those used in the HVAC system. Examples of such chiller systems are sold by The Trane Company, a Division of American Standard Inc., under the trademarks CenTraVac™, Cold Generators and Series R™. However, a person of ordinary skill in the art will recognize that such a control system including a communications bus and the communicating components connected to that bus are readily applicable to many other products including industrial tractors, construction equipment such as cranes, dump trucks and bulldozers, truck braking systems, sanitation truck control systems, automated factory equipment, medical systems, paper mills, elevator controls, security systems, and other devices with electrical power control, mechanical actuator control, hydraulic pressure control, temperature or pressure control, and/or fluid pressure control. The term ‘product’ is used generically throughout this application to encompass all such devices as well as the myriad of other devices with similar features or capability.
[0062] FIG. 1 shows a product 10 such as a chiller system for use in providing chilled water for heating, ventilating and air conditioning (HVAC) applications. The chiller is comprised of a compressor 12 , a condenser 14 and an evaporator 16 . The compressor 12 is preferably a screw compressor whose capacity is controlled by a slide valve 120 but could also be a centrifugal compressor or any other compressor with its respective form of capacity control.
[0063] Refrigerant gas is compressed within the compressor 12 and directed out a discharge 18 into piping 20 which connects the compressor 12 to the condenser 14 . In the preferred embodiment, the high pressure, relatively hot compressed refrigerant gas delivered to the condenser 14 will be cooled by air moved over the condenser 14 by one or more fans 22 , each having a motor 23 controlled by a fan controller 24 . The condenser 14 may be cooled in various other ways including the use of a fluid such as city water or the use of a cooling tower.
[0064] The heat exchange process occurring within the condenser 14 causes the relatively hot, compressed refrigerant gas to cool condense and pool in the bottom or lower area of the condenser 14 . The condensed refrigerant then flows out of the condenser 14 through discharge piping 26 and is next delivered, primarily in liquid form, into the evaporator 16 . The transfer of refrigerant from the condenser 14 to the evaporator 16 is controlled by an expansion device 28 such as an expansion valve.
[0065] Relatively cool, low pressure liquid refrigerant is delivered to the evaporator 16 , where the refrigerant undergoes heat exchange with and cools the relatively warmer medium, preferably such as water, that enters the evaporator 16 through an inlet 56 and exits through an outlet 58 . That now cooled medium is, in turn, delivered into heat exchange contact with the heat load which it is the purpose of the chiller to cool.
[0066] In the process of cooling the medium which flows through the evaporator 16 and being heated thereby, the liquid refrigerant delivered to the evaporator 16 vaporizes and is directed to piping 60 as a low pressure gas back to the compressor 12 . The refrigerant gas is then again compressed in an ongoing and repetitive process whenever the chiller is operational.
[0067] The operation of the product 10 is controlled by a controller 70 using a communications bus 72 to communicate with a plurality of components 74 , each of which provides digital or analog inputs or outputs associated with the operation of the product 10 .
[0068] Specifically referencing FIG. 2 , the variety of components 74 include quad relay outputs 76 , dual relay outputs 78 , dual triac outputs 80 , dual analog I/O 82 , dual inverter interfaces 84 , Comm 5 communication interfaces 86 , starter modules 88 , dual high voltage binary inputs 90 , dual low voltage binary inputs 92 , frame connectors 94 , devices such as expansion valves 96 , pressure sensors 98 , level sensors 102 and temperature sensors 104 . The communications interface 86 allows a building automation system 107 to integrate the operation of a product 10 with the operation of other similar or dissimilar products in a common environment. The communications bus 72 is preferably a four wire bus including a power wire supplied by a power supply 106 , a common line and two communications lines.
[0069] The controller 70 preferably includes a microprocessor 108 operably connected to the bus 72 by a line 110 , a memory portion 112 connected to the microprocessor 108 , and a user interface 114 allowing the display, reception of, and response to user input.
[0070] Now again referencing FIG. 1 , the communications bus 72 and components 74 of FIG. 2 are shown as applied in the simplified form to the product 10 of FIG. 1 . Temperature sensors 104 , 104 respectively measure the entering water temperature 120 and the leaving water temperature 122 of water cooled by the evaporator 16 . Pressure sensors 102 measure the pressure 124 within the condenser 14 , and temperature sensors 104 measure the temperature 126 . The expansion valve 28 is controlled by an expansion valve actuator 96 . Additionally, compressor capacity may be controlled by a slide valve controller 132 .
[0071] As described in the Background section, the installation, verification and configuration of a plurality of low level intelligent devices provides a plethora of opportunities for error. Operator error can be substantially reduced by limiting the number of human inputs, by cross checking each installation step, and integrating and reducing the number of installation steps.
[0072] FIGS. 3 and 4 are a diagram of the build sequence of a product 10 in accordance with the present invention.
[0073] FIG. 3 starts with a salesman 150 entering an order 152 for a product 10 into a personal computer 154 or the like and transmitting that order 152 by any conventional communication means 156 (including the internet) to a coordinating operation 160 . The coordinating operation 160 receives the order 152 , and generates a specification 162 and a bill of materials 164 .
[0074] The specification 162 describes how the parts and components are generally assembled into the product 10 . The specification 162 is stored as an electronic build document, preferably as XML format, on a server 167 with intranet and/or dialup communication access capabilities. For purposes of this application, letter codes are occasionally attached to the specification's reference numeral 162 , but the reference numeral 162 is intended to encompass all versions of the specifications.
[0075] The bill of materials 164 identifies each part and component necessary to build the product 10 identified by the order 152 . The bill of materials 164 is typically forwarded to a purchasing department 166 some period of time prior to actual manufacture of the product 10 so that the purchasing department 166 can ensure that the requisite number of parts and components are available when needed for manufacture.
[0076] Storing the specification 162 s on the server 167 with internet capabilities allows the specification 162 s to be accessed by various component suppliers 168 . The component suppliers 168 access the specification 162 , build a particular component or subassembly in accordance with the specification 162 , and test the operation of the component or subassembly. The test results are appended to the specification 162 and returned to the server 167 . Alternatively, the specification 162 could be forwarded directly to another component manufacturer to initiate the manufacture of another component, or could be forwarded to the product manufacturer for final assembly (see dashed line 165 ).
[0077] At some point, the various required components and subassemblies are completed, the results of their testing recorded in the specification 162 , and the purchasing department 167 has acquired the necessary materials as detailed on the bill of materials 164 in order to complete a final assembly of the product 10 .
[0078] In such case, the specification 162 with all component and subassembly test results is forwarded to a manufacturing unit 156 to assemble the product 10 , to attach the communications bus 72 and the components 74 to the product 10 , and to test and configure the bus 72 and the components 74 both individually and as part of a cohesive hole in the product 10 . The results of such testing and verification are appended to the specification 162 and stored in a local server database 169 . Prior to final shipment, the specification 162 L stored on the server 169 is downloaded to the manufacturing location (usually the same manufacturing location but now indicated by reference numeral 158 for the sake of clarity).
[0079] While assembly of parts, components, subassemblies and the final assembly occurs, the version of the specification 162 stored on the server 167 ( 162 s ) can be updated by “last minute” order changes from the customer. The version of the specification 162 on the server 167 ( 162 L) is therefore compared with the version of the specification stored on the local server 169 ( 162 s ) to determine if the addition of any components 74 or modifications to the product 10 are required. These modifications are made if necessary, and the components 74 are configured and verified and tested. The results are then appended to the specification 162 as integrated between the versions stored on the server 167 and the local server 169 ( 162 s , 162 L). The product 10 is then shipped to the customer.
[0080] FIG. 4 illustrates the manufacture and test of the bus 72 and component 74 in accordance with the present invention as may occur at a component manufacturer 166 or at the manufacturing location 156 , 158 .
[0081] The specification 162 is provided to a tester device 170 which generates build and test instruction 172 for building the desired product 10 . These build and test instructions 172 are preferably in the Java XML format as implemented in an XML file. The tester device 170 takes the XML file and generates installation sequence instructions 176 for the actual manufacture of the product 10 . Both the XML file 174 and the installation sequence file 176 are cross checked with the specification 162 and with the bill of materials 164 for discrepancies, errors, or omissions. Once this cross check is completed, the actual manufacture of the product 10 can be commenced. The tester device 170 builds the product 10 using the installation sequence 176 .
[0082] FIGS. 5 and 6 show a flow chart 200 directed to the manufacture of a product 10 by the tester device 170 . Although the actual manufacture of a product 10 includes the construction and assembly of the compressor 12 , evaporator 16 and condenser 14 as well as many other parts, the present invention is directed to the addition thereto of the bus 72 and its components 74 and the configuration, verification, testing and control thereof. Thus the flow chart 200 starts with the installation of the bus 72 into the product 10 as indicated by element 202 of the flow chart 200 .
[0083] Once the communications bus 72 has been installed on the product 10 , the tester device 170 verifies the operation of the bus at step 204 . Once the bus operation has been verified, the tester device 170 requests the next individual component 74 which the installation sequence 176 indicates should be installed. This is done at step 206 of the flow chart 200 . To make the request, the tester device 170 sends a signal to a display device 208 to provide a visual indication to a factory technician 210 as to the desired component 74 . Step 212 indicates that the tester device 170 waits while the technician 210 installs the requested component 74 on the product 10 and physically connects the component 74 to the bus 72 .
[0084] At step 214 the technician 210 generates a signal to the tester device 170 indicating that the component 74 has been installed. In one form of the invention, the signal is a garage door type radio signal transmitted to a receiving section 178 of the tester device 170 , identifying to the tester device 170 that the requested component 74 has been installed. In a second embodiment of the invention, the technician 210 uses a magnet actuator 220 such as a magnet or a magnetic field generator to cause the component 74 to send a signal on the bus 72 indicating to the tester device 170 that a component 74 has been added. This magnetic actuation of a signal is subsequently described.
[0085] Once the tester device 170 has received the signal from the technician 210 , the tester device 170 proceeds to step 222 and analyzes the bus 72 and the new component 74 for operability. In the first embodiment discussed above where the technician 210 uses a radio transmitter, the tester device 170 generates a further signal to the technician 210 indicating the technician 210 should use the magnetic actuator 220 . A visual or audio trigger is used to signal the technician 210 to generate step 224 and cause the component 74 to either send the electronic signal on the bus 72 or place the component 74 into a mode where it can be programmed. The technician 210 again signals the tester device 170 to indicate completion of task. In all cases, the tester device 170 recognizes the signal from the newly installed component 74 at step 230 .
[0086] At step 232 the tester device 170 then binds the component 74 as a node in the control system for the product 10 . Binding the node is a term in the industry indicating that the tester device 170 gives the component 74 a unique identity which the component 74 can use for transmitting and receiving messages on the bus 72 . The binding of a node also encompasses the tester device 170 determining the type and functionality of component 74 that has been installed (usually from the specification 162 ) and providing the appropriate operating parameters to the component 74 by means of the bus 72 as indicated by step 234 .
[0087] At step 236 , the tester device 170 checks the installation sequence 176 to determine whether all components 74 have been installed. If not, the sequence of flow chart 200 is again started at step 204 . If each component has been installed, then the tester device 170 completes operation at step 238 and appends the test results to the specification 162 .
[0088] Referring to FIG. 7 , each component 74 includes a functional portion 300 and a control portion 302 . The functional portion 300 may be any digital or analog input or output conventionally used to control product 10 including the multiplicity of components 74 described above. The control portion 302 includes a microprocessor 304 , and an external communications port 306 operably connecting the microprocessor 304 to the communications bus 72 . The microprocessor 304 includes an operable connection to the functional portion 300 allowing the control portion 302 to transfer digital or analog input or output to or from that functional portion 300 . The control portion 302 also includes a non-invasive actuating device 310 operably connected to the microprocessor 304 . Although there are a number of available non-invasive techniques, applicant prefers a normally open or normally closed (normally closed is shown) circuit which includes an element 312 movable by means of a magnetic field actuated by the magnetic actuator 220 . The technician 210 can use the magnet actuator 220 to move the element 312 from its normally closed position to an open position breaking the signal provided to the microprocessor 304 (or in the normally open position closing the circuit and providing a signal to the microprocessor 304 ). In either case, this signal change is recognized by the microprocessor 304 .
[0089] In one embodiment, the microprocessor 304 then examines a memory portion 320 to determine if the microprocessor 304 has already been provided with and has recorded an identity and operating parameters. If the microprocessor 304 does not already have an identity and operating parameters in its memory portion 320 , then the control portion 302 generates a signal on the communications bus 72 to the tester device 170 indication that the microprocessor 304 is a new node to be bound to the system. The control portion 302 then awaits a return signal from the testing device 170 providing the requisite identity and operating parameters. However, if the microprocessor 304 determined that an identity and operating parameters have already been received, then the signal from the actuating device 310 is ignored.
[0090] In another preferred embodiment, the control portion 302 always places itself in programming mode if the element 312 detects a magnetic filed. In this embodiment, the tester device 170 or controller 70 always queries a component 74 to ascertain if it has been programmed before the tester device 170 or controller 70 issues programming instructions.
[0091] FIG. 8 shows the communications bus 72 , the controller 70 , a component 74 , and a bus signal analyzer 340 electrically connected to the communications bus 72 by a flat ribbon cable 342 . The bus signal analyzer 340 is also electrically connected to the tester device 170 by an electrical connection 344 .
[0092] The communications bus 72 is shown in its preferred embodiment of a four wire flat ribbon cable including a 24 VDC line 350 , a ground line 352 , a communications plus line 354 and a communications minus line 356 . Preferably, the lines 350 , 352 are of a first larger gauge wire while the lines 354 , 356 are of a second lesser gauge wire.
[0093] The ribbon cable 342 is similarly comprised of a connection 360 to the 24 VDC line, a connection 362 to the ground line, a connection 364 to the communications plus line, and a connection 366 to the communications minus line of the bus 72 . This allows the bus signal analyzer 340 to monitor each of the lines 350 , 352 , 354 and 356 independently and in combination. Preferably, the bus signal analyzer 340 is physically attached to the bus 72 between the controller 70 and the component(s) 74 of the communications bus 72 . The bus signal analyzer 340 includes scope 370 and voltage meter 372 instruments as well as a personal computer 374 which receives signal information from these instruments 370 , 372 .
[0094] More specifically, the 24 VDC and ground signals 350 , 352 of the communications bus 72 are brought into the meter instrument 370 by lines 360 , 362 so that aspects of these signals may be analyzed. Specifically, the meter instrument 370 determines DC voltage magnitude as well as the AC component carried by the lines 350 , 352 . The DC voltage magnitude and the AC component are compared to acceptable high and low ranges stored in the PC 374 as database values. Each 24 VDC and ground signal has its own set of limits, and each signal is analyzed to determine if the signal is acceptable and, if not, which signal parameters are out of specification. The signals are also examined as a group to more intelligently pinpoint the root cause of a potential problem.
[0095] Similarly, the plus and minus communications lines 354 , 356 are brought into the scope instrument 372 as indicated by lines 364 , 366 . This enables the communications plus and minus signals to be parsed or segregated very finely to allow detailed analysis of their structure. Additionally, the magnitudes of each of the plus and minus communication signals are examined and compared to predetermined acceptable ranges. Since the preferred embodiment of the communications bus and its protocol is implemented as RS485, various aspects of the communications plus and minus signals are looked at and compared to specified acceptable ranges. For RS485, the differential signal is key to proper communications and the acceptable range is not the limits per RS485 (which can be as low as 0.2 volts differential) but rather the design limits of the controller 70 and components 74 used. The bus signal analyzer 340 verifies that the signals are within these design limits which carry significant margin above what RS485 requires. This ensures robust field operation when applied to environments with wide variations in noise.
[0096] The communication signals 354 , 356 are also looked at for proper common load characteristics. The magnitude of the communications plus and minus signals are looked at with respect to ground. Even though the RS485 specification allows for huge variations in common mode values since RS485 really only cares about the differential, the limits for common mode operations are held very tightly, in fact far tighter than what RS485 specifications require. Empirical knowledge of the communications circuitry involved is used to determine these acceptable ranges. The common mode values vary only so much based upon leakages, tolerances, fanout and other parameters including the design characteristics. Variances indicate from the common mode values causes the bus signal analyzer 340 to generate an alarm even though communications are good as far as the RS485 specifications are concerned. Using the information connected from all signals, the root cause solution is determined and annunciated to an operator such as the assembly technician 210 .
[0097] The bus signal analyzer 340 also examines differential and common load aspects of the signal in each of the logic 1 and logic 0 states since different problems manifest differently. By looking at both states and including these in the signal analysis, a root cause is more clearly identified as well as minimizing the probability of an undetected problem. The bus signal analyzer 340 also distinguishes the signals being driven by the controller 70 and the component 74 . Since the bus signal analyzer 340 is directly communicating but at line 344 with the tester device 170 , the bus signal analyzer 340 knows which component 74 is communicating at any particular time. Thus the signals from that component 74 may be directly analyzed and the identification and annunciation of any problems occurs immediately.
[0098] The bus signal analyzer 340 continually monitors the bus so that if the connection of a component 74 to the bus 72 results in the bus 72 going out of specification, immediate annunciation of the problem occurs and the problem is identified immediately.
[0099] It will be apparent to a person of ordinary skill that many modifications and alterations are contemplated in the present device and invention. Such modifications and alterations include application to the wide variety of other devices, the modification of the bus 72 to forms other than a flow wire system including fiberoptic, coaxial cable, wireless and other forms of communication. All such modifications or alterations are contemplated to fall within the spirit and scope of the claimed invention. | A method of manufacturing a product having a plurality of components where at least some of the components are manufactured by different companies at differing locations. The method comprises the steps of: providing an electronic specification sheet describing the product and its components; forwarding the specification sheet to one of the several companies; the specific company building the component or product; the specific company testing the component or product; the specific company appending the test results to the specification; the specific company determining if the product is completed; and either shipping the finished product to the customer or forwarding the specification to another one of the several companies. | 6 |
COPYRIGHT NOTICE
[0001] A portion of the disclosure of this patent document contains material, which is subject to copyright protection. The copyright owner has no objection to the facsimile reproduction by anyone of the patent document or the patent disclosure, as it appears in the Patent and Trademark Office patent file or records, but otherwise reserves all copyright rights whatsoever.
BACKGROUND OF INVENTION
[0002] The present invention relates to a novel design for a respiratory medicament and therapy data system. It enables a new level of efficiency in charting patient progress, medicament delivery, patient follow-up, therapy session data and the like that is adapted to matingly connect with all standardized respiratory devices commonly utilized in all lung and respiratory disease treatment, testing, rehabilitation, medicament delivery and life support devices.
[0003] Currently patients with lung disorders and respiratory ailments undergo testing, medicament delivery, monitoring, phlegm dislodgment therapy, lung expansion therapy and other related medical procedures. Many of these are done in the hospital under medical supervision, while others are done unsupervised at home or are used in a hospital in conjunction with a ventilator. This may be a simple as a nebulizer aerosol medicament session or a positive exhalation pressure exercise (PEP) regime done at home. The problem the results of these go uncharted and possibly may be orally reported. The overall actual physical results of these are often charted however there is no ongoing record of each of these occurrences and what actually transpired on a lung inhalation basis for future trending analyses. This is a huge downfall of respiratory disorder treatment. Because they occur so frequently and often unsupervised, the overall effect or progress of these treatments is not always discernable, even to those medically trained in the industry. One glaring example of this, is the inability to actually know how often the patient is actually personally using their portable nebulizer or rescue inhaler. More on point, would be the inability of the respiratory disease treatment industry to tabulate the actual medicament delivered to a patient's lungs, or how often they really used their PEP device.
[0004] Henceforth, a respiratory medicament and therapy data system that can provide respiratory data to reflect the therapy sessions and treatments administered to a patient would fulfill a long felt need in the respiratory disease treatment industry. This new invention utilizes and combines known and new technologies in a unique and novel configuration to overcome the aforementioned problems and accomplish this.
SUMMARY OF THE INVENTION
[0005] In accordance with the invention, the objects of the present invention, which will be described subsequently in greater detail, is to provide a respiratory medicament and therapy data system capable of using a “breath actuated” monitoring device that monitors patient interactions with all respiratory therapy and drug delivery devices.
[0006] It is a further object of this invention to provide a respiratory medicament and therapy data system that generates a signal based on values of the inhalation and exhalation pressures generated by a patient using a respiratory therapy, lung function test device or a drug delivery device.
[0007] It is another object of this invention to provide a respiratory medicament and therapy data system capable of tracking and wirelessly reporting the various sessions of therapy medicament delivery with respect to such parameters as delivery date, time, duration, total delivered dose and the like.
[0008] It is still another object of the present invention to provide a respiratory medicament and therapy data system capable of calculating and reporting the actual dose of medication delivered into a patient's lungs following an aerosol medicament delivery session.
[0009] It is still a further object of this invention to have respiratory medicament and therapy data system that may be powered by a battery, connect seamlessly and without any performance issues in a plethora of respiratory devices, and transmit its respiratory data wirelessly to a local computing device or smart phone with a wireless signal receiver.
[0010] It is a final object respiratory medicament and therapy data system to provide a fool-proof system for recording and immediately displaying the results of the respiratory therapy or drug delivery that have been algorithmically derived on a localized device and that can be sent to the medical provider's patient treatment database (health portals) for later, remote review by medical personnel.
[0011] The respiratory medicament and therapy data system has many of the advantages mentioned heretofore and many novel features that result in a new level of patient reporting which is not anticipated, rendered obvious, suggested, or even implied by any of the prior art, either alone or in any combination thereof.
[0012] 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
[0013] FIG. 1 is a side perspective view of the smart adaptor;
[0014] FIG. 2 is a side perspective view of the smart adaptor with the protective housing removed;
[0015] FIG. 3 is an exploded view of the smart adaptor;
[0016] FIG. 4 is a cross sectional view of the smart adaptor without the protective housing;
[0017] FIG. 5 is a top view of the smart adaptor without the protective housing;
[0018] FIG. 6 is a left side view of the smart adaptor without the protective housing;
[0019] FIG. 7 is a bottom view of the smart adaptor without the protective housing;
[0020] FIG. 8 is a proximal end view of the smart adaptor without the protective housing;
[0021] FIG. 9 is a right side view of the smart adaptor without the protective housing;
[0022] FIG. 10 is a distal end view of the smart adaptor without the protective housing;
[0023] FIGS. 11-19 are views of the smart phone screen displays taken from various user input requests;
[0024] FIG. 20 is a flowchart of the operational steps of obtaining respiratory session data; and
[0025] FIG. 21 is a flowchart showing the operational steps of a pressure sensing event.
DETAILED DESCRIPTION
[0026] 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.
[0027] 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.
[0028] 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.
[0029] As used herein, the term “inhaled dose” refers to the amount of inhaled drug for a time interval of nebulization (generally one minute).
[0030] As used herein, the term “delivered drug dose” refers to the aggregate amount of aerosol medicament determined to have reached the patient's lungs in a single nebulizer treatment/session. This is determined knowing how many breaths the patient took, when they took the breaths, how long each inhalation lasted, the output of the aerosol generator per unit time, the concentration of the drug and any attenuation/efficiency factors taken into consideration.
[0031] As used herein, the term “nebulizer system” refers to a respiratory medicament aerosol generator.
[0032] As used herein, the terms “microprocessor” or “logic chip” means a computer processor on a microchip that contains all, or most of, the central processing unit (CPU) functions and is the “engine” that goes into motion when the pressure sensor sees a change in the pressure exerted upon it. It incorporates a real time clock and either or both of volatile/non volatile memory and performs arithmetic and logic operations based on input signals or data from remote devices such as the pressure transmitter, or manually operated electrical switches. It outputs operational signals that integrates with other electrical circuits. It may also output algorithmically derived data to an external computing device. (This may be a local computer, smart phone, or a health provider's network via a remote server.) These operations are the result of a set of instructions that are part of the microprocessor design as is well known in the industry. In simple terms, the microprocessor is a multipurpose, programmable device that accepts digital data as input, processes it according to instructions stored in its memory, and provides results as output.
[0033] As used herein the term “pressure sensor” means an electromechanical device that converts an external pressure (or a change in a the external pressure) of a gas or fluid exerted on the sensor, into an electrical signal. The electrical signal generated is a function of the pressure exerted on the sensor. Pressure sensors are also commonly called pressure transducers, pressure transmitters, pressure senders, pressure indicators, piezometers and manometers, among other names. Common types of pressure sensors are piezoresistive strain gauges, capacitive, electromagnetic, piezoelectric, optical and potentiometric.
[0034] As used herein, the term “personal mobile device” refers to a device that is both portable and capable of collecting, storing, transmitting or processing electronic data or images. Examples include laptops or tablet PCs, personal digital assistants (PDAs), and “mobile smart” phones. This definition also includes storage media, such as USB hard drives or memory sticks, SD or CompactFlash cards, and any peripherals connected to the device.
[0035] As used herein, the term “mobile smartphone” means any web-enabled mobile phone. While the term “smartphone” is well known in the art, smartphones typically include a touch sensitive screen, a messaging client, global positioning systems (GPS) technology or any other geo-position mechanisms to determine the physical coordinates of the smartphone, and a browser application. The browser application employs any web-based language such as JavaScript Object Notation (JSON), JavaScript, HyperText Markup Language (HTML), or any other web-based programming language capable of sending and displaying messages, search queries, and search query results.
[0036] Looking at FIGS. 1 and 2 , the smart adaptor 2 of the respiratory medicament and therapy data system can best be seen. It has a generally hollow tubular, circular adaptor body 4 having an unobstructed, open proximal end 6 and an unobstructed, open distal end 8 , so as to allow the unhampered passage of respiratory gases and medicaments therebetween. As illustrated in FIGS. 3 and 4 , in the approximate center of the body 4 is an orifice 16 into which part of the “smart” assembly is affixed. The “smart assembly” is a breath monitoring and wireless reporting device. This “smart” assembly is a miniaturized pressure sensor 10 mounted on a printed circuit board 9 (which is generally laminar, non-conductive substrate) that mechanically supports and electrically, operationally connects all of the electronic components of the smart assembly. This includes the wireless transmitter's integrated circuitry, a battery 40 , a micro switch 15 , ( FIG. 9 ) the pressure sensor 10 and the microprocessor 50 necessary for functionality as is well known in the industry. (Generally, this battery will be of a “coin” style configuration.) There is a detachable battery 7 that functions to activate the micro switch 15 . There is a related health care management software application (Welltrac) that is a set of computer instructions intended for downloading onto a personal mobile device (generally a cellular smart phone or computer tablet) however it may be operated on any computing device. This software enables the microprocessor and memory in the cell phone to interact with the incoming wireless data sent from the smart adaptor 2 as well as any of its own data such as time and date, and run any software program algorithms, tabulate, store, format and display the aggregated data in a medically informative format. Basically, once installed to a mobile personal device it will allow the transmission, reception, interpretation and display of data from said breath monitoring and wireless reporting device to the personal mobile device.
[0037] It may act as a counter, considering only separate occurrences of inhalation/exhalation, or it may consider the duration and magnitude of the inhalation/exhalation pressures for additional respiratory determinations.
[0038] The only component that will be in physical contact with the gases/fluid flowing through the body 4 will be the pressure sensor 10 . The pressure sensor 10 will be sealed to or about the perimeter of the orifice 16 by its tight mechanical interference fit with an external peripheral seal of silicone or other resilient material so as to remain in operational contact with the respiratory gases. This seal may reside on the pressure sensor 10 , on the PCB plate 9 , in or adjacent the orifice 16 on the body 4 . The other components of the smart assembly 2 will be encased in a protective housing 24 . In this way the body 4 may be cleaned from time to time with water and dish soap or isopropyl alcohol without damage to the electronics.
[0039] The pressure sensor 10 of the preferred embodiment is a gauge pressure sensor that measures the pressure relative to atmospheric pressure. Thus when it indicates zero, then the pressure it is measuring is the same as the ambient pressure. Other types of pressure sensors may be utilized such as sealed pressure sensors or differential pressure sensors as is well known in the industry. These may require modifications to the body 4 as would be well known by one skilled in the art.
[0040] The pressure sensor selection has taken into consideration that it must detect an inhalation pressure (negative pull) of <(−) 2 cm H2O and when used in a positive pressure application, the pressure sensor will be exposed to positive peak pressures in excess of (+) 90 cm H2O. The pressure sensor will be exposed to temperatures and humidity consistent with human respiration; 98.6° F./37° C. at 98% RH for 30 minutes 3-4 times per day. The senor tip may come in contact with respiratory therapy medications and human saliva. The pH of the respiratory drugs range from 3.5 to 7.4. The pH of saliva is 6.5-7.5. The operating temperature ranges from 20-50 degrees C. and the cleaning temperature ranges from 20 to 110 degrees C.
[0041] It is the one of the goals to have the body 4 designed for fool-proof connection. Since the operation of the pressure sensor 10 is not affected by the direction of the gaseous flow through the tubular body 4 , the body cannot be installed in a wrong direction. There is thus no need for directional arrows on the body 4 . The pressure sensor 10 resides in orifice 16 but the wall thickness of the body 4 in that region is chosen to be thicker than the depth of the pressure sensor 10 such that the pressure sensor 10 does not extend into the flow cavity of the body 4 . In this way, while the pressure sensor 10 may be covered by an extreme insertion of a respiratory device, it cannot be damaged by such action.
[0042] However, there are two remaining areas where installation could be a problem. The first occurs when during the installation, the mated respiratory device is inserted too far into the body 4 so as to cover the internal opening 16 for pressure sensor 10 (rendering it inoperable) or jam up against the housing for the smart assembly and dislodging or operationally separating any of its components (rendering it inoperable and possibly unrepairable). Obviously, this would not be a problem if the length of the body 4 were extreme, e.g. in the range of 6 inches or more, but this is not practical, as when the length of the adapter increases so does the internal surface area which allows for more condensation of aerosol medicament, resulting in a lesser amount of medicament reaching the patient's lungs. Also, as the length increases, the frictional losses for gas flowing through the body 4 proportionally increase. This can disrupt any other readings being taken by connected respiratory equipment or reduce the strength of the pressure wave reaching a patient's lung from a PEP therapy session. Neither of these are desirable effects. For this reason the body's overall length is minimized, miniaturized components are used and the only end sized for insertion of a respiratory apparatus, is the distal end 8 which sees an interior abutment stop 20 before the orifice 16 . ( FIG. 10 ) This safeguards the smart assembly from physical damage by the unintended abutment of a mated respiratory device into the body 4 so as to cover the pressure sensor 10 .
[0043] In the same way, there is an exterior abutment stop 27 adjacent the proximal end 6 to protect the over insertion of the smart adaptor 2 into a respiratory device. ( FIG. 8 ) In the preferred embodiment the body 4 has an overall length from distal end 8 to proximal end 6 of approximately 46 mm.
[0044] The proximal end's male fitting configuration is designed to accept connection of a respiratory device on or inside of its circular body. The distal end's female socket configuration is designed for connection of a respiratory device by its insertion into the inside of its body. Looking at FIGS. 4, 8 and 10 it can be seen that the external diameter of the male fitting approximates the internal diameter of the female socket. The male fitting supports an 18 mm diameter internal connection and an external diameter that supports a 22 mm diameter external connection (it can fit internally into a 22 mm diameter connection.) The female fitting has an internal diameter that supports a 22 mm diameter fitting. In this way the body 4 may be connected in a plethora of different ways to the most common sizes of respiratory fittings.
[0045] In its simplest form, the respiratory medicament and therapy data system consists of an adaptor 2 fitted with an electronic pressure sensor 10 and a wireless transmitter powered with a coin battery 40 and operatively connected on a substrate printed circuit board 9 , that act to count the breaths taken by a patient and wirelessly report this number to a health portal (such as Microsoft HealthVault or Apple Health Kit) or to a personal mobile device that has downloaded and runs the companion mobile software application (Welltrac) thereon that tabulates, records in memory, and displays this data as a health management tool. Optionally, the actual pressures sensed and their duration will be wirelessly sent for a more intricate level of medical result reporting.
[0046] In the In the preferred embodiment the wireless transmission is done via Bluetooth wireless technology protocol (using short-wavelength UHF radio waves in the ISM band from 2.4 to 2.485 GHz) although other protocols may be substituted such as ultra wideband or induction wireless, to name a couple. The preferred embodiment uses a Bluetooth Dialog Semiconductor SmartBond (DA14580) and a SM1120-1100H-A-G or SM9520-040M-G-D SMi pressure sensor. The power switch is a Magnetic KSK-14OA Series Reed switch. It has a normally closed (NC) configuration that will control the power to the integrated circuit. The smart adaptor 2 will come packaged with an appropriately matched magnet affixed to its exterior that will hold the NC micro reed switch in the open position. When the magnet is removed the switch will revert to the NC position and the circuit will be activated. Replacing the magnet will turn off the smart adaptor 2 . The battery will be a Lithium coin style battery with a nominal voltage of 3.0 volts, generally designated in the industry as a CR1025 battery.
[0047] Dimensionally, as stated earlier the electrical components are miniaturized. In the preferred embodiment the pressure sensor will be in the 700 micron×220 micron×75 micron range, the coin battery will be in the 20 mm diameter with a 3.2 mm thickness range, the wireless transceiver will have dimensions in the 2.5 mm×2.5 mm×0.5 mm range and the power switch will have a length of 4.1 mm and a diameter in the 1.25 mm range. All components will fit onto a substrate with a maximum dimension of 15 mm×15 mm. With all components operationally assembled on substrate, the thickness will be less than 5 mm. The silicon plug to seal the pressure sensor will have a diameter of approximately 2.5 mm. FIGS. 5-7 and 9 illustrate the general spatial arrangement and relative sizing of the smart adaptor 2 .
[0048] In operation, the system works in the following way. ( FIG. 20 ) The personal mobile device accesses the internet and downloads the respiratory health kit software application (Welltrac) into its memory for integration with its operating system such that all of the application's instructions and algorithms are functionally operational. The smart adaptor 2 is fit between a respiratory treatment or therapy device and its mouthpiece. (Although placement elsewhere in the respiratory circuit may also allow for full functionality.) The exterior, detachable magnet 7 is removed from the smart adaptor 2 such that the micro switch 15 powers up the smart adaptor 2 . The smart adaptor 2 utilizing Bluetooth handshake technology, is paired with any other compatible local Bluetooth device it had been previously paired with. At this stage there is none. The personal mobile device is set to the bluetooth ‘pairing mode’ and finds the smart adaptor 2 and connects the two for wireless communication via the connection protocol for that personal mobile device's operating system. The health care management software application (Welltrac) is accessed on the personal mobile device and its operational, interactive screens and visual prompts are shown on the display. The smart adaptor's battery level is optionally displayed on the personal mobile device. A window for the input of data (initial or updated) about the date, time, patient (name, age, sex, weight, height, race, and the like) respiratory type of sessions, scheduled sessions, type of respiratory device used, and optionally, the doctor's data, medicament and medicament specifics (i.e. concentration) The smart adaptor 2 sends respiratory session data to the personal mobile device as it is available. This is accomplished by industry standard wireless data transfer protocol that includes receipt verification prior to data erasure from the smart adaptor as is well known in this field of art.
[0049] Looking at FIG. 21 the operational logic for the transfer of data from the smart adaptor 2 to the personal mobile device is set forth in flowchart format. When powered, the smart adaptor 2 sits dormant until the sensor 10 detects a pressure change. If there is an ongoing session its adds the data to that session (stored in the smart adaptor's memory) and resets its timer. If the pressure sensor 10 does not detect any further pressure changes before the timer expires, the session is closed and the complete data set for that session is sent to the personal mobile device for interpretation, storage and display. This transfer of data follows any of the conventional data transfer and verification “handshake” protocols commonly utilized and well known in the industry. If there is another pressure change detected before the timer expires it is added to the session and the timer is reset. Once the session is ended and the data is sent to the personal mobile device, after the data transfer and verification protocol is completed, that data is marked as sent, and earmarked for eventual deletion from the smart adaptor. It is to be noted that the smart adaptor 2 , having its own memory may be used without connection to a personal mobile device. (It is capable of storing numerous sessions and retaining them for eventual transfer upon pairing with a suitable personal mobile device.) Upon the establishment of the Bluetooth connection, if there is any session data on the smart adaptor 2 not marked as sent, it will be relayed to the personal mobile device. (See FIG. 21 ) The compiled data is saved to memory, displayed and optionally sent to another computing device via email or synched to a health portal where it can be tagged to the patients medical record. In this manner patients and caregivers can see and track their respiratory progress. (The health portal is accessed through the personal mobile device. On the initial setup of the Weltrac application on the personal mobile device, the user will define an account or profile for that patient, given a username and password. on a dedicated Welltrac server portal. Upon establishment of this Welltrac account, the respiratory data may be transferred for storage to this server portal. This server portal has the communication capability to link with the various healthcare information portals so as to enable the transfer of that patient's data into that patient's discrete medical file.)
[0050] The respiratory health kit software application (Welltrac) when accessed on the personal mobile device, and logged in ( FIG. 18 ) allows the user, the interactive display of user information ( FIG. 14 ), reminder input ( FIG. 16 ), active reminders ( FIG. 15 ), session schedule status ( FIG. 11 ), respiratory therapy equipment selection ( FIG. 13 ) session history ( FIG. 12 ), and equipment instructions ( FIG. 20 ), smart adaptor battery status, last date and time of synchronization, progress status based on input goals. The Welltrac application also initiates session reminders ( FIG. 17 ) in an alarm function even when it is not not active on the display screen. It is to be noted that the user assignment of the type of respiratory device that the smart adaptor 2 is connected ( FIG. 13 ) (e.g. nebulizer, PEP device, OPEP etc.) is critical to the personal mobile device's properly analyzing and reporting the respiratory therapy session. The actual identification of the type of respiratory device may also be transmitted to the personal mobile device by a wireless transmitter on the respiratory device, when available.
[0051] When the Welltrac software application is accessed it initiates the personal mobile device to attempt to detect other nearby devices operating the same type of wireless technology (such as the smart adaptor 2 ) and electronically “pair it” with the personal mobile device. (Multiple smart adaptors may be paired on the same personal mobile device.)
[0052] It is noteworthy that smart adaptor may be fabricated in various levels to work with the health kit software application (Welltrac). In the most sophisticated version when the patient inhales or exhales, the smart adaptor 2 will sense the change in atmospheric pressure whether it be a decrease or increase in pressure over the ambient atmospheric pressure and it will send a wireless signal to the paired personal mobile device that is proportional to the magnitude and direction of the pressure change throughout the duration of the pressure change. In this level the personal mobile device will open a reporting session that will record the date, the time, the magnitude and direction of the pressure changes, the number of pressure changes, and the length of the pressure changes. Using algorithms from the software application, and optionally input data (such as medicament, medicament concentration etc.) the personal mobile device will interpret the results of the session into a displayable format for the selected type of respiratory session previously chosen. This may include data as to the strength of the breath pulses, the duration, the amount of medicament received, timing between breaths and the like. This above and beyond what interpretive data the basic level of smart adaptor generates. The basic level merely counts the breath pulses, compiling them into sessions and sends them to the personal mobile device where they will show if the scheduled session was done, when for how long and the number of breaths taken.
[0053] In simplified terms the method of reporting data from a the breath monitoring and wireless reporting device comprises the steps of:
[0054] installing a breath monitoring and wireless reporting device software application onto a personal mobile device;
[0055] connecting a smart adaptor having a breath monitoring and wireless reporting device to a respiratory medicament delivery and/or respiratory therapy device;
[0056] powering on said breath monitoring and wireless reporting device of said smart adaptor;
[0057] allowing a pressure sensor to generate a data set of the number of breaths taken by a patient during a respiratory medicament delivery session or a respiratory therapy session;
[0058] storing said data set in a memory of said breath monitoring and wireless reporting device;
[0059] pairing said personal mobile device to said smart adaptor and establishing a wireless communication between said smart adaptor and said personal mobile device;
[0060] transferring said data set to an operating system of said personal mobile device utilizing a data transfer protocol with a data receipt acknowledgment;
[0061] interpreting said data set and generating a set of results on said personal mobile device; and
[0062] providing a visual display of said set of results on a screen of said personal mobile device.
[0063] Optionally, the step of allowing a pressure sensor to generate a data set of the number of breaths taken by a patient during a respiratory medicament delivery session or a respiratory therapy session, may also include associating the breaths taken with a time and date, a magnitude, a duration and a direction, and incorporating into said data set.
[0064] 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 respiratory medicament and therapy data system capable of using a “breath actuated” monitoring device that monitors patient interactions with all respiratory therapy and drug delivery devices. It generates a signal based on the magnitude, direction and duration of the inhalation and exhalation pressures generated by a patient. This allows the tracking and wireless reporting of the various therapeutic and medicament delivery sessions with respect to such parameters as delivery date, time, duration, total delivered dose and the like. The respiratory medicament and therapy data system provides a fool-proof system for recording and immediately displaying the results of the respiratory therapy or drug delivery that have been algorithmically derived on a localized device and that can be sent to the medical provider's patient treatment database (health portals) for later, remote review by medical personnel. | 0 |
PRIORITY
[0001] This application claims the benefit of the provisional application having Ser. No. 60/707,207 filed on Aug. 10, 2005, which is hereby incorporated in its entirety by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to writing instruments and more particularly to a writing instrument that has a cosmetic compartment and mirror.
[0004] 2. Description of the Prior Art
[0005] Cosmetic applicators have been known in the prior art for some time. These applicators tend to be large, bulky and heavy. The size and weight of these applicators is directly related to the need for room for the cosmetic and means of application.
[0006] In U.S. Pat. No. 2,057,085, to G. J. Danco, a cosmetic applicator for lipstick is shown comprising an outer protective casing that is adapted to serve as a handle for applying the cosmetic to the user. The disclosed device includes flexible applicator band rotatably disposed on a complicated roller assembly. The user rotates the applicator band passed the cosmetic disposed in an interior of the housing, thereby picking up the cosmetic for application on the user. The disadvantage of the present reference is that it is complicated, difficult and time consuming to use. Additionally, the device is limited to the application of the cosmetic contained in the housing.
[0007] There have also been devices developed to remove a cosmetic or make-up from a user. In U.S. Pat. No. 6,148,828, to Bourassa, a device is disclosed comprising a casing having a wiping tip protruding from one of its ends. Similar to the device to Danco above, a slidable ribbon of wiping material is disposed in the casing. The Bourassa device includes a storage compartment (an interior of the casing) for holding unused wiping material until it is advanced over the wiping tip, used and eventually feed into a refuse compartment. A disadvantage of the present device is that it includes a complicated advancement mechanism to advance the wiping material from the storage compartment to the refuse compartment. Additionally, the device is limited to the removal of a cosmetic or make-up material.
[0008] What is needed is a device that provides uncomplicated access to and/or application of a cosmetic to a user. What is additionally needed is a device that can be utilized for something other than the storage or application of a cosmetic.
SUMMARY OF THE INVENTION
[0009] The invention is a writing instrument having cosmetic compartment and/or mirror disposed to a housing or barrel that can be griped by a user during use. The housing can contain a writing implement such as a pen cartridge or a make-up applicator that can be used with the cosmetic compartment to apply a cosmetic to a user.
[0010] A wipe material can be removably stored in an interior of the housing for selective removal by a user through a slot or slit extending through and along at least a portion of the length of the housing. The wipe material can be saturated with chemical to aid in the removal of the cosmetic. In another embodiment, the wipe material can be impregnated with a scent that would be pleasant to the user. The scent can be a perfume that the user wipes upon themselves at any time of the user's choosing.
[0011] A nose cap can be removably coupled to an end of the housing to secure the ink cartridge for writing. The nose is also adapted to retain the wipe material in the interior of the housing. In one example embodiment, the nose cap can have a shape, size, or configuration to allow it to be used as the applicator for the cosmetic contained within the cosmetic compartment.
[0012] A nose cap cover can be removably coupled to and telescopically extend over the nose cap to provide a means of protecting the nose cap. The nose cap cover can have an attachment means formed, coupled and the like thereto to permit convenient transportation of the device.
[0013] An end cap can be coupled to an end of the housing opposite the nose cap. The end cap is utilized to secure a free end of the ink cartridge in the housing. In the example embodiment having a wiping material, the end cap can be utilized to retain the wiping material in the interior of the housing.
[0014] In one example embodiment of the invention, the cosmetic compartment is disposed to the end cap during transportation and/or while the device is being used as a writing instrument. An inner cover can be hingedly coupled proximate to an opening of the cosmetic compartment to define an interior for retaining the cosmetic.
[0015] A mirror cap or reflective end cover can be disposed to an end of the cosmetic compartment to allow a user to observe the application of the cosmetic.
[0016] An object of the invention is to provide a writing instrument having a cosmetic compartment that is easily manufactured and used.
[0017] Another objection of the invention is to provide a cosmetic compartment containing that is visually integrated with the housing of the writing instrument.
[0018] The above summary of the invention is not intended to describe each illustrated embodiment or every implementation of the invention. The figures in the detailed description that follow more particularly exemplify these embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The invention will be better understood and objects other than those set forth above will become apparent when consideration is given to the following detailed description thereof. Such description makes reference to the annexed drawings wherein:
[0020] FIG. 1 is an exploded view of a writing instrument and cosmetic compact according to an example embodiment of the present invention.
[0021] FIG. 2A is a perspective view of a nose cap according to an example embodiment of the present invention.
[0022] FIG. 2B is a cross section view along line 1 - 1 of the nose cap of FIG. 2A .
[0023] FIG. 2C is an end view of the nose cap of FIG. 2A .
[0024] FIG. 2D is a partial perspective view of FIG. 2C .
[0025] FIG. 3A is a cross sectional view of a nose cap cover of FIG. 1 showing an interior thereof.
[0026] FIG. 3B is an end view of the nose cap cover of FIG. 3A showing an opening extending therethrough.
[0027] FIG. 3C is cross section view of the nose cap cover of FIGS. 3A and 3B illustrating a cosmetic applicator assembly in an extended position.
[0028] FIG. 3D is a cross section view of the nose cap cover of FIGS. 3A and 313 illustrating a cosmetic applicator assembly in a retracted position.
[0029] FIG. 4A is a side view of a coupling member for receiving a tether or the like for hanging the writing instrument and cosmetic compact about a user's neck.
[0030] FIG. 4B is a perspective view of the coupling member of FIG. 4A .
[0031] FIG. 5A is an exploded perspective view of an end cap assembly comprising an outer end cap and an inner end cap according to an example embodiment of the present invention.
[0032] FIG. 5B is a cross section view of the outer end cap of FIG. 5A .
[0033] FIG. 5C is an end view of the outer end cap of FIG. 5A .
[0034] FIG. 5D is a cross section of the inner end cap of FIG. 5A .
[0035] FIG. 5E is an end view of the inner end cap of FIG. 5A .
[0036] FIG. 6A is an enlarged view of an end of the outer end cap showing a coupling assembly.
[0037] FIG. 6B is a top view of the coupling assembly of FIG. 6A .
[0038] FIG. 7A is a perspective view of a reflective member and cosmetic compact according to an example embodiment of the invention.
[0039] FIG. 7B is a side view of the cosmetic compact of FIG. 7A .
[0040] FIG. 7C is an end view of the cosmetic compact of FIG. 7A .
[0041] FIG. 7D is a side view of the reflective member of FIG. 7A .
[0042] FIG. 7E is an end view of the reflective member of FIG. 7A .
[0043] The preceding description of the drawings is provided for example purposes only and should not be considered limiting. The following detailed description is provided for more detailed examples of the present invention. Other embodiments not disclosed or directly discussed are also considered to be within the scope and spirit of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0044] Referring to FIGS. 1-7E , a writing instrument and cosmetic compact is indicated by the number 100 . Writing instrument and cosmetic compact 100 includes a housing, barrel, or pen tube 110 having an open first end 112 and an open second end 114 in registration with each other.
[0045] Referring to FIG. 1 , in a preferred embodiment, housing 110 is manufactured from a polymer such as polypropylene, polyethylene and the like. Housing 110 can be manufactured with any color, design or lettering printed on its outer surface for advertising of a particular trademark, logo, or brand. This is of particular importance if the writing instrument and cosmetic compact 110 is utilized as a marketing tool since vivid colors, designs and lettering typically attract a user's eyes and others toward the writing instrument.
[0046] To ensure that housing 110 is comfortable to use it may have a generally cylindrical shape. However, housing 110 may have any cross sectional shape such as, for example triangular, square, oval, and the like. An outer surface of housing 110 may be coated and/or ribbed to increase tactile feel and improve comfort. A compressible sleeve (not shown) can be slid over housing 110 to provide additional comfort for a user.
[0047] In one example embodiment, as illustrated in FIG. 1 , an ink, marker or similar writing cartridge 125 is removably disposed within housing 110 . Writing cartridge 125 has a first writing end 128 that can be disposed proximate open first end 112 of housing 110 and second securing end 129 proximate open second end 114 of housing 110 . Writing cartridge 125 can dispense an ink, a cosmetic such as eyeliner, lipstick, or the like. In one embodiment, ink cartridge 125 dispenses an ink having the properties to be initially invisible or undetectable to the naked eye, only to reappear after a duration of time or the application of heat, another chemical, or the like.
[0048] Referring to FIGS. 2A-2D , and initially to FIG. 2A , a nose cap 130 can be removably disposed over open first end 112 of housing 110 to provide support to writing cartridge 125 . In one example embodiment, nose cap 130 has a generally conical shape with a generally conical tip portion 132 and a generally annular collar portion 134 . Referring to FIG. 2C , the generally annular collar portion 134 has an outer diameter generally greater than an outer diameter of tip portion 132 . As particularly illustrated in FIGS. 2B-2D , nose cap 130 can have a lower or bottom wall 135 for supporting ink cartridge 125 when disposed in housing 110 . An annular channel 136 extends into annular collar portion 134 and about bottom wall 135 for receiving open first end 112 of housing 110 .
[0049] In one example embodiment, nose cap 130 can be threadedly coupled to housing 110 . In another example embodiment, nose cap 130 can be pressure fitted to housing 110 . Other fastening methods and means are also possible and should be considered to be within the spirit and scope of the invention.
[0050] Referring to FIG. 2B , when nose cap 130 is disposed on housing 110 , first writing end 128 of writing cartridge 125 extends through holes 137 and 137 ′ extending through tip portion 132 and bottom wall 135 respectively.
[0051] Referring to FIGS. 1 and 3 A and 3 B, a nose cap cover 141 can be provided to prevent first writing end 128 of writing cartridge 125 from drying out. The nose cap cover 141 has a top or upper wall 142 and a peripheral wall 144 extending away therefrom. Referring to FIGS. 7A-7C , peripheral wall 144 has an edge 146 defining an access opening 148 for receiving nose cap 130 . Nose cap cover 141 can comprise any generally rigid material such as plastic, wood, metal or the like.
[0052] Referring to FIGS. 3C 3 D, nose cap cover 141 can include a cosmetic applicator assembly 150 operatively disposed in an interior 152 thereof for applying the cosmetic on the user. In one example embodiment, the cosmetic applicator assembly 150 comprises a brush, elongate generally absorbable pad, or other like applicator 154 that is operatively disposed in and extendable from an interior of the housing 110 . The applicator can have a first end 156 that is extendable through an opening 157 in the upper wall 142 of the nose cap cover 141 .
[0053] A second end 158 of the applicator 154 can be attached to a slide mechanism 160 that is utilized by a user to move the applicator 154 between an extended position (see FIG. 3C ) and a retracted position (see FIG. 3D ). The extended position is defined by the first end 156 of the applicator 154 extending through the opening 157 of the nose cap cover 141 . The retracted position is defined by the applicator 154 being substantially enclosed in the nose cap cover 141 .
[0054] In one embodiment, the slide mechanism comprises at one elongate slide 162 having a knob portion 164 extending through an elongate slot or slit 166 in the peripheral wall 144 of the nose cap cover 141 . A user can user their thumb or finger to move the knob portion 164 along the slot or slit 166 and concomitantly, vertically move the applicator 154 between the extended and retracted positions. An outer surface of the knob portion 164 can include knobs, ribs, ridges, protrusions and the like 168 to facilitate the grip of the user's thumb or finger on the knob while moving it between the extended and retracted positions.
[0055] In one embodiment of the invention, as illustrated in FIG. 1 , an edge 170 defining the slot or slit 166 in the peripheral wall 144 of nose cap cover 141 can include spaced apart recesses or protrusions 172 that receive or interact with a portion of slide or knob portion 168 or slide 162 to retain the applicator in a relatively fixed position while being used. Other types of mechanisms are possible to facilitate the at least temporary fixing of the applicator 154 in either the extended or retracted position and should be considered to be within the spirit and scope of the invention.
[0056] In another embodiment of the invention, the applicator 154 can be removably disposed to another portion of the housing 110 . In this embodiment, the applicator 154 can be removably disposed to the second end 114 of housing 110 or other portion conducive to holding or receiving the applicator 154 in any form.
[0057] Referring to FIGS. 4A and 4B , a coupling member 180 such as an eyelet, loop, hook, strap, tether, and similar devices can be coupled to the peripheral wall 144 of nose cap cover 141 to allow a user to more easily carrying the writing instrument and cosmetic compact 100 . In an example embodiment, as illustrated in FIGS. 4A and 4B , coupling member 180 comprises an eyelet having plug portion 182 joined to and extending from an anchoring portion 184 . Plug portion 182 is adapted for operative engagement to any portion of writing instrument and cosmetic compact 100 , but preferably the peripheral wall 144 of nose cap cover 141 .
[0058] In an example embodiment, plug portion 182 can include a conical section 186 disposed on an end of a shaft section 188 that is centrally disposed on anchor portion 184 . Conical section 186 is adapted for operative engagement with at least one hole 187 extending into nose cap cover 141 .
[0059] Anchor portion 184 can include a base section 190 and an attachment section 192 . The shaft section 188 is disposed on an upper surface of base section 190 while the attachment section 192 is disposed on a lower surface of base section 190 . In on example embodiment, attachment section 192 comprises a loop that is adapted to receive a tether or similar device. Attachment member 180 can comprise any compressible material such as rubber, plastic and the like.
[0060] Referring now to FIGS. 1 and 5 A- 5 E, at least one end cap assembly 200 is detachably couplable to the open second end 114 of housing 110 for holding the second end 129 of writing cartridge 125 . In one embodiment, end cap assembly 200 comprises an inner end cap 202 and an outer end cap 204 with the outer end cap 204 adapted to receive the inner end cap 202 and a compartment 400 adapted to hold a cosmetic.
[0061] Referring to FIGS. 5A and 5B , the outer end cap 204 includes a generally centrally disposed wall 206 having a peripheral wall 208 extending diametrically from opposed surfaces of the wall 206 such that a bottom rim or lip 210 (see FIG. 5B ) of the peripheral wall 208 defines an access opening 212 for receiving the inner end cap 202 . An upper rim 214 of the peripheral wall 208 defines an access opening 216 for receiving the compartment 400 .
[0062] Outer end cap 204 includes a post 217 a having a bore 217 b extending longitudinally therein for receiving and at least temporarily securing cartridge 125 . Post 217 a is centrally disposed on and extends from the central wall 206 . In another example embodiment, as particularly illustrated in FIG. 5C , post 217 a is divided along its longitudinal axis defining first 218 and second 220 post portions that extend away from each other when writing cartridge 125 is inserted in bore 217 b . In this embodiment, an inner diameter of bore 217 b is at least slightly smaller than an outer diameter of writing cartridge 125 to create a friction fit therebetween.
[0063] Referring to FIGS. 5A, 5D , and 5 E, inner end cap 202 is operatively coupled between housing 110 and outer end cap 204 to secure outer end cap 204 to housing 110 . In an example embodiment, as particularly illustrated in FIG. 5D , inner end cap 202 has a top wall 222 and a peripheral wall 224 extending away therefrom forming an interior space 226 . A pair of supports 228 and 228 ′ can be disposed in and extend generally across the interior space 226 . Supports 228 and 228 ′ can comprise plates or panels having a length generally equal to a length of peripheral wall 224 .
[0064] Top wall 222 of inner end cap 202 has a generally centrally disposed aperture 230 extending therethrough for receiving post 217 a . In an example embodiment, post 217 a is disposed generally between supports 228 and 228 ′. Inner end cap 202 can be secured in outer end cap 204 by an adhesive or other mechanical means such as by threaded engagement.
[0065] Inner end cap 202 can also include a tab 232 extending away from an outer surface of its peripheral wall 224 for operatively engaging and securing inner end cap 202 and outer end cap 204 to housing 110 . In an example embodiment, as illustrated in FIGS. 1 , tab 232 can operatively engage a slit 234 and a notch 236 extending transversely therefrom into housing 110 . To secure inner end cap 202 to housing 110 , tab 232 is inserted and slid within slot 232 . Tab 232 becomes aligned with notch 234 . Rotation of inner end cap 204 forces tab 232 into notch 234 such that it extends transversely through notch 234 preventing its disengagement from housing 110 . Other means of engaging inner end cap 203 to housing 110 are also contemplated by the invention, for example threaded engagement, pressure fitting, and snap fitting.
[0066] Referring to FIGS. 6A-7E , and initially to FIGS. 7A-7E , the compartment 240 includes a bottom wall 242 and a peripheral wall 244 extending away therefrom defining an interior 246 . A cosmetic 247 , such as lip gloss, lipstick, eye shadow, and the like is disposed in the interior 246 of the compact 240 . As illustrated in FIG. 7C , compact 240 has a generally circular cross section. However, depending upon the cross sectional shape of housing 110 and outer end cap 204 , compact 240 can have any cross sectional shape. In one embodiment, the outer end cap 204 and the compact 240 are manufactured from a clear material such that the cosmetic 247 is visible from outside of writing instrument and cosmetic compact 100 .
[0067] Referring back to FIG. 5A , compact 540 has a size and shape adapted for fitting into recess opening 216 of outer end cap 204 . In one embodiment, compact 240 is pressure fitted in the access opening 216 to temporarily secure compact 240 within outer end cap 204 until a user pulls on an end of compact 240 thereby removing it from the outer end cap 204 . In another embodiment of the invention, an outer surface of the peripheral wall 244 of compact 240 may be threadedly coupled to an inner surface of the peripheral wall 208 of the outer end cap 204 . Other methods and means of coupling, securing, fixing, attaching the compact 240 to the outer end cap 204 are also possible and should be considered to be within the spirit and scope of the invention.
[0068] Referring to FIGS. 7A, 7D and 7 E, a mirror or similar reflective member 300 can be coupled to outer end cap 204 to permit a user to observe themselves while applying the cosmetic. Reflective member 300 can comprise a housing 302 having a top wall 304 and a peripheral wall 306 defining an interior 308 thereof. A reflective mirror or similar surface 310 can be disposed in the interior 308 . In an alternate embodiment, an inner surface of top wall 304 can be polished to create a reflective surface, thereby eliminating the need for a separate mirror.
[0069] As illustrated in FIG. 7D , a lip 312 can extend beyond the mirror. Lip 312 can be used to operatively couple reflective member 300 to the outer end cap 204 . As illustrated in FIG. 6A a pair of prongs 314 and 314 ′ can extend from lip 214 of outer end cap 204 . Each of the prongs 314 and 314 ′ includes a protrusion 316 and 316 ′ respectively that can engage a portion of reflectively member 300 . As illustrated in FIG. 7E , housing 302 of reflective member 300 can include a pair of slots 318 and 318 ′ for receiving prongs 314 and 314 ′ respectively. An inner surface of slots 318 and 318 ′ can include depressions for receiving protrusions 316 and 316 ′. In this particular embodiment, reflective member 300 is hingedly coupled to outer end cap 204 between an open position and a closed position. Reflective member 300 can also be threadedly coupled, pressure fitted, or snapped on outer end cap 204 . Other forms of engagement are also contemplated and should be considered to be within the spirit and scope of the invention.
[0070] As illustrated in FIG. 6A , the compact 240 can extend beyond the lip 214 of outer end cap 204 . The reflective member 300 can include a space defined by its lip 312 such that when the reflective member 300 is in the closed position the compact 240 can extend into at least a portion of the interior 308 of the reflective member 300 . When the reflective member 300 is closed its lip 312 surrounds the compact 240 .
[0071] After purchase, a user lifts the reflective member 300 exposing the compact 240 . The user can then pull, rotate, pivot and the like to remove the compact 240 from the outer end cap 204 . Once the compact 240 has been removed, the user can press, slide, or otherwise move knob portion 164 such that the first end 156 of the applicator 154 extends through the opening 157 of the nose cap cover 141 .
[0072] The user then places the tip or first end 156 of the applicator 154 into the cosmetic 247 to pick up some cosmetic for placing on their lips, eyelids or other bodily features. A user can then retract the applicator 154 back into the nose cap cover 141 for storage.
[0073] A user can also remove the nose cap cover 141 to expose the cartridge 125 to right a message, note, and the like on a piece of paper. However, upon writing a message on the substrate, a user notices that no ink has apparently been disposed on the substrate. In example embodiments, the ink can reappear after a predefined period of time; if the user blows their warm breath on the ink soaked substrate; or if the user applies another chemical such as lemon juice and the like.
[0074] In another embodiment, the ink may comprise a chemical or material, such as luminol. Once a light is placed on the ink soaked substrate it will illuminate the written message.
[0075] In yet another embodiment, a user can write a message in reverse with the invisible ink contained in the ink cartridge 125 . Another user can then use reflective member 300 and the light chemical, breath and the like to read the reversed message.
[0076] In another embodiment, wipes impregnated or soaked in a cleaning solution can be rolled up and placed in the interior of housing 110 such that when a user wants to remove the cosmetic they can pull the wipe through slit 234 of the housing 110 . In this example embodiment, the roll of wipes can include a plurality of wipes connected linearly by spaced transversally extending perforations.
[0077] Numerous modifications are also contemplated in the present invention. For example, all parts of writing instrument and cosmetic compact 100 can be manufactured from a single material or they may comprise any combination of various materials. Advertising, logos, designs and other indicia can be imprinted or imparted on any component of writing instrument and cosmetic compact 100 including, but not limited to, housing 110 , nose cap 130 , cover 160 , nose cap cover 140 , and/or end cap 170 .
[0078] The present invention may be embodied in these and other specific forms without departing from the spirit or essential attributes thereof, and it is therefore desired that the present embodiment be considered in all respects as illustrative and not restrictive, reference being made to the appended claims rather than to the foregoing description to indicate the scope of the invention. | A writing instrument and cosmetic compact having a writing cartridge disposed in a housing or barrel adapted to receive a compact designed to hold a cosmetic or similar makeup. The ink cartridge can be filled with an ink that is only visible upon interaction with another medium such as a light source, another chemical, or warmed or heated air. | 0 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The present application claims the benefit of the filing date of U.S. Provisional Patent Application No. 62/072,305, filed Oct. 29, 2014, the disclosure of which is hereby incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] Fibrous elements have long been used by the automotive industry to form moldable fiber products. These products may utilize knitted fabrics, woven fabrics, and nonwoven fabrics. Exemplary nonwoven fabrics may be needle punched, spun bonded, spun laced, thermally bonded, or chemically bonded.
[0003] Most thermally bonded nonwoven fabrics are made by intimately blending a high melt temperature fiber with a low melt temperature fiber. This allows the low melt temperature fiber to be melted during a heating process, such as thermoforming, to form a stiff, molded portion of the fabric. Thermoforming may be used, for example, to conform the molded portion to a surface of an automobile. Not all fibrous elements perform equally when heated. For example, most low melt temperature fibers have a glass transition temperature (“Tg”) of less than 90° C.; many high melt temperature fibers are similarly limited. As a result, many nonwoven fabrics are limited to a maximum heat deformation temperature of 90° C.
[0004] While a deformation temperature of 90° C. or less is adequate for many interior applications, the advent of using fibrous products in exterior areas as well as near engine components has driven the need for higher heat deformation temperatures. For example, many automotive manufacturers are now demanding nonwoven fabrics with a heat deformation temperature of at least 120° C. Demands for nonwoven fabrics having a heat deformation temperature of 150° C. are also common.
[0005] A deformation temperature of 120° C. can be achieved by using Polypropylene (“PP”) as the low melt temperature fiber. But PP starts to soften at 140° C. and fully melts at 165° C. Thus, PP cannot be used to meet a deformation temperature of 150° C. Polyester or Nylon may be used as high melt temperature fiber; however, they do not recyclable back into itself. Thus, neither the molding scrap nor the finished products are recyclable back into themselves for new production. Both of these challenges limit the usefulness of PP or Polyesters within moldable fabrics.
[0006] Excessive deformation is another concern. For example, deformation may be detrimental to vehicle safety if the molded portion is exposed to the exterior of the vehicle. Deformation of a molded exterior portion is also detrimental to the appearance of the vehicle and can create stress on the fastening systems. Thus, deformation resistance is also a performance requirement of any moldable fabric.
[0007] Bi-component fibers have also been used to make moldable fiber products. Typically, these fibers have a core-sheath configuration, wherein an exterior sheath formed from the low temperature melt fiber is coaxial with an interior core formed from the high temperature melt fiber. Some bi-component fibers may be adapted to have a heat deformation temperature greater than 150° C. For example, some bi-component fibers employ crystalline polymers that melt at 160-185° C. Yet even these “high temperature” fibers may not be ideal for use in a moldable fabric because, once melted, they revert to an amorphous structure with a Tg of 70-90° C. As a result, any moldable fabric made with existing bi-component fibers may suffer from excess deformation if exposed to temperatures greater than 90° C. Moreover, while most bi-component fibers can be recyclable, the recycling process may be greatly complicated by the bond between the exterior sheath and the interior core.
[0008] In addition to the performance requirements stated above, many moldable fiber products must also meet strict performance requirements for airflow, flexibility, flame resistance, smoke resistance, and durability. For example, some products must achieve a significant reduction in airflow (or increase in “Rayls,” the measurement of airflow resistance) and have a flexural modulus optimized for strength and durability.
[0009] These additional requirements can be difficult to meet because many known fiber elements are porous. As a result, many existing products may distort and fail by absorbing (or adsorbing) water, oil, and other engine fluids.
[0010] This problem is related to flame and smoke resistance. For example, a product that is more likely to absorb oil is also less likely to be flame and smoke resistant; instead, such products are more likely to generate large amounts of smoke as the oil burns off during a fire.
[0011] Generally, most fibrous products will absorb or adsorb water, oil, and other engine fluids, which increase the weight which causes them to distort and fail. Further, there is a need to improve flame resistance to a much higher standard than the MVSS-302 test. There is also a need to reduce smoke generated for the safety of vehicle occupants in case of a fire.
[0012] A need exists for a product that does not exhibit failure during heat aging up to 150° C.; has resistance to water, oil, and engine fluids, has low flame spread and low smoke, and is recyclable back into itself. Further, these moldable products must have excellent abrasion resistance against sand & gravel.
[0013] Therefore, need exists for a moldable fabric adapted to meet the performance characteristics noted above. Further improvements are required.
SUMMARY OF THE INVENTION
[0014] The invention utilizes a low melt fiber made from a co-polyester where cyclohexane dimethanol (CHDM) has been substituted for some of the ethylene glycol normally polymerized with Purified Terephthalic Acid to produce Polyester polyethylene terephthalate (PET). The result is a polymer called PETG for a glycol modified PET polymer. The melting point of the PET polymer can be adjusted from 110° C. to 170° C. by adjusting the ratio of CHDM to ethylene glycol (EG).
[0015] Mono-component fibers are made from PETG using PET melt spinning equipment and are produced in a wide variety of deniers and lengths. The drying of the resin chips must be performed at below 70° C. with desiccant air and preferably with continuous agitation. The fibers are produced using a 4.5 inch extruder with metering pumps, 1500 hole round spinnerettes, and standard air quench. The spun fiber is drawn on a standard draw line with draw ratios between 2 and 3.5:1. The fibers may be cut to length from 0.5″ to 4′ and placed in a bale. The fibers remain completely amorphous after drawing unlike regular PET, which crystallizes.
[0016] The PETG fibers are blended with standard polyester fibers that are heat set to 170° C. and above. During blending fiber finishes such as Goulston L624 (fluorocarbon) may be applied during blending. Other finishes such as Lurol 14951 may be blended with L624 to achieve fire retardant characteristics. Anti-stats such as ASY are added to improve run ability especially with low humidity in manufacturing buildings.
[0017] The blended fibers were then carded, cross-lapped, and needled on a standard nonwoven line to form fabrics from 200 gsm to 2,000 gsm. These fabrics were subsequently molded in a standard thermos-forming operation. When the PETG melted it flowed uniformly and formed meniscus at the bond points of the high melt fibers. The level of the PETG percentage control the stiffness and the air flow resistance.
[0018] Fibers made from Polylactic Acid (PLA) such as fibers made from Cargill's PLA Ingeo polymer the have been drawn and fully crystallized with a melting point of 140° C. and above are blended with Polyester (PET) fibers that have been heat set at 170° C. or above.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] FIG. 1 show a graph comparing sound transmission of various moldable fabrics by measuring normal impedance absorption coefficient against Frequency.
[0020] FIG. 2 shows the relationship between the flexural modulus of various moldable fabrics and temperature.
[0021] FIG. 3 shows relative sizes for five fibers used within some of the examples described herein.
[0022] FIG. 4 is a flow diagram illustrating applying finishing material on the composite for heat exposure in automotive applications.
DETAILED DESCRIPTION
[0023] Although the present invention is described with reference to specific embodiments of a moldable fabric for automotive applications, it is to be understood that the concepts and novelty underlying the present invention could be utilized for non-automotive applications. The present invention is also described with reference to a number of exemplary embodiments, some of which are described as having a particular range of values, such as temperature and the like. It should be further appreciated that these exemplary embodiments, and their associated numerical ranges, merely provide a convenient way of describing the present invention and are not intended to limit this description to any particular example or associated numerical range.
[0024] The present invention is directed to various embodiments of moldable fabric and methods for manufacturing the same. The fabric is comprised of a plurality of fiber elements. The moldable fabric may comprise any combination of low melt temperature fibers and high melt temperature fibers. Any portion of the plurality of fibers may also consist of mono-component fibers, bi-component fibers, or any combination thereof.
[0025] In one embodiment, the moldable fabric comprises at least one low melt temperature fiber. Each low melt fiber is preferably made from a copolyester material formed by modifying a base material, such as ethylene glycol (“EG”). Preferably still, the copolyester material includes cyclohexanedimethanol (“CHDM”). For example, CHDM may be substituted for an amount of EG that is normally polymerized with purified terephthalic acid (“PTA”) to produce polyester (“PET”). The resulting copolymer material is called polyethylene terephthalate glycol modified (“PETG”). As described fully below, the melting point of PETG can desirably be adjusted from 110° C. to 170° C. by adjusting the ratio of CHDM to EG. This makes PETG ideal for use as a low melt temperature fiber.
[0026] A moldable fabric in accordance with the present invention can also be made from biopolymer materials. For example, the low melt temperature fiber may alternatively be made with polyactid (“PLA”) polymers. An exemplary PLA fiber may include any number of PLA polymers owned by Natureworks, LLC, and sold under the trademarked brand name of Ingeo®. Specific examples include the following fiber types: 6201D, 6202D, 6204D, 6400D, 3001D, 4032D, 4043D, and 4060D. Each of these PLA fibers have a heat deformation temperature of 140° C. and, thus—like many PETG fibers, may readily serve as the low melt temperature fiber.
[0027] Each low melt temperature fiber described above is blended with at least one high melt temperature fiber to form the moldable fabric. Each high melt fiber can be made of a polyester material. In each example set forth below, at least one PETG fiber is blended with a polyster fiber that has been heat set to a temperature that exceeds the melting point of the low melt temperature fiber. In some examples, the polyester fiber is heat set to approximately 175° C. or greater. The amount of PETG or PLA fibers controls the stiffness and the air flow resistance of the moldable fabric. Preferably, the percentage of PETG or PLA fiber in the moldable fabric is between 1% to 60% by weight.
[0028] Each of the low and high melt temperature fibers may be comprised of plurality of fiber types, each type having a variable color, denier, and length. Multiple low or high melt fiber types may also be combined. An exemplary set of fibers is depicted in FIG. 3 , which corresponds to Examples 7 and 8 below. In FIG. 3 , each fiber element has a denier per filament of between 1 to 15 and a maximum length of between 0.5 inches to 6 inches. An even greater variety of fiber types may also be formed using any combination of any fiber type described below in Examples 1-10.
[0029] Any PETG fiber element described herein can be made with known melt spinning equipment, including any known equipment that was originally adapted for use with PET. Known methods of manufacture, however, must be modified to accommodate the use of PETG. For example, a fiber element produced from either PET or PETG can be produced from resin chips. PETG resin chips must be dried at a temperature of less than 70° C. using desiccated air, preferably with continuous agitation. Once dried, then the PETG resin chips may be extruded to produce a spun PETG fiber. For example, the PETG chips may be extruded through a 4.5″ extruder having at least one metering pump, a 1,500 hole round spinneret, and a standard air quench. The spun PETG fibers are then drawn on a standard draw line, cut to length, and then placed in a bale or like form. Unlike regular PET, which crystalizes, it should be appreciated that a PETG fiber element will remain completely amorphous after drawing.
[0030] In a preferred embodiment, the spun PETG fibers are drawn to have a minimum draw ratio of approximately 2 and a maximum draw ratio of approximately 3.5:1. The draw ratio may include any value intermediate of this range. For example, the draw ratio may range from approximately 2:1 to 3.5:1; from 2:1 to 3:1; from 2.5:1 to approximately 3.5:1; or any other intermediate range. Likewise, each fiber is preferably cut to have a minimum of length of approximately 0.5″ and a maximum length of approximately 4′. Intermediate values of the draw length are also contemplated. For example, the length may range from approximately 0.5″ to 6″; from 5″ to 2′; from 1′ to 3′; from 2′ to approximately 6′; or any other intermediate range.
[0031] To produce a moldable fabric, the PETG fibers described above are typically blended with another fibrous element. As noted above, the PETG fibers may serve as the low melt temperature fiber, whereas another fibrous element serves as the high melt temperature fiber. Preferably, the PETG fibers are blended with polyester fibers that have been heat set to approximately 170° C. or more. The fibers are then carded, cross-lapped, and needled on a standard nonwoven line to form a moldable fabric. This blend typically has a minimum weight of 200 grams per square meter (or “GSM”) and a maximum weight of 2,000 GSM. The fabric may also be blended to have any intermediate range of weights. For example, the blended fabric may have a weight that ranges from 200 to 2,000 GSM; from 200 to 500 GSM; from 400 to 1,000 GSM; from 500 to 1,500 GSM; or any other intermediate range.
[0032] Subsequent to blending, at least a portion of the moldable fabric may be formed into a molded portion by application of heat. The molded portion is preferably formed by heat that is applied with known thermoforming techniques. The amorphous nature of the PETG fibers is particularly suited to this process. For example, when the PETG fibers are melted, then the melted flows uniformly with respect to with the high melt temperature fibers to form a meniscus at each bond point with the high temperature melt fibers. This allows the molded portion to conform to any underlying shape without comprising the strength of the moldable fabric. Any known heating process may be used to achieve similar results. For example, the moldable fiber may be heated in any of a contact oven, an infrared oven, a convection oven, a like heating element, or a combination thereof.
[0033] Various elements of the manufacturing methods disclosed herein may be further modified to make alternate embodiments of the moldable fabric. For example, the percentage of PETG in each fiber element may be varied to control the stiffness of the molded portions. Because PETG flows in a uniform manner when melted, the percentage of PETG in each fiber may also be varied to control the air flow resistance of the fabric.
[0034] Additional materials may also be applied to any fibrous element described herein. For example, the PETG or PLA fibers described above may be treated with a performance enhancing finish, either during fiber formation or fiber blending. The finish types may vary. In some embodiments, the finish is comprised of a fluorocarbon, such as the CF fluorocarbon sold by Goulston Technologies as FC-L624. This enhances the durabity and heat resistance of the moldable fabric. In other embodiments, the finish is comprised of an inorganic phosphate salt, such as that sold by Goulston Technologies as L-14951. This enhances the durability and heat resistance of the moldable fabric. In either instance, the performance enhancing finish preferably does not exceed 0.05% to 1.0% of the fiber weight. An alternate finish may also be comprised of a combination of a fluorocarbon and an inorganic phosphate salt to achieve fire retardant characteristics. Preferably, this alternate finish does not exceed 0.05% to 2.0% of the fiber weight. An anti-static element, such as ASY, may also be added to improve run ability, especially when the moldable fiber is manufactured within a low humidity environment.
EXAMPLE 1
[0035] Historically, fiber blends at a weight of 1000 GSM were made using a combination of polyester and co-polyester fibers. A first sample in accordance with a historical blend comprises: (i) 65% of 6d×3″ polyester fibers with a heat set of 175° C. (NwN Z201); and (ii) 35% of 4d×2″ bi-component copolymer fibers with a PET internal core (Huvis). Once blended, this first sample was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and then trimmed to the shape of a trunk liner.
[0036] After aging at 90° C. for 24 hours, the first sample showed significant distortion. Water was immediately absorbed into the fabric during testing with 3 mL of water. All trim scrap was recyclable back into PET pellets.
EXAMPLE 2
[0037] A second sample was produced at 1200 GSM using polypropylene as a binding agent. This blend of fibers in this second sample comprises, for example: (i) 60% of 6d×3″ polyester fibers at with a heat set of 175° C. (NwN Z201); and (ii) 40% of 6d×3″ black PP fibers (Drake Extrusion). Once blended, this second sample was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and trimmed to the shape of a wheelhouse liner.
[0038] After aging at 90° C. for 24 hours, this second sample showed very little deformation. Water was slowly absorbed into the fabric during testing with 3 mL of water. Trim scrap was not recyclable back into PET pellets.
EXAMPLE 3
[0039] A third sample was produced at 1200 GSM using the following blend: (i) 60% of 6d×3″ polyester fibers with a heat set of 175° C. (NwN Z201); (ii) 40% of 4d×2″ bi-component copolymer fibers with a PET internal core (Huvis); (iii) 20% of 1.5d×1.5″ PLA fibers (NwN 2438). Once blended, this third sample was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and then trimmed to the shape of an underbody aero shield.
[0040] After aging at 90° C. for 24 hours, the sample showed no distortion. Water was not absorbed into the fabric during testing with 3 mL of water. Trim scrap was recyclable back into PET pellets; however, this third sample sample showed inadequate flexural modulus and marginal noise reduction.
EXAMPLE 4
[0041] A fourth sample was produced at 1350 GSM using the following blend: (i) 20% of 5d×3″ polyester fibers with a heat set of 175° C. (NwN Z201); (ii) 20% of 15d×3″ polyester fibers with a heat set of 175° C. (NwN Z202); (iii) 20% of 4d×2″ polyester fibers with a heat set of 175° C. (NwN Z203) ; and 40% of 4d×2″ bi-component copolymer fibers with a PET internal core (Huvis). Once blended, this fourth sample was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and trimmed to the shape of an underbody aero shield.
[0042] After aging at 90° C. for 24 hours, the sample showed some distortion. Water was absorbed into the fabric during testing with 3 mL of water. Trim scrap was recyclable back into PET pellets. This fourth sample desirably showed adequate flexural modulus and improved noise reduction.
EXAMPLE 5
[0043] A fifth sample was prepared at 1350 GSM using the following blend: (i) 20% 6d×3″ polyester heat set to 175° C. (NwN Z201); (ii) 20% 15d×3″ polyester heat set to 175° C. (NwN Z202); (iii) 20% 3d×2″ Polyester heat set to 175° C. (NwN Z203); and (iv) 40% of 4d×2″ bi-component copolymer fibers with a PET internal core (Huvis). Once blended, this fifth was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and trimmed to the shape of an underbody aero shield.
[0044] After aging at 90° c for 24 hours, the sample showed some distortion. Water was absorbed into the fabric during testing with 3 mL of water. Trim scrap was recyclable back into PET pellets. This fifth sample desirably showed adequate flexural modulus and improved noise reduction.
EXAMPLE 6
[0045] A sixth sample was prepared at 1200 GSM using the following blend: (i) 20% of 6d×3″ polyester heat set to 175° C. (NwN Z201); (ii) 20% of 15d×3″ polyester heat set to 175° C. (NwN Z202); (iii) 20% of 3d×2″ Polyester heat set to 175° C. (NwN Z203); (iv) 30% of 4d×2″ bi-component copolymer fibers with a PET internal core (Huvis); and (v) 10% of 1.5d×1.5″ PLA fibers (NwN 2438). Once blended, this sixth sample was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and then trimmed to the shape of an underbody aero shield.
[0046] After aging at 90° C. for 24 hours, the sample showed no distortion. Water was not absorbed into the fabric during testing with 3 mL of water. Trim scrap was recyclable back into PET pellets. This sixth sample desirably showed adequate flexural modulus and improved noise reduction.
[0047] Sample six was also tested in the “gravelometer” equipment and found to pass 300 pints of gravel showing excellent abrasion. It also passed the standard automotive Tabor test with excellent results. It had outstanding flexural modulus so that it could be installed more easily with less labor on the vehicle assembly line.
EXAMPLE 7
[0048] A seventh sample was prepared at 1200 gsm using the following blend: (i) 20% of 6d×3″ polyester heat set to 175° C. (NwN Z201); (ii) 20% of 15d×3″ polyester heat set to 175° C. (NwN Z202); (iii) 20% of 3d×2″ polyester heat set to 175° C. (NwN Z203); (iv) 30% of 4d×2″ bi-component copolymer fibers with a PET internal core (Huvis); and (v) 10% of 1.5d×1.5″ PLA fibers (NwN 2438). After blending this fourth sample was heated at 210° C. for 30 seconds, placed in cold mold for 60 seconds, and then trimmed to the shape of underbody aero shield.
[0049] After aging at 90° C. for 24 hours, the sample showed no distortion. Water was not absorbed into the fabric during testing with 3 mL of water. Trim scrap was recyclable back into PET pellets. This seventh sample desirably showed adequate flexural modulus and improved noise reduction.
[0050] There was a 50% reduction in cycle time of the seventh sample as compared to the sixth sample. This seventh sample was tested in the gravelometer equipment and was found to pass 200 pints of gravel showing excellent abrasion. This sample also passed the standard automotive Tabor test with excellent results.
EXAMPLE 8
[0051] An eighth sample was prepared at 1350 GSM using the same blend as the seventh sample set forth above. The fabric was needle punched to a thickness of 15 mm. During blending, a fluorocarbon finish (Goulston Technologies; FC L624) was applied at the rate of 0.20% on weight of fiber; and an inorganic phosphate salt finish (Lurol; FR-L987) was added at 0.5% by weight of fiber. Once blended and finished, this eighth sample was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and then trimmed to the shape of an underbody aero shield.
[0052] After aging at 90° C. for 24 hours, the sample showed no distortion. Water was not absorbed into the fabric during testing with 3 mL of water. Trim scrap was recyclable back into PET pellets. Desirably, this eighth sample showed excellent flexural modulus and improved noise reduction.
EXAMPLE 9
[0053] A ninth sample was prepared at 1600 GSM with the following blend: (i) 50% of 6d×3″ black polyester heat set to 185° C. (Z258P); (ii) 15% of 6d×3″ black polyester with Phosphate FR, heat set to 185° C. (Z2546); (iii) 25% of 4d×2″ PETG fibers with a 160° C. melt point (Z2708); and (iv) 10% of 2.5d×2″ PLA fibers with a 175° C. melt point (Z2438). During blending, a fluorocarbon finish (Goulston Technologies; FC L624) was applied at the rate of 0.20% on weight of fiber; and an inorganic phosphate salt finish (Lurol; FR-L14951) was added at 0.5% by weight of fiber. The fabric was needle punched to a thickness of 15 mm. Once blended and finished, this ninth sample was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and then trimmed to the shape of an underbody aero shield.
[0054] After aging at 120° C. for 24 hours, the sample showed no distortion. Water was not absorbed into the fabric during testing with 3 mL of water. Trim scrap was recyclable back into PET pellets. Desirably, this ninth sample showed excellent flexural modulus and improved noise reduction.
[0055] This ninth sample was also tested in the “gravelometer” equipment and was found to pass 300 pints of gravel showing excellent abrasion. It also passed the standard automotive Tabor test with excellent results. It had outstanding flexural modulus so that it could be installed more easily with less labor on the vehicle assembly line. This ninth sample also showed outstanding resistance to oil, water, anti-freeze, and other engine fluids.
EXAMPLE 10
[0056] A pair of tenth samples were run at 1200 and 1600 gsm respectively with the following blend: (i) 55% of 6d×3″ black polyester heat set to 185° C. (Z258P); (ii) 15% of 6d×3″ black polyester with Phosphate FR heat set to 185° C. (Z2546); and (iii) 30% of 4d×2″ PETG fibers with a 160° C. melt point (Z2708). During blending, a fluorocarbon finish (Goulston Technologies; FC L624) was applied at the rate of 0.20% on weight of fiber; and an inorganic phosphate salt finish (Lurol; FR-L14951) was added at 0.5% by weight of fiber. The fabric was needle punched to a thickness of 15 mm. Once blended and finished, this ninth sample was heated at 210° C. for 60 seconds, placed in cold mold for 60 seconds, and then trimmed to the shape of an underbody aero shield.
[0057] After aging at 150° C. for 24 hours, the sample showed no distortion. The finished molded part achieved the VO designation on the ASTM E-84 flame test. Water was not absorbed into the fabric during testing with 3 mL of water. Trim scrap was recyclable back into PET pellets. Desirably, this tenth sample showed excellent flexural modulus and improved noise reduction.
[0058] This tenth sample was also tested in the gravelometer and found to pass 300 pints of gravel showing excellent abrasion. It also passed the standard automotive Tabor test with excellent results. It had outstanding flexural modulus so that it could be installed more easily with less labor on the vehicle assembly line. This tenth sample showed outstanding resistance to oil, water, anti-freeze, and other engine fluids.
[0059] Adverting to the drawings FIG. 1 is a graph that illustrates the relationship between normal incidence absorption coefficient and sound frequency. As shown in the graph in FIG. 1 , at frequencies above 200 hz the normal incidence absorption coefficient maintains about a constant value as sound frequency increases for a current production LX Aero Production. Samples D, E, and F made using the teachings of the invention show a remarkable increase in absorption coefficient as frequency increases. The absorption coefficient is defined as the relationship between the acoustic energy that is absorbed by a material and the total incident energy impinging upon it. This coefficient should be limited between 0 (not absorbent at all, i.e. reflective) and 1 (totally absorbent).
[0060] FIG. 2 further illustrates the advantages of the present invention over currently available material. Shown in FIG. 2 is a bar graph that illustrates an additional acoustic property advantage over current state of the art material. Shown in FIG. 2 are samples D, E, and F as compared to the current available material tested. As shown in various testing environments both at ambient temperature (20C) and elevated temperature (90C), samples D, E, and F outperformed the current material tested.
[0061] FIG. 3 illustrates relative sizes for five fibers used within some of the examples described herein. Shown is a 3, 6 and 15 denier PET fibers. Also illustrated is a 4 denier bi-component fiber and a 1.5 denier PLA fiber. Smaller deniers are preferred for sound dampening or acoustical impedance purposes as explained below.
[0062] The surface area of a non-woven fabric is directly related to the denier and cross-sectional shape of the fibers in the fabric. Smaller deniers yield more fibers per unit weight of the material, higher total fiber surface area, and greater possibilities for a sound wave to interact with the fibers in the fabric structure. Acoustical absorption properties of nonwoven fabrics depend on a variety of variables including fiber geometry and fiber arrangement within the fabric structure. Different structures of fibers result in different total surface areas of nonwoven fabrics. Nonwoven fabrics such as vertically lapped fabrics are ideal materials for use as acoustical impedance or insulation products, because they have a high total surface. Vertically lapped nonwoven technology include for example, but are not limited to, carding, perpendicular layering of the carded webs, and through-air bonding using synthetic binder fibers.
[0063] FIG. 4 illustrates a flow diagram for a non-woven fabric. Shown as an example, PET fiber 400 , with PETG fiber 410 and PLA fiber 420 is blended in a blending machine 430 . A finishing application 450 is accomplished adding additives for example those shown, but not limited to, additives in block 440 . A fabric formation 46 is made that may be further molded as a product as shown in molding fabric 470 or utilized as a nonwoven fabric in an extrusion process.
[0064] Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as described by the appended claims. | Described are fibrous products for molding for use in Automotive products such as Underbody Aero-shields, wheel house liners, and Engine compartment applications with enhanced heat aging capability, abrasion resistance, and resistance to water, oils, and other fluids and is recyclable. The fibrous products also have acoustical benefits such as improved acoustical impedance or sound dampening properties over currently available acoustic insulation materials. | 3 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a machine tool for machining a workpiece, and more particularly, to an automatic machine tool which is kept clean, less frequent in malfunction and low in manufacturing cost. It further relates to an automatic machine tool suitable for arrangement on a transfer line.
2. Discussion of the Prior Art
In conventional machine tools and particularly, in those for cutting operation, it is often that cutting chips and coolant scatter during machining operation to contaminate the machine tool and other devices therefor.
The machine tool is provided with a plurality of slide surfaces along which a spindle head with a cutting tool is moved in vertical and horizontal directions, to be accurately positioned to a machining position. During the machining operation, parts of the scattering cutting chips, coolant and so on adhere to the slide surfaces. This causes deterioration in machining accuracy and malfunction of the machine tool. Particularly, in a transfer line system including a plurality of automatic machine tools, the malfunction of one automatic machine tool adversely affects the whole of the transfer-line system.
To overcome the aforementioned problem, each of the slide surfaces is provided with a slide cover. An assembly of plural telescopic members of steel or flexible bellow is used as the slide cover. However, the manufacturing cost of the slide cover is relatively high. Further, drawbacks are involved in that the slide covers restrict the areas for attachment of other devices such as an automatic tool changer and also harm working accessibility for workers.
SUMMARY OF THE INVENTION
Accordingly, it is a primary object of the present invention to provide an improved machine tool wherein slide surfaces for a spindle head can be protected at a low cost from contamination by coolant, cutting chips and so on.
Another object of the present invention is to provide an improved machine tool wherein its components such as an automatic tool changer and the like can also be free from contamination by coolant, cutting chips and so on.
Still another object of the present invention is to provide an improved machine tool suitable for arrangement on an automated machining line.
Briefly, a machine tool comprises a spindle head base, a spindle head rotatably supporting a vertical tool spindle, a guide mechanism provided on the spindle head base and guiding the spindle head in mutually orthogonal first and second horizontal directions and in a vertical direction, a workpiece support base provided at a front side of the spindle head base for supporting a workpiece, a side cover assembly surrounding the workpiece on the workpiece support base so as to define a machining area therewithin, and a top cover assembly cooperating with the side cover assembly to cover the upper end of the side cover assembly and having a spindle hole through which a nose portion of the spindle head passes so as to permit the tool spindle to reach the machining area. The top cover assembly is flexibly operable to follow the movements of the spindle head in the first and second horizontal directions.
With this configuration, the machining area is surrounded by the side cover assembly. The top area of the side cover assembly is covered by the top cover assembly. Therefore, the machining area is completely separated from the outside, whereby it is not required that each slide surface for the guide mechanism is covered with an expensive slide cover.
In another aspect of the present invention, the top cover assembly is provided at a lower position than the guide mechanism. As a result, cutting chips, coolant and so on are more completely prevented from adhering to the slide surfaces for the guide mechanism.
In still another aspect of the present invention, the slide cover assembly comprises a rear side cover member provided adjacent to the spindle head base, a front side cover member, and a pair of lateral side cover members. At least one of the lateral side cover members has a shutter for closing a window thereof. On loading the workpiece into the machining area the workpiece from the machining area, the shutter can be opened.
In a further aspect of the present invention, a tool magazine and an automatic tool changer are provided under the guide mechanism. A window formed at the rear side cover member is selectively opened and closed by a third shutter. The automatic tool changer is operable to present at least a part thereof into the machining area for changing tools between the tool spindle and the tool magazine. Therefore, the tool magazine and the automatic tool changer can also be protected from contamination by coolant, cutting chips and so on.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
Various other objects, features and many of the attendant advantages of the present invention will be readily appreciated as the same becomes better understood by reference to the following detailed description of the preferred embodiments when considered in connection with the accompanying drawings, in which:
FIG. 1 is a front view of a machine tool according to the first embodiment of the present invention;
FIG. 2 is a left side view of the machine tool shown in FIG. 1;
FIG. 3 is a fragmentary top plan view showing a spindle head and vicinity thereof of the machine tool;
FIG. 4 is a fragmentary top plan view showing a top cover assembly and vicinity thereof of the machine tool except for the spindle head;
FIG. 5 is a sectional view taken taken along the line V--V in FIG. 3;
FIG. 6 is an enlarged view of an end portion of the spindle head shown in FIG. 5;
FIG. 7 is a sectional view taken along the line VII--VII in FIG. 5;
FIG. 8 is a bottom view of a support bracket shown in FIG. 7;
FIGS. 9(a) and (b) are respectively top plan and front views of one of second cover members movable back and forth in a horizontal plane;
FIGS. 9(c) and (d) are respectively top plan and front views of one of first cover members movable right and left in a horizontal plane;
FIG. 9(e) is a schematic illustration for showing the entire arrangement of the first and second cover members constructing the top cover assembly;
FIG. 10 is a fragmentary front view of a tool changer shutter shown in FIG. 7;
FIG. 11 is a sectional view taken along the line XI--XI in FIG. 10 to show the tool changer shutter and vicinity thereof;
FIG. 12 is a sectional view taken along the line XII--XII in FIG. 11 to show a cylinder-lever mechanism for the tool changer shutter;
FIG. 13 is a sectional view taken along the line XIII--XIII in FIG. 11;
FIG. 14 is a top plan view of a top cover assembly used in the second embodiment;
FIG. 15 is a sectional view taken along the line XV--XV in FIG. 14; and
FIG. 16 is a sectional view taken along the line XVI--XVI in FIG. 4.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The first embodiment will be described in detail with reference to FIGS. 1 to 13 and FIG. 16. FIGS. 1 and 2 are respectively front and left side views showing the whole of a machine tool according to the first embodiment. Numeral 1 denotes a gantry-shaped bed (spindle head base), on which a pair of guide portions 1a extending parallel in Y-direction (back and forth direction) are secured at the top of the bed 1. A first slider 3 is guided on the guide portions 1a to be movable by a motor 11 in the Y-direction. On the top of the first slider 3, a second slider 4 is guided on a pair of guide portions 3a to be movable by a motor 13 in X-direction (right and left direction) perpendicular to the Y-direction. Further, a spindle head 5 is guided on a pair of guide portions 4a of the second slider 4 to be movable by a motor 12 in Z-direction (vertical direction) perpendicular to both of the X- and Y-directions. A tool spindle 14 is rotatable by a motor (not shown) built in the spindle head 5.
A jig device C for clamping a workpiece W is mounted on a workpiece support base 2 secured to the bed 1 at the front side thereof. The jig device C is surrounded at the four sides by a side cover assembly which comprises a pair of lateral side cover members 6a and 6b, a front side cover member 6c and a rear side cover member 6d. The top area of the jig device C is covered by a top cover assembly 8 at a lower position than the guide portions 1a, 3a and 4a on which the first slider 3, the second slider 4 and the spindle head 5 are movable respectively. At least one (preferably, both) of lateral side cover members 6a and 6b is provided with a window, which is normally closed with a shutter 7. To carry a workpiece in and out of the space (machining area) surrounded by the side cover members 6a-6d, the shutter 7 is moved in the vertical direction to open the window. As shown in FIG. 5, the workpiece W carried by a conveyer 23 into the machining area is positioned by a lifter 24 to a machining position and then, is clamped with a clamper 21 actuated by a fluid cylinder 22 of a clamp mechanism.
Turning back to FIGS. 1 and 2, a tool magazine 10m and an automatic tool changer 10 are located within column portions of the gantry-shaped bed 1, the space for which is separated by the rear side cover member 6d from the space for the jig device C. The column portions of the bed 1 extend parallel in the Y-direction and are connected at their tops through one or more cross beam portions (not shown). The rear side cover member 6d is provided with a window, which is normally closed with a tool changer shutter 9. In advance of exchanging a tool attached to the tool spindle 14 with another one, the tool changer shutter 9 is moved in the vertical direction by a cylinder-lever mechanism, described later, to open the window.
FIG. 3 is a fragmentary top plan view showing the spindle head 5 and the vicinity thereof of the machine tool, and FIG. 4 is a fragmentary top plan view showing the top cover assembly 8 and the vicinity thereof except for the spindle head 5. The top cover assembly 8 is composed of plural first cover member 52a-e for movement in the X-direction and plural second cover members 56a-h for movement in the Y-direction. A first cover base frame 50 incorporates the first and second cover members 52a-e and 56a-h thereinto and is supported by a pair of support beams 30 which project from the column portions of the bed 1 at the front side thereof. The top cover assembly 8 has a square spindle hole 15 into which the top spindle 14 is inserted. An outer peripheral surface of the first cover base frame 50 is surrounded by the upper end portions bent inside of the lateral side cover members 6a, 6b and the front side cover member 6c.
Referring to FIG. 5, the spindle head 5 is movable in the Z-direction (i.e., vertical direction) through a feed screw 12a. A support bracket 19 is fixed by means of bolts to the front surface of a lower portion of the second slider 4. Therefore, the support bracket 19 can be moved by the first and second sliders 3 and 4 in a horizontal plane but not in the vertical direction. A lower end plate portion of the support bracket 19 has a circular hole at a central portion thereof, in which a cylindrical cover 18 is fitted. A nose portion 16 of the spindle head 5 is inserted into the square spindle hole 15 of the top cover assembly 8 through the cylindrical cover 18. The tool spindle 14 to which a cutting tool 17 is attachable is rotatably supported in the nose portion 16.
FIG. 6 is an enlarged view of the vicinity of the support bracket 19 shown in FIG. 5. Guide rods 20 extending in the vertical direction are fixed to a horizontal flange portion of the cylindrical cover 18 at four positions around the nose portion 16. Each of the guide rods 20 has a stopper 20c at the lower end thereof. The lower end plate portion of the support bracket 19 is provided with four guide sleeves 20a to respectively receive the guide rods 20. A coil spring 20b is interposed between a bottom portion of each guide sleeve 20a and the horizontal flange portion of the cylindrical cover 18, so that the cylindrical cover 18 is always urged to move upwardly.
The cylindrical cover 18 prevents coolant, cutting chips and so on from coming up from the space between the nose portion 16 and the top cover assembly 8. When the spindle head 5 is at a relatively higher position within its movable stroke, the nose portion 16 passes through the cylindrical cover 18, with a slight clearance therebetween being sealed. When the spindle head 5 is moved down to the position shown by the solid line in FIG. 6, step-up shoulder surface 16a of the nose portion 16 comes into engagement with the horizontal flange portion. Further down movement of the spindle head 5 causes cylindrical cover 18 to be pushed down against the springs 20b. The spindle head 5 can be moved down until the horizontal flange portion of the cylindrical cover 18 comes into contact with the lower end plate portion of the support bracket 19. The movable stroke of the spindle head 5 in the vertical direction can be varied by changing the lengths of the guide rods 20.
The construction of the top cover assembly 8 will now be described in detail with reference to FIGS. 9(a)-9(e). FIG. 9(e) schematically shows the entire arrangement of the first cover members 52a-e and the second cover members. 56a-h jointly constructing the top cover assembly 8. Numeral 53 denotes a second cover base frame guiding the second cover members 56a-h. A pair of multi-stepped guide rails 54 extending in the Y-direction are secured to two inner end surfaces in parallel relation of the second cover base frame 53. Each of the multi-stepped guide rails 54 is made by piling up plural plate strips having different widths. The second cover members 56a-h are slidably guided by the opposite stepped portions of the multi-stepped guide rails 54 in the order of the member 56a being at the lowest position. The member 56a guided by the lowest step portions is the smallest in size as to not only its length but also its width. Regarding other members 56b-h, the widths are made wider and wider in correspondence with spans of the mating step portions therefor, and the lengths in the Y-direction are made longer and longer as the position of the corresponding step portions goes up. Also, the lengths in the Y-direction of rectangular openings of the second cover members 56a-h are made longer and longer as the position of the corresponding step portions goes up. As shown in FIGS. 9(a) and (b), flaps 59 are formed at the lower surface of each second cover member 56a-h to extend along front and rear edges thereof.
The first cover base frame 50 has a depth to house all of the first cover members 52a-e and the second cover base frame 53. The first cover base frame 50 is secured to a rectangular stationary frame 57, which is in turn secured to the pair of support beams 30 at its two bar portions extending in the Y-direction. A pair of multi-stepped guide rails 51 extending in the X-direction are secured to cross-beam portion 57a in parallel relation of the rectangular stationary frame 57, as shown in FIG. 16. Each of the multi-stepped guide rails 51 for the first cover members 52a-e is made in the same manner as the multi-stepped guide rails 54 for the second cover members 56a-h. The first cover members 52a-e and the second cover base frame 53 guiding the second cover members 56a-h are slidably guided by the opposite stepped portions of the multi-stepped guide rails 51 in the order of the second cover base frame 53 being at the lowest position. The second cover base frame 53 guided by the lowest step portions is the smallest in size as to not only its width and but also its length. Regarding the first cover members 52a-e, the lengths in the Y-direction are made longer and longer in correspondence With the spans of the mating step portions therefor, and the widths are made wider and wider as the position of the corresponding step portions goes up. Also, the widths in the x-direction of rectangular openings of the first cover members 52a-e are made wider and wider as the position of the corresponding step portions goes up. As shown in FIGS. 9.(c) and (d), flaps 58 are formed at the lower surface of each first cover member 52a-e to extend along right and left edges thereof.
As shown in FIGS. 6 to 8, the lower end plate portion of the support bracket 19 rotatably carries a first set of four rollers 25 and a second set of four rollers 26. The first set of four rollers 25 are in contact with two inside surface extending in the Y-direction of the second cover base frame 53, so as to slide the first cover members 52a-e when the spindle head 5 is moved in the X-direction. The second set of four rollers 26 are in contact with two inside surfaces extending in the X-direction of the square spindle hole 15 formed on the lowest second cover member 56a, so as to slide the second cover members 56a-h when the spindle head 5 is mowed in the Y-direction. Thus, the top area of the machining position can be separated from the outside through the telescopic movements of the first cover members 52a-e and the second cover members 56a-h even when the spindle head 5 is moved in the X- and Y-directions.
The tool changer shutter 9 will be explained in detail with reference to FIGS. 10-13. FIG, 10 is an enlarged detail view of the tool changer shutter shown in FIG. 7. In back space of the rear side cover member 6d, the cylinder-lever mechanism including a lever 61 and a hydraulic cylinder 60 is arranged beside the automatic tool changer 10 having an arm 10a. In order that the tool changer shutter 9 can be moved without chattering, a pair of guide bars 67 are fixedly provided at opposite sides of the tool changer shatter 9.
As best shown in FIG. 11, the rear side cover member 6d has a cross-section resembling a hat. A main partition portion of the rear side cover member 6d is arranged at a position receding somewhat from the front ends of the column portions of gantry-shaped bed 1. The rear side cover member 6d is secured to a pair of support brackets 59a and 59b which are in turn secured to the bed 1. The hydraulic cylinder 60 is pivotably carried at its lower end to the support bracket 59a. The lever 61 is carried at its base end to the support bracket 59a to be rotatable about a hinge pin 61a. An outer end of a piston rod of the hydraulic cylinder 60 is pivotably connected to the middle portion of the lever 61.
The support brackets 59a and 59b are formed with a pair of guides 58 to guide the tool changer shutter 9 in the Z-direction, wherein a plurality (six in this particularly embodiment) of rollers 64 are rotatably carried on the tool changer shutter 9 at opposite end portions thereof, three rollers being at one end portion along one of the guides 58 while the remaining three rollers being at the other end portion along the other guide 58. A cam 63 grooved in the X-direction is secured to the upper portion of the tool changer shutter 9, and a roller 62 carried at the front end of the lever 61 is engaged with the cam 63. At the opposite ends of the arm 10a, semi-circular grippers 10b are formed to hold a tool attached to the tool spindle 14 and the tool stored in the tool magazine 10m. The arm 10a is normally held in parallel to the tool changer shutter 9, as shown by the solid line in FIG. 11. After the tool changer shutter 9 is lowered to open for tool change operation, the arm 10a is pivoted through 90 degrees to the change position shown by the two-dot chain line in FIG. 11.
FIG. 13 shows a spring mechanism for preventing chattering of the tool changer shutter 9. Each of the guide bars 67 is secured by upper and lower support members 66 and 69 to a corresponding one of the support brackets 59a and 59b. Secured to the upper end of the tool changer shutter 9 are L-letter shaped thrust members 65 through which the guide bars 67 pass. Between the thrust members 65 and the lower support members 69, coil springs 68 are respectively interposed so that the tool changer shutter 9 is always urged to move upwardly. This causes the grooved cam 63 to be urged upwardly against the roller 62 of the lever 61. Therefore, chattering of the tool changer shutter 9 can be prevented not only while the tool changer shutter 9 is moved up and down but also while it remains either at its lowered position or its elevated position.
The operations of the first embodiment will be described hereinafter. The shutter 7 on the lateral side cover member 6a or those shutters on the opposite lateral side cover members 6a and 6b are opened to carry a new workpiece into the machining area. In the case where the machine tool is arranged on the transfer line, the conveyer or transfer carrier 23 which is dedicated to each machine tool unloads a workpiece from another machine tool (not shown) at the upper stream and then, loads it onto the jig device C of such each machine tool. Thus, all workpieces charged into the transfer line are simultaneously moved by the conveyers or the transfer carriers 23 which are respectively dedicated to all the machine tools of the transfer line. The workpiece finished by each machine tool is unloaded from the Jig device C through the window of the lateral side cover member 6b and a new one is loaded thereonto through the window of the lateral side cover member 6a. The lifter 24 lifts the workpiece W carried on the jig device C and then, the clamper 21 is actuated by the fluid cylinder 22 to clamp the workpiece W.
During the transfer operation of the workpiece W, the tool spindle 14 is positioned at a tool change position where the used tool 17 is exchanged by the automatic tool changer 10 with a new one necessary for the next machining operation. In tool changing operation, the hydraulic cylinder 60 is actuated to pivot the lever 61 downwardly about the hinge pin 61a. The pivotal motion of the lever 61 causes the roller 62 carried at the free end thereof to be moved along the grooved cam 63, whereby the tool changer shutter 9 is moved downwardly to open the window.
Subsequently, the arm 10a of the automatic tool changer 10 is rotated through 90 degrees from the parked position shown by the solid line in FIG. 11 to the change position shown by the two-dot chain line in FIG. 11. The semi-circular grippers 10b at the opposite ends of the arm 10a grip the tool on the tool spindle 14 and the tool of the tool magazine 10m simultaneously. The arm 10a is moved down to extract the tools from the tool spindle 14 and the tool magazine 10m. The arm 10a is then rotated through 180 degrees and is moved up to insert the tools respectively to the tool spindle 14 and the tool magazine 10m. Thereafter, the arm 10a is rotated in an opposite direction through 90 degrees to return to the parked position shown by the solid line. After such tool charging operation, the hydraulic cylinder 60 is quickly actuated to close the tool changer shutter 9. At the same time, the shutters 7 on the lateral side covers 6a and 6b are closed upon completion of the unloading and loading operation of the workpieces. After that, the tool spindle 14 having received the new tool 17 is moved to the machining position through the movements of the first slider 3, the second slider 4 and the spindle head 5, whereby the machining operation on the workpiece W is initiated with the new tool 17 then rotated.
During the movements of the nose portion 16 in the X-and Y-directions, the support bracket 19 fixed to the front surface. Of the second slider 4 is moved together with the nose portion 16. When the support bracket 19 is moved in the X-direction, the second cover base frame 53 is caused to follow the movement of the support bracket 19 since, as shown in FIG. 8, the rollers 25 carried on the support bracket 19 are in contact with two inside surfaces extending in the Y-direction of the second cover base frame 53. As schematically illustrated in FIG. 9(e), the second cover base frame 53 is supported under the lowest one (the member 52a) of the first cover members 52a-e, and the lowest first cover member 52a right over the second cover base frame 53 is wider than the second cover base frame 53. When the second cover base frame 53 is moved right, for example, it comes into engagement with the right flap 58 of the lowest first cover member 52a in the course of movement, so that the lowest first cover member 52a is moved toward the right with a delay after movement of the second cover base frame 53. Further right movement of the second cover base frame 53 brings the lowest first cower member 52a into engagement with the right flap 58 of the second lowest first cover member 52b. In this manner, each lower first cover member comes into abutting engagement with the right flap 58 of an immediately upper first cover member, whereby the first cover members 52a-e are caused to be moved one after another toward the right. When the second cover base frame 53 is moved toward the left, the first cover members 52a-e are caused to be moved one after another toward the left in the same manner as described above.
When the support bracket 19 is moved in the Y-direction, the lowest second cover member 56a is caused to follow the movement of the support bracket 19 within the second cover base frame 53 since the rollers 26 carried on the support bracket 19 are in contact with two inside surfaces extending in the X-direction of the square spindle hole 15 of the lowest second cover member 56a. The second lowest second cover member 56b right over the first lowest second cover member 56a is longer in the Y-direction than the member 56a. When the support bracket 19 is moved forward, for example, the first lowest second cover member 56a is first moved and then comes into engagement with the front flap 59 of the second lowest second cower member 56b in the course of movement, so that the second lowest second cover member 56b is moved forward with a delay after the movement of the first lowest second cover member 56a. Further forward movement of the support bracket 19 brings the second lowest second cover member 56b into engagement with the third lowest second cover member 56c to move the same in this manner, each lower second cover member comes into abutting engagement with the front flaps 58 of an immediately upper second cover member, whereby the second cover members 56a-h are caused to be moved one after another forward. When the support bracket 19 is moved backward, the second cover members 56a-h are caused to be moved one after another backward in the same manner as described above.
In FIG. 6, numeral 31 indicates a coolant nozzle for supplying coolant during machining operation. It is to be noted that the cylindrical cover 18 is relatively long, so that coolant, cutting chips and so on are prevented from coming up from the clearance between the internal surface of the cylindrical cover 18 and the nose portion 16.
Referring now to FIG. 14, there is illustrated a top cover assembly 8' used in the second embodiment. A flexible bellow 90 made of rubber is secured at its circumferential portion to a first cover base frame 50', and at its internal portion to a support bracket 19'. The bellow 90 is formed with a plurality of pleat portions 90a which are foldable in any radial direction. Thus, even when the support bracket 19 is moved together with the spindle head 5 within a horizontal plane, the bellow 90 works to reliably cover the top area over the machining position. An additional shutter may be provided on the front side cover member 6c for the loading and unloading of a workpiece from the front side of the machine tool. The provision of the additional shutter on the front side cover member 6c is particularly advantageous where the machine tool is used as "stand-alone" (i.e., without being arranged on the transfer line).
Obviously, numerous modifications and variations of the present invention are possible in light of the above teachings. It is therefore to be understood that within the scope of the appended claims, the present invention may be practiced otherwise than as specifically described herein. | In a machine tool of the present invention, a spindle head rotatably supports a vertical tool spindle. On the spindle head base, a guide mechanism is provided so as to guide the spindle head in mutually orthogonal first and second horizontal directions and in a vertical direction. A workpiece is supported on a workpiece supporting base provided at a front side of the spindle head base. The workpiece is surrounded with a side cover assembly on the workpiece support base so as to define a machining area therewithin. The upper end of the side cover assembly is covered with a top cover assembly. The top cover assembly has a spindle hole through which a nose portion of the spindle head passes so as to permit the tool spindle to reach the machining area, and is flexibly operable to follow the movements of the spindle head in the first and second horizontal directions. | 8 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to devices for controlling the temperature of pyrolysis reactions, and particularly to an adjustable heat exchanger having a plurality of alternating discs for transferring heat from one set to the other.
2. Description of the Related Art
Pyrolysis is the process of chemically breaking down or altering a substance by heat in an essentially oxygen-free environment. Pyrolysis is used in the manufacture of various materials and in the production of lighter fractions from crude oil, as well as in other industries. The process often requires very precise control of the temperature during the pyrolysis process in order to achieve the specific chemistry of the desired end result.
To date it has been extremely difficult to achieve such precisely controlled temperatures (other than in electric ovens), particularly in fluid-based ovens required for successful pyrolysis. Thus, an adjustable heat exchanger solving the aforementioned problems is desired.
SUMMARY OF THE INVENTION
The adjustable heat exchanger provides precise heat transfer, and therefore temperature control, from a high temperature heat source oven to a controlled temperature pyrolysis oven. The heat exchanger has a plurality of fixed discs and a plurality of rotating discs, which are interleaved in an alternating array. Each disc is hollow, and heat transfer fluid circulates therethrough. A first heat transfer fluid circulates from the high temperature heat source oven through the fixed discs, and a second heat transfer fluid circulates through the rotating discs and pyrolysis oven. The two fluids do not mix with one another, but are kept completely separate. Separate pumps are used to circulate the fluids through their respective discs and ovens. Any suitable fluid may be used as the working fluids in the two disc assemblies and their ovens, but helium gas is a preferred fluid, while a lithium-lead compound has been used in certain specialized heat transfer apparatus and applications.
The two sets of discs are semicircular in shape, and rotation of the rotating discs results in greater or less surface area being exposed beyond the stationary discs. This results in lesser or greater heat transfer between the stationary discs and the rotary discs, respectively. Since the discs are semicircular, the rotation of the rotary discs to a position 180° opposite the fixed discs results in maximal spatial separation between the fixed and rotating discs and minimal heat transfer between the two. Partial rotation of the rotating discs between the fixed discs results in somewhat greater heat transfer, and continued rotation of the rotary discs completely between the fixed discs results in maximum heat transfer from the fixed discs to the rotary discs, and thus to the pyrolysis oven.
These and other features of the present invention will become readily apparent upon further review of the following specification and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic view of an adjustable heat exchanger according to the present invention, illustrating its general configuration and connection to input (high temperature sink) and output (pyrolysis) ovens.
FIG. 2 is a perspective view of the stationary disc portion of the adjustable heat exchanger of FIG. 1 .
FIG. 3 is a perspective view of the rotating disc portion of the adjustable heat exchanger according to FIG. 1 , the stationary disc portion being shown in broken lines.
FIG. 4 is a perspective view of an exemplary heat exchanger disc of the adjustable heat exchanger of FIG. 1 , a portion of one disc face being broken away to show the internal baffle configuration.
FIG. 5 is a top plan view of the adjustable heat exchanger of FIG. 1 , illustrating the relationship between the alternating stationary and rotating discs and the interconnection between the discs of each set.
FIG. 6A is an end view of the adjustable heat exchanger of FIG. 1 , showing the rotary discs rotated clear of the stationary discs for minimal heat transfer therebetween.
FIG. 6B is an end view of the adjustable heat exchanger of FIG. 1 , showing the rotary discs partially interleaved with the stationary discs for partial heat transfer therebetween.
FIG. 6C is an end view of the adjustable heat exchanger of FIG. 1 , showing the rotary discs having the majority of their areas interleaved with the stationary discs for relatively high heat transfer therebetween.
FIG. 6D is an end view of the adjustable heat exchanger of FIG. 1 , showing the rotary discs completely interleaved with the stationary discs for maximal heat transfer therebetween.
Similar reference characters denote corresponding features consistently throughout the attached drawings.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The adjustable heat exchanger provides precise temperature control for pyrolysis reactions involving the breakdown of various organic compounds in a reducing atmosphere. The heat exchanger is disposed between a heat source oven providing relatively higher heat and a pyrolysis oven. Adjusting the heat exchanger provides precise heat transfer from the heat source oven to the pyrolysis oven for precise control of the reactions taking place within the pyrolysis oven.
FIG. 1 of the drawings provides a schematic view of an exemplary installation of the adjustable heat exchanger 10 in an installation having a first oven or heat source oven 12 and a second oven or pyrolysis oven 14 . The ovens 12 and 14 are shown partially in FIG. 1 in order to provide a reasonable scale, but it will be understood that each oven 12 and 14 is a closed unit when in operation. Similarly, the heat exchanger 10 is shown open, but it will be understood that it is completely enclosed by a thermally insulated housing 16 when in operation.
The adjustable heat exchanger 10 contains a first plurality of fixed hollow discs, e.g., discs 18 a through 18 l , in a parallel array to one another. The fixed discs 18 a through 18 l are spaced apart from one another to allow the placement of a movable disc between each of the fixed discs. A second plurality of mutually parallel, movable hollow discs, e.g., 20 a through 20 k , is disposed in a radial array along a rotating shaft 22 . Other than being fixed to a rotating shaft 22 , the movable discs 20 a through 20 k are substantially identical to the fixed discs 18 a through 18 l . The movable discs 20 a through 20 k are also spaced apart from one another to allow placement of the movable discs between the fixed discs 18 a through 18 l , so that the fixed discs 18 a through 18 l and the movable discs 20 a through 20 l are interleaved with one another in an alternating array when the movable discs 20 a through 20 l are rotated between the fixed discs 18 a through 18 l.
The spacing between the alternating fixed discs 18 a through 18 l and movable discs 20 a through 20 k is preferably quite close, leaving just sufficient room or space to preclude physical contact between the fixed and moving discs. This greatly improves the heat transfer between the fixed and moving discs. The discs 18 a through 18 l and 20 a through 20 k are preferably semicircular in form as shown in the various drawings, but may be any suitable shape or form, so long as rotation of the movable discs 20 a through 20 k relative to the stationary discs 18 a through 18 l results in variation in the closely adjacent surface area between the stationary and movable discs in order to adjust the heat transfer therebetween. It will be seen that the twelve fixed discs 18 a through 18 l and the eleven movable discs 20 a through 20 k are exemplary in number, and more or fewer discs may make up each set of fixed and rotating discs.
FIG. 2 provides a detailed perspective view of the fixed discs 18 a through 18 l . Each of the fixed discs includes a central channel 24 therein. The aligned channels 24 of the discs 18 a through 18 l provide for the placement of the rotary shaft 22 therein. The shaft 22 is illustrated in FIGS. 1 , 3 , 5 , and 6 A through 6 D of the drawings. The discs 18 a through 18 l are supported by legs 26 , which, in turn, rest within the housing 16 , shown in FIGS. 1 and 5 of the drawings. A plurality of peripherally disposed interconnecting tubes 28 extend between adjacent fixed discs 18 a through 18 l , and connect each of the fixed discs in sequence. That is to say, the first fixed disc 18 a is fluidly connected directly to the second fixed disc 18 b , the second fixed disc 18 b communicates fluidly with the third disc 18 c , and so on, in sequence. Thus, fluid flowing through the first fixed disc 18 a must flow through the second fixed disc 18 b in order to reach the third fixed disc 18 c , etc.
A similar sequential flow path is provided for the rotary discs 20 a through 20 k , as shown in FIG. 3 of the drawings. The various rotary discs 20 a through 20 k are affixed to the shaft 22 , and extend radially therefrom to rotate with the shaft. The heat transfer fluid flows into an axial entry port 30 at one end of the shaft 22 , and thence through a radially disposed passage 32 into a notch or channel 34 formed axially along the length of the shaft. A plurality of lateral ports 36 a and 36 b and corresponding transfer tubes 38 a and 38 b allow the heat transfer fluid to flow from the shaft channel 34 to each of the rotary discs 20 a through 20 k , and back from each of the discs into the channel 34 . A plurality of channel baffles 40 a through 40 k extend laterally across the shaft channel 34 to prevent flow of the heat transfer fluid along the channel 34 without passing through each of the discs 20 a through 20 k in sequence.
Thus, the heat transfer fluid enters the entry port 30 of the shaft 22 and flows through the inlet passage 32 into the first or entry end of the channel 34 . The first baffle 40 a precludes axial travel of the fluid along the channel 34 , so the fluid must flow into the lateral passage 36 a and corresponding transfer tube 38 a to the first rotary disc 20 a . After the fluid flows through the first rotary disc 20 a , it passes through the transfer tube 38 b and lateral passage 36 b , which is on the opposite side of the first baffle 40 from the first lateral passage 36 a . As the fluid cannot flow back to the first lateral passage due to the first baffle 40 a , it must flow into the second lateral passage 36 b and its transfer tube 38 b to flow into the second rotary disc 20 b . After flowing through the second rotary disc 20 b , the fluid flows through the transfer tube and lateral passage into the next channel chamber defined by the first and second baffles 40 a and 40 b . The process continues with the heat transfer fluid flowing through each of the rotary discs 20 a through 20 k , finally flowing from the last disc 20 k through the last transfer tube 38 b and outlet passage 36 b into the channel 34 between the last baffle 40 k and the radial exit passage 42 to depart the axial exit port 44 (shown in FIGS. 1 and 5 ) of the shaft 22 .
The internal structure of an exemplary one of the discs 18 a through 18 l and 20 a through 20 k is illustrated in FIG. 4 of the drawings. This exemplary disc is designated as disc 19 in order to avoid implication that it is a specific member of either the set of fixed discs or rotating discs. However, the structure of the disc 19 of FIG. 4 is substantially identical to the structures of each of the fixed discs 18 a through 18 l and each of the rotating discs 20 a through 20 k . All of the fixed and rotary discs, as exemplified by the disc 19 , comprise a thin hollow member having mutually opposed, parallel first and second plates 46 a and 46 b defining an interior 48 . The two plates 46 a and 46 b are surrounded by a semicircular outer wall 50 that surrounds the outer peripheries 52 of the plates and a wall 54 that extends across the diametric inner peripheries 56 of the two plates 46 a , 46 b and the central channel 24 . The interior 48 of this closed structure only communicates with the external environment by means of the interconnecting transfer tubes 28 (in the case of the fixed discs 18 a through 18 l ) or the inlet and outlet transfer tubes 38 a and 38 b to and from the shaft 22 (in the case of the rotating discs 20 a through 20 k ).
A plurality of baffles are installed within the interior 48 of each of the discs in a radial array. The baffles guide or control the flow of the heat exchange fluid through the discs. All of the baffles are identical to one another, but are designated differently according to their positions within the disc. Each baffle 58 a of a first plurality of baffles has its inner end 60 a adjacent the inner periphery of the disc, specifically the portion of the wall 54 forming the channel 24 , its opposite outer end 62 a being spaced inward from the outer circumferential wall 50 and outer peripheries 52 of the two plates 46 a , 46 b . Each baffle 58 b of a second plurality of baffles has its inner end 60 b spaced apart from the inner portion of the wall 54 forming the channel 24 of the disc, its opposite outer end 62 b being adjacent to the outer circumferential wall 50 and outer peripheries 52 of the two plates 46 a , 46 b.
The baffles 58 a and 58 b are interleaved with one another in an alternating array in the disc, e.g., a second baffle 58 b , a first baffle 58 a , another second baffle 58 b , another first baffle 58 a , etc. In this manner, heat exchange fluid entering at one edge of the disc flows generally radially inward and outward between the baffles 58 a and 58 b in a sinusoidal path 64 (this path represents the working fluid, e.g., helium, lithium-lead compound, etc.), to exit the disc opposite its entrance point. The baffle arrangement illustrated in the example of FIG. 4 is exemplary of one of the fixed discs 18 a through 18 l where the fluid enters and exits the outer edge of the disc, but it will be seen that the reversal of the locations of the baffles 58 a and 58 b , i.e., relocating the baffles 58 a to the locations illustrated for the baffles 58 b and vice versa, would provide the desired flow path when the flow enters and exits the disc adjacent the channel 24 , as in the case of the rotating discs 20 a through 20 k.
FIGS. 6A through 6D illustrate the variable relationship between the fixed and rotary discs in providing heat transfer between the two types of discs. In FIGS. 6A through 6D the single fixed disc illustrated is designated as disc 18 and represents all of the discs 18 a through 18 l , while the single rotating disc is designated as disc 20 and represents all of the rotating discs 20 a through 20 k . The various internal baffles are shown in broken lines in both discs 18 and 20 , and the rotating disc 20 is stippled to differentiate it from the fixed disc 18 throughout FIGS. 6A through 6D . The housing 16 is not shown in FIGS. 6A through 6D for clarity in the drawings.
In FIG. 6A , the rotating disc 20 is shown rotated 180° from the fixed disc 10 , so that there is no engagement or interleaving between the two discs. This results in minimal heat transfer between the two discs. However, in FIG. 6B , the rotating disc 20 is shown rotated counterclockwise approximately 30°, thereby engaging about one-sixth of the surface of the rotating disc 20 adjacent the surface of the fixed disc 18 (or, interleaving about one-sixth of the surfaces of the rotating discs 20 a through 20 k between the fixed discs 18 a through 18 l ). This results in some moderate amount of heat transfer between the fixed and rotating discs.
In FIG. 6C , the rotating disc 20 has been rotated through about 150° counterclockwise from the initial position shown in FIG. 6A . This results in about five-sixths of the area of the rotating disc 20 overlapping the fixed disc 18 , and thus producing significantly greater heat transfer than that shown in FIG. 6B . Finally, in FIG. 6D the rotating disc 20 has been rotated through 180° from its initial position, shown in FIG. 6A , so that the two discs 18 and 20 completely overlap one another in FIG. 6D . Thus, one hundred percent of their disc surfaces are immediately adjacent one another to produce the maximum amount of heat transfer possible between the two discs.
Returning to FIG. 1 , the complete adjustable heat exchanger system is shown diagrammatically. The first or heat source oven 12 provides a source of heat at least slightly greater than that desired for the pyrolysis oven 14 . A first heat transfer fluid, e.g., helium gas or a compound, such as lithium-lead (represented by the flow path 64 shown in FIG. 4 ), flows from a first fluid supply line 66 a from the first oven 12 by means of a first fluid pump 68 a , and thence to an inlet line 70 a to the first fixed disc 18 a . This fluid flows through the first fixed disc 18 a following the sinusoidal path illustrated in FIG. 4 , and passes to the second fixed disc 18 b through the peripheral interconnecting tube 28 between the first and second fixed discs 18 a and 18 b . The fluid then flows through the sinusoidal path within the second disc 18 b , thence transferring to the third disc 18 c by mean of the interconnecting tube between the two discs 18 b and 18 c . This flow path continues with the heat transfer fluid flowing through each of the discs in sequence, finally exiting the last fixed disc 18 l to return to the first oven 12 via the return line 72 a for reheating in the first oven 12 .
A second heat transfer fluid, preferably identical to the first fluid flowing through the first oven 12 and fixed or stationary discs 18 a through 181 , flows from the second or pyrolysis oven 14 by means of a second fluid supply line 66 b and second pump 68 b . The pump 68 b pumps the fluid to the entry port 30 of the rotary shaft 22 through a second fluid inlet line 70 b . The second heat transfer fluid then flows into the channel 34 of the shaft 22 and outward to the first rotating disc 20 a through the first outlet passage 36 a and transfer tube 38 a adjacent the first baffle 40 a , shown in FIG. 3 of the drawings. The flow continues in a sinusoidal path defined by the baffles 58 a and 58 b as shown in FIG. 4 , thence passing through the outlet transfer tube 38 b and passage 36 b and back into the channel 34 of the shaft 22 between the first and second channel baffles 40 a and 40 b . The flow path continues in the same manner, with the heat transfer fluid flowing progressively through each of the stationary or fixed discs 20 b through 20 k in sequence. Finally, the heat transfer fluid flows into the channel 34 of the shaft 22 through the last passage 36 b between the final channel baffle 40 k and the radially disposed exit passage 42 , as shown in FIG. 3 , and out the exit port 44 of the shaft 22 to the second return line 72 b to flow back to the second or pyrolysis oven 14 .
It will be seen that the two heat transfer fluids, i.e., the first fluid that flows through the first oven 12 and the fixed discs 18 a through 18 l and the second fluid that flows through the second oven 14 and the rotating discs 20 a through 20 k , never mix, but are maintained completely separate from one another. The essentially constant high heat provided by the first or heat source oven 12 is transferred to the first heat transfer fluid and thence to the fixed discs 18 a through 18 l , where the variable interleaving of the rotating discs 20 a through 20 k with the first discs provides precise control of the temperature of the second heat transfer fluid that circulates through the rotating discs, and thence to the second or pyrolysis oven 14 . While the system described above provides very precise control of the heat delivered to the pyrolysis oven, it will be seen that certain modifications may be made to the system. For example, the first or heat source oven may be connected to the rotating disc assembly and the second or pyrolysis oven may be connected to the fixed discs, if desired. Also, it will be seen that the twelve fixed discs 18 a through 18 l and the eleven rotating discs 20 a through 20 k are exemplary in number, and that a greater (or smaller) number of fixed and rotating discs may be assembled to form the adjustable heat exchanger. Also, while two specific examples of heat exchange fluid have been described herein, it will be seen that numerous other fluids may be used.
It is to be understood that the present invention is not limited to the embodiments described above, but encompasses any and all embodiments within the scope of the following claims. | The adjustable heat exchanger provides precise control of oven temperature in a pyrolysis reaction. The heat exchanger includes two sets of hollow non-circular discs, the discs of a movable set being interleaved with the discs of a stationary set. A first working fluid circulates through a heat source oven and through the hollow stationary discs, and a second working fluid circulates through the hollow rotating discs and a pyrolysis oven. The two fluids do not mix with one another, but are always completely separate from one another. Heat transfer depends upon the relative surface area of the rotary discs interleaved between the stationary discs. Minimum heat transfer occurs when the rotary discs are rotated to a position clear of the stationary discs, and maximum heat transfer occurs when the rotary discs are completely interleaved with the stationary discs. | 5 |
TECHNICAL FIELD
The present invention relates to a DNA molecule containing intron sequences and encoding a human protein which is, depending on the site of action, called Bile Salt-Stimulated Lipase (BSSL) or Carboxyl Ester Lipase (CEL). The DNA molecule is advantageously used in the production of recombinant human BSSL/CEL, preferably by means of production in transgenic non-human mammals. The recombinant human BSSL/CEL can be used as a constituent of infant formulas used for feeding infants as a substitute for human milk, or in the manufacture of medicaments against e.g. fat malabsorption, cystic fibrosis and chronic pancreatitis.
BACKGROUND OF THE INVENTION
Hydrolysis of Dietary Lipids
Dietary lipids are an important source of energy. The energy-rich triacylglycerols constitute more than 95% of these lipids. Some of the lipids, e.g. certain fatty acids and the fat-soluble vitamins, are essential dietary constituents. Before gastro-intestinal absorption the triacylglycerols as well as the minor components, i.e. esterified fat-soluble vitamins and cholesterol, and diacylphosphatidylglycerols, require hydrolysis of the ester bonds to give rise to less hydrophobic, absorbable products. These reactions are catalyzed by a specific group of enzymes called lipases.
In the human adult the essential lipases involved are considered to be Gastric Lipase, Pancreatic Colipase-Dependent Lipase (hydrolysis of tri- and diacylglycerols), Pancreatic Phospholipase A2 (hydrolysis of diacylphosphatidylglycerols) and Carboxylic Ester Lipase (CEL) (hydrolysis of cholesteryl- and fat soluble vitamin esters). In the breast-fed newborn, Bile Salt-Stimulated Lipase (BSSL) plays an essential part in the hydrolysis of several of the above mentioned lipids. Together with bile salts the products of lipid digestion form mixed micelles from which absorption occurs.
Bile Salt-Stimulated Lipase
The human lactating mammary gland synthesizes and secretes with the milk a Bile Salt-Stimulated Lipase (BSSL) (Blackberg et al., 1987) that, after specific activation by primary bile salts, contributes to the breast-fed infant's endogenous capacity of intestinal fat digestion. This enzyme, which accounts for approximately 1% of total milk protein (Blackberg & Hernell, 1981), is not degraded during passage with the milk through the stomach, and in duodenal contents it is protected by bile salts from inactivation by pancreatic proteases such as trypsin and chymotrypsin. It is, however, inactivated when the milk is pasteurized, e.g. heated to 62.5° C., 30 min (Bjorksten et al., 1980).
Model experiments in vitro suggest that the end products of triacylglycerol digestion are different in the presence of BSSL (Bernback et al., 1990; Hernell & Blackberg, 1982). Due to lower intraluminal bile salt concentrations during the neonatal period this may be beneficial to product absorption.
Carboxylic Ester Lipase
The Carboxylic Ester Lipase (CEL) of human pancreatic juice (Lombardo et al., 1978) seems functionally to be identical, or at least very similar, to BSSL (Blackberg et al, 1981). They also share common epitopes, have identical N-terminal amino acid sequences (Abouakil et al., 1988) and are inhibited by inhibitors of serine esterases, e.g. eserine and diisopropylfluorophosphate. In recent studies from several laboratories the cDNA structures from both the milk lipase and the pancreas lipase have been characterized (Baba et al., 1991; Hui et al., 1990; Nilsson et al., 1990; Reue et al., 1991) and the conclusion is that the milk enzyme and the pancreas enzyme are products of the same gene (in this application referred to as the CEL gene, EC 3.1.1.1). The cDNA sequence and deduced amino acid sequence of the CEL gene are described in WO 91/15234 (Oklahoma Medical Research Foundation) and in WO 91/18923 (Aktiebolaget Astra).
CEL is thus assumed to be identical to BSSL, and the polypeptide encoded by the CEL gene is in the present context called BSSL/CEL.
Lipid Malabsorption
Common causes of lipid malabsorption, and hence malnutrition, are reduced intraluminal levels of Pancreatic Colipase-Dependent Lipase and/or bile salts. Typical examples of such lipase deficiency are patients suffering from cystic fibrosis, a common genetic disorder resulting in a life-long deficiency in 80% of the patients, and chronic pancreatitis, often due to chronic alcoholism.
The present treatment of patients suffering from a deficiency of pancreatic lipase is the oral administration of very large doses of a crude preparation of porcine pancreatic enzymes. However, Colipase-Dependent Pancreatic Lipase is inactivated by the low pH prevalent in the stomach. This effect cannot be completely overcome by the use of large doses of enzyme. Thus the large doses administered are inadequate for most patients, and moreover the preparations are impure and unpalatable.
Certain tablets have been formulated which pass through the acid regions of the stomach and discharge the enzyme only in the relatively alkaline environment of the jejunum. However, many patients suffering from pancreatic disorders have an abnormally acid jejunum and in those cases the tablets may fail to discharge the enzyme.
Moreover, since the preparations presently on the market are of a non-human source there is a risk of immunoreactions that may cause harmful effects to the patients or result in reduced therapy efficiency. A further drawback with the present preparations is that their content of other lipolytic activities than Colipase-Dependent Lipase are not stated. In fact, most of them contain very low levels of BSSL/CEL-activity. This may be one reason why many patients, suffering from cystic fibrosis in spite of supplementation therapy, suffer from deficiencies of fat soluble vitamins and essential fatty acids.
Thus, there is a great need for products with properties and structure derived from human lipases and with a broad substrate specificity, which products may be orally administered to patients suffering from deficiency of one or several of the pancreatic lipolytic enzymes. Products that can be derived from the use of the present invention fulfill this need by themselves, or in combination with preparations containing other lipases.
Infant Formulas
It is well known that human milk-feeding is considered superior to formula-feeding for infants. Not only does human milk provide a well-balanced supply of nutrients, but it is also easily digested by the infant. Thus, several biologically active components which are known to have physiological functions in the infant are either a constituent of human milk or produced during the digestion thereof, including components involved in the defense against infection and components facilitating the uptake of nutrients from human milk.
In spite of the great efforts which have been invested in preparing infant formulas, it has not been possible to produce a formula which to any substantial extent has the advantageous properties of human milk. Thus, infant formulas, often prepared on the basis of cow milk, is generally incompletely digested by the infant and is lacking substances known to have effect on the physiological functions of the infant. In order to obtain an infant formula with a nutritional value similar to human milk, a number of additives including protein fragments, vitamins, minerals etc., which are normally formed or taken up during the infant's digestion of human milk, are included in the formula with the consequent risk of posing an increased strain on and possible long-term damage of important organs such as liver and kidney. Another disadvantage associated with the use of cow milk-based formulas is the increased risk for inducing allergy in the infant against bovine proteins.
As an alternative to cow milk-based infant formulas, human milk obtainable from so-called milk banks has been used. However, feeding newborn infants with human milk from milk banks has in the recent years to an increasing extent been avoided, because of the fear for the presence of infective agents such as HIV and CMV in human milk. In order to destroy the infective agents in human milk it has become necessary to pasteurize the milk before use. However, by pasteurization the nutritional value and the biological effects of the milk components are decreased, for example is BSSL inactivated, as mentioned above.
Addition of Lipases to Infant Formulas
The pancreatic and liver functions are not fully developed at birth, most notably in infants born before term. Fat malabsorption, for physiological reasons, is a common finding and thought to result from low intraluminal Pancreatic Colipase-Dependent Lipase and bile salt concentrations. However, because of BSSL, such malabsorption is much less frequent in breast-fed infants than in infants fed pasteurized human milk or infant formulas (Bernback et al., 1990).
To avoid the above disadvantages associated with pasteurized milk and bovine milk-based infant formulas, it would thus be desirable to prepare an infant formula with a composition closer to that of human milk, i.e. a formula comprising human milk proteins.
BSSL/CEL has several unique properties that makes it ideally suited for supplementation of infant formulas:
It has been designed by nature for oral administration. Thus, it resists passage through the stomach and is activated in contents of the small intestine.
Its specific activation mechanism should prevent hazardous lipolysis of food or tissue lipids during storage and passage to its site of action.
Due to its broad substrate specificity it has the potential to, on its own, mediate complete digestion of most dietary lipids, including the fat soluble vitamin esters.
BSSL/CEL may be superior to Pancreatic Colipase-Dependent Lipase to hydrolyze ester bonds containing long-chain polyunsaturated fatty acids.
In the presence of Gastric Lipase and in the absence of, or at low levels of Colipase-Dependent Lipase, BSSL/CEL can ascertain a complete triacylglycerol digestion in vitro even if the bile salt levels are low such as in newborn infants. In the presence of BSSL/CEL the end products of triacylglycerol digestion become free fatty acids and free glycerol rather than free fatty acids and monoacylglycerol generated by the other two lipases (Bernback et al., 1990). This may favour product absorption particularly when the intraluminal bile salt levels are low.
The utilization of BSSL/CEL for supplementation of infant formulas requires however access to large quantities of the product. Although human milk proteins may be purified directly from human milk, this is not a realistic and sufficiently economical way to obtain the large quantities needed for large scale formula production, and other methods must consequently be developed before an infant formula comprising human milk proteins may be prepared. The present invention provides such methods for preparation of BSSL/CEL in large quantities.
Production of Proteins in Milk of Transgenic Animals
The isolation of genes encoding pharmacologically active proteins has permitted cheaper production of such proteins in heterologous systems. An appealing expression system for milk proteins is the transgenic animal (For a review see Hennighausen et al., 1990). Dietary compositions comprising bile salt-activated lipase derived from e.g. transgenic animal technology, is described in EP 317,355 (Oklahoma Medical Research Foundation).
In the transgenic animal, the protein coding sequence can be introduced as cDNA or as a genomic sequence. Since introns may be necessary for regulated gene expression in transgenic animals (Brinster et al., 1988; Whitelaw et al., 1991) it is in many cases preferable to use the genomic form rather than the cDNA form of the structural gene. WO 90/05188 (Pharmaceutical Proteins Limited) describes the use in transgenic animals of protein-coding DNA comprising at least one, but not all, of the introns naturally occurring in a gene coding for the protein.
PURPOSE OF THE INVENTION
It is an object of the present invention to provide a means for producing recombinant human BSSL/CEL, in a high yield and at a realistic price, for use in infant formulas in order to avoid the disadvantages with pasteurized milk and formulas based on bovine proteins.
BRIEF DESCRIPTION OF THE INVENTION
The purpose of the invention has been achieved by cloning and sequencing the human CEL gene. In order to improve the yield of BSSL/CEL, the obtained DNA molecule containing intron sequences, instead of the known cDNA sequence, of the human CEL gene has been used for production of human BSSL/CEL in a transgenic non-human mammal.
Accordingly, in one aspect the present invention relates to a DNA molecule shown in the Sequence Listing as SEQ ID NO: 1, or an analogue of the said DNA molecule which hybridizes with the DNA molecule shown in the Sequence Listing as SEQ ID NO: 1, or a specific part thereof, under stringent hybridization conditions.
The procedure used for isolating the human BSSL/CEL DNA molecule is outlined in the Examples below.
The stringent hybridization conditions referred to above are to be understood in their conventional meaning, i.e. that hybridization is carried out according to an ordinary laboratory manual such as Sambrook et al. (1989).
In another aspect the present invention provides a mammalian expression system comprising a DNA sequence encoding human BSSL/CEL inserted into a gene encoding a milk protein of a non-human mammal so as to form a hybrid gene which is expressible in the mammary gland of an adult female of a mammal harbouring said hybrid gene so that human BSSL/CEL is produced when the hybrid gene is expressed.
In yet a further aspect, the present invention relates to a method of producing a transgenic non-human mammal capable of expressing human BSSL/CEL, comprising injecting a mammalian expression system as defined above into a fertilized egg or a cell of an embryo of a mammal so as to incorporate the expression system into the germline of the mammal and developing the resulting injected fertilized egg or embryo into an adult female mammal.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1
The CEL gene locus. Localization and restriction enzyme map of the two partly overlapping clones, λBSSL1 and λBSSL5A are shown. The exon-intron organization and used restriction enzyme site are shown below. Exons are represented by boxes numbered 1-11. Asp=Asp700, B=BamHI, E=EcoRI, S=SacI, Sa=SalI, Sp=SphI and X=XbaI. Positions and orientation of Alu repetitive elements are shown by bold arrows. a-h represent different subcloned fragments.
FIG. 2
Primer extension analysis of RNA from human lactating mammary gland, pancreas and adipose tissue. An end-radiolabeled 26-mer oligonucleotide, which is complementary to nt positions 33 to 58 of the CEL gene, was used to prime reverse transcription of the RNA. Lane A is a molecular size marker (a sequencing ladder), lane B pancreatic RNA, lane C adipose tissue RNA and lane D lactating mammary gland RNA.
FIG. 3 (SEQ ID NOS: 39-56 in the Sequence Listing)
Dotplot analysis of the human CEL and rat CEL gene 5'-flanking regions. The homology regions are labeled A-H and the sequences representing these parts are written, upper is human and lower is rat.
FIG. 4
Analysis of 5'-flanking sequence of the human CEL gene. The putative recognition sequences are either highlighted underline or underline representing the complementary strand. Bold letters show the locations of the homologies to the rCEL (regions A-H). The TATA-box is underlined with dots. There are two sequences that both show a 80% similarity to the consensus sequence of the glucocorticoid receptor binding site, GGTACANNNTGTTCT (SEQ ID NO: 33 in the Sequence Listing), (Beato, M., 1989), the first one on the complementary strand at nt position -231 (1A) and the second one at nt position -811 (1B). Moreover, at nt position -861 (2) there is a sequence that shows 87% similarity to the consensus sequence of the estrogen receptor binding site, AGGTCANNNTGACCT (SEQ ID NO: 34 in the Sequence Listing), (Beato, M., 1989).
Lubon and Henninghausen (1987) have analyzed the promoter and 5'-flanking sequences of the whey acidic protein (WAP) gene and established the binding sites for nuclear proteins of lactating mammary gland cells. One of them, an 11 bp conserved sequence, AAGAAGGAAGT (SEQ ID NO: 35 in the Sequence Listing), is present in a number of milkprotein genes studied e.g. the rat α-lactalbumin gene (Qasba et al., 1984) and the rat α-casein gene (Yu-Lee et al., 1986). In the CEL gene's 5'-flanking region, on the complementary strand at nt position -1299 (3) there is a sequence that shows 82% similarity to this conserved sequence.
In a study of the β-casein gene's regulation, a tissue specific mammary gland factor (MGF) was found in nuclear extracts from pregnant or lactating mice and its recognition sequence was identified (ANTTCTTGGNA, SEQ ID NO: 36 in the Sequence Listing). In the human CEL gene's 5'-flanking region there are two sequences, one on the complementary strand at nt position -368 (4A) and the other at nt position -1095 (4B), they both show 82% similarity to the consensus sequence of the MGF binding site. Beside these two putative MGF binding sites in the 5'-flanking region there is a sequence on the complementary strand at nt 275 in intron I, AGTTCTTGGCA (SEQ ID NO: 37 in the Sequence Listing), which shows 100% identity to the consensus sequence of the MGF binding site.
Furthermore, there are four sequences which all show 65% similarity to the consensus sequence of rat pancreas-specific enhancer element, GTCACCTGTGCTTTTCCCTG (SEQ ID NO: 38 in the Sequence Listing), (Boulet et al., 1986), one at nt position -359 (5A), the second at nt position -718 (5B), the third at nt position -1140 (5C) and the last at nt position -1277 (5D).
FIG. 5
Method for production of the plasmid pS452. For further details, see Example 2.
FIG. 6
Schematic structure of the plasmid pS312.
FIG. 7
Schematic structure of the plasmid pS452.
FIG. 8
Physical map representing the physical introduction of human BSSL/CEL genomic structure in the first exon of the WAP gene as described in Example 2.
FIG. 9
A. Schematic representation of the localization of PCR-primers used for identification of transgenic animals. The 5'-primer is positioned within the WAP sequence starting at the position -148 bp upstream of the fusion between the WAP and BSSL/CEL. The 3'-primer is localized in the first BSSL/CEL intron ending 398 bp downstream of the fusion point.
B. The sequences of the PCR primers used.
C. Agarose gel showing a typical analysis of the PCR analysis of the potential founder animals. M: molecular weight markers. Lane 1: control PCR-product generated from the plasmid pS452. Lanes 2-13: PCR reactions done with DNA preparations from potential founder animals.
FIG. 10
Immunoblot analysis of milk from a mouse line transgenic for the recombinant murine WAP/human CEL gene of pS452. The proteins were separated on SDS-PAGE, transferred to Immobilon membranes (Millipore) and visualized with polyclonal rabbit antibodies generated using highly purified human native CEL, followed by alkaline phosphatase labelled swine anti-rabbit IgG (Dakopatts). Lane 1, Low molecular weight markers, 106, 80, 49.5, 32.5, 27.5, and 18.5 kDa, respectively. Lane 2, High molecular weight markers, 205, 116.5, 80 and 49.5 kDa, respectively. Lane 3, 25 ng purified non-recombinant CEL from human milk. Lane 4, 2 μl milk sample from a CEL transgenic mouse diluted 1:10. Lanes 5 and 6, 2 μl milk samples from two different non-CEL transgenic mice, diluted 1:10, as control samples.
DETAILED DESCRIPTION OF THE INVENTION
The DNA molecule shown in the Sequence Listing as SEQ ID NO: 1, which has an overall length of 11531 bp, has the following features:
______________________________________Feature from base to base______________________________________5'-Flanking region 1 1640TATA box 1611 1617Exon 1 1641 1727Translation start 1653 1653Exon 2 4071 4221Exon 3 4307 4429Exon 4 4707 4904Exon 5 6193 6323Exon 6 6501 6608Exon 7 6751 6868Exon 8 8335 8521Exon 9 8719 8922Exon 10 10124 10321Exon 11 10650 114903'-Flanking region 11491 11531______________________________________
In the present context, the term "gene" is used to indicate a DNA sequence which is involved in producing a polypeptide chain and which includes regions preceding and following the coding region (5'-upstream and 3'-downstream sequences) as well as intervening sequences, the so-called introns, which are placed between individual coding segments (so-called exons) or in the 5'-upstream or 3'-downstream region. The 5'-upstream region comprises a regulatory sequence which controls the expression of the gene, typically a promoter. The 3'-downstream region comprises sequences which are involved in termination of transcription of the gene and optionally sequences responsible for polyadenylation of the transcript and the 3' untranslated region.
The DNA molecules of the invention explained herein may comprise natural as well as synthetic DNA sequences, the natural sequence typically being derived directly from genomic DNA, normally of mammalian origin, e.g. as described below. A synthetic sequence may be prepared by conventional methods for synthetically preparing DNA molecules. The DNA sequence may further be of mixed genomic and synthetic origin.
In a further aspect, the present invention relates to a replicable expression vector which carries and is capable of mediating the expression of a DNA sequence encoding human BSSL/CEL.
In the present context, the term "replicable" means that the vector is able to replicate in a given type of host cell into which it has been introduced. Immediately upstream of the human BSSL/CEL DNA sequence there may be provided a sequence coding for a signal peptide, the presence of which ensures secretion of the human BSSL/CEL expressed by host cells harbouring the vector. The signal sequence may be the one naturally associated with the human BSSL/CEL DNA sequence or of another origin.
The vector may be any vector which may conveniently be subjected to recombinant DNA procedures, and the choice of vector will often depend on the host cell into which it is to be introduced. Thus, the vector may be an autonomously replicating vector, i.e. a vector which exists as an extrachromosomal entity, the replication of which is independent of chromosomal replication; examples of such a vector are a plasmid, phage, cosmid, mini-chromosome or virus. Alternatively, the vector may be one which, when introduced in a host cell, is integrated in the host cell genome and replicated together with the chromosome(s) into which it has been integrated. Examples of suitable vectors are a bacterial expression vector and a yeast expression vector. The vector of the invention may carry any of the DNA molecules of the invention as defined above.
The present invention further relates to a cell harbouring a replicable expression vector as defined above. In principle, this cell may be of any type of cell, i.e. a prokaryotic cell, a unicellular eukaryotic organism or a cell derived from a multicellular organism, e.g. a mammal. The mammalian cells are especially suitable for the purpose and are further discussed below.
In another important aspect, the invention relates to a method of producing recombinant human BSSL/CEL, in which a DNA sequence encoding human BSSL/CEL is inserted in a vector which is able to replicate in a specific host cell, the resulting recombinant vector is introduced into a host cell which is grown in or on an appropriate culture medium under appropriate conditions for expression of human BSSL/CEL and the human BSSL/CEL is recovered.
The medium used to grow the cells may be any conventional medium suitable for the purpose. A suitable vector may be any of the vectors described above, and an appropriate host cell may be any of the cell types listed above. The methods employed to construct the vector and effect introduction thereof into the host cell may be any methods known for such purposes within the field of recombinant DNA. The recombinant human BSSL/CEL expressed by the cells may be secreted, i.e. exported through the cell membrane, dependent on the type of cell and the composition of the vector.
If the human BSSL/CEL is produced intracellularly by the recombinant host, that is, is not secreted by the cell, it may be recovered by standard procedures comprising cell disrupture by mechanical means, e.g. sonication or homogenization, or by enzymatic or chemical means followed by purification.
In order to be secreted, the DNA sequence encoding human BSSL/CEL should be preceded by a sequence coding for a signal peptide, the presence of which ensures secretion of human BSSL/CEL from the cells so that at least a significant proportion of the human BSSL/CEL expressed is secreted into the culture medium and recovered.
The presently preferred method of producing recombinant human BSSL/CEL of the invention is by use of transgenic non-human mammals capable of excreting the human BSSL/CEL into their milk. The use of transgenic non-human mammals has the advantage that large yields of recombinant human BSSL/CEL are obtainable at reasonable costs and, especially when the non-human mammal is a cow, that the recombinant human BSSL/CEL is produced in milk which is the normal constituent of, e.g., infant formulae so that no extensive purification is needed when the recombinant human BSSL/CEL is to be used as a nutrient supplement in milk-based products. Furthermore, production in a higher organism such as a non-human mammal normally leads to the correct processing of the mammalian protein, e.g. with respect to post-translational processing as discussed above and proper folding. Also large quantities of substantially pure human BSSL/CEL may be obtained.
Accordingly, in a further important aspect, the present invention relates to a mammalian expression system comprising a DNA sequence encoding human BSSL/CEL inserted into a gene encoding a milk protein of a non-human mammal so as to form a hybrid gene which is expressible in the mammary gland of an adult female of a mammal harbouring said hybrid gene.
The DNA sequence encoding human BSSL/CEL is preferably a DNA sequence as shown in the Sequence Listing as SEQ ID NO: 1 or a genomic human BSSL/CEL gene or an analogue thereof.
The mammary gland as a tissue of expression and genes encoding milk proteins are generally considered to be particularly suitable for use in the production of heterologous proteins in transgenic non-human mammals as milk proteins are naturally produced at high expression levels in the mammary gland. Also, milk is readily collected and available in large quantities. In the present connection the use of milk protein genes in the production of recombinant human BSSL/CEL has the further advantage that it is produced under conditions similar to the its natural production conditions in terms of regulation of expression and production location (the mammary gland).
In the present context the term "hybrid gene" denotes a DNA sequence comprising on the one hand a DNA sequence encoding human BSSL/CEL as defined above and on the other hand a DNA sequence of the milk protein gene which is capable of mediating the expression of the hybrid gene product. The term "gene encoding a milk protein" denotes an entire gene as well as a subsequence thereof capable of mediating and targeting the expression of the hybrid gene to the tissue of interest, i.e. the mammary gland. Normally, said subsequence is one which at least harbours one or more of a promoter region, a transcriptional start site, 3' and 5' non-coding regions and structural sequences. The DNA sequence encoding human BSSL/CEL is preferably substantially free from prokaryotic sequences, such as vector sequences, which may be associated with the DNA sequence after, e.g., cloning thereof.
The hybrid gene is preferably formed by inserting in vitro the DNA sequence encoding human BSSL/CEL into the milk protein gene by use of techniques known in the art. Alternatively, the DNA sequence encoding human BSSL/CEL can be inserted in vivo by homologous recombinantion.
Normally, the DNA sequence encoding human BSSL/CEL will be inserted in one of the first exons of the milk protein gene of choice or an effective subsequence thereof comprising the first exons and preferably a substantial part of the 5' flanking sequence which is believed to be of regulatory importance.
The hybrid gene preferably comprises a sequence encoding a signal peptide so as to enable the hybrid gene product to be secreted correctly into the mammary gland. The signal peptide will typically be the one normally found in the milk protein gene in question or one associated with the DNA sequence encoding human BSSL/CEL. However, also other signal sequences capable of mediating the secretion of the hybrid gene product to the mammary gland are relevant. Of course, the various elements of the hybrid gene should be fused in such a manner as to allow for correct expression and processing of the gene product. Thus, normally the DNA sequence encoding the signal peptide of choice should be precisely fused to the N-terminal part of the DNA sequence encoding human BSSL/CEL. In the hybrid gene, the DNA sequence encoding human BSSL/CEL will normally comprise its stop codon, but not its own message cleavance and polyadenylation site. Downstream of the DNA sequence encoding human BSSL/CEL, the mRNA processing sequences of the milk protein gene will normally be retained.
A number of factors are contemplated to be responsible for the actual expression level of a particular hybrid gene. The capability of the promoter as well of other regulatory sequences as mentioned above, the integration site of the expression system in the genome of the mammal, the integration site of the DNA sequence encoding human BSSL/CEL in the milk protein encoding gene, elements conferring post-transcriptional regulation and other similar factors may be of vital importance for the expression level obtained. On the basis of the knowledge of the various factors influencing the expression level of the hybrid gene, the person skilled in the art would know how to design an expression system useful for the present purpose.
A variety of different milk proteins are secreted by the mammary gland. Two main groups of milk proteins exist, namely the caseins and the whey proteins. The composition of milk from different species varies qualitatively as well as quantitatively with respect to these proteins. Most non-human mammals produces 3 different types of casein, namely α-casein, β-casein and κ-casein. The most common bovine whey proteins are α-lactalbumin and β-lactalbumin. The composition of milk of various origins are further disclosed in Clark et al. (1987).
The milk protein gene to be used may be derived from the same species as the one in which the expression system is to be inserted, or it may be derived from another species. In this connection it has been shown that the regulatory elements that target gene expression to the mammary gland are functional across species boundaries, which may be due to a possible common ancestor (Hennighausen et al., 1990).
Examples of suitable genes encoding a milk protein or effective subsequences thereof to be used in the construction of an expression system of the invention are normally found among whey proteins of various mammalian origins, e.g. a whey acidic protein (WAP) gene, preferably of murine origin, and a β-lactoglobulin gene, preferably of ovine origin. Also casein genes of various origins may be found to be suitable for the transgenic production of human BSSL/CEL, e.g. bovine αS1-casein and rabbit β-casein. The presently preferred gene is a murine WAP gene as this has been found to be capable of providing a high level of expression of a number of foreign human proteins in milk of different transgenic animals (Hennighausen et al, 1990).
Another sequence preferably associated with the expression system of the invention is a so-called expression stabilizing sequence capable of mediating high-level expression. Strong indications exist that such stabilizing sequences are found in the vicinity of and upstreams of milk protein genes.
The DNA sequence encoding human BSSL/CEL to be inserted in the expression system of the invention may be of genomic or synthetic origin or any combination thereof. Some expression systems have been found to require the presence of introns and other regulatory regions in order to obtain a satisfactory expression (Hennighausen et al., 1990). In some cases it may be advantageous to introduce genomic structures, rather than cDNA elements, as polypeptide encoding element in vector constructs (Brinster et al.). The intron and exon structure may result in higher steady state mRNA levels that obtained when cDNA based vectors are used.
In a further aspect, the present invention relates to a hybrid gene comprising a DNA sequence encoding human BSSL/CEL inserted into a gene encoding a milk protein of a non-human mammal, the DNA sequence being inserted in the milk protein gene in such a manner that it is expressible in the mammary gland of an adult female of a mammal harbouring the hybrid gene. The hybrid gene and its constituents have been discussed in detail above. The hybrid gene constitutes an important intermediate in the construction of an expression system of the invention as disclosed above.
In another aspect, the present invention relates to a non-human mammalian cell harbouring an expression system as defined above. The mammalian cell is preferably an embryo cell or a pro-nucleus. The expression system is suitably inserted in the mammalian cell using a method as explained in the following and specifically illustrated in the Example below.
In a further important aspect, the present invention relates to a method of producing a transgenic non-human mammal capable of expressing human BSSL/CEL, comprising injecting an expression system of the invention as defined above into a fertilized egg or a cell of an embryo of a mammal so as to incorporate the expression system into the germline of the mammal and developing the resulting injected fertilized egg or embryo into an adult female mammal.
The incorporation of the expression system into the germline of the mammal may be performed using any suitable technique, e.g. as described in "Manipulating the Mouse Embryo"; A Laboratory Manual, Cold Spring Harbor Laboratory Press, 1986. For instance, a few hundred molecules of the expression system may be directly injected into a fertilized egg, e.g. a fertilized one cell egg or a pro-nucleus thereof, or an embryo of the mammal of choice and the microinjected eggs may then subsequently be transferred into the oviducts of pseudopregnant foster mothers and allowed to develop. Normally, not all of the injected eggs will develop into adult females expressing human BSSL/CEL. Thus, about half of the mammals will from a statistically point of view be males from which, however, females can be bred in the following generations.
Once integrated in the germ line, the DNA sequence encoding human BSSL/CEL may be expressed at high levels to produce a correctly processed and functional human BSSL/CEL in stable lines of the mammal in question.
Of further interest is a method of producing a transgenic non-human mammal capable of expressing human BSSL/CEL and substantially incapable of expressing BSSL/CEL from the mammal itself, comprising (a) destroying the mammalian BSSL/CEL expressing capability of the mammal so that substantially no mammalian BSSL/CEL is expressed and inserting an expression system of the invention as defined above or a DNA sequence encoding human BSSL/CEL into the germline of the mammal in such a manner that human BSSL/CEL is expressed in the mammal; and/or (b) replacing the mammalian BSSL/CEL gene or part thereof with an expression system of the invention as defined above or a DNA sequence encoding human BSSL/CEL.
The mammalian BSSL/CEL expressing capability is conveniently destroyed by introduction of mutations in the DNA sequence responsible for the expression of the BSSL/CEL. Such mutations may comprise mutations which make the DNA sequence out of frame, or introduction of a stop codon or a deletion of one or more nucleotides of the DNA sequence.
The mammalian BSSL/CEL gene or a part thereof may be replaced with an expression system as defined above or a DNA sequence encoding human BSSL/CEL by use of the well known principles of homologous recombination.
In a further aspect, the present invention relates to a transgenic non-human mammal prepared by a method as described above.
While the transgenic non-human mammal of the invention in its broadest aspect is not restricted to any particular type of mammal, the mammal will normally be selected from the group consisting of mice, rats, rabbits, sheep, pigs, goats and cattle. For large scale production of human BSSL/CEL the larger animals such as sheep, goats, pigs and especially cattle are normally preferred due to their high milk production. However, also mice, rabbits and rats may be interesting due to the fact that the manipulation of these animals is more simple and results in transgenic animals more quickly than when, e.g. cattle, are concerned.
Also progeny of a transgenic mammal as defined above, capable of producing human BSSL/CEL is within the scope of the present invention.
In a further aspect the present invention includes milk from a non-human mammal comprising recombinant human BSSL/CEL.
In a still further aspect, the present invention relates to an infant formula comprising recombinant human BSSL/CEL, in particular a polypeptide of the invention as defined above. The infant formula may be prepared by adding the recombinant human BSSL/CEL or polypeptide in a purified or partly purified form to the normal constituents of the infant formula. However, normally it is preferred that the infant formula is prepared from milk of the invention as defined above, especially when it is of bovine origin. The infant formula may be prepared using conventional procedures and contain any necessary additives such as minerals, vitamins etc.
EXAMPLES
EXAMPLE 1: GENOMIC ORGANIZATION, SEQUENCE ANALYSIS AND CHROMOSOMAL LOCALIZATION OF THE CEL GENE
Standard molecular biology techniques were used (Maniatis et al., 1982; Ausubel et al., 1987; Sambrook et al., 1989) if nothing else is mentioned.
Isolation of Genomic Recombinants
Two different human genomic phage libraries, λDASH (Clonetech Laboratories Inc., Palo Alto, Calif., USA) and λEMBL-3 SP6/T7 (Stratagene, La Jolla, Calif., USA), were screened by plaque hybridization using various subcloned cDNA restriction fragments (Nilsson et al., 1990) as probes, labeled with [α- 32 P]dCTP by the oligolabeling technique (Feinberg et al., 1983).
Mapping, Subcloning and Sequencing of Genomic Clones
Positive clones were digested with various restriction enzymes, electrophoresed on 1% agarose gels and then vacuumtransfered (Pharmacia LKB BTG, Uppsala, Sweden) to a nylon membrane. The membrane was hybridized with various cDNA probes. Restriction fragments, hybridizing with the probes, were isolated using the isotachophoreses method (Ofverstedt et al., 1984). Smaller fragments, <800 bp, were directly inserted into M13mp18, M13mp19, M13BM20 or M13BM21 vectors and sequenced, using E. coli TG1 as host bacteria, whereas larger fragments were subcloned into pTZ18R or pTZ19R vectors, using E. coli DH5α as host bacteria, and further digested. (The plasmids pS309, pS310 and pS451 used in Example 2 below were produced accordingly.) Some of the isolated fragments were also used as probes in hybridizations. All of the nucleotide sequence was determined by the dideoxy chain termination method (Sanger et al., 1977) using Klenow enzyme and either the M13 universal sequencing primer of specific oligonucleotides. Sequence information was retrieved from autoradiograms by the use of the software MS-EdSeq as described by Sjoberg et al. (1989). The sequences were analyzed using the programs obtained from the UWGCG software package (Devereux et al., 1984).
Primer Extension
Total RNA was isolated from human pancreas, lactating mammary gland and adipose tissue by the guanidinium isothiocyanate-CsCl procedure (Chirgwin et al., 1979). Primer extension was performed according to (Ausubel et al., 1987) using total RNA and an antisense 26-mer oligonucleotide (5'-AGGTGAGGCCCAACACAACCAGTTGC-3', SEQ ID NO: 2 in the Sequence Listing), nt position 33-58. Hybridization of the primer with 20 μg of the total RNA was performed in 30 μl of 0.9M NaCl, 0.15M Hepes pH 7.5 and 0.3M EDTA at 30° C. overnight. After the extension reaction with reverse transcriptase, the extension products were analyzed by electrophoresis through a 6% denaturing polyacrylamide gel.
Somatic Cell Hybrids
DNA from 16 human-rodent somatic cell hybrid lines, obtained from NIGMS Human Genetic Mutant Cell Repository (Coriell Institute for Medical Research, Camden, N.J.) were used for the chromosomal assignment of the CEL gene. Human-mouse somatic cell hybrids GM09925 through GM09940 were derived from fusions of fetal human male fibroblasts (IMR-91), with the thymidine kinase deficient mouse cell line B-82 (Taggart et al., 1985; Mohandas et al., 1986). Hybrids GM10324 and GM02860 with the HPRT and APRT deficient mouse cell line A9 (Callen et al., 1986), while hybrid GM10611 resulted from a microcell fusion of the retroviral vector SP-1 infected human lymphoblast cell line GM07890 with the Chinese hamster ovary line UV-135 (Warburton et al., 1990). Hybrid GM10095 was derived from the fusion of lymphocytes from a female with a balanced 46,X,t(X;9)(q13;34) karyotype with the Chinese hamster cell line CHW1102 (Mohandas et al., 1979). The human chromosome content of the hybrid lines, which was determined by cytogenetic analysis as well as by Southern blot analysis and in situ hybridization analysis, are shown in Table 1. High molecular weight DNAs isolated from mouse, Chinese hamster and human parental cell line and the 16 hybrid cell lines were digested with EcoRI, fractionated in 0.8% agarose gels, and transferred to nylon filters. A [α- 32 P]dCTP-labeled CEL cDNA probe (a full-length cDNA) was prepared by oligolabeling (Feinberg and Vogelstein, 1983) and hybridized to the filters. The filters were washed for 60 min each at 65° C. in 6×SSC/0.5% SDS and in 2×SSC/0.5% SDS.
Polymerase Chain Reaction
Total human genomic DNA isolated from leukocytes, DNA from somatic cell hybrids and from some of the positive genomic recombinants and total RNA from human lactating mammary gland and human pancreas were amplified for exon 10 and exon 11. Two μg of DNA were used. The primers used are listed in Table 2 (SEQ ID NOS: 6-11). Thirty cycles of PCR were performed in 100 μl volume [10 mM Tris-HCl, pH 8.3, 50 mM KCl, 1.5 mM MgCl 2 , 200 μM of each dNTP, 100 μg/ml gelatin, 100 pmol of each primer, 1.5 U Taq DNA polymerase (Perkin-Elmer Cetus, Norwalk, Conn., USA)] and the annealing temperature 55° C. for all the primer pairs. The RNA sequence was amplified by the use of combined complementary DNA (cDNA) and PCR methodologies. cDNA was synthesized from 10 μg total RNA in 40 μl of a solution containing 50 mM Tris-HCl, pH 8.3, 50 mM KCl, 10 mM MgCl 2 , 10 μg/ml BSA, 1 mM of each dNTP, 500 ng of oligo(dt) 12-18 , 40 U ribonuclease inhibitor, and 200 U reverse transcriptase (MoMuLV), (BRL, Bethesda Research Laborataries, N.Y., USA) for 30 min at 42° C. The cDNA was precipitated and resuspended in 25 μl H 2 O; 2 μl of this was amplified, as described above. The amplified fragments were analyzed on a 2% agarose gel. Some of the fragments were further subcloned and sequenced.
Gene Structure of the Human CEL Gene
In each genomic library, 10 6 recombinants were screened and the screenings yielded several positive clones, which were all isolated and mapped. Two clones, designated λBSSL1 and λBSSL5A, were further analyzed. Restriction enzyme digestions with several enzymes, Southern blotting followed by hybridization with cDNA probes, indicated that the λBSSL5A clone covers the whole CEL gene and that the λBSSL1 clone covers the 5'-half and about 10 kb of 5'-flanking region (FIG. 1). Together these two clones cover about 25 kb of human genome.
After subcloning and restriction enzyme digestion, suitable fragments for sequencing were obtained and the entire sequence of the CEL gene could be determined, including 1640 bp of the 5'-flanking region and 41 bp of the 3'-flanking region. These data revealed that the human CEL gene (SEQ ID NO: 1) span a region of 9850 bp, containing 11 exons interrupted by 10 introns (FIG. 1). This means that the exons and especially the introns are relatively small. In fact, exons 1-10 range in sizes from 87-204 bp respectively while exon 11 is 841 bp long. The introns range in sizes from 85-2343 bp respectively. As can be noted in Table 3, (SEQ ID NOS: 12-31) all exon/intron boundaries obey the AG/GT rule and conform well to the consensus sequence suggested by Mount et al. (1982). When the coding part of the CEL gene was compared with the cDNA (Nilsson et al., 1990), only one difference in nucleotide sequence was found; the second nt in exon 1, a C, which in the cDNA sequence is a T. Since this position is located 10 nt upstream the translation start codon ATG, this difference does not influence the amino acid sequence.
Seven members of the Alu class of repetitive DNA elements are present in the sequenced region, labeled Alu1-Alu7(5'-3')(FIG. 1), one in the 5'-flanking region and the six others within the CEL gene.
Transcription Initiation Sites and 5'-Flanking Region
To map the human CEL gene transcription initiation site(s), primer extension analysis was performed using total RNA from human pancreas, lactating mammary gland and adipose tissue. The results indicated a major transcription start site located 12 bp, and a minor start site located 8 bases, upstream of the initiator methionine. The transcription initiation sites are the same in both pancreas and lactating mammary gland whereas no signal could be detected in adipose tissue (FIG. 2). The sequenced region includes 1640 nt of 5'-flanking DNA. Based on sequence similarities a TATA-box-like sequence, CATAAAT was found 30 nt upstream the transcription initiation site (FIG. 4, SEQ ID NO: 32 in the Sequence Listing). Neither a CAAT-box structure nor GC boxes were evident in this region.
The 5'-flanking sequence was computer screened, in both strands, for nucleotide sequences known as transcription factor binding sequences in other mammary gland- and pancreatic-specific genes. Several putative recognition sequences were found, see FIG. 4.
Chromosomal Localization of the CEL Gene
In human control DNA the CEL cDNA probe detected four EcoRI fragments of approximately 13 kb, 10 kb, 2.2 kb and 2.0 kb, while in the mouse and hamster control DNAs single fragments of about 25 kb and 8.6 kb, respectively, were detected. The presence of human CEL gene sequences in the hybrid clones correlated only with the presence of human chromosome 9 (Table 1). Only one of the 16 hybrids analyzed were positive for the human CEL gene; this hybrid contained chromosome 9 as the only human chromosome. No discordancies for localization to this chromosome were found, whereas there were at least two discordancies for localization to any other chromosome (Table 1). To further sublocalize the CEL gene we utilized a human-Chinese hamster hybrid (GM 10095) retaining a der(9) translocation chromosome (9pter→9q34:Xq13→Xqter) as the only human DNA. By Southern blot we failed to detect any CEL gene sequences in this hybrid, indicating that the CEL gene resides within the 9q34-qter region.
EXAMPLE 2: CONSTRUCTION OF EXPRESSION VECTORS
To construct an expression vector for production of recombinant human CEL in milk from transgenic animals the following strategy was employed (FIG. 5).
Three pTZ based plasmids (Pharmacia, Uppsala, Sweden) containing different parts of the human CEL gene, pS309, pS310 and pS311 were obtained using the methods described above. The plasmid pS309 contains a SphI fragment covering the the CEL gene from the 5' untranscribed region to part of the fourth intron. The plasmid pS310 contains a SacI fragment covering the CEL gene sequence from part of the first intron to a part of the sixth intron. Third, the plasmid pS311 contains a BamHI fragment covering a variant of the CEL gene from a major part of the fifth intron and the rest of the intron/exon structure. In this plasmid, the repetitive sequence of exon 11 that normally encodes the 16 repeats was mutated to encode a truncated variant having 9 repeats.
Another plasmid, pS283, containing a part of the human CEL cDNA cloned into the plasmid pUC19 at the HindIII and SacI sites was used for fusion of the genomic sequences. pS283 was also used to get a convenient restriction enzyme site, KpnI, located in the 5' untranslated leader sequence of CEL. Plasmid pS283 was then digested with NcoI and SacI and a fragment of about 2.7 kb was isolated. Plasmid pS309 was digested with NcoI and BspEI and a fragment of about 2.3 kb containing the 5'-part of the CEL gene was isolated. Plasmid pS310 was digested with BspEI and SacI and a fragment of about 2.7 kb containing a part of the middle region of the CEL gene was isolated. These three fragments were ligated and transformed into competent E. coli, strain TG2, and transformants were isolated by ampicillin selection. Plasmids were prepared from a number of transformants, and one plasmid called pS312 (FIG. 6), containing the desired construct was used for further experiments.
To obtain a modification of pS311, in which the BamHI site located downstream of the stop codon was converted to a SalI site to facilitate further cloning, the following method was used. pS311 was linearized by partial BamHI digestion. The linearized fragment was isolated and a synthetic DNA linker that converts BamHI to a SalI site (5'-GATCGTCGAC-3', SEQ ID NO: 3 in the Sequence Listing), thereby destroying the BamHI site, was inserted. Since there were two potential positions for integration of the synthetic linker the resulting plasmids were analyzed by restriction enzyme cleavage. A plasmid with the linker inserted at the desired position downstream of exon 11 was isolated and designated pS313.
To obtain the expression vector construct that harbours CEL genomic sequences and encodes the truncated CEL variant, the plasmid pS314 which was designed to mediate stage and tissue specific expression in the mammary gland cells under lactation periods was used. Plasmid pS314 contains a genomic fragment from the murine whey acidic protein (WAP) gene (Campbell et al. 1984) cloned as a NotI fragment. The genomic fragment has approximately 4.5 kb upstream regulatory sequences (URS), the entire transcribed exon/intron region and about 3 kb of sequence downstream of the last exon. A unique KpnI site is located in the first exon 24 bp upstream of the natural WAP translation initiation codon. Another unique restriction enzyme site is the SalI site located in exon 3. In pS314, this SalI site was destroyed by digestion, fill in using Klenow and religation. Instead, a new SalI site was introduced directly downstream of the KpnI site in exon 1. This was performed by KpnI digestion and introduction of annealed synthetic oligomers SYM 2401 5'-CGTCGACGTAC-3' (SEQ ID NO: 4 in the Sequence Listing), and SYM 2402 5'-GTCGACGGTAC-3' (SEQ ID NO: 5 in the Sequence Listing), at this position (FIG. 8) The human CEL genomic sequence was inserted between these sites, KpnI and SalI, by the following strategy. First, pS314 was digested with KpnI and SalI and a fragment representing the cleaved plasmid was electrophoretically isolated. Second, pS312 was digested with KpnI and BamHI and a approximately 4.7 kb fragment representing the 5' part of the human CEL gene was isolated. Third, pS313 was digested with BamHI and SalI and the 3'-part of the human CEL gene was isolated. These three fragments were ligated, transformed into competent E. coli bacteria and transformants were isolated after ampicillin selection. Plasmids were prepared from several transformants and carefully analyzed by restriction enzyme mapping and sequence analysis. One plasmid representing the desired expression vector was defined and designated pS317.
In order to construct a genomic CEL expression vector encoding full-length CEL pS317 was modified as follows (FIG. 5). First, a pTZ18R plasmid (Pharmacia) containing a 5.2 kb BamHI fragment of the human CEL gene extending from the fifth intron to downstream of the eleventh exon, pS451, was digested with HindIII and SacI. This digestion generated a fragment of about 1.7 kb that extends from the HindIII site located in intron 9 to the SacI site located in exon 11. Second, the plasmid pS313 was digested with SacI and SalI, and a 71 bp fragment containing the 3' part of exon 11 and the generated SalI site was isolated. Third, the rest of the WAP/CEL recombinant gene and the plasmid sequences was isolated as a SalI/HindIII fragment of about 20 kb from pS317. These three fragments were ligated and transformed into bacteria. Plasmids were prepared from several transformants. The plasmids were digested with various restriction enzymes and subjected to sequence analysis. One plasmid containing the desired recombinant gene was identified. This final expression vector was designated pS452 (FIG. 7).
To remove the prokaryotic plasmid sequences, pS452 was digested with NotI. The recombinant vector element consisting of murine WAP sequence flanking the human CEL genomic fragment was then isolated by agarose electrophoresis. The isolated fragment was further purified using electroelution, before it was injected into mouse embryos.
The recombinant WAP/CEL gene for expression in mammary gland of transgenic animals is shown in FIG. 8.
DEPOSITS
The following plasmids have been deposited in accordance with the Budapest Treaty at DSM (Deutsche Samlung von Mikroorganismen und Zellkulturen):
______________________________________Plasmid Deposit No. Date of deposit______________________________________pS309 DSM 7101 12 June 1992pS310 DSM 7102pS451 DSM 7498 26 February 1993pS452 DSM 7499______________________________________
EXAMPLE 3: GENERATION OF TRANSGENIC ANIMALS
A NotI fragment was isolated from the plasmid pS452 according to Example 2. This DNA fragment contained the murine WAP promoter linked to a genomic sequence encoding human BSSL/CEL. The isolated fragment, at a concentration of 3 ng/μl, was injected into the pronucleus of 350 C57B1/6JxCBA/2J-f 2 embryos obtained from donor mice primed with 5 IU pregnant mare's serum gonadotropin for superovulation. The C57B1/6JxCBA/2J-f 1 animals were obtained from Bomholtgard Breeding and Research Centre LTD, Ry, Denmark. After collection of the embryos from the oviduct, they were separated from the cumulus cells by treatment with hyaluronidase in the medium M2 (Hogan et al., 1986). After washing the embryos were transferred to the medium M16 (Hogan et al., 1986) and kept in an incubator with 5% CO 2 -atmosphere. The injections were performed in a microdrop of M2 under light paraffin oil using Narishigi hydraulic micromanipulators and a Nikon inverted microscope equipped with Nomarski optics. After injection, healthy looking embryos were implanted into pseudopregnant C57B1/6JxCBA/2J-f 1 recipients given 0.37 ml of 2.5% Avertin intraperitoneally. Mice that had integrated the transgene were identified with PCR analysis of DNA from tail biopsy specimens obtained three weeks after birth of the animals. Positive results were confirmed with Southern blot analysis.
EXAMPLE 4: EXPRESSION OF BSSL/CEL IN TRANSGENIC MICE
Transgenic mice were identified by analysis of DNA which has been prepared from excised tail samples. The tissue samples were incubated with proteinase K and phenol/chloroform extracted. The isolated DNA was used in polymerase chain reactions with primers which amplify specific fragments if the heterologous introduced DNA representing the expression vector fragment is present. The animals were also analyzed by DNA hybridization experiments to confirm PCR data and to test for possible rearrangements, structure of the integrated vector elements and to obtain information about the copy number of integrated vector elements.
In one set of experiments, 18 mice were analyzed with the two methods and the results demonstrated that 1 mouse was carrying the heterologous DNA vector element derived from pS452. The result from the PCR analysis and the hybridization experiments were identical (FIG. 9, SEQ ID NOS: 57 and 58 in the Sequence Listing).
The mouse identified to carry vector DNA element (founder animal) was then mated and the F1 litter was analyzed for transgene by the same procedures.
Female lactating animals were injected with 2 IU oxytocin intraperitoneally and 10 minutes later anaesthetized with 0.40 ml of 2.5% Avertin intraperitoneally. A milk collecting device was attached to the nipple via a siliconized tubing and milk was collected into a 1.5 ml Eppendorf tube by gentle massage of the mammary gland. The amount of milk varied, dependent on the day of lactation, between 0.1 and 0.5 ml per mouse and collection.
Analyze for the presence of recombinant human BSSL/CEL was done by SDS-PAGE, transfer to nitrocellulose membranes and incubation with polyclonal antibodies generated against native human BSSL/CEL. The obtained results demonstrated expression of recombinant human BSSL/CEL in milk from transgenic mice. FIG. 10 demonstrates presence of recombinant human BSSL/CEL in milk from transgenic mice: the band at about 116.5.
Stable lines of transgenic animals are generated. In a similar manner, other transgenic animals such as cows or sheep capable of expressing human BSSL/CEL may be prepared.
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TABLE 1__________________________________________________________________________Correlation of CEL sequences with human chromosomes in 16 human-rodentsomatic cell hybrids. PERCENTAGE OF CELLS WITH HUMAN CHROMOSOMES.sup.aCHROMOSOME 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 X Y CEL__________________________________________________________________________HYBRIDGM09925 74 24 0 74 76 60 82 78 0 0 4 68 6 86 78 14 98 96 46 84 0 76 0 0 -GM09927 69 83 75 77 0 93 79 73 0 82 0 0 77 79 90 0 81 73 87 89 0 0 0 0 -GM09929 0 0 61 59 0 43 2 49 0 0 33 49 0 59 2 0 96 0 2 31 0 0 2 0 -GM09930A 0 34 62 4 12 0 26 4 0 0 6 22 56 82 12 0 86 78 0 22 82 76 6 8 -GM09932 0 0 0 68 86 46 0 80 0 2 28 26 0 0 0 0 96 0 2 0 92 0 0 0 -GM09933 50 0 84 16 54 76 92 54 0 6 0 50 84 78 92 0 88 70 80 32 94 88 0 32 -GM09934 0 50 0 0 83 79 4 87 0 0 77 87 0 2 89 0 90 89 0 91 89 2 0 0 -GM09935A 0 0 52 10 28 12 0 0 0 8 0 22 74 72 0 0 93 59 0 9 91 71 0 0 -GM09936 0 0 0 18 0 46 70 10 0 16 34 0 2 88 2 0 100 0 44 24 0 18 0 0 -GM09937 0 0 54 38 0 62 54 70 0 4 0 42 0 70 60 0 96 66 0 0 0 0 0 0 -GM09938 0 0 2 88 60 88 86 4 0 0 36 92 0 80 4 0 92 0 4 80 76 60 0 2 -GM09940 0 0 46 0 0 0 84 62 0 0 0 0 0 0 62 0 100 0 0 0 0 0 0 0 -GM10324 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 90 0 -GM10567 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 98 0 0 0 0 0 0 0 0 -GM10611 0 0 0 0 0 0 0 0 69 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 +GM10095 0 0 0 0 0 0 0 0 94.sup.b 0 0 0 0 0 0 0 0 0 0 0 0 0 94.sup.b 0 -Discordancy 4 5 8 7 7 10 9 9 0 2 6 10 5 10 7 2 13 8 5 9 7 6 3 2ratio 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16__________________________________________________________________________ .sup.a In general, a human chromosome has to be present in more than 20 t 22% of the cells to be detected by Southern blot analysis .sup.b Contains 9pter→q34 and Xq13→qter.
TABLE 2__________________________________________________________________________Primers Used for DNA AmplificationOligonucleotide nt Position.sup.a Sequence amplified__________________________________________________________________________P1: 5'-AGACCTACGCCTACCTG-3' 8492-8508 Exon 10P2: 5'-TCCAGTAGGCGATCATG-3' 8646-8662P4: 5'-GACCGATGTCCTCTTCCTGG-3' 7220-7239 Exon 10 with primers fromP5: 5'-CAGCCGAGTCGCCCATGTTG-3' 9016-9035 exons surrounding exon 10.sup.bP6: 5'-ACCAAGAAGATGGGCAGCAGC-3' 9089-9109 The repetition in exon 11P7: 5'-GACTGCAGGCATCTGAGCTTC-3' 9722-9742__________________________________________________________________________ .sup.a The nucleotide position is given as the number of bases from the start of the first exon. In order to compare the nucleotide position with SEQ ID NO: 1, add 1640 bases to the number in the column. .sup.b For amplification of "exon 10" from cDNA
TABLE 3__________________________________________________________________________Exon-Intron organization of the CEL geneExon Intronnucleotide length amino acids sequence at exon-intron junction lengthno. position.sup.a (nt) pos. no. 5' splice doner 3' splice acceptor no. (nt)__________________________________________________________________________1 1-87 87 1- (25) GCC GCG AAG gtaaga....gtgtctccctcgcag CTG GGC GCC I 2343 252 2431-2581 151 26- (50) TGG CAA G gtggga....tcctgccacctgcag GG ACC CTG II 85 753 2667-2789 123 76- (41) AAG CAA G gtctgc....gctcccccatctcag TC TCC CGG III 277 1164 3067-3264 198 117- (66) CTG CCA G gtgcgt....ctgccctgcccccag GT AAC TAT IV 1288 1825 4553-4683 131 183- (44) TCT CTG CAG gtctcg....ttctgggtcccgtag ACC CTC TCC V 177 2266 4861-4968 108 227- (36) GCC AAA AAG gtaaac....tggttctgcccccag GTG GCT GAG VI 142 2627 5111-5228 118 263- (39) CTG GAG T gtgagt....ggctctcccacccag AC CCC ATG VII 1466 3018 6695-6881 187 302- (63) GTC ACG GA gtaagc....acttgattcccccag G GAG GAC VIII 197 3649 7079-7282 204 365- (68) AAT GCC AA gtgagg....gtctctcccctccag G AGT GCC IX 1201 43210 8484-8681 198 433- (66) AAA ACA GG gtaaga....cttctcactctgcag G GAC CCC X 328 49811 9010-9850 841 499- (247) 745__________________________________________________________________________ .sup.a The nucleotide position is given as the number of bases from the start of the first exon. In order to compare the nucleotide position with SEQ ID NO: 1, add 1640 bases to the number in the column.
__________________________________________________________________________SEQUENCE LISTING(1) GENERAL INFORMATION:(iii) NUMBER OF SEQUENCES: 58(2) INFORMATION FOR SEQ ID NO:1:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 11531 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: double(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(vi) ORIGINAL SOURCE:(A) ORGANISM: Homo sapiens(F) TISSUE TYPE: Mammary gland(ix) FEATURE:(A) NAME/KEY: CDS(B) LOCATION: join(1653..1727, 4071..4221, 4307..4429, 4707..4904, 6193..6323, 6501..6608, 6751..6868, 8335..8521, 8719..8922, 10124..10321, 10650..11394)(ix) FEATURE:(A) NAME/KEY: mat.sub.-- peptide(B) LOCATION: join(1722..1727, 4071..4221, 4307..4429, 4707..4904, 6193..6323, 6501..6608, 6751..6868, 8335..8521, 8719..8922, 10124..10321, 10650..11391)(D) OTHER INFORMATION: /EC.sub.-- number=3.1.1.1/product="Bile Salt-Stimulated Lipase"(ix) FEATURE:(A) NAME/KEY: 5'UTR(B) LOCATION: 1..1640(ix) FEATURE:(A) NAME/KEY: TATA.sub.-- signal(B) LOCATION: 1611..1617(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 1641..1727(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 4071..4221(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 4307..4429(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 4707..4904(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 6193..6323(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 6501..6608(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 6751..6868(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 8335..8521(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 8719..8922(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 10124..10321(ix) FEATURE:(A) NAME/KEY: exon(B) LOCATION: 10650..11490(ix) FEATURE:(A) NAME/KEY: 3'UTR(B) LOCATION: 11491..11531(xi) SEQUENCE DESCRIPTION: SEQ ID NO:1:GGATCCCTCGAACCCAGGAGTTCAAGACTGCAGTGAGCTATGATTGTGCCACTGCACTCT60AGCCTGGGTGACAGAGACCCTGTCTCAAAAAAACAAACAAACAAAAAACCTCTGTGGACT120CCGGGTGATAATGACATGTCAATGTGGATTCATCAGGTGTTAACAGCTGTACCCCCTGGT180GGGGGATGTTGATAACGGGGGAGACTGGAGTGGGGCGAGGACATACGGGAAATCTCTGTA240ATCTTCCTCTAATTTTGCTGTGAACCTAAAGCTGCTCTAAAAATGTACATAGATATAAAC300TGGGGCCTTCCTTTCCCTCTGCCCTGCCCCAGCCCTCCCCCACCTCCTTCCTCTCCCTGC360TGCCTCCCCTCTGCCCTCCCCTTTCCTCCTTAGCCACTGTAAATGACACTGCAGCAAAGG420TCTGAGGCAAATGCCTTTGCCCTGGGGCGCCCCAGCCACCTGCAGGCCCCTTATTTCCTG480TGGCCGAGCTCCTCCTCCCACCCTCCAGTCCTTTCCCCAGCCTCCCTCGCCCACTAGGCC540TCCTGAATTGCTGGCACCGGCTGTGGTCGACAGACAGAGGGACAGACGTGGCTCTGCAGG600TCCACTCGGTCCCTGGCACCGGCCGCAGGGGTGGCAGAACGGGAGTGTGGTTGGTGTGGG660AAGCACAGGCCCCAGTGTCTCCTGGGGGACTGTTGGGTGGGAAGGCTCTGGCTGCCCTCA720CCCTGTTCCCATCACTGCAGAGGGCTGTGCGGTGGCTGGAGCTGCCACTGAGTGTCTCGG780TGAGGGTGACCTCACACTGGCTGAGCTTAAAGGCCCCATCTGAAGACTTTGTTCGTGGTG840TTCTTTCACTTCTCAGAGCCTTTCCTGGCTCCAGGATTAATACCTGTTCACAGAAAATAC900GAGTCGCCTCCTCCTCCACAACCTCACACGACCTTCTCCCTTCCCTCCCGCTGGCCTCTT960TCCCTCCCCTTCTGTCACTCTGCCTGGGCATGCCCCAGGGCCTCGGCTGGGCCCTTTGTT1020TCCACAGGGAAACCTACATGGTTGGGCTAGATGCCTCCGCACCCCCCCACCCACACCCCC1080TGAGCCTCTAGTCCTCCCTCCCAGGACACATCAGGCTGGATGGTGACACTTCCACACCCT1140TGAGTGGGACTGCCTTGTGCTGCTCTGGGATTCGCACCCAGCTTGGACTACCCGCTCCAC1200GGGCCCCAGGAAAAGCTCGTACAGATAAGGTCAGCCACATGAGTGGAGGGCCTGCAGCAT1260GCTGCCCTTTCTGTCCCAGAAGTCACGTGCTCGGTCCCCTCTGAAGCCCCTTTGGGGACC1320TAGGGGACAAGCAGGGCATGGAGACATGGAGACAAAGTATGCCCTTTTCTCTGACAGTGA1380CACCAAGCCCTGTGAACAAACCAGAAGGCAGGGCACTGTGCACCCTGCCCGGCCCCACCA1440TCCCCCTTACCACCCGCCACCTTGCCACCTGCCTCTGCTCCCAGGTAAGTGGTAACCTGC1500ACAGGTGCACTGTGGGTTTGGGGAAAACTGGATCTCCCTGCACCTGAGGGGGTAGAGGGG1560AGGGAGTGCCTGAGAGCTCATGAACAAGCATGTGACCTTGGATCCAGCTCCATAAATACC1620CGAGGCCCAGGGGGAGGGCCACCCAGAGGCTGATGCTCACCATGGGGCGCCTG1673MetLeuThrMetGlyArgLeu23-20CAACTGGTTGTGTTGGGCCTCACCTGCTGCTGGGCAGTGGCGAGTGCC1721GlnLeuValValLeuGlyLeuThrCysCysTrpAlaValAlaSerAla15-10-5GCGAAGGTAAGAGCCCAGCAGAGGGGCAGGTCCTGCTGCTCTCTCGCTCAATCAGA1777AlaLysTCTGGAAACTTCGGGCCAGGCTGAGAAAGAGCCCAGCACAGCCCCGCAGCAGATCCCGGG1837CACTCACGCTCATTTCTATGGGGACAGGTGCCAGGTAGAACACAGGATGCCCAATTCCAT1897TTGAATTTCAGATAAACTGCCAAGAACTGCTGTGTAAGTATGTCCCATGCAATATTTGAA1957ACAAATTTCTATGGGCCGGGCGCAGTGGCTCACACCTGCAATCCCACCAGTTTGGGAGGC2017CGAGGTGGGTGGATCACTTGAGGTCAGGAGTTGGAGACCAGCCTGGCCAACATGGTGAAA2077CCCCGTCTCTACTAAAAATACAAATATTAATCGGGCGTGGTGGTGGGTGCCTGTAATCCC2137AGCTACTCGGGAGGCTGAGGCAGGAGAACCGCTTGAAGCTGGGAGGTGGAGATTGCGGTG2197AGCTGAGATCACGCTACTGCACTCCAGCCTGGGTGACAGGGCGAGACTCTGTCTCAAAAA2257ATAGAAAAAGAAAAAAATGAAACATACTAAAAAACAATTCACTGTTTACCTGAAATTCAA2317ATGTAACTGGGCCTCTTGAATTTACATTTGCTAATCCTGGTGATTCCACCTACCAACCTC2377TCTGTTGTTCCCATTTTACAGAAGGGGAAACGGGCCCAGGGGCAGGGAGTGTGGAGAGCA2437GGCAGACGGGTGGAGAGAAGCAGGCAGGCAGTTTGCCCAGCATGGCACAGCTGCTGCCTC2497CTATTCCTGTGCAGGAAGCTGAAAGCCGGGCTACTCCACACCCGGGTCCGGGTCCCTCCA2557GAAAGAGAGCCGGCAGGCAGGAGCTCTCTCGAGGCATCCATAAATTCTACCCTCTCTGCC2617TGTGAAGGAGAAGCCACAGAAACCCCAAGCCCCACAGGAAGCCGGTGTCGGTGCCCGGCC2677CAGTCCCTGCCCCCAGCAGGAGTCACACAGGGGACCCCAGATCCCAACCACGCTGTTCTG2737CTGCCTGCGGTGTCTCAGGCCCTGGGGACTCCTGTCTCCACCTCTGCTGCCTGCTCTCCA2797CACTCCCTGGCCCTGGGACCGGGAGGTTTGGGCAGTGGTCTTGGGCTCCTGACTCAAAGG2857AGAGGTCACCTTCTTCTTGGGCGAGCTCTTCTTGGGGTGCTGAGAGGCCTTCGGCAGGTC2917ATCACGACCCCTCCCCATTTCCCCACCCTGAGGCCCTCTGGCCAGTCTCAATTGCACAGG2977GATCACGCCACTGGCACAAGGAGACACAGATGCCTCGCAGGGGATGCCCACGATGCCTGC3037ATGTGTTGCTTCTGGTTCCTTTCCTCCAGTTCCAACCGCCGCACTCTCCCACACCAGTGT3097GACAGGGGGCCCATCACCCTAGACTTCAGAGGGCTGCTGGGACCCTGGCTGGGCCTGGGG3157GTGTAGGGCCACCCTGCCCTTCCCCACCTGGAACCTGGCACAGGTGACAGCCAGCAAGCA3217ATGACCTGGTCCCACCATGCACCACGGGAAGAGGGAGCTGCTGCCCAAGATGGACAGGAG3277GTGGCACTGGGGCAGACAGCTGCTTCTCAACAGGGTGACTTCAAGCCCAAAAGCTGCCCA3337GCCTCAGTTCCGTCAGGGACAGAGGGTGGATGAGCACCAACCTCCAGGCCCCTCGTGGGG3397GTGGACAGCTTGGTGCACAGAGGCCATTTTCATGGCACAGGGAAGCGTGGCGGGGGTGGG3457AGGTGTGGTCCCTAGGGGGTTCTTTACCAGCAGGGGGCTCAGGAACTGTGGGGACTTGGG3517CATGGGGCCATCGACTTTGTGCCCAGCCAGCTAGGCCCTGTGCAGGGAGATGGGAGGAGG3577GAAAAGCAGGCCCCACCCCTCAGAAAGGAGGAAGGTTGGTGTGAAACATCCCGGGTACAC3637TGAGCATTGGGTACACTCCTCCCGGGAGCTGGACAGGCCTCCCATGTGATGGCAAACAGG3697CCGACAGGAGACACGGCTGTTGCTCGTCTTCCACATGGGGAAACTGAGGATCGGAGTCAA3757AGCTGGGCGGCCATAGCCAGAACCCAAACCTCCATCCCACCTCTTGGCCGGCTTCCCTAG3817TGGGAACACTGGTTGAACCAGTTTCCTCTAAGATTCTGGGAGCAGGACACCCCCAGGGAT3877AAGGAGAGGAACAGGAATCCTAAAGCCCTGAGCATTGCAGGGCAGGGGGTGCTGCCTGGG3937TCTCCTGTGCAGAGCTGTCCTGCTTTGAAGCTGTCTTTGCCTCTGGGCACGCGGAGTCGG3997CTTGCCTTGCCCCCTCCGGATTCAGGCCGATGGGGCTTGAGCCCCCCTGACCCTGCCCGT4057GTCTCCCTCGCAGCTGGGCGCCGTGTACACAGAAGGTGGGTTCGTGGAA4106LeuGlyAlaValTyrThrGluGlyGlyPheValGlu510GGCGTCAATAAGAAGCTCGGCCTCCTGGGTGACTCTGTGGACATCTTC4154GlyValAsnLysLysLeuGlyLeuLeuGlyAspSerValAspIlePhe15202530AAGGGCATCCCCTTCGCAGCTCCCACCAAGGCCCTGGAAAATCCTCAG4202LysGlyIleProPheAlaAlaProThrLysAlaLeuGluAsnProGln354045CCACATCCTGGCTGGCAAGGTGGGAGTGGGTGGTGCCGGACTGGCCCTG4251ProHisProGlyTrpGln50CGGCGGGGCGGGTGAGGGCGGCTGCCTTCCTCATGCCAACTCCTGCCACCTGCAGGG4308GlyACCCTGAAGGCCAAGAACTTCAAGAAGAGATGCCTGCAGGCCACCATC4356ThrLeuLysAlaLysAsnPheLysLysArgCysLeuGlnAlaThrIle556065ACCCAGGACAGCACCTACGGGGATGAAGACTGCCTGTACCTCAACATT4404ThrGlnAspSerThrTyrGlyAspGluAspCysLeuTyrLeuAsnIle70758085TGGGTGCCCCAGGGCAGGAAGCAAGGTCTGCCTCCCCTCTACTCC4449TrpValProGlnGlyArgLysGln90CCAAGGGACCCTCCCATGCAGCCACTGCCCCGGGTCTACTCCTGGCTTGAGTCTGGGGGC4509TGCAAAGCTGAACTTCCATGAAATCCCACAGAGGCGGGGAGGGGAGCGCCCACTGCCGTT4569GCCCAGCCTGGGGCAGGGCAGCGCCTTGGAGCACCTCCCTGTCTTGGCCCCAGGCACCTG4629CTGCACAGGGACAGGGGACCGGCTGGAGACAGGGCCAGGCGGGGCGTCTGGGGTCACCAG4689CCGCTCCCCCATCTCAGTCTCCCGGGACCTGCCCGTTATGATCTGGATC4738ValSerArgAspLeuProValMetIleTrpIle95100TATGGAGGCGCCTTCCTCATGGGGTCCGGCCATGGGGCCAACTTCCTC4786TyrGlyGlyAlaPheLeuMetGlySerGlyHisGlyAlaAsnPheLeu105110115120AACAACTACCTGTATGACGGCGAGGAGATCGCCACACGCGGAAACGTC4834AsnAsnTyrLeuTyrAspGlyGluGluIleAlaThrArgGlyAsnVal125130135ATCGTGGTCACCTTCAACTACCGTGTCGGCCCCCTTGGGTTCCTCAGC4882IleValValThrPheAsnTyrArgValGlyProLeuGlyPheLeuSer140145150ACTGGGGACGCCAATCTGCCAGGTGCGTGGGTGCCTTCGGCCCTGAGGTGGG4934ThrGlyAspAlaAsnLeuPro155GCGACCAGCATGCTGAGCCCAGCAGGGAGATTTTCCTCAGCACCCCTCACCCCAAACAAC4994CAGTGGCGGTTCACAGAAAGACCCGGAAGCTGGAGTAGAATCATGAGATGCAGGAGGCCC5054TTGGTAGCTGTAGTAAAATAAAAGATGCTGCAGAGGCCGGGAGAGATGGCTCACGCCTGT5114AATCCCAGCACTTTAGGAGGCCCACACAGGTGGGTCACTTGAGCGCAGAAGTTCAAGACC5174AGCCTGAAAATCACTGGGAGACCCCCATCTCTACACAAAAATTAAAAATTAGCTGGGGAC5234TGGGCGCGGCGGCTCACCTCTGTAATCCCAGCACGTTGGGAGCCCAAGGTGGGTAGATCA5294CCTGAGGTCAGGAGTTTGAGACCAGCCTGACTAAAATGGAGAAACCTCTTCTCTACTAAA5354AATACAAAATTAGCCAGGCGTGGTGGCGCTTGCCTGTAATCCCAGCTACTCGGGAGGCTG5414AGGCAGGAGAATCGCTTGAACTCAGGAGGCGGAGGTTGCGGTGAGCCGAGATCATGCCAC5474TGCACTCCAGCCTGGAGAACAAGAGTAAAACTCTGTCTCAAAAAAAAAAAAAAAAAAAAA5534ATAGCCAGGCGTGGTATCTCATGCCTCTGTCCTCAGCTACCTGGGAGGCAGAGGTGGAAG5594GATCGCTTGAGCCCAGGGGTTCAAAGCTGCAGTGAGCCGTGGTCGTGCCACTGCACTCCA5654GCCTGGGCGACAGAGTGAGGCCCCATCTCAAAAATAAGAGGCTGTGGGACAGACAGACAG5714GCAGACAGGCTGAGGCTCAGAGAGAAACCAGGAGAGCAGAGCTGAGTGAGAGACAGAGAA5774CAATACCTTGAGGCAGAGACAGCTGTGGACACAGAAGTGGCAGGACACAGACAGGAGGGA5834CTGGGGCAGGGGCAGGAGAGGTGCATGGGCCTGACCATCCTGCCCCCGACAAACACCACC5894CCCTCCAGCACCACACCAACCCAACCTCCTGGGGACCCACCCCATACAGCACCGCACCCG5954ACTCAGCCTCCTGGGACCCACCCACTCCAGCAACCAACGTGACCTAGTCTCCTGGGACCC6014ACCCCCTCCAGCACCCTACCCGACCCAGCTTCTTAGGGACCCACCATTTGCCAACTGGGC6074TCTGCCATGGCCCCAACTCTGTTGAGGGCATTTCCACCCCACCTATGCTGATCTCCCCTC6134CTGGAGGCCAGGCCTGGGCCACTGGTCTCTAGCACCCCCTCCCCTGCCCTGCCCCCAGGT6194Gly160AACTATGGCCTTCGGGATCAGCACATGGCCATTGCTTGGGTGAAGAGG6242AsnTyrGlyLeuArgAspGlnHisMetAlaIleAlaTrpValLysArg165170175AATATCGCGGCCTTCGGGGGGGACCCCAACAACATCACGCTCTTCGGG6290AsnIleAlaAlaPheGlyGlyAspProAsnAsnIleThrLeuPheGly180185190GAGTCTGCTGGAGGTGCCAGCGTCTCTCTGCAGGTCTCGGGATCCCTGTGGGG6343GluSerAlaGlyGlyAlaSerValSerLeuGln195200AGGGCCTGCCCCACAGGTTGAGAGGAAGCTCAAACGGGAAGGGGAGGGTGGGAGGAGGAG6403CGTGGAGCTGGGGCTGTGGTGCTGGGGTGTCCTTGTCCCAGCGTGGGGTGGGCAGAGTGG6463GGAGCGGCCTTGGTGACGGGATTTCTGGGTCCCGTAGACCCTCTCCCCCTACAAC6518ThrLeuSerProTyrAsn205AAGGGCCTCATCCGGCGAGCCATCAGCCAGAGCGGCGTGGCCCTGAGT6566LysGlyLeuIleArgArgAlaIleSerGlnSerGlyValAlaLeuSer210215220225CCCTGGGTCATCCAGAAAAACCCACTCTTCTGGGCCAAAAAG6608ProTrpValIleGlnLysAsnProLeuPheTrpAlaLysLys230235GTAAACGGAGGAGGGCAGGGCTGGGCGGGGTGGGGGCTGTCCACATTTCCGTTCTTTATC6668CTGGACCCCATCCTTGCCTTCAAATGGTTCTGAGCCCTGAGCTCCGGCCTCACCTACCTG6728CTGGCCTTGGTTCTGCCCCCAGGTGGCTGAGAAGGTGGGTTGCCCTGTGGGT6780ValAlaGluLysValGlyCysProValGly240245GATGCCGCCAGGATGGCCCAGTGTCTGAAGGTTACTGATCCCCGAGCC6828AspAlaAlaArgMetAlaGlnCysLeuLysValThrAspProArgAla250255260265CTGACGCTGGCCTATAAGGTGCCGCTGGCAGGCCTGGAGTGTGAGTAGCT6878LeuThrLeuAlaTyrLysValProLeuAlaGlyLeuGlu270275GCTCGGGTTGGCCCATGGGGTCTCGAGGTGGGGGTTGAGGGGGGTACTGCCAGGGAGTAC6938TCCGGAGGAGAGAGGAAGGTGCCAGAGCTGCGGTCTTGTCCTGTCACCAACTAGCTGGTG6998TCTCCCCTCGAAGGCCCCAGCTGTAAGGGAGAGGGGGTGCCGTTTCTTCTTTTTTTTTGA7058GATGGAGTCTCACTGTTGCCCAGGCTGGAGTGCAGTGTCACGATCTCAGCTCACTGCAAC7118CTCCACCTCCTGGGTTCAAGTGATTCTCTGACTCAACCTCCCATGTAGCTGGGACTACAG7178GCACATGCCACCATGCCCAGATAATTTTTCTGTGTGTTTAGTAGGGATGGAGTTTCATCG7238TGTTAGCTAGGATGATCTCGGTCTTGGGACCTCATGATCTGCCCACCTCGGCCTCCCAAA7298GTGCTGGAATTACAGGCGTGAGCCACTGTGCCCGGCCCCTTCTTTATTCTTATCTCCCAT7358GAGTTACAGACTCCCCTTTGAGAAGCTGATGAACATTTGGGGCCCCCTCCCCCACCTCAT7418GCATTCATATGCAGTCATTTGCATATAATTTTAGGGAGACTCATAGACCTCAGACCAAGA7478GCCTTTGTGCTAGATGACCGTTCATTCATTCGTTCATTCATTCAGCAAACATTTACTGAA7538CCGTAGCACTGGGGCCCAGCCTCCAGCTCCACTATTCTGTACCCCGGGAAGGCCTGGGGA7598CCCATTCCACAAACACCTCTGCATGTCAGCCTTACCAGCTTGCTACGCTAAGGCTGTCCC7658TCACTCATTCTTCTATGGCAACATGCCATGAAGCCAAGTCATCTGCACGTTTACCTGACA7718TGAGCTCAACTGCACGGGCTGGACAAGCCCAAACAAAGCAACCCCCACGGCCCCGCTAGA7778AGCAAAACCTGCTGTGCTGGGCCCAGTGACAGCCAGGCCCCGCCTGCCTCAGCAGCCACT7838GGGTCCTCTAGGGGCCCGTCCAGGGGTCTGGAGTACAATGCAGACCTCCCACCATTTTTG7898GCTGATGGACTGGAACCCAGCCCTGAGAGAGGGAGCTCCTTCTCCATCAGTTCCCTCAGT7958GGCTTCTAAGTTTCCTCCTTCCTGCTTCAGGCCCAGCAAAGAGAGAGAGGAGAGGGAGGG8018GCTGCCGCTGAAGAGGACAGATCTGGCCCTAGACAGTGACTCTCAGCCTGGGGACGTGTG8078GCAGGGCCTGGAGACATCTGTGATTGTCACAGCTGGGGAGGGGGTGCTCCTGGCACCTCG8138TGGGTCGAGGCCGGGGATGCTCTAAACATCCTACAGGGCACAGGATGCCCCTGATGGTGC8198AGAATCAACCCTGCCCCAAGTGTCCATAGATCAGAGAAGGGAGGACATAGCCAATTCCAG8258CCCTGAGAGGCAAGGGGCGGCTCAGGGGAAACTGGGAGGTACAAGAACCTGCTAACCTGC8318TGGCTCTCCCACCCAGACCCCATGCTGCACTATGTGGGCTTCGTCCCT8366TyrProMetLeuHisTyrValGlyPheValPro280285GTCATTGATGGAGACTTCATCCCCGCTGACCCGATCAACCTGTACGCC8414ValIleAspGlyAspPheIleProAlaAspProIleAsnLeuTyrAla290295300305AACGCCGCCGACATCGACTATATAGCAGGCACCAACAACATGGACGGC8462AsnAlaAlaAspIleAspTyrIleAlaGlyThrAsnAsnMetAspGly310315320CACATCTTCGCCAGCATCGACATGCCTGCCATCAACAAGGGCAACAAG8510HisIlePheAlaSerIleAspMetProAlaIleAsnLysGlyAsnLys325330335AAAGTCACGGAGTAAGCAGGGGGCACAGGACTCAGGGGCGACCCGTGCGGG8561LysValThrGlu340AGGGCCGCCGGGAAAGCACTGGCGAGGGGGCCAGCCTGGAGGAGGAAGGCATTGAGTGGA8621GGACTGGGAGTGAGGAAGTTAGCACCGGTCGGGGTGAGTATGCACACACCTTCCTGTTGG8681CACAGGCTGAGTGTCAGTGCCTACTTGATTCCCCCAGGGAGGACTTCTACAAG8734GluAspPheTyrLys345CTGGTCAGTGAGTTCACAATCACCAAGGGGCTCAGAGGCGCCAAGACG8782LeuValSerGluPheThrIleThrLysGlyLeuArgGlyAlaLysThr350355360ACCTTTGATGTCTACACCGAGTCCTGGGCCCAGGACCCATCCCAGGAG8830ThrPheAspValTyrThrGluSerTrpAlaGlnAspProSerGlnGlu365370375AATAAGAAGAAGACTGTGGTGGACTTTGAGACCGATGTCCTCTTCCTG8878AsnLysLysLysThrValValAspPheGluThrAspValLeuPheLeu380385390GTGCCCACCGAGATTGCCCTAGCCCAGCACAGAGCCAATGCCAA8922ValProThrGluIleAlaLeuAlaGlnHisArgAlaAsnAlaLys395400405GTGAGGATCTGGGCAGCGGGTGGCTCCTGGGGGCCTTCCTGGGGTGCTGCACCTTCCAGC8982CGAGGCCTCGCTGTGGGTGGCTCTCAGGTGTCTGGGTTGTCTGGGAAAGTGGTGCTTGAG9042TCCCCACCTGTGCCTGCCTGATCCACTTTGCTGAGGCCTGGCAAGACTTGAGGGCCTCTT9102TTTACCTCCCAGCCTACAGGGCTTTACAAACCCTATGATCCTCTGCCCTGCTCAGCCCTG9162CACCCCATGGTCCTTCCCACTGGAGAGTTCTTGAGCTACCTTCCATCCCCCATGCTGTGT9222GCACTGAGAGAACACTGGACAATAGTTTCTATCCACTGACTCTTATGGGCCTCAACTTTG9282CCCATAATTTCAGCCCACCACCACATTAAAAATCTTCATGTAATAATAGCCAATTATAAT9342AAAAAATAAGGCCAGACACAGTAGCTCATGCCTGTAATCCCAGCACATTGGGAGGTCAAG9402GTGGGAGGATCACTTGAGGTCAGGAGTCTGAGACTAGTCTGGCCAACATGGCAAAACCCC9462ATCTCTACTAAAAATACAAAAATTATCCAGGCATGGTGGTGCATGCCTATAATCCTAGCT9522ACTCAGGAGGCTGAGGTAGCAGAATTGATTGACCCAGGGAGGTGGAGGTTGCAGTGAGCC9582GAGATTACGCCACTGCACTCCAGCAGGGGCAACAGAGTGAGACTGTGTCTCGAATAAATA9642AGTAAATAAATAATAAAAATAAAAAATAAGTTAGGAATACGAAAAAGATAGGAAGATAAA9702AGTATACCTAGAAGTCTAGGATGAAAGCTTTGCAGCAACTAAGCAGTACATTTAGCTGTG9762AGCCTCCTTTCAGTCAAGGCAAAAAGGGAAACAGTTGAGGGCCTATACCTTGTCCAATCT9822AATTGAAGAATGCACATTCACTTGGAGAGCAAAATATTTCTTGATACTGAATTCTAGAAG9882GAAGGTGCCTCACAATGTTTTGTGGAGGTGAAGTATAAATTCAGCTGAAATTGTGGAACC9942CATGAATCCATGAATTTGGTTCTCAGCTTTCCCTTCCCTGGGTGTAAGAAGCCCCATCTC10002TTCATGTGAATTCCCCAGACACTTCCCTGCCCACTGCCCGGGACCTCCCTCCAAGTCCGG10062TCTCTGGGCTGATCGGTCCCCAGTGAGCACCCTGCCTACTTGGGTGGTCTCTCCCCTCCA10122GGAGTGCCAAGACCTACGCCTACCTGTTTTCCCATCCCTCTCGGATG10169SerAlaLysThrTyrAlaTyrLeuPheSerHisProSerArgMet410415420CCCGTCTACCCCAAATGGGTGGGGGCCGACCATGCAGATGACATTCAG10217ProValTyrProLysTrpValGlyAlaAspHisAlaAspAspIleGln425430435440TACGTTTTCGGGAAGCCCTTCGCCACCCCCACGGGCTACCGGCCCCAA10265TyrValPheGlyLysProPheAlaThrProThrGlyTyrArgProGln445450455GACAGGACAGTCTCTAAGGCCATGATCGCCTACTGGACCAACTTTGCC10313AspArgThrValSerLysAlaMetIleAlaTyrTrpThrAsnPheAla460465470AAAACAGGGTAAGACGTGGGTTGAGTGCAGGGCGGAGGGCCACAGCCG10361LysThrGly475AGAAGGGCCTCCCACCACGAGGCCTTGTTCCCTCATTTGCCAGTGGAGGGACTTTGGGCA10421AGTCACTTAACCTCCCCCTGCATCGGAATCCATGTGTGTTTGAGGATGAGAGTTACTGGC10481AGAGCCCCAAGCCCATGCACGTGCACAGCCAGTGCCCAGTATGCAGTGAGGGGCATGGTG10541CCCAGGGCCAGCTCAGAGGGCGGGGATGGCTCAGGCGTGCAGGTGGAGAGCAGGGCTTCA10601GCCCCCTGGGAGTCCCCAGCCCCTGCACAGCCTCTTCTCACTCTGCAGGGACCCC10656AspProAACATGGGCGACTCGGCTGTGCCCACACACTGGGAACCCTACACTACG10704AsnMetGlyAspSerAlaValProThrHisTrpGluProTyrThrThr480485490GAAAACAGCGGCTACCTGGAGATCACCAAGAAGATGGGCAGCAGCTCC10752GluAsnSerGlyTyrLeuGluIleThrLysLysMetGlySerSerSer495500505ATGAAGCGGAGCCTGAGAACCAACTTCCTGCGCTACTGGACCCTCACC10800MetLysArgSerLeuArgThrAsnPheLeuArgTyrTrpThrLeuThr510515520525TATCTGGCGCTGCCCACAGTGACCGACCAGGAGGCCACCCCTGTGCCC10848TyrLeuAlaLeuProThrValThrAspGlnGluAlaThrProValPro530535540CCCACAGGGGACTCCGAGGCCACTCCCGTGCCCCCCACGGGTGACTCC10896ProThrGlyAspSerGluAlaThrProValProProThrGlyAspSer545550555GAGACCGCCCCCGTGCCGCCCACGGGTGACTCCGGGGCCCCCCCCGTG10944GluThrAlaProValProProThrGlyAspSerGlyAlaProProVal560565570CCGCCCACGGGTGACTCCGGGGCCCCCCCCGTGCCGCCCACGGGTGAC10992ProProThrGlyAspSerGlyAlaProProValProProThrGlyAsp575580585TCCGGGGCCCCCCCCGTGCCGCCCACGGGTGACTCCGGGGCCCCCCCC11040SerGlyAlaProProValProProThrGlyAspSerGlyAlaProPro590595600605GTGCCGCCCACGGGTGACTCCGGGGCCCCCCCCGTGCCGCCCACGGGT11088ValProProThrGlyAspSerGlyAlaProProValProProThrGly610615620GACTCCGGGGCCCCCCCCGTGCCGCCCACGGGTGACTCCGGCGCCCCC11136AspSerGlyAlaProProValProProThrGlyAspSerGlyAlaPro625630635CCCGTGCCGCCCACGGGTGACGCCGGGCCCCCCCCCGTGCCGCCCACG11184ProValProProThrGlyAspAlaGlyProProProValProProThr640645650GGTGACTCCGGCGCCCCCCCCGTGCCGCCCACGGGTGACTCCGGGGCC11232GlyAspSerGlyAlaProProValProProThrGlyAspSerGlyAla655660665CCCCCCGTGACCCCCACGGGTGACTCCGAGACCGCCCCCGTGCCGCCC11280ProProValThrProThrGlyAspSerGluThrAlaProValProPro670675680685ACGGGTGACTCCGGGGCCCCCCCTGTGCCCCCCACGGGTGACTCTGAG11328ThrGlyAspSerGlyAlaProProValProProThrGlyAspSerGlu690695700GCTGCCCCTGTGCCCCCCACAGATGACTCCAAGGAAGCTCAGATGCCT11376AlaAlaProValProProThrAspAspSerLysGluAlaGlnMetPro705710715GCAGTCATTAGGTTTTAGCGTCCCATGAGCCTTGGTATCAAGAGGCCACAAGAGT11431AlaValIleArgPhe720GGGACCCCAGGGGCTCCCCTCCCATCTTGAGCTCTTCCTGAATAAAGCCTCATACCCCTG11491TCGGTGTCTTTCTTTGCTCCCAAGGCTAAGCTGCAGGATC11531(2) INFORMATION FOR SEQ ID NO:2:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 26 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(iv) ANTI-SENSE: YES(xi) SEQUENCE DESCRIPTION: SEQ ID NO:2:AGGTGAGGCCCAACACAACCAGTTGC26(2) INFORMATION FOR SEQ ID NO:3:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 10 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:3:GATCGTCGAC10(2) INFORMATION FOR SEQ ID NO:4:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 11 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:4:CGTCGACGTAC11(2) INFORMATION FOR SEQ ID NO:5:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 11 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:5:GTCGACGGTAC11(2) INFORMATION FOR SEQ ID NO:6:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 17 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:6:AGACCTACGCCTACCTG17(2) INFORMATION FOR SEQ ID NO:7:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 17 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:7:TCCAGTAGGCGATCATG17(2) INFORMATION FOR SEQ ID NO:8:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 20 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:8:GACCGATGTCCTCTTCCTGG20(2) INFORMATION FOR SEQ ID NO:9:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 20 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:9:CAGCCGAGTCGCCCATGTTG20(2) INFORMATION FOR SEQ ID NO:10:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 21 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:10:ACCAAGAAGATGGGCAGCAGC21(2) INFORMATION FOR SEQ ID NO:11:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 21 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:11:GACTGCAGGCATCTGAGCTTC21(2) INFORMATION FOR SEQ ID NO:12:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 15 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:12:GCCGCGAAGGTAAGA15(2) INFORMATION FOR SEQ ID NO:13:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 24 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:13:GTGTCTCCCTCGCAGCTGGGCGCC24(2) INFORMATION FOR SEQ ID NO:14:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 13 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:14:TGGCAAGGTGGGA13(2) INFORMATION FOR SEQ ID NO:15:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 23 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:15:TCCTGCCACCTGCAGGGACCCTG23(2) INFORMATION FOR SEQ ID NO:16:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 13 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:16:AAGCAAGGTCTGC13(2) INFORMATION FOR SEQ ID NO:17:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 23 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:17:GCTCCCCCATCTCAGTCTCCCGG23(2) INFORMATION FOR SEQ ID NO:18:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 13 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:18:CTGCCAGGTGCGT13(2) INFORMATION FOR SEQ ID NO:19:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 23 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:19:CTGCCCTGCCCCCAGGTAACTAT23(2) INFORMATION FOR SEQ ID NO:20:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 15 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:20:TCTCTGCAGGTCTCG15(2) INFORMATION FOR SEQ ID NO:21:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 24 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:21:TTCTGGGTCCCGTAGACCCTCTCC24(2) INFORMATION FOR SEQ ID NO:22:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 15 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:22:GCCAAAAAGGTAAAC15(2) INFORMATION FOR SEQ ID NO:23:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 24 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:23:TGGTTCTGCCCCCAGGTGGCTGAG24(2) INFORMATION FOR SEQ ID NO:24:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 13 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:24:CTGGAGTGTGAGT13(2) INFORMATION FOR SEQ ID NO:25:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 23 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:25:GGCTCTCCCACCCAGACCCCATG23(2) INFORMATION FOR SEQ ID NO:26:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 14 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:26:GTCACGGAGTAAGC14(2) INFORMATION FOR SEQ ID NO:27:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 22 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:27:ACTTGATTCCCCCAGGGAGGAC22(2) INFORMATION FOR SEQ ID NO:28:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 14 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:28:AATGCCAAGTGAGG14(2) INFORMATION FOR SEQ ID NO:29:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 22 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:29:GTCTCTCCCCTCCAGGAGTGCC22(2) INFORMATION FOR SEQ ID NO:30:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 14 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:30:AAAACAGGGTAAGA14(2) INFORMATION FOR SEQ ID NO:31:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 22 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:31:CTTCTCACTCTGCAGGGACCCC22(2) INFORMATION FOR SEQ ID NO:32:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 1640 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:32:GGATCCCTCGAACCCAGGAGTTCAAGACTGCAGTGAGCTATGATTGTGCCACTGCACTCT60AGCCTGGGTGACAGAGACCCTGTCTCAAAAAAACAAACAAACAAAAAACCTCTGTGGACT120CCGGGTGATAATGACATGTCAATGTGGATTCATCAGGTGTTAACAGCTGTACCCCCTGGT180GGGGGATGTTGATAACGGGGGAGACTGGAGTGGGGCGAGGACATACGGGAAATCTCTGTA240ATCTTCCTCTAATTTTGCTGTGAACCTAAAGCTGCTCTAAAAATGTACATAGATATAAAC300TGGGGCCTTCCTTTCCCTCTGCCCTGCCCCAGCCCTCCCCCACCTCCTTCCTCTCCCTGC360TGCCTCCCCTCTGCCCTCCCCTTTCCTCCTTAGCCACTGTAAATGACACTGCAGCAAAGG420TCTGAGGCAAATGCCTTTGCCCTGGGGCGCCCCAGCCACCTGCAGGCCCCTTATTTCCTG480TGGCCGAGCTCCTCCTCCCACCCTCCAGTCCTTTCCCCAGCCTCCCTCGCCCACTAGGCC540TCCTGAATTGCTGGCACCGGCTGTGGTCGACAGACAGAGGGACAGACGTGGCTCTGCAGG600TCCACTCGGTCCCTGGCACCGGCCGCAGGGGTGGCAGAACGGGAGTGTGGTTGGTGTGGG660AAGCACAGGCCCCAGTGTCTCCTGGGGGACTGTTGGGTGGGAAGGCTCTGGCTGCCCTCA720CCCTGTTCCCATCACTGCAGAGGGCTGTGCGGTGGCTGGAGCTGCCACTGAGTGTCTCGG780TGAGGGTGACCTCACACTGGCTGAGCTTAAAGGCCCCATCTGAAGACTTTGTTCGTGGTG840TTCTTTCACTTCTCAGAGCCTTTCCTGGCTCCAGGATTAATACCTGTTCACAGAAAATAC900GAGTCGCCTCCTCCTCCACAACCTCACACGACCTTCTCCCTTCCCTCCCGCTGGCCTCTT960TCCCTCCCCTTCTGTCACTCTGCCTGGGCATGCCCCAGGGCCTCGGCTGGGCCCTTTGTT1020TCCACAGGGAAACCTACATGGTTGGGCTAGATGCCTCCGCACCCCCCCACCCACACCCCC1080TGAGCCTCTAGTCCTCCCTCCCAGGACACATCAGGCTGGATGGTGACACTTCCACACCCT1140TGAGTGGGACTGCCTTGTGCTGCTCTGGGATTCGCACCCAGCTTGGACTACCCGCTCCAC1200GGGCCCCAGGAAAAGCTCGTACAGATAAGGTCAGCCACATGAGTGGAGGGCCTGCAGCAT1260GCTGCCCTTTCTGTCCCAGAAGTCACGTGCTCGGTCCCCTCTGAAGCCCCTTTGGGGACC1320TAGGGGACAAGCAGGGCATGGAGACATGGAGACAAAGTATGCCCTTTTCTCTGACAGTGA1380CACCAAGCCCTGTGAACAAACCAGAAGGCAGGGCACTGTGCACCCTGCCCGGCCCCACCA1440TCCCCCTTACCACCCGCCACCTTGCCACCTGCCTCTGCTCCCAGGTAAGTGGTAACCTGC1500ACAGGTGCACTGTGGGTTTGGGGAAAACTGGATCTCCCTGCACCTGAGGGGGTAGAGGGG1560AGGGAGTGCCTGAGAGCTCATGAACAAGCATGTGACCTTGGATCCAGCTCCATAAATACC1620CGAGGCCCAGGGGGAGGGCC1640(2) INFORMATION FOR SEQ ID NO:33:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 12 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:33:GGTACATGTTCT12(2) INFORMATION FOR SEQ ID NO:34:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 12 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:34:AGGTCATGACCT12(2) INFORMATION FOR SEQ ID NO:35:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 11 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:35:AAGAAGGAAGT11(2) INFORMATION FOR SEQ ID NO:36:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 9 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:36:ATTCTTGGA9(2) INFORMATION FOR SEQ ID NO:37:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 11 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:37:AGTTCTTGGCA11(2) INFORMATION FOR SEQ ID NO:38:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 20 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:38:GTCACCTGTGCTTTTCCCTG20(2) INFORMATION FOR SEQ ID NO:39:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 32 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:39:TGACCTTGGATCCAGCTCCATAAATACCCGAG32(2) INFORMATION FOR SEQ ID NO:40:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 32 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:40:TGACCTTGGTTCCAGCTCCATAAATACTGGAG32(2) INFORMATION FOR SEQ ID NO:41:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 19 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:41:CACAGGTGCACTGTGGGTT19(2) INFORMATION FOR SEQ ID NO:42:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 19 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:42:CACAGGTGCACTCCGGGTT19(2) INFORMATION FOR SEQ ID NO:43:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 7 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:43:CCTTGCC7(2) INFORMATION FOR SEQ ID NO:44:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 20 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:44:ACCTGCCTCTGCTCCCAGGT20(2) INFORMATION FOR SEQ ID NO:45:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 28 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:45:CCATGCCGACCGGCCTCTGCTCCCAGGT28(2) INFORMATION FOR SEQ ID NO:46:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 33 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:46:GCACTGTGCACCCTGCCCGGCCCCACCATCCCC33(2) INFORMATION FOR SEQ ID NO:47:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 5 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:47:GCACT5(2) INFORMATION FOR SEQ ID NO:48:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 25 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:48:CAGCCAGCCCTCCCCCACCCTTCCC25(2) INFORMATION FOR SEQ ID NO:49:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 10 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:49:TGACAGTGAC10(2) INFORMATION FOR SEQ ID NO:50:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 10 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:50:TGACACTAAC10(2) INFORMATION FOR SEQ ID NO:51:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 15 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:51:TCTGTCCCAGAAGTC15(2) INFORMATION FOR SEQ ID NO:52:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 15 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:52:TCTGGCTCAGGAGTC15(2) INFORMATION FOR SEQ ID NO:53:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 15 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:53:TCAGCCACATGAGTG15(2) INFORMATION FOR SEQ ID NO:54:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 15 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:54:TCAGCCACACCAGTG15(2) INFORMATION FOR SEQ ID NO:55:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 11 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:55:CTGCCTTGTGC11(2) INFORMATION FOR SEQ ID NO:56:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 11 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:56:CTGCCTCCTGC11(2) INFORMATION FOR SEQ ID NO:57:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 25 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:57:CTGTGTGGCAAGAAGGAAGTGTTGT25(2) INFORMATION FOR SEQ ID NO:58:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 22 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(xi) SEQUENCE DESCRIPTION: SEQ ID NO:58:CAACTCCTGACCTCAAGTGATC22__________________________________________________________________________ | The present invention relates to a DNA molecule containing intron sequences and encoding a human protein which is, depending on the site of action, called Bile Salt-Stimulated Lipase (BSSL) or Carboxyl Ester Lipase (CEL). The DNA molecule is advantageously used in the production of recombinant human BSSL/CEL, preferably by means of production in transgenic non-human mammals. The recombinant human BSSL/CEL can be used as a constituent of infant formulas used for feeding infants as a substitute for human milk, or in the manufacture of medicaments against e.g. fat malabsorption, cystic fibrosis and chronic pancreatitis. | 0 |
FIELD OF THE INVENTION
[0001] The present invention relates generally to the field of optical communications and in particular to methods and apparatus for demodulating and receiving optical signals having Differential-Quadrature-Phase-Shift-Keying (DQPSK) format(s).
BACKGROUND OF THE INVENTION
[0002] Optical DQPSK is a promising modulation format that is attracting considerable commercial attention as a result of its high receiver sensitivity, high spectral efficiency (SE), high filtering and dispersion tolerance(s). Of particular interest, DQPSK may be used in combination with amplitude modulation to achieve even higher spectral efficiencies.
[0003] In optical DQPSK transmission, data is conveyed by an optical phase difference between adjacent bits. In order to detect the data contained within a DQPSK transmission, an optical demodulator is used to convert the phase-coded signal into intensity-coded signals. Typically, such optical demodulators are constructed from a pair of optical delay interferometers (ODIs).
[0004] Unfortunately, contemporary optical demodulators so constructed are quite complex, requiring precise control of the absolute phase difference between the two arms of each of the two ODIs, and precise length matching among the multiple optical paths prior to any data recovery circuits. In addition, conventional ODIs are fiber-based or planar-waveguide-based, which are temperature sensitive and therefore require precise temperature control and stabilization, particularly when employed in high performance optical transmission systems.
SUMMARY OF THE INVENTION
[0005] I have developed an optical demodulator that, together with accompanying method(s), demodulates a DQPSK signal without exhibiting the infirmities that plague the prior art. More particularly, this inventive optical demodulator and method employs a single optical delay interferometer comprising a free-space Michelson interferometer having two optical paths, connected to a 1×2 coupler. Positioned within an arm of the Michelson interferometer is a phase shifter that produces a phase difference of π/2 between the two paths.
[0006] This innovative demodulator construction—from a single free-space Michelson interferometer—results in a demodulator that is compact, reliable, and may be constructed to be substantially immune from undesirable thermal sensitivities.
BRIEF DESCRIPTION OF THE DRAWING
[0007] A more complete understanding of the present invention may be realized by reference to the accompanying drawing in which:
[0008] FIG. 1 is a schematic of a generalized, PRIOR ART DQPSK receiver having two optical delay interferometers for demodulation;
[0009] FIG. 2 is a schematic of a DQPSK demodulator according to the present invention; and
[0010] FIG. 3 is a flowchart depicting the inventive method according to the present invention.
DETAILED DESCRIPTION
[0011] With initial reference to FIG. 1 , there is shown a generalized, PRIOR ART optical DQPSK demodulator 100 . With such a PRIOR ART optical demodulator, an optical DQPSK signal 110 having 2 bit/symbol say, is amplified through the effect of an optical amplifier 120 , the output of which is subsequently filtered by an optical filter 130 and then split by 1×2 optical coupler/splitter 140 .
[0012] Since a DQPSK signal comprises two tributaries, the 1×2 split of the optical coupler 140 is necessary to provide signal(s) to the two optical delay interferometers (ODIs) 150 , 152 each including a delay loop 155 , 156 and a phase shifter 157 , 158 , respectively. (Note that the phase shift in this exemplary discussion is shown as +π/4 and −π/4). As noted before, these two phase shifts have to be precisely controlled and maintained. More specifically, for 40-Gb/s DQPSK systems, the free spectral range (FSR) of the ODI is approximately 20 GHz. The tolerance to the frequency mismatch resulting from non-perfect phase shifts is less or about ±0.5 GHz. Additionally, the fiber-based or planar-waveguide based ODIs usually exhibit a temperature sensitivity of about 1 GHz/° C., so the temperature of the ODIs has to be controlled and maintained within less or about 0.5 ° C., which is quite demanding.
[0013] Continuing with our discussion of the PRIOR ART apparatus shown in FIG. 1 , optical signals output from the ODIs 150 , 152 are received by balanced detectors 160 , 162 , the output of which is provided to clock and data recovery circuitry 170 , 172 . As can be readily appreciated at this point, each of the “branches” of the PRIOR ART demodulator 100 permits the extraction of the two tributaries comprising the DQPSK signal by the clock data recovery circuitry 170 , 172 , respectively. As also noted before however, the four optical paths starting from the optical coupler 140 and ending at the four detectors situated in the two balanced detectors 160 and 162 have to have essentially the same length. In addition, the electrical path length between the balanced detector 160 and the clock and data recovery circuitry 170 has to be essentially equal to that between the other balanced detector 162 and its respective clock and data recovery circuitry 172 . More specifically, for 40-Gb/s DQPSK systems, the bit period is 50 ps. Consequently, the tolerance to delay mismatch resulting from unequal path lengths is only about 10% of the bit period or 5 ps, which translates into only about 1 mm in length in optical fiber!
[0014] As noted before and as can be readily appreciated, such a PRIOR ART implementation is quite susceptible to variations in temperature, and any temperature variations that may exist between the two ODIs 150 and 152 . As a result, in order to provide such temperature control and stabilization, additional performance monitoring and feedback control components are required which unfortunately, adds to the complexity and cost of such PRIOR ART implementations.
[0015] Turning now to FIG. 2 , there is shown a schematic of a DQPSK demodulator 200 constructed according to the inventive teachings of the instant application. As can be readily observed from that FIG. 2 , this inventive demodulator 200 uses a single ODI—based on a free-space Michelson interferometer comprising a beam splitter 220 and two reflectors (mirrors) 230 and 240 —the reflectors being positioned substantially perpendicular to the plane formed by the signal optical paths. This arrangement results in two distinct optical paths, each having a characteristic path length of L and L+ΔL, respectively. The path length difference ΔL is such that the resulting delay is about a bit period of the signal. For 40-Gb/s DQPSK, ΔL is about 15 mm in free-space. If we use a FSR of 25 GHz so that the ODI can be used for multiple wavelength channels that are on the ITU 50-GHz channel grid, ΔL is about 12 mm in free-space.
[0016] The first optical path having a characteristic path length of L includes those paths between optical splitter 220 and reflector 240 . The second optical path having a characteristic path length of L+ΔL includes those paths between the optical splitter 220 and reflector 230 . In addition, and as shown in this FIG. 2 , one of the optical paths (in this example, the second optical path) may include a π/2 phase shifter 280 , and/or a thermal/athermal waveplate 270 , which may advantageously be coupled or otherwise combined with the phase shifter 280 .
[0017] A single DQPSK signal having 2 bits/symbol is split into two optical signals ( 215 , 217 ) through the effect of a 1×2 optical coupler 210 (e.g., a 3 dB coupler). The optical coupler 210 splits the single DQPSK signal light into two separate signals, 215 , 217 , each exhibiting substantially equal power(s). These two split signals 215 , 217 are directed into the interferometer where portions traverse the two optical paths.
[0018] More specifically, the split optical signal 215 strikes the beam splitter 220 (Point A) where it is further split. A first portion of that further split signal 215 is directed to reflector 240 (Point E) where it is reflected back to beam splitter 220 (Point C). This path, defined by the round trip between the beam splitter 220 and reflector 240 , exhibits a path length of L.
[0019] It should be noted that reflectors (mirrors) 240 , and 230 , preferably have a reflectivity of essentially 100%.
[0020] A second portion of that further split signal 215 is directed to another reflector 230 (Point G) from which it is reflected back along an optical path to beam splitter 220 (Point C). This second optical path, defined by the round trip between the beam splitter 220 and reflector 230 , exhibits a path length of L+ΔL. Upon striking Point C, the two split signals interfere with each other both constructively- and destructively. Without losing generality, the constructive interference component emits from Point C and is directed to a first detector 250 , while the destructive interference component emits from Point C and is directed to a second detector 260 . The difference between the signals received by the detectors 250 and 260 , which can be obtained through a differential amplifier situated inside a differential amplification unit 290 , is then used to recover the first-tributary of the original DQPSK signal.
[0021] Similarly, the split optical signal 217 strikes the beam splitter 220 (Point B) where it is further split. A first portion of that further split signal 217 is directed to reflector 240 (Point F) where it is reflected back to beam splitter 220 (Point D). This path exhibits a path length of L.
[0022] A second portion of that further split signal 217 is directed to another mirror 230 (Point H) from which it is reflected back along an optical path to beam splitter 220 (Point D). This second optical path exhibits a path length of L+ΔL. Upon striking Point D, the two split signals interfere with each other both constructively and destructively. Without losing generality, the constructive interference component emits from Point D and is directed to a third detector 255 , and the destructive interference component emits from Point D and is directed to a fourth detector 265 . The difference between the signals received by the detectors 255 and 265 , which can be obtained through another differential amplifier inside the differential amplification unit 290 , is then used to recover the second-tributary of the original DQPSK signal.
[0023] Shown further in that FIG. 2 , is a π/2 phase shifter 280 interposed in the optical path traversed by optical signal 217 , and having a path length of L+ΔL. This π/2 phase shifter 280 introduces an optical phase delay of π/2 between path A-G-C and path B-H-D. Those skilled in the art will quickly recognize that such a phase shifter may be implemented through the application of a suitable thin-film coating, applied to a suitable transparent substrate 270 or the mirror 230 . The phase shifter can also be interposed in the optical path traversed by optical signal 215 , and having a path length of L. Note that not shown in FIG. 2 are precise phase controls that ensure that a +π/4 (or −π/4) phase shift between the path A-E-C and A-G-C, and a −π/4 (or +π/4) phase shift between the path B-F-D and B-H-D at the signal center frequency.
[0024] From this FIG. 2 , it should be readily apparent to those skilled in the art that the inventive DQPSK demodulator allows the beam splitter, reflectors/mirror(s), and an entire optical package so constructed to be shared by two tributaries. In addition, the use of the π/2 phase shifter ensures that the two tributaries are also aligned correctly with respect to each other, essentially independent of changes in laser frequency and ambient temperature. Accordingly, this inventive design permits the construction of a compact, yet highly reliable demodulator.
[0025] In those instances where source laser frequency is locked with sufficient precision, this inventive demodulator may be made athermal and passive, thereby permitting the DQPSK tributaries to be received without any monitoring and feedback control. The athermal operation of the ODI can be achieved by fixing the free-space path length using an athermal material, so no temperature stabilization is required.
[0026] Alternatively, if an adjustable demodulator is desired—for tracking the laser frequency drift, say—a temperature sensitive waveplate 270 may be interposed along an optical path. Shown in the FIG. 2 is a thermal/athermal waveplate 270 , positioned in the optical path taken by optical signal 217 , and having a path length of L+ΔL. For design and or construction convenience, the waveplate 270 may be combined with phase shifter 280 .
[0027] Of further advantage—because the size of beam splitter 220 may be much larger than the beam size of the optical signals 215 , 217 , the four detectors may be optically coupled directly to the beam splitter 220 with, for example, fiber-coupled lenses 253 , 257 , 263 , 267 . The fiber connections can be made having matched length(s) so that not any additional fiber or other coupling mechanism(s) are needed. As a result, demodulators constructed according to the inventive teachings of the present application exhibit low loss and permit a more compact design while, at the same time enhancing the manufacturability and reliability.
[0028] Finally with reference to FIG. 2 ., the detector outputs are appropriately subtracted to obtain the differences between the detected constructive interference signals and the detected destructive interference signals. This is performed by the differential amplification unit 290 . The results, after clock and data recovery, recover the two tributaries of the original DQPSK signal.
[0029] Turning now to FIG. 3 , there is shown a flowchart which depicts an overview of the inventive method. As indicated by Block 310 of that FIG. 3 , a DQPSK signal is split into two signals exhibiting substantially equal power. These two signals are then introduced into a Michelson interferometer where they strike a beam splitter and are further split into two, sub-signals each (Block 320 ).
[0030] The sub-signals that are split from the same equal power signal(s) traverse two different paths within the Michelson interferometer, wherein each of the paths have a different length (Block 330 ).
[0031] The light emission due to the constructive interference of the two sub-signals is directed to a first detector, while the light emission due to the destructive interference of the two sub-signals is sent to a second detector. (Block 340 ). One tributary of the original DQPSK signal is determined from the difference between these two detected signals (Block 350 ).
[0032] At this point, while we have discussed and described our invention using some specific examples, those skilled in the art will recognize that our teachings are not so limited. Accordingly, our invention should be only limited by the scope of the claims attached hereto. | An optical demodulator and accompanying method(s) that demodulates a DQPSK signal employing a single optical delay interferometer comprising a free-space Michelson interferometer having two optical paths, connected to a 1×2 coupler. Positioned within an arm of the Michelson interferometer is a phase shifter that produces a phase difference of π/2 between the two paths. The resulting demodulator is compact, reliable, and may be constructed to be substantially immune from undesirable thermal sensitivities. | 7 |
PRIORITY CLAIM
This patent application is a U.S. National Phase of International Patent Application No. PCT/NL2007/050678, filed Dec. 20, 2007, which claims priority to Netherlands Patent Application No. 2000405, filed Dec. 22, 2006, the disclosures of which are incorporated herein by reference in their entirety.
FIELD
The present disclosure relates to a wood product and a method for preserving wood. The present disclosure also relates to an apparatus for performing the method of preserving wood.
BACKGROUND
Upgrading of wood by hydrothermolysis is known in the art. In a hydrothermolysis, wood is treated with saturated steam at a temperature between 130-220° C., wherein a hemicellulose and lignin become reactive. In a subsequent step the wood is cooled and cured by drying, wherein the reactive hemicellulose and lignin form cross-links. The final product is wood which has acquired a greater durability and fungal resistance than the untreated wood. Since all that is required for the reaction is water in the form of steam, hydrothermolysis is particularly advantageous compared to preserving methods in which the wood is upgraded with impregnating agents usually having an environmental impact.
Drawbacks of known hydrothermolysis methods are that the methods are particularly time-consuming. The wood is treated in multiple individual steps with interim cooling and heating of the wood. Time is lost here and the wood is placed under great internal stresses as a result of contraction and expansion, which result in splitting and deformation. This results in high costs due to longer production times on the one hand and to a decrease in the economic value of the wood on the other.
More rapid methods of thermal preservation are known wherein dried wood is heated to very high temperatures above 220 degrees Celsius. The drawback of these rapid methods is, however, that the mechanical strength of the product decreases greatly when compared to the starting products. Rapid thermal treatment methods with less high temperatures result in products with a reduced durability when compared to the products at higher temperatures. The known, relatively rapid methods also produce a high percentage of products of low-grade quality due to splitting and deformation, leading to a relatively high loss of material and a high amount of wasted wood
SUMMARY
The present disclosure describes several exemplary embodiments of the present invention.
One aspect of the present disclosure provides a method for preserving wood, comprising A) placing wood for treating in a treatment space; B) removing air, in particular, oxygen, from the treatment space; C) feeding steam into the treatment space, wherein the temperature of the wood is simultaneously increased, wherein the temperature is raised from 70 degrees Celsius with a temperature gradient of a maximum of 60 degrees Celsius per hour, to a temperature of at least 150 degrees Celsius; wherein the wood is heated at a temperature above 150 degrees Celsius during a reaction time of at least 10 minutes; D) polymerizing wood constituents thermally activated in step C by removing moisture from the wood up to a moisture content lower than 5% at a temperature of at least 130 degrees Celsius; and, E) cooling the wood, wherein the moisture content of the wood is simultaneously increased to at least 7% by weight, in the temperature path below 140 degrees.
Another aspect of the present disclosure provides a preserved wood product produced by the method comprising A) placing wood for treating in a treatment space; B) removing air, in particular, oxygen, from the treatment space; C) feeding steam to the treatment space, wherein the temperature of the wood is simultaneously increased, wherein the temperature is raised from 70 degrees Celsius with a temperature gradient of a maximum of 60 degrees Celsius per hour, to a temperature of at least 150 degrees Celsius, wherein the wood is heated at a temperature above 150 degrees Celsius during a reaction time of at least 10 minutes; D) polymerizing wood constituents thermally activated in step C by removing moisture from the wood up to a moisture content lower than 5% at a temperature of at least 130 degrees Celsius; and E) cooling the wood, wherein the moisture content of the wood is simultaneously increased to at least 7% by weight, in the temperature path below 140 degrees.
A further aspect of the present disclosure provides a an apparatus for preserving wood, comprising A) a treatment space sealable in medium-tight manner; B) a vacuum pump connected to the treatment space; C) a steam source connected to the treatment space; D) a heating device which is in thermal contact with the treatment space; E) a dispenser for adding predetermined amounts of either a base or an acid to the treatment space; F) pH measuring device for determining the pH value of steam in the treatment space; and G) measuring and control equipment adapted to monitor at least the pH temperature and pressure inside the treatment space and to control the vacuum pump, the steam source and the heat source, and the pH by dispensing either a base or an acid.
One feature of the present disclosure provides a rapid preservation of wood with relatively little loss in mechanical strength.
The present disclosure provides a method for preserving wood, comprising the processing steps of: A) placing wood for treating in a treatment space, B) removing air, in particular, oxygen, from the treatment space, C) feeding steam to the treatment space, wherein the temperature of the wood is simultaneously increased, wherein from a temperature of 70 degrees Celsius the temperature is raised with a temperature gradient of a maximum of 60 degrees, preferably between 30-50 degrees Celsius per hour, to a temperature of at least 150 degrees Celsius; wherein the wood is heated at a temperature above 150 degrees Celsius during a reaction time of at least 10 minutes; D) polymerizing wood constituents thermally activated in step C) by removing moisture from the wood up to a moisture content of between 3 and 5% at a temperature of at least 130 degrees Celsius, and E) cooling the wood, wherein the moisture content of the wood is simultaneously increased to at least 7% by weight, preferably between 7-8%, in the temperature path below 140 degrees.
The starting temperature of the wood in step A is normally the ambient temperature, usually between 15 and 25 degrees Celsius. In the starting situation, the wood generally has a moisture content of between 10-18% by weight.
The removal of air, in particular, oxygen, from the treatment space in step B can, for instance, take place by displacement of air by an inert gas such as nitrogen or argon, or by steam. If air is not removed, oxygen from the air can produce unwanted reactions during the preservation process. The best results are achieved if the oxygen is removed by creating a vacuum in the treatment space.
In step C steam is fed to the treatment space. If a vacuum has been created in the treatment space in step B, the steam can be used to supplement the vacuum. The temperature of the wood is simultaneously increased at a rate of between 20-60 degrees Celsius per hour, preferably approximately 40 degrees Celsius per hour, to a temperature of at least 150 degrees Celsius. Deformations and damage to the wood are prevented by raising the temperature gradually. Up to a temperature of 70 degrees Celsius, the rate of heating can be higher than 40 degrees Celsius per hour. Above 70 degrees, however, heating rates higher than 40 degrees per hour can be detrimental to the wood. Above 150 degrees, activation reactions of wood constituents take place in the wood at a sufficiently high speed, wherein a reaction time of at least 10 minutes is required in order to eventually achieve a good preservation of the wood. The reaction time is preferably at least 30 minutes. Unwanted reactions can take place in the wood at temperatures above 220 degrees Celsius. The temperature is preferably held between 150-220 degrees Celsius during the reaction time. At higher temperatures, reactions generally proceed more rapidly so that the reaction time can be shortened. A minimum reaction time of 10 minutes does, however, ensure a good result.
The wood activated by the heating with steam in step C is then polymerized in step D by removing moisture from the wood up to a moisture content lower than 5% by weight, preferably between 3 and 5% by weight, at a temperature of at least 130 degrees Celsius. This is possible, for instance, by gradually decreasing the vapour pressure and/or increasing the wall temperature of the treatment space in order to achieve a combination of vapour pressure and temperature whereby wood with a moisture content of 3 to 5% by weight is in hygroscopic equilibrium.
In step E the polymerization reaction of step D is stopped by reducing the temperature to below 140 degrees Celsius, preferably to below 100 degrees Celsius, and then further to room temperature. The moisture content of the wood is simultaneously increased to at least 7% by weight, preferably 7 to 8% by weight. Deformations during the continuous cooling are hereby prevented. During the cooling, the vapour pressure of water in the treatment space is adjusted to the value at which wood with a moisture content of 7% to 8% is in hygroscopic equilibrium. The wood is then conditioned for final processing and further manufacturing of wooden products.
It has been found that the wood has a good increased resistance to fungal damage following this treatment, while the mechanical strength decreases on average by only 10% to 15%, this being much lower than in the known rapid methods at high temperatures. Waste of wood components due to damage by, for instance, splitting is also exceptionally low.
In one exemplary embodiment of the method, a step F is performed between steps C and D wherein the heated wood is compressed. Compression results in a wood product with a greater density.
It is advantageous if the steam has a maximum degree of saturation of 95% during step C. The degree of saturation is the percentage relative to 100% saturated steam at the same pressure and temperature. This produces a better wood product and, in particular, less splitting than a comparable process in which saturated steam is used. A significant factor here is probably that condensation of water is largely prevented.
At least a part of the oxygen is preferably removed in step B by placing the treatment space under reduced pressure. Placing the treatment space under reduced pressure (creating a vacuum) is found to be a more rapid and effective method of removing oxygen than other methods, such as displacing air by means of nitrogen or steam. Creating a vacuum moreover simplifies control of the process. The degree of pressure decrease can be determined using a simple pressure gauge and is a reliable measure of the quantity of air, and thereby oxygen, removed.
In another exemplary embodiment, the reduced pressure is lower than 13 kPa. This results in a proper removal of oxygen from the treatment space. During the reduced pressure, the wall temperature of the treatment space can optionally be increased to 50-70 degrees Celsius for an even better removal of oxygen. The time required for the process is moreover shortened since a start is already made with pre-heating for the subsequent processing step C.
During step C the pH of the steam is preferably adjusted to a value between 3.0 and 6.0 by adding a base and/or an acid. Acids which result during heating with steam (in particular, acetic acid) are neutralized by adding a base, and this is found to provide an improved product wherein corrosion of metal components of the apparatus used is also less than at a pH below 3.0. Excess of added base can be balanced by adding an acid. Furthermore, at a pH below 3.0, the reactions are accelerated such that the reactions are difficult to keep under control. At a pH higher than 6.0, the desired acid hydrolysis reaction proceeds too slowly. At a basic pH (higher than 7.0), acid hydrolysis does not occur while basic hydrolysis does, which results in undesirable products. Contrary to other wood treatment methods, the base is not used to actually treat the actual wood but only to neutralize the volatile acids resulting from the heat treatment of the wood. The amounts of base needed are, therefore, much smaller than by base treatment of woods, and also the products obtained are significantly different.
The pH of the steam is determined by collecting and measuring a condensate of the steam using a pH-meter which is commercially available. A dosed quantity of base can be supplied subject to the measured value. Preferably, a volatile base and a volatile acid are used, as volatile bases and acids readily spread in the treatment space and react rapidly, leading quickly to the predetermined pH of steam in the treatment space. Non-volatile basic or acidic compounds, such as sodium hydroxide, leave a solid residue on the wood. Examples of volatile bases are ammonia (NH 3 ), and volatile lower alkyl amines having from 1-6 carbon atoms, in particular, methylamine, ethylamine, n-propylamine, i-propylamine, diethylamine, triethylamine and diisopropylamine. Examples of volatile acids include carbon dioxide, hydrochloric acid, or lower alkyl acids having 1-3 carbon atoms, including formic acid, acetic acid and propanoic acid. Volatile bases or acids that already are gaseous may be dispensed from a pressurized container by a simple automated valve. Volatile bases and acids with a higher boiling temperature may be introduced using an inert carrier gas, such as nitrogen or argon.
The best balance between reaction rate and controllability is obtained if the pH is held between 4.2 and 4.7 during the reaction time.
It is recommended that the added base comprises ammonia. Ammonia (NH 3 ) is a volatile base which can be easily removed again as gas without leaving residue on the wood. Ammonia can be easily dispensed from a pressurized container.
Preferably, the added acid is carbon dioxide. Carbon dioxide can be added from a pressurized container and does not leave a residue on the wood. Moreover, corrosion problems associated with acids are virtually non-existent when carbon dioxide is used.
It is preferred if during step C the pH is monitored and maintained at a value between 3.0 and 6.0, preferably between 4.2 and 4.7, by adding a base and/or an acid. Thus, the process and the quality of the resulting product are optimized.
In step C the reaction temperature is preferably held between 160 and 190 degrees Celsius. At this temperature a good preservation is realized in combination with a minimal loss of mechanical strength.
In yet another exemplary embodiment, the wood has a temperature higher than 150 degrees Celsius for between 10 and 60 minutes during step C. At the reaction temperature above 150 degrees Celsius, a thermal activation of the wood constituents lignin and hemicellulose occurs for such a time, while excessive depolymerization of wood constituents is avoided by limiting the reaction time. Wood temperature can be monitored by inserting a thermometer between the wood parts in the treatment space.
During step C the steam preferably has a pressure of at least 4 bar. Heat and water are transferred rapidly to the wood at such a pressure. Step C is preferably performed at a steam pressure between 4 and 12 bar.
Another feature of the present disclosure provides a wood product which is obtainable according to the method disclosed hereinabove. Such a wood product has a good durability combined with a mechanical strength which is a maximum of only 10-15% lower than the wood before the treatment.
Yet another feature of the present disclosure provides an apparatus suitable for performing the method disclosed hereinabove. In one exemplary embodiment the apparatus comprises a treatment space sealable in medium-tight manner, a vacuum pump connected to the treatment space, a steam source connected to the treatment space, a heating device which is in thermal contact with the treatment space, dispensing means for adding predetermined amounts of a base and/or an acid to the treatment space, pH measuring means for determining the pH value of steam in the treatment space, and measuring and control equipment adapted to monitor at least the pH temperature and pressure inside the treatment space and to control the vacuum pump, the steam source and the heat source, and the pH by dispensing a base and/or an acid. The method disclosed hereinabove can be performed using such an apparatus. The apparatus can herein be programmed optimally for the treatment of determined types of wood. It is advantageous if the apparatus also comprises a device for adding a base and/or an acid, wherein the measuring and control equipment is also adapted to measure the pH of a condensate in the treatment space.
Preferably, the measuring and control equipment is programmed to maintain the pH in the treatment space at a predetermined value by adding base or acid by activating the dispensing means. During the treatment according to the method disclosed hereinabove, the pH can hereby be readily monitored and, in the case of acidification, easily increased by adding base. Excess base can be balanced by adding an acid. Hence it is relatively easy to maintain a predetermined pH value within the treatment space. The base is, for instance, ammonia, and the acid is, for instance, carbon dioxide, which can be added as an aqueous solution or as a gas dispensed by means of a dispensing device such as an automated valve.
In one exemplary embodiment, the apparatus also comprises homogenizing means for spreading the steam homogeneously over the treatment space. Such homogenizing means improve homogenous treatment of the wood. Also the monitoring of temperature and pH are more accurate. For instance, adding a predetermined amount of base or acid more rapidly results in a homogenously adjusted pH in the treatment space when homogenizing means are used. Preferably, at least part of the homogenizing means are located adjacent to the dispensing means. The homogenizing means may, for instance, be a mechanical ventilator.
In another exemplary embodiment, the steam source includes a container for water comprising heating means. Such means allow for an easy way of generating steam. Preferably, also the temperature within the container for water is monitored in order to precisely control water evaporation.
In a preferred apparatus, the treatment space is bounded by a double wall provided with thermally conducting oil. The temperature inside the treatment space can hereby be readily controlled and kept homogeneous. The thermal oil is situated between the two walls of the double wall.
The apparatus according to the present disclosure is preferably programmed for performing a method as disclosed hereinabove. The apparatus can be provided for this purpose with a computer with which the measuring and control equipment is read and the vacuum pump, the steam source and the heat source and possible other components are controlled.
BRIEF DESCRIPTION OF THE DRAWINGS
Various aspects of the present disclosure are described hereinbelow with reference to the accompanying figures.
FIG. 1 shows a schematic view of one exemplary embodiment of an apparatus according to the present disclosure;
FIG. 2 is a graph of the progression of various reaction parameters during the process of the preservation of wood according to one method of the present disclosure; and
FIG. 3 shows a schematic view of another exemplary embodiment of an apparatus according to the present disclosure.
DETAILED DESCRIPTION
FIG. 1 shows a treatment space 1 filled with wood parts 4 . The treatment space 1 is provided with a double wall 1 in which thermally conducting oil 2 is arranged. Connected to the treatment space is a vacuum pump 5 with which the air pressure in the sealed treatment space can be reduced to 10 kPa (abs) in order to remove air from the space 1 and thereby reduce undesirable chemical reactions of oxygen with wood components which can result in permanent loss of mechanical strength of wood 4 . Steam from a steam generator 8 can then be fed to vacuumized treatment space 1 via a control valve 7 , wherein the temperature and pressure in treatment space 1 is adjusted such that it is unsaturated, with a degree of saturation of a maximum of 95%. Both the wall temperature and the wood temperature remain at least several degrees Celsius higher than the vapour dew point temperature at all times by a thermostat and heating device in order to avoid condensation anywhere in the treatment space. The rise in temperature is limited to 20 to 60 degrees Celsius per hour in order to achieve the required uniformity of temperature over the whole volume, most preferably approximately 30-50 degrees Celsius per hour. Lower temperature increase rates are easier to control, whereas a higher increase rate shortens the procedure time. During the whole heating phase, the steam in treatment space 1 remains below 95% saturation relative to the saturation at that temperature. The measuring and control equipment 6 comprises thermometers for vapour temperature and wall temperature, a pressure gauge and a pH meter. Condensation of water from the steam can result in unwanted variation in water contents in treatment space 1 . In order to prevent condensation, the wall temperature is held above the temperature of steam inside the boiler 1 .
As the temperature increases, in particular, from 130 degrees Celsius and, in particular, from 150 degrees Celsius, degradation reactions of hemicelluloses and lignin take place in the wood at a sufficiently critical speed. Organic acids (for instance, acetic acid), aldehydes (for instance, fururals, such as hydroxymethylfurfural) and monomeric sugars (for instance, xylose) result here among others. Lignin will then partially depolymerize. The extent to which the degradation reactions take place is determined by, among other factors, the chemical composition of the wood and further by the controllable process conditions:
the highest temperature reached (typical values are respectively 160 to 190 degrees Celsius),
the reaction time at this temperature (10 to 60 minutes),
the pressure (4 to 12 bar),
the pH (3.0 to 6.0), and
the relative humidity of the steam.
The process conditions are optimized for each type of wood and depend partly on each other. The pH can be regulated by adding a base for the purpose of neutralizing released organic acids. In the shown exemplary embodiment, the base is ammonia which is fed as a gas from a pressure cylinder 8 , wherein the pH is measured in a pH meter 6 which measures the pH of a condensate of the steam.
After the reaction time has ended, most degradation products are still situated in the wood. The wood is then in a soft state, at or above the glass temperature. The wood can optionally be compressed in this phase for the purpose of compaction thereof by means of pressure means which are not shown here.
In the subsequent process, the reaction products are linked together again under dry conditions. The wall temperature is here maintained or increases slightly, while the relative humidity decreases gradually by discharging gas from the boiler. The equilibrium moisture content decreases in controlled manner such that the wood dries gradually and uniformly to a moisture content of 3 to 5%. The polymerization of the degradation products comes about as this drying progresses, wherein the material strength is restored. Finally, the wood must be cooled in a controlled manner, wherein the equilibrium moisture content is raised again to 7-8% by weight from 100 degrees Celsius (or another temperature, well below 140 degrees Celsius) in order to condition the wood for subsequent final processing.
It is found that the wood has an increased fungal resistance after this treatment, while the mechanical strength decreases by a maximum of 10% to 15%.
FIG. 2 shows a schematic example of the progression of various reaction parameters during the preservation of wood according to the present disclosure. The shown reaction is optimized for spruce wood ( Picea Abies ) but can be adapted for use with other types of wood, such as pinewood ( Pinus Sylvestris ). The wood is placed in a treatment space in wood parts (planks) with a thickness of about 25 mm, as shown in FIG. 1 . With modifications to reaction times, the method can optionally be adapted to other thicknesses of the wood parts, wherein the times for thicker wood parts will generally be longer. The temperature and vapour pressure of steam are regulated by a programmed control unit and adjusted if necessary on the basis of the measured values. The parameters (temperature in degrees Celsius, pressure in bar) are plotted against the time in hours. The saturation pressure of steam is also indicated at the temperature, wherein the graph shows that the vapour pressure of the steam in the treatment space is held below 100% saturation during the treatment. Condensation of water in the treatment space is hereby prevented.
In step A the wood for treating is placed in the treatment space and vacuum is then created in step B). During the creation of vacuum, the boiler can already be pre-heated to 70 degrees Celsius for additional time-savings. In step C steam is subsequently supplied and the temperature is simultaneously increased from 20 to 180 degrees in a period of 4 hours (40 degrees per hour), wherein the wood is at a temperature higher than 150 degrees for a reaction time of about 15 minutes. The pressure herein rises to about 9 bar, wherein the steam is held at all times below the saturation pressure. The high steam pressure serves to accelerate the hydrolysis reaction, as well as stabilizing the moisture content of the treated wood. The pressure is then reduced in step D and steam is thus discharged by discharging steam at 180 degrees, whereby water is discharged and the wood constituents activated in step C are polymerized, wherein cross-links occur between, for instance, lignin and hemicellulose. At the shown combination of temperature and vapour pressure, a hygroscopic equilibrium between the wood and the vapour is achieved wherein the moisture content of the wood is lower than 5% by weight. In step E the polymerization is then stopped by cooling and steam is supplied again, wherein the hygroscopic equilibrium is such that the moisture content of the wood is between 7 and 8% by weight. The wood is hereby conditioned for further treatment. The produced wood is particularly durable and fungal-resistant, and also has a mechanical strength which is no more than 10-15% lower than the starting material. The whole process is completed within 10 hours. The known slow processes for preservation take at least a day and are comparable in respect of durability, but display more damage, such as splitting, whereby the mechanical strength can decrease to less than 80%. The known rapid preservation processes, with temperatures of 240 degrees Celsius, likewise produce an inferior product due to brittleness and a greatly reduced mechanical strength. As a side-effect, the wood treated according to the present disclosure also shows a darkening in colour appearance.
FIG. 3 describes another exemplary embodiment of an apparatus 20 according to the present disclosure. The treatment space 21 is confined by a thermally isolated outer reactor wall 22 and a thermally conducting inner reactor wall 23 which is filled with a thermally conductive oil. The treatment space 21 connects to a water container 24 containing water 25 that is heated by heating means 26 in order to generate steam, which is led to the treatment chamber 21 through a steam channel 27 . The amount of water should be sufficient for achieving the desired steam pressure in the reactor chamber 21 , taking into account the additional water consumed by hydrolysis reactions and the amount of water adsorbed by the wood. The container is sufficiently large to store the initial amount of water plus the amount released by condensation reactions, dehydration reactions and drying. The reactor chamber 21 is provided with a mechanical stirrer 28 used to homogenize the generated steam and volatile reaction products leading to a homogenous exposure of the treated wood parts 29 . The wood parts 29 are preferably spaced apart, preferably having mutual distances of 8-15 mm, allowing for an even more homogenous treatment. If wood parts 29 are packed closely together, inner parts in a pile of wood parts 29 are less exposed than outer parts, leading to different treatment of the parts. Preferably, the reactor space 21 and the water container 24 form a closed system, in order to optimize the use of water. Preferably, the system is provided with a safety pressure valve. During the processing of the wood, the water container can be used as a cold spot wherein the water container 24 has a temperature lower than the reactor space 21 in order to ensure that water condenses in the water container and not in the reactor space 21 where it could possibly condense on the wood 29 . For safety reasons, the reactor space 21 is provided with at least one standard safety pressure release valve set at a pressure below the maximum pressure the reactor walls 22 , 23 can withstand. Under operating conditions according to the present disclosure, the pressure typically ranges from vacuum to a maximum of approximately 12 bar, hence the safety pressure release valve could, for instance, be set at 14 bar. The pressure inside the reactor space 21 can be monitored by a standard pressure meter 47 covering the operating range.
The reactor space 21 also connects to a first pressurized cylinder 30 comprising carbon dioxide (CO 2 ) which is connected through a first automated dispensing valve 31 . Carbon dioxide may be used to lower the pH in the reactor as carbon dioxide acidifies steam. The apparatus 20 also comprises a second pressurized cylinder 32 of ammonia (NH 3 ) also connected to a second automated dispensing valve 33 . Having the possibility to add predetermined amounts of acid or base may be used to maintain the pH at a predetermined value during the treatment according to the present disclosure. The pH is monitored by taking samples of the steam in the reactor space 21 by temporarily opening a sample valve 34 , condensing the sampled steam in a condensator 35 , and collecting the condensed steam 36 for pH measurement using regular electrochemical pH measurement equipment 37 .
The reactor chamber is also provided with a vacuum pump system 38 for evacuating the reactor chamber, in particular, for removing oxygen gas. The vacuum system 38 optionally includes a pressure meter for monitoring pressure within the chamber. Instead of the optional pressure meter, it is also possible to rely on temperature and pH measurements only.
The apparatus 20 is provided with heating means 45 for heating the reactor chamber 21 , and a temperature measurement units ( 40 , 41 , 42 ) for the inner reactor wall 23 (unit 40 ), the wood 29 (unit 41 ) and the water 25 of the steam generator 24 (unit 42 ). A central control unit 43 monitors the temperature of the wood 41 , the temperature of the inner reactor wall 23 , the temperature of the steam water 25 , the pressure within the reactor space 21 , and the pH within the reactor space. The control unit 43 will then, following the preset program or manual control, adjust these parameters. For instance, pressure can be increased by turning up the heater 26 of the steam generator leading to increased steam evaporation, or the pressure can be lowered by lowering the temperature, water evaporation and/or opening the vacuum valve 44 of the vacuum system 38 . The vacuum valve 44 is a three-way valve that can also be used to depressurize the reaction vessel 21 or to let air or an inert gas, such as nitrogen, into the reactor space 21 in order to remove vacuum. The temperature in the chamber 21 can be adjusted by the wall heater unit 45 . pH can be lowered by adding carbon dioxide 30 , or pH can be increased by adding ammonia 32 . | An apparatus for preserving wood product comprising, in one embodiment, a treatment space sealable in medium-tight manner; a vacuum pump connected to the treatment space; a steam source connected to the treatment space; a heating device which is in thermal contact with the treatment space; a dispenser for adding predetermined amounts of either a base or an acid to the treatment space; pH measuring device for determining the pH value of steam in the treatment space; and measuring and control equipment adapted to monitor at least the pH temperature and pressure inside the treatment space and to control the vacuum pump, the steam source and the heat source, and the pH by dispensing either a base or an acid. Also disclosed is a method for preserving wood. The preservation process has a relatively short process time, wherein a good preservation is realized while the mechanical strength of the wood is largely retained. The amount of waste wood material is greatly reduced. | 8 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to remote procedure call (RPC), and more particularly, to streaming remote procedure call.
[0003] 2. Description of the Related Art
[0004] With the increasing prevalence of multimedia application software, more and more dual-core processors, or even multi-core processors, utilize such multimedia application software to meet efficiency requirements. An ordinary multi-core processor comprises a plurality of processing units, which can be connected via many types of communication mechanisms, such as shared memory, memory mapping interrupts, mailbox and channel-based protocol.
[0005] One advantage of multi-core processors is that each processing unit executes its own procedure with parallel computing. However, due to the varieties of the programming environment of each processing unit, the complexity of the software development has increased. Accordingly, one technique, known as Remote Procedure Call (RPC) has been widely applied to improve the software development efficiency. RPC is the technique for a client calling a server to execute a specific procedure. In other words, whether on a client or a server, a software designer can write the same computer program without making adjustments to accommodate different programming environments.
[0006] One present challenge for multi-core processors is providing a suitable data streaming mechanism for multimedia applications. Various multimedia applications, such as video encoding and decoding, image processing, data mining and graphical rendering all require the data streaming mechanism. However, when executing RPC, most present multi-core processors used with multimedia applications will not send data back to the client until the server finishes its procedure. Such waiting is not time-efficient for real-time multimedia applications. Therefore, finding a method to execute RPC by streaming is the one of the most crucial issues for RPC technique.
SUMMARY OF THE INVENTION
[0007] One objective of the present invention is to provide a method of streaming remote procedure invocation for multi-core systems and a middleware to implement the method. The method temporarily stores data to be transmitted to a server to prevent the need for a client to repeatedly call the server and thus improves the data transmitting efficiency.
[0008] The method of streaming remote procedure invocation for multi-core systems to execute a transmitting thread and an aggregating thread of a multi-core system according to one embodiment of the present invention comprises the steps of: temporarily storing data to be transmitted; activating the aggregating thread if the amount of the temporarily stored data is equal to or greater than a threshold and the aggregating thread is at pause status; pausing the transmitting thread if there is no space to temporarily store the data to be transmitted; retrieving data to be aggregated; activating the transmitting thread if the amount of the data to be aggregated is less than a threshold and the transmitting thread is at pause status; and pausing the aggregating thread if there is no data to be retrieved.
[0009] In some embodiments of the present invention, the method of streaming remote procedure invocation for multi-core systems is executed by a middleware. The middleware comprises a streaming channel module, a plurality of streaming buffer modules and a streaming controller module. The streaming channel module is configured to be the communication channel for transmitting streaming data between the clients and the servers. The plurality of streaming buffer modules is configured to temporarily store the data to be transmitted on the streaming channel module. The streaming controller module is configured to control the streaming channel module and the streaming buffer modules
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The objectives and advantages of the present invention will become apparent upon reading the following description and upon referring to the accompanying drawings of which:
[0011] FIG. 1 shows the development procedure of an embedded software, wherein the embedded software is one embodiment of the method of streaming remote procedure invocation for multi-core systems of the present invention;
[0012] FIG. 2 shows a software framework of a conventional dual-core system applied to an ordinary RPC mechanism;
[0013] FIG. 3 shows a middleware framework of the method of streaming remote procedure invocation for multi-core systems according to one embodiment of the present invention;
[0014] FIG. 4 shows a flow chart of the method of streaming remote procedure invocation for multi-core systems according to one embodiment of the present invention;
[0015] FIG. 5 shows a flow chart of the method of streaming remote procedure invocation for multi-core systems according to another embodiment of the present invention; and
[0016] FIG. 6 shows a block diagram of a multi-core system utilizing the method of streaming remote procedure invocation for multi-core systems of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0017] FIG. 1 shows the development procedure of an embedded software, wherein the embedded software is one embodiment of the method of streaming remote procedure invocation for multi-core systems of the present invention. As shown in FIG. 1 , the development procedure is accomplished by developing software 90 on an operating system 80 . The developing software 90 comprises a compiler, an assembler and a linker. In step 10 , the standard of the application software corresponding to the developing software is established. In step 20 , the middleware of the streaming remote procedure invocation is constructed. In step 30 , the communication model of the embedded software is constructed by the middleware. In step 40 , the hardware communication model, including shared memory, mailbox and direct memory access, is designed according to the hardware realization which is compatible with the communication model of the embedded software. Steps 50 and 60 are for verification. In step 50 , the embedded software is simulated on a virtual platform. In step 60 , the embedded software is realized on a hardware development platform. In step 70 , the performance of the embedded software is evaluated. If the performance of the embedded software does not meet the requirement, step 40 is executed to refine the hardware communication model, or step 20 is executed to modify the middleware.
[0018] As shown in FIG. 1 , a middleware is constructed on the communication model of the embedded software in this embodiment to provide a high hierarchy developing environment such that the tedious software developing procedures specific to individual hardware platforms is reduced.
[0019] FIG. 2 shows a software framework of a conventional dual-core system applied to an ordinary RPC mechanism. The software framework 200 is constructed on a hardware communication model 240 . The dual-core system comprises a client 510 and a server 520 . As shown in FIG. 2 , when the client 510 requires the service of RPC, RPC stubs 210 and 220 are executed first for the processing of the RPC. As shown in FIG. 2 , the RPC stubs 210 and 220 exchange data with each other via a register module 230 . The middleware applied to the streaming remote procedure invocation for multi-core systems of some embodiments of the present invention is constructed on the hardware communication model 240 .
[0020] FIG. 3 shows a middleware framework of the method of streaming remote procedure invocation for multi-core systems according to one embodiment of the present invention. The middleware 300 applied to the multi-core system comprising a plurality of client 510 and a plurality of servers 520 . The middleware 300 comprises a streaming channel module 310 , a plurality of streaming buffer modules 320 and a streaming controller module 330 . The streaming channel module 310 is configured to be the communication channel for transmitting streaming data between the client 510 and the server 520 . The streaming channel module 310 comprises a plurality of streaming channels, and such streaming channels can be distinguished by their own identification codes. The streaming buffer modules 320 are configured to temporarily store the data to be transmitted through the streaming channels, wherein each streaming channel comprises a plurality of streaming buffers to support buffering data when a streaming operation interface is executed. The streaming controller module 330 is configured to control the streaming channel module 310 and the streaming buffer modules 320 .
[0021] As shown in FIG. 3 , the middleware 300 is configured to control the streaming mechanism for remote procedure invocation between the client 510 and the server 520 . As described above, the middleware 300 of the streaming remote procedure invocation for multi-core systems of the embodiments of the present invention is constructed on the hardware communication model 240 such that software designers can develop software based on the middleware 300 without considering the underlying hardware.
[0022] FIGS. 4 and 5 show flow charts of executing a transmitting thread and an aggregating thread in a multi-core system according to one embodiment of the method of streaming remote procedure invocation for multi-core systems of the present invention, wherein this embodiment is realized by the middleware 300 . FIG. 4 shows the flow chart of executing a transmitting thread in a multi-core system according to one embodiment of the method of streaming remote procedure invocation for multi-core systems of the present invention. In step S 1 , it is determined whether there are enough streaming buffer modules 320 available. If the result is negative, step S 6 is executed; otherwise, step S 2 is executed. In step S 2 , it is determined whether the execution of the transmitting thread is complete. If the result is positive, the transmitting thread is ended; otherwise, step S 3 is executed. In step S 3 , a datum is stored in a streaming buffer module 320 , and step S 4 is executed. In step S 4 , it is determined whether the number of the streaming buffer modules 320 with stored streaming data is equal to or greater than a threshold and the aggregating thread is at pause status. If the result is negative, step S 1 is executed; otherwise, step S 5 is executed. In step S 5 , the aggregating thread is activated. In step S 6 , the transmitting thread is paused, and step S 7 is executed. In step S 7 , it is determined whether the transmitting thread is activated. If the result is positive, step S 1 is executed; otherwise, step S 6 is executed.
[0023] FIG. 5 shows the flow chart of executing an aggregating thread in a multi-core system according to one embodiment of the method of streaming remote procedure invocation for multi-core systems of the present invention. In step P 1 , it is determined whether there is a streaming buffer module 320 with stored streaming data. If the result is negative, step P 6 is executed; otherwise, step P 2 is executed. In step P 2 , it is determined whether the execution of the aggregating thread is complete. If the result is positive, the aggregating thread is ended; otherwise, step P 3 is executed. In step P 3 , a datum is retrieved from a streaming buffer module 320 with stored streaming data, and step P 4 is executed. In step P 4 , it is determined whether the number of the streaming buffer modules 320 with stored streaming data is less than a threshold and the transmitting thread is at pause status. If the result is negative, step P 1 is executed; otherwise, step P 5 is executed. In step P 5 , the transmitting thread is activated. In step P 6 , the aggregating thread is paused, and step P 7 is executed. In step P 7 , it is determined whether the aggregating thread is activated. If the result is positive, step P 1 is executed; otherwise, step P 6 is executed.
[0024] As shown in FIGS. 4 and 5 , the middleware 300 acts as a buffer between the client 510 and the server 520 such that the client 510 can continue to process another procedure after the client 510 invocates the server 520 to execute the procedure without waiting for the server 520 to return the result of the invocated procedure.
[0025] Referring back to FIG. 3 , the middleware 300 is utilized to realize the embodiments of the method of streaming remote procedure invocation for multi-core systems of the present invention, wherein the streaming controller module 330 is configured to control the process shown in FIGS. 4 and 5 , and the aforementioned threshold controls the communication speed between the processors of the multi-core system. The threshold can prevent the transmitting thread and the aggregating thread from being paused and activated repeatedly, which lowers the performance of the multi-core systems, due to the difference of the execution time between the transmitting thread and the aggregating thread. Ordinarily, a greater threshold can compensate a larger difference of the execution time between the transmitting thread and the aggregating thread. However, a greater threshold can also slow down the computing speed and thus violates the real-time processing requirement. Therefore, a proper threshold value is required.
[0026] FIG. 6 shows a block diagram of a multi-core system utilizing an embodiment of the method of streaming remote procedure invocation for multi-core systems of the present invention. The multi-core system 500 comprises the client 510 , the server 520 and the streaming channel module 310 and applies the middleware 300 and an embodiment of the method of streaming remote procedure invocation for multi-core systems of the present invention. The client 510 and the server 520 access the streaming channel module 310 at average rates of ε and δ respectively. The response time of the server 520 to the nextprocessor stage is T r , the time required to activate the server 520 is T trigger , the data processing time required by the server 520 is α, and the threshold value is n. If the transmitting thread of the server 520 is paused, the transmitting thread of the server 520 is not activated again until n streams of data are transmitted by the client 510 . Therefore, the requirement of T r is:
[0000]
T
r
≥
T
trigger
+
n
ɛ
+
α
.
[0000] It can be obtained that the proper value for the threshold n is: n≦(T r −T trigger −α)*ε. In other words, the proper value for the threshold n is equal to or less than the result of the response time of the next processor stage of the server 520 minus the activation time of the server 520 and the data processing time required by the server 520 multiplied by the rate of the client 510 access to the streaming channel module 310 .
[0027] In conclusion, the method of streaming remote procedure invocation for multi-core systems of the present invention and the middleware to implement the method provide the software designer with a developing environment with hierarchy higher than that of the communication module of the multi-core system. In addition, the method and the middleware enable the processors of the multi-core system to continue their own procedure while communicating with each other and hence improve the performance. Further, the method can significantly alleviate the problem of the difference between the computing speeds of the client and the server.
[0028] The above-described embodiments of the present invention are intended to be illustrative only. Those skilled in the art may devise numerous alternative embodiments without departing from the scope of the following claims. | A method of streaming remote procedure invocation for multi-core systems to execute a transmitting thread and an aggregating thread of a multi-core system comprises the steps of: temporarily storing data to be transmitted; activating the aggregating thread if the amount of the temporarily stored data is equal to or greater than a threshold and the aggregating thread is at pause status; pausing the transmitting thread if there is no space to temporarily store the data to be transmitted; retrieving data to be aggregated; activating the transmitting thread if the amount of the data to be aggregated is less than a threshold and the transmitting thread is at pause status; and pausing the aggregating thread if there is no data to be retrieved. | 6 |
BACKGROUND
[0001] This invention relates generally to memories that use phase-change materials.
[0002] Phase-change materials may exhibit at least two different states. The states may be called the amorphous and crystalline states. Transitions between these states may be selectively initiated, for example, through temperature changes. The states may be distinguished because the amorphous state generally exhibits higher resistivity than the crystalline state. The amorphous state involves a more disordered atomic structure and the crystalline state involves a more ordered atomic structure. Generally, any phase-change material may be utilized; however, in some embodiments, thin-film chalcogenide alloy materials may be particularly suitable.
[0003] The phase-change may be induced reversibly. Therefore, the memory may change from the amorphous to the crystalline state and may revert back to the amorphous state thereafter, or vice versa. In effect, each memory cell may be thought of as a programmable resistor that reversibly changes between higher and lower resistance states in response to temperature changes. The temperature changes may be induced by resistive heating.
[0004] In some situations, the cell may have a large number of states. That is, because each state may be distinguished by its resistance, a number of resistance-determined states may be possible, allowing the storage of multiple bits of data in a single cell.
[0005] A variety of phase-change alloys are known. Generally, chalcogenide alloys contain one or more elements from column VI of the periodic table. One particularly suitable group of alloys is GeSbTe alloys.
[0006] A phase-change material may be formed within a passage or pore defined through a dielectric material. The phase-change material may be coupled to electrodes on either end of the passage. The contacts may pass current through the passage in order to program the cell through resistive heating or to read the programmed state of the cell.
[0007] Current phase-change memories rely on the poor thermal conductivity of the chalcogenide phase-change memory material itself to thermally insulate the programmable volume from heat loss to the upper electrode. Consequently, in order to achieve better thermal isolation and, therefore, more energy efficient programming of the programmable volume, the thickness of the chalcogenide layer has to be increased. An increase of the thickness of the layer, however, also increases the volume of material that is capable of undergoing a phase-change during programming. Increasing the volume of material that undergoes the phase-change can adversely affect reliability, stability, and cycle life of the memory.
[0008] Thus, there is a need for a phase-change memory with improved characteristics and performance.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] [0009]FIG. 1 is an enlarged, cross-sectional view of one embodiment of the present invention;
[0010] [0010]FIG. 2 is an enlarged, cross-sectional view of an initial stage of manufacturing of the device shown in FIG. 1 in accordance with one embodiment of the present invention;
[0011] [0011]FIG. 3 is an enlarged, cross-sectional view of the embodiment shown in FIG. 2 at a later stage of manufacturing in accordance with one embodiment of the present invention;
[0012] [0012]FIG. 4 is an enlarged, cross-sectional view of the embodiment shown in FIG. 3 at still a later stage of manufacturing in accordance with one embodiment of the present invention;
[0013] [0013]FIG. 5 is an enlarged, cross-sectional view corresponding to FIG. 4 at still a later stage of manufacturing in accordance with one embodiment of the present invention; and
[0014] [0014]FIG. 6 is an enlarged, cross-sectional view of the embodiment shown in FIG. 5 at a later stage of manufacturing in accordance with one embodiment of the present invention.
DETAILED DESCRIPTION
[0015] Referring to FIG. 1, a phase-change memory 10 may be formed on an integrated circuit substrate 12 . The phase-change memory 10 may include a lower electrode 14 that in one embodiment may be made of cobalt silicide. An upper electrode 28 sandwiches a lower, programmable phase-change layer 22 and an upper phase-change layer 26 . Between the phase-change layers 22 and 26 is a chemical barrier layer 24 .
[0016] The pore of the phase-change memory 10 may be defined by sidewall spacer 20 . That is, the region of contact between the lower electrode 14 and the phase-change layer 22 may be of a size determined through the imposition of the cylindrical sidewall spacer 20 . In one embodiment, the pore, including the phase-change layers 22 and 26 , may be defined within an opening formed in a pair of insulator layers, such as the upper insulating layer 18 and the lower insulating layer 16 . The upper insulating layer 18 may be silicon dioxide in one embodiment, and the lower insulating layer 16 may be silicon nitride in one embodiment.
[0017] While a structure is illustrated in which two layers of phase-change material are utilized, more layers may be utilized in other embodiments. The thickness of the first phase-change layer 22 may be in the range of 300 to 500 Angstroms. The thickness of this layer may be chosen so as to reduce the vertical dimension of the programmed volume. The phase-change layer 22 may be deposited in a cup-shaped opening formed by the sidewall spacer 20 , resulting in a cup-shaped phase-change layer 22 . A similar shape is therefore defined for the barrier layer 24 and the overlying phase-change layer 26 . In one embodiment, the phase-change layers 22 and 26 may be formed using vapor deposition.
[0018] The barrier layer 24 provides a chemical barrier between the underlying programmable phase-change layer 22 and the overlying phase-change layer 26 . The overlying phase-change layer 26 may be provided primarily for thermal isolation in some embodiments. The barrier layer 24 may have adequate electrical conductivity so that the programming current passing through the programmable phase-change layer 22 can flow laterally around any resistive region of the thermal isolation phase-change layer 26 and may contact to the conductive regions of this layer distant from the programming region.
[0019] Typical thickness of the barrier layer 24 may be in the range of 50 to 200 Angstroms. The thermally insulating phase-change material layer 26 may also be vapor deposited in situ onto the barrier layer 24 . The thermally insulating phase-change material layer 26 can be made of the same composition as the programmable phase-change layer 22 or it can be chosen from a range of available chalcogenide materials with poor thermal conductivity. In one embodiment, it is advantageous that the layer 26 has a thermal conductivity of less than 1E-2 W/cm.K and good electrical conductivity, for example, greater than 40 Ω −1 cm −1 . The thickness of the layer 26 can be in the range of from 100 to more than 1,000 Angstroms.
[0020] Referring to FIG. 2, a mask 30 may be defined on a stack including the substrate 12 covered by the lower electrode 14 , the first insulating layer 16 , the second insulating layer 18 .
[0021] Turning next to FIG. 3, an opening 32 may be etched through the insulating layers 16 and 18 , stopping on the lower electrode 14 . In one embodiment, an etchant that is selective to the layers 16 and 18 and that is less effective against the electrode 14 may be utilized. Thereafter, the insulating material 20 may be deposited into the pore and over the layer 18 , as shown in FIG. 4. A variety of insulating layers may be utilized including oxide. In one embodiment, a tetraethylorthosilicate (TEOS) oxide deposition process may be utilized. The deposited layer 20 is then subjected to an anisotropic etch to form the cylindrical sidewall spacer 20 as shown in FIG. 5.
[0022] The sidewall spacer 20 and insulating layer 18 may then be coated with the programmable phase-change layer 22 . The layer 22 may then be coated with the barrier layer 24 and the insulating phase-change layer 26 . Finally, the upper electrode 28 may be deposited. Because of the imposition of the sidewall spacer 20 , each of the layers 22 , 24 , 26 and 28 , to some degree, may be defined in a cup-shaped configuration. The structure shown in FIG. 6 may then be subjected to patterning and etching to result in the structure shown in FIG. 1 in some embodiments.
[0023] Through the use of multiple chalcogenide layers, the memory cell 10 benefits from the enhanced thermal isolation. At the same time, the volume of material that undergoes a phase-change during programming may be relatively limited. In other words, the insulating effect of the combined layers 22 and 26 may reduce heat loss from the memory 10 , improving programming performance. At the same time, it is not necessary to program the insulating layer 26 , reducing the volume of material that must undergo the phase-change during programming. This may improve reliability, stability, and cycle life of the memory 10 in some embodiments.
[0024] While the present invention has been described with respect to a limited number of embodiments, those skilled in the art will appreciate numerous modifications and variations therefrom. It is intended that the appended claims cover all such modifications and variations as fall within the true spirit and scope of this present invention. | A phase-change memory may be formed with at least two phase-change material layers separated by a barrier layer. The use of more than one phase-change layer enables a reduction in the programming volume while still providing adequate thermal insulation. | 7 |
FIELD OF THE INVENTION
The present invention generally relates to micromachined accelerometers, and more particularly relates to tungsten coatings applied to arrays of suspended silicon fingers in a highly integrated accelerometer.
BACKGROUND OF THE INVENTION
MEMS (Micro-Electro-Mechanical Systems) accelerometers, also sometimes referred to as Highly Integrated Accelerometers (HIA), are used in a variety of applications including as triggering sensors for air bag deployment. An HIA is designed to sense changes in acceleration at a defined sensitivity threshold. Events that satisfy the defined acceleration criteria electronically activate a signal, which in turn is used to initiate a desired device response, such as, for example, inflation of a safety air bag.
A MEMS accelerometer typically includes structures known as sensing fingers. In a common design, the sensing fingers are fabricated of silicon from the underlying silicon substrate of the electronic device. A sensing finger is a three dimensional structure, typically with high aspect ratio, and in the general shape of a wall. A sensing finger is designed to deflect physically in response to a sensed acceleration. Thus, it is typically desired to fabricate a sensing finger, or preferably an array of sensing fingers, with a given spacing and resistance to deflection.
Typically, an array of sensing fingers is integrally created in an HIA. Electrical charge in the finger array creates a capacitance between adjacent fingers. Rapid accelerations of the HIA result in a physical deflection of neighboring fingers. This physical deflection affects the capacitance of the array. The device to which the array is attached senses the change in capacitance, and this initiates the device signal.
One drawback to current methods of fabricating sensing fingers is finger stiction. If two or more fingers bend or deflect, they may come into contact with one another. The contact can also result in the fingers adhering to each other. This is finger stiction. Stiction can arise for a variety of reasons including capillary forces, electrostatic forces, and Van der Walls attraction. Stiction is undesirable for the reason that it leads to failure of the accelerometer. Contact between fingers can cause an electrical short thereby upsetting the designed electrical function of the device. Additionally, the result of two fingers in contact results in a mechanical stiffening of the structure, which may itself affect the designed deflection resistance of the device.
There is a further movement in the design of HIAs and MEM accelerometers to increase the aspect ratio of the silicon fingers such that the fingers grow in height for a given width. This trend results from a desire to decrease the footprint of the finger array on a base without decreasing the capacitance area in the array. One way to achieve this is to increase the vertical height of a silicon finger. However, finger elongation further aggravates stiction problems; it creates a physical setting in which any bending of the silicon fingers are additionally susceptible to stiction. The geometry of elongated fingers lowers the threshold at which bending or warping places adjacent fingers in contact.
It is further desired to improve the sensitivity of HIAs. As these devices are often used in the triggering of safety equipment, it is desired to improve the functional sensitivity if possible. Generally sensitivity of a finger array is a function of displacement/acceleration. Additionally the sensitivity may be characterized as mass of the finger/finger spring constant. Thus, adding mass to silicon fingers has the added benefit of improving the device sensitivity.
Accordingly, it is desirable to redesign currently used accelerometers. In particular it is desired to design and manufacture an accelerometer so as to reduce finger stiction. In addition, it is desirable to design an accelerometer with improved sensitivity. Furthermore, other desirable features and characteristics of the present invention will become apparent from the subsequent detailed description of the invention and the appended claims, taken in conjunction with the accompanying drawings and this background of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will hereinafter be described in conjunction with the following drawing figures, wherein like numerals denote like elements, and
FIG. 1 is a profile view of an array of silicon fingers on a substrate;
FIG. 2 is a profile view of an array of silicon fingers subject to stiction;
FIG. 3 is a view of a multilayer structure that may be fabricated into a silicon finger array according to an embodiment of the present invention;
FIG. 4 is a profile view of an array of silicon fingers positioned on a substrate that may be further processed according to an embodiment of the present invention;
FIG. 5 is a profile view of an array of silicon fingers positioned on a substrate that has received a tungsten coating according to an embodiment of the present invention; and
FIG. 6 is a photomicrograph of a tungsten layer deposited on a silicon substrate according to an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The following detailed description of the invention is merely exemplary in nature and is not intended to limit the invention or the application and uses of the invention. Furthermore, there is no intention to be bound by any theory presented in the preceding background of the invention or the following detailed description of the invention.
Referring to FIG. 1 there is shown an array 1 of silicon fingers 2 positioned on a substrate 3 . The fingers in this representation do not include a coating. The array is a structure that may be included in an HIA. The fingers 2 are generally elongate structures with a high aspect ratio. The structure of FIG. 1 represents fingers in an ideal setting. The fingers are parallel in orientation and do not display any contact between them.
Referring now to FIG. 2 there is shown an array 1 of fingers 2 under less than ideal conditions. Again the fingers 2 are uncoated. In FIG. 2 some fingers 2 of the array are in contact due to stiction. Forces have warped and bent the fingers. As a result adjacent fingers have come into contact with each other at one point. This contact can degrade the capacitance that would otherwise between the fingers, and thus affects performance of the accelerometer to which the fingers are attached.
It has now been discovered that a tungsten coating can be selectively deposited on silicon fingers. The tungsten-coated fingers display improved resistance to stiction. Further, the tungsten-coated fingers display improved sensitivity over non-coated fingers. The tungsten-coated fingers thus display improved performance as triggering sensors in a highly integrated accelerometer.
A method of fabricating the tungsten-coated silicon fingers is now described. Referring to FIG. 3 there is shown one embodiment of a structure from which the coated silicon fingers may be constructed. The structure comprises a first layer of silicon 11 , such as monosilicon. Above the silicon layer 11 is an oxide layer 12 ; the oxide layer may comprise silicon dioxide. Above oxide layer 12 is a second silicon layer 13 , which may comprise monosilicon or polycrystalline silicon. Above layer 13 is a hard mask 14 . And above hard mask 14 is a photo resist 15 . The structure of FIG. 3 can be fabricated using methods known in the semiconductor industry.
As is known in the semiconductor manufacturing art, the structure in FIG. 3 may be subjected to a patterning whereby channels are cut into the hard mask 14 and the silicon layer 13 up to the oxide layer 12 . One process to accomplish the patterning is a dry etching technique. The photo resist 15 may then be removed by known techniques.
What then remains is a structure as shown in FIG. 4 . In that figure, the general shape of the silicon fingers 20 has now been defined. Generally, the finger is a high aspect structure (height/width). The finger is also a three dimensional structure although two dimensions are illustrated in FIG. 4 . Thus, the finger may continue, for example, in the dimension that extends into and out of the surface of the page. A hard mask cap 14 remains on the upper surface of the fingers 20 . This hard mask cap is the remnant of the hard mask layer 14 in the structure of FIG. 3 .
Fingers 20 are preferably a silicon material. They may be polysilicon or single crystal silicon. Bulk micromachining techniques generally call for the use of single crystal. The industry tendency is to go to bulk micromachining. Surface micromachining techniques allow the use of polysilicon materials.
It will be appreciated by those skilled in the art that fingers 20 are partly defined by their width and the spacing between them. These dimensions may be set by the width and spacing of the photo resist 15 as shown in FIG. 3 . In one preferred embodiment, the spacing between the silicon fingers is approximately 1.5 μm. Other spacings are also possible. It is optionally preferred to fabricate an array with inter-finger spacing of between approximately 1.0 μm to approximately 2.0 μm. Likewise the length of the fingers can be determined by the thickness of silicon layer 13 as shown in FIG. 3 . That is because the etching that cuts through this layer terminates at oxide layer 12 . Thus the thickness of the layer 13 corresponds to the length of a finished finger 20 in FIG. 4 .
Fingers 20 can thus be fabricated with different lengths. In a preferred embodiment, the length of fingers 20 is between about 5 microns to about 21 microns. It is preferred to design a finger with dimensions and spacing so as to achieve a desired capacitance for the array. The capacitance is related to the area between the fingers. Thus, to achieve a given area between fingers, an increase in the height of the finger dimension can lead to a reduction in the number of fingers or the length of the fingers.
At this point, the tungsten coating can be grown on fingers 20 . In a preferred embodiment, the finger array receives the tungsten coating while the hard mask cap 14 remains on the silicon finger. Optionally, the hard mask cap 14 may be removed prior to deposition of the tungsten coating. Techniques known in the semiconductor industry may be used to remove a hard mask cap.
The formation of the tungsten layer preferably takes place by a combination of deposition and growth steps. A first reaction involves the formation of a tungsten seed layer by the silane reduction of tungsten hexafluoride. The seed layer is preferably a layer of tungsten silicide. There follows a growth step involving the continued reduction of tungsten hexafluoride using hydrogen gas. Preferably both process steps follow chemical vapor deposition (CVD) procedures. CVD deposition techniques are well known. The equipment is readily available and reasonably priced. CVD is also preferred for the reason that it provides good coverage of the substrate.
The formation of a tungsten seed layer follows the reaction represented in the following equation:
WF 6 +3SiH 4 →WSi x +SiF 4 +2HF+5H 2
The reaction begins to occur even at moderate temperatures, as low as 90° C. Lower temperature reactions tend to promote formation of alpha phase tungsten, and higher temperature reactions tend to develop beta phase tungsten layers. However, higher temperatures are generally preferred in order to limit the amount of fluorine appearing in the tungsten layer and to speed the reaction. Reactant ratios of WF 6 /SiH 4 also may affect the reaction. Higher silane concentration favors the development of beta phase tungsten layers. In this reaction, a seed layer of tungsten silicide is formed on the silicon finger.
The growth step follows the reaction in the following equation:
WF 6 +3H 2 →W+6HF
The hydrogen reduction results in good coverage with a well-crystalized film. This reaction occurs at a temperature of between approximately 300° C. to approximately 500 C. Deposition rates increase at increased pressure of 10 to 60 Torr. However, lower pressures favor tungsten layers with lower tensile stresses.
The hydrogen reaction is generally not preferred as a mechanism to deposit a seed layer in that the high reactivity of WF 6 with Si can result in excessive Si consumption, encroachment of the Si/SiO 2 interface, and wormhole formations. In contrast the silane reduction reaction generally does not disturb the silicon substrate.
The tungsten deposition involves a temperature dependent chemical reaction. Thus, the deposition may take place at any temperature that promotes the reaction. It is preferred that the reaction take place at approximately 400° C. Alternatively, the reaction may take place at a temperature of between approximately 300° C. to approximately 500° C.
Tungsten depositions are further characterized by good conformality. The thickness of the coating is generally even at differing points of the underlying surface. 0 Preferably the seed layer is coated on all exposed surfaces of the silicon fingers.
Tungsten hexafluoride is a proven and well-characterized source of tungsten. It is a popular tungsten precursor due to its availability with high purity and at low cost. Tungsten hexafluoride is a volatile liquid at room temperature. The vapor may be delivered in the CVD process directly through a metering device. WF 6 will react readily with moisture to produce tungsten oxides and hydrofluoric acid (HF). Thus, it is important to avoid moisture in the mass flow and reaction apparatus. Tungsten hexafluoride reactions produce HF as a byproduct of the reaction. HF is a potentially hazardous material, and good operating procedures should be followed in dealing with this material.
Other reducing agents may also be used with WF 6 . In one embodiment, a dichlorosilane (SiCl 2 H 2 ) is used as a reducing agent. Thus a dichlorosilane reduction may also be used in a reaction step. Combinations of reducing agents, SiCl 2 H 2 and SiH 4 may also be used.
Following the deposition of a seed layer, such as the formation of a layer of tungsten silicide, there preferably takes place a growth step of the tungsten crystal. In one embodiment, the growth step continues in the same CVD chamber in which the seed layer was deposited. The growth step is a continuation of the seed deposition step in that reactants introduced into the chamber are changed, if desired, while other parameters such as temperature, pressure, and flow rates can similarly be modified, if desired. In a preferred embodiment, the reducing agent is changed from a silane to hydrogen as described above.
Both the seed formation and growth steps are selective reactions in that the tungsten will not readily react with the silicon dioxide surfaces. Thus, the tungsten material grows only on the exposed silicon of the finger. When the finger is capped, as with silicon dioxide, growth of the tungsten layer is limited to the walls of the finger.
It will be understood by those skilled in the art that reaction parameters such as time, temperature, and pressure can be varied so as to affect the amount of tungsten that is deposited on the surface of the silicon fingers. The amount of tungsten material corresponds to the thickness of the coating. The thickness of the coating may be set by design requirements, and thus, for varying designs, the thickness of the coating may change.
Additionally, the thickness of the tungsten coating affects the mass of the silicon finger structure. The coating, depending on its microstructure and thickness, further affects the spring constant of the finger. Both mass and spring constant are factors in the sensitivity of the finger. Thus, the tungsten coating can improve the HIA sensitivity. In the application of tungsten-coated silicon finger arrays for use in HIAs it is preferred to provide a coating thickness of approximately 2000 Å.
Without wishing to be bound by any theory, the following theoretical explanation of the way in which tungsten coated fingers operate is offered to further illustrate the invention. The surface of the tungsten coating that is deposited on the silicon surface is characterized by a certain degree of roughness. The tungsten crystal surface is not smooth; rather it displays a series of bumps and general unevenness. An illustration of the tungsten surface on a silicon substrate is shown in FIG. 6 . The rough surface of the tungsten coating results in a decrease of the contact area when neighboring fingers happen to come into contact. The decrease in the contact area also results in a decrease in the potential attractive force between neighboring fingers. Thus, tungsten-coated fingers are less likely to remain attached when they come into contact from incidental bending forces. Rather the spring force within the finger is more likely to overcome any attractive force, and the spring force tends to right the finger by returning it to an original position.
The structure of the silicon fingers, after completion of the tungsten and tungsten silicide layer, is illustrated in FIG. 4 . The tungsten and tungsten silicide layer 16 has been deposited on the side walls of the fingers. The protective cap 14 remains. If desired, tungsten can be deposited on the end walls of the fingers. The end walls are not illustrated in the figure, but correspond to the limit of the finger as it extends in a third dimension out of the page and end to the end of the page. Preferably, end walls are not coated, as they are not contact points between fingers.
If tungsten is deposited on the top of the finger, it can tend to bend the silicon. Tungsten coating on silicon does create a certain level of stressed film on the silicon layer. By balancing the finger, by placing tungsten on opposing sides of the finger, the forces are equalized. However, tungsten on the top of the finger would not be opposed, which could lead to warping or bending of the finger. Thus it is preferred to avoid deposition on the top portion of a finger.
Referring now to FIG. 5 there is shown an array of tungsten-coated silicon fingers after removal of the protective cap. A protective cap is removed by any of the methods known in the art of chip manufacturing. The method chosen depends on the composition of the cap material.
The structure shown in FIG. 5 represents the completion of the coating method. The silicon array may then be processed in a standard manner to develop the desired device, such as an HIA. The aspect ratio of the coated fingers is preferably between about 4 to about 20.
In operation of the coated finger array, the silicon fingers, having increased mass by virtue of the tungsten layer, display improved performance. Increase of the mass of the fingers in the array results in an increase in the sensitivity. The spring constant is the tendency to keep the finger centered. A spring force tends to keep silicon fingers in the center position, the originally fabricated position. An acceleration changes that position. As you go to devices that pick up lower and lower accelerations, the spring constant must be weakened. However, the weakening of the spring constant also weakens the force that tends to keep the fingers vertically arranged on their originally designed position. A weakening allows the fingers to wag, and you get more stiction effects with weaker spring constants.
As described above the tungsten-coated silicon fingers are suitable for use in finger arrays as part of an accelerometer. In particular, the finger array may be used as an acceleration sensor in a highly integrated accelerometer. Additionally, the coated fingers and an array of such may be used as an acceleration sensor for use in a gyroscope.
While at least one exemplary embodiment has been presented in the foregoing detailed description of the invention, it should be appreciated that a vast number of variations exist. It should also be appreciated that the exemplary embodiment or exemplary embodiments are only examples, and are not intended to limit the scope, applicability, or configuration of the invention in any way. Rather, the foregoing detailed description will provide those skilled in the art with a convenient road map for implementing an exemplary embodiment of the invention, it being understood that various changes may be made in the function and arrangement of elements described in an exemplary embodiment without departing from the scope of the invention as set forth in the appended claims. | Methods and apparatus are provided for preparing sensing fingers for use in a highly integrated accelerometer. The method includes steps for forming a tungsten/tungsten silicide coating on a silicon finger. The tungsten/tungsten silicide coating adds mass to the silicon finger. The method includes steps of forming silicon fingers from layers of silicon, oxides, and capping material. The silicon fingers are then exposed to tungsten containing gases under conditions to promote the formation of a tungsten silicide seed layer on the exposed silicon surfaces. The tungsten layer is then grown to a desired thickness through a growth step. The coated silicon fingers display improved resistance to stiction as compared to uncoated silicon fingers. | 2 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The present application is a continuation of PCT/EP2014/002669 filed on Oct. 1, 2014, which is based upon and claims the benefit to DE 10 2013 220 945.2 filed on Oct. 16, 2013, the entire contents of each of which are incorporated herein by reference.
BACKGROUND
[0002] 1. Field
[0003] The present application relates to an endoscope, in particular a video endoscope, having an adjustable viewing direction at a viewing angle, said endoscope comprising an endoscope shaft having a longitudinal axis, wherein the endoscope shaft has a distal viewing window, wherein a movable optical device for capturing objects is provided in the endoscope shaft, preferably at the proximal end.
[0004] 2. Prior Art
[0005] Endoscopes, and in particular video endoscopes, in which the light of a field of operation which is incident at a distal tip of an endoscope shaft of the endoscope is directed through an optical system to one or more image sensors, are known in different embodiments. Thus, endoscopes are available with a forward viewing direction, a so-called 0° viewing direction, or endoscopes are available with a lateral viewing direction, which for example have a lateral viewing direction of 30°, 45°, 70° or the like deviating from the 0° viewing direction. In this case, the aforementioned number of degrees is understood as the angle between the central viewing axis and the longitudinal axis of the endoscope shaft. Moreover, endoscopes or respectively video endoscopes are available with an adjustable lateral viewing direction, in which the viewing angle, i.e. the deviation from the view straight ahead, is adjustable.
[0006] During an adjustment of the viewing angle, therefore, the deviation from the view straight ahead is altered, in particular relative to the longitudinal axis of the endoscope shaft.
[0007] Moreover, an optical system for a video endoscope is disclosed in EP 2 369 395 A1 in which the viewing angle is altered by a prism of a prism unit with three prisms being rotated about an axis of rotation which is located perpendicular or respectively transversely to the longitudinal axis of the endoscope shaft. The two other prisms which, together with the first prism, define the optical beam path, are not rotated therewith so that the reflective surface of the first prism which is rotated, rotates relative to the corresponding reflective surface of the second prism.
[0008] A further endoscope with a variable viewing direction is disclosed in DE 10 2010 028 147 A1.
SUMMARY
[0009] Proceeding from this prior art, an object is to provide an endoscope having an adjustable viewing direction in which, when adjusting the viewing angle, the capture of desired objects and improved focusing of the captured object images are permitted in a simple manner, for different viewing angle settings.
[0010] Such object can be achieved by an endoscope, such as a video endoscope, having an adjustable viewing direction at a viewing angle, said endoscope comprising an endoscope shaft having a longitudinal axis, wherein the endoscope shaft has a distal viewing window, wherein a movable optical device for capturing objects is provided in the endoscope shaft, said endoscope being developed in that a focusing optical unit is arranged between the distal viewing window and the movable optical device, wherein the focal distance of the focusing optical unit can be changed or is changed in dependence on the viewing angle.
[0011] The exemplary embodiments disclosed herein are based on the idea that, by the use of a focusing optical unit having a plurality of focal distances, for example a gradient index lens or optionally a plurality of gradient index lenses or a diffractive and/or refractive optical unit, between the distal viewing window arranged on the end of the endoscope shaft inside the endoscope and an optical device which is movable in the endoscope shaft for capturing light beams and/or objects, the focusing of captured objects is improved, as the focusing optical unit has focal distances which are dependent on the viewing angle(s) of the device for capturing objects. In this case, the focusing optical unit, for example a gradient index lens, is configured such that when changing a viewing angle, for example when using a prism unit with a pivotable prism, the focal distances of the focusing optical unit are varied, whereby, depending on the viewing angle in the endoscope with an adjustable viewing direction, the focusing of the objects is facilitated in a simple manner due to the variable focal distances at different viewing angles. For example, when using at least one gradient index lens for the focusing optical unit, the focusing of the objects is achieved in a simple manner due to the variable refractive index of the gradient index lens.
[0012] As the focusing optical unit is arranged between the distal viewing window of the endoscope shaft and the movable optical device this results in the endoscope shaft having a compact character.
[0013] A focusing optical unit, for example a gradient index lens or a diffractive optical element (DOE), is a translucent element which produces a lens effect, which can be by means of a discontinuous or continuous alteration to the refractive index. In this case, the light beams are deflected and bundled at a focal point in the focusing optical unit at a predetermined viewing angle. When the viewing angle is changed, the light beams are bundled at a different focal point since, due to the focusing which is dependent on the viewing angle, the focusing optical unit has different focal distances at different viewing angles.
[0014] In this case, at least one image sensor can be arranged in the endoscope, for example at the proximal end downstream of the prism unit, wherein a prism of the prism unit arranged distally or altering a viewing angle is rotatable about an axis of rotation transversely to the longitudinal axis of the endoscope shaft. Moreover, the prism unit and the at least one image sensor can be arranged in a hermetically sealed space inside the cladding tube. Moreover, an operating element for adjusting the viewing angle of the rotatable prism can be provided, for example, on a handle of the endoscope.
[0015] The focusing optical unit can be configured such that when altering the viewing direction the focal distance of the focusing optical unit is shortened subject to an increase in the viewing angle, or the focal distance of the focusing optical unit is increased subject to a reduction in the viewing angle.
[0016] In addition, the focusing optical unit can be arranged on the viewing window and/or the focusing optical unit can be adhesively bonded to the viewing window.
[0017] An embodiment includes the focusing optical unit having a gradient index lens and/or a diffractively acting optical body, such as a film, and/or a refractively acting optical body, such as a film.
[0018] In one embodiment, the gradient index lens can be arranged on the distal viewing window of the endoscope shaft.
[0019] In one embodiment, the gradient index lens or the diffractively or refractively acting film can be adhesively bonded onto the viewing window, such as a viewing window made of sapphire.
[0020] The refractive index of a gradient index lens provided as a focusing optical unit can vary transversely to the optical axis of the lens, whereby the gradient index lens can be of compact construction and produced with a very small diameter.
[0021] Moreover, the gradient index lenses can be focusing optical units, in that the lens length is adjustable in a variable manner, wherein it is possible that the focal distance and the operating distance may be brought very close to the ends of the gradient index lenses. Moreover, in the gradient index lens, the refractive index can be designed to be different or respectively variable transversely to the optical axis of a lens. By means of the variable refractive index transversely to the optical axis a lens effect is produced so that when light beams pass through the gradient index lens the light beams are bundled or respectively focused at a focal point located in the vicinity of the gradient index lens.
[0022] By means of the arrangement of the focusing optical unit, the focal distances thereof varying depending on the viewing angle of the endoscope, between the distal viewing window and the movable optical device in the endoscope shaft, the focusing of the incident light beams from the objects and thus the optical capture of desired objects can be improved.
[0023] Moreover, in one embodiment, the optical device can be movably arranged in the direction of the longitudinal axis of the endoscope shaft and/or transversely to the longitudinal axis of the endoscope shaft. If, for example, the optical device is configured as a prism unit, the prism unit may be rotated about the longitudinal axis of the endoscope shaft. Moreover, a pivotable prism can be provided in the prism unit, said pivotable prism being pivotable about an axis which can be oriented transversely or respectively perpendicular to the longitudinal axis of the endoscope shaft.
[0024] By the pivoting of a prism, it is possible to alter the viewing direction relative to the longitudinal axis of the endoscope shaft.
[0025] The optical device can be configured as a prism unit, wherein the prism unit as a movable unit has at least one prism which is pivotable about a pivot axis.
[0026] Moreover, the optical device can be configured as an optical image sensor unit, the light beams incident from an object through the viewing window being captured thereby. The image sensor unit can be a CCD camera.
[0027] Moreover, the focusing optical unit can be configured such that the focusing optical unit has a predetermined freeform surface. As a result, it is possible that a diffractive or refractive film or respectively a diffractive optical element (DOE) is able to be produced as a focusing optical unit, wherein the film or the diffractive optical element (DOE) is arranged or respectively adhesively bonded on the inside, such as on a distal viewing window configured as a sapphire dome.
[0028] Furthermore, the focusing optical unit can be produced from plastics material. As a result, diffractive optical elements (DOE) or gradient index lenses can be produced to be of compact construction and in a simple manner.
[0029] Moreover, a focusing optical unit can be used in an endoscope, such as a video endoscope, such as for surgical investigations, wherein the endoscope or respectively video endoscope can be configured as described above.
[0030] Further features are revealed from the description of embodiments together with the claims and accompanying drawings. Embodiments may be fulfilled by individual features or a combination of several features.
BRIEF DESCRIPTION OF THE DRAWINGS
[0031] The embodiments are described hereinafter without limiting the general inventive idea using such exemplary embodiments with reference to the drawings, wherein with regard to all of the details not described in more detail in the text, reference is expressly made to the drawings, in which:
[0032] FIG. 1 illustrates a schematic perspective view of a video endoscope,
[0033] FIG. 2 illustrates a schematic side view of a prism unit at the distal tip of an endoscope shaft,
[0034] FIG. 3 illustrates a schematic plan view of the prism unit of FIG. 2 ,
[0035] FIG. 4 illustrates a cross section through the distal tip of an endoscope shaft according to a further exemplary embodiment.
[0036] In the drawings in each case the same or similar elements and/or parts are provided with the same reference numerals, so that in each case a further image is dispensed with.
DETAILED DESCRIPTION
[0037] FIG. 1 shows a schematic perspective view of a video endoscope 1 having a proximal handle 2 and a rigid endoscope shaft 3 . A viewing window 5 is arranged at the distal tip 4 of the endoscope shaft 3 , a distal portion 6 of the endoscope shaft 3 being arranged to the rear of said viewing window, said distal portion having a prism unit, not shown, and an image sensor unit, not shown.
[0038] The viewing window 5 at the distal tip 4 is curved and of asymmetrical design. Thus the viewing window 5 is configured to assist a variable lateral viewing angle. An alteration to the viewing direction, i.e. an alteration to the azimuth angle about the longitudinal axis of the endoscope shaft 3 , is effected by a rotation of the handle 2 about the central axis of rotation or respectively longitudinal axis of the endoscope shaft 3 . The cladding tube of the endoscope shaft 3 is connected to the handle 2 . The prism unit, not shown, is also rotated at the distal tip 4 by the rotation of the handle 2 . In one embodiment, the viewing window is configured as a sapphire dome.
[0039] The handle 2 has a first operating element configured as a rotary wheel 7 and a second operating element configured as a sliding switch 8 . For maintaining the horizontal position of the image shown, the rotary wheel 7 is secured during a rotation of the handle 2 . As a result, the image sensor in the inside of the endoscope shaft 3 does not perform the movement therewith.
[0040] In order to alter the viewing angle, i.e. the deviation of the viewing direction from the view straight ahead, the sliding switch 8 is moved. Moving the sliding switch 8 to the distal end, for example, leads to an increase in the viewing angle, and a return of the sliding switch 8 to the proximal end in this case causes the viewing angle to be reduced to the view straight ahead. The actuation of the sliding switch 8 causes a rotation of the image sensor, in order to maintain the horizontal position of the image shown, even with a rotation of the prism units relative to one another.
[0041] In FIG. 2 , the distal end of the endoscope shaft 3 with a prism unit 10 is shown schematically from the side. On the left-hand side of the image, light of a central beam path 21 which is shown as a dashed-dotted line enters a viewing window 5 of the endoscope shaft and passes through a gradient index lens 22 arranged on the viewing window 5 into a first distal prism 12 of the prism unit 10 . The gradient index lens 22 is arranged or adhesively bonded in the endoscope shaft 3 on the inside, for example by being adhesively bonded to the viewing window 5 .
[0042] By means of the gradient index lens 22 which is arranged in contact with the distal viewing window 5 , the incident light beams are focused due to the different refractive indices of the gradient index lens 22 which are variable, depending on the distance from the optical axis.
[0043] By means of an entry lens 11 arranged on the prism 12 , the incident light beams are focused immediately downstream of the gradient index lens 22 due to the refractive index, which changes depending on the distance from the optical axis, after the passage of the light beams therethrough. The light is incident on the reflective surface 13 of the prism 12 and is reflected downwardly in the direction of a second prism 14 of the prism unit 10 and a reflective surface 15 of the second prism 14 .
[0044] The reflective surface 15 of the prism 14 has an acute angle to the lower face 17 of the second prism 14 so that the central beam path is initially reflected on a central portion of the lower face 17 , which is also reflective, and from there to a second reflective surface 16 of the second prism 14 . This second reflective surface 16 also has an acute angle to the lower face 17 , so that the central beam path in turn is reflected upwardly (axis B). Here the light is incident in a third prism 18 of the prism unit 10 with a reflective surface 19 , the light of the central beam path 21 in turn being reflected centrally therethrough in a direction parallel to the longitudinal axis of the endoscope shaft 3 and emerging from the prism unit 10 through an exit lens 20 .
[0045] Moreover, a part of an optical fiber bundle 25 is shown above the prism unit 10 , light being conducted thereby from the proximal tip to the distal tip in order to illuminate an otherwise unilluminated field of operation.
[0046] The first prism 12 of the prism unit 10 is rotated or respectively pivoted about the perpendicular axis A, which is also denoted as the pivot axis, in order to adjust the lateral viewing angle. As a result, the reflective surface 13 of the first prism 12 and the reflective surface 15 of the fixed prism 14 of the prism unit 10 rotate relative to one another so that the horizontal position of the image, which is forwarded to the proximal end, is altered with a rotation of the first pivotable prism 12 about the axis A. This has to be compensated by a rotation of the image sensor or the image sensors.
[0047] In FIG. 3 the prism unit 10 of FIG. 2 is shown in a schematic plan view. The first prism 12 is arranged in a 0° viewing direction. The first prism 12 is pivotably mounted together with the entry lens 11 about the pivot axis A. In this case, the overlapping region between the reflective surfaces 13 of the first prism 12 and 15 of the second prism 14 is rotated. With a rotational or respectively pivoting movement of the first prism 12 the horizontal line is rotated, as is to be described below. If the prism unit 10 is arranged such that the axis of rotation A in FIG. 2 is arranged upwardly, i.e. perpendicular to the horizontal, which is an imaginary horizontal line, this horizontal line represents a line which is level with the reflective surface 13 of the prism 12 . With a rotation of the first prism 12 about the axis of rotation this is independent of the angle of rotation.
[0048] In FIG. 4 , a further exemplary embodiment of the arrangement of a gradient index lens 22 between the distal viewing window 5 and the prism unit 10 is shown schematically in cross section. According to the exemplary embodiment in FIG. 4 , the gradient index lens 22 is arranged in the endoscope shaft 3 between the prism unit 10 and the distal viewing window 5 , wherein the gradient index lens 22 in this case is not in contact with the viewing window 5 or with the entry lens 11 of the prism 12 of the prism unit 10 . For the arrangement of the gradient index lens 22 between the viewing window 5 and the prism unit 10 a mount 23 is provided so that the gradient index lens 22 is enclosed in the endoscope shaft 3 .
[0049] Within the scope of the invention according to an alternative (not shown here), instead of a gradient index lens or the gradient index lens 22 it is also provided to arrange a focusing optical unit with a diffractive and/or refractive property or action, for example a diffractive film and/or refractive film, between the viewing window 5 and the prism unit 10 . Moreover, corresponding combinations may be also implemented.
[0050] While there has been shown and described what is considered to be preferred embodiments of the invention, it will, of course, be understood that various modifications and changes in form or detail could readily be made without departing from the spirit of the invention. It is therefore intended that the invention be not limited to the exact forms described and illustrated, but should be constructed to cover all modifications that may fall within the scope of the appended claims.
LIST OF REFERENCE NUMERALS
[0051] 1 Video endoscope
[0052] 2 Handle
[0053] 3 Endoscope shaft
[0054] 4 Distal tip
[0055] 5 Viewing window
[0056] 6 Distal portion
[0057] 7 Rotary wheel
[0058] 8 Sliding switch
[0059] 9 Cladding tube
[0060] 10 Prism unit
[0061] 11 Entry lens
[0062] 12 First prism
[0063] 13 Reflective surface
[0064] 14 Second prism
[0065] 15 , 16 Reflective surface
[0066] 17 Lower face
[0067] 18 Third prism
[0068] 19 Reflective surface
[0069] 20 Exit lens
[0070] 21 Central beam path
[0071] 22 Gradient index lens
[0072] 23 Mount
[0073] 25 Optical fiber bundle | An endoscope having an adjustable viewing direction at a viewing angle, the endoscope including: an endoscope shaft having a longitudinal axis, wherein the endoscope shaft has a distal viewing window, a movable optical device for capturing objects provided in the endoscope shaft, and a focusing optical unit arranged between a distal viewing window and the movable optical device, wherein a focal distance of the focusing optical unit is changed in dependence on the viewing angle. | 0 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority from U.S. Provisional Patent Application No. 60/795,718 filed Apr. 29, 2006, which is hereby incorporated by reference.
BACKGROUND
[0002] The present invention relates to a spinal fixation system connector for maintaining predetermined positions of vertebrae in the spinal column of a patient. More particularly, the present invention relates to a component of a spinal fixation system for connecting a first spinal linkage member (e.g., a rod) to a second spinal linkage member. The component allows angles between the connected spinal linkage members to vary.
[0003] Spinal fixation systems are commonly used to align, adjust and/or stabilize portions of a spinal column of a patient. These systems frequently include vertebral anchors such as pins, bolts, screws, hooks and/or cables that attach to vertebrae in the spinal column. The spinal linkage members can be connected to the anchors to maintain the relative positions of the corresponding vertebrae. Thus, the members maintain the spacing and alignment of the connected vertebrae. To provide desired alignment across several levels of the spine, more than one spinal linkage member may be used and connected by one or more fixation system connectors.
[0004] Frequently, the connector is used to connect portions of two linkage members positioned side-by-side. The connector spans between linkage members to maintain the positions of the members relative to each other. Frequently, the portions of the spinal linkage members connected by the connector are not parallel. Instead, the members are non-parallel so they are oriented at various angles and in various positions due to the anatomical structure of the spine and alignment desired by the surgeon.
[0005] Many conventional connectors are designed to accommodate linkage members aligned at a particular angle. Variations in angular alignment from the particular angle accepted by the linkage may make it difficult to optimally align members using the conventional connectors. When there is a difference between the desired alignment and the fixed alignment of conventional connectors, the linkage members must be deformed. Deforming members may weaken portions of the spinal fixation system or cause the vertebrae to fail.
BRIEF SUMMARY
[0006] The present invention relates to a spinal fixation system connector for maintaining a predetermined position of a first spinal linkage member fastened to vertebrae of a patient to a second spinal linkage member fastened to vertebrae of the patient. The connector comprises a body having a first opening extending through the body along a first axis. The first opening is sized and shaped for receiving the first spinal linkage member. The connector also includes a second opening extending through the body along a second axis. The second opening is sized and shaped for receiving the second spinal linkage member. Further, the connector includes a first fastener mounted on the body for fastening the first spinal linkage member in the first opening of the body and a second fastener mounted on the body for fastening the second spinal linkage member in the second opening of the body. Prior to the first fastener fastening the first spinal linkage member in the first opening of the body and the second fastener fastening the second spinal linkage member in the second opening of the body, the body is manipulatable to adjust an angle between the first axis and the second axis. When the first fastener fastens the first spinal linkage member in the first opening of the body and the second fastener fastens the second spinal linkage member in the second opening of the body, the angle between the first axis and the second axis is fixed.
[0007] In another aspect, the invention includes a surgical system for maintaining a predetermined position of vertebrae of a patient. The system comprises a first elongate spinal linkage member, a first anchor for attaching the first member to a first vertebra, a second elongate spinal linkage member, a second anchor for attaching the second member to a second vertebra, and a connector. The connector includes a body having a first opening extending through the body along a first axis. The first opening is sized and shaped for receiving the first spinal linkage member. In addition, the connector includes a second opening extending through the body along a second axis. The second opening is sized and shaped for receiving the second spinal linkage member. The system also comprises a first fastener mounted on the body for fastening the first spinal linkage member in the first opening of the body and a second fastener mounted on the body for fastening the second spinal linkage member in the second opening of the body. Prior to the first fastener fastening the first spinal linkage member in the first opening of the body and the second fastener fastening the second spinal linkage member in the second opening of the body, the body is manipulatable to adjust an angle between the first axis and the second axis. When the first fastener fastens the first spinal linkage member in the first opening of the body and the second fastener fastens the second spinal linkage member in the second opening of the body, the angle between the first axis and the second axis is fixed.
[0008] The invention also includes a method of connecting a first spinal linkage member fastened to vertebrae of a patient to a second spinal linkage member fastened to vertebrae of the patient and maintaining a predetermined position of the first spinal linkage member to the second spinal linkage member. The method comprises inserting a portion of the first spinal linkage member into a first opening in the connector and inserting a portion of the second spinal linkage member into a second opening in the connector. The connector is manipulated so the first spinal linkage member and the second spinal linkage member are aligned in a predetermined orientation with respect to one another. The method also includes fastening the connector to the first spinal linkage member and fastening the connector to the second spinal linkage member.
[0009] Other aspects of the present invention will be in part apparent and in part pointed out hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a perspective of a connector of one embodiment of the present invention having a closed passage including a variable angle mechanism for receiving a linkage member and an open lateral groove to receive a linkage member.
[0011] FIG. 2 is a top plan of the connector shown in FIG. 1 connecting two linkage members.
[0012] FIG. 3 is a perspective of the connector connecting two linkage members.
[0013] FIG. 4 is a side elevation of the connector shown in FIG. 1 .
[0014] FIG. 5 is a rear elevation of the connector connected two linkage members.
[0015] FIG. 6 is a top plan of a connector of a second embodiment of the present invention having a closed passage including a variable angle mechanism for receiving a linkage member and an open lateral groove to receive a linkage member.
[0016] FIG. 7 is a rear elevation of the connector of the second embodiment connecting two linkage members.
[0017] Corresponding reference characters indicate corresponding parts throughout the several views of the drawings. Directional terms such as top and side are used for convenience and correspond only to one orientation of the connector.
DETAILED DESCRIPTION
[0018] Referring now to the drawings and in particular FIG. 1 , a first embodiment of a connector of the present invention is designated in its entirety by the reference number 10 . The connector 10 includes a closed passage or opening 12 for receiving a first spinal linkage member (designated 20 in FIG. 2 ) and an open lateral groove or slot or opening 14 for receiving a second spinal linkage member (designated 22 in FIG. 2 ). The connector 10 may be used adjacent all areas of the spine.
[0019] FIG. 2 illustrates a top plan of the connector 10 . The connector 10 includes a closed passage 12 having a variable angle mechanism, generally designated by 24 , for receiving a spinal linkage member (e.g., member 20 ) and an open lateral groove 14 for receiving another linkage member (e.g., member 22 ) according to one embodiment of the invention. The connector 10 has a body 30 having an opening 32 sized and shaped for receiving the variable angle mechanism 24 . The mechanism 24 includes a housing 34 that is pivotally mounted in the opening 32 on axles formed by pins 36 rotatably mounted in recesses 38 in the body 30 . The housing 34 has the closed passage 12 through which the spinal linkage member 20 is passed. A threaded hole 40 extends through the housing 34 intersecting the passage 12 generally perpendicular to the passage. A fastener such as a setscrew 42 is inserted into the threaded hole 40 for securing the connector 10 to the spinal linkage member 20 received in the closed passage 12 . As shown in FIG. 3 , the connector body 30 includes an opening 44 for accessing the fastener 42 to tighten the fastener once the connector 10 is in place.
[0020] As illustrated in FIGS. 2 and 4 , at least one surface 50 of the housing 34 and a corresponding surface 52 of the connector body 30 are spherical. Further, the pins 36 are smaller (both shorter and narrower) than the recesses 38 , allowing the housing 34 to pivot in any direction within the body 30 . The housing 34 includes a slot 54 that extends from the surface 50 to the closed passage 12 . As the fastener 42 is tightened, the linkage member 20 presses against the slot 54 so the slots spreads open. As the slot 54 spreads, the corresponding spherical surfaces 50 , 52 of the housing 34 and body 30 frictionally engage to prevent the housing from moving in the body. Thus, as the fastener 42 is tightened, the spinal linkage member 20 is locked in place in the closed passage 12 and the housing 34 is locked in place in the body 30 .
[0021] The open groove or slot 14 in the body 30 receives the second spinal linkage member 22 . A threaded hole 60 extends through the body 30 and intersects the passage 14 generally perpendicular to the passage. A fastener such as a setscrew 62 is inserted into the threaded hole 60 for securing the connector 10 to the spinal linkage member 22 received in the open groove 14 . In one embodiment, the groove 14 includes a hooked lip 64 which ensures the spinal linkage member 22 is retained in the groove when the fastener 62 is tightened to firmly lock of the member in place in to the body 30 of the connector 10 . Although the slot 14 faces laterally in the illustrated embodiment, those skilled in the art will appreciate that the slot may have alternative orientations without departing from the scope of the present invention.
[0022] FIG. 5 shows the connector 10 with both spinal linkage members 20 , 22 seated in the body 30 . As will be apparent to those skilled in the art, the selectively pivotable nature of the variable angle mechanism 24 allows the spinal linkage members 20 , 22 to be angled relative to each other. Further, once the connector 10 accepts the spinal linkage members 20 , 22 , the fasteners 42 , 62 are tightened to lock the connector in position on the members and the members in position relative to one another.
[0023] FIG. 6 illustrates another embodiment of a connector of the present invention, generally designated in its entirety by the reference number 70 . The connector 70 of the this embodiment includes a body constructed in two pieces 72 , 74 . The first piece 72 includes a closed passage 82 for receiving a first spinal linkage member (designated 20 in FIG. 7 ) and the second piece 74 includes an open lateral groove or slot 84 for receiving a second spinal linkage member (designated 22 in FIG. 7 ). The slot 84 of connector 70 of the second embodiment is substantially identical to the slot 14 of the first embodiment. A threaded hole 90 similar to hole 60 of the first embodiment extends through the piece 74 and intersects the passage 84 generally perpendicular to the passage. A fastener such as a setscrew 92 is inserted into the threaded hole 90 for securing the connector 70 to the spinal linkage member 22 received in the open groove 84 . As the open lateral groove 84 is similar to the slot 14 in the connector 10 of the first embodiment, it will not be described in further detail.
[0024] As further illustrated in FIG. 6 , the second piece 74 includes a post 100 extending generally perpendicular to both the threaded hole 90 and the slot 84 . The first piece 72 has an opening 102 having a shape that complements the post 100 . The post 100 is sized relative to the opening 102 to permit the first piece 72 and second piece 74 to move relative to each other. Although the post 100 and opening 102 may have other shapes without departing from the scope of the present invention, in one embodiment both the post and opening have generally conical shapes. It is envisioned that the post and opening may have generally spherical shapes in an alternate embodiment (not shown). In the illustrated embodiment, both the post 100 and the opening 102 include ridges and grooves to improve gripping between surfaces when they are engaged. In an alternate embodiment (not shown), it is envisioned that the surfaces may have other treatments (e.g., grit blasting or knurling) to improve gripping during engagement.
[0025] A threaded hole 120 extends through the first piece 72 and intersects the closed passage 82 generally perpendicular to the passage. A fastener such as a setscrew 122 is inserted into the threaded hole 120 for securing the first piece 72 to the spinal linkage member 20 received in the closed passage 82 . As the fastener 122 is tightened, the linkage member 20 presses against the post 100 and forces it to seat in the opening 102 . When the post 100 seats in the opening 102 , the corresponding conical surfaces of the post and opening frictionally engage to prevent the first and second pieces 72 , 74 of the connector 70 from moving relative to each other. Thus, as the fastener 122 is tightened, the spinal linkage member 20 is locked in place in the closed passage 82 and the first and second pieces of the connector 70 are locked in place.
[0026] FIG. 7 shows the connector 70 with both spinal linkage members 20 , 22 seated in the body 80 and the halves of the body immobilized relative to each other. As will be apparent to those skilled in the art, the post 100 and opening 102 of the first and second pieces 72 , 74 form a variable angle mechanism 140 of a second embodiment that allows the spinal linkage members 20 , 22 to be angled relative to each other. Further, once the connector 70 accepts the spinal linkage members 20 , 22 , the fasteners 92 , 122 are tightened to lock the connector in position on the members and the members in position relative to one another.
[0027] As will be appreciated by those skilled in the art, the spinal linkage members may extend at any suitable angle within a predetermined range of angles to accommodate a particular configuration of spinal instrumentation and spinal alignment.
[0028] The sizes of the closed passages and the open grooves that accommodate the spinal linkage members are selected so the linkage members can move laterally in the corresponding passage and groove. In one embodiment, the radii of the passages and grooves vary around their circumferences so that the radii at positions opposite the fasteners are approximately equal to or small than those of the linkage members to improve engagement between the connectors and members. One skilled in the art will recognize that the shape and size of the passages and grooves are not limited to the illustrated embodiments, and that any suitable size and/or shape, as well as relative location in the connector is envisioned.
[0029] According to an alternate embodiment, a locking mechanism for securing the position of the rods within the connector may comprise a plurality of setscrews. For example, the locking mechanism may comprise a first screw and a second screw disposed around the closed passage for the first linkage member for locking the connector components together and fixing the angular relation of the spinal linkage member relative to the body.
[0030] The present invention provides an improved connector for a spinal fixation system intended for connecting a first spinal linkage member to a second spinal linkage member. The connector provides an angled or non-parallel connection between the linkage members allowing for desired alignment or angular variation between portions of the spinal fixation system. The connector may include a first passage for receiving a portion of the first spinal linkage member, and a groove or slot for receiving a portion of the second spinal linkage member. Thus, the orientation of the first linkage member may vary relative to the second linkage member. The connector may comprise a variable connection mechanism functionally separating the passage of the first member and the groove of the second member. The variable connection mechanism may include a swivel type joint and surface treatments to reliably lock angular offset between portions of the connector and thus the angle between the linkage members.
[0031] The invention will be described relative to illustrative embodiments, though one skilled in the art will recognize that the invention is not limited to the described embodiments. While the connector may be primarily applied in spinal surgery, the connector may also be employed to couple any type of components of an implant system. The material composition of the connector and its components may be formed of any suitable bio-compatible material, including, but not limited to stainless steel, titanium, nitinol, metal alloys, plastic, polymers, carbon based materials, ceramics, and mixtures or combinations thereof.
[0032] When introducing elements of the present invention or the preferred embodiment(s) thereof, the articles “a”, “an”, “the” and “said” are intended to mean that there are one or more of the elements. The terms “comprising”, “including” and “having” are intended to be inclusive and mean that there may be additional elements other than the listed elements.
[0033] As various changes could be made in the above constructions without departing from the scope of the invention, it is intended that all matter contained in the above description or shown in the accompanying drawings shall be interpreted as illustrative and not in a limiting sense. | A spinal fixation system connector for maintaining a predetermined positions of a spinal linkage members fastened to vertebrae of a patient. The connector includes a body having first and second openings extending along first and second axes, respectively. The connector includes a first fastener for fastening the first member in the first opening and a second fastener for fastening the second member in the second opening. Prior to the first fastener fastening the first spinal linkage member in the first opening and the second fastener fastening the second spinal linkage member in the second opening, the body is manipulatable to adjust an angle between the first axis and the second axis. When the first fastener fastens the first member in the first opening and the second fastener fastens the second member in the second opening, the angle between the first axis and the second axis is fixed. | 0 |
BACKGROUND OF THE INVENTION
[0001] The present invention relates to downhole fishing and drilling operations, or removing obstructions to a drilling line when such a line becomes lodged or otherwise stuck in a well bore. Consequences of failure to remove the obstruction can be failure of the well to produce at all or in part, also, current methods of removing obstructions can result in failure to loosen the work string, both of which result in having to relocate the drilling operation, which necessarily involves lost time and money.
[0002] This problem can be overcome, as it is now, by various devices which exert pressure or mechanical energy on the work string in an attempt to dislodge it. These tools are generally large, complex and expensive, and many are not easily configured to apply varying amounts of force to the work string, which can result in imprecise application of energy to the work string. This, in turn, can break or otherwise damage the work string, resulting in a requisite move of a project, or at the very least, lost time and energy in repairing the work string.
[0003] The current invention fills the existing gap in technology by providing a relatively small, simple, adjustable tool which can be easily transported and implemented and be tailored to specific applications.
[0004] It is known in the art to apply force to dislodge a work string, however the current devices in this field do not offer the unique combination of the small, simple and configurable characteristics inherent in the configuration presented herein.
OBJECTS OF THE INVENTION
[0005] One object of this invention is to provide a configurable device which can apply specific amounts of pressure to a work string.
[0006] Another object of the invention is to provide a device that is small and easily transported.
[0007] Still another object of the invention is to provide a device that is able to shield an adjustment mechanism with a sleeve.
[0008] Other objects and advantages of this invention shall become apparent from the ensuing descriptions of the invention.
SUMMARY OF THE INVENTION
[0009] According to the present invention, the invention is a downhole tool for manipulating a work string which is easily configured to deliver a specific amount of force to the work string in a small and simple apparatus.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The accompanying drawings illustrate an embodiment of this invention. However, it is to be understood that this embodiment is intended to be neither exhaustive, nor limiting of the invention. They are but examples of some of the forms in which the invention may be practiced.
[0011] [0011]FIG. 1A shows a side view of the top half of the jarring tool, partially disassembled.
[0012] [0012]FIG. 1B shows a side view of the bottom half of the jarring tool, partially disassembled.
[0013] [0013]FIG. 2A shows a cutaway view of the top half of the jarring tool.
[0014] [0014]FIG. 2B shows a cutaway view of the bottom half of the jarring tool.
[0015] [0015]FIG. 3 shows a top view of the aligning collar.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0016] Without any intent to limit the scope of this invention, reference is made to the figures in describing the various embodiments of the invention. Referring to FIGS. 1 through 3, line downhole jarring tool 100 is pictured.
[0017] Jarring tool 100 has a hammer mandrel 101 near the top end of jarring tool 100 which is formed with shaft 113 extending from the bottom end of hammer mandrel 101 . Shaft 113 can be formed such that a portion of shaft 113 has beveled sides, providing a flat surface that permits the shaft to be turned with a wrench, as well as forming a “keyed” relationship with the square opening 122 of retaining mandrel 102 's aligning collar 121 . This “keyed” relationship prevents relational torquing between shaft 113 and retaining mandrel 102 . This arrangement also precludes the need for aligning screws or other components, which detract from the simplicity and effectiveness of a tool.
[0018] At the end of shaft 113 , shaft 113 forms a releasable bolt 103 which can be shaped conically as pictured, but could conceivably take various shapes, so long as releasable bolt 103 could be grasped and retained by another device, as explained in further detail below. The conical or “spear” shape of releasable bolt 103 also facilitates the re-entry of releasable bolt 103 into collet 105 , explained in greater detail below.
[0019] Retaining mandrel 102 surrounds shaft 113 , and is usually threaded at one end to receive firing mandrel 104 which lies below it on jarring tool 100 . Firing mandrel 104 is generally cylindrical in shape, and having unlatching recess 117 along firing mandrel's 104 inner diameter, which is shaped to accommodate collet 105 as outlined below. Releasable bolt 103 also prevents shaft 113 from disengaging retaining mandrel 102 by virtue of releasable bolt's 103 size being larger than that of the edge 116 of retaining mandrel 102 .
[0020] Collet 105 is attached to a kinetic energy shaft 118 toward the top end of jarring tool 100 . Collet 105 can have longitudinal slits 114 around its body, such that the overall diameter of collet 105 can be permitted to increase by radially expanding or separating slits 114 . The top end 115 of collet 105 should also be configured to be of larger diameter than the remainder of collet 105 to create a section that can enter either latching recess 117 or unlatching recess 123 of firing mandrel 104 permitting collet 105 to expand. This will be explained in greater detail below.
[0021] Positioned between collet 105 and middle joint 107 is reloading mechanism 106 , generally a spring or spring-type device, which is held in place between collet 105 and middle joint 107 . It is positioned such that pressure is exerted upwardly on collet 105 and downwardly on middle joint 107 .
[0022] Kinetic energy store 109 is positioned around kinetic energy shaft 118 , and can be any mechanical kinetic energy store, like a Belleville washer stack or a spring. Kinetic energy store 109 is usually a Belleville washer stack, which is generally an assemblage of concave washers stacked end to end such that resistance and linear energy is built up when the kinetic energy store 109 is compressed.
[0023] At the base of kinetic energy shaft 118 is threaded or otherwise attached adjuster collar 110 . This is configured such that as adjuster collar 110 is threaded onto the bottom end of kinetic energy shaft 118 , such that as adjuster collar 110 is turned up the tool, compression is naturally increased on the kinetic energy store 109 , and thus upward resistance is increased.
[0024] There is also in some exemplary forms of the invention threaded hole 119 drilled in kinetic energy shaft 118 , generally perpendicular to the lateral axis of jarring tool 100 . This provides for setscrew 120 which, when engaged in threaded hole 119 , prevents adjuster collar 110 from turning about its axis.
[0025] Surrounding and encasing kinetic energy shaft 118 and kinetic energy store 109 is bottom mandrel 112 . Integrated in bottom mandrel 112 is adjuster collar guard 108 . Collar guard 108 has opening 111 which is essentially a window used to access adjuster collar 110 . Collar guard 108 is able to be turned about the axis of the tool, such that opening 111 only reveals a small portion of the surface beneath it. When properly actuated, however, opening 111 of collar guard 108 reveals adjuster collar 110 so that it may be accessed, and thus adjusted via various means. If collar guard 108 is then turned further, it effectively conceals adjuster collar 108 , thus preventing contaminants from entering, or from accidental adjustment of the components.
[0026] Joining bottom mandrel 112 to firing mandrel 104 is middle joint 107 , which also houses a portion of kinetic energy shaft 118 .
[0027] Each of the parts which lie along the central axis, if they are to be used in an application which requires electrical, data or other connections at the base of the tool can have a bore drilled parallel to this axis to permit runs of electrical or other wire through the center of jarring tool 100 . In such an application, parts along the center portion of the tool, such as shaft 113 , releasable bolt 103 , hammer mandrel 101 , collet 105 and kinetic energy shaft 118 have a bore in the center of them, permitting a wire or other ductile compound to be threaded through them, and thus, the entire tool.
[0028] In operation, line downhole jarring tool 100 will be attached on its top and bottom ends to the work string. Jarring tool 100 will be likely initially “set,” whereby releasable bolt 103 is inserted into the center of collet 105 . This “setting” procedure is accomplished by moving shaft 113 , and thus bolt 103 , toward the bottom end of jarring tool 100 . Bolt will press against collet 105 , pushing it down whereby the top 115 of collet 105 will enter latching recess 117 , and bolt 103 will enter collet 105 . In this way, bolt 103 becomes mechanically coupled with collet 105 , and is ready for the impact stroke of jarring tool 100 .
[0029] Adjuster collar guard 108 will be rotated about the axis of jarring tool 100 so that opening 111 will permit access to setscrew 120 , such that setscrew 120 may be removed, in turn permitting adjuster collar 110 to be threaded up or down, providing a corresponding increase or decrease in the tension stored in kinetic energy store 109 . In an exemplary embodiment, each full turn of adjuster collar 110 will raise or lower the pressure stored in kinetic energy store 109 by one hundred (100) pounds. Setscrew 120 can then be replaced, effectively locking adjuster collar 110 in place. Adjuster collar guard 108 can then be rotated back around to re-conceal setscrew 120 and related parts of adjuster collar 110 . Naturally, the setting need not be one hundred pounds, but is helpful to the operator to be in whole number increments, as to provide easy administration of pressure changes.
[0030] When an obstruction is encountered, or the drill string otherwise needs to be loosened, force will be applied to jarring tool 100 , drawing back on the end of jarring tool 100 . When this force is applied to hammer mandrel 101 , shaft 113 is also drawn upward by virtue of its mechanical connection to hammer mandrel 101 . Releasable bolt 103 will similarly be drawn back, and move with it collet 105 and thus kinetic energy shaft 118 .
[0031] As the force is applied, kinetic energy will continue to build as a result of the compression of kinetic energy store 109 under the force applied to hammer mandrel 101 . As this force increases, hammer mandrel 101 , shaft 113 , releasable bolt 103 , collet 105 , and kinetic energy shaft 118 all move toward the top end of jarring tool 100 until collet's 105 top end 115 slides into unlatching recess 117 , at which point longitudinal slits 114 expand, and releasable bolt 103 is released.
[0032] As a result of this, the full store of kinetic energy in kinetic energy store 109 is exerted up and away, such that releasable bolt 103 travels quickly up within retaining mandrel 102 until it strikes edge 116 of retaining mandrel 102 , delivering the upward stroke, which, by design, helps to loosen the work string.
[0033] At this time, the previous force exerted upon tool should be reversed, mechanically or otherwise, such that releasable bolt 103 will be inserted back into collet 105 . As bolt 103 is inserted into collet 105 , collet 105 is pushed back beyond unlatching recess 117 such that slits 114 are compressed, once again holding and retaining releasable bolt 103 within the confines of collet 105 . This cycle is thus repeated to achieve the desired hammering effect to loosen or otherwise manipulate the work string.
[0034] Although only a few exemplary embodiments of this invention have been described in detail above, those skilled in the art will readily appreciate that many modifications are possible in the exemplary embodiments without materially departing from the novel teachings and advantages of this invention. Accordingly, all such modifications are intended to be included within the scope of this invention as defined in the following claims. | According to the present invention, the line downhole jarring tool is a downhole tool for manipulating a work string which is easily configured to deliver a specific amount of force to the work string in a small and simple apparatus. | 4 |
RELATED APPLICATIONS
This application is a national phase application claiming benefit of priority under 35 U.S.C. §371 to Patent Convention Treaty (PCT) International Application Serial No: PCT/US2013/051414, filed Jul. 21, 2013, which claims benefit of priority to U.S. Provisional Patent Application Ser. No. (“USSN”) 61/674,298, filed Jul. 21, 2012. The aforementioned applications are expressly incorporated herein by reference in their entirety and for all purposes.
TECHNICAL FIELD
This invention generally relates to inorganic chemistry and environmental pollution control. In particular, in alternative embodiments, the invention provides processes and methods for the recovery of silicofluorides and phosphoric acid from phosphoric acid-generating plant facilities, for example, from contaminated wastewater systems associated with a phosphoric acid-generating facility, e.g., gypsum and cooling ponds, or recovery from vapors evolved from specific process steps to barometric condensers. In alternative embodiments, the invention provides a subsequent separation of the silica and fluoride to produce purified fluoride and silica products.
BACKGROUND
In phosphate rock sources there are naturally occurring fluoride contaminants that dissolve with the phosphate materials during the reaction of the phosphate rock with an acid. In most of the phosphoric acid processes, sulfuric acid is used to acidulate the rock, which results in the production of phosphoric acid and by-product gypsum (calcium sulfate dihydrate, with the chemical formula CaSO 4 .2H 2 O). This is generally referred to as the “wet” phosphoric acid process.
In the acidulation stage, as the rock is reacted with the sulfuric acid, the fluoride contained in the rock also dissolves into the acid phase. Once the fluoride is in solution it has a relatively high vapor pressure, and a portion of the fluoride will evolve from the acid/gypsum slurry in the form of a silico-fluoride vapor, primarily silicon tetrafluoride (SiF 4 ) and/or hydrofluosilicic acid (H 2 SiF 6 ), along with some hydrofluoric acid (HF). Also during the reaction of phosphate rock and sulfuric acid there is heat generated as a result of the reaction.
To maintain the temperature in the reaction system many plants typically use a method referred to as flash cooling to remove heat from the phosphoric acid/gypsum. In this approach the slurry is pumped into a vessel that is under vacuum, and at this reduced pressure the slurry will begin to boil and evaporate water plus other vapors from the slurry, which in turn results in the cooling of the slurry.
The vacuum for the cooler is generally supplied via the use of a so-called barometric condenser, where water (typically from a recirculating cooling pond system) is pumped into a spray-tower-like vessel and the condensing of the water vapor exiting the flash cooler generates a vacuum. This technique is well established in the industry, and thus results in fluoride species from the plant generally ending up in, and contaminating, the associated pond wastewater systems.
In many facilities, a large cooling pond is used to provide the water for the various barometric condensers that are used within the phosphoric acid process. The water leaving the barometric condensers is now warm and the use of a large area cooling pond allows for the cooling of the used water, primarily via evaporation of some of the water in the ponds, and the eventual recycle of the cooled water back to the barometric condensers.
As a result of the fluoride species vapor pressure in the slurry, a portion of the fluoride species will evolve with the water vapor in the flash cooler and combine with the water used to provide vacuum for the cooler. The used barometric condenser water will then begin to accumulate the fluoride species, along with other contaminants such as entrained phosphoric acid. Over a period of time, the fluoride species concentration in the pond water will tend to build up to somewhat of a pseudo-steady-state value.
In most operations, the phosphoric acid produced in the digestion system is evaporated to produce a higher concentration material for use in subsequent fertilizer manufacture or production of merchant grade acid (MGA). These systems are generally operated under vacuum which is supplied via direct contact barometric condensers. As in the flash cooling case, fluoride vapors are evolved during the evaporation step and are collected in the recirculated water used for the condenser. The cool water supplying the barometric condenser heats up as it condenses both water vapor and the accompanying fluoride vapors. This warm water is returned to the pond system for cooling.
Additional fluoride vapors are also emitted from other sections of the process and are typically recovered via the use of a scrubber system, where the vapors are contacted with pond water to “scrub” the contaminants from the vapor stream. Typically, the same water that is used for the barometric condensers in the plant is used for the various scrubbers used for general emissions.
After production of the phosphoric acid, the mixture of gypsum (CaSO 4 .2H 2 O) solids and phosphoric acid (P 2 O 5 ) solution is filtered to separate the phosphoric acid from the gypsum. The gypsum is then washed with water, typically from the pond water system, and the wash carried out in a counter-current fashion, with the resulting phosphoric acid (P 2 O 5 )-enriched water added into the phosphate rock/sulfuric acid reaction or digestion circuit. Even though the counter-current washing is efficient, there is still some phosphoric acid lost as a result of entrainment of dilute solution in the moist gypsum cake solids. While the amount is generally small, with the scale of modern phosphoric acid plants, this small loss can still represent an appreciable cost to the operation.
The gypsum by-product is generally discharged into so-called “gypsum ponds”. These ponds are relative large since there are roughly 5.5 tons of gypsum produced for every ton of phosphoric acid (P 2 O 5 ) produced. Also, as the gypsum “stacks” up in the pond it also entrains some of the contaminated water within the gypsum material itself and acts as somewhat of a storage pile for soluble fluoride species and dilute phosphoric acid that accumulate in the pond water. As a result of this “stacking” effect, the gypsum stack acts as an accumulator of the various contaminants, e.g. fluoride species, dissolved phosphoric acid (P 2 O 5 ), etc. Due to the ratio of the gypsum produced to phosphoric acid (P 2 O 5 ) produced, and the interaction of the gypsum and cooling ponds, the contaminants will tend to build up to a pseudo steady-state value.
Once the phosphoric acid system has operated for a period of time, the amount of contaminants being stacked with the gypsum will closely approximate the net input of these contaminants into the pond systems. As this occurs, the pond water will exhibit somewhat of a constant contaminant concentration level. The gypsum is continuously acting as a surge reservoir for contaminated pond water and as a result can serve as an on-site inventory source.
Fluoride species can also evolve in other unit operations within the overall complex such as fertilizer production facilities. Again, recirculated pond water is generally used for scrubbing these vapors emitted by the other operations.
Since the majority of the fluoride vapors are evolved in the evaporation systems, there have been previous efforts to recover the fluoride via the installation of so-called fluosilicic acid (FSA) towers. These towers are essentially spray or other form of direct contact towers that are installed between the evaporator vapor discharge and the barometric condenser units. A recirculated stream of fluosilicic acid (FSA) is used to scrub the vapors from the evaporators and produce a more concentrated and higher purity stream of FSA.
Since the use of conventional FSA recovery involves the installation of additional equipment with the vacuum portion of the evaporation system, it can have a negative impact on the operation of the vacuum evaporator because it adds pressure drop into the circuit. Further, any up-sets in the evaporation system or efforts to operate at higher than designed flow rates, which are common in the industry during certain seasons, can result in off-specification FSA. Since FSA is a true by-product of the operation and not a primary product, any detrimental impacts of the FSA recovery operation on the phosphoric acid (P 2 O 5 ) operation are generally viewed as negatives.
It would therefore be desirable to have a process which would allow for the recovery of fluorides from the phosphoric acid complex but have no potential negative impacts on the phos-acid operations. Further, in the past the FSA has generally been sold commercially as an FSA solution which has a relatively low unit fluoride value due to the presence of the silica component within the compound. Earlier efforts to separate the fluoride from the silica have used ammonia to precipitate the silica as an amorphous silica material and an intermediate ammonium fluoride solution. This ammonium fluoride can be further treated to produce various fluoride products, but in general the silica produced in the previous processes was of relatively low quality and was not competitive in the higher value industrial silica markets.
Due to the negatives associated with installing FSA recovery equipment within the evaporation system, the recovery of fluoride materials from phosphoric acid sources has been somewhat limited. Industrial economies require fluoride products for a variety of applications, and in many cases countries do not have domestic conventional fluoride sources such as fluorspar. This results in the need to import fluorides, and thus a dependency on a foreign fluoride source is created.
Therefore it would be desirable to have a process for the recovery of fluorides that has no negative impact on the existing phosphoric acid operation and allows for the production of high purity fluoride products as well as an industrially acceptable precipitated silica product. Further, it would be desirable for such a process to be able to recover fluoride species from the pond systems or barometric condenser waters, and which would also allow the phosphoric acid producer to recover not only the current fluoride being produced in the facility but material that had been previously stacked or inventoried in the gypsum and cooling pond systems.
A system that would recover not only the fluoride species from the pond waters but also a portion of the contained phosphoric acid (P 2 O 5 ) that is in the water would also be desirable. In this manner the pond systems can now serve as a potentially value-added source of fluoride species and recovered P 2 O 5 for the phosphoric acid operation.
Further such a system would reduce the costs associated with any wastewater treatment that might be required in the event of excess wastewater build-up in the pond systems. Treatment of the contaminated pond water is well established, but does represent a significant cost that is dependent on the concentration of the fluoride and P 2 O 5 in the water. Reduction of contained contaminants prior to excess water treatment would significantly reduce the costs associated with water treatment.
SUMMARY
The invention provides processes and methods for the recovery of fluoride species, silica, and phosphoric acid from wastewaters and industrial pond systems. In alternative embodiments, the invention provides methods comprising a continuous ion exchange system which removes the fluoride and phosphoric acid (P 2 O 5 ) from the wastewater and industrial pond systems to produce an intermediate silicofluoride solution and a more concentrated P 2 O 5 solution. In alternative embodiments, this intermediate solution is then further processed to separate the silicofluoride material from the P 2 O 5 fraction. In alternative embodiments, the P 2 O 5 fraction is returned to the phosphoric acid plant as recovered phosphoric acid, or processed separately into technical grade P 2 O 5 acid.
In alternative embodiments, the silicofluoride material is then used to produce a soluble bifluoride salt that is combined with a recycled fluoride salt to produce a solid bifluoride salt. This solid bifluoride can then be calcined (decomposed) to produce high quality anhydrous hydrofluoric acid (HF). The resulting single fluoride salt from the calcining operation is recycled to produce additional bifluoride solids.
The soluble bifluoride solution can also be used to produce a range of industrial fluoride products, such as aluminum fluoride, single and double fluoride salts, and the like.
In alternative embodiments, during the separation of the silica component from the silicofluoride solution to produce the intermediate fluoride solution, the process is such that a higher quality of precipitated silica can be produced. This then allows for both components in the original silicofluoride (Si/F) solution to be separated to produce high quality products from both of the contained components.
In alternative embodiments, the invention provides methods and processes for the simultaneous recovery or removal of a fluoride, a silica and a phosphate contaminant from a sample, and production of a fluosilicic acid (FSA) (H 2 SiF 6 ), a phosphoric acid (P 2 O 5 ) and a phosphoric acid (H 3 PO 4 ), comprising:
(a) providing a continuous ion exchange system comprising an anion exchange resin or material or composition to remove or recover the fluoride, silica and phosphate contaminants,
wherein optionally the anion exchange resin or material or composition comprises:
a clear gel Type 1 strong-base anion exchanger, or a PUROLITE A-600 (Purolite, Bala Cynwyd, Pa.), having a gel polystyrene crosslinked with divinylbenzene, or equivalents thereof; a LEWATIT® K 6462 (Lanxess, Maharashtra, India), or equivalents thereof; or a DOWEX 21K XLT™ or DOWEX 21K 16/300™ (DOW, Midland, Mich.), or equivalents thereof; or
a resin, a composition or a material, or a non-resin solid or a semi-solid material, comprising chelating groups, functionalities or moieties that can a fluoride, a silica and a phosphate contaminant from a sample, wherein optionally the compositions comprise beads, wires, meshes, nanobeads, nanotubes, nanowires or other nano-structures, or hydrogels;
(b) providing a liquid or an aqueous sample, or making a liquid or aqueous solution from a sample to be processed, wherein the liquid or aqueous solution is an acidic solution,
and optionally the acidic liquid or aqueous solution has a pH at about pH 2, or above pH 2, or pH 2.5, or pH 3, or higher (but remaining acidic);
(c) applying the liquid or the aqueous sample to the anion exchange resin of the continuous ion exchange system under conditions such that fluoride, silica and phosphate contaminants remain on the anion exchange resin to produce an effluent substantially free of fluoride, silica and phosphate contaminants, thereby removing fluoride, silica and phosphate contaminants; and
(d) washing of the anion exchange resin with water, followed by regenerating the anion exchange resin with a sulfuric acid solution by applying the sulfuric acid solution the anion exchange resin to regenerate the anion exchange resin and produce an eluate of fluosilicic acid (FSA) (H 2 SiF 6 ), phosphoric acid (P 2 O 5 ) and phosphoric acid (H 3 PO 4 ),
wherein the concentration or amount of sulfuric acid applied to the anion exchange resin for the regeneration of the anion exchange resin is in a range of from between about 5%/weight to about 95%/weight,
and optionally the sulfuric acid solution has a pH of about 1.0, or a pH between about pH 1.0 and pH 2.0.
In alternative embodiments, the fluoride, silica or phosphate contaminants removed by the anion exchange resin and recovered as an eluate in step (d) comprise a SiF 6 −2 , a PO 4 −3 , a H 2 PO 4 −1 or a HPO 4 −2 anionic species.
In alternative embodiments, the sample is derived from an environmental source, or a contaminated wastewater system, a cooling pond system, or a wastewater system or cooling pond system associated with a phosphoric acid plant, or a gypsum or a cooling pond system, and optionally the wastewater is pretreated and/or has solids removed before its application to the anion exchange resin.
In alternative embodiments, the concentration or amount of sulfuric acid applied to the anion exchange resin for the regeneration of the anion exchange resin is in a range of from between about 10%/weight to about 25%/weight.
In alternative embodiments, processes of the invention can further comprise concentrating the regeneration solution to a concentration of at least about 20% sulfate content, or between about 20% to 50% sulfate content, or between about 15% to 55% sulfate content, thereby further concentrating the phosphoric acid (P 2 O 5 ), with the resulting evolution of the fluosilicic acid (FSA) (H 2 SiF 6 ) contaminant along with evaporated water, wherein optionally the concentrating is by a single effect or a multiple effect conventional evaporation system, or by vapor recompression.
In alternative embodiments, processes of the invention can further comprise returning the concentrated phosphoric acid solution to a phosphoric acid plant, or using the concentrated phosphoric acid solution directly as a make-up solution to a fertilizer or a fertilizer operation.
In alternative embodiments, processes of the invention can further comprise recovering the fluosilicic acid (FSA) (H 2 SiF 6 ) vapor by contacting with a recirculating stream of water, to produce a concentrated FSA solution.
In alternative embodiments, processes of the invention can further comprise indirectly cooling the recirculating stream of FSA to about 130 degrees F., or about 110 degrees F., or between about 100 to 140 degrees F., or between about 110 to about 130 degrees F., to maintain a temperature that is low enough to minimize any loss of FSA from the recovery system.
In alternative embodiments, processes of the invention can further comprise continuously treating the concentrated FSA stream with a solution of: ammonium hydroxide (optionally recovered ammonium hydroxide), at a concentration the range of between about 5% and 28% as NH 3 , or in the range of between about 10% to 20% as NH 3 ; and, ammonia (optionally make-up ammonia) between about 25% and 100%, or at about 28% for NH 3 or at about 100% for anhydrous NH 3 material, to precipitate a hydrated silica material and an ammonium fluoride solution, optionally comprising a silica/ammonium fluoride (AF) slurry. In alternative embodiments, the ammonia solution and make-up ammonia are added rapidly mixed to produce a fast silica precipitation.
In alternative embodiments, processes of the invention can further comprise neutralizing the solution at a pH range of between about pH 7.6 to about pH 9.2, or at a range of about pH 8.1 to about pH 8.8, optionally neutralizing the solution with ammonia.
In alternative embodiments, processes of the invention can further comprise rapidly cooling the resulting silica/ammonium fluoride (AF) slurry in a continuous indirect contact heat exchanger to cool the slurry temperature to a target level within a target period of time, wherein optionally the target temperature for the cooled silica slurry is between about 90° F. to about 125° F., or at a range of between about 100° F. to about 110° F., and optionally the target cooling time is between about 0.5 minutes to about 30 minutes, or between about 1 minute to about 5 minutes.
In alternative embodiments, processes of the invention can further comprise filtering the cooled silica/AF and washing the silica with water to remove entrained AF liquid from the silica.
In alternative embodiments, processes of the invention can further comprise the rapid drying of the filtered silica to produce and industrial high surface area precipitated silica product, wherein the drying time is between about 0.20 minutes to about 10 minutes; or about 0.25 minutes to about 5 minutes; or between about 0.5 minutes and about 2 minutes.
In alternative embodiments, processes of the invention can further comprise separating the AF from the silica and further concentrating the AF solution to decompose the AF and produce a solution of ammonium bifluoride (ABF) and vaporized ammonia for recycle.
wherein optionally the concentrating is by a single effect or a multiple effect conventional evaporation system, or by vapor recompression.
In alternative embodiments, processes of the invention can further comprise reacting the resulting ABF solution from the decomposition step with an alkali fluoride (optionally a sodium fluoride), to produce an insoluble alkali bifluoride (optionally a sodium bifluoride (NaHF 2 )) and an ammonium fluoride (AF) solution, wherein optionally the AF solution comprises between about 10% and 30% fluoride (F). In alternative embodiments the alkali fluoride comprises an alkali that will produce an alkali bi-fluoride that is insoluble in an ammonium fluoride solution and that will decompose to form an alkali fluoride and hydrofluoride acid (HF) vapor, wherein optionally the alkali comprises a sodium, a potassium or a lithium alkali, and optionally the sodium fluoride can be recycled within the process, and optionally a small amount of make-up alkali may be required and optionally this comprises a sodium carbonate or a sodium hydroxide. In alternative embodiments, processes of the invention can further comprise recovering the HF vapor via cooling with the subsequent production of HF, optionally HF materials, such as anhydrous HF; or, all or a portion of the HF is used to produce an AlF 3 .
In alternative embodiments, processes of the invention can further comprise reaction of the intermediate ABF solution with an alumina source to produce an aluminum fluoride product, wherein optionally the alumina source comprises an industrial-grade alumina, an Al 2 O 3 , or an aluminum hydroxide (Al(OH) 3 ).
In alternative embodiments, processes of the invention can further comprise reacting the intermediate ABF solution with a reagent to produce a fluoride “single-salt” product, wherein optionally the fluoride “single-salt” product comprises a magnesium fluoride (optionally using magnesium oxide or hydroxide or sulfate as the magnesium source), or a potassium fluoride (optionally using potassium hydroxide or carbonate or sulfate as the potassium source), wherein optionally the reagent comprises any cationic-hydroxide or carbonate material, a calcium oxide, a calcium carbonate, a sodium hydroxide, a potassium hydroxide, a magnesium hydroxide/oxide/carbonate, or any combination thereof. In alternative embodiments, the resulting fluoride products comprise a double-salt material, or a K2TiF6; a K2TaF6; a K2ZrF6; a KBF4 and equivalents, and optionally the resulting fluoride products are produced from commercially available non-fluoride raw materials or scrap materials.
In alternative embodiments, processes of the invention can further comprise reacting the intermediate ammonium bifluoride (ABF) solution with a reagent to produce a bifluoride material, and optionally the bifluoride material comprises a potassium bifluoride (optionally using a potassium hydroxide or a carbonate as the K source), a lithium bifluoride (optionally using a lithium hydroxide or a carbonate as the Li source), or equivalents.
In alternative embodiments, processes of the invention can further comprise reacting the ABF solution with an alkali, an alkaline, or a cationic compound, to produce a fluoride salt, optionally to produce: a magnesium fluoride (optionally MgF 2 using magnesium oxide or hydroxide or carbonate as the Mg source); a calcium fluoride (optionally CaF 2 using calcium oxide; hydroxide or carbonate as the Ca source, optionally a divalent cationic material in the hydroxide or carbonate oxide form is used as the cation source); and equivalents. In alternative embodiments, the fluoride-containing solution source is a purge stream of recycled water that is used in the phosphoric acid plant condensing systems and indirectly cooled via indirect contact in a conventional heat exchanger system with a stream of recycled fresh water obtained from a cooling tower unit.
The invention provides industrial processes for the recovery of a fluoride, a phosphoric acid (P 2 O 5 ), or a silicofluoride from a phosphoric acid-generating plant facility or a contaminated wastewater system associated with a phosphoric acid-generating facility, or a gypsum or a cooling pond, comprising an industrial process as set forth in FIG. 1 , or any portion or sub-process thereof.
The details of one or more embodiments of the invention are set forth in the accompanying drawings and the description below. Other features, objects, and advantages of the invention will be apparent from the description and drawings, and from the claims.
All publications, patents, patent applications cited herein are hereby expressly incorporated by reference for all purposes.
BRIEF DESCRIPTION OF THE DRAWINGS
The drawings set forth herein are illustrative of embodiments of the invention and are not meant to limit the scope of the invention as encompassed by the claims.
Figures are described and discussed herein.
FIG. 1 schematically illustrates an exemplary process of the invention, an overall process flow diagram for an exemplary fluoride recovery process of the invention, hereinafter referred to as the “F/Si Recovery from WasteWater” process.
Like reference symbols in the various drawings indicate like elements.
Reference will now be made in detail to various exemplary embodiments of the invention, examples of which are illustrated in the accompanying drawings. The following detailed description is provided to give the reader a better understanding of certain details of aspects and embodiments of the invention, and should not be interpreted as a limitation on the scope of the invention.
DETAILED DESCRIPTION
The invention provides processes and methods for the recovery of fluoride species and phosphoric acid from wastewaters and industrial pond systems. In alternative embodiments, the invention provides methods comprising a continuous ion exchange system which removes the fluoride (F) and phosphoric acid (P 2 O 5 ) from the wastewater and industrial pond systems, e.g., as the exemplary process illustrated in FIG. 1 , in which wastewater from a gypsum/cooling pond system ( 1 ), is fed to a Pretreatment System where the water is clarified to allow for removal of any of the larger suspended solids. The solids ( 3 ) can be returned to the gypsum pond system and the low solids water ( 2 ) is fed forward to the exemplary system, the so-called “CIX F/Si/P2O5 Recovery System” of the invention. This exemplary system comprises a continuous ion exchange unit and the associated peripheries to allow for loading, washing, and regeneration to be carried out in a continuous fashion.
In exemplary embodiments of the so-called “CIX F/Si/P2O5 Recovery System” of the invention, the fluoride species is removed from the pond water as an anionic material using a strong anion resin. The general reaction for this extraction step is as follows:
R 2 —SO 4 +H 2 SiF 6 =>R2-SiF 6 +H 2 SO 4 ,
wherein the R— is the ion exchange resin phase.
In exemplary embodiments, the phosphate materials are removed from the pond water with the same resin as follows:
1.5 R 2 —SO 4 +H 3 PO 4 =>R 3 —PO 4 +1.5H 2 SO 4
In exemplary embodiments, the low Si/fluoride (F)/phosphoric acid (P 2 O 5 ) pond water is then returned to the phosphoric acid plant as make-up water. Alternatively the treated water can be returned to the pond system.
Using the treated water as a make-up to the phos-acid plant can have distinct advantages in that the sulfuric acid used in the exemplary CIX system (or the exemplary continuous ion exchange process of the invention) for regeneration can be mostly reclaimed via the filter washes and the like. This results in a lower operating cost for the fluoride (F) recovery operation since+H 2 SO 4 is required in the phos-acid plant, thus the treated water contains a useable material.
From an overall standpoint, using this exemplary ion exchange process of the invention, one mole of H 2 SO 4 (98 lbs/lb-mole) is required for each mole of hydrofluosilicic acid (H 2 SiF 6 ) treated. This results in a sulfuric acid requirement of about 98 lbs H 2 SO 4 /114 lbs F recovered, or about 0.82 lbs H 2 SO 4 /lb of recovered F as HF.
Now consider the production of HF from conventional fluoride sources, such as fluorspar (CaF 2 ) and sulfuric acid. In the traditional route, the fluorspar is reacted with sulfuric acid to form a gaseous hydrofluoric acid stream. The reaction for this general approach is as follows: CaF 2 +H 2 SO 4 =>2 HF+CaSO 4 . In this traditional HF approach it can be seen that the sulfuric acid requirement is about 98 lbs H 2 SO 4 /40 lbs of HF produced. This is about 2.45 pounds H 2 SO 4 per pound of HF produced.
This is a significantly greater amount than that needed for this invention's exemplary ion exchange process, thus there can be immediate inherent cost savings associated when using the present invention. In alternative embodiments, in this invention's ion exchange approach, the majority of the H 2 SO 4 in the treated water can be reused in the phos-acid process, thus actual H 2 SO 4 requirements are somewhat less than indicated for the ion exchange method.
In alternative embodiments the resin in this invention's exemplary so-called “CIX system” is loaded with SiF 6 −2 or a PO 4 −3 anions. The resin is washed with a small amount of water ( 7 ) then contacted with a regeneration solution consisting of sulfuric acid ( 5 ). The sulfate ion displaces the SiF 6 −2 or a PO 4 −3 anions from the resin and results in the production of an intermediate stream of a fluosilicic acid (FSA, or H 2 SiF 6 ) and a phosphoric acid (H 3 PO 4 ).
In alternative embodiments, the resin is the returned to the sulfate form, and after washing with a small amount of water, the resin is returned to the fluoride and phosphate species extraction step. The general reaction for this regeneration step is as follows:
R2-SiF 6 +H 2 SO 4 =>R2-SO 4 +H 2 SiF 6
for the SiF6 species and
R3-PO 4 +1.5 H 2 SO 4 =>1.5 R2 SO 4 +H 3 PO 4 for the PO 4 species
The sulfuric acid with the recovered silicofluoride and phosphate values ( 6 ) is next transferred to a Sulfuric Acid Evaporation system. In this stage of the process, the F/Si/P 2 O 5 -containing solution is concentrated and as the concentration increases the Si/F fractions evaporate from the acidic solution along with water vapor. A portion of the concentrated sulfuric acid stream is recycled ( 5 ) for regeneration of the resin to the exemplary process, the so-called “CIX system”. As the solution continues to recycle, additional P 2 O 5 is recovered and the concentration of P 2 O 5 continues to increase since the phosphate solution has a very low vapor pressure.
In alternative embodiments, once the operation achieves steady-state, a small purge stream of the concentrated sulfuric acid/P 2 O 5 solution ( 5 A) is returned to the phosphoric acid plant. This purge stream contains appreciable quantities of phosphoric acid which represents a direct incremental increase in P 2 O 5 recovery for the plant. Make-up sulfuric acid ( 9 ) is added into the system in the evaporation system.
In alternative embodiments, the Si/F vapor exiting the evaporation system ( 10 ) flows to the F/Si Recovery Scrubber/Condensing System. In this step the vapors are contacted with a recirculating solution of fluosilicic acid (FSA) and water ( 11 ). The solution scrubs the Si/F vapors from the stream and also allows for a portion of the contained water vapor to condense in order to maintain a specific silicofluoride content in the solution.
In alternative embodiments, the Si/F-containing solution exiting the recovery scrubber system ( 12 ) is returned to the Cooling Vessel and cooled via indirect heat exchange. It is then recirculated to the F/Si scrubber. Cooling water for this step ( 100 ) is supplied from the existing cooling pond system.
In alternative embodiments, the fluosilicic acid (H 2 SiF 6 or FSA), solution ( 14 ) is then transferred to the Silica Precipitation/Filtration system where recycled ammonium hydroxide ( 21 ) and ammonia ( 15 ) are added to neutralize the FSA, increase the pH and precipitate the silica from the solution as a precipitated silica compound. This reaction is conducted using a rapid mixing approach on a continuous basis to precipitate the silica quickly at a controlled terminal pH of between 8.0 and 8.9, depending on the nature of the silica product required. The general reaction for this step is as follows:
H 2 SiF 6 +6 NH 4 OH=>6NH 4 F+Si(OH 4 )+2H 2 O
In the reaction approach itself, the FSA solution is transferred to a centrifugal pump inlet along with a stream of recovered ammonium hydroxide solution ( 21 ) and make-up ammonia ( 15 ). The mixture is intensely mixed in the impellor section of the pump then discharged into a pipe reactor unit and flows through this unit for a specific residence time; in one embodiment, at less than about 10 minutes, or alternatively, at less than about 1 minute.
In alternative embodiments, after the short hold-up period the slurry is transferred to an indirect cooling system and cooled over a relatively short period of time. The cooling is achieved via indirect heat exchange and systems such as shell and tube; wide gap plate heat exchangers and the like are acceptable methods for cooling. The key is rapid cooling, i.e. less than 10 minutes, and preferably less than 2 minutes, from cooling start to finish.
In alternative embodiments, the cooled silica slurry is then filtered. The filtered silica is washed with water ( 16 ) then transferred ( 17 ) to the Silica Drying/Preparation system where the material is dried, via spray drying or other flash drying-type system, then stored for packaging and shipment as technical-grade precipitated silica products ( 18 ).
In alternative embodiments, the ammonium fluoride solution ( 20 ) generated in the silica precipitation system is transferred to the Ammonium Fluoride Decomposition (AF to ABF) system. In this step, the ammonium fluoride solution is evaporated to increase the salt concentration. As the AF concentration increases, the ammonium fluoride will decomposes and the salt will convert to a bifluoride form as follows:
2 NH 4 F+(heating)=>NH 4 FHF 2 +NH 3 (vapor)
In alternative embodiments, the ammonia evolved from the decomposition reaction is recovered and recycled to the silica precipitation circuit. The resulting ammonium bifluoride, NH4HF2 or ABF, ( 22 ), is transferred to the Sodium Bifluoride Production step. In this step, the ABF is mixed with recycled sodium fluoride, NaF ( 26 ), and an insoluble sodium bifluoride, NaHF2 or SBF, is produced as follows:
NH 4 F HF 2 +NaF=>NaHF 2 (solid)+NH 4 F
Other alkali fluoride salts may be used for this step, such as potassium fluoride and the like provided that the resulting alkali bifluoride salt is insoluble in a solution of ammonium fluoride and further that the alkali bifluoride will decompose to produce an HF vapor and solid alkali fluoride suitable for recycle to the bifluoride production stage.
In alternative embodiments, the ammonium fluoride solution ( 24 ) is recycled to the ammonium fluoride decomposition step to return the AF to its bifluoride form. The sodium bifluoride solids ( 25 ) are then transferred to the Sodium Bifluoride Decomposition stage. In this step the sodium bifluoride is heated and the material decomposed to produce an anhydrous hydrofluoride acid vapor ( 30 ) and a sodium bifluoride solid ( 26 ) which is recycled to the Sodium Bifluoride Production step. The decomposition reaction is as follows:
NaHF2+(heat)=>HF(vapor)+NaF
In alternative embodiments, the HF vapor is process to recover the HF as an anhydrous product. Alternatively, HF solutions (e.g. 70% HF) could be produced if need be. This HF can be sold as a primary product ( 31 ) or alternatively used for the production of other salts such as aluminum fluoride, AlF 3 .
In alternative embodiments, for aluminum fluoride production, the HF is mixed with an alumina source ( 33 ) to produce the AlF 3 solids. This technique, i.e. direct reaction of alumina with HF, is used in various conventional aluminum fluoride production methods. The aluminum fluoride product ( 34 ) can then be used as a commercial product.
Aluminum fluoride can also be produced via the reaction of the intermediate ammonium bifluoride ( 35 ) with an alumina source ( 33 ). In this case, the aluminum fluoride is precipitated from the solution and then filtered, washed and dried to product the AlF 3 product ( 34 ). The ammonium solution resulting from this reaction is recycled. Another alternative available for the production of value-add materials is to utilize a portion of the intermediate ammonium bifluoride solution ( 22 ) and further concentrate it to produce a dry ammonium bifluoride product. In this scenario, the ABF solution is concentrated to crystallize ammonium bifluoride (NH 4 HF 2 ). This material is then filtered, dried and can be used or sold as an ammonium bifluoride product ( 40 ). There are various industrial applications where ABF may be preferred as a fluoride source over HF and this option allows the producer to supply this market.
Yet another alternative is to take a portion of the concentrated ABF ( 41 ) and combine it with selected reagents ( 42 ) to produce a range of fluoride single and double salt products. As an example, consider the option wherein the double salt potassium titanium fluoride is the desired target product.
In alternative embodiments, the ABF solution is combined with a titanium source, such as rutile, ilmenite, etc. and a potassium source, such as potassium sulfate, to produce a double salt of K2TiF6. Likewise, with the appropriate reagent make-ups, materials such as potassium tantalum fluoride (K2TaF6); potassium zirconium fluoride (K2ZrF6); potassium fluoborate (KBF4); potassium bifluoride (KHF2); potassium fluoride (KF); and the like can be produced from the intermediate fluoride source as specialty fluoride salt products ( 43 ).
In alternative embodiments, the production of the specialty fluoride salts will result in a co-product ammonium solution, such as ammonium sulfate. In most phosphate complexes this material can be returned ( 44 ) to the fertilizer operations for incorporation in the various ammonium products, such as diammonium phosphate (DAP).
The application of this invention to existing and future wastewater, e.g., pond water, sources associated with phosphoric acid complexes allows for the production of strategic materials and recovers valuable resources which are currently being wasted. In addition, the process allows for increased P 2 O 5 recovery, as a weak phosphoric acid solution, via the recovery of the P 2 O 5 losses from the phosphoric acid plant that end up in the pond water.
Another alternative that can be utilized with this processing approach is a barometric condenser contacting approach whereby the barometric condenser discharge water is transferred to an indirect heat exchanger and contacted (indirectly) with a stream of cool, fresh water that has been obtained from a conventional cooling tower system. The barometric condenser water is cooled (indirectly) then recycled to the barometric condensers for reuse. The warm cooling tower water is returned to the cooling tower for cooling and reuse.
In this manner, the need for cooling pond systems, (with associated handling and potential emission problems) is eliminated. This could represent a significant advantage to some types of operations.
The use of recycled barometric condenser water has been considered attractive but to date the problem has been that fluoride will continue to build up in the barometric condenser water and eventually its effectiveness will be reduced. Typically as the fluoride concentration increased, barometric condenser water would be purged and treated, for instance with lime, to precipitate the fluoride species. This would result in a considerable operating cost for the recycle system.
By application of the present invention, the purge solution from the recycled barometric condenser water can be treated in the continuous ion exchange system for removal of the fluoride. This allows for the purged barometric condenser water to be treated for fluoride removal and then reused. Recovery of the fluoride via the CIX approach is economically attractive thus the applicability of the recycle barometric condenser water method can now be realistically considered. The fluoride recovered from the barometric condenser water via the CIX system would be processed in the same manner as the fluoride recovered from the pond water systems.
A number of embodiments of the invention have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of the invention. Accordingly, other embodiments are within the scope of the following claims. | In particular, in alternative embodiments, the invention provides for a method to recover silicofluoride and phosphate species from wastewaters, or barometric condenser waters, that are typically utilized in wet-process phosphoric acid facilities. The species are recovered via a continuous ion exchange approach that allows for economic recovery of the materials and especially with the silicofluoride component allows for the production of valuable industrial materials such as hydrofluoric acid and other fluoride salts as well as industrial-grade precipitated silica materials. Return of the treated waste water to the phos-acid plant allows for optimization of reagent usage. | 2 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. application Ser. No. 13/234,826, filed Sep. 16, 2011, which claims the benefit of U.S. Provisional Application No. 61/439,882, filed Feb. 5, 2011, the contents of each of which are hereby incorporated by reference in their respective entireties.
BACKGROUND
The biological test kit relates to the field of patient operated biological testing apparatus
The use of Lancets in biological testing is well known in the art. In some inventions the Lancet is placed in or formed as part of a blister or bubble. A user causes the blister to collapse and thereby move the lancet to puncture the skin of the patient or user. U.S. Pat. No. 5,231,993 to Haber et al, U.S. Pat. No. 5,636,640 to Staehlin, U.S. Pat. No. 5,505,212 to Keljmann et al, U.S. Pat. No. 5,054,499 to Swierczeck, published patent applications 20080058726 to Jina, 20070129620 to Krulevich et al, and 20090099427 also to Jina are all typical of this approach. The present invention provides an array of lancets, each of which is housed and protected in a well which is covered by a flexible cover.
BRIEF SUMMARY OF THE INVENTION
The biological test kit is a device for drawing and, optionally, testing biological samples. The biological test kit comprises: a rigid first layer, one or more lancets secured to the rigid first layer, said lancets each having a sharp region disposed substantially away from the rigid first layer, one or more second layers disposed in an opposed arrangement relative to the rigid first layer, the rigid first layer and second layers being arranged to form one or more cavities, each of the one or more second layers forming one or more covers, each cover over one of the lancets; and each of the one or more covers having a first unconstrained configuration in which the lancet sharp region does not protrude past or through the cover and having a second compressed configuration in which the lancet's sharp region protrudes through the cover. In one embodiment the biological test kit employs distinct covers for each lancet and in another the covers are formed from sheet material formed into blisters which cover the lancet.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
FIG. 1 is a top view of the biological test kit.
FIG. 2 is a front view taken from FIG. 1 .
FIG. 3 is a section view taken from FIG. 1 .
FIG. 4 is a second embodiment of a biological test kit.
FIG. 5 is a front view taken from FIG. 4 .
FIG. 6 is a section view taken from FIG. 4 .
FIG. 7 is a front view of a kit pressed between a thumb and index finger.
FIG. 8 is a front view of a second embodiment pressed upon a hard surface by another body part.
FIG. 9 is a perspective view of a second embodiment in use.
FIG. 10 is an enlarged detail view taken from FIG. 6 , in unconstrained configuration.
FIG. 11 is a view like FIG. 10 in a compressed configuration.
FIG. 12 is a detail view of collecting the biological sample by producing a wound.
FIG. 13 is a front view of collecting a biological sample from a wound.
FIG. 14 is a top view of the testing apparatus measuring a sample.
DETAILED DESCRIPTION OF THE INVENTION
The biological test kit 1 comprises: a rigid first layer 2 , one or more lancets 3 secured to the rigid first layer 2 , said lancets 3 each having a sharp region 4 disposed substantially away from the rigid first layer 2 , one or more second layers 5 disposed in an opposed arrangement relative to the rigid first layer 2 , the rigid first layer 2 and second layers 5 being arranged to form one or more cavities 6 there-between, each of the one or more second layers 5 forming one or more covers 7 , each cover 7 over one of the lancets 3 ; and each of the one or more covers 7 having a first unconstrained configuration 8 in which the lancet 3 sharp region 4 does not protrude past or through the cover 7 and having a second compressed configuration 9 in which the lancet's 3 sharp region 4 protrudes through the cover 7 .
The rigid first layer 2 is composed of a rigid material such as plastic, wood, or metal. The rigid first layer 2 provides a foundation for construction of the biological test kit 1 .
Lancets 3 are small rods or bars constructed of metal or plastic with one end flattened and sharpened to facilitate making a small puncture site 10 , often optimized for puncturing human skin. In the biological test kit 1 , one or more lancets 3 are fixed in the rigid first layer 2 such that the sharp region 4 of the lancet 3 is positioned at a distance from the rigid first layer 2 . The lancets 3 may be placed in any pattern.
The second layer 5 is made of resilient material and is formed over the rigid first layer 2 to provide a cover 7 for each of the lancets 3 . This may be accomplished in any number of ways including, but not limited to, forming the second layer 5 into a number of blisters where each blister forms a cover 7 for one of the lancets 3 and forms an airtight cavity 6 covering and surrounding the lancet 3 . These blisters are sized so that when a user applies sufficient compressive force against the rigid first layer 2 and the second layer 5 the blister is pierced by the lancet 3 along with the skin of the user. The user may accomplish this by pinching the blister between a thumb and index finger, or any other suitable body parts 20 . Alternatively, the user may apply this pinching force by placing the rigid first layer 2 on a supporting surface and pressing the appropriate body part 20 on the blister. The material chosen for the second layer 5 , and therefore the blisters, may be sufficiently resilient to cause the blister to reform into its original position, and cover 7 the lancet 3 , when the user applied pressure is removed.
The biological test kit 1 may include any number of second layers 5 . However, each of the second layers 5 may serve a unique purpose such as resealing the hole made by passage of the Lancet 3 through the cover 7 or providing a dose of antibiotic, or providing an indication as to the chemical analysis of the biological sample 13 .
The biological test kit 1 may also include test strips 12 which capture biological samples 13 resulting from the action of the lancet 3 such as fluid exuded from the puncture site 10 created by the lancet 3 .
The biological test kit 1 may also include a test apparatus 14 for analysis of the samples 13 gathered as above. This test apparatus 14 may include the ability to display the results of the analysis in any suitable manner, such as a digital readout or color change of the test strip 12 .
In a second embodiment 15 the biological test kit 1 includes a rigid first layer 2 and lancets 3 as above with a distinct well 16 provided for each lancet 3 within the rigid first layer 2 and a distinct cover 7 for each lancet 3 . Each well 16 has a closed end 17 and an open end 18 . A lancet 3 is fixed to the closed end 17 of each well 16 . Each well 16 is formed with a ledge 19 around the interior of its open end 18 . The well 16 and the ledge 19 are sized to permit insertion of a cover 7 said cover 7 supported by the ledge 19 .
Each cover 7 is formed as a compound curve and formed from a flexible and resilient material such that the cover 7 can be compressed by an applied force into a compressed configuration 9 and when said force is removed the cover 7 returns to its unconstrained configuration 8 . When the cover 7 is placed in the well 16 with the convex surface facing away from the closed end 17 of the well 16 and the cover 7 is in the unconstrained configuration 8 the cover 7 conceals the lancet 3 . When so placed and pressed into the compressed configuration 9 the lancet 3 protrudes through the cover 7 to a prescribed distance. When a user desires to produce a puncture site 10 from which a biological sample 13 may be taken, the user presses the cover 7 with sufficient force that the lancet 3 pierces the cover 7 and the user's finger, or other body part 20 . It is to be noted that the cover 7 may or may not include a hole through which the lancet 3 passes.
The biological test kit 1 may be further provided with one or more protective or indicative layers 21 . The protective or indicative layers 21 may be made of a material which is flexible yet non porous to prevent intrusion of foreign material when serving a protective function and made of a chemically reactive material when serving an indicative function or be made of a material suitable for protection and treated with an indicative substance to serve both purposes.
As above the rigid first layer 2 may be provided with a test apparatus 14 and test strips 12 .
The biological test kit 1 may be used according to the following steps: collecting biological samples 13 comprising the steps, compressing a lancet 3 cover 7 onto a stationary lancet 3 until said lancet 3 pierces said cover 7 and said user, producing a puncture site 10 . This method may further include the step of collecting biological samples 13 from said puncture site 10 . This method may also comprise the step of using a testing apparatus 14 to measure one or more chemical properties of said biological sample 13 . | The biological test kit is a device for drawing and, optionally, testing biological samples. The biological test kit is an array of lancets set in wells in a rigid base. Each lancet well is covered by a protective cover which when deformed permits the lancet to puncture a user or other patient. In one embodiment the biological test kit employs distinct covers for each lancet and in another the covers are formed from sheet material formed into blisters which cover the lancet. | 0 |
[0001] This application draws priority from U.S. Provisional Patent Application Serial No. 60/340,277, filed Dec. 18, 2001.
FIELD AND BACKGROUND OF THE INVENTION
[0002] The present invention relates to a neuroprosthetic device for activating the body with functional electrical stimulation (FES), and more particularly, to a surface neuroprosthetic device that enables the device user facile on-line adjustment and fine-tuning of the local current density over the surface of the scanning electrode, so as to achieve optimal muscle response.
[0003] Neuroprostheses and therapeutic FES devices, based on surface stimulation, typically interface with the body limb through an array of surface electrodes positioned over the limb surface. Electrical stimulation delivered to the underlying limb musculature and neurological structures through the surface electrode array causes activation of the muscles, and controlled movement of the limb. Such devices are used for restoring active function to paralyzed or plegic body limbs in patients suffering disease or trauma to the central nervous system, in neurological conditions such as stroke, spinal cord injury, head injury, cerebral palsy and multiple sclerosis. Surface neuroprostheses use controlled electrical currents through electrodes placed on the surface of the body, in order to elicit contraction of selected muscles or to input sensory stimulus. Neuroprostheses can activate paralyzed muscles of the limb in an independent fashion, or in coordination with voluntary activation of muscles under natural neurological control. These devices are in use today for functional activities such as walking, standing, gripping or releasing objects, and are used both as a therapeutic modality and for improvement or restoration of activities of daily living.
[0004] The aspiration to facilitate the positioning of stimulating electrodes of FES devices over the activation points of impaired limb has evoked, in the prior art, the design and manufacture of devices that substantially conform to the shape of particular body sites and limb. Accurate positioning of the electrodes enables optimal muscle activation to give correct movement of the limb with minimum discomfort and fatigue. Typical examples of devices for stimulating particular body sites are Liberson et al., Arch. Phys. Med., 1961, 42: 101-105 and U.S. Pat. No. 4,697,808 to Larson, et al., for activating the lower limb, and U.S. Pat. No. 5,330,516 to Nathan and U.S. Pat. No. 5,562,707 to Prochazka, for activating the wrist or forearm.
[0005] The contact area of the surface electrode is an important factor in the performance of a neuroprosthesis device. Large surface area electrodes tend to disperse the stimulation field over a large skin area, and the stimulation current density passing through the skin is relatively low, resulting in relative sensory comfort. In this case, however, the resolution of the electrode is correspondingly low, as a relatively large region of excitable tissue immediately underlying the electrode may be activated (see Sagi et al., 3-D Current Density Distributions Under Surface Stimulation Electrodes, Med. & Biol. Eng. & Comp., 33, pp. 403-408, 1995).
[0006] Earlier electrodes, such as set forth in U.S. Pat. No. 4,736,752 to Munck, et al., teach the control of the current density across the electrode through the use of conductive ink and adhesive patterns. The deficiencies of such electrodes are manifest from the description hereinbelow.
[0007] It should be emphasized that accurate electrode placement is very important for surface neuroprostheses. The patient is required to ensure, each time he wishes to set up the neuroprosthesis device, that all the electrodes are positioned accurately over the motor points of the muscles to be activated. Even slight deviations in the placement of the electrode may deleteriously effect the response of the limb. Alternatively or additionally, such deviations from the proper positioning may cause undesired movements, discomfort and unnecessary fatigue. This phenomenon is particularly pronounced at certain body limb sites that have a number of different excitable tissues disposed within a small region, within which a controlled current must be applied. These systems often have electrode placement problems, because the stimulating electrode is relatively large and consequently, does not enable precise activation by selectively focussing on a small target region of excitable tissue while avoiding excitation of unwanted tissue underlying the electrode This phenomenon, which may be termed “crowding” of excitable tissue, is particularly problematic at two limb sites: the dorsal surface of the forearm, and the dorsi-flexor surface of the lower leg. In these locations, small variations in electrode placement tend to generate large changes in hand and foot posture respectively.
[0008] U.S. Pat. No. 6,038,485 to Axelgaard discloses a transcutaneous medical electrode. The electrode has a highly conductive grid including a plurality of arrays of electrical conductors (conductive inkspots) for controlling current distribution of directed electrical pulses. Electrical connectors are provided for establishing electrical communication with the conductive grid for switching ON or OFF the electrical conductors in each array. The conductive grid is supported by a moderately conductive sheet, or film, and a conductive adhesive is provided for removably coupling the sheet or film and the conductive grid to the body of a user. The device is configured such that the conductive ink spots can be switched on and off so as to control the local current density across the electrode.
[0009] In addition, U.S. Pat. No. 6,038,485 teaches thickening of the support layer in areas that a reduced current density is needed, or thinning of the support layer in areas that require a higher current density. However, this adjustment procedure requires removal of the electrode and considerable technical knowledge and experience. Adjustments of this electrode would clearly be carried out “off-line”, as the electrode is unsuitable for on-line adjustment of a neuroprosthesis. Moreover, the tuning of a device having such an electrode would be generally beyond the skill of the user, such that the ministrations of an expert in the field of FES would be required.
[0010] It would be highly desirable in neuroprostheses for the device to be adjustable, while the system is in use, so as to enable the use of direct feedback from the resulting limb posture and movements to guide the system user to adjust the system proprioceptively to achieve an optimal response.
[0011] In summary, there is no known neuroprosthetic device that enables the patient to tune the local current density delivered to the skin surface, while working with the device, and without the help of a clinician. There is, therefore, a recognized need for, and it would be highly advantageous to have, a neuroprosthetic device that enables the patient to tune the local current density delivered to the skin surface, with facility, and without the help of a clinician, so as to activate the muscles in an optimal manner.
SUMMARY OF THE INVENTION
[0012] The present invention is a surface neuroprosthetic device that enables facile adjustment and fine-tuning of the local current density over the surface of a transcutaneous scanning electrode, so as to achieve optimal muscle response.
[0013] The design of the present invention enables adjustment of the effective positioning of the device electrodes, even by the patient, while the device is stimulating, hence giving the patient direct, on-line feedback of the efficacy of the adjustment. This enables the patient to set up the device on his limb, and carry out the fine adjustment of the electrode position by observing his limb respond to the adjustment. Having achieved optimal response, the patient works with the device until the electrode may require readjusting.
[0014] Thus, according to the teachings of the present invention there is provided a scanning electrode system for a neuroprosthetic device, the system enabling facile adjustment and fine-tuning of a spatial distribution of a local electrical stimulation field across a scanning electrode, by a system user, the scanning electrode system including: (a) at least one scanning electrode for the neuroprosthetic device, the scanning electrode for performing functional electrical stimulation (FES) of at least one muscle of a limb of the user; (b) a distribution mechanism for distributing a current to the at least one scanning electrode so as to produce a biased electrical stimulation field across the at least one scanning electrode, the distribution mechanism for operative connection to a muscle stimulator providing electrical stimulation to the scanning electrode system, and (c) control means for adjustment of the biased electrical stimulation field by means of the distribution mechanism, the control means designed and configured so as to be accessable to and operable by the system user.
[0015] According to another aspect of the present invention there is provided a method of performing functional electrical stimulation (FES) using a scanning electrode system for a neuroprosthetic device, so as to enable facile adjustment and fine-tuning of a spatial distribution of a local electrical stimulation field across a scanning electrode, by a user, the method including the steps of: (a) providing a device including: (i) at least one scanning electrode for the neuroprosthetic device, the scanning electrode for performing functional electrical stimulation (FES) of at least one muscle of a limb of the user; (ii) a distribution mechanism for distributing current to the at least one scanning electrode, the distribution mechanism for operative connection to a muscle stimulator providing power to the scanning electrode system, and (iii) control means for adjustment of the biased electrical stimulation field by means of the distribution mechanism, the control means designed and configured so as to be accessable to and operable by the user, and (b) operating the control means to produce a biased electrical field across the at least one scanning electrode, so as to adjust a response of the muscle.
[0016] According to yet another aspect of the present invention there is provided a scanning electrode system for a neuroprosthetic device, the system enabling facile adjustment and fine-tuning of a spatial distribution of a local electrical stimulation field across a scanning electrode, by a system user, the scanning electrode system including: (a) at least one scanning electrode for the neuroprosthetic device, the scanning electrode for performing functional electrical stimulation (FES) of at least one muscle of a limb of the user; (b) a distribution mechanism for distributing current to the at least one scanning electrode so as to produce a biased electrical stimulation field across the at least one scanning electrode, the distribution mechanism for operative connection to a muscle stimulator providing electrical stimulation to the scanning electrode system, and (c) control means for adjustment of the biased electrical stimulation field by means of the distribution mechanism, wherein the distribution mechanism is designed and configured to bias the electrical field in a substantially monotonic fashion.
[0017] According to further features in the described preferred embodiments, the scanning electrode is a transcutaneous stimulation electrode for covering at least a portion of a skin surface of the limb.
[0018] According to still further features in the described preferred embodiments, the electrical stimulation field is biased in a substantially monotonic fashion.
[0019] According to still further features in the described preferred embodiments, the at least one scanning electrode has two adjacent conductive regions, each of the regions being electrically connected with the distribution means, the regions being electrically isolated from one another.
[0020] According to still further features in the described preferred embodiments, the distribution mechanism includes a potentiometer.
[0021] According to still further features in the described preferred embodiments, the control means are designed and configured for facile adjustment of the biased electrical field by a typical user.
[0022] According to still further features in the described preferred embodiments, the control means are intuitive control means.
[0023] According to still further features in the described preferred embodiments, the intuitive control means are proprioceptive control means.
[0024] According to still further features in the described preferred embodiments, the control means are designed and configured such that a movement of the control means in a first direction effects a limb movement correction of the limb in the same direction.
[0025] According to still further features in the described preferred embodiments, the distribution mechanism and the control means are designed and configured such that the adjustment of the biased electrical stimulation field is effected simultaneously with the functional electrical stimulation of the muscle.
[0026] According to still further features in the described preferred embodiments, the scanning electrode system further includes: (d) a voice command unit for operating the control means.
[0027] According to still further features in the described preferred embodiments, the control means is operated by electromyograph-triggered commands.
[0028] According to still further features in the described preferred embodiments, the control means are designed and configured such that the adjustment of the biased electrical stimulation field is effected in a continuous fashion.
[0029] According to still further features in the described preferred embodiments, the scanning electrode system further includes: (d) an electrogoniometer, disposed on the limb, the control means being responsive to input from the electrogoniometer.
[0030] According to still further features in the described preferred embodiments, the operating of the control means responsive to input from the electrogoniometer is performed by the user.
[0031] According to still further features in the described preferred embodiments, the control means are designed and configured such that the adjustment of the biased electrical field is effected in a continuous fashion.
[0032] According to still further features in the described preferred embodiments, the operating of the control means to produce a biased electrical field across the at least one scanning electrode is performed so as to achieve an optimal muscle response.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] The invention is herein described, by way of example only, with reference to the accompanying drawing. With specific reference now to the drawing in detail, it is stressed that the particulars shown are by way of example and for purposes of illustrative discussion of the preferred embodiments of the present invention only, and are presented in the cause of providing what is believed to be the most useful and readily understood description of the principles and conceptual aspects of the invention. In this regard, no attempt is made to show structural details of the invention in more detail than is necessary for a fundamental understanding of the invention, the description taken with the drawings making apparent to those skilled in the art how the several forms of the invention may be embodied in practice.
[0034] In the drawings:
[0035] [0035]FIG. 1 is a schematic diagram of a transcutaneous surface scanning electrode device, according to the present invention, and
[0036] [0036]FIG. 2 is a schematic diagram depicting the monitoring of an ankle joint angle by an electrogoniometer, and the resultant feedback control on the potentiometer settings.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0037] The present invention is a surface neuroprosthetic device that enables facile adjustment and fine-tuning of the local current density over the surface of a transcutaneous scanning electrode, so as to achieve optimal muscle response.
[0038] The transcutaneous surface electrode of the present invention allows for adjustment of the local current density, by the user, while the device is stimulating, hence giving the user direct feedback of the efficacy of the adjustment. This enables the user to set up the device on his limb, and carry out the fine adjustment of the electrode position by observing and feeling the limb response to the adjustment. Having achieved optimal response, the patient works with the device until he finishes his exercise, or until the electrode requires an additional readjustment.
[0039] The principles and operation of the system and method according to the present invention may be better understood with reference to the drawing and the accompanying description.
[0040] 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 the arrangement of the components set forth in the following description or illustrated in the drawing. The invention is capable of other embodiments or of being practiced or carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein is for the purpose of description and should not be regarded as limiting.
[0041] The basis for the present invention is best understood against the background of the known art. One main drawback of the art taught by the above-referenced patent to Axelgaard is that the control of the local current density is achieved by switching in and out a plurality of conductive inkspots ranged as a two-dimensional grid. This requires very high level of expert knowledge on the part of the patient to understand the correspondence between switching in or out of an inkspot and the resulting change in limb posture and movement. Having made a change to the stimulation field distribution over the electrode surface, the patient has no methodically logical means to know how to proceed further with the adjustment
[0042] Referring now to the drawing, FIG. 1 is a schematic diagram of a transcutaneous surface scanning electrode device for FES of impaired limbs, according to the present invention.
[0043] A scanning electrode 10 , which conforms to the site for which it is intended, preferably has the approximate shape of the skin region over the intended stimulation site. Scanning electrode 10 includes conductive area 20 and conductive area 30 , separated by insulating area 25 . Insulating area 25 may simply be a gap between conductive areas 20 and 30 , or alternatively, insulating area 25 may consist of a material having a significantly reduced electrical conductivity with respect to the materials used in conductive areas 20 and 30 .
[0044] A potentiometer 40 , powered by stimulation current source 50 , is electrically connected to conductive areas 20 and 30 . A first end of potentiometer 40 is connected via electrical wire 38 a and via conductive connectors 35 a to conductive area 30 . A second end of potentiometer 40 is connected via electrical wire 38 b and via conductive connectors 35 b to conductive area 20 . Conductive connectors 35 a and 35 b are disposed on conductive areas 30 and 20 , respectively. Potentiometer 40 is connected to a muscle stimulator 50 .
[0045] Potentiometer 40 is used to produce a substantially continuous electrical field across scanning electrode 10 , the field having a gradient between conductive area 20 and conductive area 30 . The bias of the electrical field is adjusted by means of moving lever 45 of potentiometer 40 , as will be explained in further detail hereinbelow.
[0046] Scanning electrode 10 is intended to be positioned within the neuroprosthesis such that when placed on to the body limb, scanning electrode 10 overlies the body of a single target muscle, of multiple target muscles, or muscle/nerve complex such that adjustment of the electrode field bias by moving lever 45 of potentiometer 40 in one direction tends to direct the limb posture or limb movement correction to the same direction—allowing proprioceptive and hence “obvious” or “natural” control of the limb. The simplicity afforded by the present invention, of lever 45 -controlled movement corresponding to limb movement adjustment, allows a patient to carry out a time-consuming and difficult adjustment of the electrode placement, in a very fast and simple manner. Consequently, the patient can effectively use the neuroprosthesis at home on a daily basis, without clinical supervision.
[0047] It must be emphasized that in contrast to a regular stimulation electrode, which generates a spatially fixed electrical field in the underlying body tissue, the scanning electrode utilized in the present invention enables the user-guided movement of the electrical field through the tissue.
[0048] It must be further emphasized that while the scanning electrode described hereinabove is a transcutaneous stimulation electrode, other electrode types fall within the broad scope of the invention, including various implanted scanning electrodes, e.g., scanning electrodes for direct stimulation of nerves disposed on adjacent nerve branches, scanning micro-electrodes for direct stimulation of nerve fascicles, scanning epimysial electrodes contacting the muscle epimysium, and scanning electrodes for intramuscular implantation.
[0049] Other possible ways for the system user to adjust the scanning electrode may depend on availability of residual voluntary movements that can be utilized by the user to slide potentiometer lever 45 . Voice commands and EMG (electromyograph)-triggered input command systems are well-known technologies that could be applied to control the distribution of the stimulation between the two sections of the scanning electrode. Instead of potentiometer 40 , other electronic means could be used to control the distribution of the stimulation current between the two sides of the scanning electrode.
[0050] The sliding of lever 45 of potentiometer 40 to one extreme position of slider 48 elicits one extreme of motion or of posture; moving lever 45 to the other extreme of slider 48 elicits the other motion or posture extreme. A full-range value of typically 500Ω, is suitable for the resistor of potentiometer 40 . The patient can also slide lever 45 to any position between these two extremes of slider 48 in order to elicit an intermediate motion or posture, as desired.
[0051] As used herein in the Specification and in the claims section that follows, the term “typical user” refers to a user having routine knowledge and experience with neuroprosthetic devices. The term “typical user” is meant to specifically exclude doctors, clinicians, etc., having expertise in the field of neuroprostheses.
[0052] As used herein in the Specification and in the claims section that follows, the term “monotonic” is used in the mathematical sense to refer to a sequence or set of points, the successive members of which either consistently increase or decrease, but do not oscillate in relative value. In a preferred embodiment of the scanning electrode of the instant invention, the stimulation current is distributed across regions of at least one scanning electrode to produce a monotonically increasing or decreasing stimulation field.
[0053] Even if moving lever 45 is oriented in a direction that is not proprioceptive, e.g., in a forward-backward orientation instead of the above-described left-right orientation, there are several inventive distinctions with respect to the prior art. Moving lever 45 , which could be a knob or another type of activator known in the art, provides the user with an intuitive means of controlling the limb, similar to moving a knob or lever for proprioceptive centering of the stereophonic output between two speakers using audio feedback. The desired position lies upon a continuum. The user can perform a tuning operation, moving the knob or lever back and forth until the optimal position is attained, for example, rotating his foot to the left and to the right until the foot points straight forward. It is intuitively obvious to the user to reverse the direction of the knob or lever once the optimal point has been passed, such that the user can move towards the optimal point with confidence and certainty, and in the event that the point has been passed, the user can also return towards the optimal point with confidence and certainty.
[0054] Moreover, in sharp contrast to the device disclosed by U.S. Pat. No. 6,038,485, the adjustment is continuous, and is designed to be effected while the device is stimulating. The user can see the change in movement or posture visually, while carrying out the proprioceptive adjustment of lever 45 . This arrangement allows simple, fast fine-tuning of the effective position of electrode 10 while the neuroprosthesis is in use.
[0055] It follows from all of the above that the donning and adjusting of a neuroprosthesis device with a scanning electrode of the present invention can be done by the user whenever he wishes, without the help of a clinician or other trained personnel.
[0056] In another preferred embodiment, automatic self-tuning of the neuroprosthesis is enabled by utilizing a sensor such as an electrogoniometer, force sensors or electromyographic monitoring to sense the movement or posture of the limb, and to provide feedback information thereon. The potentiometer could be adjusted in closed loop to optimize or balance the biomechanical output.
[0057] The monitoring of an ankle joint angle by an electrogoniometer 75 is illustrated schematically in FIG. 2. The correction required to reach the target ankle joint angle is used in a feedback loop 80 to adjust/control potentiometer 40 , which carries out the desired correction to the distribution of the stimulation current over scanning electrode 10 , and the muscle activation is modulated to achieve this correction. As in FIG. 1, potentiometer 40 is connected to a muscle stimulator 50 .
[0058] Although 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. Accordingly, it is intended to embrace all such alternatives, modifications and variations that fall within the spirit and broad scope of the appended claims. All publications, patents and patent applications mentioned in this specification are herein incorporated in their entirety by reference into the specification, to the same extent as if each individual publication, patent or patent application was specifically and individually indicated to be incorporated herein by reference. In addition, citation or identification of any reference in this application shall not be construed as an admission that such reference is available as prior art to the present invention. | A scanning electrode system for a neuroprosthetic device, the system enabling facile adjustment and fine-tuning of a spatial distribution of a local electrical stimulation field across a scanning electrode, by a system user, the scanning electrode system including: (a) at least one scanning electrode for the neuroprosthetic device, the scanning electrode for performing functional electrical stimulation (FES) of at least one muscle of a limb of the user; (b) a distribution mechanism for distributing a current to the at least one scanning electrode so as to produce a biased electrical stimulation field across the at least one scanning electrode, the distribution mechanism for operative connection to a muscle stimulator providing electrical stimulation to the scanning electrode system, and (c) control means for adjustment of the biased electrical stimulation field by means of the distribution mechanism, the control means designed and configured so as to be accessable to and operable by the system user. | 0 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of an earlier filing date from U.S. Provisional Application Ser. No. 61/985,104 filed Apr. 28, 2014, the entire disclosure of which is incorporated herein by reference.
BACKGROUND
[0002] In the downhole industry ubiquitous use is made of packers of all sorts. Advancements over the years have made them nearly impervious to chemical or thermal attack and they work extremely well for their various intended purposes. One condition inherent in packer use that continues to be a noticeable detriment is the extrusion gap or the annular space between a tubular against which the packer is to seal and the mandrel or other structure having a gage diameter less than that of the inside diameter of the tubular against which the packer is intended to seal. It is of course axiomatic that such a gap must exist as if it did not, the difficulty with which components run into the tubular against which the packer is intended to seal would be overwhelming and hence contraindicated. Many different back up configurations have been tried with varying success to reduce the extrusion gap but the art always welcomes other apparatus that will allow for reduction in the extrusion gap either more effectively or in additional scenarios.
SUMMARY
[0003] An extrusion gap reduction device includes an outer housing; an inner housing movably disposed relative to the outer housing; and a plurality of petals movably connected to the inner housing, one or more of the plurality of petals including a follower responsive to a cam surface of the outer housing.
[0004] A packer system includes an element; and at least one extrusion gap reduction device including an outer housing; an inner housing movably disposed relative to the outer housing; and a plurality of petals movably connected to the inner housing, one or more of the plurality of petals including a follower responsive to a cam surface of the outer housing.
BRIEF DESCRIPTION OF DRAWINGS
[0005] FIG. 1 is a perspective view of an extrusion gap reduction device in a closed position;
[0006] FIG. 2 is a perspective view of the device illustrated in FIG. 1 with the outer housing removed to allow visualization of the more radially inwardly located components of the device;
[0007] FIG. 3 is the device illustrated in FIG. 1 in a set position still in perspective view;
[0008] FIG. 4 is the device illustrated in FIG. 1 in a set position from one end;
[0009] FIG. 5 is a perspective view of another embodiment of the device illustrated in FIG. 1 with the outer housing removed to allow visualization of an alternate petal configuration;
[0010] FIG. 6 is a perspective view of a packer system having an element and an extrusion gap reduction device of FIG. 1 at each axial end of the element;
[0011] FIGS. 7-9 illustrate alternate edge shapes.
DETAILED DESCRIPTION
[0012] Referring to FIGS. 1 through 4 simultaneously, the device 10 comprises an outer housing 12 and an inner housing 14 that are rotatable relative to one another. The degree of relative rotation between the outer housing 12 and the inner housing 14 is limited by a groove 16 (see FIG. 2 ) located in inner housing 14 and a lug 18 configured to move with the outer housing 12 . In the illustrated embodiment, the lug 18 is affixed to outer housing 12 . It is to be understood that any means of attachment to the outer housing would be acceptable and is contemplated in order to prevent motion between the lug and the outer housing that would affect outer housing to inner housing relative position. For example the lug could be press fit, welded, adhesively affixed, integrally machined, etc. It is not required that the lug 18 not, for example, spin relative to outer housing 12 .
[0013] Further illustrated in each Figure is a plurality of petals 20 . Each petal is independently rotatable about a connection such as, for example, a pivot pin 22 and positionally affected by a displacement follower 24 such as a pin. The relative rotation between the outer housing 12 and the inner housing 14 causes the displacement followers to each ride a cam surface 26 from a recess 28 to an outside surface 30 of the outer housing 12 . It is to be noted however that while the followers 24 riding onto outside surface 30 is illustrated, it is of course contemplated that the followers 24 need not actually exit the recesses 28 but rather only that the petals collectively actually achieve a larger diametric dimension in the set position than in the closed position. This can occur with the cam surface urging the displacement followers 24 radially outwardly even though the followers are not displaced enough to reach the outer housing surface 30 and such might occur in a tubular that is somewhat smaller diametrically than one for which the device 10 is specifically designed. It is also contemplated that a particular device is not intended to use the outer surface of outer housing 12 in order to, for example, maintain the displacement followers 24 in a more protected condition within the outer housing 12 when in the set position, for example, in an embodiment where the recesses are closed grooves instead of open as illustrated.
[0014] The number of petals may be as illustrated or may be another number as desired for a particular application. The more petals that are used, the closer the resultant outside dimensions of the flower will be to the inside surface of the tubular against which the packer is intended to be set, assuming the tubular is circular in cross section.
[0015] In one embodiment, as shown, each petal is configured as a simple arcuate section and produces the shape of petals illustrated in FIG. 4 . One will notice that the outermost surface in FIG. 4 is more flowerlike than a circle. This leaves much smaller extrusion gaps than would exist without the device described herein and the remaining gaps are not annularly complete so the device will in this configuration significantly reduce extrusion. In this embodiment, the arc length of each petal is sufficient to span a distance between a next adjacent petal of the plurality of petals on both sides of the subject petal. In another embodiment, referring to FIG. 5 , the extrusion gap can be reduced even further by modifying the shape of the of the petals to have a first region 32 that is roughly curved to exhibit an arcuate edge 34 to roughly match the outer surface 30 of the outer housing while a second region 36 is roughly curved to approximate the inside diameter of the tubular. In this way, the coverage will be complete when deployed but still allow collapse to the gage diameter of the outer housing. In other embodiments, the edge 32 or 36 need not be arcuate but may be linear or even reverse arcuate or other shapes (see FIGS. 7 , 8 and 9 ). The second region 36 may also be linear or reverse arcuate or other shapes. Where the edge is arcuate, it will have an arc length sufficient to span a distance between where the first and second regions meet and a next adjacent petal's second region to provide for the complete coverage against extrusion noted above.
[0016] Referring to FIG. 6 , a packer system is illustrated having the extrusion gap reduction devices 10 disposed at either axial end of a packing element 40 . It will be understood that a product could be configured this way or could be configured with one of the devices 10 and not the one on the opposite side of the packing element. It is also to be understood that any kind of packing element 40 can be substituted for that shown.
[0017] A borehole with the packer system illustrated is beneficial to the industry as the element is better contained and will be more resistant to extrusion than an equivalent element used without the device(s) described herein.
[0018] It will be understood that the operable parts can be reversed such that the petals are pinned to the outer housing and cammed with the inner housing rather than described above without departing from the scope of the invention.
[0019] While the invention has been described with reference to an exemplary embodiment or embodiments, 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 not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out this invention, but that the invention will include all embodiments falling within the scope of the claims. Also, in the drawings and the description, there have been disclosed exemplary embodiments of the invention and, although specific terms may have been employed, they are unless otherwise stated used in a generic and descriptive sense only and not for purposes of limitation, the scope of the invention therefore not being so limited. Moreover, the use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another. Furthermore, the use of the terms a, an, etc. do not denote a limitation of quantity, but rather denote the presence of at least one of the referenced item. | An extrusion gap reduction device includes an outer housing; an inner housing movably disposed relative to the outer housing. A plurality of petals movably connected to the inner housing. One or more of the plurality of petals including a follower responsive to a cam surface of the outer housing. | 4 |
STATEMENT OF RELATED APPLICATIONS
This patent application claims priority on German Patent Application No. DE 10 2013 009 795.9 having a filing date of 12 Jun. 2013.
BACKGROUND OF THE INVENTION
1. Technical Field
The invention relates to an arrangement for filling watering cans.
2. Prior Art
Typical watering cans for use in the garden have on their top side a large filling opening and a handle which extends in a curved manner over the opening. Filling the watering can from a tap or by means of a garden hose is time-consuming and/or tedious.
BRIEF SUMMARY OF THE INVENTION
It is the object of the invention to create an arrangement for quicker or easier filling of watering cans.
The arrangement according to the invention is an arrangement for filling watering cans, having a container for receiving liquid, wherein the container is assigned a closable outlet and an in particular closable inlet. A constituent part of the arrangement is a container for receiving liquid, wherein the container is assigned a closable outlet and an in particular closable inlet. Via the inlet, the container can be filled even in the absence of a watering can. The outlet can be dimensioned such that quick filling of the watering can is possible. A common type of watering can has a volume of about 10 liters. Complete filling can take place with a sufficiently large outlet in about 10 seconds or less. The volume flow is then 1 liter per second or more. Filling takes place in a pressureless manner, that is to say only atmospheric pressure and no positive pressure bears down on the liquid column in the container.
According to a further concept of the invention, an effective cross section of the outlet is larger than an effective cross section of the inlet, in particular at least four times as large. Preferably, the outlet is ten times as large as the inlet or larger. A filled watering can is emptied slowly in the garden while the water flows into the container. If the watering can is empty, it can be filled again from the container in a very short period of time.
According to the invention, the inlet may be assigned a closure which automatically closes the inlet as soon as the liquid in the container has reached an upper liquid level or a defined quantity of liquid has flowed into the container. As a result, it is possible to connect the container to a water line that is always open, without the container overflowing.
Advantageously, the closure for the inlet is actuable by a float in the container. The principle for a closure, controlled by a float, of a water line is known from cisterns for toilets and does not need to be explained in more detail.
According to the invention, the inlet may be assigned a connection for a water line or a garden hose, in particular a plug-in coupling, preferably for a ½″ or ¾″ coupling. These are commercially customary coupling sizes for garden hoses. Of course, other sizes can also be used.
Alternatively, the inlet may also be connected to a downpipe for roof drainage (gutter) directly or via a line/hose. In this case, operation without a float is also possible, since the connection is pressureless. Finally, the connection to the downpipe may also be provided in addition to the connection for a garden hose or some other waterline.
According to a further concept of the invention, the outlet may be assigned a manually operable closure which has to be actuated only for the purpose of opening and closes again automatically, in particular after a defined quantity of liquid has run through, when the container is empty or after a defined period of time has elapsed. The principle of manual opening and automatic closing is likewise known from cisterns in toilets. As a result, operation is particularly easy.
Preferably, the outlet is assigned a siphon bell which closes an end opening or container opening and is liftable for the purpose of opening. The lifting of the siphon bell can take place manually via a linkage or a cable pull or by a change of pressure in the container or in some other way. The use of a siphon bell is again known in connection with cisterns for toilets.
The opening and closing of the outlet can take place in various ways, for example manually, pneumatically, hydraulically and/or electrically. Preferably, opening is carried out manually, while closing of the outlet takes place automatically after a defined quantity of liquid has run through, when the container is empty or after a defined period of time has elapsed. For the purpose of closing and optionally also for the purpose of opening, an electrically actuated valve can also be provided, in particular in conjunction with an electronic unit for control purposes. A time interval for example is stored in the electronic unit. The time interval starts when the outlet is opened. After the time interval has elapsed, the valve receives a signal for closing. Alternatively or in addition, a flow meter can be provided. Once a previously defined flow rate has been achieved, the valve receives a signal for closing.
According to the invention, the outlet may have an outflow nozzle which is configured in a curved manner such that a free nozzle opening is not located in a central upright container plane under the container but is located at a distance in front of the upright container plane. The height and width dimensions of the container define the upright container plane, which extends approximately centrally through the container. In this case, the container may have a relatively small depth (dimension perpendicular to the upright container plane). The depth may be smaller than the corresponding dimension of a watering can to be filled, on account of the curved outflow nozzle. The outflow nozzle is preferably arranged such that, while the watering can indeed stand underneath the container during filling, it is offset in an inclined manner with respect thereto, that is to say at a distance from the upright container plane. In this case, the outflow nozzle passes between the opening in the watering can and the curved handle thereof. The outlet is advantageously provided in the region of a lowest point of the container in order that no solids can accumulate in the container. Preferably, the outlet is arranged in a bottom wall of the container or in a side wall of the container close to the bottom wall.
According to a further concept of the invention, the arrangement may have securing means for securing to a wall. In the simplest case, holes are provided for suspending on hooks in the wall. However, height-adjustable securing means, for instance a rail having lockable slides arranged thereon, are also possible. Preferably, the slides are then assigned to the arrangement and the rail is assigned to the wall.
According to the invention, the container may be embodied as floor-standing model or a holder for the container may be provided, such that an outlet opening of the container, or a lower container opening, is arranged at a distance from the ground, in particular at a distance of about half a meter. The holder may be provided as a stand for standing on the ground or for leaning against and/or securing to a wall. The distance from the ground should be dimensioned such that a watering can provided for the arrangement can be positioned easily under the outlet opening.
Advantageously, the container functions according to the principle of a toilet cistern and is constructed in a corresponding manner, in particular with a float-controlled inlet and torrent-like emergence of the water.
A further subject of the invention is also an ensemble made up of an arrangement of the abovementioned type and a watering can, wherein the watering can has on its top side a filling opening, and wherein the arrangement is assigned a holding device which holds the container at a height such that an outlet opening on the container, or a lower container opening or a nozzle opening, is arranged approximately in the region of the opening for filling the watering can or thereabove. The aim is a distance of at most 1 to 2 centimeters. The watering can can then be positioned easily under the outlet opening and be moved away again after filling. Spray scarcely occurs.
BRIEF DESCRIPTION OF THE DRAWINGS
Further features of the invention can be gathered from the rest of the description and from the claims. Advantageous embodiments of the invention are explained in more detail in the following text with reference to drawings, in which:
FIG. 1 shows a lateral plan view of an arrangement for filling together with a watering can standing therebeneath,
FIG. 2 shows a side view of the arrangement from FIG. 1 ,
FIG. 3 shows a top view of the arrangement from FIG. 1 ,
FIG. 4 shows a perspective illustration of an arrangement for filling watering cans,
FIG. 5 shows a lateral plan view of the arrangement according to FIG. 4 ,
FIG. 6 shows a cross section of the arrangement along the line VI-VI in FIG. 5 ,
FIG. 7 shows a lateral plan view of a further embodiment of the arrangement,
FIG. 8 shows a cross section of the arrangement along the line VIII-VIII in FIG. 7 .
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
A filling arrangement for watering cans has a container 10 for receiving water. The container 10 is intended to be secured to an upright wall (not shown), for instance to an outside wall of a house. To this end, the container 10 is formed in a relatively flat manner, specifically with a small depth, in relation to height and width. The height and width in this case define an upright container plane 11 which extends approximately centrally through a lower container opening 12 .
An outflow nozzle 13 which is connected to the container opening 12 by way of a threaded flange 14 adjoins at the bottom of the container opening 12 . The outflow nozzle 13 is configured in an elbowed manner with a free nozzle opening as the outlet opening beneath the container opening 12 and offset with respect to the container plane 11 .
Beneath the container 10 , a watering can 16 is positioned on a stand 17 . On its side, the watering can has a spout pipe 18 and, above a top side 19 , a handle 20 . Underneath the handle 20 , the top side 19 is provided with an opening which is not visible in the figures. The watering can 16 is positioned on the stand 17 such that the nozzle opening 15 is directed precisely into the opening in the top side 19 . Accordingly, the watering can 16 does not stand in the upright container plane 11 but in front of the latter, see in particular FIG. 2 .
In its upper region, the container 10 has on its side a connection 21 , specifically a plug connection for connecting a garden hose. Provided in a manner not shown in the interior of the container 10 is a closure for the connection 21 that acts as an inflow, in particular in conjunction with a float, such that the connection 21 closes automatically as soon as a defined water level has been reached in the container 10 .
The watering can 16 is filled like the water inlet in the case of a toilet cistern. The container 10 is filled relatively slowly from a garden hose. On account of the automatic closure in the region of the connection 21 , the garden hose can remain attached. The supply of water does not have to be turned off.
In order to let the water out of the container 10 , two variants are shown in the figures, specifically FIGS. 4 to 6 for one and FIGS. 7 to 8 for the other. In both variants, the lower container opening is closed by a siphon bell 22 and, in order to let out the water, the siphon bell 22 has to be lifted. According to FIGS. 4 to 6 , a linkage having a pull lever 23 is provided for this purpose. By contrast, FIG. 8 shows a push button 24 by way of which a pressure change is briefly generated in the container 10 such that the siphon bell 22 is briefly lifted as a result or a stored water volume is discharged in some other way.
By way of the pull lever 23 or the push button 24 , the lower container opening 12 is opened and the container contents pour in a torrent into the watering can 16 through the outflow nozzle 13 . The cross sections of the outflow nozzle 13 and the container opening 12 are dimensioned in a relatively large manner with respect to the connection 21 , so that approximately 0.5 to 2 liters per second of water can flow out, even more in the case of larger cross sections. With a container content of 8 to 10 liters, a conventional 1-liter watering can can be filled with a torrent of water for example within 10 seconds.
LIST OF REFERENCE SIGNS
10 Container
11 Upright container plane
12 Lower container opening
13 Outflow nozzle
14 Threaded flange
15 Nozzle opening
16 Watering can
17 Stand
18 Spout pipe
19 Top side
20 Handle
21 Connection
22 Siphon bell
23 Pull lever
24 Push button | An arrangement for filling watering cans ( 16 ), having a container ( 10 ) for receiving liquid, wherein the container is assigned a closable outlet and an in particular closable inlet. In this case, an effective cross section of the outlet may be larger than an effective cross section of the inlet. | 8 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a method for the formation of a multilayer film and more particularly to a method for the formation of a multilayer film constituting itself such a semiconductor device as a thin-film transistor.
2. Description of the Related Art
Methods for forming a multilayer film on a substrate by plasma discharge have been known for long. One of the methods utilizes parallel planar electrodes to generate plasma. This method consists in forming a deposited film on a substrate or on a film already formed on a substrate by introducing a material gas into a reduced-pressure reaction chamber provided with parallel planar electrodes and supplying a high-frequency electric power between the electrodes thereby generating a plasma therein. To generate the plasma state, a microwave discharge and a electron cyclotron resonance have been known other than high frequency discharge. A multilayer film is formed by repeating this procedure.
The manufacture of thin-film transistors, solar cells, etc. by the application of the method for the formation of a multilayer film to processes for the production of semiconductor devices has been realized. Particularly, thin-film transistors (TFT) have been attracting keen attention on account of their adaptability for liquid crystal display devices and contact sensors. As respects the TFT's for use in the liquid crystal display devices, amorphous silicon (a-Si) type semiconductors are mainly used because they allow their active layers to enjoy a large increase in surface area and they can be formed at a relatively low temperature. For the a-Si type TFT's, the inverted staggered (bottom gate) construction or the normal staggered (top gate) construction in which a gate electrode is disposed on one side and a source electrode and a drain electrode are disposed on the other side of a semiconductor film formed of an a-Si film to serve as an active layer are adopted often.
For the multilayer films which function as semiconductor devices, the qualities of the interfaces between the component films of the multilayer film are extremely important. The interface between a gate insulating film and a semiconductor film in a TFT, for example, constitutes itself a channel for the TFT and plays an extremely important role in improving the switching characteristics of the TFT. The interface between the semiconductor film and a etching-stopper film on channel constitutes itself a rear channel for the TFT and plays a very important role in improving the switching characteristics of TFT similarly to the interface between the gate insulating film and the semiconductor film.
Heretofore, in the production of a inverted staggered type TFT, for example, a gas for the formation of a gate insulating film is introduced into a reduced-pressure reaction chamber provided with parallel planar electrodes and a high-frequency electric power is supplied between the electrodes so as to generate a plasma state and deposit a gate insulating film on a glass insulating substrate having a gate electrode formed in advance thereon. Subsequently, the plasma state is stopped, the reaction chamber is evacuated, and a gas for the formation of a semiconductor is introduced into the empty reaction chamber to generate a plasma state and deposit a semiconductor film. For the purpose of further forming a etching-stopper-film on channel on the semiconductor film, the plasma state is stopped after the deposition of the semiconductor layer, the reaction chamber is evacuated, and a gas for the deposition of an etching-stopper-film on the channel is introduced into the empty reaction chamber to generate a plasma state and deposit the etching-stopper-film on channel.
In the production of the TFT of the normal staggered construction, the order in which the gate insulating film and the semiconductor film are superposed is reversed.
When the formation of a multilayer film is effected by a method which comprises depositing a first film, then stopping a plasma state, and again generating a plasma state to deposit a second film, the plasma state in the initial stage of the deposition of the second film is unstable, a defective density (dangling bond) is formed near the interface between the first and the second deposited film, and the multilayer film is not formed in a desirable form because the films are blistered or separated.
When the production of a TFT is effected by a method which comprises depositing a gate insulating film or a semiconductor film as the first deposited film, then stopping a plasma state, and again generating a plasma state to deposit a semiconductor film or a gate insulating film as the second deposited film, the plasma state in the initial stage of the deposition of the second film is unstable and a defective density (dangling bond) is formed near the interface between the semiconductor layer and the gate insulating film. This method, therefore, is at a disadvantage in forming no satisfactory interface and conferring no ideal characteristics on the produced TFT. It further has the problem that the interface between the first and the second deposited film is blistered and separated to the extent of lowering the yield of production. The fact that the plasma state to be formed again after the stop of the first plasma state takes no small time before it is stabilized impairs the productivity of this method.
The same remarks hold good for the operation of forming a semiconductor film as the first deposited film and a etching-stopper-film on channel as the second deposited film.
Incidentally, a method causes a state of plasma to last between a step of cleaning and a step of film forming in the plasma CVD process for forming a metallic or a ceramic coating on the surface of a tool, a metal die, or a machine part is disclosed under the title of "method for formation of highly adhesive thin film by plasma CVD technique" in JP-A-63-79,970. This particular invention attains the retention of the state of plasma by means of an electrode adapted exclusively therefor in addition to a discharge electrode to be used for the formation of the coating.
This invention is incapable of optimizing the state of plasma because of purpose of this invention is not focused on formation of multilayer film, and it adjusts neither the distance between the electrodes nor the internal pressure of the reaction chamber during the retention of the plasma state between the steps of depositing films. It, therefore, produces a multilayer film containing ideally formed interfaces only with difficulty.
SUMMARY OF THE INVENTION
As described above, the methods heretofore adopted for the formation of a multilayer film are at a disadvantage in failing to form highly satisfactory interfaces between the component films of multilayer films because the plasma state is stopped or because the plasma state, if not stopped, cannot be optimized during the step of film forming. The fact that no satisfactory interfaces are formed entails the problem that the interfaces are blistered or separated to the extent of degrading the yield of production. When the multilayer film constitutes itself such a semiconductor device as a TFT, the inferior interfaces go to impair the characteristics of the device.
When the plasma state is once stopped, regeneration of the plasma state thereafter takes no small time before it is stabilized. The time thus spent goes to degrade the efficiency of the production.
The present invention has been produced for the purpose of solving such problems of the related art as are mentioned above. An object of this invention is to provide for the formation of a multilayer film a method which enables the interfaces of the component layers of the film to be formed highly satisfactorily.
Another object of this invention is to provide for the formation of a multilayer film which constitutes a semiconductor device, particularly a TFT, a method which allows a thin-film transistor of excellent characteristics by forming a highly satisfactory interface between a gate insulating layer and a semiconductor layer or between a semiconductor layer and a etching-stopper-film on channel.
Yet another object of this invention is to provide a method for forming a multilayer film with a highly satisfactory yield.
Still another object of this invention is to shorten the time spent in the component steps of process and improve the efficiency of the production.
The basic aspect of this invention resides in a method for forming a multilayer film by introducing a material gas into a reduced-pressure chamber and generating a plasma state therein by activating an electromagnetic field and depositing a film on a substrate disposed outside of the plasma state in the chamber, which method comprises the steps of (a) introducing a first material gas into the chamber and generating a plasma state therein by activating the electromagnetic field and depositing a first film on the substrate, (b) adjusting the electromagnetic field while continuously retaining the plasma state subsequently to step (a), and (c) introducing a second material gas into the chamber while continuously retaining the plasma state thereby generating the plasma state and depositing a second film on the first film.
The plasma state can be generated by a microwave discharge, a electron cyclotron resonance and a high frequency discharge. The remarks of the way of generating the plasma state hold good invariably hereinafter.
The aspect of this invention resides in a method for forming a multilayer film by introducing a material gas into a reduced-pressure reaction chamber provided with a pair of parallel planar electrodes and supplying a high-frequency electric power between the electrodes thereby generating plasma state therein and depositing a film on a substrate disposed on one of the electrodes or on a substrate having a predetermined film already formed thereon, which method comprises (a) a step of introducing a first material gas into the reaction chamber and supplying the high-frequency electric power between the electrodes thereby forming the state of plasma and producing a first film on the substrate disposed on one of the electrodes or on the substrate having a predetermined film already formed thereon and (b) a step of introducing a second material gas into the reaction chamber while retaining the state of plasma without interruption thereby producing the state of plasma and forming a second film on the first deposited film.
As a result, the state of plasma is retained without interruption at least from the start of the formation of the first deposited film through the completion of the formation of the second deposited film.
The method for the formation of a multilayer film according to this invention naturally can be applied to the continuous formation of an additional deposited film on the second deposited film which has been formed as described above. To be specific, this addition of the deposited film is attained by using the second deposited film as the first deposited film and superposing thereon the new deposited film. It is naturally allowable to give a stated treatment such as, for example, an etching treatment to the multilayer film already formed and superpose a deposited film on the treated multilayer film.
The method for the formation of a multilayer film according to this invention, therefore, may be combined with a predetermined treatment for the purpose of manufacturing such devices as a TFT, a liquid crystal display device, and a solar cell, etc.
The same remarks hold good for the following aspects of this invention unless otherwise specified.
Other aspect of this invention resides in a method for forming a multilayer film by introducing a material gas into a reduced-pressure reaction chamber provided with at least one pair of parallel planar electrodes and supplying a high-frequency electric power between the electrodes thereby generating plasma state therein and depositing a film on a substrate disposed on one of the electrodes or on a substrate having a predetermined film already formed thereon, which method comprises (a) a step of introducing a first material gas into the reaction chamber and supplying the high-frequency electric power between the electrodes thereby generating the plasma state and depositing a first film on the substrate disposed on one of the electrodes or on the substrate having a predetermined film already formed thereon, (b) a step of effecting stepwise adjustment of the distance between the electrodes while continuously retaining the plasma state without interruption subsequently to the step of (a), and (c) a step of introducing a second material gas into the reaction chamber continuously while retaining the plasma state without interruption thereby producing the plasma state and depositing a second film on the first film.
As a result, the plasma state is continuously generated without interruption at least from the start of the deposition of the first film through the completion of the deposition of the second film.
As regards the second material gas, it is desirable that the components thereof be introduced stepwise.
Yet, other aspect of this invention resides in a method for forming a multilayer film by introducing a material gas into a reduced-pressure reaction chamber provided with at least one pair of parallel planar electrodes and supplying a high-frequency electric power between the electrodes thereby generating plasma state therein and depositing a film on a substrate disposed on one of the electrodes or on a substrate having a predetermined film already formed thereon, which method comprises (a) a step of introducing a first material gas into the reaction chamber and supplying the high-frequency electric power between the electrodes thereby generating the plasma state and depositing a first film on the substrate disposed on one of the electrodes or on the substrate having a predetermined film already formed thereon, (b) a step of making stepwise introduction into the reaction chamber of a preparatory gas constituting itself one of the components of the second material gas and not forming substantially in itself a second film while continuously retaining the state of plasma without interruption subsequently to the step of (a), (c) a step of effecting stepwise adjustment of the distance between the electrodes while continuously retaining the plasma state without interruption, and (d) a step of introducing a second material gas into the reaction chamber while continuously retaining the plasma state without interruption thereby generating the plasma state and depositing a second film on the first deposited film.
As a result, the plasma state is continuously retained without interruption at least from the start of the deposition of the first film through the completion of the deposition of the second film.
The adjustment of the distance between the electrodes in this invention is basically carried out by increasing the distance between the electrodes when the internal pressure of the reaction chamber falls and decreasing the distance when the internal pressure rises.
As the preparatory gas, at least one member selected from the group consisting of H 2 , He, Ar, N 2 , NH 3 , N 2 O, and Kr may be used.
The remarks of the preparatory gas hold good invariably hereinafter.
Further, other aspect of this invention resides in a method for forming a multilayer film by introducing a material gas into a reduced-pressure reaction chamber provided with at least one pair of parallel planar electrodes and supplying a high-frequency electric power between the electrodes thereby generating plasma state therein and depositing a film on a substrate disposed on one of the electrodes or on a substrate having a predetermined film already formed thereon, which method comprises (a) a step of introducing a first material gas into the reaction chamber and supplying the high-frequency electric power between the electrodes thereby forming the state of plasma and producing a first film on the substrate disposed on one of the electrodes or on the substrate having a predetermined film already formed thereon, (b) a step of making multistage introduction into the reaction chamber of a preparatory gas made of gas or dilute gas constituting itself one of the components of the second material gas and not forming substantially in itself a second film while retaining the state of plasma without interruption subsequently to the step of (a), (c) a step of effecting multistage adjustment of the pressure in the reaction chamber to the exhaust gas pressure or to a level equal to or lower than the pressure existing at the step of forming the second deposited film while retaining the state of plasma without interruption, (d) a step of effecting multistage adjustment of the distance between said electrodes while retaining the state of plasma without interruption, and (e) a step of introducing a second material gas into the reaction chamber while retaining the state of plasma without interruption thereby producing the state of plasma and forming a second film on the first deposited film.
There is a sequence between the steps of the film deposition the pressure which exists in the state in which the introduced gas is flowing into the reaction chamber and not to the state of vacuum. The multilayer film to be formed is allowed to acquire a highly desirable interface when the pressure existent during the formation of a deposited film is adjusted to a level equal to or lower than the pressure which exists during the step of film forming.
The distance between the electrodes is subjected to multi-stage adjustment in conformity with the internal pressure of the reaction chamber so as to ensure retention of the state of plasma without interruption.
As a result, the state of plasma is retained without interruption at least from the start of the formation of the first deposited film through the completion of the formation of the second deposited film.
As described above, this invention allows formation of a plurality of deposited films while continuously retaining the plasma state without interruption.
The term "plasma state" refers to the state in which a gas is decomposed into an ion and an electron, and is not dependent on the gas species generating the plasma. Therefore the plasma state is able to retain continuously though the gas species changed.
It also allows optimization of the plasma state between the step for the formation of a deposited film and the step for the film deposition.
By entirely the same procedure, a multilayer film for constituting a TFT can be formed.
To be specific, the multilayer film constituting itself a stated TFT can be produced by forming an insulating film, a semiconductor film, and a semiconductor protective film as deposited films.
In the method for the formation of a multilayer film which is composed of a gate insulating film, a semiconductor film, and an etching-stopper-film on the channel to constitute itself a thin-film transistor, the formation of the semiconductor film on the gate insulating film is attained by effecting stepwise adjustment of the distance between the discharge electrodes while retaining the plasma state subsequently to the formation of the gate insulating film and then forming the semiconductor film and the formation of the etching-stopper-film on channel on the semiconductor film is attained by effecting stepwise adjustment of the distance between the discharge electrodes while retaining the plasma subsequently to the formation of the semiconductor film and then forming the etching-stopper-film on channel.
This invention, as described above, concerns a method for forming a multilayer film while continuously retaining a state of plasma without interruption. The state of plasma between the steps for formation of a deposited film can be optimized by adjusting such conditions as the distance between the electrodes, the kinds of gas introduced, the internal pressure of the reaction chamber, and the magnitude of the high-frequency electric power supplied. Thus, a multilayer film of uniform quality can be formed from a stable plasma state. The multilayer film possesses a highly desirable interface because of freedom from blister or separation. The multilayer film is formed in a high yield. Since the state of plasma does not need to be reformed, the time spent for the formation of the multilayer film can be decreased and the efficiency of the production can be improved.
Thus, the TFT to be consequently produced is enabled to acquire outstanding characteristics mainly because the defective density (dangling bond) near the interface between the gate insulating film and the semiconductor film, the interface between the semiconductor film and the etching-stopper-film on channel, and the interface between the semiconductor film and the gate insulating film is decreased.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view showing a construction of a inverted staggered TFT in the example 1.
FIG. 2A is a sectional view showing the TFT of FIG. 1 according to a prossesing scheme.
FIG. 2B is a sectional view showing the TFT of FIG. 1 according to a prossesing scheme.
FIG. 2C is a sectional view showing the TFT of FIG. 1 according to a prossesing scheme.
FIG. 2D is a sectional view showing the TFT of FIG. 1 according to a prossesing scheme.
FIG. 2E is a sectional view showing the TFT of FIG. 1 according to a prossesing scheme.
FIG. 3 is a sectional view showing the construction of the essential part of an apparatus to be used for the formation of the multilayer film.
FIG. 4 is a sectional view showing a construction of a inverted staggered TFT in the example 2.
FIG. 5A is a sectional view showing the TFT of FIG. 4 according to a prossesing scheme.
FIG. 5B is a sectional view showing the TFT of FIG. 4 according to a prossesing scheme.
FIG. 5C is a sectional view showing the TFT of FIG. 4 according to a prossesing scheme.
FIG. 5D is a sectional view showing the TFT of FIG. 4 according to a prosseseing scheme.
FIG. 6 is a sectional view showing a construction of a normal staggered TFT in the example 3.
FIG. 7 is a sectional view showing the construction of a liquid crystal display device in the example 4.
FIG. 8 is a sectional view showing a multilayer film in the example 5.
FIG. 9 is a schematic diagram of the multilayer film processing in the example 5.
FIG. 10 shows the mobility of the TFT formed by the method of this invention.
FIG. 11 shows the threshold voltage of the TFT formed by the method of this invention.
FIG. 12 is a sectional view showing a multilayer film in the example 6.
FIG. 13 is a schematic diagram of the multilayer film processing in the example 6.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
EXAMPLE 1
The method of this invention for the formation of a multilayer film is applied to the manufacture of a inverted staggered (bottom-gate) TFT for use in an active matrix type liquid crystal display device.
FIG. 1 shows a TFT in an active matrix type liquid crystal display device of Example 1.
This TFT is composed of a gate electrode 2 of a predetermined shape formed of molybdenum-tantalum integrally with a gate line (not shown) on a glass insulating substrate 1, a gate insulating film 3 of SiN x formed in a thickness of 0.3 μm in such a manner on the insulating substrate 1 as to cover the gate electrode 2, a semiconductor film 4 of a predetermined shape formed of a-Si film, microcrystalline silicon, or polycrystalline silicon in a thickness of 0.05 μm in such a manner as to cover the gate insulating film 3 in conformity with the gate electrode 2, a etching-stopper-film on channel 5 of a predetermined shape formed of SiN x film in a thickness of 0.3 μm so as to cover part of the semiconductor film 4, a n type semiconductor film 6 of n + a-Si formed in a thickness of 0.05 μm in such a manner as to cover the etching-stopper-film on channel film 5 and a source region and a drain region on the semiconductor film, a source electrode 7 of chromium (cr) or aluminum (Al) superposed on the n type semiconductor film 6 as partly extended into the source region on the gate insulating film 3, a drain electrode 8 of Cr or Al formed likewise on the n type semiconductor film 6 as partly integrated with column lines (not shown) extended into the drain region on the gate insulating film 3, and an insulating protective film 9 of SiN x formed so as to cover the channel region on the source electrode 7, the drain electrode 8, and the n type semiconductor film 6. The source electrode 7 is connected to a pixel electrode 10 of ITO (indium tin oxide) formed on the gate insulating film 3.
Now, a typical method used for the manufacture of this TFT will be described below.
The manufacture of this TFT is started with the formation of a metal film of Mo-Ta by the sputtering technique on the glass insulating substrate 1. By photolithographically etching this metal film, the gate electrode 2 of the predetermined shape is formed in conjunction with the gate line (FIG. 2A).
The glass insulating substrate 1 having the gate electrode 2 formed thereon is set in place in a reaction chamber and heated to 623K. Then, a material gas for the deposition of the gate insulating film which is composed of silane (SiR 4 ), ammonia (NH 3 ), and nitrogen (N 2 ) is introduced into the reaction chamber and generated to a plasma state to form the gate insulating film 3 of SiN x having a thickness of 0.3 μm as shown in FIG. 2B.
Subsequently, with the plasma state existent during the deposition of the gate insulating film 3 retained continuously, the gas introduced into the reaction chamber is switched from the material gas for the deposition of the gate insulating film 3 to the hydrogen (H 2 ) or the helium (He) gas.
Next, the SiH 4 gas is introduced in conjunction with the H 2 or the He gas to form an a-Si film 4 as a semiconductor film in a thickness of 0.05 μm.
The introduction of the SiH 4 gas is subsequently stopped and, at the same time, the H 2 or the He gas is introduced with the plasma state continuously retained.
Then, the NH 3 gas is combined with the H 2 gas to continue the plasma state.
The introduction of the H 2 gas is stopped and the introduction of the N 2 gas is started to continue the plasma state.
The material gas for the deposition of the semiconductor protective film is produced by adding the SiH 4 gas to the NH 3 gas and the N 2 gas to produce a SiN x film 5 as the etching-stopper-film on channel 0.3 μm in thickness.
By photolithography method, etching this SiN x film 5, the etching-stopper-film on channel 5 is formed in the predetermined shape as shown in FIG. 2C.
Then, the glass insulating substrate 1 having the etching-stopper-film on channel 5 and other films formed thereon is heated and the gas formed of phosphine (PH 3 ) and SiH 4 for the formation of the n type semiconductor film is introduced to form a n + a-Si film in a thickness of 0.05 μm in such a manner as to cover the etching stopper film 5. Subsequently, by the photolithography method, this n + a-Si film is etched to form the n type semiconductor film 6 of the predetermined shape and the underlying a-Si film is etched to form the n type semiconductor film 4 of the predetermined shape as shown in FIG. 2D.
Thereafter, a transparent electrical conductive film of ITO is formed by the sputtering technique on the glass insulating substrate 1 having the n type semiconductor film 6 and other films formed thereon. This transparent electroconductive film is photolithographically etched to form the pixel electrode 10 of the predetermined shape at a stated position on the gate insulating film 3.
Further, on the glass insulating substrate 1 having the pixel electrode 10 and other films formed thereon, the metal film of Cr or Al is formed by the sputtering technique. Then, by the photolithography technique, the source electrode 7 for connecting the n type semiconductor film 6 and the pixel electrode 10 and the drain electrode 8 connected to the n type semiconductor film 6 are formed integrally with the column lines. The part of the n type semiconductor film 6 in the channel region is removed by the photolithographic etching technique as masked by the source electrode 7 and the drain electrode 8 FIG. 2E.
Thereafter, the insulating protective film of SiN x is formed by the plasma CVD method on the glass insulating substrate 1 having the source electrode 7, the drain electrode 8, and other films deposited thereon to complete the TFT (FIG. 1).
The method for the formation of the multilayer film which is composed of the SiN x gate insulating film, the a-Si semiconductor film, and the SiN x etching-stopper film on channel to constitute the inverted staggered type TFT will be described more specifically hereinbelow.
FIG. 3 shows the construction of the essential part of a apparatus to be used for the formation of the multilayer film. This device is the so-called plasma CVD device with the parallel planar electrode. Inside a reaction chamber 12, a disklike high-frequency electrode 13 about 15 cm in diameter is set in place and a disklike grounding electrode 14 of about the same diameter is disposed thereunder as opposed to the high-frequency electrode 13. This grounding electrode 14 is adapted to be vertically moved so as to change freely the distance thereof from the high-frequency electrode 13 accurately within ±0.01 mm by means of an elevating unit 15 disposed outside the reaction chamber 12. The reaction chamber 12 is adapted to be evacuated by an evacuating unit 16. Further, the reaction chamber 12 is provided on the outside thereof with a gas inlet unit 17 for introducing a series of material gas and a series of preparatory gas into the reaction chamber 12 from the high-frequency electrode 13 side. The grounding electrode 14 is provided with a resistance heating unit 18 for heating a glass insulating substrate 1 seated on the grounding electrode 14 accurately within ±10° C. A high-frequency power source 19 is connected to the high-frequency electrode 13.
The plasma state is generated by a high frequency discharge in the apparatus shown in FIG. 3. It is also applicable to generate the plasma state by a microwave discharge or a electron cyclotron resonance (ECR) employing a known apparatus.
First, the glass insulating substrate 1 having the gate electrode formed thereon is fixed on the grounding electrode 14 of the reaction chamber 12 of the device mentioned above and the reaction chamber 12 is evacuated. The glass insulating substrate 1 is heated to 623K by the resistance heating unit 18 disposed on the grounding electrode 14 and, as the material gas for the deposition of the gate insulating film, SiH 4 gas fed at a flow volume of 10 sccm, NH 3 gas at 60 sccm, and N 2 gas at 400 sccm are introduced into the reaction chamber 12. A plasma state is generated between the high-frequency electrode 13 and the grounding electrode 14 to form the gate insulating film of SiN x , with the internal pressure of the reaction chamber 12 adjusted at 0.8 Torr, the distance between the electrodes 13 and 14 at 30 mm, and the electric power supplied from the high-frequency power source 19 at 50 W.
At the same time that the introduction of the material gas for the deposition of the gate insulating film is stopped, the introduction of H x gas as the preparatory gas is started at a flow volume of 500 sccm. The plasma state existent during the formation of the gate insulating film mentioned above is retained without interruption with the internal pressure of the reaction chamber 12 adjusted at 0.3 Torr, the distance between the electrodes at 35 mm, and the electric power supplied from the high-frequency power source 19 at 35 W. This plasma state is desired to continue at least 3 seconds.
The influence of the material gas during the deposition of the gate insulating film can be eliminated by introducing the H 2 gas in a large amount and fixing the pressure of the gaseous atmosphere inside the reaction chamber 12 at 0.3 Torr as mentioned above. Further, the plasma state can be stably retained by setting the distance between the electrodes at such a large magnitude as 35 mm.
Then, the H 2 gas is introduced at a flow volume of 500 sccm. The plasma state is stably retained with the pressure inside the reaction chamber 12 fixed at 1.2 Torr, the distance between the electrodes at 28 mm, and the electric power supplied from the high-frequency power source 19 at 50 W.
Thereafter, the H 2 gas plus the SiH 4 gas are introduced as the material gas at a flow volume of 30 sccm. Thus, the semiconductor film of a-Si is deposited in a thickness of 0.05 μm, with the distance between the electrodes adjusted at 26 mm.
During the formation of the semiconductor film, the plasma state can be stably retained until the formation of the a-Si film by introducing H 2 as the preparatory gas and adjusting the internal pressure of the reaction chamber, the electric power to be supplied, and the distance between the electrodes. The dangling bond of the interface between the SiN x gate insulating film and the a-Si semiconductor film can be decreased by keeping the pressure prior to the formation of the a-Si film at a level lower than the pressure during the formation of the a-Si film.
Then, the introduction of the SiH 4 gas mentioned above is stopped and, at the same time, the introduction of H 2 gas as the preparatory gas is started at a flow volume of 500 sccm. The plasma state is retained without interruption by adjusting the internal pressure of the reaction chamber 12 at 0.3 Torr and, at the same time, adjusting the distance between the electrodes at 35 mm. This plasma state is desired to continue at least 5 seconds.
Subsequently, the hydrogen gas plus the NH 3 gas are introduced at a flow volume of 400 sccm. The plasma state is retained with the internal pressure of the reaction chamber 12 at 1.5 Torr, the distance between the electrodes at 24 mm, and the electric power supplied from the high-frequency power source 19 at 60 W. The state of plasma under the conditions mentioned above is desired to continue at least than 3 seconds.
Then, the introduction of the H 2 gas is stopped and, at the same time, the introduction of N 2 gas as the preparatorly gas is started at a flow volume of 500 sccm. The introduction of the NH 3 gas is still continued. The plasma state is stably retained by having the distance between the electrodes adjusted at 20 mm.
Subsequently, the SiH 4 gas is introduced at a flow volume of 50 sccm to form a material gas for deposition of an etching-stopper-film with the N 2 gas and NH 3 gas already introduced.
From the material gas with the plasma state continuously retained the SiNx etching-stopper-film on channel is deposited in a 0.3 μm thickness.
When the distance between the electrodes is adjusted in the stepwise pattern as described above, the plasma state can be stably retained without interruption in conformity with the kind of gas to be introduced and the pressure inside the reaction chamber. As a result, the TFT to be produced is enabled to acquire highly desirable properties because the dangling bond near the interface between the gate insulating film 3 and the semiconductor film 4 and the interface between the semiconductor film 4 and the etching-stopper film on channel 5.
In the conventional method for the formation of a multilayer film, the practice of stably retaining the plasma state by varying such conditions as the kind of gas to be introduced, the internal pressure of the reaction chamber, the high-frequency electric power to be supplied, and the distance between the electrodes as mentioned above is not followed. When the distance between the electrodes is adjusted in the stepwise pattern as in the case of the present example, however, the plasma state can be stably retained without interruption, for example, by decreasing the distance between the electrodes when the internal pressure of the reaction chamber is high and increasing the distance when the internal pressure is low in conformity to the kind of gas to be introduced, the internal pressure of the reaction chamber, and the high-frequency electric power to be supplied.
When a liquid crystal display substrate containing the TFT manufactured by the method of this invention for the formation of a multilayer film is incorporated by the standard process in an active matrix type liquid crystal display device and this device is operated, the TFT manifests an outstanding switching property.
The continuous plasma state functions as a means for continuing the plasma state from the gate insulating film 3 to the semiconductor film 4 and from the semiconductor film 4 to the etching-stopper-film 5. For the purpose of preventing the surface of the gate insulating film 3 and the surface of the semiconductor film 4 from being adversely affected by the chemical action of the plasma, the duration between the steps of film forming is desired to be in the range of from 3 to 20 seconds with a view to stabilizing the state of plasma and precluding the exertion of adverse effect on the surface.
The plasma state can be generated by a microwave discharge and a electron cyclotron resonance other than a high frequency discharge. The remarks of the way of generating the plasma state hold good invariably hereinafter.
As the preparatory gas, at least one member selected from the group consisting of H 2 , He, Ar, N 2 , NH 3 , N 2 O and Kr can be used. The remarks of the preparatory gas hold good invariably hereinafter.
EXAMPLE 2
FIG. 4 shows a TFT in an active matrix type liquid crystal display device according to Example 2. This TFT is composed of a gate electrode 2 formed in a predetermined shape of Mo-Ta integrally with a gate line (not shown) on a glass insulating substrate 1, a gate insulating film 3 of SiN x formed in a thickness of 0.3 μm in such a manner on the insulating substrate 1 as to cover the gate electrode 2, a semiconductor film 4 formed in a predetermined shape of a-Si, microcrystalline silicon, or polycrystalline silicon in a thickness of 0.05 μm in such a manner as to cover the gate insulating film 3 in conformity to the gate electrode 2, an n type semiconductor film 6 formed of n + a-Si in such a manner as to cover the source region and the drain region other than the channel region on the semiconductor film 4, a source electrode 7 formed on the n type semiconductor film 6 as partly extended into the source region on the gate insulating film 3, a drain electrode 8 formed likewise on the n type semiconductor film 6 as partly integrated with a signal line (not shown) extended into the drain region on the gate insulating film 3, and an insulating protective film 9 formed of SiN x in such a manner as to cover the channel region on the source electrode 7, the drain electrode 8, and the n type semiconductor film 6. The source electrode 7 is connected to a pixel electrode 10 formed of ITO on the gate insulating film 3.
The manufacture of the TFT is started with the formation of a metal film of Mo-Ta by the sputtering technique on the glass insulating substrate 1 as shown in FIG. 5A. This metal film is photolithographically etched to form the gate electrode 2 of the predetermined shape in conjunction with the gate line.
Then, the glass insulating substrate 1 having the gate electrode 2 formed thereon is heated to 623K and the material gas for the formation of the gate insulating film which is composed of SiH 4 , NH 3 , and N 2 is introduced to give rise to a plasma state and deposit the gate insulating film 3 of SiN x with a thickness of 0.3 μm as shown in FIG. 5B. The plasma state existent daring the deposition of the gate insulating film is subsequently retained without interruption and the gas being introduced is switched from the material gas for the deposition of the gate insulating film to the H 2 gas. The SiH 4 gas is introduced in conjunction with the H 2 gas to form an a-Si film 4 of a thickness of 0.05 μm as a semiconductor film.
The glass insulating substrate 1 having the a-Si film 4 and the like formed thereon is heated and the material gas for the deposition of the n type semiconductor film which is composed of PH 3 and SiH 4 is introduced to give rise to a plasma state as will be specifically mentioned hereinbelow and deposit a n + a-Si film of a thickness of 0.05 μm in such a manner as to cover the a-Si film 4. Then, by the photolithographic method, this n + a-Si film is etched to form the n type semiconductor film 6 of the predetermined shape and the underlying a-Si film is etched to produce the semiconductor film 4 of the predetermined shape as shown in FIG. 5C.
Thereafter, a transparent electrical conductive film of ITO is formed by the sputtering technique on the glass insulating substrate 1 having the n type semiconductor film 6 formed thereon and is then etched by the photolithographic method to form a pixel electrode 10 of a transparent electrical conductive film in a predetermined shape at a stated position on the gate insulating film 3 as shown in FIG. 5D.
Further, on the glass insulating substrate 1 having the pixel electrode 10 formed thereon, a metal film of Cr or Al is formed by the sputtering technique. Then, by the photolithographic method, the source electrode 7 connecting the n type semiconductor film 6 and the pixel electrode 10 and the drain electrode 8 connected to the n type semiconductor film 6 are formed integrally with the column lines. The part of the n type semiconductor film 6 in the channel region is removed by photolithographic etching as masked by the source electrode 7 and the drain electrode 8. Then, the TFT is completed by forming an insulating protective film of SiN x by the plasma CVD technique on the glass insulating substrate 1 having the source electrode 7 and the drain electrode 8 formed thereon (FIG. 4).
For the formation of the SiN x film intended for the gate insulating film and the a-Si film intended for the semiconductor film in this TFT, the glass insulating substrate 1 having the gate electrode formed thereon is fixed on the grounding electrode 14 in the reaction chamber 12 of the device shown in FIG. 3 and the reaction chamber 12 is evacuated. The glass insulating substrate 1, when necessary, may be fixed on the high-frequency electrode 13 instead. Then, the glass insulating substrate 1 is heated to 623K by means of the resistance heating unit 18 disposed on the grounding electrode 14 and, as the material gas for the deposition of the gate insulating film, SiH 4 gas fed at a flow volume of 10 sccm, NH 3 gas at 60 sccm, and N 2 gas at 400 sccm are introduced into the reaction chamber 12 to adjust the pressure in the reaction chamber 12 to 0.8 Torr. With the distance between the high-frequency electrode 13 and the grounding electrode 14 adjusted at 30 mm, an electric power of 50 W is supplied from the high-frequency power source 19 to generate a plasma state between the electrodes and form the gate insulating film of SiN x with a thickness of 0.3 μm.
The introduction of the material gas for the deposition of the gate insulating film is stopped and, at the same time, the introduction of the H 2 gas is started at a flow volume of 500 sccm to adjust the pressure of the gaseous atmosphere in the reaction chamber 12 at 0.3 Torr. With the distance between the electrodes set at 35 mm and the electric power from the high-frequency power source 19 set at 35 W, the plasma state existent during the deposition of the gate insulating film is continuously retained without interruption on the electrode 14. The effect of the residual gas during the deposition of the gate insulating film can be eliminated by introducing the H 2 gas in such a large amount as mentioned above and setting the pressure in the reaction chamber 12 at 0.3 Torr. The chemical effect by the H 2 plasma on the gate insulating film can be avoided and the plasma state can be stably retained by setting the distance between the electrodes at a large magnitude of 35 mm. For the sake of avoiding the chemical effect inflicted by the H 2 plasma on the gate insulating film, the duration of the plasma state is desired to be in the range of from 3 to 20 seconds.
Further, by the H 2 plasma, the interface between the gate insulating film mentioned above and the a-Si film to be formed subsequently thereon can be kept clean.
Then, by introducing the H 2 gas at a flow volume of 500 sccm thereby adjusting the pressure in the reaction chamber 12 at 2 Torr and, at the same time, setting the distance between the electrodes at 28 mm and the electric power from the high-frequency power source 19 at 50 W. the plasma state is stably retained. Owing to the stability of the state of plasma, the interface between the gate insulating film and the a-Si film subsequently formed thereon can be desirably formed and the dangling bond can be abated.
Further, the SiH 4 gas is introduced at a flow volume of 30 sccm and the distance between the electrodes is changed to 26 mm to deposit the a-Si film with a thickness of 0.05 μm.
Incidentally, when the distance between the high-frequency electrode 13 and the grounding electrode 14 is continuously adjusted in the stepwise pattern as described above, the plasma state can be stably retained without interruption in conformity with the kind of gas introduced, the internal pressure of the reaction chamber, and the high-frequency electric power supplied in the same way as in Example 1. As a result, the dangling bond near the interface between the gate insulating film 3 and the semiconductor film 4 and the interface between the semiconductor film 4 and the etching-stopper film on channel 5 can be obviously alleviated.
To be specific, the SiN x film which constitutes itself the gate insulating film 3 and the a-Si film 4 of the semiconductor film 4 can be deposited under the optimized condition and the dangling bond near the interface between the gate insulating film 3 and the semiconductor film 4 can be abated by effecting continuous stepwise adjustment of the distance between the high-frequency electrode 13 and the grounding electrode 14 and consequently regulating the process conditions so as to increase the distance between the electrodes when the pressure in the reaction chamber is high and decrease the distance when the pressure is low in conformity with the kind of gas introduced and the pressure it the reaction chamber. When a liquid crystal display substrate containing the TFT manufactured by the method of this invention is incorporated by the standard process in an active matrix type liquid crystal display device and this device is operated, the TFT manifests an outstanding switching property.
EXAMPLE 3
FIG. 6 shows a normal staggered (top-gate) TFT according to Example 3. In this TFT, an insulating substrate 1 made of glass (such as, for example, a product of Corning Glass marketed under product code of "7059") is heated to 623K and a gas composed of SiH 4 and nitrogen suboxide (N 2 O) is introduced and, by the plasma CVD technique using the plasma state which is consequently generated, an undercoat film 21 of SiO 2 is deposited in a thickness of 0.5 μm.
Then, an ITO film of a thickness of 0.1 μm for the formation of a pixel electrode 10 is formed and a metal of Mo-W is deposited in the form of a film by the sputtering technique. These films are photolithographically etched to form a source electrode 7 and a drain electrode 8 in predetermined shapes.
Then, the insulating substrate 1 is heated to 623K and the material gas for the deposition of a semiconductor layer which is composed of SiH 4 and H 2 is introduced to generate a plasma state and deposit an a-Si film 22 of a thickness of 0.1 μm. After the deposition of this film, the plasma state existent during the deposition of the a-Si film 22 is retained, the introduction of the SiH 4 gas is stopped, the gas being introduced is switched from the material gas for the deposition of the a-Si film to the H 2 or the He gas, and the SiH 4 gas is again introduced to deposit a gate insulating film 3 of SiN x in a thickness of 0.02 μm. subsequently, the introduction of the SiH 4 gas is stopped and the plasma state with the N 2 gas is continuously retained and the SiH 4 and the N 2 O gas are introduced to form an SiO film in a thickness of 0.02 μm. Then, the introduction of the SiH 4 and the N 2 O gas is stopped and, with the plasma state with the N 2 gas continued, the SiH 4 and the NH 3 gas are introduced to form a SiN x film in a thickness of 0.4 μm.
Subsequently, a metal film consisting of an aluminum (Al) film 0.3 μm in thickness and a Mo film 0.2 μm in thickness is formed on the insulating substrate 1 by the sputtering technique. This metal film and the gate insulating film 3 are subjected to chemical dry etching effected by the photolithographic technique to form the gate electrode 2 in a predetermined shape in conjunction with the gate line and expose the part of the a-Si/SiN x /SiO structure from the part devoid of the gate electrode 2. At this time, a fluorine type gas is used to etch exclusively the SiN x film in the upper layer and expose the SiO film. When the a-Si/SiN x /SiO structure is left intact as described above, the laser anneal can be easily effected.
Further, the a-Si film is doped with P ions with the gate a electrode 2 improvised as a mask. This ion doping is implemented by decomposing by a plasma the PH 3 gas diluted to 5% with H 2 , causing the consequently generated ion species to be collectively accelerated by an electric field without mass separation, and driving the accelerated ion species into the a-Si film. In this case, the amount of the ion species used for the doping is 3×10 15 cm -2 and the accelerating voltage is 60 kV.
Then, the insulating substrate 1 is irradiated with an XeCl excimer laser of a wavelength of 308 nm and an energy density of 70 mJ which is projected from above. As concrete examples of the laser which is usable for this purpose, the excimer lasers of ArF, KrF, and XeF and the YAG laser, and the Ar laser may be cited. In this case, the gate electrode 2 serves as a mask and the part of the a-Si film which has been doped with P ions is exclusively crystallized. Thus, an n type polycrystalline silicon of low resistance is formed. By photolithographically etching this n type polycrystalline silicon film, a source region 23 and a drain region 24 are formed.
Thereafter, an insulating protective film 9 of SiN x is formed by the plasma CVD technique on the insulating substrate 1 and is photolithographically etched to remove the part of the insulating protective film on the pixel electrode 10. Further, the part of the metal film of Mo-W on the picture element electrode 10 is removed.
When a liquid crystal display substrate containing the TFT manufactured as described above is incorporated by the standard process in an active matrix type liquid crystal display device and this device is operated, the liquid crystal display device manifests an outstanding switching property.
EXAMPLE 4
The construction of a liquid crystal display device (LCD) using the aforementioned TFT as a switching element is shown in FIG. 7. This liquid crystal display device is composed of an active element substrate 26, a counter substrate 27 opposed to the active element substrate 26 across a predetermined interval, and a liquid crystal 28 filling the gap between these substrates 26 and 27.
On the main surface of this active element substrate 26 which confronts the counter substrate 27 of the transparent insulating substrate 1 made of glass, a TFT 30 which is composed of a gate electrode 2, a gate insulating film 3, a semiconductor film 4, a etching stopper film on channel 5, an n type semiconductor film 6, a source electrode 7, a drain electrode 8, and an insulating protective film 9 as shown in FIG. 1 and a pixel electrode 10 are formed. Further, an aligning film 31 made of a cold curing type polyimide resin, for example, is provided on the TFT 30 and the pixel electrode 10. A polarizer 32 is formed to cover the outer main surface (the main surface on the opposite side) of the transparent insulating substrate 1. On the main surface of the counter substrate 27 which confronts the active element substrate 26 of a transparent insulating substrate 33 made of glass, a common electrode 34 made of ITO is formed. On this common electrode 34, like the active element substrate 26, an aligning film 35 made of a cold curing type polyimide resin is provided. The main surface (on the opposite side) of the counter substrate 27 outside the transparent insulating substrate 33 is covered with a polarizer 36. The aligning films 31 and 35 of the substrates 26 and 27 are rubbed severally with cloth in predetermined directions to acquire axes of orientation which intersect each other at an angle of about 90°.
The directions in which the aligning films 31 and 35 of the substrates 26 and 27 are rubbed are so set that the respective optimum viewing direction toward the front side. This liquid crystal display element is illuminated from the outside of the main surface of either of the active element substrate 26 and the counter substrate 27.
Owing to the construction described above, the liquid crystal display device excels in TFT property, stability, and insulating property and enjoys a high yield of production.
EXAMPLE 5
The method for the formation of a multilayer film which constitutes itself a thin-film transistor will be described in greater detail below. The TFT is constructed in the same inverted staggered (bottom gate) type as shown in FIG. 1.
FIG. 8 shows a gate insulating film 51, a semiconductor film 52, and a etching-stopper-film on channel 53 which jointly constitute the TFT. The gate insulating film 51 is formed of SiN x in a thickness of 0.05 μm, the semiconductor film 52 formed of a-Si in a thickness of 0.05 μm, and the etching-stopper-film 53 formed of SiN x in a thickness of 0.3 μm.
The device used for the manufacture has the same construction as is shown in FIG. 3.
In this example, the part of the TFT which continuously forms the SiN x gate insulating film 52, a-Si semiconductor film 52, and SiN x etching-stopper-film on channel 53 will be described. The process used for the manufacture is shown in FIG. 9.
A glass insulating substrate 55 having a gate electrode 54 formed by a predetermined method thereon is fixed on a grounding electrode 14 inside a reaction chamber 12 and the reaction chamber 12 is evacuated.
Step 1: The material gas composed of SiH 4 , NH 3 , and N 2 is introduced into the reaction chamber 12 to generate a plasma state and deposit the SiN x insulating film 51. The temperature of the substrate is 573 K.
Step 2: After the deposition of the SiN x gate insulating film 51, the introduction of the material gas is stopped and the introduction of H 2 gas as a preparatory gas is started at the same time. The plasma state is continuously retained by adjusting the distance between the electrodes wider. Though the interior of the reaction chamber is in an evacuated state, the partial pressure of the H 2 gas which is flowing is present in the reaction chamber and allows to retain the plasma state.
Step 3: With the introduction of the H 2 gas as the preparatory gas continued, the internal pressure of the reaction chamber 12 is adjusted to 1.2 Torr. The plasma state continues. The interface can be advantageously formed by adjusting the pressure at a level lower than the pressure, 3 Torr, which will exist during the subsequent deposition of the a-Si semiconductor film 52. Otherwise, the high-frequency electric power may be adjusted in the range of from 150 to 200 W, with the pressure kept intact.
Step 4: The SiH 4 gas is added to form a material gas and the internal pressure of the reaction chamber is adjusted to 3 Torr to form the a-Si semiconductor film 52.
Step 5: The introduction of SiH 4 is stopped and the introduction of H 2 gas as the preparatory gas is started simultaneously. The plasma state is continuously retained by adjusting the distance between the electrodes wider. Though the interior of the reaction chamber 12 is in an evacuated state, the partial pressure of the H 2 gas which is still flowing is present in the reaction chamber 12 and allows to retain the plasma state continuously.
Step 6: The introduction of NH 3 gas add to the H 2 gas as the preparatory gas is started to adjust the internal pressure of the reaction chamber 12 to 3.5 Torr.
Step 7: The introduction of the H 2 gas is stopped and the introduction of N 2 gas as the preparatory gas is started simultaneously to adjust the internal pressure of the reaction chamber at 3.5 Torr. The interface can be advantageously formed by adjusting the pressure to a level equaling the pressure, 3.5 Torr, which will exist during the subsequent deposition of the SiN x etching-stopper-film on channel 53.
Step 8: The SiH 4 gas is added to form the material gas to deposit the SiN x etching-stopper-film on channel 53.
The plasma state continues to be generated throughout the entire process for the formation of the multilayer film as clearly remarked from the description given above. The multilayer film to be produced is enabled to acquire a highly desirable interface by effecting stepwise adjustment of such conditions as the kind of gas introduced, the internal pressure of the reaction chamber, the distance between the electrodes, and the high-frequency electric power supplied thereby optimizing the state of plasma.
The durations of the steps of film forming at Steps 2, 3, 5, 6, and 7 are desired to be in the range of from 3 to 20 seconds for the purpose of preventing the surfaces under treatment from being degraded by the chemical action of the H 2 plasma particularly when the H 2 gas is introduced as the preparatory gas.
The process described above is just one example. The plasma state can be retained and the multilayer film produced in high quality by varying the conditions in conformity with the speed of film depositing desired, the duration of film depositing, the temperature of the substrate, or the like.
FIG. 10 shows the mobility of a thin-film transistor which is formed by the method described above. The symbols A through D represent conditions of multilayer films intended for thin-film transistors according to the present invention. The symbol E represents a condition of the conventional method which stops the plasma state after each step. In each condition, 3 samples 1-3 are shown. The symbol A represents sample obtained with Step 3 performed under the conditions of 3 Torr and 100 W. The symbol B represents samples obtained with Step 3 performed under the conditions of 3 Torr and 150 W. The symbol C represents samples obtained with Step 3 performed under the conditions of 3 Torr and 200 W. The symbol D represents samples obtained with Step 3 performed under the conditions of 1.2 Torr and 100 W. The symbol E represents samples obtained by the conventional method which stops the plasma state after each step.
It is clearly noted from the data of FIG. 10 that the thin-film transistors obtained by continuously retaining the plasma state are excel in the mobility. This is because the interfaces corresponding to the channel the thin-film transistors are desirably formed.
For the adjusted magnitude of the pressure at Step 3, the desirability of the interface and the mobility of the thin-film transistor are exalted in proportion as the high-frequency electric power supplied is increased. The desirability of the interface and the mobility of the thin-film transistor are further exalted by adjusting the pressure existent at Step 3 to a level lower than the pressure which will exist during the subsequent deposition of the a-Si semiconductor film.
FIG. 11 shows the threshold voltage, Vth, of a thin-film transistor formed by the method described above. The symbols A through D represent conditions of multilayer films obtained by this invention for the construction of thin-film transistors. The symbol E represents a condition of the conventional method which stops the plasma state after each step. In each condition, 3 samples are shown.
The symbol A represents samples obtained with step 3 performed under the conditions of 3 Torr and 100 W. The symbol B represents samples obtained with Step 3 performed under the conditions of 3 Torr and 150 W. The symbol C represents samples obtained with Step 3 performed under the conditions of 3 Torr and 200 W. The symbol D represents samples obtained with Step 3 performed under the conditions of 1.2 Torr and 100 W. The symbol E represents samples obtained by the conventional method which stops the state of plasma after each step.
It is clearly noted from the data of FIG. 11 that the thin-film transistors produced by continuously retaining the plasma state are excel in the threshold voltage. This is because the interfaces corresponding to the channel parts of the thin-film transistors are desirably formed.
For the adjusted magnitude of the pressure at Step 3, the desirability of the interface is increased and the magnitude of the threshold voltage of the thin-film transistor is decreased in proportion as the high-frequency electric power supplied is increased. The desirability of the interface is further increased and the mobility of the thin-film transistor is further decreased by adjusting the pressure existent at Step 3 to a level lower than the pressure which will exist during the subsequent deposition of the a-Si semiconductor film.
When a liquid crystal display device is manufactured by using as a switching element therefor a thin-film transistor obtained by the method of this invention for the formation of a multilayer film, it enjoys highly satisfactory qualities such as high response speed and small power consumption.
This invention can be utilized for the formation of multilayer films intended for the construction of other semiconductor devices. The multilayer films may be used for contact sensors, solar cells, etc.
EXAMPLE 6
The method for the formation of a multilayer film for the construction of a thin-film transistor will be described more specifically below.
The construction of the TFT is of the same normal staggered (top-gate) type as is shown in FIG. 6. FIG. 12 is a diagram showing with a model the part of the TFT forming a semiconductor film and gate insulating films. A semiconductor film 61 is formed of a-Si in a thickness of 0.1 μm. A gate insulator film 62 is composed of the three layers, SiN x film, SiO film, and SiN x film (not shown). Specifically, the gate insulating film 62 is formed of SiNe in a thickness of 0.02 μm, the gate insulating film 63 formed of SiO in a thickness of 0.02 μm, and the gate insulating film formed of SiN x (not shown) in a thickness of 0.4 μm.
The device used for the manufacture is in the same construction as is shown in FIG. 3.
In this example, the part of the TFT in which the a-Si semiconductor film 61, the SiN x gate insulating film 62, and the Sio gate insulating film 63 are continuously deposited will be described. The process used for the manufacture is shown in FIG. 13.
A glass insulating substrate 67 having a SiO 2 undercoat film 64, a source electrode 65, and a drain electrode 66 formed by the predetermined method thereon is fixed on the grounding electrode 14 in the reaction chamber 12 and the reaction chamber 12 is evacuated.
Step 1: The material gas composed of SiH 4 and N 2 is introduced into the reaction chamber 12 to generate a plasma state and deposit the a-Si film. The temperature of the substrate is 593 K.
Step 2: After the deposition of the a-Si semiconductor film 61, the introduction of SiH 4 is stopped and the introduction of H 2 gas a preparatory gas is started at the same time. The plasma state is continuously retained by increasing the distance between the electrodes. Though the interior of the reaction chamber is in an evacuated state, the partial pressure of the H 2 gas which is flowing is present in the reaction chamber and allows to retain the plasma state.
Step 3: The introduction of H 2 gas is stopped and the introduction of NH 3 gas and N 2 gas are started simultaneously. The internal pressure of the reaction chamber 12 is adjusted to 0.5 Torr. The interface can be advantageously formed by adjusting the existent pressure at a level lower than the pressure, 0.8 Torr, which will exist during the subsequent deposition of the SiN x gate insulating film 62.
Step 4: The SiH 4 gas is added over the NH 3 gas and N 2 gas to form a material to deposit the SiN x gate insulating film 62.
Step 5: The introduction of SiH 4 and NH 3 is stopped and the introduction of N 2 gas as the preparatory gas is started. The plasma state is continuously retained by increasing the distance between the electrodes. Though the interior of the reaction chamber 12 is in an evacuated state, the partial pressure of the N 2 gas which is still flowing is present in the reaction chamber 12 and allows to retain the plasma state.
Step 6: The N 2 O gas is introduced as the preparatory gas to adjust the internal pressure of the reaction chamber 12 to 0.8 Torr. The interface can be advantageously formed by adjusting the existent pressure at a level lower than the pressure, 1.2 Torr, which will exist during the subsequent deposition of the SiO gate insulating film 63.
Step 7: The SiH 4 gas is added over the N 2 gas and N 2 O gas to form the material gas to deposit the SiO gate insulating film 63.
The interface can be advantageously formed by effecting the multistage adjustment of such conditions as the kind of gas introduced, the internal pressure of the reaction chamber, thee distance between the electrodes, and the high-frequency electric power supplied thereby optimizing and retaining the plasma state.
The durations of the steps of film forming at Steps 2, 3, 5 and 6 desired to be in the range of from 3 to 20 seconds for the purpose of preventing the surfaces under treatment from being degraded by the chemical action of the H 2 plasma particularly when the H 2 gas is introduced as the preparatory gas.
The process described above is just one example. The plasma state can be retained and the multilayer film produced in high quality by varying the conditions in conformity with the speed of film depositing desired, the temperature of the substrate, or the like.
When a liquid crystal display device is manufactured by using as a switching element therefor a thin-film transistor obtained by the method of this invention for the formation of a multilayer film, it enjoys highly satisfactory qualities such as high response speed and small power consumption.
This invention can be utilized for the formation of multilayer films intended for the construction of other semiconductor devices. The multilayer films may be used for contact sensors, solar cells, etc. | A method for forming a multilayer film by introducing a material gas into a reduced-pressure reaction chamber provided with a pair of parallel planer electrodes and supplying a high-frequency electric power to the electrodes thereby generating a plasma state therein and depositing a film on a substrate disposed on one of the electrodes, comprising the steps of (a) introducing a first material gas into the reaction chamber and supplying the high-frequency electric power to the electrodes thereby generating the plasma state and depositing a first film on the substrate, (b) introducing stepwise a preparatory gas and adjusting stepwise a distance between the electrodes, a pressure inside the chamber and a RF power supplied to the electrodes while continuously retaining the plasma state subsequently to step (a), and (c) introducing a second material gas into the reaction chamber while continuously retaining the plasma state thereby and depositing a second film on the first film. According to the method the surface between the films is desirably formed, and this cause a promotion of characteristics when applied to produce a multilayer films constitutes semiconductor device, a TFT and a solar cell for example. | 7 |
This application is a continuation-in-part of Ser. No. 08/815,725 filed Mar. 12, 1997, issued as U.S. Pat. No. 5,831,156 on Nov. 3, 1998.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a surface and downhole system for the control, monitoring and operation of a single or multiple wells. The downhole portion of the system is entirely self contained and once in place requires no communications, power or control function to be provided from the surface. The surface portion of the system communicates by movable module with the downhole portion of the system. The surface portion of the system itself is remotely addressable via satellite line, microwave line, or via land line. If desired, various components of the modular system may be interrogated, evaluated, and/or replaced independently of the well completion and production schedule.
2. Brief Description of the Prior Art
Many oil and gas wells being drilled at the present time are drilled through and have multiple perforation and producing zones. Additionally, particularly in offshore field development, the use of multi-lateral wells drilled from a single central well borehole have become an accepted practice. Each production zone, or lateral well of a multi-lateral system, has its own set of operating parameters. These parameters of pressure and flow rate are determined by the physical characteristics of the reservoir rock and the borehole conditions at each production zone, or lateral well, such as permeability, porosity, formation pressure, formation gas content, formation water content, etc. In other words, in present day well completion practice, a single well borehole may comprise a series or set of different production parameters of flow rate and pressure wherein each member of the series of set requires its own separate handling logic to optimize its production of hydrocarbon. In a typical well each producing zone may contain oil, water and gas. It is desirable to produce the maximum possible rate.
In recognition of these completion practices well control systems utilizing microprocessor logic circuitry both at the surface and downhole have been developed. In such prior art systems, ultimate control of the operating system has always heretofore been maintained from the surface. For example, U.S. Pat. No. 5,132,904 discloses a well control system having a microprocessor to monitor well pressure levels, timed sampling limits and their combination. The sensors are connected by wire to the microprocessor at the surface in this system. Similarly, is the disclosure of PCT International Publication No. WO 96/10123 published Apr. 4, 1996 a surface microprocessor is connected by wire to downhole pressure and flow sensors in several different completion zones of a well. In U.S. Pat. No. 5,273,112 a surface controller communicates with a downhole instrument set for measuring pressure and flow via an annulus pressure modulation system which utilizes annulus pressure as a communication conduit to the downhole instruments.
In the cases where communications to the surface are performed by wire, special production tubing is required having communication and power wire and protectors therefor run along its length from the surface to the downhole tool. This wire is a weak link in the system, even using the best of available protection systems due to short term mechanical stress placed on it, for example during installation, and due to longer term stress placed on it due to lengthy timewise exposure to borehole temperatures, pressures and chemical activity. Similarly, in the case where tubing or annulus pressure modulation systems are used to control downhole tool settings, very heavy and bulky high pressure pumping systems are required at the well head to perform the communication function. Such pressure pumping systems may not always be available in remote location and when they are, their use can be very expensive.
Accordingly, it would be very desirable to have an entirely self contained downhole well monitoring and control system. Such a system would be even more desirable if it were repairable without decompleting the well. Decompletion (or the cessation of fluid production) is presently required for repair of known well control systems, such as those previously mentioned. Killing the well requires loading the well with fluids that made a higher hydrostatic pressure than the reservoir pressure. This requires that the well be "unloaded" (or the fluid removed) in order to begin production again. This is very expensive, time consuming and the fluids used may damage the formation permanently, inhibiting optimum production from the well.
BRIEF DESCRIPTION OF THE INVENTION
The downhole portion of the system of the present invention provides entirely downhole methods and apparatus for the monitoring and control of wells. The components of the system are modular. There are sensor and control valve components located in each of the multi zone production intervals or lateral well completions. The production zones are isolated by production packers equipped with feed through conductors for communication to upper system components. There are a monitor and control module containing a programmable microprocessor controller and a power supply module which are located at the uppermost end of the system. The system provides for removing, decommissioning and/or replacement of the power module or the monitor and control module without decompleting the well. The system provides for connecting to and charging or recharging the power module in place in the borehole with the well in operation. The system provides for surface connection to and monitoring of the power module or the monitor and control module from the surface while the well is in operation. The system provides for updating or reprogramming the monitor and control module in place in the well borehole. Upper modules of the system can be placed out of service by appropriate connection of a replacement upper module above it in the system having a means for controlling switches inside the power or control module. The system modules also provide for a mechanical well completion which is substantially open to remedial operations through their center bores, thereby providing repair of the mechanical completion of the well (perforating, squeeze cementing, acidizing, etc) without the removal of any of the system modules. The system also allows for production tubing to be run in the well to assist in production or well parameter change.
For example, when formation pressure decreases or water production increases in a formation the well will begin to "load up" i.e. the produced fluids become too heavy for formation pressure to lift to the surface. In these cases it is customary to run smaller production tubing or insert gas lift valves or other artificial lift systems. The surface portion of the system may be operated from the well head or by remote control via a communications link such as microwave, satellite link or the like. A surface located test, question, or reprogram module is contained in a controlled buoyancy carrier mounted at the well head. The carrier is controlled by a surface control computer which is, in turn, in communication with the remote located human/machine operator of the entire production system. A production tubing string connects the downhole portion of the system to the surface located production manifold and fluid flow lines for carrying off produced fluids. When it is decided to query or change the operating parameters of the downhole reduction system, the command is sent via the communication link to the surface control computer. The computer temporarily shuts off well output at the surface manifold and allows the controlled buoyancy carrier to "fall" down through the production tubing and "land" on the downhole monitor and control module of the downhole system. The carrier then interrogates the memory in the monitor and control module and/or reprograms its internal microprocessor as it has been instructed. The carrier then alters its own buoyancy to return via the production tubing to the surface. At the surface it reports the status or sends back the requested data it has gathered via the communications link to the operator.
These and other features and advantages of the system of the present invention are best understood from the following detailed description thereof when taken in conjunction with the accompanying drawings. It will be understood that the drawings are intended as illustrative and not as limitative of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic sectional view showing the downhole portion of a system according to the concepts of the present invention in a well borehole.
FIG. 2 is a block diagram showing the overall layout of a system according to concepts of the invention.
FIG. 3 is a schematic diagram illustrating the mechanical layout of the system of FIG. 2.
FIGS. 4A-4C are schematic sectional views showing different embodiments of connectors useful with modular components according to the invention.
FIGS. 5A and 5B are a schematic block diagrams illustrating power supply and control module switching arrangements according to one embodiment of the invention.
FIG. 6A is a schematic sectional view showing a remotely controllable stand alone system according to the invention deployed with the downhole well operating and control system of FIG. 1.
FIG. 6B shows the casing head portion of FIG. 6A in more detail.
FIG. 7 is a schematic diagram showing a system deployed on dedicated coiled tubing unit at the surface.
FIG. 8 is a schematic diagram showing a system deployed on a dedicated wireline unit at the surface.
FIG. 9 schematically shows in section an alternative embodiment known as a "pump up/down" U tube arrangement for use with carrier 86 of FIG. 6A.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The production of hydrocarbons from a reservoir by a well penetrating one or more producing formations requires downhole production equipment to control the produced fluid flow. Production equipment usually includes a production tubing string to convey the fluid from each producing zone to the surface, well packers to isolate discrete producing zones, or lateral completions in the case of multi lateral wells from each other, and other tools such as pressure and flow sensors and valves to monitor and control fluid flow from each of the producing zones. Production operations may be complicated by variables such as multiple producing zones having different rock properties, fluid chemical composition, temperatures and pressures and fluid migration from one producing zone to another in the same completion set. All of these factors cause variable performance of each producing zone over time. There is a need to control a single zone to maximize hydrocarbon production and flow rate while reducing the production of water and while maintaining formation energy and pressure for producing the well. Prior art well control systems have, heretofore, not efficiently monitored and controlled these production variables in multiple completion sets.
Typically, downhole conditions in each producing zone have been monitored by a single gauge permanently installed in a side pocket mandrel above the production packer. The gauge is capable of measuring fluid pressure and temperature, which data is communicated to a surface control system via a dedicated wireline which is also permanently installed as part of the production tubing string, or the like. In some systems the gauge may be retrievable to the surface via a wireline or coiled tubing system used for that purpose.
Additionally to the need for monitoring well conditions, operating and control systems must provide a means for operating production control equipment, such as valves, in each separate producing zone. In some prior art systems hydraulic lines extending to the surface have been used to provide hydraulic power to remotely control downhole valve devices, or even safety valves. Typically such valves may be held in an open position when a hydraulic line is pressurized and be closed when the pressure is reduced or removed by a spring driven actuator. These systems thus require additional hydraulic lines be run to the surface which, again, provides a weak link in the system.
The system of the present invention will be described with respect to a well control system for a dual (or multi) zone production completed vertical single well borehole. It will be understood by those of skill in the art that the concepts of the downhole well control systems according to the invention may also be used for dual or multiple zone injection wells, if desired, or could be used to control dual or multiple lateral well boreholes in a multi lateral well completion system.
In the completion of a oil or gas well one of several types of "drive" mechanism provides the energy to produce the oil or gas. There are several types of "drive" mechanisms, of which there are three primary, these are Depletion Drive, Water Drive and Gas Drive. In all of these normal Drive mechanisms there is not a means of controlling the proportions of production of oil, water or gas on a continual basis. For this reason there is still large quantities of hydrocarbons remaining in reservoirs that are abandoned because they are considered not commercial.
In depletion drive systems the total energy to produce the hydrocarbon is contained in the hydrocarbon system itself. In this drive mechanism the compressed hydrocarbon in a fixed formation volume provides the energy for production. Generally this compressed energy will consist of the compression of the fluid (oil) or gas in solution (solution gas). As the well is produced it is not uncommon for solution gas to "break out of solution" and form a gas cap in the reservoir due to the difference in specific gravity of the oil and gas. In systems which form a gas cap as the gas is separated from the oil in the reservoir and if allowed to the gas is produced separately as free gas, while the oil continues to be produced. It would be a great benefit for the gas cap to form above the oil and continue to provide energy for the production of the oil without being produced itself. After the oil is produced the gas will flow easily to the surface and be fully produced with its own energy.
Gas caps formed above the oil column cause another problem at the intersection of the well bore and formation in both vertical and horizontal wells. The high pressure gradient at the formation wellbore intersection causes the fluid or gas with the highest relative permeability to flow much easier than fluids with lower relative permeabilties. It is a well known fact that formations have the highest relative permeability to gas, then water, and lastly oil. This means that the gas and water will encroach into the oil bearing formation at the well bore effectively reducing the flow of oil. In a gas drive system the gas is known to encroach or cone near the well bore and is generally described as "gas coning". Methods for producing the oil first in a gas drive system have consisted of perforating the formation at the lowest possible position in the formation which is exposed to the well in vertical wells or placing the well bore near the bottom of the oil column in a horizontal well. Another method used is to reduce the flow rate from the well. Other methods consists of remedial well operations whereby the perforations are squeeze cemented and new perforations made below the gas cap or gas producing perforations. These methods have not been successful as approximately 50% of the original oil found is still in place when reservoirs are abandoned as non-commercial.
In water drive systems water in the lower portion of the reservoir provides the energy for producing the oil or gas in the reservoir. Since water generally flows easier through the formation than does the oil and with a high pressure gradient existing at the well bore formation interface, the water like the gas, will begin to encroach into the oil bearing formation at the well bore effectively reducing the flow of oil. In this type of drive system the water is known to cone near the well bore and is generally described as "water coning".
The solution to both the gas and water coning problem would be to isolate the entire reservoir into intervals with packer or other isolation systems. These intervals could be monitored for gas and water production by means of a three phase flow meter or gas/water cut meter. Production from each interval could then be adjusted by incrementally opening or closing of a down hole control valve such as a side door or sliding sleeve valve located in each isolated interval to maintain the water or gas cut to within given parameters. Reducing the flow rate would decrease the pressure gradient near the well bore thereby preventing or reversing the tendency for the water or gas coning and decrease the water or gas portion of the production.
Another solution would be to divide the production interval into small portions by using packers or other isolation devices closely spaced within the well with sensors and a control valve in each of these smaller intervals. The sensors, like gas and water cut meters, could be monitored and the control valve incrementally opened or closed to adjust the production of oil/gas or oil/water in each of the intervals within a preset parameter.
When injecting fluids into a reservoir as a drive or displacement mechanism it is desirable for the fluid to be distributed throughout the well bore interval in order for fluid front to displace the oil that is in place in the reservoir to the producing well. This would mean that the fluid front would reach the entire well bore interval of the producing well at the same time thereby completely displacing the oil in the reservoir.
The problem is that due to permeability variations, injected fluids are not equally distributed throughout the well bore interval. In addition, there is not ideal communication through each perforation to the reservoir. This causes high volumes of injected fluids to find the path of least resistance and migrate to the neighboring producing well in a fashion known as channeling. Once this injected fluid progresses through the reservoir to the neighboring producing well this path becomes progressively easier for the injected fluid to flow through. In these situation large volumes of oil or by-passed by the displacing fluids. This causes operators to incur high costs for producing fluid and re-injecting the same again in the injecting well.
The solution to distributing the injection fluid over the entire injection interval is much the same as the producing well. The entire interval would be divided into small (short) intervals by using packers or other isolation systems with flow sensors and a control valve in each interval. By monitoring the flow rate in each interval, controlling the injection rate in each interval, the reservoir would be more evenly swept by the injected fluid.
Referring initially to FIG. 2 a schematic diagram arrangement showing a well control system in accordance with the concepts of the invention is given. In the diagram of FIG. 2, two production zones or intervals labeled interval #1 and Interval #2 are shown downhole. These zones are isolated from each other and from the wellbore above by production packers (not shown here) which will be illustrated subsequently. In each isolated interval there is a sensor package and an electromechanical device. In interval #1 is sensor package 29 and electromechanical device 30. In interval #2 is sensor package 31 and electromechanical device 32. Sensor packages 29 and 31 include a temperature and pressure sensor such as the PANEX MICROBEAM® TORQUE CAPACITANCE SENSOR manufactured by PANEX Corp. of Houston, Tex., or the even more accurate model VANGUARD resonating quartz temperature and pressure sensor manufactured by Baker Oil Tools, Inc. of Houston, Tex. A water cut meter could be included. The electromechnical devices of packages 30 and 32 can include solenoid operated valves such as those described as manufactured by Petroleum Engineering Services of Houston, TX. The sensor and electromechnical devices are connected to the power and control module shown generally at 20 and located at the top end of the downhole tool string. The power and control module 20 comprises a power source 24 which can comprise a rechargeable battery of the series PMX1 50 or CSC93 type sold by the Electrochem Lithium Batteries of Wilson Greatbatch LTD. of Clarence, N.Y. or Battery Engineering Inc. of Hyde Park, Mass., together with a downhole telemetry transceiver 25 for communicating with the earth's surface. The power and control module 20 also includes a dedicated programmable microprocessor 26 and a memory unit 27 which may be a "FLASH" memory or EEPROM (electrically erasable programmable read only sensor) such as the Motorola 68HC16 family or the like. The microprocessor 26 could comprise, for, example, the Texas Instruments TMS320C240, which is capable of 20 MIPS operating speed in an extremely compact package. The flash memory requires extremely low operating power to retain its programmed data. The Texas Instruments TMS 320 series microprocessors each contain some "flash" memory in themselves (i.e. about 16K words). The supplemental memory 27 can be used to store historical well data for "uploading" to the surface in the future, if desired. The data acquisition and control system (DAC) 28 is essentially an interface between the microprocessor 28 and the analog sensors 29 and 31 and the electromechnical devices 30 and 32. This DAC receives control signals from the microprocessor 26 and formats and conducts these to the electromechnical valves 30 and 32 to control the fluid flow from intervals #1 and #2 into the production tubing. Similarity, the interface 28 receives measured pressure and temperature data from sensor packages 29 and 31 and digitizes and formats it correctly for presentation to the microprocessor 26.
The separation line in FIG. 2 separates the downhole system components which are permanently installed in the well borehole from the optional surface components of the system. For example, a charging unit 23 may be lowered into the well periodically (an interval of weeks or months) to recharge the downhole battery or power source 24. Also, if desired, a surface transceiver 22 and a surface display system 21 may be linked via a running tool and diagnostic system to receive data generated by the downhole telemetry transceiver and to conduct new operating instructions (i.e. reprogram the microprocessor) to processor 26, if desired. The surface display system may comprise a video monitor, a printer, a fax system or whatever data recording device is desired.
Referring now to FIG. 1 the mechanical layout of the system of FIG. 2 is shown in a highly schematic, sectional view in a well borehole. In the view of FIG. 1 the production tubing string which normally would conduct produced fluids to the surface has been removed and pulled from the borehole 10. The borehole 10 is lined with a steel casing 11. A conductor string 12, which may comprise coiled tubing housing several electrical conductors or armored multi-conductor cable if desired, is used to lower and stab into the uppermost module of the completion system, which is a running tool and diagnostic system sub assembly 13. The diagnostic sub 13 contains the necessary interface and charging system to run tests on the permanently installed down hole system from power and control sub 14 on down to the bottom of the hole. Such tests may, if desired, be conducted as each module is sequentially installed. It will be noted that each of the downhole subs has a permanently open center bore 10A passing through it. This enables fluid production to continue even as some system components are repaired or replaced. The power and control sub 14 is shown in the drawing FIG. 1.
Below the power and control module 14 and sealingly attached thereto is upper packer module 15. This together with lower packer module 15A and the seal sub 7 isolate perforations 16 of Interval #1 from the perforations 17 of interval #2 below. A spacer sub 9 contains an electromechnical control valve 8 of the type previously described and also houses a sensor package 19 of the type previously described which are use to sense and control fluid flow conditions in interval #1. Similarity a second spacer sub 19A, having a sealed lower end 9B, is equipped with a corresponding sensor package 9A and a control valve 8A. All of the system components are electrically connected by conductors 18 comprising the control line. The mechanical form of these will be discussed in more detail subsequently.
While FIGS. 1 and 2 describe the system with respect to two production intervals, it is apparent that the same concepts may be utilized and extended to sense and control operating conditions on three or more intervals, if desired. The control of only one interval is important to optimize production of the desired hydrocarbon. FIG. 3 schematically shows a perspective view of this extension of up to N (integer) stages. In FIG. 3 a running tool and diagnostic system is shown at 31 connected to the surface via coiled tubing 32. The power and control module of the system is shown at 33. Packers 34, 35, 36 and etc. are used to isolate production zones as previously described. Sensors 37, 38, and 39 are provided on a spacer sub 40 as previously described. The sensor 37 may be a pressure sensor as previously described as is sensor 38. Sensor 39 can be a position sensor on the motor driven valve 39A used to control fluid flow into the central opening of the system modules. Similar sensors 37A, 38A, 39B etc to 37N, 38N and 39N may be placed in each of N intervals of the well being controlled by the control sub 33 of FIG. 3.
Referring now to FIGS. 4A, 4B, and 4C several alternative mechanical arrangements are shown for making up different connectors for joining various modules or components of the system of the present invention. In FIG. 4A two lines 52A and 53A, whether hydraulic or electric, are connected from an upper module 51 to a lower module 52 each having corresponding center bores 50. The upper module 51 has a smaller diameter lower portion 51 A which is grooved to accept O ring seals 55. This lower portion 51A is stabbed into the lower module 52. Simultaneously upper hydraulic or electric lines 52 and 53 following smaller diameter guides 52D and 53B which enter bores in line continuations 52A and 53A provide fluid tight hydraulic and/or electric connections between the modules.
In FIG. 4B a similar arrangement is shown but having only a single electrical or hydraulic connection 52B which is above and within the wall of the module 51 as shown. The lower module 52 shown in section receives the reduced diameter portion 51 A of the upper module 51 which has the electric or hydraulic connection 52B disposed between a pair of O-ring seals 55. This is received by a fluid groove 52B connected to a bore 52B in the wall of lower module 52. Again, when joined, a continuous center bore 50 is formed between the two modules.
In FIG. 4C a similar arrangement to either FIG. 4A or FIG. 4B is shown. Here, however, when the smaller diameter portion of the upper module 51 is stabbed into the lower module 52 an alignment lug 60 on the upper module enters an alignment slot 61 on the lower module 52, thereby establishing a selected circumferential orientation of both modules 51 and 52 with respect to each other.
Referring now to FIGS. 5A and 5B a switching arrangement whereby when a new upper module (i.e. Corresponding to a new power and control sub 14 of FIG. 1) is plugged into the top of the system it automatically disconnects and places out of service the previous power and control sub being used by the system. In FIG. 5A, an original power and control sub 71 has been in use in the system. It is powered by its power supply 71A which is also connected to the remaining system modules located below it by power buss 71C and switch 71B in the up position. When module 72 replaces original power and control module 71, it operates off its internal power supply 72A which supplies power to its process control module 72B and the remaining system modules located below it by power buss 72C and switch 72S1 in the down position. Similarly when module 71 is in control of the system via its process and control module 71B, then switch 71S2 is in the up position and module 71B communicates via signal Buss 71T with the downstream modules. When module 72 is plugged into the system switch 71S2 is placed in the down position, disconnecting process and control module 71B and process and control module 72B takes over via switch 72S2 in its normally up position and Signal Buss 72T. In FIG. 5B a new power module 73 replaces power supply 71A with power supply 73A as switch 71S1 is moved to the down position disconnecting supply 71A. However, when switch 71S2 is thrown down, process and control module 71B remains in control of the system via switches 71S2 (down) and 73S2 (up) and signal Busses 73T and 71T. Placement of the new module 72 or 73 on top of the old module 71 activates the switches 7151 and 7152 for this purpose. In this manner, new power and control modules or new power modules may be placed into service without recompleting the system. Similarly, when the running tool and diagnostic system module 13 of FIG. 1 is placed on top of the upper power and control sub 14, the diagnostic system may be operated from its power supply and microprocessor module which are similarly switched into use automatically by switches 71S1 and 71S2.
Referring now to FIGS. 6A and 6B the remotely operated system of the present invention is shown in a partially sectional view deployed in a well borehole 11. FIG. 6B schematically shows in section the casing head portion of FIG. 6A in more detail. The portion of the system of FIG. 6A located from module 14 downwardly is the same as that described previously with respect to FIG. 1 and hence will not be repeated. In FIG. 6A the downhole system is connected to the surface via a string of production tubing 12A. At the surface tubing string 12A terminates in a tree 88 (FIG. 6B) having a master valve 91 and a production control and entry valve 87 connecting tubing 12A to a production flow line 89 which carries off produced fluids for transport or disposal. Atop the tree 88 (which is supported by casing flange 90) sits a carrier housing 85 and within it a variable buoyancy carrier 86. The carrier housing 85 is controlled via line 83 from a surface control computer 82. The computer 82 also controls valves 87, 88, and 91 in manifold 188 via control line 84.
A satellite dish antenna 80, which may be of the small 18 inch diameter Ku bond type if desired, houses a transceiver unit connected via line 81 to computer 82. The dish antenna 80 and control computer 82 form a communications system allowing a two way link via satellite with a remote located control operator (human or machine). When the remote operator desires to interrogates the memory unit of downhole control module 14, it communicates this via the satellite link 80, 81, 82 to the control computer 82. Computer 82 transmits a control signal via line 83 to housing unit 85 to set the buoyancy of the carrier module 86 to minimum (so it will sink). This signal also is used to convey the desired command to the downhole portion of the system by placing the command in the microprocessor control computer located in the carrier 86. Such commands can include those to interrogate the memory unit of the downhole control module 14 for well performance data, to reset the valves 8 and 8A of the downhole sensor modules 18 etc. as desired.
The control computer 82 also sends a signal to valves 87, 88 and 91 to temporarily shunt production from output line 89 and to open housing 85 into fluid communication with the production tubing 12A. This allows carrier module 86 and its associated electronics (a microprocessor and memory unit) to fall down production tubing 12A and land onto downhole control module 14. Carrier module 86 computer then programs the control module 14 microprocessor to carry out the desired command such as reset valves transfer sensor data from memory of module 14 to carrier module 86 etc. When the performance of the command has been finished the variable buoyancy of carrier module 86 is increased and it rises up production tubing 12A to the surface and re-enters housing 85 via valves 87 and 91. When again housed in the housing the computer can interrogate the carrier module and communicate results to the "main office".
Referring now to FIG. 7 a similar remotely controlled system to that of FIG. 6 is depicted schematically. In FIG. 7 the carrier module 86 (corresponding to FIG. 6) is deployed on a coil tubing 101 dispensed from a coil tubing roll 100. The coil tubing roll 100 is controlled by the operation of surface control computer 82 and satellite transceiver system 80 as previously described. Valve 87 in manifold 88 is controlled by computer 82 via line 83. The valve 87 is opened when command signal is received from antenna/transceiver 80. This allows carrier 86 to enter production tubing 12A where it is conducted downhole to land on the downhole control module 14 as previously described. When the desired commands have been executed the coil tubing dispenser 100 pulls tubing 101 and carrier 86 to the surface where it re-enters housing 102 via the valve 87.
Similarly, in FIG. 8 an electrical (or non-electric) wireline 201 is dispensed from a cable winch 200 via sheave wheels 202 and 203 and is connected to a carrier module 86 in a housing 85. When it is desired to command the downhole control module 14 in some manner the communications link 80 and computer 82 open valve 87 in housing 88 as before. Under control of computer 82 the winch unit 200 dispenses wireline cable 201 to lower carrier 86 into the production tubing 12A. When all commands are finished the wireline winch 200 retrieves wireline 201 and carrier 86, as before.
Referring now to FIG. 9 an alternative arrangement for moving carrier 86 (FIG. 6A) up and down in the borehole under the control of computer 82 is shown schematically. A pump 191 and valve combination comprising computer controllable valves 192, 193, 194 and 195 and carrier 86 are connected via Y members 196, 197 and 198 into a dual tubing system for sending carrier 86 up and down. With valves 193, and 195 open, and valves 194 and 192 closed, pump 191 pumps fluid down straight tubing sections 300 or 301 to "land" at Y member 198, downhole where it "stabs in" to unit 14 (FIG. 6A) and gathers data as previously described. When it is desired to return carrier 86 back to the surface the flow is reversed, sending fluid down tubing section 301 to retrieve the new module 86 through tubing 300. This type of arrangement may be described as a pump up/down U tube. Production tubing 12A remains open for continued production throughout this operation.
The foregoing descriptions may make other alternative arrangements apparent to those of skill in the art. For example, the mechanical switches described could be replaced with digital switches, if desired. The aim of the appended claims is to cover all such changes and modifications that fall within the true spirit and scope of the invention. | The downhole portion of the system of the present invention provides entirely downhole methods and apparatus for the monitoring and control of wells. The components of the system are modular. There are sensor and control valve components located in each of the multi-zone production intervals or lateral well completions. The production zones are isolated by production packers equipped with feed-through conductors for communication to upper system components. There are a monitor and control module containing a programmable microprocessor controller and a power supply module which are located at the uppermost end of the system. The system provides for removing, decommissioning and/or replacement of the power module or the monitor and control module without decompleting the well.
The surface portion of the system may be operated from the wellhead or by remote control. In a preferred embodiment, a surface-located test, question, or reprogram module is contained in a controlled buoyancy carrier mounted at the wellhead. The carrier is controlled by a surface control computer. The computer allows the controlled buoyancy carrier to "fall" down through the production tubing and "land" on the downhole monitor and control module. The carrier then interrogates the memory in the monitor and control module and/or reprograms its internal microprocessor as it has been instructed. The carrier then alters its own buoyancy to return via the production tubing to the surface. At the surface it reports the status or sends back the requested data it has gathered via the communications link to the operator. | 4 |
PRIORITY
[0001] This application claims priority to U.S. Provisional Application No. 61/050,915 filed May 6, 2008, which is hereby incorporated by reference in its entirety.
TECHNICAL FIELD OF THE INVENTION
[0002] This invention is related to the area of gastrointestinal inflammation. In particular, it relates to compounds and methods for the treatment of gastrointestinal inflammation.
BACKGROUND OF THE INVENTION
[0003] Environmental stimuli, such as microorganisms and gluten, can lead to increased permeability of biological barriers and initiate significant pathological events in the intestine, brain, heart, and other organs. The pathological consequences of such stimuli include the development of inflammatory diseases. Such external stimuli are presumed to exert physiological effects on biological barriers, possibly through interaction with specific cell surface receptors. However, the mechanisms used remain unclear, and specific cell surface receptors have yet to be confirmed.
[0004] Many inflammatory diseases, including those that are understood to involve increased permeability of biological barriers, are thought to be autoimmune. Such diseases include celiac disease, rheumatoid arthritis, multiple sclerosis, immune-mediated or type 1 diabetes mellitus, inflammatory bowel diseases, systemic lupus erythematosus, psoriasis, scleroderma, necrotizing enterocolitis and autoimmune thyroid diseases. Prolonged inflammation is often associated with these diseases, although the inflammation is thought to be a sequela rather than a primary pathological insult.
Biological Barrier Dysfunction
[0005] Biological barrier function relies upon the structural and functional integrity of tight junctions (TJ), which are one of the hallmarks of absorptive and secretory epithelia. They act as a boundary that physically separates apical and basolateral compartments of epithelial cells, and they selectively regulate the passage of materials through the epithelia by controlling access to the space between the epithelial cells (the paracellular pathway). To meet the many diverse physiological and pathological challenges to which epithelia are subjected, the tight junctions must be capable of rapid, physiologic, reversible, transient, energy dependent, and coordinated responses that require the presence of a complex regulatory system. Examples of epithelia containing tight junctions include, but are not limited to, the intestines (particularly the small intestine), and the blood brain barrier.
[0006] In the absence of stimuli, tight junctions are closed restricting access to the paracellular pathway. In the presence of stimuli, the tight junctions are reversibly opened. Certain bacteria have been shown to have toxins that stimulate the opening of tight junctions. Vibrio cholerae infected with the filamentous bacteriophage CTXΦ, produces a toxin (zonula occludens toxin, ZOT) that has been shown to cause opening of tight junctions. It has been shown that 6 His-ΔG, an N-terminal deletion of ZOT in which the first 264 amino acids, have been deleted and replaced with a six histidine purification tag, retains the ability to open tight junctions.
[0007] Physiological changes in paracellular permeability, which are due to TJ regulation, can be measured as variations in transepithelial conductance. Such variations can usually be attributed to changes in paracellular permeability since the resistances of epithelial plasma membranes are relatively high. TJ represent the major barrier in the paracellular pathway, and the electrical resistance of epithelial tissues seems to depend on their integrity.
[0008] Environmental stimuli, including for example, microorganisms and gluten, can increase permeability of biological barriers as measured by a decrease in trans-epithelial electrical resistance (TEER) (ex vivo) or the Lactulose/mannitol test (in vivo). Such increases in barrier permeability are due primarily to TJ rearrangements, and they are believed to underlie many diseases including a large number of inflammatory conditions.
[0009] TJ dysfunction occurs in a variety of clinical conditions, including food allergies, infections of the gastrointestinal tract, autoimmune diseases, celiac disease and inflammatory bowel diseases. Healthy, mature gut mucosa with its intact tight junction serves as the main barrier to the passage of macromolecules. During the healthy state, small quantities of immunologically active antigens cross the gut host barrier. These antigens are absorbed across the mucosa through at least two pathways. Up to 90% of the absorbed proteins cross the intestinal barrier via the transcellular pathway, followed by lysosomal degradation that converts proteins into smaller, non-immunogenic peptides. These residual peptides are transported as intact proteins through the paracellular pathway, which mediates a subtle, but sophisticated, regulation of intercellular tight junction that leads to antigen tolerance.
[0010] In normal bowels, the immune reaction is regulated to maintain homeostasis of the gut. When TJ integrity is compromised, in premature infants or on exposure to environmental stimuli, radiation, chemotherapy, or toxins, a deleterious immune response to environmental antigens may develop. This response can result in autoimmune diseases and food allergies that lead to inflammation.
[0011] Inflammatory bowel disease (IBD) is a phrase used to describe an inappropriate immune response that occurs in the bowels of affected individuals. Two major types of IBD have been described: Crohn's disease and ulcerative colitis (UC). Both forms of IBD show abnormal profiles of T cell mediated immunity. In the gut of Crohn's disease a strong Th1 reaction is induced; the Th2 response is upregulated in the colon of UC.
[0012] The barrier function of the intestines is impaired in IBD. For example, Crohn's disease is associated with increased permeability of the intestinal barrier even in quiescent patients. A TNF-α-induced increase in intestinal epithelial tight junction (TJ) permeability has been proposed to be an important proinflammatory mechanism contributing to intestinal inflammation in Crohn's disease and other inflammatory conditions. Increased intestinal permeability during episodes of active disease correlates with destruction or rearrangement of TJ protein complexes.
[0013] Examples of inflammatory diseases and disorders that may be treated using the instant invention include, for example, celiac disease, necrotizing enterocolitis, rheumatoid arthritis, multiple sclerosis, immune-mediated or type 1 diabetes mellitus, inflammatory bowel diseases (Crohn's disease and ulcerative colitis), systemic lupus erythematosus, psoriasis, scleroderma, and autoimmune thyroid diseases. Prolonged inflammation is often associated with these diseases, although the inflammation is thought to be a sequela rather than a primary pathological insult.
[0014] Other diseases and disorders associated with biological barrier dysfunction and which may be treated using the instant inventions include, for example, celiac disease, asthma, acute lung injury, acute respiratory distress syndrome, chronic obstructive pulmonary disease, inflammation (e.g., psoriasis and other inflammatory dermatoses), asthma, allergy, cell proliferative disorders (e.g., hyperproliferative skin disorders including skin cancer), metastasis of cancer cells, ion transport disorders such as magnesium transport defects in the kidney, and exposure to Clostridium perfringens enterotoxin (CPE). autoimmune encephalomyelitis, optic neuritis, progressive multifocal leukoencephalopathy (PML), primary biliary cirrhosis, IgA nephropathy, Wegener's granulomatosis, multiple sclerosis, scleroderma, systemic sclerosis, Hashimoto's thyroiditis (underactive thyroid), Graves' disease (overactive thyroid), autoimmune hepatitis, autoimmune inner ear disease, bullous pemphigoid, Devic's syndrome, Goodpasture's syndrome, Lambert-Eaton myasthenic syndrome (LEMS), autoimmune lymphproliferative syndrome (ALPS), paraneoplastic syndromes, polyglandular autoimmune syndromes (PGA), alopecia greata, gastrointestinal inflammation that gives rise to increased intestinal permeability, intestinal conditions that cause protein losing enteropathy, C. difficile infection, enterocolitis, shigellosis, viral gastroenteritis, parasite infestation, bacterial overgrowth, Whipple's disease, diseases with mucosal erosion or ulcerations, gastritis, gastric cancer, collagenous colitis, and mucosal diseases without ulceration, Menetrier's disease, eosinophilic gastroenteritis, diseases marked by lymphatic obstruction, congenital intestinal lymphangiectasia, sarcoidosis lymphoma, mesenteric tuberculosis, after surgical correction of congenital heart disease, and food allergies, primarily to milk.
Inflammation
[0015] Inflammation plays a central role in the pathology of disease conditions that adversely affect a considerable proportion of the population in developed countries. This process is mediated by cytokines, a system of polypeptides that enable one cell to signal to initiate events in another cell that initiate inflammatory sequelae. Normally, the system acts as part of a defensive reaction against infectious agents, harmful environmental agents, or malignantly transformed cells. But when inflammation exceeds the requirements of its defensive role, it can initiate adverse clinical effects, such as arthritis, septic shock, inflammatory bowel disease, and a range of other human disease conditions.
[0016] Immune cells such as monocytes and macrophages secrete cytokines including tumor necrosis factor-α (TNFα) and tumor necrosis factor-β (TNFβ) in response to endotoxin or other stimuli. Cells other than monocytes or macrophages also make cytokines including TNFα. For example, human non-monocytic tumor cell lines produce TNF. CD4 + and CD8 + peripheral blood T lymphocytes and some cultured T and B cell lines also produce TNFα. A large body of evidence associates cytokines such as TNFα with infections, immune disorders, neoplastic pathologies, autoimmune pathologies and graft-versus host pathologies.
[0017] Small-molecule antirheumatic drugs such as methotrexate and sulfasalazine are insufficient to control inflammation in about two-thirds of arthritis patients. New biological agents developed in the last decade have proved to be effective for a majority of patients unresponsive to traditional drugs. The target for such agents is often one of the cytokine pathways—either capturing the ligand conveying the signal from one cell to another, or blocking the receptor at the surface of the effector cell, preventing transduction of the cytokine signal, thereby forestalling the inflammatory events.
[0018] A leading biological agent for treating inflammatory conditions is Enbrel™ (Etanercept), marketed by Amgen Corp. It is a chimeric molecule comprising the extracellular portion of the human TNF receptor linked as a dimer to the IgG Fc region. The compound interferes with the binding of TNF to cell-surface TNF receptors—showing the importance of modulating the TNF pathway for clinical therapy of inflammatory conditions.
[0019] Other TNFα modulating agents currently licensed in the U.S. for treating inflammatory conditions include Cimzia™ (certolizumab pegol), a pegylated antibody fragment that binds to TNFα; Remicade™ (Infliximab), a chimeric antibody that binds TNFα; and Humira™ (adalimumab), a humanized anti-TNFα antibody.
Celiac Disease
[0020] Celiac disease (CD) is a chronic autoimmune disease that is HLA-DQ2/DQ8 haplotype restricted. Glutens, the major protein fraction of wheat, and related proteins in rye and barley are the triggering agents of the disease. Ingested gluten or its derivative fractions (gliadin and subunits) elicit a harmful T cell-mediated immune response after crossing the small bowel epithelial barrier, undergoing deamidation by tissue transglutaminase (tTG) and engaging class II MHC molecules.
[0021] While the earliest events leading to CD involve innate immune responses, evidence in the literature seems to suggest that a dysfunctional cross talk between innate and adaptive immunity is also an important pathogenic element in the autoimmune process of the disease. Under physiological circumstances, the intestinal epithelium, with its intact intercellular tight junctions (tj), serves as a key barrier to the passage of macromolecules such as gluten. When the integrity of the tj system is compromised, as in CD, a paracellular leak (“leaky gut”) and an inappropriate immune response to environmental antigens (i.e., gluten) may develop.
[0022] In celiac intestinal tissues and in in vitro, ex vivo, and in vivo animal experiments, gluten/gliadin causes a rapid increase in permeability in normal and diseased states. Animal models likewise have demonstrated the association of gluten, increased paracellular permeability and other autoimmune diseases, including type 1 diabetes (T1D).
[0023] AT-1001 is an orally administered octapeptide (Gly Gly Val Leu Val Gln Pro Gly (SEQ ID NO:1), that appears to inhibit gliadin-induced TJ disassembly and prevent the associated increase in paracellular permeability. Experiments with ex vivo human tissue and in mice demonstrate that AT-1001 blocks the peak of F-actin increment induced by gliadin and inhibits gliadin induced reduction in intestinal Rt (resistance).
[0024] There is a continuing need in the art for methods to treat inflammatory and autoimmune diseases as well as diseases associated with biological barrier dysfunction more effectively and to discover or identify drugs which are suitable for treating inflammatory and autoimmune diseases as well as diseases associated with biological barrier dysfunction.
SUMMARY OF THE INVENTION
[0025] One object of the present invention is to inhibit increased permeability of biological barriers in response to secreted signals.
[0026] Another object of the present invention is to provide compounds that inhibit secretion of signals that cause increased permeability of biological barriers.
[0027] In particular embodiments the present invention provides compounds that inhibit the secretion of signals that cause increased permeability of biological barriers, wherein the signals are secreted in response to exposure of lymphocytes to lipopolysaccharide (LPS). In other particular embodiments the present invention provides compounds that inhibit the secretion of signals that cause increased permeability of biological barriers, wherein the signals are secreted in response to exposure of lymphocytes to pepsin/trypsin treated gliadin (PTG).
[0028] Another object of the present invention is to provide pharmaceutical compositions that inhibit secretion of signals that cause increased permeability of biological barriers.
[0029] In particular embodiments the present invention provides pharmaceutical compositions that inhibit the secretion of signals that cause increased permeability of biological barriers, wherein the signals are secreted in response to exposure of lymphocytes to lipopolysaccharide (LPS). In other particular embodiments the present invention provides pharmaceutical compositions that inhibit the secretion of signals that cause increased permeability of biological barriers, wherein the signals are secreted in response to exposure of lymphocytes to pepsin/trypsin treated gliadin (PTG).
[0030] Another object of the present invention is to provide methods of treating a patient showing an increased secretion of signals that cause increased permeability of biological barriers.
[0031] In particular embodiments the present invention provides methods of treating a patient showing an increased secretion of signals that cause increased permeability of biological barriers, wherein the signals are secreted in response to exposure of lymphocytes to lipopolysaccharide (LPS). In other particular embodiments the present invention provides methods of treating a patient showing an increased secretion of signals that cause increased permeability of biological barriers, wherein the signals are secreted in response to exposure of lymphocytes to pepsin/trypsin treated gliadin (PTG).
[0032] In certain embodiments, the invention provides a method of treating a patient with an autoimmune or inflammation-associated disease. The disease is selected from the group consisting of inflammatory bowel disease, including Crohn's disease and ulcerative colitis, necrotizing enterocolitis, type 1 diabetes, celiac disease, autoimmune hepatitis, multiple sclerosis, autism, dermatitis herpetiformis, IgA nephropathy, primary biliary chirrosis, rheumatoid arthritis, systemic lupus erythematosus, Grave's disease, Hashimoto's disease, and depression. A compound that inhibits the production, release and/or the biological effects of TNFα is administered to the patient.
[0033] Another object of the present invention is to provide methods to inhibit paracellular passage of gluten derived peptides across an epithelial barrier. Such methods comprise contacting the epithelial barrier with one or more peptide permeability inhibitors. Peptide permeability inhibitors for use in methods of the invention may comprise a peptide of any length. Such peptide permeability inhibitors may comprise a peptide from three to ten amino acids in length. In some embodiments, a peptide permeability inhibitor of the invention may comprise, consist essentially of, or consist of a peptide that comprises, consists essentially of or consists of an amino acid sequence selected from the group consisting of SEQ ID NOs: 1-162. In some embodiments, a peptide permeability inhibitor of the invention may comprise, consist essentially of, or consist of a peptide that comprises, consists essentially of or consists of an amino acid sequence selected from the group consisting of SEQ ID NOs: 1-5, 10-17, 19-23, 27, 32, 34, 36, 48, 49, 55, 58, 67-77, 79-85, 87, 88, 91, 92, 94, 98-104, 106, 110, 111, 113-125, 127, 128, 147, 150, and 160-162. In some embodiments, the invention does not include SEQ ID NOs: 15, 24, and 25.
[0034] The present invention also provides novel methods to inhibit increased paracellular permeability associated with exposure of a biological barrier to gluten derived peptides. Such methods comprise contacting the epithelial barrier with one or more peptide permeability inhibitors. Peptide permeability inhibitors for use in methods of the invention may comprise a peptide of any length. Such peptide permeability inhibitors may comprise a peptide from three to ten amino acids in length. In some embodiments, a peptide permeability inhibitor of the invention may comprise, consist essentially of, or consist of a peptide that comprises, consists essentially of or consists of an amino acid sequence selected from the group consisting of SEQ ID NOs: 1-162. In some embodiments, a peptide permeability inhibitor of the invention may comprise, consist essentially of, or consist of a peptide that comprises, consists essentially of or consists of an amino acid sequence selected from the group consisting of SEQ ID NOs: 1-5, 10-17, 19-23, 27, 32, 34, 36, 48, 49, 55, 58, 67-77, 79-85, 87, 88, 91, 92, 94, 98-104, 106, 110, 111, 113-125, 127, 128, 147, 150, and 160-162. In some embodiments, the invention does not include SEQ ID NOs: 15, 24, and 25.
[0035] The present invention also provides compositions, e.g., pharmaceutical compositions, comprising one or more peptide permeability inhibitors of the invention, useful to inhibit paracellular passage of gluten derived peptides across an epithelial barrier. Peptide permeability inhibitors for use in compositions of the invention may comprise a peptide of any length. In some embodiments, such peptide permeability inhibitors may comprise a peptide of between three to ten amino acids in length. Suitable peptide permeability inhibitors for use in the compositions of the invention include, but are not limited to, peptide permeability inhibitors that comprise, consist essentially of, or consist of an amino acid sequence selected from the group consisting of SEQ ID NOs: 1-162. In some embodiments, peptide permeability inhibitors for use in the compositions of the invention include, but are not limited to, peptide permeability inhibitors comprising peptides that comprise, consist essentially of, or consist of an amino acid sequence selected from the group consisting of SEQ ID NOs: 1-5, 10-17, 19-23, 27, 32, 34, 36, 48, 49, 55, 58, 67-77, 79-85, 87, 88, 91, 92, 94, 98-104, 106, 110, 111, 113-125, 127, 128, 147, 150, and 160-162. In some embodiments, the invention does not include SEQ ID NOs: 15, 24, and 25.
[0036] Compositions of the invention, for example, pharmaceutical compositions, may be formulated for any type of delivery. For example, compositions of the invention may be formulated for intestinal delivery, e.g., may be delayed release compositions. Compositions of the invention may also be formulated for pulmonary delivery, oral delivery and/or transcutaneous delivery.
[0037] In one embodiment, the present invention provides a method of treating a disease in a subject in need thereof. Methods of the invention may comprise administering to the subject a pharmaceutical composition comprising one or more peptide permeability inhibitors of the invention. Methods of the invention may comprise administering to the subject a pharmaceutical composition comprising one or more peptide permeability inhibitors and one or more additional therapeutic agents. In one embodiment, the present invention provides a method of treating celiac disease in a subject in need thereof. In another embodiment, the present invention provides a method of treating necrotizing enterocolitis in a subject in need thereof. In another embodiment, the present invention provides a method of treating an excessive or undesirable immune response in a subject in need thereof. In another embodiment, the present invention provides a method of treating inflammation in a subject in need thereof. In specific embodiments, the present invention provides methods of treating inflammatory bowel disease in a subject in need thereof. Inflammatory bowel disease that can be treated using methods of the present invention may be Crohn's disease or ulcerative colitis.
[0038] In further embodiments the invention provides methods of treating an autoimmune or inflammation-associated disease in a patient in need of such treatment. The disease is selected from the group consisting of type 1 diabetes, celiac disease, autoimmune hepatitis, multiple sclerosis, autism, dermatitis herpetiformis, IgA nephropathy, primary biliary chirrosis, rheumatoid arthritis, systemic lupus erythematosus, Grave's disease, Hashimoto's disease, and depression.
[0039] The foregoing has outlined rather broadly the features and technical advantages of the present invention in order that the detailed description of the invention that follows may be better understood. Additional features and advantages of the invention will be described herein, which form the subject of the claims of the invention. It should be appreciated by those skilled in the art that any conception and specific embodiment disclosed herein may be readily utilized as a basis for modifying or designing other structures 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. The novel features which are believed to be characteristic of the invention, both as to its organization and method of operation, together with further objects and advantages will be better understood from the following description when considered in connection with the accompanying figures. It is to be expressly understood, however, that any description, figure, example, etc. is provided for the purpose of illustration and description only and is by no means intended to define the limits the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0040] FIG. 1 is a schematic representation of the events leading to Celiac disease pathology. Gliadin fragments cross the intestinal epithelium and activate immune cells to produce soluble factors including cytokines that lead to increased permeability of the intestinal epithelium.
[0041] FIG. 2 is a schematic representation of the blockade of the gliadin fragment entry, the initial step leading to Celiac disease pathology. Gliadin fragments cross the intestinal epithelium and activate immune cells to produce soluble factors including cytokines that lead to increased permeability of the intestinal epithelium.
[0042] FIG. 3 shows the effect of a peptide permeability inhibitor (SEQ ID NO:1) on permeability of a CaCO2 cell monolayer to a gliadin fragment. Apical exposure of the monolayer to the gliadin peptide PYPQPQLPY (SEQ ID NO:163) lead to an increase in permeability to that peptide, which could be blocked by apical treatment with a peptide permeability inhibitor (SEQ ID NO:1).
[0043] FIG. 4 shows the effect of a 13-mer gliadin peptide (LGQQQPFPPQQPY; SEQ ID NO:164) on permeability of a CaCO2 cell monolayer induced by a. Apical exposure of the monolayer to the gliadin peptide FITC-C6-PYPQPQLPY lead to an increase in permeability that could be blocked by treatment with a peptide permeability inhibitor (SEQ ID NO:1).
[0044] FIG. 5A shows the effects on CaCO2 cell permeability of 72 hours treatment with peptide permeability inhibitor (SEQ ID NO:1) in combination with culture supernatants prepared from donor PBMCs (00022). After formation of tight junctions CaCO2 cells were exposed basolaterally to control supernatant (control), untreated PBMC supernatant (PBMC sup), LPS treated PBMC supernatant (PBMC-LPS) and PTG treated PBMC supernatant (PBMC-PTG). Lucifer yellow permeability was measured after 72 hours (day3). Simultaneous apical addition of peptide permeability inhibitor (SEQ ID NO:1) on day 0 abolished baseline permeability to Lucifer yellow (control+AT-1001; and PBMC sup+AT1001) but had no significant effect on permeability changes induced by LPS (PBMC-LPS+AT1001) or PTG treated PBMC supernatant (PBMC-PTG+AT1001).
[0045] FIG. 5B shows the effects on CaCO2 cell permeability of 72 hours exposure to culture supernatants prepared from donor PBMCs (00022) followed by addition of peptide permeability inhibitor (SEQ ID NO:1) after 48 hours treatment. After formation of tight junctions CaCO2 cells were exposed basolaterally to PBMC supernatants as described above. Peptide permeability inhibitor (SEQ ID NO:1) was added apically to the cultures after 48 hours (day 2), and lucifer yellow permeability was measured after 72 hours (day3). Apical addition of peptide permeability inhibitor (SEQ ID NO:1) on day 2 abolished baseline permeability to Lucifer yellow (control+AT-1001; and PBMC sup+AT1001), and it significantly reduced permeability changes induced by LPS (PBMC-LPS+AT1001) or PTG treated PBMC supernatant (PBMC-PTG+AT 1001).
[0046] FIG. 6A shows the effects on CaCO2 cell permeability of 72 hours treatment with peptide permeability inhibitor (SEQ ID NO:1) in combination with culture supernatants prepared from donor PBMCs (00023). After formation of tight junctions CaCO2 cells were exposed basolaterally to control supernatant (control), untreated PBMC supernatant (PBMC sup), LPS treated PBMC supernatant (PBMC-LPS) and PTG treated PBMC supernatant (PBMC-PTG). Lucifer yellow permeability was measured after 72 hours (day3). Simultaneous apical addition of peptide permeability inhibitor (SEQ ID NO:1) on day 0 abolished baseline permeability to Lucifer yellow (control+AT-1001; and PBMC sup+AT1001) but had no significant effect on permeability changes induced by LPS (PBMC-LPS+AT1001) or PTG treated PBMC supernatant (PBMC-PTG+AT1001).
[0047] FIG. 6B shows the effects on CaCO2 cell permeability of 72 hours exposure to culture supernatants prepared from donor PBMCs (00023) followed by addition of peptide permeability inhibitor (SEQ ID NO:1) after 48 hours treatment. After formation of tight junctions CaCO2 cells were exposed basolaterally to PBMC supernatants as described above. Peptide permeability inhibitor (SEQ ID NO:1) was added apically to the cultures after 48 hours (day 2), and lucifer yellow permeability was measured after 72 hours (day3). Apical addition of peptide permeability inhibitor (SEQ ID NO:1) on day 2 abolished baseline permeability to Lucifer yellow (control+AT-1001; and PBMC sup+AT1001), and it significantly reduced permeability changes induced by LPS (PBMC-LPS+AT1001) or PTG treated PBMC supernatant (PBMC-PTG+AT1001).
[0048] FIG. 7A shows the effects on CaCO2 cell permeability of 72 hours treatment with peptide permeability inhibitor (SEQ ID NO:1) in combination with culture supernatants prepared from donor PBMCs (00064). After formation of tight junctions CaCO2 cells were exposed basolaterally to control supernatant (control), untreated PBMC supernatant (PBMC sup), LPS treated PBMC supernatant (PBMC-LPS) and PTG treated PBMC supernatant (PBMC-PTG). Lucifer yellow permeability was measured after 72 hours (day3). Simultaneous apical addition of peptide permeability inhibitor (SEQ ID NO:1) on day 0 abolished baseline permeability to Lucifer yellow (control+AT-1001; and PBMC sup+AT1001) but had no significant effect on permeability changes induced by LPS (PBMC-LPS+AT1001) or PTG treated PBMC supernatant (PBMC-PTG+AT 1001).
[0049] FIG. 7B shows the effects on CaCO2 cell permeability of 72 hours exposure to culture supernatants prepared from donor PBMCs (00064) followed by addition of peptide permeability inhibitor (SEQ ID NO:1) after 48 hours treatment. After formation of tight junctions CaCO2 cells were exposed basolaterally to PBMC supernatants as described above. Peptide permeability inhibitor (SEQ ID NO:1) was added apically to the cultures after 48 hours (day 2), and lucifer yellow permeability was measured after 72 hours (day3). Apical addition of peptide permeability inhibitor (SEQ ID NO:1) on day 2 abolished baseline permeability to Lucifer yellow (control+AT-1001; and PBMC sup+AT1001), and it significantly reduced permeability changes induced by LPS (PBMC-LPS+AT1001) or PTG treated PBMC supernatant (PBMC-PTG+AT 1001).
[0050] FIG. 8A shows the effects on CaCO2 cell permeability of 72 hours treatment with peptide permeability inhibitor (SEQ ID NO:1) in combination with culture supernatants prepared from donor PBMCs (00065). After formation of tight junctions CaCO2 cells were exposed basolaterally to control supernatant (control), untreated PBMC supernatant (PBMC sup), LPS treated PBMC supernatant (PBMC-LPS) and PTG treated PBMC supernatant (PBMC-PTG). Lucifer yellow permeability was measured after 72 hours (day3). Simultaneous apical addition of peptide permeability inhibitor (SEQ ID NO:1) on day 0 abolished baseline permeability to Lucifer yellow (control+AT-1001; and PBMC sup+AT1001) but had no significant effect on permeability changes induced by LPS (PBMC-LPS+AT1001) or PTG treated PBMC supernatant (PBMC-PTG+AT1001).
[0051] FIG. 8B shows the effects on CaCO2 cell permeability of 72 hours exposure to culture supernatants prepared from donor PBMCs (00065) followed by addition of peptide permeability inhibitor (SEQ ID NO:1) after 48 hours treatment. After formation of tight junctions CaCO2 cells were exposed basolaterally to PBMC supernatants as described above. Peptide permeability inhibitor (SEQ ID NO:1) was added apically to the cultures after 48 hours (day 2), and lucifer yellow permeability was measured after 72 hours (day3). Apical addition of peptide permeability inhibitor (SEQ ID NO:1) on day 2 abolished baseline permeability to Lucifer yellow (control+AT-1001; and PBMC sup+AT1001), and it significantly reduced permeability changes induced by LPS (PBMC-LPS+AT1001) or PTG treated PBMC supernatant (PBMC-PTG+AT1001).
DETAILED DESCRIPTION OF THE INVENTION
[0052] The inventors have discovered that peripheral blood mononuclear cells (PBMCs) secrete signals that increase epithelial monolayer permeability on response to stimulation with lipopolysaccharide (PLPS) and pepsin/trypsin treated gliadin (PTG). These secreted signals are present in PBMC culture supernatant, and they increase permeability of CaCO2 cell monolayers to Lucifer yellow when presented to the basolateral aspect of these cells. These permeability changes are inhibited by treatment of the cells with peptide permeability inhibitors of the invention ( FIGS. 5A , 5 B, 6 A, 6 B, 7 A, 7 B, 8 A and 8 B). The inventors have also discovered that specific peptides within the PTG mixture are capable of crossing epithelial cell monolayers in vitro, and that this peptide specific mechanism can be inhibited by peptide permeability inhibitors of the invention ( FIGS. 3 and 4 ).
DEFINITIONS
[0053] Unless otherwise noted, technical terms are used according to conventional usage. Definitions of common terms in molecular biology may be found, for example, in Benjamin Lewin, Genes VII, published by Oxford University Press, 2000 (ISBN 019879276X); Kendrew et al. (eds.); The Encyclopedia of Molecular Biology, published by Blackwell Publishers, 1994 (ISBN 0632021829); and Robert A. Meyers (ed.), Molecular Biology and Biotechnology: a Comprehensive Desk Reference, published by Wiley, John & Sons, Inc., 1995 (ISBN 0471186341); and other similar technical references.
[0054] As used herein, “a” or “an” may mean one or more. As used herein in the claim(s), when used in conjunction with the word “comprising”, the words “a” or “an” may mean one or more than one. As used herein “another” may mean at least a second or more. Furthermore, unless otherwise required by context, singular terms shall include pluralities and plural terms shall include the singular.
[0055] As used herein, “biological effect” refers to a biochemical and physiological effect. Biological effect includes, for example, increases or decreases in the activity of the immune system and any of its components (including, for example, complement activation), increases or decreases in receptor binding and increases or decreases in subsequent downstream effector cellular constituents (including, for example, growth factor receptor and downstream effector cellular constituents), increases or decreases in cell signaling, increases or decreases in gene expression, increases or decreased in post-translation modification of proteins (including, for example, phosphorylation), and increases or decreases in protein activity.
[0056] As used herein, “modulate” and all its forms and tenses refer to either increasing or decreasing a particular biochemical or physiological effect.
[0057] As used herein, A “component of the immune system” or an “immune cell” refers to a component or cell of the immune system that is involved in enhancing, eliciting, or maintaining an immune response. The immune system responds to various foreign particles (including, for example, viruses, bacteria, and allergens) and non-foreign particles (including, for example, native endogenous proteins). An immune response includes, for example, antibody production, chemotaxis, phagocytosis, inflammation, complement activation, production of cytotoxic molecules (including, for example, reactive oxygen species and reactive nitrogen species), cell adhesion, cell infiltration, and production and recruitment of mediators of any of the foregoing or other immune responses. A component or cell of the immune system involved in enhancing, eliciting, or maintaining an immune response includes, for example, neutrophils, complement proteins (including, for example, C1q, C1r and C1s), eosinophils, basophils, lymphocytes (including for example, T cells (including, for example, cytotoxic T cells, memory T cells, helper T cells, regulatory T cells, natural killer T cells, and γδ T cells) and B cells (including, for example, plasma B cells, memory B cells, B-1 cells, and B-2 cells)), monocytes, macrophages, dendritic cells (DC), cell adhesion molecules (including, for example, ICAM and VCAM), myeloperoxidase, nitric oxide synthase, cyclooxygenase, and prostaglandin synthase.
[0058] As used herein, “treat” and all its forms and tenses refer to both therapeutic treatment and prophylactic or preventative treatment. Those in need of treatment include those already with the condition or disease as well as those in which the condition or disease is to be prevented.
[0059] Present Invention
[0060] The inventors have identified novel methods and compounds that inhibit increased permeability of biological barriers in response to stimuli that are known to induce secretion of pro-inflammatory cytokines. In specific embodiments the inventors have identified methods and compounds that inhibit increased permeability of biological barriers after stimulation by factors secreted by immune cells on exposure to LPS. In further specific embodiments the inventors have identified methods and compounds that inhibit increased permeability of biological barriers after stimulation by factors secreted by immune cells on exposure to PTG. Exemplary compounds of the invention that inhibit increased permeability of biological barriers are presented in Table 20.
[0061] The inventors have also identified novel methods and compounds that inhibit, reduce and/or prevent translocation of PTG-derived peptides across biological barriers. In specific embodiments the inventors have identified methods and compounds that inhibit, reduce and/or prevent translocation of the peptide comprising the amino acid sequence PYPQPQLPY (SEQ ID NO:163). Exemplary compounds of the invention that inhibit, reduce and/or prevent translocation of PTG-derived peptides across biological barriers are presented in Table 20.
[0062] Inhibitors of biological barrier permeability may be used in the practice of the present invention. Such permeability inhibitors may also be antagonists of mammalian tight junction opening. Antagonists of mammalian tight junction opening may also be used in the practice of the present invention. As used herein, permeability inhibitors prevent, inhibit or reduce the permeability of biological barriers to macromolecules including, for example, proteins, peptides and nucleic acids. For example, permeability inhibitors of the invention may comprise peptide permeability inhibitors. Examples of peptide permeability inhibitors that may be used in the practice of the present invention include, but are not limited to, peptides that comprise an amino acid sequence selected from the group consisting of: consist of an amino acid sequence selected from the group consisting of SEQ ID NOs: 1-5, 10-17, 19-23, 27, 32, 34, 36, 48, 49, 55, 58, 67-77, 79-85, 87, 88, 91, 92, 94, 98-104, 106, 110, 111, 113-125, 127, 128, 147, 150, and 160-162.
[0063] Examples of peptide permeability inhibitors include, but are not limited to, peptides that consist of an amino acid sequence selected from the group consisting of SEQ ID NOs:1-162.
[0064] When the permeability inhibitor is a peptide, any length of peptide may be used. Generally, the size of the peptide antagonist will range from about 6 to about 100, from about 6 to about 90, from about 6 to about 80, from about 6 to about 70, from about 6 to about 60, from about 6 to about 50, from about 6 to about 40, from about 6 to about 30, from about 6 to about 25, from about 6 to about 20, from about 6 to about 15, from about 6 to about 14, from about 6 to about 13, from about 6 to about 12, from about 6 to about 11, from about 6 to about 10, from about 6 to about 9, or from about 6 to about 8 amino acids in length. Peptide antagonists of the invention may be from about 8 to about 100, from about 8 to about 90, from about 8 to about 80, from about 8 to about 70, from about 8 to about 60, from about 8 to about 50, from about 8 to about 40, from about 8 to about 30, from about 8 to about 25, from about 8 to about 20, from about 8 to about 15, from about 8 to about 14, from about 8 to about 13, from about 8 to about 12, from about 8 to about 11, or from about 8 to about 10 amino acids in length. Peptide antagonists of the invention may be from about 10 to about 100, from about 10 to about 90, from about 10 to about 80, from about 10 to about 70, from about 10 to about 60, from about 10 to about 50, from about 10 to about 40, from about 10 to about 30, from about 10 to about 25, from about 10 to about 20, from about 10 to about 15, from about 10 to about 14, from about 10 to about 13, or from about 10 to about 12 amino acids in length. Peptide antagonists of the invention may be from about 12 to about 100, from about 12 to about 90, from about 12 to about 80, from about 12 to about 70, from about 12 to about 60, from about 12 to about 50, from about 12 to about 40, from about 12 to about 30, from about 12 to about 25, from about 12 to about 20, from about 12 to about 15, or from about 12 to about 14 amino acids in length. Peptide antagonists of the invention may be from about 15 to about 100, from about 15 to about 90, from about 15 to about 80, from about 15 to about 70, from about 15 to about 60, from about 15 to about 50, from about 15 to about 40, from about 15 to about 30, from about 15 to about 25, from about 15 to about 20, from about 19 to about 15, from about 15 to about 18, or from about 17 to about 15 amino acids in length.
[0065] The peptide permeability inhibitors can be chemically synthesized and purified using well-known techniques, such as described in High Performance Liquid Chromatography of Peptides and Proteins: Separation Analysis and Conformation , Eds. Mant et al., C.R.C. Press (1991), and a peptide synthesizer, such as Symphony (Protein Technologies, Inc); or by using recombinant DNA techniques, i.e., where the nucleotide sequence encoding the peptide is inserted in an appropriate expression vector, e.g., an E. coli or yeast expression vector, expressed in the respective host cell, and purified therefrom using well-known techniques.
Compositions
[0066] Typically, compositions, such as pharmaceutical compositions, comprise one or more compounds of the invention, and optionally one or more additional active agents. Compounds of the invention may be present in an amount sufficient to inhibit the increased biological barrier permeability in a subject in need thereof. Compounds of the invention may be present in an amount sufficient to inhibit, reduce and/or prevent translocation of a gliadin-derived peptide across a biological barrier in a subject in need thereof. The amount of a compound of the invention employed in any given composition may vary according to factors such as the disease state, age, sex, and weight of the subject. Dosage regimens may be adjusted to provide the optimum therapeutic response. For example, a single bolus may be administered, several divided doses may be administered over time or the dose may be proportionally reduced or increased as indicated by the exigencies of the therapeutic situation.
[0067] Generally, a pharmaceutical composition of the invention will comprise an amount of a compound of the invention in the range of about 1 μg to about 1 g, preferably about 1 mg to about 1000 mg, from about 10 mg to about 100 mg, from about 10 mg to about 50 mg, or from about 10 mg to about 25 mg of the compound. As used herein, “about” used to modify a numerical value means within 10% of the value.
[0068] Compositions of the invention may comprise one or more compounds of the invention at a level of from about 0.1 wt % to about 20 wt %, from about 0.1 wt % to about 18 wt %, from about 0.1 wt % to about 16 wt %, from about 0.1 wt % to about 14 wt %, from about 0.1 wt % to about 12 wt %, from about 0.1 wt % to about 10 wt %, from about 0.1 wt % to about 8 wt %, from about 0.1 wt % to about 6 wt %, from about 0.1 wt % to about 4 wt %, from about 0.1 wt % to about 2 wt %, from about 0.1 wt % to about 1 wt %, from about 0.1 wt % to about 0.9 wt %, from about 0.1 wt % to about 0.8 wt %, from about 0.1 wt % to about 0.7 wt %, from about 0.1 wt % to about 0.6 wt %, from about 0.1 wt % to about 0.5 wt %, from about 0.1 wt % to about 0.4 wt %, from about 0.1 wt % to about 0.3 wt %, or from about 0.1 wt % to about 0.2 wt % of the total weight of the composition. As used herein, “about” used to modify a numerical value means within 10% of the value. Compositions of the invention may comprise one or more compounds of the invention at a level of about 0.1 wt %, about 0.2 wt %, about 0.3 wt %, about 0.4 wt %, about 0.5 wt %, about 0.6 wt %, about 0.7 wt %, about 0.8 wt %, or about 0.9 wt % based on the total weight of the composition.
[0069] Compositions of the invention may comprise one or more compounds of the invention at a level of from about 1 wt % to about 20 wt %, from about 1 wt % to about 18 wt %, from about 1 wt % to about 16 wt %, from about 1 wt % to about 14 wt %, from about 1 wt % to about 12 wt %, from about 1 wt % to about 10 wt %, from about 1 wt % to about 9 wt %, from about 1 wt % to about 8 wt %, from about 1 wt % to about 7 wt %, from about 1 wt % to about 6 wt %, from about 1 wt % to about 5 wt %, from about 1 wt % to about 4 wt %, from about 1 wt % to about 3 wt %, or from about 1 wt % to about 2 wt % of the total weight of the composition. As used herein, “about” used to modify a numerical value means within 10% of the value. Compositions of the invention may comprise one or more compounds of the invention at a level of about 1 wt %, about 2 wt %, about 3 wt %, about 4 wt %, about 5 wt %, about 6 wt %, about 7 wt %, about 8 wt %, or about 9 wt % based on the total weight of the composition.
[0070] Compositions of the invention, for example, pharmaceutical compositions comprising one or more compounds of the invention and one or more additional active agents, may be formulated for pulmonary delivery (e.g., may be pulmonary dosage forms). Typically such compositions may be provided as pharmaceutical aerosols, e.g., solution aerosols or powder aerosols. Those of skill in the art are aware of many different methods and devices for the formation of pharmaceutical aerosols, for example, those disclosed by Sciarra and Sciarra, Aerosols , in Remington: The Science and Practice of Pharmacy, 20th Ed., Chapter 50, Gennaro et al. Eds., Lippincott, Williams and Wilkins Publishing Co., (2000).
[0071] In one embodiment, the dosage forms are in the form of a powder aerosol (i.e, comprise particles). These are particularly suitable for use in inhalation delivery systems. Powders may comprise particles of any size suitable for administration to the lung.
[0072] Powder formulations may optionally contain at least one particulate pharmaceutically acceptable carrier known to those of skill in the art. Examples of suitable pharmaceutical carriers include, but are not limited to, saccharides, including monosaccharides, disaccharides, polysaccharides and sugar alcohols such as arabinose, glucose, fructose, ribose, mannose, sucrose, trehalose, lactose, maltose, starches, dextran, mannitol or sorbitol. In one embodiment, a powder formulation may comprise lactose as a carrier.
[0073] Powder formulations may be contained in any container known to those in the art. Containers may be capsules of, for example, gelatin or plastic, or in blisters (e.g. of aluminum or plastic), for use in a dry powder inhalation device. In some embodiments, the total weight of the formulation in the container may be from about 5 mg to about 50 mg. In other embodiments, powder formulations may be contained in a reservoir in a multi-dose dry powder inhalation device adapted to deliver a suitable amount per actuation.
[0074] Powder formulations typically comprise small particles. Suitable particles can be prepared using any means known in the art, for example, by grinding in an airjet mill, ball mill or vibrator mill, sieving, microprecipitation, spray-drying, lyophilisarion or controlled crystallisation. Typically, particles will be about 10 microns or less in diameter. Particles for use in the compositions of the invention may have a diameter of from about 0.1 microns to about 10 microns, from about 0.1 microns to about 9 microns, from about 0.1 microns to about 8 microns, from about 0.1 microns to about 7 microns, from about 0.1 microns to about 6 microns, from about 0.1 microns to about 5 microns, from about 0.1 microns to about 4 microns, from about 0.1 microns to about 3 microns, from about 0.1 microns to about 2 microns, from about 0.1 microns to about 1 micron, from about 0.1 microns to about 0.5 microns, from about 1 micron to about 10 microns, from about 1 micron to about 9 microns, from about 1 micron to about 8 microns, from about 1 micron to about 7 microns, from about 1 micron to about 6 microns, from about 1 micron to about 5 microns, from about 1 micron to about 4 microns, from about 1 micron to about 3 microns, from about 1 micron to about 2 microns, from about 2 microns to about 10 microns, from about 2 microns to about 9 microns, from about 2 microns to about 8 microns, from about 2 microns to about 7 microns, from about 2 microns to about 6 microns, from about 2 microns to about 5 microns, from about 2 microns to about 4 microns, or from about 2 microns to about 3 microns. As used herein, “about” used to modify a numerical value means within 10% of the value. In some embodiments, particles for use in the invention may be about 1 micron, about 2 microns, about 3 microns, about 4 microns, about 5 microns, about 6 microns, about 7 microns, about 8 microns, about 9 microns, or about 10 microns in diameter.
[0075] In one embodiment, the dosage forms are in the form of a solution aerosol (i.e., comprise droplets). Typically, droplets will be about 10 microns or less in diameter. Droplets for use in the compositions of the invention may have a diameter of from about 0.1 microns to about 10 microns, from about 0.1 microns to about 9 microns, from about 0.1 microns to about 8 microns, from about 0.1 microns to about 7 microns, from about 0.1 microns to about 6 microns, from about 0.1 microns to about 5 microns, from about 0.1 microns to about 4 microns, from about 0.1 microns to about 3 microns, from about 0.1 microns to about 2 microns, from about 0.1 microns to about 1 micron, from about 0.1 microns to about 0.5 microns, from about micron to about 10 microns, from about 1 micron to about 9 microns, from about 1 micron to about 8 microns, from about 1 micron to about 7 microns, from about 1 micron to about 6 microns, from about 1 micron to about 5 microns, from about 1 micron to about 4 microns, from about 1 micron to about 3 microns, from about 1 micron to about 2 microns, from about 2 microns to about 10 microns, from about 2 microns to about 9 microns, from about 2 microns to about 8 microns, from about 2 microns to about 7 microns, from about 2 microns to about 6 microns, from about 2 microns to about 5 microns, from about 2 microns to about 4 microns, or from about 2 microns to about 3 microns. As used herein, “about” used to modify a numerical value means within 10% of the value. In some embodiments, particles and/or droplets for use in the invention may be about 1 micron, about 2 microns, about 3 microns, about 4 microns, about 5 microns, about 6 microns, about 7 microns, about 8 microns, about 9 microns, or about 10 microns in diameter.
[0076] The compositions of the invention may be formulated for enteric delivery, for example, may comprise one or more coatings including, for example, a delayed release coating containing one or more enteric agents. A delayed release coating is typically substantially stable in gastric fluid and substantially unstable (e.g., dissolves rapidly or is physically unstable) in intestinal fluid, thus providing for substantial release of the compounds of the invention and/or additional active agent from the composition in the duodenum or the jejunum.
[0077] The term “stable in gastric fluid” refers to a composition that releases 30% or less by weight of the total compound of the invention and/or additional active agent in the composition in gastric fluid with a pH of 5 or less, or simulated gastric fluid with a pH of 5 or less, in approximately sixty minutes. Examples of simulated gastric fluid and simulated intestinal fluid include, but are not limited to, those disclosed in the 2005 Pharmacopeia 23NF/28USP in Test Solutions at page 2858 and/or other simulated gastric fluids and simulated intestinal fluids known to those of skill in the art, for example, simulated gastric fluid and/or intestinal fluid prepared without enzymes.
[0078] Compositions of the of the invention may release from about 0% to about 30%, from about 0% to about 25%, from about 0% to about 20%, from about 0% to about 15%, from about 0% to about 10%, from about 5% to about 30%, from about 5% to about 25%, from about 5% to about 20%, from about 5% to about 15%, from about 5% to about 10% by weight of the total compound of the invention and/or additional active agent in the composition in gastric fluid with a pH of 5 or less, or simulated gastric fluid with a pH of 5 or less, in approximately sixty minutes. As used herein, “about” used to modify a numerical value means within 10% of the value. Compositions of the invention may release about 1%, about 2%, about 3%, about 4%, about 5%, about 6%, about 7%, about 8%, about 9%, or about 10% by weight of the total compound of the invention in the composition in gastric fluid with a pH of 5 or less, or simulated gastric fluid with a pH of 5 or less, in approximately sixty minutes.
[0079] The term “unstable in intestinal fluid” refers to a composition that releases 70% or more by weight of the total amount of the compound of the invention and/or additional active agent in the composition in intestinal fluid or simulated intestinal fluid in approximately sixty minutes. The term “unstable in near neutral to alkaline environments” refers to a composition that releases 70% or more by weight of the total amount of the compound of the invention and/or additional active agent in the composition in intestinal fluid with a pH of 5 or greater, or simulated intestinal fluid with a pH of 5 or greater, in approximately ninety minutes. For example, a composition that is unstable in near neutral or alkaline environments may release 70% or more by weight of a compound of the invention and/or additional active agent in a fluid having a pH greater than about 5 (e.g., a fluid having a pH of from about 5 to about 14, from about 6 to about 14, from about 7 to about 14, from about 8 to about 14, from about 9 to about 14, from about 10 to about 14, or from about 11 to about 14) in from about 5 minutes to about 90 minutes, from about 10 minutes to about 90 minutes, from about 15 minutes to about 90 minutes, from about 20 minutes to about 90 minutes, from about 25 minutes to about 90 minutes, from about 30 minutes to about 90 minutes, from about 5 minutes to about 60 minutes, from about 10 minutes to about 60 minutes, from about 15 minutes to about 60 minutes, from about 20 minutes to about 60 minutes, from about 25 minutes to about 60 minutes, or from about 30 minutes to about 60 minutes. As used herein, “about” used to modify a numerical value means within 10% of the value.
[0080] Compositions of the invention may be formulated for transcutaneous delivery (e.g., may be transcutaneous dosage forms). Typically such compositions may be provided as topical solutions and/or gels. Those of skill in the art are aware of many different methods and devices for the formation of topical medications, for example, those disclosed by Block, Medicated Topicals , in Remington: The Science and Practice of Pharmacy, 20th Ed., Chapter 44, Gennaro et al. Eds., Lippincott, Williams and Wilkins Publishing Co. (2000).
[0081] Various delivery systems are known and can be used to administer a compound of the invention, e.g., encapsulation in liposomes, microparticles, microcapsules, recombinant cells capable of expressing the compound, receptor-mediated endocytosis etc. Methods of introduction include but are not limited to intradermal, intramuscular, intraperitoneal, intravenous, subcutaneous, intranasal, epidural, and oral routes. The compounds or compositions may be administered by any convenient route, for example by infusion or bolus injection, by absorption through epithelial or mucocutaneous linings (e.g., oral mucosa, rectal and intestinal mucosa, etc.) and may be administered together with other biologically active agents. Administration can be systemic or local. In addition, it may be desirable to introduce the pharmaceutical compounds or compositions of the invention into the central nervous system by any suitable route, including intraventricular and intrathecal injection; intraventricular injection may be facilitated by an intraventricular catheter, for example, attached to a reservoir, such as an Ommaya reservoir. Pulmonary administration can also be employed, e.g., by use of an inhaler or nebulizer, and formulation with an aerosolizing agent.
[0082] In a specific embodiment, it may be desirable to administer the pharmaceutical compounds or compositions of the invention locally to the area in need of treatment; this may be achieved by, for example, and not by way of limitation, local infusion during surgery, topical application, e.g., in conjunction with a wound dressing after surgery, by injection, by means of a catheter, by means of a suppository, or by means of an implant, said implant being of a porous, non-porous, or gelatinous material, including membranes, such as sialastic membranes, or fibers. Preferably, when administering a protein, including an antibody, of the invention, care must be taken to use materials to which the protein does not adsorb.
[0083] In another embodiment, the compound or composition can be delivered in a vesicle, in particular a liposome.
[0084] In yet another embodiment, the compound or composition can be delivered in a controlled release system. In one embodiment, a pump may be used. In another embodiment, polymeric materials can be used. In yet another embodiment, a controlled release system can be placed in proximity of the therapeutic target, i.e., the brain, thus requiring only a fraction of the systemic dose. Other controlled release systems are well known in the art.
[0085] The present invention also provides pharmaceutical compositions. Such compositions comprise a therapeutically effective amount of a compound, and a pharmaceutically acceptable carrier. In a specific embodiment, the term “pharmaceutically acceptable” means approved by a regulatory agency of the Federal or a state government or listed in the U.S. Pharmacopeia or other generally recognized pharmacopeia for use in animals, and more particularly in humans. The term “carrier” refers to a diluent, adjuvant, excipient, or vehicle with which the therapeutic is administered. Such pharmaceutical carriers can be sterile liquids, such as water and oils, including those of petroleum, animal, vegetable or synthetic origin, such as peanut oil, soybean oil, mineral oil, sesame oil and the like. Water is a preferred carrier when the pharmaceutical composition is administered intravenously. Saline solutions and aqueous dextrose and glycerol solutions can also be employed as liquid carriers, particularly for injectable solutions. Suitable pharmaceutical excipients include starch, glucose, lactose, sucrose, gelatin, malt, rice, flour, chalk, silica gel, sodium stearate, glycerol monostearate, talc, sodium chloride, dried skim milk, glycerol, propylene, glycol, water, ethanol and the like. The composition, if desired, can also contain minor amounts of wetting or emulsifying agents, or pH buffering agents. These compositions can take the form of solutions, suspensions, emulsion, tablets, pills, capsules, powders, sustained-release formulations and the like. The composition can be formulated as a suppository, with traditional binders and carriers such as triglycerides. Oral formulation can include standard carriers such as pharmaceutical grades of mannitol, lactose, starch, magnesium stearate, sodium saccharine, cellulose, magnesium carbonate, etc. Examples of suitable pharmaceutical carriers are described in “Remington's Pharmaceutical Sciences” by E. W. Martin. Such compositions will contain a therapeutically effective amount of the compound, preferably in purified form, together with a suitable amount of carrier so as to provide the form for proper administration to the patient. The formulation should suit the mode of administration.
[0086] In a preferred embodiment, the composition is formulated in accordance with routine procedures as a pharmaceutical composition adapted for intravenous administration to human beings. Typically, compositions for intravenous administration are solutions in sterile isotonic aqueous buffer. Where necessary, the composition may also include a solubilizing agent and a local anesthetic such as lignocaine to ease pain at the site of the injection. Generally, the ingredients are supplied either separately or mixed together in unit dosage form, for example, as a dry lyophilized powder or water free concentrate in a hermetically sealed container such as an ampoule or sachette indicating the quantity of active agent. Where the composition is to be administered by infusion, it can be dispensed with an infusion bottle containing sterile pharmaceutical grade water or saline. Where the composition is administered by injection, an ampoule of sterile water for injection or saline can be provided so that the ingredients may be mixed prior to administration.
[0087] The compounds of the invention can be formulated as neutral or salt forms. Pharmaceutically acceptable salts include those formed with anions such as those derived from hydrochloric, phosphoric, acetic, oxalic, tartaric acids, etc., and those formed with cations such as those derived from sodium, potassium, ammonium, calcium, ferric hydroxides, isopropylamine, triethylamine, 2-ethylamino ethanol, histidine, procaine, etc.
[0088] The amount of the compound of the invention that will be effective in the treatment, inhibition and/or prevention of a disease or disorder associated with increased biological barrier permeability can be determined by standard clinical techniques. The amount of the compound of the invention that will be effective in the treatment, inhibition and/or prevention of a disease or disorder associated with translocation of one or more gliadin-derived peptides across a biological barrier can be determined by standard clinical techniques. In addition, in vitro assays may optionally be employed to help identify optimal dosage ranges. The precise dose to be employed in the formulation will also depend on the route of administration, and the seriousness of the disease or disorder, and should be decided according to the judgment of the practitioner and each patient's circumstances. Effective doses may be extrapolated from dose-response curves derived from in vitro or animal model test systems.
[0089] The invention also provides a pharmaceutical pack or kit comprising one or more containers filled with one or more of the ingredients of the pharmaceutical compositions of the invention. Optionally associated with such container(s) can be a notice in the form prescribed by a governmental agency regulating the manufacture, use or sale of pharmaceuticals or biological products, which notice reflects approval by the agency of manufacture, use or sale for human administration.
Additional Active Agents
[0090] In addition to one or more compounds of the invention, compositions of the invention may further comprise one or more additional active agents, e.g., therapeutic agents, immunogenic agents and/or imaging agents.
[0091] Additional therapeutic agents that can be used in the compositions of the invention include agents that act on any organ of the body, such as heart, brain, intestine, or kidneys. Suitable additional therapeutic agents include, but are not limited to, glucose metabolism agents (e.g., insulin), antibiotics, antineoplastics, antihypertensives, antiepileptics, central nervous system agents, anti-inflammatory agents and immune system suppressants.
[0092] Additional therapeutic agents that can be used in the compositions of the invention include immunosuppressive agents. Such immunosuppressants used in the method and composition of the invention can be any agent which tends to attenuate the activity of the humoral or cellular immune systems. In particular, in one aspect the invention comprises compositions wherein the immunosuppressant is selected from the group consisting of cyclosporin A, FK506, prednisone, methylprednisolone, cyclophosphamide, thalidomide, azathioprine, and daclizumab, physalin B, physalin F, physalin G, seco-steroids purified from Physalis angulata L., 15-deoxyspergualin (DSG, 15-dos), MMF, rapamycin and its derivatives, CCI-779, FR 900520, FR 900523, NK86-1086, depsidomycin, kanglemycin-C, spergualin, prodigiosin25-c, cammunomicin, demethomycin, tetranactin, tranilast, stevastelins, myriocin, gliooxin, FR 651814, SDZ214-104, bredinin, WS9482, mycophenolic acid, mimoribine, misoprostol, OKT3, anti-IL-2 receptor antibodies, azasporine, leflunomide, mizoribine, azaspirane (SKF 105685), paclitaxel, altretamine, busulfan, chlorambucil, ifosfamide, mechlorethamine, melphalan, thiotepa, cladribine, fluorouracil, floxuridine, gemcitabine, thioguanine, pentostatin, methotrexate, 6-mercaptopurine, cytarabine, carmustine, lomustine, streptozotocin, carboplatin, cisplatin, oxaliplatin, iproplatin, tetraplatin, lobaplatin, JM216, JM335, fludarabine, aminoglutethimide, flutamide, goserelin, leuprolide, megestrol acetate, cyproterone acetate, tamoxifen, anastrozole, bicalutamide, dexamethasone, diethylstilbestrol, bleomycin, dactinomycin, daunorubicin, doxirubicin, idarubicin, mitoxantrone, losoxantrone, mitomycin-c, plicamycin, paclitaxel, docetaxel, topotecan, irinotecan, 9-amino camptothecan, 9-nitro camptothecan, GS-211, etoposide, teniposide, vinblastine, vincristine, vinorelbine, procarbazine, asparaginase, pegaspargase, octreotide, estramustine, and hydroxyurea, and combinations thereof. In one more particular aspect, the immunosuppressant is cyclosporin A.
[0093] Furthermore, the additional therapeutic agent can be selected from the group consisting of a chemotherapeutic, a gene therapy vector, a growth factor, a contrast agent, an angiogenesis factor, a radionuclide, an anti-infection agent, an anti-tumor compound, a receptor-bound agent, a hormone, a steroid, a protein, a complexing agent, a polymer, a thrombin inhibitor, an antithrombogenic agent, a tissue plasminogen activator, a thrombolytic agent, a fibrinolytic agent, a vasospasm inhibitor, a calcium channel blocker, a nitrate, a nitric oxide promoter, a vasodilator, an antihypertensive agent, an antimicrobial agent, an antibiotic, a glycoprotein IIb/IIIa inhibitor, an inhibitor of surface glycoprotein receptors, an antiplatelet agent, an antimitotic, a microtubule inhibitor, a retinoid, an antisecretory agent, an actin inhibitor, a remodeling inhibitor, an antisense nucleotide, an agent for molecular genetic intervention, an antimetabolite, an antiproliferative agent, an anti-cancer agent, a dexamethasone derivative, an anti-inflammatory steroid, a non-steroidal anti-inflammatory agent, an immunosuppressive agent, a PDGF antagonist, a growth hormone antagonist, a growth factor antibody, an anti-growth factor antibody, a growth factor antagonist, a dopamine agonist, a radiotherapeutic agent, an iodine-containing compound, a barium-containing compound, a heavy metal functioning as a radiopaque agent, a peptide, a protein, an enzyme, an extracellular matrix component, a cellular component, an angiotensin converting enzyme inhibitor, a 21-aminosteroid, a free radical scavenger, an iron chelator, an antioxidant, a sex hormone, an antipolymerase, an antiviral agent, an IgG2 Kappa antibody against Pseudomonas aeruginosa exotoxin A and reactive with A431 epidermoid carcinoma cells, monoclonal antibody against the noradrenergic enzyme dopamine beta-hydroxylase conjugated to saporin or other antibody targeted therapy agents, gene therapy agents, a prodrug, a photodynamic therapy agent, and an agent for treating benign prostatic hyperplasia (BHP), a 14 C-, 3 H-, 131 I-, 32 P- or 36 S-radiolabelled form or other radiolabelled form of any of the foregoing, and combinations thereof.
[0094] More particularly, the additional therapeutic agent can be selected from the group consisting of parathyroid hormone, heparin, human growth hormone, covalent heparin, hirudin, hirulog, argatroban, D-phenylalanyl-L-poly-L-arginyl chloromethyl ketone, urokinase, streptokinase, nitric oxide, triclopidine, aspirin, colchicine, dimethyl sulfoxide, cytochalasin, deoxyribonucleic acid, methotrexate, tamoxifen citrate, dexamethasone, dexamethasone sodium phosphate, dexamethasone acetate, cyclosporin, trapidal, angiopeptin, angiogenin, dopamine, 60 Co, 192 Ir, 32 P, 111 In, 90 Y, 99m Tc, pergolide mesylate, bromocriptine mesylate, gold, tantalum, platinum, tungsten, captopril, enalapril, ascorbic acid, α-tocopherol, superoxide dismutase, dcferoxamine, estrogen, azidothymidine (AZT), acyclovir, famciclovir, rimantadine hydrochloride, ganciclovir sodium, 5-aminolevulinic acid, meta-tetrahydroxyphenylchlorin, hexadecafluoro zinc phthalocyanine, tetramethyl hematoporphyrin, and rhodamine 123, and combinations thereof.
[0095] Compositions of the invention may comprise one or more immunogenic agents, for example, antigens. Examples of antigens that can be used in the compositions of the invention (e.g., immunogenic and/or vaccine compositions) include peptides, proteins, microorganisms (e.g., attenuated and/or recombinant microorganisms), cells (e.g., cancer cells and/or recombinant cells) and viruses (e.g., attenuated and/or recombinant viruses). Examples of peptide antigens include the B subunit of the heat-labile enterotoxin of enterotoxigenic E. coli , the B subunit of cholera toxin, capsular antigens of enteric pathogens, fimbriae or pili of enteric pathogens, HIV surface antigens, cancer antigens (e.g., cancer cells comprising antigens, isolated antigens, etc.), dust allergens, and acari allergens. Other immunogenic compounds as are known in the art can also be used.
[0096] Examples of attenuated microorganisms and viruses that can be used in the compositions of the invention (e.g., vaccine compositions) include those of enterotoxigenic Escherichia coli , enteropathogenic Escherichia coli, Vibrio cholerae, Shigella flexneri, Salmonella typhi and rotavirus (Fasano et al, In: Le Vaccinazioni in Pediatria, Eds. Vierucci et al, CSH, Milan, pages 109-121 (1991); Guandalini et al, In: Management of Digestive and Liver Disorders in Infants and Children, Elsevior, Eds. Butz et al, Amsterdam, Chapter 25 (1993); Levine et al, Sem. Ped. Infect. Dis., 5.243-250 (1994); and Kaper et al, Clin. Micrbiol. Rev., 8:48-86 (1995), each of which is incorporated by reference herein in its entirety).
[0097] Any antigen capable of inducing a protective immune response may be used in the vaccine compositions of the invention. Examples of suitable antigens include, but are not limited to, measles virus antigens, mumps virus antigens, rubella virus antigens, Corynebacterium diphtherias antigens, Bordetella pertussis antigens, Clostridium tetani antigens, Bacillus anthracis antigens, Haemophilus influenzae antigens, smallpox virus antigens, and influenza virus antigens.
[0098] Compositions of the invention may further comprise one or more protease inhibitors. Any protease inhibitor can be used, including, but not limited to, a proteinase, peptidase, endopeptidase, or exopeptidase inhibitor. A cocktail of inhibitors can also be used. Alternatively, the protease inhibitors can be selected from the group consisting of bestatin, L-trans-3-carboxyoxiran-2-carbonyl-L-leucylagmatinc, ethylenediaminetetra-acetic acid (EDTA), phenylmethylsulfonylfluoride (PMSF), aprotinin, amyloid protein precursor (APP), amyloid beta precursor protein, α1-proteinase inhibitor, collagen VI, bovine pancreatic trypsin inhibitor (BPTI), 4-(2-aminoethyl)-benzenesulfonyl fluoride (AEBSF), antipain, benzamidine, chymostatin, E-aminocaproate, N-ethylmaleimide, leupeptin, pepstatin A, phosphoramidon, and combinations thereof. Novel protease inhibitors can also be used. Indeed, protease inhibitors can be specifically designed or selected to decrease the proteolysis of the tight junction agonist and/or the therapeutic agent.
[0099] Compositions of the invention may also comprise one or more pharmaceutically acceptable excipients. Suitable excipients include, but are not limited to, buffers, buffer salts, bulking agents, salts, surface active agents, acids, bases, sugars, binders, and the like.
Methods of Treatment
[0100] Compounds and pharmaceutical compositions of the invention can be used for treating, ameliorating, and/or preventing a disease. Any disease may be treated using the compositions of the invention by selection of an appropriate active agent, e.g., therapeutic and/or immunogenic agent. In one embodiment, the present invention provides a method of treating diabetes response in a subject (e.g., a mammal such as a human) by administering a composition comprising one or more compounds of the invention together with one or more insulins and/or derivatives thereof. In another embodiment, the invention provides a method of suppressing an excessive or undesirable immune response in a subject (e.g., a mammal such as a human) by administering a composition comprising one or more compounds of the invention together with one or more immune-suppressive drugs that may include, for example, cyclosporin A.
[0101] Examples of diseases that can be treated using the compositions of the invention include, but are not limited to, cancer, autoimmune diseases, vascular disease, bacterial infections, gastritis, gastric cancer, collagenous colitis, inflammatory bowel disease, necrotizing enterocolitis, osteoporosis, systemic lupus erythematosus, food allergy, asthma, celiac disease and irritable bowel syndrome. For example, to treat inflammatory bowel disease, a composition comprising one or more compounds of the invention may be administered to the subject (e.g., a mammal such as a human) in need thereof.
[0102] In another example, to treat cancer of the colon or rectal area, a composition comprising a therapeutically effective amount of Erbitux® (Cetuximab) together with a GM-CSF and/or IL-16 inhibiting amount of one or more compounds of the invention may be administered to the subject (e.g., a mammal such as a human) in need thereof. In another example, to treat breast cancer, a composition comprising a therapeutically effective amount of Herceptin® (Trastuzumab) together with a GM-CSF and/or IL-16 inhibiting amount of one or more compounds of the invention may be administered to the subject (e.g., a mammal such as a human) in need thereof. In another example, to treat various types of cancer, a composition comprising a therapeutically effective amount of Avastin® (Bevacizumab) together with a GM-CSF and/or IL-16 inhibiting amount of one or more compounds of the invention may be administered to the subject (e.g., a mammal such as a human) in need thereof. Another example involves treatment of osteoporosis by administration of a composition comprising one or more compounds of the invention together with a therapeutically effective amount of Fosamax® (Alendronate) to the subject in need thereof. Another example involves treatment of transplant rejection by administration of a composition comprising one or compounds of the invention together with a therapeutically effective amount of Cyclosporin A to the subject in need thereof. Another example involves treatment of anemia by administration of a composition comprising one or more compounds of the invention together with a therapeutically effective amount of erythropoietin to the subject in need thereof. Another example involves treatment of hemophilia by administration of a composition comprising one or more compounds of the invention together with a therapeutically effective amount of Factor VIII to the subject in need thereof.
[0103] In some embodiments, compositions of the invention (e.g., pharmaceutical compositions) may be given repeatedly over a protracted period, i.e., may be chronically administered. Typically, compositions may be administered one or more times each day in an amount suitable to prevent, reduce the likelihood of an attack of, or reduce the severity of an attack of the underlying disease condition (e.g., diabetes, cancer, transplant rejection, etc). Such compositions may be administered chronically, for example, one or more times daily over a plurality of days.
[0104] In some embodiments, compositions of the invention (e.g., pharmaceutical compositions) may be used to treat acute attacks of the underlying disease (e.g., diabetes, cancer, transplant rejection, etc). Typically, embodiments of this type will require administration of the compositions of the invention to a subject undergoing an attack in an amount suitable to reduce the severity of the attack. One or more administrations may be used.
[0105] In some embodiments, compounds of the invention may be used in the manufacture of compositions and pharmaceutical compositions for use in the methods described above.
[0106] While the invention has been described with reference to certain particular embodiments thereof, those skilled in the art will appreciate that various modifications may be made without departing from the spirit and scope of the invention. The scope of the appended claims is not to be limited to the specific embodiments described.
Methods of Screening
[0107] Screening for inhibitors of gliadin-derived peptide translocation across biological barriers can be accomplished by a variety of techniques. Likewise, screening for inhibitors of PTG-induced factors that increase biological barrier permeability can be accomplished by a variety of techniques. Gliadin-derived peptide binding to test compounds (inhibitor candidates) can be directly measured, or inhibition of binding of gliadin-derived peptides to a cell preparation can be measured. Gliadin-derived peptides can be labeled to facilitate measurement of binding. Assays may be in cell-free systems or in cell-based systems. Any binding assay format can be used, including formats where the receptor is attached to a solid support, either directly or indirectly.
[0108] Test compounds which can be tested are any compounds. The compounds may be tested as single compounds or in combinations of compounds. The compounds may be structurally identified or of unknown structure. The compounds may be novel or previously known. The compounds may be natural products or synthetic.
[0109] According to one embodiment of the invention the test compounds are fragments of gliadin. Gliadin is a family of proteins which are produced by wheat and other grains. Examples of gliadins are gliadin alpha, gamma, and omega. Gliadins are the aqueous alcohol-soluble storage proteins in the seed. There is great heterogeneity even within a single class of gliadins. At least six, seven, eight, nine, ten, eleven, fifteen, twenty, thirty, thirty-five, fifty, or seventy-five amino acid residues may be used in fragments of gliadin as test compounds. Fragments include any molecule which is less than full length. Fragments may be, e.g., synthesized or the result of proteolytic degradation. The following tables provide the sequences of a representative number of gliadins.
[0000]
TABLE 1
Amino acid sequence of alpha-gliadin from Triticum aestivum
(NCBI accession no. CAB76964, (SEQ ID NO: 165))
1
mvrvpvpqlq pqnpsqqqpq eqvplvqqqq fpgqqqpfpp qqpypqpqpf
51
psqqpylqlq pfpqpqlpyp qpqlpypqpq lpypqpqpfr pqqpypqsqp
101
qysqpqqpis qqqqqqqqqq qqkqqqqqqq qilqqilqqq lipcrdvvlq
151
qhsiaygssq vlqqstyqlv qqlccqqlwq ipeqsrcqai hnvvhaiilh
201
qqqqqqqqqq qqplsqvsfq qpqqqypsgq gsfqpsqqnp qaqgsvqpqq
251
lpqfeeirnl aletlpamcn vyippyctia pvgifgtnyr
[0000]
TABLE 2
Amino acid sequence of alpha-gliadin precursor from
Triticum turgidum subsp. durum (NCBI accession no.
CA135909, (SEQ ID NO: 166))
1
mktflilall aivattatta vrvpvpqlqr qnpsqqqpqe qvplvqqqqf
51
lgqqqpfppq qpypqpqpfp sqqpylqlqp fpqpqlpysq pqpfrpqqpy
101
pqpqprysqp qqpisqqqqq qhqqhqqhhq eqqilqqilq qqlipcmdvv
151
lqqhniahrr sqvlqqstyq llgelccqhl wqipeqsqcq aihnvvhaii
201
phqqqkqqqq pssqfsfqqp lqqyplgqgs frpsqqnpqa qgsvqpqqlp
251
qfeeirnlal qtlpamcnvy ippyctiapf gifgtn
[0000]
TABLE 3
Amino acid sequence of alpha/beta-gliadin precursor from
Triticum aestivum (NCBI accession no. AAA34280,
(SEQ ID NO: 167))
1
mktflilvll aivattatta vrfpvpqlqp qnpsqqqpqe qvplvqqqqf
51
lgqqqpfppq qpypqpqpfp sqlpylqlqp fpqpqlpysq pqpfrpqqpy
101
pqpqpqysqp qqpisqqqqq qqqqqqqqqq qqqilqqilq qqlipcmdvv
151
lqqhniahgr sqvlqqstyq llgelccqhl wqipeqsqcq aihnvvhaii
201
lhqqqkqqqq pssqvsfqqp lqqyplgqgs frpsqqnpqa qgsvqpqqlp
251
qfeeirnlal qtlpamcnvy ippyctiapf gifgtn
[0000]
TABLE 4
Amino acid sequence of Gamma-gliadin precursor from Triticum
aestivum (NCBI accession no. P21292, (SEQ ID NO: 168))
1
mktlliltil amattiatan mqvdpsgqvq wpqqqpfpqp qqpfcqqpqr
51
tipqphqtfh hqpqqtfpqp qqtyphqpqq qfpqtqqpqq pfpqpqqtfp
101
qqpqlpfpqq pqqpfpqpqq pqqpfpqsqq pqqpfpqpqq qfpqpqqpqq
151
sfpqqqqpai qsflqqqmnp cknfllqqcn hvslvsslvs iilprsdcqv
201
mqqqccqqla qipqqlqcaa ihsvahsiim qqeqqqgvpi lrplfcalaqg
251
lgiiqpqqpa qlegirslvl ktlptmcnvy vppdcstinv pyanidagig
301
gq
[0000]
TABLE 5
Amino acid sequence of Gamma-gliadin B precursor
from Triticum aestivum (NCBI accession no.
P06659, (SEQ ID NO: 169))
1
mktlliltil amaitiatan mqadpsgqvq wpqqqpflqp hqpfsqqpqq
51
ifpqpqqtfp hqpqqqfpqp qqpqqqflqp rqpfpqqpqq pypqqpqqpf
101
pqtqqpqqpf pqskqpqqpf pqpqqpqqsf pqqqpsliqq slqqqlnpck
151
nfllqqckpv slvsslwsii 1ppsdcqvmr qqccqqlaqi pqqlqcaaih
201
svvhsiimqq eqqeqlqgvq ilvplsqqqq vgqgilvqgq giiqpqqpaq
251
levirslvlq tlptmcnvyv ppycstirap fasivasigg q
[0000]
TABLE 6
Amino acid sequence of Gamma-gliadin (Gliadin B-III) from
Triticum aestivum (NCBI accession no. P04730, (SEQ ID NO: 170))
1
pqqpfplqpq qsflwqsqqp flqqpqqpsp qpqqvvqiis patpttipsa
51
gkptsapfpq qqqqhqqlaq qqipvvqpsi lqqlnpckvf lqqqcspvam
101
pqrlarsqml qqsschvmqq qccqqlpqip qqsryqaira iiysiilqeq
151
qqvqgsiqsq qqqpqqlgqc vsqpqqqsqq qlgqqpqqqq laqgtflqph
201
qiaqlevmts ialrilptmc svnvplyrtt tsvpfgvgtg vgay
[0000]
TABLE 7
Amino acid sequence of Gamma-gliadin precursor from
Triticum aestivum (NCBI accession no. P08453, (SEQ ID NO: 171))
1
mktlliltil amaitigtan iqvdpsgqvg wlqqqlvpql qqplsqqpqq
51
tfpqpqqtfp hqpqqqvpqp qqpqqpflqp qqpfpqqpqq pfpqtqqpqq
101
pfpqqpqqpf pqtqqpqqpf pqqpqqpfpq tqqpqqpfpq lqqpqqpfpq
151
pqqqlpqpqq pqqsfpqqqr pfiqpslqqq lnpcknillq qskpaslvss
201
lwsiiwpqsd cqvmrqqccq qlaqipqqlq caaihsvvhs iimqqqqqqq
251
qqqgidiflp lsqheqvgqg slvqgqgiiq pqqpaqleai rslvlqtlps
301
mcnvyvppec simrapfasi vagiggq
[0000]
TABLE 8
Amino acid sequence of Gamma-gliadin B-I precursor from
Triticum aestivum (NCBI accession no. P04729, (SEQ ID NO: 172))
1
mktflvfali avvatsaiaq metscisgle rpwqqqplpp qqsfsqqppf
51
sqqqqqplpq qpsfsqqqpp fsqqqpilsq qppfsqqqqp vlpqqspfsq
101
qqqlvlppqq qqqqlvqqqi pivqpsvlqq lnpckvflqq qcspvampqr
151
larsqmwqqs schvmqqqcc qqlqqipeqs ryeairaiiy siilqeqqqg
201
fvqpqqqqpq qsgqgvsqsq qqsqqqlgqc sfqqpqqqlg qqpqqqqqqq
251
vlqgtflqph qiahleavts ialrtlptmc svnvplysat tsvpfgvgtg
301
vgay
[0000]
TABLE 9
Amino acid sequence of Gamma-gliadin precursor from
Triticum aestivum (NCBI accession no. P08079, (SEQ ID NO: 173))
1
mktlliltil amaitigtan mqvdpssqvg wpqqqpvpqp hqpfsqqpqq
51
tfpqpqqtfp hqpqqqfpqp qmpqqqflqp qqpfpqqpqq pypqqpqqpf
101
pqtqqpqqlf pqsqqpqqqf sqpqqqfpqp qqpqqsfpqq qppfiqpslq
151
qqvnpcknfl lqqckpvslv sslwsmiwpq sdcqvmrqqc cqqlaqipqq
201
lqcaaihtii hsiimqqeqq eqqqgmhill plyqqqqvgq gtlvqgqgii
251
q
[0000]
TABLE 10
Amino acid sequence of Alpha/beta-gliadin MM1 precursor
(Prolamin) from Triticum aestivum
(NCBI accession no. P18573, (SEQ ID NO: 174))
1
mktflilall aivattaria vrvpvpqlqp qnpsqqqpqe qvplvqqqqf
51
pgqqqpfppq qpypqpqpfp sqqpylqlqp fpqpqlpypq pqlpypqpql
101
pypqpqpfrp qqpypqsqpq ysqpqqpisq qqqqqqqqqq qkqqqqqqqq
151
ilqqilqqql ipcrdvvlqq hsiaygssqv lqqstyqlvq qlccqqlwqi
201
peqsrcqaih nvvhaiilhq qqqqqqqqqq qplsqvsfqq pqqqypsgqg
251
sfqpsqqnpq aqgsvqpqql pqfeeirnla letlpamcnv yippyctiap
301
vgifgtn
[0000]
TABLE 11
Amino acid sequence of Alpha/beta-gliadin clone
PTO-A10 (Prolamin) from Triticum aestivum
(NCBI accession no. P04728, (SEQ ID NO: 175))
1
pqpqpqysqp qqpisqqqqq qqqqqqqqqq eqqilqqilq qqlipcmdvv
51
lqqhniahgr sqvlqqstyq llqelccqhl wqipeqsqcq aihnvvhaii
101
lhqqqqkqqq qpssqfsfqq plqqyplgqg sfrpsqqnpq aqgsvqpqql
151
pqfeirnlal qtlpamcnvy ippyctiapf gifgtn
[0000]
TABLE 12
Amino acid sequence of Alpha/beta-gliadin clone PW8142
precursor (Prolamin) from Triticum aestivum
(NCBI accession no. P04727, (SEQ ID NO: 176)).
1
mktflilalv attattavrv pvpqlqpknp sqqqpqeqvp lvqqqqfpgq
51
qqqfppqqpy pqpqpfpsqq pylqlqpfpq pqpflpqlpy pqpqsfppqq
101
pypqqrpkyl qpqqpisqqq aqqqqqqqqq qqqqqqqqil qqilqqqlip
151
crdvvlqqhn iahassqvlq qstyqllqql ccqqllqipe qsrcqaihnv
201
vhaiimhqqe qqqqlqqqqq qqlqqqqqqq qqqqqpssqv sfqqpqqqyp
251
ssqgsfqpsq qnpqaqgsvq pqqlpqfaei rnlalqtlpa mcnvyipphc
301
sttiapfgif gtn
[0000]
TABLE 13
Amino acid sequence of Alpha/beta-gliadin clone PW1215
precursor (Prolamin) from Triticum aestivum
(NCBI accession no. P04726, (SEQ ID NO: 177))
1
mktflilall aivattatta vrvpvpqpqp qnpsqpqpqg qvplvqqqqf
51
pgqqqqfppq qpypqpqpfp sqqpylqlqp fpqpqpfppq lpypqpppfs
101
pqqpypqpqp qypqpqqpis qqqaqqqqqq qqqqqqqqqq qqilqqilqq
151
gliperdvvl qqhniahars qvlqqstyqp lqqlccqqlw qipeqsrcqa
201
ihnvvhaiil hqqqrqqqps sqvslqqpqq qypsgqgffq psqqnpqaqg
251
svqpqqlpqf eeirnlalqt lprmcnvyip pycsttiapf gifgtn
[0000]
TABLE 14
Amino acid sequence of Alpha/beta-gliadin A-IV
precursor (Prolamin) from Triticum aestivum
(NCBI accession no. P04724, (SEQ ID NO: 178))
1
mktflilalr aivattatia vrvpvpqlqp qnpsqqqpqk qvplvqqqqf
51
pgqqqpfppq qpypqqqpfp sqqpymqlqp fpqpqlpypq pqlpypqpqp
101
frpqqsypqp qpqysqpqqp isqqqqqqqq qqqqqqqilq qilqqqlipc
151
rdvvlqqhsi ahgssqvlqq styqlvqqfc cqqlwqipeq srcqaihnvv
201
haiilhqqqq qqqqqqqqqq qplsqvcfqq sqqqypsgqg sfqpsqqnpq
251
aqgsvqpqql pqfeeirnla letlpamcnv yippyctiap vgifgtn
[0000]
TABLE 15
Amino acid sequence of Alpha/beta-gliadin A-III
precursor (Prolamin) from Triticum aestivum
(NCBI accession no. P04723, (SEQ ID NO: 179))
1
mktflilall aivattatsa vrvpvpqlqp qnpsqqqpqe qvplmqqqqq
51
fpgqqeqfpp qqpyphqqpf psqqpypqpq pfppqlpypq tqpfppqqpy
101
pqpqpqypqp qqpisqqqaq qqqqqqqtlq qilqqqlipc rdvvlqqhni
151
ahassqvlqq ssyqqlqqlc cqqlfqipeq srcqaihnvv haiilhhhqq
201
qqqqpssqvs yqqpqeqyps gqvsfqssqq npqaqgsvqp qqlpqfqeir
251
nlalqtlpam cnvyippycs ttiapfgifg tn
[0000]
TABLE 16
Amino acid sequence of Alpha/beta-gliadin A-II
precursor (Prolamin) from Triticum aestivum
(NCBI accession no. P04722, (SEQ ID NO: 180))
1
mktfpilall aivattatta vrvpvpqlql qnpsqqqpqe qvplvqeqqf
51
qgqqqpfppq qpypqpqpfp sqqpylqlqp fpqpqlpypq pqpfrpqqpy
101
pqpqpqysqp qqpisqqqqq qqqqqqqqqq ilqqilqqql ipcrdvvlqq
151
hniahgssqv lqestyqlvq qlccqqlwqi peqsrcqaih nvvhaiilhq
201
qhhhhqqqqq qqqqqplsqv sfqqpqqqyp sgqgffqpsq qnpqaqgsfq
251
pqqlpqfeei rnlalqtlpa mcnvyippyc tiapfgifgt n
[0000]
TABLE 17 Amino acid sequence of Alpha/beta-gliadin A-I
precursor (Prolamin) from Triticum aestivum
(NCBI accession no. P04721, (SEQ ID NO: 181))
1
mktflilall aivattatta vrvpvpqlqp qnpsqqqpqe qvplvqqqqf
51
lgqqqpfppq qpypqpqpfp sqqpylqlqp flqpqlpysq pqpfrpqqpy
101
pqpqpqysqp qqpisqqqqq qqqqqqqqqq qqqqiiqqil qqqlipcmdv
151
vlqqhnivhg ksqvlqqsty qllgelccqh lwqipeqsqc qaihnvvhai
201
ilhqqqkqqq qpssqvsfqq plqqyplgqg sfrpsqqnpq aggsvqpqql
251
pqfeeirnla rk
[0000]
TABLE 18
Amino acid sequence of gamma gliadin from Triticum aestivum
(NCBI accession no. AAQ63860, (SEQ ID NO: 182))
1
mniqvdpssq vpwpqqqpfp qphqpfsqqp qqtfpqpqqt fphqpqqqfs
51
qpqqpqqqfi qpqqpfpqqp qqtypqrpqq pfpqtqqpqq pfpqsqqpqq
101
pfpqpqqqfp qpqqpqqsfp qqqpsliqqs lqqqlnpckn fllqqckpvs
151
lvsslwsmil prsdcqvmrq qccqqlaqip qqlqcaaihs ivhsiimqqe
201
qqeqrqgvqi lvplsqqqqv gqgtivqgqg iiqpqqpaql evirslvlqt
251
latmcnvyvp pycstirapf asivagiggq yr
[0000]
TABLE 19
Amino acid sequence of Omega-gliadin
from Triticum monococcum
(NCBI accession no. P02865, (SEQ ID NO: 183))
1
arqlnpsdqe lqspqqlypq qpypqqpy
[0110] Inhibitors of gliadin-derived peptide translocation across biological barriers are useful for treating diseases characterized by inflammation, including autoimmune diseases and particularly including celiac disease. Inhibitors of PTG-induced factors that increase biological barrier permeability are useful for treating diseases characterized by inflammation, including autoimmune diseases and particularly including celiac disease.
[0111] Activity of inhibitors of gliadin-derived peptide translocation and/or inhibitors of PTG-induced permeability can be measured by any means known in the art. Signaling events which can be determined include decrease in TEER, increase in LY permeability, increase in cytokine release, microglial recruitment, tyrosine kinase phosphorylation and chemotaxis, and increase in MMP-2 and MMP-9 gelatinolytic activity in cell-conditioned media.
[0112] The invention provides methods of identifying agents, compounds or lead compounds for agents active in inhibiting PTG-induced alterations in biological barrier permeability and/or peptide translocation. Generally, screening methods of the invention involve assaying for compounds which modulate the interaction of one or more gliadin fragments with one or more cells (e.g., epithelial cells, immune cells). A wide variety of assays for binding agents is provided including labeled in vitro protein-ligand binding assays, cell based assays, immunoassays, etc. A wide variety of formats may be used, including co-immunoprecipitation, 2-hybrid transactivation, fluorescent polarization, NMR, fluorescent resonance energy transfer (FRET), transcriptional activation, etc. For example, a wide variety of NMR-based methods are available to rapidly screen libraries of small compounds for binding to protein targets (Hajduk, P. J., et al. Quarterly Reviews of Biophysics, 1999. 32 (3): 211-40). In some embodiments, methods of the invention may be automated (e.g., high throughput screening) and may be used to screen chemical libraries for lead compounds. Identified compounds may be used to treat diseases involving increased biological barrier permeability including, for example, celiac disease, inflammatory bowel diseases and autoimmune diseases. Compounds identified by the methods of the invention may be further optimized to modulate biological barrier modulation, for example, may be derivatized. Multiple iterations of screening and derivatization may be employed to optimize the modulation of biological barrier permeability.
[0113] In vitro ligand binding assays employ a mixture of components including one or more gliadin-derived peptides or fragments and one or more gliadin binding components. Gliadin-derived peptides or fragments may be provided as fusion proteins (e.g., with purification tags such as 6-His). Assay mixtures typically further comprise a compound to be tested for inhibitory activity. Compounds to be tested may be of any kind known to those skilled in the art, for example, may be organic compounds, peptides, proteins, nucleic acids, lipids, carbohydrates and mixtures thereof. A variety of other reagents may also be included in the mixture including, but not limited to, salts, buffers, neutral proteins, e.g. albumin, detergents, protease inhibitors, nuclease inhibitors, antimicrobial agents, etc.
[0114] In general, assay mixtures may be incubated under conditions in which, but for the presence of the compound to be tested, gliadin-derived peptides or fragments specifically bind the gliadin binding components with a reference binding affinity. The mixture components can be added in any order that provides for the requisite bindings and incubations may be performed at any temperature which facilitates optimal binding. Incubation periods are likewise selected for optimal binding. In some embodiments, incubation periods may be minimized to facilitate rapid, high-throughput screening.
[0115] After incubation, the effect of the compound to be tested on the gliadin binding may be detected by any convenient way. For example, the gliadin-derived peptide or fragment or the gliadin binding component may be immobilized, and the other labeled; then in a solid-phase format, any of a variety of methods may be used to detect the label depending on the nature of the label and other assay components, e.g. through optical or electron density, radiative emissions, nonradiative energy transfers, etc. or indirectly detected with antibody conjugates, etc.
[0116] A difference in the binding affinity of the gliadin-derived peptide or fragment and the gliadin binding component in the absence of the compound to be tested as compared with the binding affinity in the presence of the compound to be tested indicates that the compound modulates the binding of the gliadin-derived peptide or fragment and the gliadin binding component. A difference, as used herein, is statistically significant and preferably represents at least a 50%, 60%, 70%, 80%, or 90% difference.
[0117] The above disclosure generally describes the present invention. All references disclosed herein are expressly incorporated by reference. A more complete understanding can be obtained by reference to the following specific examples which are provided herein for purposes of illustration only, and are not intended to limit the scope of the invention.
Example 1
Measurement of Trans Epithelial Electric Resistance (TEER) and Epithelial Flux of a Fluorescent Marker Lucifer Yellow
[0118] CaCo2 cells form monolayers that exhibit tight junctions between adjacent cells. Agonists of tight junctions can be identified by their ability to enhance the flux of compounds (e.g. ions, Lucifer Yellow) through a cell monolayer that comprises tight junctions; or by their ability to reduce TEER across a cell monolayer that comprises tight junctions. Treatment of CaCo2 monolayers with peptide tight junction agonist compounds leads to enhancement of Lucifer Yellow permeability through CaCo2 monolayers compared to vehicle alone. Treatment of CaCo2 monolayers with peptide tight junction agonist compounds leads to a decrease in TEER across CaCo2 monolayers compared to vehicle alone.
[0119] Tight junction agonists and agonists of the Clorf43 and CCDC78 proteins can be identified using the following method, and this method may be easily modified to identify antagonists and inhibitors of the Clorf43 and CCDC78 proteins:
[0120] Determination of TEER and Lucifer Yellow flux
[0121] Prepare Modified Hank's Balanced Salt Solution (MHBSS) by obtaining 1 L bottle of HBSS removing 10 ml of HBSS and replacing it with 10 ml HEPES buffer pH 7.0. Adjust pH to 7.4±0.1 using concentrated NaOH (10N).
[0122] Remove CaCo-2 cells from incubator, grown on 12-well, 3.0 μM, polycarbonate Transwell® filters (Corning) and record passage#, date cells seeded and age in days.
[0123] Aspirate cell culture medium from both the apical (AP) and basolateral (BL) compartments, replacing with 0.5 ml and 1.5 ml of MHBSS, respectively. Incubate cells at 37° C. for 30 minutes.
[0124] Using the MilliCell®-ERS instrument (Millipore), measure and record the transepithelial electrical resistance (TEER) across each filter and record.
[0125] Aspirate solution from the apical compartment of each filter (n=3 per condition) and replace with 0.5 ml of control and test solutions containing Lucifer Yellow and test compound If appropriate.
[0126] Place all plates into incubator set at 37° C. (±0.2), 50 RPM (±5) for a total of 180 minutes.
[0127] At t=30, 60, 120 and 180 minutes, measure and record the transepithelial electrical resistance (TEER) across each filter using the MilliCell-ERS instrument.
[0128] At t=60, 120 and 180 minutes remove 100 μl from each basolateral compartment and place it in a 96-well plate for Lucifer Yellow analysis, replace with 100 μl of MHBSS.
[0129] Make a Lucifer Yellow standard curve with the following dilutions (7500 μM, 3750 μM, 750 μM, 375 μM, 75 μM, 37.5 μM, 3.75 μM, 0.75 μM) and pipette 100 μL of each into a 96-well plate except for the first three standards mentioned above which require a 1:10 dilutions prior to transferring to the 96-well plate.
[0130] Harvest the remaining start solutions and what is left in each apical compartment into 1.5 ml vials. Freeze at −20° C. for future analysis.
[0131] Analyze each 96-well plate in a Tecan Spectra Fluor Plus using Magellan at 485 and 535 nm.
[0132] Materials:
[0133] Cells: CaCo-2 cells passage 40-60 grown on Transwell® plates for 21-28 days
[0134] Culture Medium: DMEM supplemented with 10% fetal bovine serum, 1% NEAA, 1% Penn/Strep
[0135] Buffers: Hank's Balanced Salt Solution (HBSS) without calcium and magnesium
[0136] Flasks: 100×20 mm Tissue culture dish Falcon.
[0137] Plates: 12 well polycarbonate Transwell® filters; 0.3 uM pore size
Example 2
Identification of Cytokines Upregulated on Treatment of THP-1 Cells by PT-Gliadin (PTG)
[0138] The monocytic cell line THP-1 was used to characterize the profile of cytokines whose expression was upregulated on exposure to protease treated gliadin (PTG). THP-1 cells were diluted to 5×10 5 cells/ml in RPMI medium supplemented with 10% heat inactivated fetal bovine serum.
[0139] 5×10 5 (1 ml) cells were plated in each well of a 12 well plate, and cells were incubated at 37° C. overnight. Test compounds (PTG 1 mg/ml; LPS 1 μg/ml) were added to the cultures, and incubation was continued a further 18 hours at 37° C.
[0140] Culture supernatants were harvested, and cytokines/chemokines were measured in each sample using a nitrocellulose membrane based proteomic profiler assay (R&D Systems). Assays were performed in triplicate. The cytokines screened in this assay included C5a, CD40 ligand, G-CSF, GM-CSF, GRO-α/CXCL1, I-309/CCL1, ICAM-1, IFNγ, IL-1α, IL-1β, IL-1ra, IL-2, IL-4, IL-5, IL-6, IL-8, IL-10, IL-12p70, IL-13, IL-16, IL-17, IL-17E, IL-23, IL-27, IL-32α, IP-10/CXCL10, I-TAC/CXCL11, MCP-1/CCL2, MIF, MIP-1α/CCL3, MIP-1β/CCL3, RANTES/CCL5, SDF-1/CXCL12, Serpin-E1/PAI-1, TNFα, and TREM-1.
[0141] After 6 hours of PTG exposure THP-1 cells demonstrated increased expression of the cytokines IL-8, MIP-1α, MIP-1β, TNF-α and Gro-α. After 24 hours of exposure to PTG increased expression of RANTES and MIF were also observed.
Example 3
Identification of Cytokines Upregulated on Treatment of PBMCs by PT-Gliadin (PTG)
[0142] Peripheral blood mononuclear cells were isolated from donated human blood samples using methods known in the art, and these PBMCs were used to characterize the profile of cytokines whose expression was upregulated on exposure to protease treated gliadin (PTG). PBMCs were suspended in RPMI medium supplemented with 5% heat inactivated human AB serum, and 2×10 5 cells were plated in each well of a 96 well plate. Cells were incubated at 37° C. with PTG (1 mg/ml) or LPS (1 μg/ml) in the presence or absence of test compounds being examined for the ability to suppress cytokine production. Supernatant samples were harvested following treatment, and cytokines were assayed by ELISA (R&D Systems).
[0143] Expression of IL-6, IL-8, MIP-1α, and Gro-α were induced by treatment with LPS and PTG. Expression of these cytokines was not reduced by treatment with peptide GGVLVQPG (SEQ ID NO:1).
[0144] Increased expression of GM-CSF and IL-16 was induced by exposure to LPS and PTG. This increased expression of these cytokines was inhibited by treatment with peptide GGVLVQPG (SEQ ID NO:1).
[0145] Having now fully described the present invention in some detail by way of illustration and example for purposes of clarity of understanding, it will be obvious to one of ordinary skill in the art that the same can be performed by modifying or changing the invention within a wide and equivalent range of conditions, formulations and other parameters without affecting the scope of the invention or any specific embodiment thereof, and that such modifications or changes are intended to be encompassed within the scope of the appended claims. All publications, patents and patent applications mentioned in this specification are indicative of the level of skill of those skilled in the art to which this invention pertains, and are herein incorporated by reference to the same extent as if each individual publication, patent or patent application was specifically and individually indicated to be incorporated by reference.
[0000]
TABLE 20
Peptide permeability inhibitors
SEQ
Prevented TEER
Reduced LY
ID NO:
Sequence
Reduction
Permeability
1
Gly-Gly-Val-Leu-Val-Gln-Pro-Gly
−
+
2
Ala-Gly-Val-Leu-Val-Gln-Pro-Gly
−
+
3
Gly-Ala-Val-Leu-Val-Gln-Pro-Gly
−
+
4
Gly-Gly-Ala-Leu-Val-Gln-Pro-Gly
−
+
5
Gly-Gly-Val-Ala-Val-Gln-Pro-Gly
−
+
6
Gly-Gly-Val-Leu-Ala-Gln-Pro-Gly
−
−
7
Gly-Gly-Val-Leu-Val-Ala-Pro-Gly
−
−
8
Gly-Gly-Val-Leu-Val-Gln-Ala-Gly
−
−
9
Gly-Gly-Val-Leu-Val-Gln-Pro-Ala
−
−
10
Gly-Asp-Val-Leu-Val-Gln-Pro-Gly
+
+
11
Gly-Glu-Val-Leu-Val-Gln-Pro-Gly
+
+
12
Gly-Gln-Val-Leu-Val-Gln-Pro-Gly
+
+
13
Gly-Phe-Val-Leu-Val-Gln-Pro-Gly
+
+
14
Gly-His-Val-Leu-Val-Gln-Pro-Gly
+
+
15
Gly-Arg-Val-Leu-Val-Gln-Pro-Gly
+
+
16
Gly-Lys-Val-Leu-Val-Gln-Pro-Gly
+
+
17
Gly-Ile-Val-Leu-Val-Gln-Pro-Gly
+
+
18
Gly-Trp-Val-Leu-Val-Gln-Pro-Gly
−
−
19
Gly-Pro-Val-Leu-Val-Gln-Pro-Gly
+
+
20
Gly-Val-Val-Leu-Val-Gln-Pro-Gly
+
+
21
Gly-Leu-Val-Leu-Val-Gln-Pro-Gly
+
+
22
Gly-Asn-Val-Leu-Val-Gln-Pro-Gly
+
+
23
Gly-Thr-Val-Leu-Val-Gln-Pro-Gly
+
+
24
Gly-Gly-Gly-Leu-Val-Gln-Pro-Gly
−
−
25
Gly-Gly-Leu-Leu-Val-Gln-Pro-Gly
−
−
26
Gly-Gly-Ile-Leu-Val-Gln-Pro-Gly
−
−
27
Gly-Gly-Phe-Leu-Val-Gln-Pro-Gly
+
+
28
Gly-Gly-Arg-Leu-Val-Gln-Pro-Gly
−
−
29
Gly-Gly-Asp-Leu-Val-Gln-Pro-Gly
−
−
30
Gly-Gly-Gln-Leu-Val-Gln-Pro-Gly
−
−
31
Gly-Gly-His-Leu-Val-Gln-Pro-Gly
−
−
32
Gly-Gly-Met-Leu-Val-Gln-Pro-Gly
+
+
33
Gly-Gly-Ser-Leu-Val-Gln-Pro-Gly
−
−
34
Gly-Gly-Thr-Leu-Val-Gln-Pro-Gly
+
+
35
Gly-Gly-Pro-Leu-Val-Gln-Pro-Gly
−
−
36
Gly-Gly-Val-Gly-Val-Gln-Pro-Gly
+
+
37
Gly-Gly-Val-Val-Val-Gln-Pro-Gly
−
−
38
Gly-Gly-Val-Ile-Val-Gln-Pro-Gly
−
−
39
Gly-Gly-Val-Phe-Val-Gln-Pro-Gly
−
−
40
Gly-Gly-Val-Arg-Val-Gln-Pro-Gly
−
−
41
Gly-Gly-Val-Asp-Val-Gln-Pro-Gly
−
−
42
Gly-Gly-Val-Gln-Val-Gln-Pro-Gly
−
−
43
Gly-Gly-Val-His-Val-Gln-Pro-Gly
−
−
44
Gly-Gly-Val-Met-Val-Gln-Pro-Gly
−
−
45
Gly-Gly-Val-Ser-Val-Gln-Pro-Gly
−
−
46
Gly-Gly-Val-Thr-Val-Gln-Pro-Gly
−
−
47
Gly-Gly-Val-Pro-Val-Gln-Pro-Gly
−
−
48
D-Ala-Gly-Val-Leu-Val-Gln-Pro-Gly
+
+
49
Asp-Gly-Val-Leu-Val-Gln-Pro-Gly
+
+
50
Glu-Gly-Val-Leu-Val-Gln-Pro-Gly
−
−
51
Gln-Gly-Val-Leu-Val-Gln-Pro-Gly
NT
NT
52
Phe-Gly-Val-Leu-Val-Gln-Pro-Gly
NT
NT
53
His-Gly-Val-Leu-Val-Gln-Pro-Gly
NT
NT
54
Arg-Gly-Val-Leu-Val-Gln-Pro-Gly
−
−
55
Lys-Gly-Val-Lcu-Val-Gln-Pro-Gly
+
+
56
Ile-Gly-Val-Leu-Val-Gln-Pro-Gly
−
−
57
Trp-Gly-Val-Leu-Val-Gln-Pro-Gly
−
−
58
Pro-Gly-Val-Leu-Val-Gln-Pro-Gly
+
+
59
Val-Gly-Val-Leu-Val-Gln-Pro-Gly
−
−
60
Leu-Gly-Val-Leu-Val-Gln-Pro-Gly
−
−
61
Thr-Gly-Val-Leu-Val-Gln-Pro-Gly
NT
NT
62
Asn-Gly-Val-Leu-Val-Gln-Pro-Gly
NT
NT
63
D-Phe-Gly-Val-Leu-Val-Gln-Pro-Gly
−
−
64
Cha-Gly-Val-Leu-Lav-Gln-Pro-Gly
NT
NT
65
Met(O)2-Gly-Val-Leu-Val-Gln-Pro-Gly
NT
NT
66
Gly-Val-Leu-Val-Gln-Pro-Gly
−
−
67
Val-Leu-Val-Gln-Pro-Gly
+
+
68
Leu-Val-Gln-Pro-Gly
+
+
69
Val-Gln-Pro-Gly
+
+
70
Gln-Pro-Gly
+
+
71
Gly-Gly-Val-Leu-Val-Gln-Pro
−
+
72
Gly-Gly-Val-Leu-Val-Gln
+
+
73
Gly-Gly-Val-Leu-Val
+
+
74
Gly-Gly-Val-Leu
+
+
75
Gly-Gly-Val
+
+
76
Gly-Gly-D-Val-Leu-Val-Gln-Pro-Gly
+
+
77
Gly-Gly-Val-D-Leu-Val-Gln-Pro-Gly
+
+
78
Gly-Gly-Val-Leu-D-Val-Gln-Pro-Gly
−
−
79
Gly-Gly-Val-Leu-Val-D-Gln-Pro-Gly
+
+
80
Gly-Gly-Val-Leu-Val-Gln-D-Pro-Gly
+
+
81
Gly-D-Pro-D-Gln-D-Val-D-Leu-D-Val-
+
+
Gly-Gly
82
Gly-D-Pro-D-Gln-D-Val-D-Leu-Val-Gly-
+
+
Gly
83
Gly-D-Pro-D-Gln-D-Val-Leu-D-Val-Gly-
+
+
Gly
84
Gly-D-Pro-D-Gln-Val-D-Leu-D-Val-Gly-
+
+
Gly
85
Gly-D-Pro-Gln-D-Val-D-Leu-D-Val-Gly-
+
+
Gly
86
Gly-Pro-D-Gln-D-Val-D-Leu-D-Val-Gly-
−
−
Gly
87
Gly-Pro-Gln-Val-Leu-Val-Gly-Gly
+
+
88
Gly-D-Pro-Gln-Val-Leu-Val-Gly-Gly
+
+
89
Gly-Pro-D-Gln-Val-Leu-Val-Gly-Gly
−
−
90
Gly-Pro-Gln-D-Val-Leu-Val-Gly-Gly
−
−
91
Gly-Pro-Gln-Val-D-Leu-Val-Gly-Gly
+
+
92
Gly-Pro-Gln-Val-Leu-D-Val-Gly-Gly
+
+
93
Gly-Gly-D-Val-D-Leu-D-Val-D-Gln-D-
Pro-Gly
94
Gly-Gly-D-Val-D-Leu-D-Val-D-Gln-Pro-
+
−
Gly
95
Gly-Gly-D-Val-D-Leu-D-Val-Gln-D-Pro-
−
−
Gly
96
Gly-Gly-D-Val-D-Leu-Val-D-Gln-D-Pro-
−
−
Gly
97
Gly-Gly-D-Val-Leu-D-Val-D-Gln-D-Pro-
−
−
Gly
98
Gly-Gly-Val-D-Leu-D-Val-D-Gln-D-Pro-
+
+
Gly
99
Gly-D-Phe-Val-Leu-Val-Gln-Pro-Gly
+
+
100
Ala-Pro-Gly
+
+
101
Gln-Ala-Gly
+
+
102
Gln-Pro-Ala
+
+
103
(d)Gln-Pro-Gly
+
+
104
Gln-(d)Pro-Gly
+
+
105
(d)Gln-(d)Pro-Gly
−
−
106
Gly-Pro-Gln
+
+
107
Gly-(d)Pro-Gln
−
−
108
Gly-Pro-(d)Gln
−
−
109
Gly-(d)Pro-(d)Gln
−
−
110
Ala-Pro-Gly
+
+
111
His-Pro-Gly
+
+
112
Asp-Pro-Gly
−
−
113
Arg-Pro-Gly
+
+
114
Phe-Pro-Gly
+
+
115
Gly-Pro-Gly
+
+
116
Glu-Pro-Gly
+
+
117
Lys-Pro-Gly
+
+
118
Leu-Pro-Gly
+
+
119
Met-Pro-Gly
+
+
120
Asn-Pro-Gly
+
+
121
Ser-Pro-Gly
+
+
122
Tyr-Pro-Gly
+
+
123
Thr-Pro-Gly
−
+
124
Ile-Pro-Gly
+
+
125
Trp-Pro-Gly
+
+
126
Pro-Pro-Gly
−
−
127
Val-Pro-Gly
−
+
128
Glp-Pro-Gly
+
+
129
Glp-Val-Gly
−
−
130
Glp-Gln-Gly
−
−
131
Glp-Ser-Gly
−
−
132
Glp-Lys-Gly
−
−
133
Glp-Phe-Gly
−
−
134
Glp-Glu-Gly
−
−
135
Glp-Thr-Gly
−
−
136
Glp-Ile-Gly
−
−
137
Glp-Tyr-Gly
−
−
138
Glp-His-Gly
−
−
139
Glp-Asn-Gly
−
−
140
Glp-Arg-Gly
−
−
141
Glp-Gly-Gly
−
−
142
Glp-Trp-Gly
−
−
143
Glp-Asp-Gly
−
−
144
Glp-Met-Gly
−
−
145
Glp-Leu-Gly
−
−
146
Glp-Pro-Gln
−
−
147
Glp-Pro-Asn
+
−
148
Glp-Pro-Gln
−
−
149
Glp-Pro-Ser
−
−
150
Glp-Pro-Pro
+
−
151
Glp-Pro-Trp
−
−
152
Glp-Pro-Asp
−
−
153
Glp-Pro-His
−
−
154
Glp-Pro-Leu
−
−
155
Glp-Pro-Arg
−
−
156
Glp-Pro-Val
−
−
157
Glp-Pro-Lys
−
−
158
Glp-Pro-Glu
−
−
159
Glp-Pro-Phe
−
−
160
Glp-Pro-Ile
+
−
161
Glp-Pro-Met
+
−
162
Glp-Pro-Tyr
+
−
Met(O)2 = Methioninedioxide,
Cha = cyclohexyl-Ala | Novel compounds and methods for the inhibition of biological barrier permeability and for the inhibition of peptide translocation across biological barriers are identified. Assays for determining modulators of biological barrier permeability and for peptide translocation across biological barriers are provided. Methods for treating diseases relating to aberrant biological barrier permeability and peptide translocation across biological barriers are provided. Such diseases include celiac disease, necrotizing enterocolitis, diabetes, cancer, inflammatory bowel diseases, asthma, COPD, excessive or undesirable immune response, gluten sensitivity, gluten allergy, food allergy, rheumatoid arthritis, multiple sclerosis, immune-mediated or type 1 diabetes mellitus, systemic lupus erythematosus, psoriasis, scleroderma and autoimmune thyroid diseases. | 0 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to medical needles, and more particularly to an Advanced Biopsy Needle.
[0003] 2. Description of the Related Art
[0004] Biopsy needles are commonly used to retrieve tissue, fluids, or other bodily samples for testing. Fine needle aspiration, for example, is a procedure where a needle is passed through the skin into areas of concern such as cysts, nodules, internal organs or other masses. The sample of fluids and/or cells is then aspirated through the needle into a syringe or similar collection device. The sample of cells then undergoes a cytology exam or perhaps a histology exam should tissue be collected along with the aspirated cells. Another common biopsy procedure is a core needle biopsy where a larger, hollow needle is used to remove cores of tissue from the area of concern. A core biopsy at times involves multiple insertions to ensure that adequate tissue samples are collected for a histology exam. While there are other biopsy procedures, fine needle aspiration and core needle biopsy are the most common, and at times both procedures are used on a patient.
[0005] What is therefore needed and beneficial is a biopsy needle that provides both fine needle aspiration and core biopsy with a single insertion, thus reducing trauma and pain to the patient. What is also needed is a biopsy needle that provides superior tissue retrieval and sampling with a single insertion.
[0006] It is thus an object of the present invention to provide an Advanced Biopsy Needle. While the Advanced Biopsy Needle comprises an inner and outer needle, the term Advanced Biopsy Needle refers to both needles and the novel coaxial arrangement of the inner aspiration needle and the outer core needle. These and other objects of the present invention are not to be considered comprehensive or exhaustive, but rather, exemplary of objects that may be ascertained after reading this specification with the accompanying drawings and claims.
BRIEF SUMMARY OF THE INVENTION
[0007] In accordance with the present invention, there is provided an Advanced Biopsy Needle comprising an outer needle comprising a hollow metal wire having a shaft, a sharp end, a fastening end and a cutting slot, the cutting slot comprising at least one fenestration opening having lateral walls wherein at least one lateral wall has a sharp cutting surface; an outer needle hub affixed to the fastening end of the outer needle; an inner needle comprising a hollow metal wire having a shaft, a sharp end and a fastening end; and an inner needle hub affixed to the fastening end of the inner needle; wherein the outer needle and the inner needle are arranged coaxial with each other such that the outer needle and the inner needle penetrate tissue together and wherein the inner needle can be removed from the outer needle once aspiration is performed.
[0008] The foregoing paragraph has been provided by way of introduction, and is not intended to limit the scope of the invention as described by this specification and the attached drawings and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] The invention will be described by reference to the following drawings, in which like numerals refer to like elements, and in which:
[0010] FIG. 1 depicts a perspective view of the Advanced Biopsy Needle;
[0011] FIG. 2 is an exploded view of the Advanced Biopsy Needle of FIG. 1 ;
[0012] FIG. 3 is a plan view of the Advanced Biopsy Needle;
[0013] FIG. 4 is a cross sectional view of the Advanced Biopsy Needle taken along line A-A of FIG. 3 ;
[0014] FIG. 5 is a plan view of the outer needle of the Advanced Biopsy Needle of FIG. 1 ;
[0015] FIG. 6 is a close up cross sectional view of the outer needle of FIG. 5 taken along line B-B of FIG. 5 ;
[0016] FIG. 7 is a plan view of the outer needle of the Advanced Biopsy Needle of FIG. 1 ;
[0017] FIG. 8A is a cross sectional view of the outer needle taken along line C-C of FIG. 7 ;
[0018] FIG. 8B is a cross sectional view of the outer needle taken along line C′-C′ of FIG. 7 ;
[0019] FIG. 9 is a perspective view of the Advanced Biopsy Needle without an attached syringe;
[0020] FIG. 10 is a rotated plan view of the Advanced Biopsy Needle;
[0021] FIG. 11 is a plan view of the Advanced Biopsy Needle with an attached syringe;
[0022] FIG. 12 is a rotated plan view of the Advanced Biopsy Needle with an attached syringe;
[0023] FIG. 13 is a further rotated plan view of the Advanced Biopsy Needle with an attached syringe;
[0024] FIG. 14 is a cross sectional view of the Advanced Biopsy Needle taken along line D-D of FIG. 11 ;
[0025] FIG. 15 is a plan view of a second embodiment of the outer needle of the Advanced Biopsy Needle;
[0026] FIG. 16 is a cross sectional view of the outer needle of the Advanced Biopsy Needle taken along line E-E of FIG. 15 .
[0027] FIG. 17 is a close-up plan view of the outer needle of the Advanced Biopsy Needle of FIG. 15 ;
[0028] FIG. 18 is a rotated close-up plan view of the outer needle of the Advanced Biopsy Needle of FIG. 15 ;
[0029] FIG. 19 is a further rotated close-up plan view of the outer needle of the Advanced Biopsy Needle of FIG. 15 :
[0030] FIG. 20 is a perspective view of the outer needle of the Advanced Biopsy Needle of FIG. 15 ;
[0031] FIG. 21 is a rotated perspective view of the outer needle of the Advanced Biopsy Needle of FIG. 15 ; and
[0032] FIGS. 22-26 depict the Advanced Biopsy Needle in use for fine aspiration and core biopsy.
[0033] The present invention will be described in connection with a preferred embodiment, however, it will be understood that there is no intent to limit the invention to the embodiment described. On the contrary, the intent is to cover all alternatives, modifications, and equivalents as may be included within the spirit and scope of the invention as defined by this specification, drawings and claims provided herein.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0034] The Advanced Biopsy Needle of the present invention may have various embodiments, some of which are described herein, and others of which may be inferred from or otherwise envisioned based on the disclosure contained herein.
[0035] Medical needles, including those of the present invention, are generally constructed from a hollow metal wire where a shaft is formed with a sharp end and a fastening end for placement of a fastening device that is then removably connected to a syringe or the like. Stainless steel is a commonly used material for medical needles. To manufacture a medical needle, the hollow metal wire, or cannula, is formed from a larger metal tube which is fabricated by rolling a sheet of metal into a tube and then welding the resulting seam. Laser welding is commonly used to join the tube together. Another technique to create a medical needle is where a solid piece of metal may be bored and machined, however such an approach is significantly more costly than welding a formed tube. Once the rolled and welded metal tube is created, it is heated and drawn through a series of progressively smaller dies to stretch the length of the tube while at the same time decrease the diameter of the tube until the final draw is performed typically without heat. Cold working of the tube increases the strength and hardness of the tube. At times a mandrel of similar form is placed inside the tube to prevent tube wall collapse, but usually the tolerances provided by the equipment and related manufacturing processes are such that a mandrel or form is not necessary. Once a hollow metal wire is created, it is cut to a specified length and a sharp end is created on a first end of the cut hollow metal wire by grinding, cutting a bevel, or the like. For the Advanced Biopsy Needle of the present invention, the outer needle then receives a secondary operation where cutting slots are formed in the wall of the needle by grinding, cutting, or the like. Lastly, with medical needles, a Luer fastener such as a LUER-LOCK® or a LUER-SLIP® connector is placed on the fastening end of the hollow metal wire by press fitting, friction fitting, adhesion, or the like. LUER-LOCK® and LUER-SLIP® are registered trademarks of Becton Dickinson and Company of Franklin Lakes, N.J.
[0036] The present invention and the various embodiments described and envisioned herein will be further described herein, with the drawings forming an essential part of the disclosure. The drawings were created using 3D modeling software, and portray exemplary, but not limiting, embodiments of the present invention.
[0037] The Advanced Biopsy Needle of the present invention allows for the extraction of both cells as well as tissue through a novel slotted sleeve and retractable core arrangement. The hollow slotted sleeve of the biopsy needle has at least one fenestration opening such as a slot in the sleeve, as well as a sharpened tip for insertion. The lateral walls of the slot are blade-sharp to facilitate cutting and sampling of tissue. The hollow slotted sleeve or outer needle is coaxial with a retractable core or inner needle, and both inserted in the anatomical area to be sampled. The hollow slotted sleeve or outer needle has a handle to facilitate rotation of the outer needle once inserted. A retractable core inner needle, also hollow and with a sharpened tip, is inserted within the sleeve or outer needle to prevent passageway tissue(s) from collapsing into the hollow slotted sleeve or outer needle. Once the desired target tissue is reached, the inner needle retractable core is used to aspirate cells for cytology examination and/or fluids. The inner needle retractable core is then withdrawn, while the hollow slotted sleeve outer needle is left in place for the desired tissue sample retrieval. Tissue sample is then obtained by rotation of the hollow slotted sleeve outer needle. Upon removal of the hollow slotted sleeve outer needle, the tissue sample is captured and can be extracted for subsequent testing and analysis.
[0038] Two exemplary embodiments of the Advanced Biopsy Needle are depicted by way of example and depicted with the attached figures. Both embodiments have two cutting slots with differing placement along the axis of the outer needle. In some embodiments of the present invention, one cutting slot or more than two cutting slots are employed. In describing the present invention and the various embodiments described and envisioned herein, the term axis is used. The axis of each needle is parallel with the length of the needle, in other words the axis follows the open inner passageway of the needle.
[0039] Turning now to the various figures provided, FIG. 1 depicts a perspective view of the Advanced Biopsy Needle 100 . The inner needle and outer needle are assembled in coaxial relation to each other, and the inner needle cannot be seen in FIG. 1 . The outer needle 109 can be seen with a first cutting slot 111 and a second cutting slot 113 . Each of these fenestration openings will be depicted in further detail in subsequent figures. The outer needle 109 has a shaft 119 with a sharp end or outer needle tip 115 and a fastening end 117 . The sharp end or outer needle tip 115 may be provided with a bevel or similar sharpened feature for ease of insertion into bodily tissue. The fastening end 117 receives an outer needle hub 105 that may include, in some embodiments of the present invention, a Luer fastener or the like. The outer needle hub may also include, in some embodiments of the present invention, a grip 107 such as a pair of outwardly extending wings, a lever, a knurled surface, a textured surface, a cylindrical surface, a rectangular extension, a triangular extension, a curved or non-linear surface, or the like. The outer needle hub 105 and related grip 107 may be made from a plastic such as nylon, polypropylene, or the like, and may be made by injection molding, blow molding, printing, machining, or the like. Fastened to the outer needle 109 by way of the outer needle hub 105 and related fastener is a syringe 101 that comprises a barrel (body of the syringe as indicated by 101 ) and a plunger 103 . The syringe may be made from a plastic such as, for example, polypropylene, nylon, and may be made by injection molding, blow molding, printing, machining, or the like, or may be made from other material such as glass, metal, or the like. The plunger 103 may include a sealing tip made from silicone, a rubber, or the like, in order to push or pull fluid in or out of the syringe barrel. The plunger 103 and barrel 101 (syringe) may also be made from a plastic such as, for example, polypropylene, nylon, and may be made by injection molding, blow molding, printing, machining, or the like, or may be made from other material such as glass, metal, or the like. Also shown in FIG. 1 , and depicted in more detail in FIG. 2 , is an inner needle hub 205 that is fastened to a fastening end of the inner needle (not shown in FIG. 1 , see FIG. 2 ). The inner needle hub 205 may be made from a plastic such as polypropylene or nylon, and may be made by injection molding, blow molding, printing, machining, or the like.
[0040] FIG. 2 is an exploded view of the Advanced Biopsy Needle of FIG. 1 . The inner needle 201 can be clearly seen with an inner needle tip or sharp end 203 , a shaft 209 , a fastening end 211 with an inner needle hub 205 attached thereto. A syringe hub 207 can also be seen for removable coupling of the inner needle 201 to the syringe 101 . The inner needle hub 205 may be made from a plastic such as, for example, polypropylene, nylon, and may be made by injection molding, blow molding, printing, machining, or the like, or may be made from other material such as metal, or the like. The inner needle hub 205 may also include a fastener such as a Luer fastener or the like. The inner needle hub 205 removably attaches to the syringe hub 207 . Further, in some embodiments of the present invention, the inner needle hub 205 fits at least partially within the outer needle hub 105 or further mates together. In some embodiments of the present invention, the inner needle hub 205 and the outer needle hub 105 contain mating surfaces such that each hub receives and couples with the other. Such mating surfaces may contain ridges, valleys, locking features, or the like. In one embodiment of the present invention, the inner needle tip 203 and the outer needle tip 115 are in alignment with each other when initially installed in coaxial relation one to the other. In some embodiments of the present invention, guides, tabs, slots, or other features may be employed to ensure that the inner needle tip 203 and the outer needle tip 115 stay in alignment with each other.
[0041] FIG. 3 is a plan view of the Advanced Biopsy Needle showing the outer needle 109 and an exemplary needle hub 105 that has been fitted with a grip 107 . FIG. 4 is a cross sectional view of the Advanced Biopsy Needle taken along line A-A of FIG. 3 so that the first cutting slot 111 and the second cutting slot 113 are clearly depicted. The first and second cutting slots are depicted as rectangular fenestration openings; however, other geometries such as square openings, oval openings, circular openings, and the like may also be employed. In addition, variation of needle size, fenestration to tip spacing, slot to slot spacing, direction of slots, percent of total circumference of the needle removed or remaining for each slot, and other dimensional attributes are to be considered within the scope and content of the present invention. Such changes may be made for a variety of reasons, including but not limited to, the tissue to be biopsied. FIG. 5 is a plan view of the outer needle 109 of the Advanced Biopsy Needle of FIG. 1 without an outer needle hub attached. To more clearly see an example of a first cutting slot 111 and a second cutting slot 113 , FIG. 6 is a close up cross sectional view of the outer needle of FIG. 5 taken along line B-B of FIG. 5 . Each fenestration opening has two lateral walls where at least one lateral wall has a sharp cutting surface. The lateral walls are essentially the perimeter or edge of the fenestration opening that is generally parallel to the axis of the outer needle 109 . To create a sharp cutting surface along a lateral wall, a bevel or taper is created by grinding, machining, cutting or the like. FIG. 7 is a plan view of the outer needle of the Advanced Biopsy Needle of FIG. 1 that depicts one embodiment of the fenestration openings. For a better understanding of the sharp cutting surface of each cutting slot, FIG. 8 is a cross sectional view of the outer needle taken along line C-C of FIG. 7 . Since a portion of the perimeter of the outer needle wall has been removed in order to create each fenestration opening, a lateral section 801 has been created where the wall of the outer needle does not span the entire perimeter of the outer needle, as seen in FIG. 8 . This lateral section 801 in turn has two lateral walls, each of which in one embodiment have been sharpened to create a first cutting edge lateral wall 803 and a second cutting edge lateral wall 805 . In one embodiment of the present invention, the cutting edge of each lateral wall is tapered inwardly.
[0042] FIG. 9 is a perspective view of the Advanced Biopsy Needle without an attached syringe and with only the outer needle 109 visible.
[0043] FIG. 10 is a rotated plan view of the Advanced Biopsy Needle showing the first cutting slot 111 and the second cutting slot 113 . It should be noted that the placement of the cutting slots, and the quantity thereof, may vary. A change in placement of each cutting slot along the axis of the outer needle provides for tissue sampling at varying depths of penetration, which may prove useful for various procedures.
[0044] FIG. 11 is a plan view of the Advanced Biopsy Needle with an attached syringe showing an exemplary embodiment of the visible outer needle 109 . The inner needle cannot be seen. FIG. 12 is a rotated plan view of the Advanced Biopsy Needle with an attached syringe. FIG. 13 is a further rotated plan view of the Advanced Biopsy Needle with an attached syringe. FIG. 14 is a cross sectional view of the Advanced Biopsy Needle taken along line D-D of FIG. 11 . In FIG. 14 , the inner workings of the syringe 101 can be seen including the plunger 103 and sealing end that traverses the interior of the syringe barrel in order to maintain a seal and associated pressure or suction thereof.
[0045] As previously stated, the cutting slot fenestrations may vary in shape, position, and quantity. FIGS. 15-21 provide a second example of an embodiment of the outer needle. In the example provided by FIGS. 15-21 , there are two fenestration openings opposing each other along the axis of the outer needle. FIG. 15 depicts a plan view of this second embodiment of the outer needle of the Advanced Biopsy Needle showing the second embodiment of the outer needle 1501 . The outer needle comprises a first cutting slot 1503 and a second cutting slot 1505 where the two fenestration openings of each cutting slot oppose each other along the axis of the outer needle. The outer needle tip 1507 is also depicted in this example as a bevel. This will become clear upon reviewing FIGS. 16 and 17 where FIG. 16 is a cross sectional view of the outer needle of the Advanced Biopsy Needle taken along line E-E of FIG. 15 . A first lateral section 1601 and a second lateral section 1607 can be seen in cross section where a first cutting edge 1603 and a second cutting edge 1605 are formed at the edge or along a contour or geometry of the first lateral section 1601 . In a similar manner, a third cutting edge 1609 and a fourth cutting edge 1605 are formed at the edge or along a contour or geometry of the second lateral section 1607 . These lateral sections each have two lateral walls, each of which in one embodiment have been sharpened to create the corresponding cutting edges referred to above. In one embodiment of the present invention, the cutting edge of each lateral wall is tapered inwardly.
[0046] FIG. 17 is a close-up plan view of the outer needle of the Advanced Biopsy Needle of FIG. 15 which clearly shows the second cutting slot 1505 with the first cutting slot 1503 in opposing spatial relation to the second cutting slot 1505 .
[0047] FIG. 18 is a rotated close-up plan view of the outer needle of the Advanced Biopsy Needle of FIG. 15 . FIG. 19 is a further rotated close-up plan view of the outer needle of the Advanced Biopsy Needle of FIG. 15 . FIG. 20 is a perspective view of the outer needle of the Advanced Biopsy Needle of FIG. 15 . FIG. 21 is a rotated perspective view of the outer needle of the Advanced Biopsy Needle of FIG. 15 . In one embodiment of the present invention, the angle of the outer needle tip is in alignment with an opening in a cutting slot. In other words, when viewed from the side of the outer needle (a plan view) where the bevel of the outer needle tip is oriented such that the interior of the needle can be seen, the cutting slots will also be oriented such that there is maximum visibility through the needle from one side to the other. This alignment and orientation can be clearly seen by way of FIG. 21 .
[0048] Lastly, FIGS. 22-26 sequentially depict the Advanced Biopsy Needle in use for fine aspiration and core biopsy. FIG. 22 depicts the Advanced Biopsy Needle being inserted into tissue 2203 in the direction of travel indicated by the accompanying arrow. The outer needle 2201 (any of the embodiments described or envisioned herein) can be seen being inserted in the tissue 2203 along with a (not visible) inner needle such as the inner needle 201 of FIG. 2 . In FIG. 23 the plunger 103 of the syringe 101 is withdrawn to draw (aspirate) fluid and perhaps tissue into the barrel of the syringe by way of the inner needle 201 (see FIG. 2 ) that is connected to the syringe 101 by way of inner needle hub 205 . The plunger 103 is withdrawn in accordance with the arrow that accompanies FIG. 22 . In FIG. 24 , the aspirated sample has been collected and the syringe 101 and attached inner needle 201 are withdrawn from the outer needle 2201 , leaving the outer needle 2201 remaining in the tissue. The obtained sample can then be sent for appropriate analytical tests. FIG. 25 then depicts a series of illustrations where the outer needle 2201 is rotated using the grip 107 while remaining in the tissue 2203 such that a core sample of tissue is obtained by way of the inserted and embedded cutting slots of the outer needle 2201 . Once the rotation is completed, the outer needle 2201 is withdrawn from the tissue 2203 as depicted by way of FIG. 26 and the associated directional arrow. The outer needle 2201 is then placed in a suitable sample receiving device where it can be sent for appropriate analytical tests.
[0049] It is, therefore, apparent that there has been provided, in accordance with the various objects of the present invention, an Advanced Biopsy Needle.
[0050] While the various objects of this invention have been described in conjunction with preferred embodiments thereof, it is evident that many alternatives, modifications, and variations will be apparent to those skilled in the art. Accordingly, it is intended to embrace all such alternatives, modifications and variations that fall within the spirit and broad scope of this specification, drawings, and claims provided herein. | An Advanced Biopsy Needle is disclosed that provides both fine needle aspiration and core biopsy with a single insertion, thus reducing trauma and pain to the patient. An inner needle for aspiration and an outer needle for core biopsy are in coaxial relation to each other, thus providing both histology and cytology functions with a single medical device and also with a single insertion. Lateral cutting edges along fenestration openings in the outer needle ensure that adequate tissue samples are taken. A syringe is attached to the inner needle for collection of aspirate. | 0 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 11/586,392, filed Oct. 25, 2006, which is a continuation of U.S. patent application Ser. No. 11/234,627, filed Sep. 23, 2005, which claims priority of British Patent Application No. 0421149.6, filed Sep. 23, 2004, the entirety of which are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to a process for preparing oxycodone having low levels of impurities. In particular, the process is useful for preparing oxycodone with low levels of α,β-unsaturated ketones.
BACKGROUND OF THE INVENTION
[0003] Oxycodone is a narcotic analgesic having the structure (I):
[0000]
[0004] Oxycodone can be manufactured from the natural product thebaine (II) by a well-known process as disclosed in U.S. Pat. No. 6,090,943:
[0000]
[0000] Thebaine (II) or a salt thereof is reacted with hydrogen peroxide in isopropanol, water and formic acid, producing 14-hydroxycodeinone (III). The double bond in the 14-hydroxycodeinone (III) is reduced by reaction with hydrogen in the presence of a Pd/BaSO 4 catalyst, providing oxycodone (I).
SUMMARY OF THE INVENTION
[0005] Recently there has been a concern about the presence of α,β-unsaturated ketone impurities in pharmaceutical products. 14-hydroxycodeinone (III) is an α,β-unsaturated ketone, and unsurprisingly, small quantities of this compound may be found in oxycodone (I). The present inventors have sought to provide a method for preparing oxycodone having low levels of impurities and in particular, low levels of α,β-unsaturated ketone impurities, preferably below 10 ppm.
[0006] In one aspect, the invention provides a method of purifying oxycodone or a salt thereof, including the steps of:
a) preparing a solution including the oxycodone or salt thereof in a solvent, the solution having a pH less than 6, and; b) maintaining the solution at a temperature of at least 55° C. for a period of at least 1 hour;
wherein the step of maintaining is performed in the absence of hydrogenation reagents.
[0009] In another aspect, the invention provides a method of purifying oxycodone or a salt thereof, including the steps of:
a) preparing a solution including the oxycodone or salt thereof in a solvent, the solution having a pH less than 6, and; b) maintaining the solution at a temperature of at least 55° C. for a period of at least 1 hour;
wherein the solution includes, after the maintaining step, a level of 14-hydroxycodeinone that is higher than a level of 14-hydroxycodeinone before the maintaining step.
[0012] In yet another aspect, the invention provides crystalline oxycodone hydrochloride including less than 2 ppm of 14-hydroxycodeinone.
[0013] The present invention provides a process for preparing oxycodone or an oxycodone salt, wherein the oxycodone or oxycodone salt has low levels of impurities, comprising the steps of:
a) preparing a mixture comprising oxycodone and a solvent and adjusting the pH of the mixture to less than 6; and subsequently b) exposing the mixture to hydrogenation reagents for a period of at least 1 hour.
[0016] The inventors have found that this process surprisingly provides oxycodone with low levels of α,β-unsaturated ketone impurities, i.e. 14-hydroxycodeinone at less than 15 ppm. The inventors have found that in order to achieve low levels of 14-hydroxycodeinone, the pH must be adjusted before the hydrogenation step. Suitably the mixture is heated after the pH of the mixture is adjusted, so that the process comprises the steps of:
a) preparing a mixture comprising oxycodone and a solvent, adjusting the pH of the mixture to less than 6 and heating the mixture at the temperature of at least 55° C. for a period of at least 1 hour; and subsequently b) exposing the mixture to hydrogenation reagents for a period of at least 1 hour.
This process provides oxycodone with very low levels of α,β-unsaturated ketone impurities, i.e. 14-hydroxycodeinone at less than 5 ppm.
DETAILED DESCRIPTION OF THE INVENTION
[0019] The mixture comprising oxycodone and a solvent can be prepared by a number of methods. In a first method, oxycodone base or a salt of oxycodone, prepared and isolated using any of the methods known to those skilled in the art, is mixed with a solvent to form the mixture. In a second method, 14-hydroxycodeinone is hydrogenated in a solvent using known hydrogenation reagents, thereby providing a mixture comprising oxycodone and a solvent. In a third method, a mixture comprising thebaine and a solvent is subjected to oxidation conditions (e.g. hydrogen peroxide in formic acid and water), followed by hydrogenation conditions, thereby providing a mixture comprising oxycodone and a solvent. Other methods of preparing a mixture comprising oxycodone and a solvent may be known to those skilled in the art.
[0020] The pH of the mixture is adjusted to less than 6, suitably less than 5, more suitably less than 3 and preferably about 1. The pH is suitably adjusted by the addition of a strong acid such as concentrated hydrochloric acid to the mixture. Preferably at least one equivalent of acid is added to the mixture.
[0021] The solvent in the mixture is suitably an organic solvent such as isopropanol, ethanol or SD3A (a 95:5 mixture of ethanol:methanol). Preferably the mixture further comprises water.
[0022] After the pH is adjusted, the mixture is suitably heated to a temperature of at least 55° C., preferably at least 60° C. and most preferably about 70-75° C. The temperature is suitably not higher than the boiling point of the solvent. The mixture is suitably heated for a period of at least 1 hour, preferably at least 3 hours and most preferably between 5-10 hours.
[0023] Suitable hydrogenation reagents are well known to the skilled person and typically include a hydrogenation catalyst and either hydrogen or a hydrogen transfer reagent, such as sodium hypophosphite. Preferred hydrogenation catalysts are precious metal catalysts such as palladium or platinum dispersed on a support material such as carbon or barium sulfate. In a preferred embodiment, a precious metal catalyst is added to the mixture and hydrogen is passed through the mixture at a pressure of 10 psi or more (162 kPa or more). The hydrogenation step is suitably carried out at a temperature of at least ambient, preferably at a temperature between room temperature and 70° C. The temperature should be sufficient to dissolve the solids in the mixture, thereby providing a solution. The mixture is exposed to the hydrogenation reagents for at least 1 hour, suitably at least 2 hours and preferably about 6 hours.
[0024] The product of step (b) is a mixture comprising oxycodone and a solvent. Hydrogenation catalysts may be removed by filtering the mixture. A purified oxycodone salt may be obtained from the mixture by reducing the temperature, and allowing the salt to crystallise out. For example, if hydrochloric acid was used in step (a), the hydrochloride salt of oxycodone will be produced. Alternatively, oxycodone base may be provided by adding a base such as sodium hydroxide to the mixture and allowing the mixture to cool.
[0025] If precious metal catalysts are used in the hydrogenation step, it is possible that unacceptable levels of the metals will remain in the final product (desirably the heavy metal content of the final product is less than 20 ppm). In one embodiment of the present invention, the oxycodone or oxycodone salt produced in step (b) is subjected to a further process wherein a mixture comprising the oxycodone or oxycodone salt and a solvent is treated with charcoal. Suitably the mixture is heated to a temperature of approx. 60-65° C., the charcoal is added, the mixture is stirred at 60-65° C. for 5 to 10 hours and the hot mixture is filtered to remove the charcoal. Cooling the hot mixture provides the oxycodone salt or oxycodone. Suitably the weight ratio of oxycodone or oxycodone salt to charcoal is between 20:1 and 1:1, preferably about 5:1. The charcoal is suitably a charcoal such as Darco® G-60 (Norit, USA).
[0026] Oxycodone or an oxycodone salt produced according to the process of the invention has low levels of α,β-unsaturated ketones and is advantageously incorporated into pharmaceutical products.
EXAMPLES
[0027] The following examples are illustrative but not limiting of the invention.
Preparation of Oxycodone Base: Route A
[0028] Thebaine (15.94 g) was added to a 250 ml flask. Water (18 ml) was added and the mixture was stirred at room temperature. Formic acid (42 ml) was added over 3 minutes and then the mixture was cooled in an ice bath. Hydrogen peroxide (30%, 6.7 g) was added and the mixture was stirred for 1 hour. The mixture was removed from the ice bath, allowed to warm to room temperature and then heated to 48° C. for 2 hours. The mixture was transferred to a hydrogenation bottle. A 5 wt % palladium on carbon catalyst (2 g) was added and hydrogen was passed through the mixture at approximately 20 psi for 15 hours. The catalyst was removed by passing the mixture through a pad of celite and rinsing the filtered solid with water/formic acid (3:1, 8 ml). The mixture was cooled in an ice bath and 25% sodium hydroxide (109 ml) was added dropwise over 50 minutes to increase the pH to 9-10. The mixture was stirred for 1 hour and 15 minutes and the solid product was filtered, rinsed with cold water and dried under vacuum pump for 3 hours. The product was oxycodone base (14.152 g, 87.7% yield) and contained 178 ppm of the α,β-unsaturated ketone impurity, 14-hydroxycodeinone.
Preparation of Oxycodone Base: Route B
[0029] Thebaine (100.0 g dry weight) was dissolved in 85% formic acid (252.3 g). 30% Hydrogen peroxide (43.6 g) was added over a period of about two hours. The mixture was stirred for three hours. Ammonium hydroxide solution was added to the mixture to increase the pH to 8-9. The solid precipitate was filtered and washed with water and ethanol. The solid was dried on the filter and in an oven. The product was 14-hydroxycodeinone (150.52 g damp, 75.32 g dry weight, 75% yield).
[0030] The 14-hydroxycodeinone (39.45 g of the damp solid) was dissolved in water (81.13 ml) and 80% acetic acid (16.17 ml). 10 wt % palladium on carbon catalyst (0.33 g wet weight, 0.16 g dry weight) was added and hydrogen was passed through the mixture for about 6 hours at about 12 psi. The mixture was filtered to remove the catalyst. An ammonium hydroxide solution was added to the mixture up to pH 9. The solid precipitate was washed with water and with ethanol, and was dried. The product was oxycodone (18.8 g, 79% yield).
Comparative Example 1
Heating and Recrystallisation of Oxycodone
[0031] 13.257 g of oxycodone prepared via Route A was added to a 250 ml flask. An ethanol/methanol mixture (70 ml) was added to the flask and the mixture was stirred at room temperature, heated to reflux (78° C.) for 1 hour, cooled to room temperature and then stirred at room temperature. The mixture was cooled in an ice bath for 30 minutes and the solid product was filtered and rinsed with an ethanol/methanol mixture. The solid was dried under vacuum for 3 hours. The product was oxycodone base (11.393 g, 85.95%) and contained 210 ppm of the α,β-unsaturated ketone impurity, 14-hydroxycodeinone.
[0032] Dissolving the oxycodone, heating to 78° C. for 1 hour and recrystallising did not reduce the amount of 14-hydroxycodeinone in the oxycodone.
Comparative Example 2
Heating and Recrystallisation of Oxycodone
[0033] 11 g of the oxycodone product from comparative example 1 was added to a 250 ml flask. An ethanol/methanol mixture (55 ml) was added to the flask and the mixture was stirred at room temperature, heated to reflux (78° C.) for 1 hour, cooled to room temperature and then stirred at room temperature. The mixture was cooled in an ice bath for 35 minutes and the solid product was filtered and rinsed with an ethanol/methanol mixture. The solid was dried under vacuum overnight. The product was oxycodone base (10.682 g, 97.1%) and contained 165 ppm of the α,β-unsaturated ketone impurity, 14-hydroxycodeinone.
[0034] A second step of dissolving the oxycodone, heating to 78° C. for 1 hour and recrystallising did not significantly reduce the amount of 14-hydroxycodeinone in the oxycodone.
Example 1
Preparation of Oxycodone Hydrochloride Having Low Level of Impurities
[0035] 5 g of oxycodone product from comparative example 2 was added to a 100 ml flask. Water (10 ml) and isopropanol (10 ml) were added and the mixture was stirred. Concentrated hydrochloric acid (2.64 ml) was added. The mixture was heated to 75° C. for 10 hours and stirred at ambient temperature overnight. The mixture was transferred to a hydrogenation bottle and was heated to 45° C. 5 wt % palladium on carbon catalyst (0.5 g) was added to the mixture and hydrogen was passed through the mixture at about 12 psi for 6.5 hours. The mixture was warmed to 55° C., passed through a filter paper, cooled to room temperature and then placed in an ice bath for 30 minutes. The solid product was filtered, rinsed with cold isopropanol and dried overnight under a vacuum pump. The product was oxycodone hydrochloride (5.533 g, 99.2%) and contained less than 2 ppm 14-hydroxycodeinone (measured by HPLC and MS-SIM (mass spectrometry with selected ion monitoring)).
Example 2a
Preparation of Oxycodone Base Having Low Level of Impurities
[0036] 1.2 g of crude oxycodone prepared via Route A was added to a 50 ml flask. Water (3.6 ml), isopropanol (3.6 ml) and formic acid (4.8 ml) were added. Concentrated hydrochloric acid (0.24 ml) was added. The mixture was heated to 75° C. and stirred at 75° C. for 10 hours. The mixture was cooled to room temperature and stirred. HPLC showed that the level of 14-hydroxycodeinone in the oxycodone increased during the heating step. Treatment with acid and heating does not prepare oxycodone with a low level of impurities.
[0037] The mixture was transferred to a hydrogenation bottle. 5 wt % palladium on carbon catalyst (120 mg) was added to the mixture and hydrogen was passed through the mixture at room temperature and about 12 psi for 24 hours. The mixture was passed through a pad of celite and then placed in an ice bath. 50% sodium hydroxide (5.3 ml) was added dropwise over 17 minutes to a pH of 9-10. The mixture was stirred at 0-5° C. for 1 hour and 10 minutes. The solid product was filtered, rinsed with cold water and dried under a vacuum pump for four hours. The product was oxycodone base (1.072 g, 89.33%) and contained approximately 3 ppm 14-hydroxycodeinone (measured by MS-SIM).
Example 2b
Preparation of Oxycodone Hydrochloride Having Low Level of Impurities
[0038] 0.8 g of oxycodone base produced in Example 2a was added to a 50 ml flask. Water (1.6 ml) and isopropanol (3.76 ml) were added. Concentrated hydrochloric acid (0.32 ml) was added and the mixture was heated to 73° C. After 5 minutes at 73° C. the mixture was cooled to room temperature and was then stirred at room temperature for 1 hour. The mixture was placed in an ice bath and stirred for 1.5 hours. The solid product was filtered, rinsed with cold isopropanol and dried under a vacuum pump overnight. The product was oxycodone hydrochloride (0.892 g) and contained approximately 5 ppm 14-hydroxycodeinone (measured by MS-SIM).
Example 3
Preparation of Oxycodone Hydrochloride Having Low Level of Impurities
[0039] 18.8 g oxycodone prepared via Route B was added to a flask containing ethanol (43.9 ml) and water (10.14 ml). Ethanol (5.71 ml) and concentrated hydrochloric acid (7.37 ml) were mixed and then added to the flask, providing a mixture with a pH of 1. The mixture was heated at 75° C. for 5 hours and was then cooled to 65° C. The mixture was hydrogenated at 10-12 psi for six hours using a 10 wt % palladium on carbon catalyst (175.6 mg wet weight, 88 mg dry weight). The mixture was filtered to remove the catalyst and cooled. The solid product was filtered and washed with ethanol. The product was oxycodone hydrochloride (20.13 g, 75.3%) and contained approximately 0 ppm 14-hydroxycodeinone.
Comparative Example 3a
Hydrogenation of Oxycodone
[0040] 3 g of crude oxycodone prepared by essentially the same method as route A and containing 535 ppm 14-hydroxycodeinone was added to a hydrogenation bottle. Isopropanol (9 ml), water (9 ml) and formic acid (12 ml) were added. The mixture was hydrogenated for 23 hours using a 5 wt % palladium on carbon catalyst (0.3 g). The mixture was passed through a pad of celite and the hydrogenation bottle was rinsed with isopropanol and water. The mixture was cooled in an ice bath. 50% sodium hydroxide (14 ml) was added dropwise over 22 minutes to a pH of 9-10. The mixture was stirred at 0-5° C. for 1 hour and 20 minutes. The solid product was filtered, rinsed with cold water and dried under a vacuum pump overnight. The product was oxycodone base (2.822 g, 94.1%) and contained approximately 26 ppm 14-hydroxycodeinone (measured by HPLC). The hydrogenation step reduced the amount of 14-hydroxycodeinone in the oxycodone, but this method, wherein the pH of the mixture was not adjusted before the hydrogenation, did not afford oxycodone with an impurity level of less than 10 ppm.
Comparative Example 3b
Acidification of Oxycodone
[0041] 2 g of oxycodone base produced in Comparative Example 3a was added to a 100 ml flask. Water (4 ml) and isopropanol (9.4 ml) were added. Concentrated hydrochloric acid (0.8 ml) was added and the mixture was heated to 70-72° C. After 5 minutes at 70-72° C. the mixture was slowly cooled to room temperature. The mixture was placed in an ice bath and stirred for 1 hour and 20 minutes. The solid product was filtered, rinsed with cold isopropanol and dried under a vacuum pump overnight. The product was oxycodone hydrochloride (2.401 g) and contained approximately 38 ppm 14-hydroxycodeinone (measured by HPLC). Adjusting the pH of the oxycodone to ˜1 and heating did not further reduce the concentration of 14-hydroxycodone. Comparative Examples 3a and 3b demonstrate that oxycodone with very low level of impurities (less than 10 ppm 14-hydroxycodeinone) is not prepared by hydrogenating the oxycodone and then treating with acid.
Example 4
Preparation of Oxycodone Hydrochloride Having Low Level of Impurities
[0042] 4.35 g oxycodone prepared by essentially the same method as Route B was added to a flask containing ethanol (12.5 ml) and water (2.7 ml). Concentrated hydrochloric acid (approximately 1.5 ml) was added to the flask, providing a mixture with a pH of about 2. The pH of the mixture was increased to 5 by adding ammonia. The mixture was hydrogenated at 45 psi and 50° C. for 1.5 hours and then at 10-12 psi and 50-55° C. for 4 hours using a 10 wt % palladium on carbon catalyst (0.06 g). The mixture was filtered to remove the catalyst and cooled. The solid product was filtered and washed with ethanol. The product was oxycodone hydrochloride (3.706 g, 76.1%) and contained approximately 12 ppm 14-hydroxycodeinone.
Example 5
Preparation of Oxycodone Hydrochloride Having Low Level of Impurities
[0043] 3 g of oxycodone product from comparative example 2 was added to a 50 ml flask. Water (1.3 ml) and ethanol (5.58 ml) were added and the mixture was stirred. Concentrated hydrochloric acid (1.58 ml) was added. Further water was added so that in total 4.5 ml of water was added. The mixture was heated to 75° C. for 10 hours, slowly cooled to room temperature and stirred overnight. The mixture was heated to 40° C. and transferred to a hydrogenation bottle. 5 wt % palladium on carbon catalyst (0.3 g) was added to the mixture and hydrogen was passed through the mixture at between 11 and 12 psi for 6.5 hours. The mixture was warmed to 56° C. and passed through two layers of filter paper. The bottle and filtrate were rinsed with a hot solution of 1 ml water and 5 ml ethanol, and with 20 ml of hot ethanol. The filtrate was slowly cooled to room temperature and then placed in an ice bath for 30 minutes. The solid product was filtered, rinsed with cold ethanol and dried overnight under a vacuum pump. The product was oxycodone hydrochloride (2.663 g, 79.6% yield). A further 0.334 g of oxycodone hydrochloride was obtained by washing the filter cake and hydrogenation bottle with water and water/ethanol (1:1), giving a combined yield of 2.997 g and 89.5%. Both samples of oxycodone hydrochloride contained 0 ppm 14-hydroxycodeinone (measured by HPLC and MS-SIM (mass spectrometry with selected ion monitoring)). | A method of purifying oxycodone or a salt thereof includes the steps of:
a) preparing a solution including the oxycodone or salt thereof in a solvent, the solution having a pH less than 6, and; b) maintaining the solution at a temperature of at least 55° C. for a period of at least 1 hour; wherein the step of maintaining is performed in the absence of hydrogenation reagents. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an electric discharge machine, and more particularly to a method and apparatus for controlling an electric discharge machine in which the ratio of occurrence of abnormal electric discharge occurring from the interpolar insulation malfunction is detected. The optimum value for the interpolar status during the interruption of the electric discharge is automatically adjusted corresponding to the interpolar condition, while a plurality of combinations of the electrical processing conditions by the input of process characteristics, such as process velocity and degree of roughness of the finishing surface, such as the maximum value of the electric discharge current and the time of interruption of the electric discharge, corresponding to those process characteristics are displayed, in order, on a display apparatus.
2. Description of the Related Art
It is well known that in order to be able to increase the efficiency of the electric discharge process the time of interruption of electric discharge may be reduced. However, if this interruption time is reduced excessively, a fine powder of processed metal and so on removed in the melted form is not adequately discharged from the working gap. Then the insulating conditions of the working gap do not adequately recover before a pulse voltage is applied. Abnormal discharge, such as arcing, is produced, so that the accuracy and efficiency of the machining of the workpiece is reduced. Accordingly, the time of interruption of electric discharge must be suitably controlled to match the interpolar insulation conditions.
However, the speed of restoration of these insulation conditions is not uniform, but is, for example, effected by the flow conditions of the dielectric fluid and the electric discharge time, etc. Accordingly, it is difficult for the operator to set the time of interruption of the electric discharge to match the conditions existing each time this occurs.
In addition, it is necessary to set the processing conditions, such as appropriate electrodes, polarity, maximum value of electric discharge current, time of interruption of electric discharge, etc., according to the processing characteristics, such as the material of the workpiece, the roughness of the finished surface, process speed, etc. Because there are a great number of combinations of these processing conditions, it becomes an extremely complex and difficult problem for the operator to set these conditions individually.
Accordingly, with conventional equipment, the method is used by which many matched process characteristics and process characteristics and process conditions are stored in the memory of the control equipment, and the operator selects the appropriate conditions to conform to the desired process characteristics from among the matching conditions displayed on the display equipment, and sets these conditions, in the control device. In such a method, a plurality of process conditions are generally required to satisfy a single process characteristic. For example, in the case where among the process characteristics, only the finished surface roughness is important, and other characteristics are not looked upon as being particularly important, the number or freedom of process conditions which can be selected becomes fairly large. In other words, the smaller the number of required process characteristics is, the more the freedom of the process conditions. Accordingly, it is not desirable to set process characteristics and process conditions one against one when the freedom of process characteristics is large because the operator's selection is unduly limited.
SUMMARY OF THE INVENTION
A first object of the present invention is to provide a method and apparatus for optimum control of the time of interruption of the electric discharge, based on a comparison of a previously set allowable ratio and the detected ratio of abnormal discharge occurrence.
In order to achieve this object, in the present invention, when the time of interruption of the electric discharge is excessive and when the interpolar voltage exceeds a standard voltage, a pulse voltage is applied over the working gap, and when the rate of abnormal discharge occurrence becomes greater than an allowable rate, the standard voltage is increased, and the time of interruption of the electric discharge is lengthened. When the rate of abnormal electric discharge occurrence is less than the allowable rate, the standard voltage is lowered and the time of interruption of the electric discharge is reduced. All the necessary circuits for implementing this method are provided.
A second object of the present invention is to provide a method by which the processing conditions are automatically set by inputting the process characteristics into the control device, and by which it is possible for the operator to make selections and settings when there is a plurality of a group of corresponding process conditions.
In order to achieve this object in the present invention, a plurality of groups of a matched plurality of processing characteristics corresponding to a plurality of processing conditions, and a plurality of process characteristics which are classified into ranges of process characteristics, are stored in the memory of a control device. The combined processing conditions and characteristics are retrieved by specifying process characteristics based on the above-mentioned classification. In addition, combinations which satisfy the input process characteristics are displayed in order, and the displayed combinations are set as operating conditions.
Other and further objects and advantages of the present invention will be apparent from the following description and accompanying drawings which, by way of illustration, show a preferred embodiment of the present invention and the principle thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view showing, an electric discharge machine which is an embodiment of the present invention.
FIG. 2 is a block diagram showing a first embodiment of the present invention.
FIG. 3 is a block diagram showing the configuration of the control circuit shown in FIG. 2.
FIG. 4 is a block diagram showing the configuration of the abnormal discharge circuit shown in FIG. 2.
FIG. 5 is a block diagram showing the configuration of the circuit shown in FIG. 2.
FIG. 6 is a timing chart for auxiliary equipment of the first embodiment of the present invention.
FIG. 7 is a block diagram showing a second embodiment of the present invention.
FIG. 8 is an explanatory drawing showing an example of memory.
FIG. 9 is an explanatory drawing of the input section shown in FIG. 7.
FIG. 10 is an explanatory drawing showing an example of the input data.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Now referring to FIG. 1, an electric discharge machine 1 comprises a box-shaped base 3, an XY cross table device 5 installed on the base 3, and a processing head 9 installed so that it is able to travel vertically on a hollow column 7 vertically erected on the upper surface of the back section of the base 3. The XY cross table device 5 comprises a Y-axis table 13 which freely moves along the Y-axis direction guided on a guide table 11 installed on the upper surface of the base 3, and an X-axis table 15 installed so that it freely moves along the X-axis on the Y-axis table 13. The Y-axis table 13 is constructed so that it moves along the Y-axis by means of a Y-axis servomotor 17 installed on the guide table 11. The X-axis table 15 is constructed so that it moves along the X-axis by means of an X-axis servomotor 19 installed on the Y-axis table 13. Mounted on the X-axis table 13 is a process tank 21 within which a work table 23 for supporting a workpiece W is installed.
The process head 9 is constructed so that it moves vertically by means of a servomotor 25 mounted on the upper section of the column 7. A tool electrode 27 for carrying out the electric discharge machining process on the workpiece W is mounted in a freely movable and removably exchangeable manner on the process head 9.
By means of the construction described above, the tool electrode 27 and the workpiece W can be brought into proximity, and by applying a pulse voltage to the working gap between the electrode 27 and the workpiece W, an electric discharge is produced so that electric discharge machining can be carried out on the workpiece W.
Now referring to FIG. 2, a minute working gap 29 is maintained between the process electrode 27 and the workpiece W. A processing power source 31, a resistance 33, and a switching element, such as a transistor 35, are connected in series to the electrode 27 and the workpiece W.
In the connection circuit for the resistance 33 and the transistor 35, a resistance 37, for the normal flow of a minute electric current of a degree that does not produce an electric discharge in the working gap 29, is connected in parallel. Furthermore, a detection resistance 39, for detecting the voltage across the working gap 29, is connected in parallel with the working gap 29. The voltage output of the detection resistance 39 is split at a suitable position to apply the divided voltage to both the input section (a) of a comparison control circuit 41 for controlling the ON-OFF status of the transistor 35 and the input section (b) of an abnormal discharge detection circuit 43.
The comparison control circuit 41, as will be later described, compares an interpolar voltage V G , suitably split off from the resistance 39, and a first standard voltage V1. The ON-OFF configuration of the transistor 35 is controlled based on the result of that calculation.
The voltages at both ends of the resistance 33 are input to the comparison control circuit 41, and an output section (e) of this circuit is connected to the transistor 35. An output section of a D/A converter 45 is connected to an input section (f) of the comparison control circuit 41.
The abnormal discharge detector circuit 43, as will be later described, is constructed to output a pulse signal for each abnormal electric discharge detected, and has an output section (g) connected to an input section (h) of a logical operation circuit 47.
The logical operation circuit 47, as will be later described, counts the pulse signals received from the abnormal discharge detection circuit 43 and compares the total count within a prescribed time to a set allowable value. Based on the results of this calculation, the logical operation circuit 43 outputs an instruction signal to the D/A converter 45.
The D/A converter 45 outputs an analogue signal, based on the instruction signal from the logical operation circuit 43, to the input section (f) of the comparison control circuit 41.
The comparative control circuit 41, as shown in FIG. 3, comprises such components as a first reference voltage setting circuit 49, a comparator circuit 51, a first AND gate 53, a first RS flip-flop 55, an inverter 57, an insulation breakdown detection circuit 59, a first monostable multivibrator 61, and a second monostable multivibrator 63.
Specifically, the first standard voltage setting circuit 49 is used for setting the first reference voltage slightly higher than the electric discharge voltage in the working gap 29. The first reference voltage V1 is set by means of an analogue signal output from the D/A converter 45. The first reference voltage V1, set by means of the first reference voltage setting circuit 49, is input to one section of the comparator circuit 51.
The comparator circuit 51 compares the first reference voltage V1 with the interpolar voltage V G which is input to the input section (a). When V G is greater than V1, a high level signal (H) is output to one section of the first AND gate 53. When V G is less than V1, a low level signal (L) is output to one section of the first AND gate 53.
The insulation breakdown detection circuit 59 detects any breakdown in the interpolar insulation. By means of the ON action of the transistor 35, it detects the rise of the flow of the interpolar current at the resistance 33 as a change in voltage. When the rise of the interpolar current is detected by the circuit 59, it acts as a trigger signal and is input to the first monostable multivibrator 61.
The first monostable multivibrator 61 is activated almost simultaneously with the electric discharge in the working gap 29, and its output is input to the second monostable multivibrator 63.
The second monostable multivibrator 63 uses the pulse signal of the first monostable multivibrator 61 at the fall from the high level to the low level as a trigger, so that it can output a high level pulse. The output section of the second monostable multivibrator 63 is connected to the reset of the first RS flip-flop 55, and is, also connected to the other input section of the AND gate 53 through the inverter 57.
The AND gate 53 takes the logical product of the input signal from the comparator circuit 51 and the output signal from the second monostable multivibrator 63 inverted through the inverter 57, and when both input signals are high level, it outputs a high level signal. The output section of the AND gate 53 is connected to the set terminal S of the first RS flip-flop 55.
The first RS flip-flop 55 is set by the high level signal output from the AND gate 53 and reset by the high level signal output from the second monostable multivibrator 63. The output terminal Q of the first RS flip-flop 55 is connected to the base of the transistor 35 through the output section (e). The first RS flip-flop 55 when set, outputs a high level signal from the output terminal Q; and when reset, outputs a low level signal. Accordingly, the ON-OFF status of the transistor 35 is controlled by the first RS flip-flop 55.
Now referring to FIG. 4, the abnormal discharge detection circuit 43 comprises a second basic voltage setting circuit 65, a second comparator circuit 67, a second RS flip-flop 69, and a second AND gate 71.
Specifically, the second reference voltage setting circuit 65 sets the second basic voltage V2 to a value which is higher than the first reference voltage V1 and slightly lower than the ignition voltage of the working gap 29. Its output section is connected to one of the input sections of the second comparator circuit 67. The first reference voltage V1 and the second reference voltage V2 set the reference value of the impedance of the working gap 29 by the respective interpolar voltages. The first reference voltage V1 is a variable, while the second reference voltage V2 is a fixed value.
The second comparator circuit 67 compares the second reference voltage V2, which is set by the second reference voltage setting circuit 65, with the interpolar voltage V G which is applied to the other input section (b). The second comparator circuit 67 outputs a high level signal H to the set terminal S of the second RS flip-flop 69 when V G is greater than V2, and a low level signal when V G is less than V2.
The second RS flip-flop 69 is set by the input of the high level signal output from the second comparator circuit 67 to the set terminal S. It is reset by the input of the process pulse, and a signal synchronized with the off time width (Toff) of the process pulse to the reset terminal R for resetting. When this second RS flip-flop 69 is set by the high level signal from the second comparator 67, the low level signal converted from the output terminal Q is output to one of the input sections of the second AND gate 71.
The second AND gate 71 obtains the logical product of the input signal provided from the output terminal Q of the second RS flip-flop 69, and the sampling pulse Ts, generated either directly after insulation breakdown of the working gap 29 or during ontime continuation of the process pulse after the insulation breakdown. Accordingly, the second AND gate 71 only outputs a high level signal when the signal input to it from the second RS flip-flop 69 reaches the high level resulting from the input of the sampling pulse Ts. The output section (g) of the second AND gate 71 is connected to the logical operation circuit 47. When the high level signal is output from the second AND gate 71, the electric discharge has commenced before the interpolar voltage V G reaches the value of the second reference voltage V2. This means that abnormal discharge has occurred.
The logical operation circuit 47, as shown in FIG. 5, comprises a programmable counter 73, a CPU 75, and an output circuit 77.
Specifically, the programmable counter 73 comprises a counter (A) and a counter (B). Its output section is connected to the input section of the CPU 75. The counter (A) counts the pulse signal input from the AND gate 71 of the abnormal discharge detection circuit 43 through the input section (h). Counter (B) counts the clock pulses, and when a prescribed time has passed, outputs an interrupt request signal to the CPU 75.
On receiving the interrupt request from the counter (B) of the programmable counter 73, the CPU 75 accepts the total count (D) from the counter (A), calls up a pair of abnormal discharge generation normal values N1 and N2 (where N1 is greater than N2), which have been previously set as allowable values, and carries out a comparison operation. The CPU 75 is connected to the input section of the output circuit 77 so as to output an instruction signal to the output circuit 77, such that when the result of the comparison of the total count (D) with the reference values N1 and N2 shows that D is greater than N1, the first reference voltage V1 is raised one stage, and when D is less than N2, the first reference voltage V1 is lowered one stage. When the relationship N1>D>N2 exists, no instruction signal is output and the existing conditions are maintained.
The output circuit 77 receives the instruction signal from the CPU 75 and transmits it to the D/A converter 45. The D/A converter 45 is connected to the first reference voltage setting circuit 49 so as to output an analogue signal based on the instruction signal from the CPU 75 to change the set value of the first reference voltage setting circuit 49.
In a configuration such as outlined above, when a voltage is applied by the process current 31 through the resistance 37 to the working gap 29, a voltage proportional to the impedance of the working gap 29 is generated on the resistance 39. This voltage is divided at one of the input terminals of the comparator circuit 51 of the comparison control circuit 41 and is provided as the interpolar voltage V G . The comparator circuit 51 compares the first reference voltage V1 obtained from the first reference voltage setting circuit 49 with the interpolar voltage V G . When V G is found to be greater than V1, a high level signal is input to one of the input terminals of the first AND gate 53.
Then an electric discharge is not being produced in the working gap 29 between the tool electrode 27 and the workpiece W, and the insulation breakdown detection circuit 59 is not activated, the signal output from the second monostable multivibrator 63 is a low level signal so that a high level signal inverted by the inverter 57 is provided to the other part of the input terminal of the AND gate 53. Accordingly, when a high level signal is output by the comparator circuit 51, the AND gate 53 obtains the logical product of both high level signals and outputs a high level signal to the set terminal S of the first RS flip-flop 55. The first RS flip-flop 55 is set by means of this signal, and a high level signal is output to the base of the transistor 35 from the output terminal Q. The transistor 35 then is in the ON status.
With the transistor 35 in the ON status, as described above, when the working gap 29 is suitably narrowed, a discharge is produced in the working gap 29, and the voltage in the working gap 29 suddenly drops, as shown in the upper stage of FIG. 6. In addition, at the same time as the discharge is produced, a voltage drop is produced at both ends of the resistance 33 by the current flowing through the resistance 33. Accordingly, the insulation breakdown detection circuit 59 detects the voltage produced at both ends of the resistance 33, and triggers the first monostable multivibrator 61. The first monostable multivibrator 61 receives the trigger signal and outputs a pulse signal of the ON time width (Ton in FIG. 6) of a previously set process pulse. This pulse signal is output to the second monostable multivibrator 63. Simultaneously with the fall of this pulse signal, the second monostable multivibrator 63 is triggered, and a pulse signal is output with the OFF time width (Toff in FIG. 6) of a previously set process pulse.
When the pulse signal output by the second monostable multivibrator 63 is provided to the reset terminal R of the first RS flip-flop 55, it resets the first RS flip-flop 55. Accordingly, the output from the output terminal Q is a low level signal, putting the transistor 35 into the OFF status. In addition, the pulse signal from the second monostable multivibrator 63 is inverted in the invertor 57, and a low level signal is provided to one of the input terminals of the first AND gate 53. For this reason, the reset of the first RS flip-flop 55 is prevented by a high level signal output from the comparator circuit 51 during the OFF-time width (Toff) of the process pulses. From the above sequence of events, the ON time (discharge time) is determined by the first monostable multivibrator 61, and the OFF-time (discharge interruption time) is determined by the second monostable multivibrator 63.
When the transistor 35 is OFF, corresponding to discharge interruption time, the impedance of the working gap 29 enters a restoration period, and eventually is restored. The impedance of the working gap 29 is detected as the interpolar voltage V G of the detection resistance 39, and is input to the comparator circuit 51. By the restoration of the impedance, when V G becomes greater than V1, the output from the first monostable multivibrator 61 is low in level, so that the first RS flip-flop 55 is reset through the AND gate 53, and the previously outlined actions are repeated.
In the abnormal electric discharge detection circuit 43, by taking the logical product of the result of comparing the second reference voltage V2 with the interpolar voltage V G , and the sampling pulse Ts produced after the breakdown of the insulation, a pulse signal is output to the logical operation circuit 47 each time an abnormal discharge is detected due to the malfunction of the interpolar insulation recovery.
This pulse signal is input to the programmable counter 73 of the logical operation circuit 47 and counted by the counter (A). The count (D) made by the counter (A) is input to the CPU 75 at the every count-up of the counter (B). The CPU 75 compares the count (D) with the suitable set values N1 and N2. When D is greater than N1, the conclusion is made that there are many abnormal discharges, so that an instruction signal is output to the D/A inverter 45 through the output circuit 77 to increase the first reference voltage V1. When D is less than N2, an instruction signal is output to the D/A inverter 45 through the output circuit 77 to reduce the first reference voltage V1. The D/A converter 45 outputs an analogue signal V1 to the first reference voltage setting circuit 49 in conformance with the instruction signal, and the set value of the first reference voltage V1 is changed. As a result, the time for the interpolar voltage to recover to the first reference voltage V1, i.e. for the discharge interruption time to recover, is suitably changed.
In other words, by means of the present invention, the number of abnormal discharges within a set time is counted, and this number of abnormal discharges is compared to a preset fixed value. When the number of abnormal discharges is small, the discharge interruption time is shortened according to this ratio. When the number of abnormal discharges is large, the suspension time is lengthened. As a result, the process can always be made stable, and its efficiency is increased.
FIG. 7 to FIG. 10 show a second embodiment of the present invention. In this embodiment, a control device 81 comprises an I/O section 87 and a memory section 85 connected to a CPU 83. This control device 81 controls, e.g., a processing power source 89 connected to the CPU 83. Such electrical processing characteristics as roughness of finished surface, tool electrode wear rate, process speed, processing clearance, etc., and such electrical processing conditions as polarity, maximum value of electric discharge current, discharge ON3#time and OFF3#time (interrupted time), etc., are recorded in the memory section 85. The memory mode is made from suitable combinations of process characteristics and conditions, for example, as shown in FIG. 8.
The I/O section 87, as shown in FIG. 9, comprises a display section 91 in which input and output data for the process condition set number, process condition, process characteristic, etc., are displayed, and a plurality of input key section 93 for roughness of surface finish (R), tool electrode wear rate (W), process velocity (V), processing clearance (E), retrieval (S), input (IN), and numerical values setting.
In this configuration, in the case where, for example, the maximum surface finish roughness, Rmax, is set at 15 μm, and the tool electrode wear rate W is set at less than 1%, because surface finish roughness R, as shown in FIG. 10, is classified into 15 ranks, the keys of the input key section 93 are used as shown in FIG. 9 for input of (surface roughness (W)), rank (1), input (IN)). Next, as shown in FIG. 10 (B), based on the table in which the tool electrode wear rate (W) is classified into 10 ranks, through the keys in the input key section 93 are used for the input of (wear rate (W)), rank (1), input (IN)). Next, by pressing the (retrieval (S)) key, a retrieval instruction is given. The combination of process conditions and process characteristics (referred to below as the process condition set) is stored in the memory section 85. After finding the process condition set which satisfies the conditions input by the operator, (that is 8 to 15 μm Rmax; surface roughness, 8 to 15 μm Rmax; tool electrode wear rate, less than 1% in this case), the display becomes, for example, as shown in the upper boxes of FIG. 9. When the displayed process condition set is not satisfied, another process condition set, which satisfies the input conditions, is displayed on the display section 91 by pressing the retrieval key (S) once more. This operation can be repeated, and once the last process condition set has been retrieved, the retrieval process is repeated from the beginning.
In this manner, when the operator's requested conditions are satisfied by the process condition sets which are displayed in order, the process power supply 89 is automatically set to the above-mentioned process conditions for example, by repeating the key-in of (input (IN)). Setting process conditions while paying attention to other process characteristics is done in a similar way.
By means of the above embodiment, the optimum process conditions corresponding to specific process characteristics can easily be set.
Although only preferred embodiments are specifically illustrated and described herein, it will be appreciated that many modifications and variations of the present invention are possible in light of the above teachings and within the purview of the appended claims without departing from the spirit and intended scope of the invention. | A process and apparatus for controlling an electric discharge machine consisting of applying a pulse voltage across a working gap when the predetermined time of interruption of the electric discharge has lapsed and when the interpolar voltage has exceeded a reference voltage, increasing the reference voltage and lengthening the time of interruption of the electric discharge when the rate of abnormal discharge occurrence becomes greater than an allowable rate and decreasing the reference voltage and reducing the time of interruption of the electric discharge when the rate of abnormal electric discharge occurrence is less than an allowable rate. | 1 |
FIELD OF THE INVENTION
The application is directed to a window insert that may be inserted into a gap near a window such that the insert may be visible through the window. More specifically, the application is directed to a window insert having a visible area that may be visible through the window and may also have a ledge area that may support, hold, or otherwise retain a removable product or removable accessory on, near, or around the window insert.
BACKGROUND
Today's busy and ambulant society spends significant amounts of time in vehicles moving between destinations or performing work on the job. This time can be in substantial blocks and can extend though periods of the day when meals are consumed. The convenience and other advantages associated with consuming meals in a vehicle have led to the development and growth of drive-in window restaurants and other eat-on-the-go food offerings. Indeed, societies' busy schedule has supported the near ubiquitous development and proliferation of drive-in window restaurants and other eat-on-the-go food offerings.
SUMMARY OF THE INVENTION
The invention includes embodiments where a window insert is placed in or around a gap or space near a window such that the insert can stay positioned near the window and can also retain, hold or support a condiment or food item being consumed by an individual. The person consuming the meal may include an operator or passenger of the vehicle as well as someone near the vehicle, but perhaps outside of it. The window in which the window insert is positioned near, may be in locations other than a vehicle as well. Also, the window may contain glass or other transparent or translucent materials and may be an opening with or without glass or other materials as well as openings with only some glass or other material.
In embodiments, the window insert can have an anchor area, a ledge area, and a visible area. The ledge area may contain wells or other features that can hold or retain food stuffs including condiments and other items being consumed during a meal. The ledge area or other portions of the window insert may be stored in a collapsed or folded configuration such that assembly of the window insert may be required prior to a user using the window insert. In some embodiments, the unfolding may require assembly or fitting of parts while in other embodiments it may require expansion of parts or combinations of expansion of parts and assembly or fitting of parts.
The visible area of the window insert may contain advertising or messages that are visible from outside the vehicle when the window insert is placed in the gap near the window. Thus, when a window insert is being used by a user, individuals outside of the vehicle or on the other side of the window may be informed by the visible printing or pictures on the visible area of the window insert, of a particular message, picture, or other information. In some embodiments these pictures and messages may contain advertising and other material; they can even designate the restaurant from which the meal was purchased or specials of the day. There may be printing, pictures, instructions of use, and other information on all or some surfaces of the window insert as well.
The window insert may be folded or stored such that it can be unfolded, expanded, or otherwise assembled prior to its use. By folding or storing the window insert in this fashion, the space occupied by stored window inserts and the transportation costs of the window inserts can be reduced.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 a - 1 c show top, side, and front views of a window insert in accord with one or more embodiments of the invention.
FIGS. 2 a - 2 b show side perspective views of a window insert in accord with one or more embodiments of the invention.
FIGS. 3 a - 3 c show a window insert, in accord with one or more embodiments of the invention, being placed into a gap near a vehicle window.
FIGS. 4 a - 4 c show top plan views of a window insert in accord with one or more embodiments of the invention.
FIGS. 5 a - 5 c show top plan views of a window insert in accord with one or more embodiments of the invention.
FIG. 6 shows views of a window insert being expanded in accord with one or more embodiments of the invention.
FIGS. 7 a - 7 e shows views of various embodiments of a window insert in accord with one or more embodiments of the invention.
FIG. 8 shows sectional side views of various folding configurations of a window insert in accord with one or more embodiments of the invention.
FIG. 9 shows steps that may be taken while performing a method in accord with one or more embodiments of the invention.
DETAILED DESCRIPTION
When a meal is consumed in a motor vehicle, such as in an automobile, tractor-trailer, or work vehicle, the operator or passenger may choose to consume the meal while the vehicle is running, perhaps even when the vehicle is moving and being operated. When different types of food are consumed during a meal eaten in a vehicle, for instance a “French-dip” sandwich and drink, the operator or passenger can be confronted with a lack of space to hold or retain some of the food or drinks being consumed during the meal. Cups may be placed in cup-holders, but little, if anything else, exists within the vehicle to support or retain the food being eaten, including the condiments that may be consumed to compliment the meal. For example, with respect to the “French-dip” sandwich, the aus-ju broth may be placed on an adjacent seat or the dash board, neither of which is within easy reach of an occupant of the vehicle. Indeed, the aus ju broth may be prone to spilling and sliding if the vehicle is moving when placed in either of these locations.
Embodiments of the invention include inserts for holding or supporting portions of a meal, where the inserts may be placed next to a window of a motor vehicle or other opening. These inserts may be slid into a gap near the window and may be further supported by a flange or shelf near the window. When in use, the window insert may support or hold condiments, or other portions of a meal being consumed by a user. The gap into which the window insert may be slid may be the gap associated with windows that retract into a door or side panel of a vehicle as well as a gap associated with a window that swings away from its frame, much like a casement window. The gap may be on other types of windows or openings as well.
A portion or all of the insert sliding down into the gap next to the window, may anchor or provide stabilization to the insert. The insert may also include a ledge that may rest on a shelf, flange, or other surface near the window. This shelf, flange, or other surface may provide stabilization to the insert. The cooperation between the anchor of the insert, the ledge of the insert, and the shelf or other surface near the window, can provide an adequately stable area in which condiments, or parts of a meal being consumed by a user, may be placed. Thus, in a vehicle, the window insert takes advantage of the presence of an arm rest shelf area and the gap near a retractable window, in order to provide support or otherwise hold condiments or other portions of a meal being consumed by a user.
Being positioned near the window, the window insert may be visible from outside of the vehicle. As noted above, this visible area may be used for advertising or for other purposes as well. The visible area may contain previously printed images or words to be viewed by someone outside of the vehicle or on the other side of the window when the insert is positioned at the window. The advertising can contain the name of the restaurant that is the source of the meal as well as specials or other information about the restaurant. It may contain images and text that are unrelated to the restaurant or is only tangentially related to the restaurant that provided the insert. For example, a local radio station may be advertised on the visible area and/or a local promotion being sponsored by the restaurant may each or both be advertised. Various combinations of text and figures may be provided in the visible area and/or on other portions of the window insert.
As noted above, a user of the window insert may be asked, prompted, or required to expand, unfold, partially assemble, or fully assemble the window insert. The window insert may be comprised of a heavy paper card stock or other flexible material and may be assembled by unfolding portions of the insert away from other portions of the insert. Wells present in the ledge may need to be punched out by the user or otherwise assembled as well. These wells may provide an area for holding or retaining condiments or other food items. In some embodiments the wells may be specifically designed and sized to accommodate a specific condiment container, such as a dipping sauce container. In an expanded position and during assembly, the ledge may need to be glued or otherwise secured back to the insert by the user. The ledge may be assembled such that the user need not do more than simply expand it, place the window insert into a gap near a window, and begin to use the window insert.
In use, customers may specifically request that they are provided a window insert when purchasing their meals. Restaurants may provide one for certain meals or for all meals. The design and preferable ease of manufacture of embodiments of the invention may enable restaurants to provide a window insert at no cost to the user. A restaurant may decide to charge for the window inserts as well. Other entities may also provide the window inserts to users.
Various bendable or flexible stock materials may be used to manufacture the window inserts. These would include thin fiber boards or card boards and relatively stiff paper boards. Other pulp based products may also be suitable as bendable or flexible stock materials. Flexible polymer sheets may also be used as stock materials. It is advantageous to use low cost materials that can be readily folded and punched to form the shape of the window insert and the one or more wells that the window insert may contain. Also, it is advantageous to select stock materials that may be readily printed on or embossed such that the information printed on the window insert may be readily seen and viewed by others who are able to see the visible area of the window insert when the window insert is being used.
FIGS. 1 a - 1 c show a two-dimensional view of the top, side, and front of a window insert 100 in accord to one embodiment. Visible in FIG. 1 is the body of a window insert 100 . The body of the window insert 100 in this embodiment comprised wells 110 , creases 140 , and a ledge 120 with a top surface 121 of the ledge 120 , a front surface 123 of the ledge 120 , and a bottom surface 122 of the ledge 120 . The window insert 100 in these figures also has a visible area 170 , an anchor 130 , and a lip 150 . Also visible in these figures is the attachment point 160 , where the stock material comprising the window insert 100 is secured to itself to form the ledge 120 . Various methodologies may be used to secure the stock material onto itself at the attachment point. These include adhesives and the physical configuration of the window insert itself. Examples of how this attachment may be made are provided later in the specification.
The creases 140 and the lip 150 of the window insert 100 , as well as the length of the anchor 130 , provide structural rigidity along the width of the window insert 100 . The wells 110 on the top surface 121 of the ledge 120 provide chambers, spaces or voids in which a condiment or other portion of a meal may be placed in and held by the window insert 100 . In this embodiment, the voids are rectangular in shape and spaced equidistant apart and in the top surface. Other orientations and spacings may also be possible to accommodate various food items or condiments. Likewise, the depth of the ledge 120 may be determined to accommodate a specific condiment container or food item such that the food item rests atop the top surface and extends near or completely to the bottom surface 122 of the ledge 120 . The top and side views of the window insert show its rectangular design, however, other designs and configurations are also possible. For example, the edges of the anchor may be rounded or cut out in various applications. Also, the top may be triangular or have other configurations. These other shapes may accommodate specific food items, specific placements, and may also contribute to the structural integrity of the window insert. In certain preferred embodiments the window inserts may range in size from two or so inches in width to six of more inches in width. The anchors may fall in this range as well. Other sizes are possible and also fall within the scope of the disclosure and the invention.
Images and text may be printed or embossed onto the visible area 170 as well as onto other surfaces of the window insert 100 . This may include placing instructions for assembly or use on one or more surfaces of the window insert 100 .
FIGS. 2 a - 2 b show perspective side views of a window insert embodiment As can be seen in this view, the bottom surface 122 of the ledge 120 need not be parallel to the top surface 121 of the ledge 120 . As can also be seen in FIG. 2 b , the attachment point 160 of the bottom surface 122 to the back of the window support may be below a crease 140 . Also, the transition between the top surface 121 and the visible area 170 may not include a lip and multiple creases as in FIG. 1 b . Thus, multiple configurations of a window insert in accord with the invention are plausible. The visible area 170 may contain printing and pictures in the entire area as well as in portions of the visible area 170 . The visible area 170 and the anchor 130 form a back of the widow insert in this embodiment.
FIGS. 3 a - 3 c show internal and external views of a window insert 100 being placed in a window of a vehicle door 300 in accord with embodiments of the invention. As shown by the arrow 320 , the anchor 130 is intended to be inserted into the gap 310 of the vehicle door 300 and the window 330 . As shown in FIG. 3 c once the window insert is in place, the visible area 170 is visible through the window 330 . Also evident, and as shown in FIG. 3 b is that the ledge 120 is resting on the shelf 380 of the vehicle door 300 . Thus, the combination of the ledge 120 resting on the shelf 380 , and the creases of the window insert design, provide adequate rigidity and support for food items that may be retained by the window insert, including condiment containers placed in the wells of the ledge.
The window may be in various open or closed positions when the window insert is placed in the gap 310 . The window may even be retracted when the window insert is positioned. Conversely, however, it is not recommended that the window be raised when the window insert is in the gap because the raising forces of the window may lift the window insert up and out of the gap. Nevertheless, raising the window may be considered within the scope of the invention.
FIGS. 4 a - 4 c show various top views of embodiments of the window insert. FIG. 4 a shows that the lip 150 and creases 140 may extend out away from the back of the window insert when the ledge is assembled. FIG. 4 b shows a window insert 400 having a single well 410 . FIG. 4 c shows a window insert 401 having double wells but no lip or creases on the top surface. Support for the top surface may be provided here, or in other embodiments, through creases in other areas of the window insert and through other supports, such as through a center beam made from the card stock the window insert is made from where the center beam extends from the back of the window insert to the front of the ledge and provides additional support opposing collapse of the ledge.
FIGS. 5 a - 5 c show various well configurations of an exemplary window insert. Wells 510 , 511 , and 512 are shown with square, hexagonal, and circular dimensions. Other dimensions are also plausible. In this and other embodiments, while a uniform depth is shown in the ledge and the wells within the ledge, various depths may be considered such that short and tall food items or food items having significantly different shapes, may be retained by the window insert. Thus, the ledge may have different heights or depths and so too may the wells. For example, one well may be 0.5 inches deep while an adjacent well may be 0.35 inches deep. Likewise, the ledge may be 1.0 inches high on one end and 0.5 inches high on another end.
FIG. 6 shows how a window insert may be stored and subsequently expanded in use. Beginning in step one, the window insert may be manufactured such that the ledge is folded down across the anchor of the window insert. As can be seen, in this folded configuration the bottom surface may be sized such that its length is approximately equal to the combined length of the lip, the top surface and the front surface of the ledge. As the ledge is pulled forward and expanded in step two, the creases and lip near the bottom surface may begin to move away from the back along with the ledge itself. In step three, the creases and lips of the top surface and the bottom surface may be crimped such that they provide the rigidity and support to the assembled window insert. Once expanded or during the expansion process, the window insert may be placed in the gap near a window for use. The wells in this embodiment are shown punched out. In some embodiments additional steps may be needed to punch out or otherwise assemble the wells in the top surface of the ledge as well. In this embodiment the attachment point between the back and the bottom surface of the ledge has been affixed prior to assembly by the user. In other embodiments, the user may be required to attach the bottom surface of the ledge to an inside back surface of the window insert.
FIGS. 7 a - 7 e show various methods in which the bottom surface of the ledge may be affixed to the back of the window insert. FIG. 7 a shows a slit 761 in the back of the window insert in which a tab 760 from the bottom surface of the ledge may be inserted. Once inserted, the tab may be bent to inhibit removal of the tab from the slit 761 . FIG. 7 b shows a line of glue 762 being used to secure the bottom surface of the ledge to the back of the window insert. This glue may be adhered by the manufacturer, by the user, or a combination of both. For instance, one surface may have glue applied to it by the manufacturer while the mating surface may have glue applied by the user. FIG. 7 e shows a variation of this as a peel and stick adhesive is used to secure the bottom surface to the back of the window insert. FIG. 7 c shows tabs 763 that may be folded over the back from the bottom surface in order to assemble the ledge of the window insert. FIG. 7 d shows how slits 765 and 764 may be cut in the bottom surface and back and then mated with each other to secure the bottom surface to the back of the window insert. Each of the slit, the line of glue, the peel and stick surfaces, and the tabs may be considered means for securing the ledge to the body of the window insert.
FIG. 8 shows various side sectional elevations of a window insert in accord with the invention. As can be seen, various lengths of the top surface and bottom surface may be used and some embodiments may or may not have creases and/or top lips in their designs. The window inserts 821 - 829 each have four sides in these embodiments, however, four sides are not required as three or other another number may be used. When three sides comprise the ledge, a side sectional view of the ledge would generally form a triangular shape.
FIG. 9 shows a method of manufacturing a window insert in accord with the disclosed embodiments of the invention. As shown in the boxes of FIG. 9 , the method may include sizing and cutting bendable stock, such as paper or cardboard or plastic or laminated sheeting, to a preselected size and shape. The preselected size and shape may include rectangular, square, trapezoidal shapes occupying one or less square feet. Other dimensions and sizes may also be used. It is preferred that the selected shapes allow for the window insert to be assembled from a single card stock, although assembling the window insert from multiple card stocks may be possible. Images may also be printed on sides of the card stock as indicated in box 910 . These images and text may include advertising for the visible area that can be viewed through the window as well as assembly instructions for an end user. The manufacturing process may also include scoring, folding, cutting and otherwise assembling the card stock such that a partially assembled window insert is constructed. Still further, the manufacturing process may include embossing or scoring the stock such that subsequent steps may be drawn or folded along the embossment or score to create features such as the openings or wells of the ledge and the slits for securing the ledge to the window insert body. Vacuum forces as well as mechanical presses may be used during the various steps of the manufacturing process.
Box 930 shows that in addition to instructions being placed on the card stock itself, additional instructions may be packaged with a plurality of window inserts that are gathered for shipment and storage. Box 940 shows that the manufacturing steps may include gathering, packaging, and wrapping the window inserts for shipment to and storage at restaurants or other institutions that distribute or sell the window inserts to its customers. Thus, the finished manufacturing product can include the partially assembled window inserts as well as window inserts that have been packaged together for storage and shipment to restaurants or other end users.
Various configurations of a window insert as well as methods for assembly and manufacture have been provided. In addition to these embodiments and examples others are also possible within the scope of the invention. Moreover, features and aspects from the disclosed embodiments may be readily exchanged with each other as well as removed and added to the various embodiments. These changes can include the manner in which the window insert is designed, the manner in which it is displayed, and the manner in which it is supported. Likewise, the methods described herein may include each of the steps provided as well as additional and fewer steps. The order of the steps may be different as well. | The application is directed to a window insert that may be inserted into a gap near a window such that the insert may be visible through the window. In certain embodiments, the application is directed to a window insert having a visible area that may be visible through the window and may also have a ledge area that may support, hold, or otherwise retain a removable product or removable accessory on, near, or around the window insert. The window insert may further comprise an anchor and a visible area wherein the ledge contains one or more wells for holding or retaining food stuffs. | 1 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to European Patent Application No. 02257217.6, filed 17 Oct. 2002, which is hereby incorporated by reference as if fully disclosed herein.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a power conversion unit for a window covering, in particular a powered movable window covering, and a method of providing power to such a window covering.
[0004] 2. Description of the Relevant Art
[0005] Various types of window covering are well known and include, for instance, Venetian blinds, roller blinds, vertical-slat blinds, pleated and cellular shades. These coverings have well known uses for selectively covering not only windows, but any other form of architectural opening.
[0006] Window coverings usually include a headrail for supporting or at least controlling the covering or blind itself. EP-A-1020613 considers such a headrail. It will be appreciated that headrails are usually positioned above the blind with a horizontal orientation. However, headrails may also be used in other orientations, such as a vertical orientation.
[0007] Traditionally, headrails are provided with pull cords and/or rotatable wands for operating the covering. In particular, the headrails incorporate mechanisms whereby movement of the cords or wands causes a corresponding movement of the covering.
[0008] It is also known to provide a powered window covering whereby powered actuators such as motors provide the moving forces previously required from the cords or wands. While these powered window coverings are very effective and desirable, the additional actuators (such as motors) and associated power supplies require extra space and result in the overall arrangement being undesirably bulky.
SUMMARY OF THE INVENTION
[0009] The present application is particularly concerned with the power supply and recognises for the first time the possibility of incorporating a power conversion unit within the headrail of a window covering in order to reduce the overall size of the assembly.
[0010] Based on this recognition, it is an object of the present invention to miniaturize the transformer required for power conversion such that it can be mounted within a headrail. However, as is well known, all transformers, in particular, high frequency transformers, fall short of their theoretical ideal. As a result, for instance, of magnetic field leakage, voltage spikes can occur which are traditionally handled by resistive snubber circuits. The snubber circuits and transformers generate undesirable amounts of heat which prevent such a power conversion unit from being installed within a headrail.
[0011] It is an object of the present invention to overcome or at least reduce these problems.
[0012] According to the present invention, there is provided a method of providing power to a powered movable window covering using conversion circuitry with a transformer to obtain relatively low voltage supply from mains supply, the method including a) providing in the conversion circuitry a snubber circuit for the transformer, the snubber circuitry absorbing power from the transformer and supplying power absorbed from the transformer back to the conversion circuitry such that heat generation from the conversion circuit with the transformer is minimised and b) mounting the conversion circuitry in the headrail of the window covering so as to reduce the overall size of the window covering.
[0013] Thus, similarly, according to the present invention there is also provided a power conversion unit for a powered movable window covering, the unit including power conversion circuitry having a transformer, a snubber circuit for absorbing power from the transformer and a housing containing the power conversion circuitry and snubber circuit, wherein the snubber circuit provides power absorbed from the transformer to the power conversion circuitry.
[0014] In this way, the overall heat generation of the power conversion unit is significantly reduced such that it does become possible to provide the power conversion unit in the confined space of a headrail. Suitable snubber circuits, incorporating for instance, capacitive measures for absorbing and then releasing the power from the transformer, are known for other transformer applications. Many of these snubber circuits may be adapted for use with the present invention. However, according to the preferred embodiment the snubber circuit provides absorbed power to the primary side of the transformer.
[0015] It will be appreciated that transformers are often constructed with an additional secondary coil which is used to provide power to components on the primary side. By using the snubber circuit to provide this power, this additional secondary coil can be eliminated and the overall construction simplified and reduced in size. Furthermore, with power provided from the snubber circuit to the primary side, there is no connection from the high voltage primary side to the low voltage secondary side, thereby enhancing safety.
[0016] Preferably the transformer includes high frequency ferrite transformer cores.
[0017] Thus, the method may include supplying the transformer with high frequency AC power.
[0018] In this way, in comparison to using a transformer at a normal mains frequency of 50 Hz to 60 Hz, it is possible to substantially reduce the overall size of the transformer. In particular, high frequency ferrite cores can be of significantly reduced size for the same power/voltage transformation.
[0019] Preferably, the power conversion circuitry includes a rectifier for converting mains power to DC power and an inverter for converting the DC power to high frequency AC power for supply to the transformer.
[0020] In this way, the power conversion unit may be connected to a normal mains supply and yet still use high frequency ferrite transformer cores to provide a low voltage supply for any control circuitry and actuators in the window covering. By using the high frequency ferrite transformer cores of reduced dimensions in conjunction with the snubber circuit for providing power from the transformer back to the power conversion circuitry, it is possible to provide a power conversion unit of significantly reduced dimensions and heat generation.
[0021] Preferably, the high frequency is over 100 KHz. This allows the use of suitable cores. Indeed, for lower frequencies, undesirably large induction coils are required as filters.
[0022] It would be desirable to provide a frequency which is as high as possible. However, 300 KHz is the approximate practical upper limit. As the frequency is increased, so the size of the induction coils for filtering can be reduced. However, at higher frequencies, it becomes necessary to incorporate additional, more elaborate, circuitry, such that the overall size again starts to increase.
[0023] Preferably, the inverter converts the DC power to high frequency AC power with a fluctuating frequency.
[0024] This results in electromagnetic emissions which have a spread spectrum rather than a high peak point. As a result, the overall effect of emissions is reduced together with any noise production of the power supply. Preferably, the frequency fluctuates between 250 KHz and 300 KHz.
[0025] This range is sufficient to give a good spread spectrum and is positioned at a high frequency to allow the reduction in size of the ferrite cores.
[0026] Preferably, the housing has a cross section suitable for insertion into a headrail of a window covering.
[0027] Hence, the power conversion unit may be used to meet the objective of the present invention.
[0028] Preferably, the housing is elongated in a direction substantially perpendicular to the cross section.
[0029] In this way, for a headrail of relatively small cross section, it is still possible to insert the power conversion unit by arranging the components of the power conversion unit in an elongate fashion.
[0030] In particular, preferably, the power conversion circuitry includes first and second circuit boards extending in the elongate direction, the first circuit board supporting at least the transformer and the second circuit board supporting at least other components of the power conversion circuitry.
[0031] Preferably, the transformer is divided into a plurality of serially connected sub-transformers arranged along the first circuit board in an array in the elongate direction.
[0032] This is particularly advantageous in allowing the dimensions of the transformer to be reduced still further in at least two dimensions. The transformer is extended by means of the sub-transformers, along the third dimension in the elongate direction. This allows the transformer to be inserted in a headrail of small cross section.
[0033] Preferably, large components, such as capacitors, are supported at one or both ends of the first and circuit boards and extend generally in the elongate direction.
[0034] In this way, to minimise the cross section required by the power conversion unit, the large components are mounted so as to encompass an extension of the cross section of the circuit boards rather than to add to that cross section by being mounted on one side.
[0035] In one embodiment, the first and second boards may be joined end to end so as to form a single elongate circuit board.
[0036] The power conversion unit of the present invention may be used with a headrail having a rotatable shaft extending along the headrail at a generally central position. With this embodiment, the housing preferably has a cross section suitable for insertion into the headrail on generally one side of the rotatable shaft. All of the components of the power conversion unit extend along one side of the rotatable shaft.
[0037] According to another embodiment, the first and second circuit boards preferably extend in generally parallel spaced apart planes so as to define at least a central space therebetween.
[0038] The housing preferably has openings at each end in line with the central space such that the housing can be inserted in the headrail with the rotatable shaft of the headrail extending through the central space.
[0039] Thus, in this way, the components associated with the first circuit board extend on one side of the shaft and the components associated with the second circuit board extend along the other side of the shaft. Of course it will also be possible for components to extend into the space between the first and second circuit boards either side of the central space occupied by the rotatable shaft.
[0040] Preferably, the housing includes end caps at each end, the end caps defining the openings.
[0041] The housing preferably also includes an inner wall defining an elongate central passageway extending through the housing in the central space, the passageway allowing the shaft to be located extending through the housing.
[0042] The inner wall prevents the interference between the components of the power conversion unit and the rotatable shaft.
[0043] According to the present invention, there is also provided a headrail for a window covering including the power conversion unit.
[0044] Preferably the headrail includes the rotatable shaft extending generally centrally along its length. The shaft may be used for retracting/deploying a covering and/or tilting slats on the covering.
[0045] The power conversion unit may also be mounted outside the headrail and still provide significant advantages. In particular it allows the overall assembly to be of reduced size and can be mounted in small spaces adjacent to the headrail.
[0046] According to the present invention, there is also provided a window covering assembly including the headrail.
[0047] The invention will be more clearly understood from the following description, given by way of example only, with reference to the accompanying drawings, in which:
BRIEF DESCRIPTION OF THE DRAWING
[0048] [0048]FIG. 1 illustrates a perspective view of a power conversion unit according to the present invention;
[0049] [0049]FIG. 2 illustrates an exploded view of the power conversion unit of FIG. 1;
[0050] [0050]FIG. 3 illustrates a perspective view of the power conversion unit of FIG. 1 with end portions of the housing broken away;
[0051] [0051]FIG. 4 illustrates a lower plan view of the circuit board of the embodiment of FIG. 3;
[0052] [0052]FIG. 5 illustrates a perspective view of the embodiment of FIG. 2 with the power conversion circuitry extended from one end of the housing;
[0053] [0053]FIG. 6 illustrates a top plan view of the printed circuit board of FIG. 4;
[0054] [0054]FIG. 7 illustrates a circuit diagram of the input circuit connected to the primary side of the transformer;
[0055] [0055]FIG. 8 illustrates a circuit diagram of the output circuit connected to the secondary side of the transformer;
[0056] [0056]FIG. 9A illustrates a circuit diagram of a local voltage controlled oscillator for controlling the circuit diagram of FIG. 7;
[0057] [0057]FIGS. 9B, 9C and 9 D illustrate various voltages within the circuit of FIG. 9A;
[0058] [0058]FIG. 10 illustrates a control circuit for use with the circuit of FIG. 7 for eliminating the effects of load or input variations;
[0059] [0059]FIG. 11 illustrates a circuit diagram for a snubber providing an auxiliary power supply;
[0060] [0060]FIG. 12 illustrates a window covering arrangement in which the present invention may be embodied;
[0061] [0061]FIG. 13 illustrates an end view of a headrail incorporating the power conversion unit of FIG. 1;
[0062] [0062]FIG. 14 illustrates an end view of a headrail with two alternative positions for supporting the power conversion unit of FIG. 1, one inside and one outside of the headrail;
[0063] [0063]FIG. 15 illustrates an end view of a headrail supporting the power conversion unit of FIG. 1 on the rear side of the headrail;
[0064] [0064]FIG. 16 illustrates a roller blind headrail supporting the power conversion unit of FIG. 1;
[0065] [0065]FIG. 17 illustrates an end view of a headrail, such as for a pleated or cellular shade, incorporating the power conversion unit of FIG. 1;
[0066] [0066]FIG. 18 illustrates in an exploded arrangement an alternative power conversion unit embodying the present invention; and
[0067] [0067]FIG. 19 illustrates the power conversion unit of FIG. 18 partially fitted in a headrail.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0068] The following description relates to two principal embodiments, the first of which is intended to fit within approximately half the cross section of a headrail on one side of a rotatable shaft and the second of which is intended to approximately fill the cross section of a headrail and is provided with a central space for accommodating the shaft. The electronic components making up the power conversion circuitry may be the same in each embodiment and are described with reference to the first embodiment.
[0069] [0069]FIG. 1 illustrates an assembled power conversion unit 1 according to the first embodiment. The unit includes a housing 3 with an input lead 5 and an output lead 7 . The housing 3 preferably has a constant cross section along its elongate length, with the respective input and output leads extending from opposite longitudinal lengths.
[0070] The elongate housing 3 is provided with a generally semi-circular recessed groove 9 which, as will be described below, provides clearance for a longitudinally arranged shaft. Preferably, the longitudinal ends are closed off with end caps of which only end cap 11 is visible in FIG. 1. The illustrated housing 3 is also provided with longitudinal ridges 13 and 15 along opposite sides of the housing. These ridges may be used for mounting the housing.
[0071] [0071]FIG. 2 illustrates the housing 3 with its two end caps 11 , 11 a detached and the power conversion circuitry moved. In particular, the circuit board 17 is illustrated at a position above the housing 3 .
[0072] The circuit board 17 has components of the power conversion circuitry arranged on it so as to make more use of the space within the housing 3 . For example, components of large size, such as condensers/capacitors 19 , 21 , 23 , 25 are positioned at the end of the circuit board 17 to take maximum advantage of the available space within the housing 3 . These components are arranged so as to extend generally along the plane of the circuit board 17 . They extend at least partly within an extended volume of the circuit board 17 and hence avoid extending to one side of the circuit board 17 by an unnecessary amount. It is particularly advantageous to position there the primary and secondary capacitors/elcos C 8 ,C 9 ,C 20 and C 2 ,C 4 respectively of FIGS. 7 and 8, to be described further below.
[0073] The circuit board 17 is also arranged with the power conversion transformer divided into a number of serially connected sub-transformers, each having cores 27 , 29 , 31 , 33 of relatively reduced size.
[0074] Other electrical components on the circuit board 17 may be kept within the boundaries of a cross section defined by the condensers 19 - 25 and transformer cores 27 - 23 . For convenience, therefore, these components are not noted particularly in FIG. 2.
[0075] The resulting arrangement of components on the circuit board 17 has an elongate length and a cross section of low profile. This allows it to be fitted within the elongate profile housing 3 illustrated in FIGS. 1 and 2. End cap 11 is provided with an aperture 35 to guide the input lead 5 outside of the housing 3 . A similar aperture is provided in end cap 1 la on the opposite longitudinal end of housing 3 so as to lead the output lead 7 outside of the housing 3 .
[0076] [0076]FIG. 3 shows a bottom perspective view of a power conversion unit with end sections of the housing 3 removed so as to expose the circuit board 17 . It should be noted how the contours of the transformer core 33 fit snugly within the contours of the interior of the housing 3 . FIG. 5 illustrates a similar perspective view from the top of housing 3 showing the circuit board 17 only partially inserted into the housing 3 .
[0077] [0077]FIGS. 4 and 6 illustrate respectively the bottom side and top side of a circuit board 17 without the housing 3 discussed above. In this embodiment, the circuit board 17 is a single elongate structure. However, according to alternative embodiments to be mentioned below, the circuit board 17 could be divided in two and provided as first and second elongate circuit boards.
[0078] On the bottom side of the circuit board 17 illustrated in FIG. 4, a circuit layout is imprinted for the primary circuit. Primary windings 37 , 39 , 41 , 43 are provided for each of the transformer cores 27 , 29 , 31 , 33 . In this respect primary winding 43 is visible under transformer core 33 in FIG. 3. At the other end of the circuit board 17 , a section 45 is provided for carrying other components of the power conversion circuitry, for instance a rectifier, inverter and snubber circuit to be discussed below.
[0079] [0079]FIG. 6 shows the top side of circuit board 17 . On one end of the elongate circuit board, there is imprinted the combined secondary windings 47 , 49 of the core pairs 27 , 29 and 31 , 33 respectively. In this respect, secondary winding 47 and core pairs 27 , 29 are illustrated in FIG. 5. The other end of the circuit board 17 , as discussed for the bottom side with relation to FIG. 4, has a section for carrying other components of the power conversion circuitry.
[0080] The following description relates to a preferred arrangement for the power conversion circuitry. It will be appreciated that a substantial number of variations may be made to this circuitry without departing from the scope of the invention. Indeed, parts of the power conversion circuitry have well known functions which can be replaced by equivalent alternative circuitry.
[0081] [0081]FIG. 7 illustrates a third input circuit 59 including a transformer 51 . The transformer 51 has at least one primary winding, schematically represented by numeral 53 , at least one core, schematically represented by numeral 55 , and a secondary winding, schematically represented by numeral 57 . As will be explained below, the core 55 is preferably a high frequency ferrite core and the transformer 51 is used to transform AC power at high frequencies, for instance 250 KHz to 300 KHz. The transformer 51 may be embodied as discussed above with reference to FIGS. 1 to 6 , as a plurality of serially connected transformers, each having a reduced sized core 27 , 29 , 31 and 33 . The cores are preferably constructed of a ferrite material having a high saturation flux density, high Curie temperature and low dissipation losses. High frequency ferrite core transformers of this type allow significant reduction in overall size and provision of the transformer(s) within the relatively confined housing 3 .
[0082] The input circuit 59 is intended to receive, from an input header 61 , mains power supply, such as conventional 220/240 volt or 110 volt alternating at 50 Hz or 60 Hz.
[0083] The input power passes through a bridge rectifier 63 to convert the alternating power supply into a DC power supply. A preferred rectifier for use as rectifier 63 is the Fairchild P/N MB 6 S 0.5A bridge rectifier. Capacitors C 20 , C 13 and C 15 receive and smooth the power and then a half-bridge driver 65 cycles transistors T 1 and T 2 on and off in order to convert the DC power provided by the capacitors C 20 , C 13 and C 15 into a high frequency power supply for the primary winding(s) of the transformer 51 . In the preferred embodiment, this AC power supply alternates with a frequency in the order of 250 KHz to 300 KHz.
[0084] The half-bridge driver 65 is preferably embodied as an IR2104 (S) type of an International Rectifier. In this arrangement, a first port 57 , labelled “IN”, and a second port 69 , labelled “ENABLE”, are provided. These ports will be referred to below in relation to FIGS. 9 and 10 respectively.
[0085] [0085]FIG. 8 illustrates the secondary side of the power conversion circuitry of the preferred embodiment. The high frequency transformed power induced in the secondary windings 57 is provided to a bridge arrangement of diodes, D 1 , D 4 , D 6 and D 7 . The bridge converts the transformed alternating power into a DC signal. Which converts the transformed alternating power into a DC signal. In the preferred embodiment, the diodes are preferably power Schottky rectifiers, for instance those having SMD code U34 as manufactured by ST Microelectronic of Veldhoven.
[0086] An array of elcos C 2 and C 4 , together with parallel capacitors C 10 and C 32 and inductor L 8 further stabilise the output from the bridge rectifier from diodes D 3 to D 7 . A low voltage DC supply of 24 volts is thus available between terminals 71 and 73 .
[0087] In order to reduce electromagnetic emissions from the transformer 51 , it is proposed that the actual frequency at which the transformer 51 operates is fluctuated in a controlled manner. In this way, the power of any emissions from the transformer 51 is spread over a predetermined spectrum and the power for any particular frequency is significantly reduced when compared to operating the transformer only at that frequency. This has significant advantages with regard to reducing noise.
[0088] [0088]FIG. 9A illustrates a preferred arrangement for achieving the required fluctuation in frequency. It includes a local voltage controlled oscillator which provides a signal to the first port 67 of the half-bridge driver of 65 of FIG. 7. This signal controls the half-bridge driver 65 such that the inverter formed in the circuit 59 of FIG. 7 produces an AC signal in the primary winding 53 which fluctuates in frequency. In the preferred embodiment, the local oscillator of FIG. 9A causes the frequency to fluctuate between 250 KHz and 300 KHz.
[0089] [0089]FIGS. 9B, 9C and 9 D illustrate voltages at points B, C and D as marked in FIG. 9A.
[0090] Period t v is determined by the supply voltage (provided through resistors R 5 and R 7 , the +325V supply charges capacitor C 3 ), whereas the period t f is a fixed value (the discharge through R 4 , D 8 , R 5 and R 7 is negligible). Hence, t v is variable whereas t f is not.
[0091] U1.A functions as a divider (in half) such that a frequency results which has a period or duration of 2 t v +2 t f . The frequency thereby depends on the supply voltage.
[0092] When the supply is loaded, the supply voltage will fluctuate with the result of a fluctuating frequency.
[0093] [0093]FIG. 10 provides a signal to the enable port 69 of the half-bridge driver 65 . This circuit is a control circuit for keeping the output voltage at a fixed level and for eliminating mode or input variations.
[0094] A significant feature of the present invention is the provision of a snubber circuit which absorbs unwanted power from the transformer 51 , but does not merely dissipate this power as resistive losses. Instead, the power is fed back to the power conversion circuitry. FIG. 11 illustrates the preferred arrangement for the snubber circuit. However, although this circuit is believed to have significant advantages in its application in the power conversion circuitry of the present invention, it should be appreciated that other snubber circuits could also be used.
[0095] A number of known dissipitive snubber circuits have been considered in a number of previous publications, such as U.S. Pat. No.4,438,485, U.S. Pat. No. 4,899,270, U.S. Pat. No. 5,548,503, U.S. Pat. No. 5,615,094 and U.S. Pat. No. 6,285,567 B1 and the teachings of these documents are incorporated by reference.
[0096] It will be appreciated from these documents that a number of imperfections in any practical implementation of a transformer will result in undesirable outputs from the transformer, for instance in the nature of voltage spikes. By way of example, inevitably there will be some leakage flux from the primary side of the transformer and collapse of this flux will cause undesirable voltage spikes. Snubber circuits have been provided to absorb this excess energy, but, traditionally these snubber circuits have dissipated the power into resistive loads. This resistive dissipation produces undesirable amounts of heat, thereby preventing the transformer from being installed within the headrail of a window covering.
[0097] The power conversion circuitry of the present invention allows a power conversion unit to be installed in the headrail of a window covering by using a snubber circuit which provides the absorbed power back into the conversion circuitry itself.
[0098] As illustrated, the snubber circuit of FIG. 11 is connected at 101 to the primary winding 53 of the transformer 51 . The snubber circuit 91 then absorbs any excess energy in the form of voltage peaks and provides this back to the power supply VCC labelled as 103 in FIGS. 7 and 11.
[0099] By means of the arrangement discussed above, it is possible to incorporate all of the components of the power conversion circuitry into a compact housing 3 as illustrated in FIG. 1.
[0100] The housing 3 may be installed in the headrail 111 of a window covering arrangement 113 . The headrail 111 can take a variety of forms. However, many headrails incorporate a rotatable shaft which is mounted centrally along the length of the headrail. Rotation of this shaft may be used to deploy or retract the covering 105 and/or, where the covering 105 includes slats, rotate those slats.
[0101] FIGS. 13 to 17 illustrate a housing 3 as installed in a variety of different headrails. In particular, these Figures illustrate cross sections through the headrails. In FIG. 13 the power conversion unit is inserted in the lower portion of a headrail 117 and mates with the inner side and bottom surfaces of the headrail 117 . As illustrated, the groove 9 provides a central space through which a rotatable shaft 119 may extend. An insert or clip 121 then keeps the power conversion unit to the lower side of the headrail 117 .
[0102] In FIG. 14, two power units 1 a and 1 b are mounted to a headrail 123 a , 123 b . The first power conversion unit la is mounted within the headrail 123 a , 123 b towards the right side as illustrated in FIG. 14 and the groove 9 a leaves a central space for a rotatable shaft if required. The unit 1 a may be held in place by a clip, not illustrated, but similar to that of FIG. 13.
[0103] The second power conversion unit la is attached to a lower surface of the headrail 123 a , 123 b by means of ridges 13 b and 15 b discussed above with relation to FIG. 1. In particular, the headrail 123 a , 123 b is provided on its lower surface with inwardly facing grooves 125 b which slidingly engage in the ridges 13 b and 15 b to secure the second power conversion unit 1 b in place.
[0104] It will be appreciated that the headrail of this embodiment is composed of two parts, an upper part 123 a and a lower part 123 b . However, this is of no significant relevance to the present invention.
[0105] In the embodiment of FIG. 15, the power conversion unit is attached to the side of a headrail 127 by means of its ridges 13 and 15 . In the same way as described for FIG. 14, inwardly facing grooves 129 slidingly engage in the ridges 13 and 15 . In this arrangement, it will be appreciated that the power conversion unit is not installed within the headrail 127 . Nevertheless, the small size of the power conversion unit 1 still reduces the overall size of the assembly. Indeed, it might be possible to install the power conversion unit 1 between the headrail 27 and a wall in situations in which this would otherwise not be possible. The low heat production by the power conversion circuitry still allows the power conversion unit to be installed in confined spaces.
[0106] The embodiment of FIG. 16 shows an alternative headrail 131 in conjunction with a roll 133 which may operate a window covering under power from the power conversion unit 1 .
[0107] [0107]FIG. 17 illustrates a headrail 135 in which the power conversion unit I is mounted with a slanted or diagonal orientation. In this embodiment, the groove 9 again provides a central space in which a shaft 137 may extend and rotate.
[0108] As mentioned above, it is also possible to divide the circuit boards 17 in two. FIG. 18 illustrates an embodiment of this type.
[0109] A first circuit board 217 a includes a primary and secondary windings and the transformer cores are arranged along its length. A second circuit board 217 b is spaced apart from the first circuit board 217 a and is orientated within a generally parallel plane. This circuit board can support other components of the power conversion circuitry, noting that some other components could also be mounted on the first circuit board 217 a . As with the embodiments described above, in particular as shown in FIG. 2, bulky components 223 , 225 may be mounted on one or more ends of the circuit boards 217 a , 217 b . However, in addition, further bulky components 227 , 229 may be mounted between the circuit boards.
[0110] With this arrangement, it is possible to provide an arrangement which has the same width as that of FIG. 2, but at least half its length. Indeed, it is possible to reduce the length by more than half whilst retaining a square cross section by mounting components such as components 227 and 229 between the first and second circuit boards 217 a , 217 b.
[0111] The illustrated preferred embodiment is intended for use with a headrail 231 similar to that of FIG. 13 having a central rotatable shaft 233 . Therefore, for this embodiment, the first and second circuit boards are arranged with a central space therebetween. Indeed, where bulky components, such as 227 and 229 are mounted between the first and second circuit boards, these bulky components are arranged only along the sides either sides of a central space such that a shaft can pass between the first and second circuit boards along their length.
[0112] As illustrated, the housing 203 includes an inner wall 209 defining a central passageway extending the length of the housing 203 . The central wall 209 is supported by wall 209 a which extends between the inner wall 209 and at least one outer wall of the housing 203 . The first and second circuit boards and any components attached to them may thus be fitted within the housing 203 outside the inner wall 209 . The passageway within the wall 209 allows the shaft 233 to extend through the power conversion unit without interference with the circuit boards or components. In the preferred embodiment, end caps 211 and 211 a are provided on opposite ends of the housing 203 . The end caps define openings though which the shaft 233 may extend into the passage within the inner wall 209 . The input lead 205 and output lead 207 may also extend from respective end caps.
[0113] The power conversion unit 201 may be slidingly inserted into the headrail 231 as illustrated in FIG. 19. Indeed, in the illustrated embodiment, the outer profile of the housing 203 is arranged to fit an inner profile of the headrail 231 such that the power conversion unit is secured in place. | A power conversion unit and a method of providing power to a powered movable window covering using a conversion circuitry with a transformer to obtain relatively low voltage supply from main supply, the method including (a) providing in the conversion circuitry a snubber circuit for the transformer, the snubber circuit absorbing power from the transformer and supplying power absorbed from the transformer back to the conversion circuitry such that heat generation from the conversion circuitry with the transformer is minimised and (b) mounting the conversion circuitry in the headrail of the window covering so as to reduce the overall size of the window covering. | 4 |
BACKGROUND OF THE INVENTION
This invention relates to boilers and more particularly to a new and improved modular boiler.
The combustion chamber of a boiler is closed by a cover to which the burner is fastened. This cover is formed by a cast iron plate which is generally solid. When the gases or the gas-liquid mixture is introduced into the combustion chamber with a slight turbulent movement, a dead eddy is formed at the corner formed by the sidewall of the chamber and the cover. This dead eddy increases the total loss in the head of the boiler and decreases the transfer of heat by radiation by forming a screen between the flame and the wall of the cover. This is why the cover is generally solid, as there is no reason to provide water circulation at this point of the combustion chamber.
The presence of the dead eddy is also harmful to the stability of the flow of the gases in the combustion chamber and to the flame itself.
SUMMARY OF THE INVENTION
An object of the present invention is to remedy the drawbacks of the aforementioned solutions, at least in part. For this purpose, the present invention relates to a fluid fuel boiler comprising a combustion chamber formed of sidewalls, a bottom, and a cover which has an opening for a burner shaped to impart the mixture introduced into said chamber a pre-rotation coaxial to said opening, a water circulation circuit surrounding said chamber and connecting a source of cold water to a hot water collector, and a burned-gas circulation circuit in contact with the water circulation circuit and connecting the combustion chamber to at least one exhaust collector. This boiler is characterized by the fact that the cover is shaped in such a manner as to form the wall of the chamber, gradually flaring out from the opening towards the inside of the chamber, forming an angle with the axis thereof of between 15° and 55°, and by the fact that the wall of the cover is hollowed and communicates on the one hand with the source of cold water and on the other hand with the hot water collector.
Although in the following description the cover to which the present invention more particularly relates is associated with a boiler of a specific type which forms the object of other inventions, it should be pointed out that this cover may be used with any type of known boiler, providing said boilers with the same advantages as those enumerated in the following description. It is, for example, obvious that the invention applies to boilers which do not have an expansion vessel.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawing shows, by way of example, one embodiment of the boiler forming the object of the present invention.
FIG. 1 is a sectional view along the section line I--I of FIG. 2.
FIG. 2 is a sectional view along the section line II--II of FIG. 1.
FIG. 3 is a sectional view along the section line III--III of FIG. 1.
FIG. 4 is a sectional view along the section line IV--IV of FIG. 1.
FIG. 5 is a developed view along the section line V--V of FIG. 2.
FIG. 6 is a sectional view through a convection duct shown on a larger scale, in which the secondary movements of the gaseous mixture have been shown.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The boiler shown in FIG. 1 is a modular boiler which comprises a hollow cover 1, a bottom 2, three intermediate elements 3, and an expansion vessel 4 fastened to the bottom 2. The cover 1 has an opening 5 adapted to receive a burner 6. This opening 5 communicates with a combustion chamber 7 formed by the inner walls of the cover 1 and of the bottom 2 as well as by the central openings 8 provided through each of the intermediate elements 3. The inner wall of the cover 1 has a shape whose aerodynamic properties have been designed for a purpose which will be explained further below.
The bottom of the boiler, which closes off the combustion chamber 7, gives access to six ducts 9 having the shape of annular segments, which are concentric to the longitudinal axis of said chamber 7.
Before describing the boiler in further detail, we shall describe an intermediate element 3, with reference to FIG. 2. This element, shown in plan view, is of generally annular shape. On this element there can be noted the central opening 8 as well as the six ducts 9. The opening 8 and the ducts 9 pass through the element 3 which extends between two parallel planes perpendicular to the axis of the opening 8. This element is a hollow cast iron body produced by casting. The inner space 3a (FIGS. 1 and 5) of this hollow element communicates with two openings 10 and 11 which are diametrically opposite each other with respect to the opening 8 and pass through the element 3 parallel to the axis of the central opening 8. The opening 10 is connected to the cold water feed circuit while the opening 11 is connected to the hot water distribution circuit. Six radial segments 12 provided between the ducts 9 connect the body of the element 3, that is to say the portion located outside the ducts 9, to an inner ring 13 which surrounds the central opening 8. These radial segments 12 and the ring 13 are hollow on the inside so that they communicate with the inner space 3a located at the periphery of the ducts 9.
As shown in FIG. 1, the ring 13 extends over the entire width or length of the intermediate element 3 so that these rings 13 are assembled alongside of each other. This is not true of the portion of these elements 3 which extends along the periphery of the ducts 9. In this portion, the hollow space does not extend over the entire width or length of the element, the rest of this width or length being occupied by the three ribs 16, 19 and 20 provided on each of the two faces of the element and intended to form convection conduits 17 and 18 between the ducts 9 and the exhaust gas collectors 14 and 15 respectively which are diametrically opposite each other with respect to the axis of the combustion chamber 7. These collectors are closed by covers only some of which, 15', are visible in FIG. 1. As can be seen from this figure, the convention conduits 17, 18 alternate with the inner spaces 3a of the elements 3.
If one refers again to FIG. 2, it will be noted that the provision of the conduits 17 and 18 is obtained by means of two spiral ribs 19 and 20 which are 180° apart from each other and extend around a circular rib 16 forming the periphery wall of the ducts 9. Each of these ducts is connected to the conduits 17 or 18 or even to both of these conduits by two injection nozzles 21 extending over a portion of the length of the conduit, for the purposes which will be explained subsequently.
From FIGS. 1 and 3 it can be noted that a series of spaces 22, distributed over the same circumference, is formed between the cover 1 and the inner ring 13 of the modular element 3 adjacent the cover. These spaces 22 cause the downstream ends of the ducts 9 to communicate with the combustion chamber 7, so as to permit the reinjection of a certain amount of hot gases upstream in the combustion chamber and better balance the pressure in the ducts 9. The temperature of the burned gases thus becomes more uniform in these ducts, so that the heat transfer is better distributed. This reinjection favors blue-flame combustion which gives better efficiency and is less noisy than yellow-flame combustion.
This film of gas is thus reinjected along the wall of the chamber 7 in a zone which is particularly exposed by virtue of the temperature of the flame. As the reinjected gases are not as hot as the flame, they form a protective film locally. This is of particular importance when the boiler is provided with a cover such as that shown, which, as will be seen subsequently, causes the flame to hug the wall of the chamber. In this case, particularly if the boiler is powerful and has numerous intermediate elements 3, it is advisable that the film of reinjected gas at least partially prevent the flame from coming into contact with this wall and make it possible to avoid reactions between the flame and the carbon of the cast iron of the walls of the combustion chamber.
Finally, the internal recirculation of the burned gases causes a diluting of the gases in the boiler and leads to a reduction in the rate of formation of NO x .
The bottom 2 of the boiler also has an inner ring 23. The six ducts 9 having the shape of annular segments, commence between said ring 23 and the wall 24 which closes off the chamber 7. Like the other rings 13, the ring 23 communicates on the one hand with an opening 10' and on the other hand with an opening 11'. These openings are located in the extension of the openings 10 and 11 respectively, thus forming a conduit for the distribution of cold water to the boiler and a hot water collector respectively.
The bottom 2 also has an annular wall 25 which extends around the wall 24 and creates a communication with the openings 10' and 11'.
This annular wall 25 is intended for the attachment of the expansion vessel 4. This expansion vessel 4 has a wall 26 provided with a small opening 27 and is fastened in airtight manner to the end of the annular wall 25 thus forming, except for the opening 27, a closed space between the walls 24 and 26. The expansion vessel also has a diaphragm 28 whose edges are clamped between the edge of the wall 26 and the edge of a receptacle 29. These three elements are assembled on the annular wall 25 by a fastening collar 30. A guide ring 31 is fastened to the back of the wall 26, concentrically to the sidewall of the receptacle 29, and constitutes a guide support when the diaphragm 28 is folded towards the wall 26. This expansion vessel 4 also has an opening 32 through the wall of the receptacle 29, which serves to introduce a fluid between the diaphragm 28 and the receptacle in order to exert a certain pressure on the diaphragm 28.
The burner 6 is mounted coaxially to the chamber 7. It has a spiral supply well 36 fastened in the opening 5 of the cover 1. This well 36 is provided with vanes 37 intended to impart a pre-rotation to the jet of recirculated gases and air entering the chamber 7, the well being connected to the recirculation device for the burnt gases (not shown), which is connected to one of the exhaust collectors 14 and 15.
In operation, the combustion gases produced in the chamber 7 penetrate into the six ducts 9 having a shape of annular segments and flow in the direction towards the cover 1. As they advance in the ducts 9, the combustion gases enter the spiral conduits 17 and 18 via the injection nozzles 21 provided through the circular ribs 16. These spiral conduits 17 and 18 guide the combustion gases towards the exhaust collectors 14 and 15 respectively. One of the collectors is connected to the stack while the other is connected to the burner by a recirculation circuit (not shown). As has already been stated, the downstream ends of the channels of the ducts 9 communicate with the combustion chamber 7 via spaces 22. Thus a part of the combustion gases is reinjected into the combustion chamber through the spaces 22. This reinjection, as well as the recirculation of the gases in the burner, assures blue-flame combustion.
Various works have shown the curvature effect of a conduit of a given length on the flow of a fluid in said conduit. This curvature effect causes secondary movements within the flow in a plane perpendicular to the direction of advance of the fluid. The arrows included in the sectional view of such a conduit, shown on a larger scale in FIG. 6, indicate the path of these secondary movements. Now, these secondary movements greatly increase the heat transfer between the fluid and the walls of the conduit. They come from the centrifugal effect caused by the curvature, which effect is substantial only if the Dean's number of the flow is greater than a certain maximum. This maximum is a function of the Prandtl (Pr) number of the fluid, given by the ratio of the kinematic viscosity of the fluid to the thermal diffusivity of this fluid. The Dean's number is defined by the formula: ##EQU1## in which Re is the Reynolds number of the flow D H is the hydraulic diameter of the duct Rc is the radius of curvature of the duct.
By way of example, it may be stated that for a gas or a gaseous mixture in which Pr is of the order of 0.7, the minimum Dean's number which must be present in order for the secondary movements to be substantial is about 10. If Pr is about 5 (as in the case of water) De min is about 5 and if Pr is about 30 (as in the case of a light oil), De min is about 1.
The presence of injection nozzles 21, located along the inner face of the spiral convection conduits, has the effect of locally reinforcing these secondary movements by a factor which is a function of the difference between the velocities produced by the curvature, along the direction of the radius of curvature, and the velocity of injection. It can be said that if a flow of gas is injected through the nozzles extending through the inner face of the curvature (see FIG. 6) at a velocity 20 times greater than the secondary velocities produced by the curvature, the reinforcement factor of the curvature effects is of the order of 2, which is considerable.
The secondary movements effectively distribute the injected gases and make the temperature field at the periphery of the spiral duct more uniform. This results in a greater transfer of heat and a decrease in the thermal stresses in the metal.
It has been stated that the cross section of the different injection nozzles 21 decreases from nozzle to nozzle, in the downstream direction of the spiral convection conduits 17 and 18. This feature takes into account the losses in head present upon going from the upstream end towards the downstream end of these conduits and makes it possible to obtain uniform rates of flow for all of the injection nozzles.
Aside from the curvature of the convection ducts, the existence of the nozzles has several advantages, particularly the advantage of making the weight rate of flow uniform between the different elements 3 so that the last element will have substantially the same rate of flow as the first element, and moreover of maintaining an intense turbulence in the convection conduits, thus increasing the heat transfer coefficient, and finally of reinjecting hot gases into the gases which have already cooled down, which increases the average temperature of the gases and therefore the flow of heat transferred from the gases to the water.
One will also note the equiangular arrangement of the nozzles with respect to the longitudinal axis of the combustion chamber 7, which distributes the hot points in the metal uniformly, better distributing the thermal stresses.
It will furthermore be noted from FIG. 5 that the cross section of the convection ducts decreases from one nozzle 21 to the next, then increases suddenly again at each nozzle. This cross-section is selected so as to take into account the decrease in volume of the gases as a result of the cooling down thereof and the new conditions resulting from each reinjection. This cross-section is therefore calculated so as to maintain a substantially constant velocity of flow of the gases in the convection ducts.
While the combustion gases flow spirally in two separate streams between each element 3, the flow of the water takes place within these elements from the opening 10 to the opening 11. A part of the cold water entering into the inner space 3a of the intermediate elements 3 passes into the ring 13 via the radial segments 12 connecting the body of the element 3 to said ring.
Upon the placing in operation of the boiler, a certain pressure is created in the expansion vessel 4 between the receptacle 29 and the diaphragm 28 by introducing a gas under pressure through the opening 32, which is then hermetically closed. When the water is introduced, the pressure within the expansion vessel 4 is equalized via the opening 27. This arrangement of the expansion vessel is advantageous due to the fact that it makes it possible to integrate it in the boiler, thus forming a more compact installation.
During the course of the description mention has already been made of certain advantages of the boiler which is the object of the present invention. Still others may be mentioned which make is possible to solve many problems posed by the boilers today on the market.
Among such advantages, we may first of all mention the fact that the flow of the combustion gases between the ducts 9 and the collectors 14 and 15 takes place via convection conduits 17, 18, connected in parallel to the ducts 9. This arrangement of the convection conduits in parallel is extremely important due to the fact that it makes it possible to adapt the area of the cross-sections of passage of the combustion gases to the power of the boiler.
Each modular element is provided with two convection conduits 17, 18 which lead to two exhaust collectors 14 and 15, which makes it possible to effect the recirculation of the exhaust gases coming from one of the two collectors.
As can be noted particularly well from the cross-sectional views of the boiler, its geometry is symmetrical both with respect to the water, feed, and discharge conduits and with respect to the convection conduits and the exhaust collectors. This symmetry makes it possible to have uniformly distributed specific heat loads, thus avoiding strong internal stresses in the cast iron.
From these same cross-sectional views of the boiler it can also be seen that the second half of each convection conduit, located downstream of the nozzles 21 which discharge into said conduits, decreases in cross section as one approaches the exhaust collectors 14 and 15. As the cooling of the gases leads to a decrease in their specific volume, their absolute pressure remaining substantially constant, this decrease in cross-section makes it possible to make the velocity of these gases uniform and contributes to a good heat transfer. Turbulence generators (not shown) can also be placed in these conduits. This measure is however optional.
FIG. 1 shows that the ribs 16, 19 and 20 forming the convection conduits 17 and 18 constitute heat transfer vanes for the water circulation ducts.
It has been mentioned that the inner wall of the hollow cover 1 is of a special shape which, starting at the opening 5, provides a space of progressively increasing cross section of generally frusto-conical shape with an angle of between 30°0 and 110°. This cover 1 closes the combustion chamber 7 which is cylindrical. The conical portion connecting the opening 5 to the cylindrical chamber 7 is cooled by the circulation of water within the hollow cover. Moreover, the pre-rotation imparted to the feed gases by the vanes of the spiral well 36 imparts to these gases or to the gas-liquid mixture a turbulent movement which follows the conical portion of the cover. The value of the angle θ is selected as a function of the angular speed imparted to these gases or to the gas-liquid mixture. The inner shape of the cover 1 has the advantage of eliminating the dead eddyings which occur in the corners of boilers with flat covers. This conicity makes it possible to stabilize the flow and to elongate the flame, which spreads out on the periphery of the combustion chamber, located in the extension of the conical portion of the cover. The temperature of the flame is made more uniform and the volume of radiating burned gases is greater, which increases the heat transfer to the wall of the combustion chamber 7.
The elimination of the dead eddy which takes place in boilers with a flat cover at the corner between said cover and the combustion chamber, decreases the total loss in head of the boiler and increases the transfer of heat by radiation. This is due to the fact that the dead eddy is relatively cold and constitutes a screen against the radiation of the flame.
The suppression of this dead eddy therefore makes it possible to utilize the volume provided within the hollow cover in order to increase the total exchange surface of the boiler. Another reason for this circulation of water in the cover is that the water lowers the temperature of the surface of the cover. This cooling of the wall of the cover reduces the formation of nitrogen oxides NO x by the action of heat and reactions between the flame and the carbon of the cast iron of the cover. | A modular boiler having a cylindrical combustion chamber made of three modules and a module comprising a cover and a module comprising an expansion vessel mounted coaxially on the boiler adjacent the combustion chamber at opposite ends thereof. The cover has a frustro-conical configuration with the inner walls thereof diverging from an opening in the cover toward the interior of the combustion chamber at an angle of between 15° and 55°. The combustion chamber is formed of three castings that define the cylindrical combustion chamber and six axial hot gas flow paths spaced circumferentially from each other and disposed axially of and radially of the combustion chamber. Hot gases from the downstream end of the combustion chamber are recirculated to the upstream end of the combustion chamber to improve the combustion. Hot gas is diverted from these hot gas flow paths and flowed spirally of these flow paths along axially spaced flow paths immersed in the water circuit of the boiler to improve heat transfer. Liquid fuel is fed into the combustion chamber from a burner at the opening of the cover. The fuel is mixed with air to which a rotation has been imparted about the axis of the arrangement and entering the opening of the cover. The cover is jacketed and the jacket defines part of the inlet cold water circuit and the heated hot water circuit. | 5 |
RELATED APPLICATIONS
This is a continuation application of U.S. patent application Ser. No. 08/906,213, filed on Aug. 4, 1997, titled “A Concave Capacitor and Method of Making”, now U.S. Pat. No. 6,043,119.
BACKGROUND OF THE INVENTION
1. The Field of the Invention
The present invention is directed to the fabrication of microelectronic storage devices. In particular the present invention is concerned with methods of making a concave shaped capacitor in a stacked capacitor memory device such as a dynamic random-access memory (DRAM) where a large ratio of surface area to capacitor volume is desired.
2. The Relevant Technology
In fabrication of microelectronic devices there exists a relentless pressure to continue miniaturization for higher device density on a single chip and to increase device speed and reliability. It is advantageous to form integrated circuits with smaller individual elements so that as many elements as possible may be formed in a single chip. In this way, electronic equipment becomes smaller and more reliable, assembly and packaging costs are minimized, and integrated circuit performance is improved.
One device that is subject to the ever-increasing pressure to miniaturize is the DRAM. DRAMs comprise arrays of memory cells that contain two basic components—a field effect access transistor and a capacitor. Typically, one side of the transistor is connected to one side of the capacitor. The other side of the transistor and the transistor gate electrode are connected to external connection lines called a bit line and a word line, respectively. The other side of the capacitor is connected to a reference voltage. Therefore, the formation of the DRAM memory cell comprises the formation of a transistor, a capacitor and contacts to external circuits. The DRAM has one MOS transistor and one capacitor within a semiconductor substrate on which a plurality of spaced gates, that is, word lines, and a plurality of spaced metal wires, that is, bit lines are aligned perpendicular to each other in width-wise and lengthwise directions. Additionally, one capacitor having a contact hole in the center thereof is formed for every two gates and extends across the bit lines.
The recent trend of high integration of semiconductor devices, especially DRAM devices, has been based on the diminution of the capacitor storage cell, which leads to difficulty in providing a capacitor with sufficient capacitance to hold a charge long enough between refreshes for an optimally desired length of time.
The capacitor is usually the largest element of the integrated circuit chip. Consequently, the development of smaller DRAMs focuses to a large extent on the capacitor. Three basic types of capacitors are used in DRAMs—planar capacitors, trench capacitors, and stacked capacitors. Most large capacity DRAMs use stacked capacitors because of their greater capacitance, reliability, and ease of formation. For stacked capacitors, the side of the capacitor connected to the transistor is commonly referred to as the storage node, and the side of the capacitor connected to the reference voltage is called the cell plate. The cell plate is a layer that covers the entire top array of all the substrate-connected devices, and the storage node is compartmentalized for each respective bit storage site.
In a stacked capacitor, a conductor is usually made mainly of polysilicon, and a dielectric material is selected from a group consisting broadly of an oxide, a nitride and an oxide-nitride-oxide (ONO) laminator. In general, a capacitor occupies a large area on a semiconductor chip. Accordingly, it is one of the most important factors for high integration of DRAM devices to reduce the size of the capacitor yet to maintain the capacitance thereof.
The capacitance of a capacitor is represented by C=(κ∈ o A)/T, where C is capacitance, ∈ o is permitivity of vacuum, κ is the dielectric constant of the dielectric layer, A is the surface area of the capacitor, and T is the thickness of dielectric layer. The equation illustrates that the capacitance can be increased by employing dielectric materials with high dielectric constants, making the dielectric layer thin, and increasing the surface area of the capacitor.
The areas in a DRAM to which electrical connections are made are generally referred to as active areas. Active areas, which serve as source and drain regions for transistors, are discrete specially doped regions in the surface of the silicon substrate.
The ever-increasing pressure to miniaturize has placed capacitors of DRAMs under the strain of becoming ever smaller without losing the ability to hold a sufficient charge between refreshes. The challenge of making a capacitor that can hold a charge between refreshes can be approached by a larger capacitor surface area in a smaller space, or by insulating the capacitor to resist significant charge bleed-off between refreshes.
A need exists in the art for a capacitor that is contained in a small total volume that optimizes the surface area for charge storage, which capacitor is fabricated without costly and difficult extra processing steps.
SUMMARY OF THE INVENTION
In the microelectronics industry, a substrate refers to one or more semiconductor layers or structures which includes active or operable portions of semiconductor devices. In the context of this document, the term “semiconductor substrate” is defined to mean any construction comprising semiconductive material, including but not limited to bulk semiconductive material such as a semiconductor wafer, either alone or in assemblies comprising other materials thereon, and semiconductive material layers, either alone or in assemblies comprising other materials. The term substrate refers to any supporting structure including but not limited to the semiconductor substrates described above.
The present invention is directed to fabrication of capacitors that have concave shapes and optional convoluted surfaces in order to optimize surface area in a confined volume. The capacitors are fabricated in microelectronic fashion in order to make dense DRAM arrays. Capacitors that hold significant charges for a given volume assist in increased miniaturization efforts in the microelectronic field where a significant charge is stored in a smaller volume.
Methods of fabrication include stack building with storage nodes that extend both above the semiconductor substrate surface in some embodiments of the inventive method, and above and below the semiconductor substrate in others. Isolation trenches are included in the manufacturing methods in order to resist charge bleed off between refreshes.
The first twelve embodiments of the present inventive method are methods of stacked capacitor formation in which a polysilicon plug between gate stacks forms part of the structure. The thirteenth through twentieth embodiments of the inventive method are methods of stacked capacitor formation with no polysilicon plug between the gate stacks.
A preferable aspect to each of the first through the twentieth embodiment of the inventive method is that each said embodiment requires only a single masking step in the formation of the concave storage container cell into which a capacitor is formed.
These and other features of the present invention will become more fully apparent from the following description and appended claims, or may be learned by the practice of the invention as set forth hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
In order that the manner in which the above-recited and other advantages of the invention are obtained, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. The appended drawings depict structures accomplished by methods of the present invention but the structures are depicted qualitatively and dimensions are not quantitatively restrictive. Understanding that these drawings depict only typical embodiments of the invention and are not therefore to be considered to be limiting of its scope, the invention will be described and explained with additional specificity and detail through the use of the accompanying drawings in which:
FIG. 1 shows a cross-sectional view of semiconductor device before fabrication of a concave shaped capacitor.
FIG. 2 shows the device of FIG. 1 after a partially-penetrating etch as a precursor hole that will become a concave storage container cell after an isotropic etch.
FIG. 3 shows the device of FIG. 2 where there is depicted a space that has been etched out of the oxide layer after an isotropic etch to form the concave storage container cell.
FIG. 4 shows the device of FIG. 3 and further depicts the concave storage container cell with a precursor polysilicon layer coating the cell that will become the storage node.
FIG. 5 shows the structure of FIG. 4 with sacrificial layers removed.
FIG. 6 shows the device of FIG. 5 with a completed stacked capacitor having concave interior walls.
FIG. 7 shows an alternative completed capacitor in which the cell polysilicon has a larger surface area wrapped around the storage node than that which is shown in FIG. 6 .
FIG. 8 shows a cross-sectional view of a semiconductor device before fabrication of a concave shaped capacitor in which spacers are formed in order to create a convoluted capacitor surface.
FIG. 9 shows a cross-sectional view of a semiconductor device before fabrication of a concave shaped capacitor, wherein a single etch has etched through a photomask layer, hard mask, an oxide layer, and onto a polysilicon plug between two gate stacks.
FIG. 10 shows the device of FIG. 9 further processed to incorporate a completed capacitor, wherein the storage node contacts the polysilicon plug across the upper surface thereof.
FIG. 11 shows a cross-sectional view of a semiconductor device before fabrication of a concave shaped capacitor, wherein a single etch has etched through a photomask layer, hard mask, an oxide layer, and partially into a polysilicon plug between two gate stacks.
FIG. 12 shows the device of FIG. 11 after a completed capacitor has been formed between and above the dual gate stack and on the polysilicon plug having a recess in a top surface thereof.
FIG. 13 shows a cross-sectional view of a semiconductor device before fabrication of a concave shaped capacitor, wherein a single etch has etched through a hard mask, an oxide layer, and partially into a polysilicon plug between two gate stacks, wherein the etch is a mid-process anisotropic etch following by a spacer formation at an opening to volume created by the single etch, the opening being for the placement for an eventual convoluted capacitor surface.
FIG. 14 shows the device of FIG. 13 having a completed capacitor structure in which both a storage node and a cell plate polysilicon have convoluted surfaces.
FIG. 15 shows a cross-sectional view of semiconductor device before fabrication of a concave shaped capacitor, wherein a single etch has etched through a photomask layer, a hard mask, and an oxide layer to expose an opening on a surface of a substrate of a semiconductor wafer between two gate stacks, wherein the single etch, unlike that process illustrated in FIG. 9, has no polysilicon plug between the two gate stacks.
FIG. 16 shows a cross-sectional view of a completed capacitor made from a process option depicted in FIG. 15 .
FIG. 17 shows a cross-sectional view of semiconductor device before fabrication of a concave shaped capacitor, wherein a single etch has etched through a hard mask and has partially etched into an oxide layer to a depth extending between two gate stacks but above a surface of a substrate of a semiconductor wafer therebetween, wherein an incomplete isotropic etch with spacers extending vertically towards the substrate from the hard mask, the device requiring an additional step of removing the oxide layer between the gate stacks prior to formation of the intended capacitor structure.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is directed to methods of formation of a concave shaped capacitor. The methods of the present invention are used to obtain novel capacitor structures as well.
The concave shape for a capacitor is desirable in the present invention in order to increase surface area beyond that of prior art stacked capacitors that are straight cylinders or open boxes in shape. Although the concave shape of the present invention can be a simple, virtually enclosed container, the container can also include additional surfaces, such as convoluted surfaces.
Various means for achieving desired structural and functional results are used in the practice of the instant methods and in the achieved structures. The integrated circuit DRAM device of the present invention is comprised of dual gate structures that are situated above a substrate on a semiconductor substrate. The substrate integrally has active areas that enable the gate structures to function as respective transistors. Transistor structures of this type are well known in the art in which various capacitor structures for use on an integrated circuit DRAM have first and second word lines and first and second digit lines, the integrated circuit being fabricated on the semiconductor substrate.
The methods disclosed herein and the achieved structures preferably incorporate a doped or undoped polysilicon storage node, which can be employed within a stacked capacitor. A polysilicon plug is used to contact the polysilicon storage node. A hard mask, which is preferably a nitride or oxide layer, is described below, which is preferably easily formed and sacrificed. The cell dielectric is preferably composed of oxide or nitride dielectric materials that deposit and cover thinly and evenly upon storage node materials. The cell plate is preferably made of doped polysilicon and is formed by known methods. The spacers discussed below are made from polysilicon and oxides or nitrides that can be etched selectively over materials into which the spacers are formed.
The first twelve embodiments of the present inventive method are methods of stacked capacitor formation in which a polysilicon plug between gate stacks forms part of the structure.
The first embodiment of the present invention involves a starting structure illustrated in FIG. 1 . In FIG. 1 a semiconductor device 10 is being fabricated from a semiconductor substrate 12 with active areas (not shown) and two gate stacks 14 to form portions of a transistor. A polysilicon plug 20 is formed between gate stacks 14 . An oxide layer 16 , preferably borophospho silicate glass (BPSG), is formed over gate stacks 14 and polysilicon plug 20 . A hard mask layer 18 , preferably made of undoped or doped polysilicon or of a nitride composition, is formed over oxide layer 16 . To this structure a photomask 22 is spun on, aligned, exposed and patterned, as illustrated in FIG. 2 . Patterning and etching of hard mask 18 and a partially-penetrating etch into oxide layer 16 can be accomplished simultaneously or in a series of etching steps to result in the structure illustrated in FIG. 2 .
Following the partially-penetrating dry etch into oxide layer 16 illustrated in FIG. 2, an isotropic etch, preferably wet, is conducted in which hard mask 18 is undercut, as illustrated in FIG. 3 . The isotropic etch creates the concave storage container cell. Undercutting creates a greater surface area to be layered over by a plate of the capacitor structure that forms on the undercut-exposed surface of hard mask 18 .
If the isotropic etch does not remove oxide layer 16 down to the upper surface of polysilicon plug 20 , as illustrated in FIG. 3, an optional etch that is preferably anisotropic is needed to expose polysilicon plug 20 . This optional etch can be accomplished while leaving photomask 22 in place or it can be accomplished by using hard mask 18 as the masking medium. Because either photomask 22 or hard mask 18 are in place during both the isotropic concave shape forming etch and the optional anisotropic etch to expose polysilicon plug 20 , the anisotropic etch is self-aligning to photomask 22 or hard mask 18 such that the concave shape formed by the anisotropic etch will be centered in the bottom thereof.
Following the optional anisotropic etch to expose polysilicon plug 20 , storage node formation is done by chemical vapor deposition (CVD). The CVD process is a deposition of a polysilicon which is preferably doped with a doping that is similar to the doping of polysilicon plug 20 . The CVD process forms a storage node precursor or a doped polysilicon storage layer 24 . Doped polysilicon storage layer 24 is formed in such a way that the entire inside of the concave storage container cell is coated, and the upper surface of hard mask layer 18 is incidentally also coated, as illustrated in FIG. 4 .
In a next step, all material above oxide layer 16 is to be removed. Removal of both hard mask 18 and that portion of polysilicon storage layer 24 covering hard mask layer 18 can be accomplished by one of at least three methods.
The first method of removing all material above oxide layer 16 is to optionally fill the concave storage container cell with photomasking material and to planarize such as by chemical-mechanical polishing (CMP) of the superficial portions of polysilicon storage layer 24 and all of hard mask layer 18 , stopping on oxide layer 16 . Filling the concave storage container cell with photomasking material prevents fine slurry particulates used in CMP from becoming lodged in the concave storage container cell. Removal of photomasking material can be done by any method known and preferred in the art. In this first method, the sacrificial portions of polysilicon storage layer 24 can be removed before the CMP by a dry etch of upper portions of polysilicon storage layer 24 .
The second method of removing all material above oxide layer 16 is a dry anisotropic etch of both the superficial portions of polysilicon storage layer 24 and of hard mask layer 18 . In this etch, some etching of horizontally-situated portions of polysilicon storage layer 24 within the concave storage container cell will occur, such as at the bottom of the concave storage container cell where polysilicon storage layer 24 contacts substrate 12 . The anisotropic dry etch will likely etch away any horizontally-situated portions of polysilicon storage layer 24 to form what has now become storage node 26 . The anisotropic dry etch can also etch into polysilicon plug 20 to create a recessed area at a top surface thereof Such an etch will lessen the contact area between storage node 26 and polysilicon plug 20 . FIG. 5 illustrates the accomplished removal of superficial polysilicon storage layer 24 and of hard mask layer 18 by use of any of the first to the third methods as set forth above and below, respectively.
The third method of removing all material above oxide layer 16 is accomplished with a wet etch that is selective to oxide layer 16 and is not selective to polysilicon storage layer 24 . In this etch there will be some inevitable etching of the storage node portions of polysilicon storage layer 24 unless the concave storage container cell is likewise filled with a photomasking material such as in the CMP option described above. In such case, the wet etch will also be selective to the photomasking material within the concave storage container cell.
To complete the capacitor, FIG. 6 illustrates formation of a cell dielectric 28 that both coats the exposed surface of storage node 26 and the upper surface of oxide layer 16 where hard mask layer 18 formerly was situated. Cell dielectric 28 is deposited preferably by CVD. Finally, a cell plate polysilicon layer 30 is formed over cell dielectric 28 , and a superficial insulating layer 34 is formed over the entire structure and optionally CMP processed.
The second embodiment of the present inventive method, aspects of which are seen in FIG. 7, is accomplished with an additional process step in the first embodiment in which, following removal of superficial portions of polysilicon storage layer 24 and prior to formation of cell dielectric 28 , external lateral surfaces of storage node 26 are exposed through an additional etch of oxide layer 16 . By the additional etch to remove some of oxide layer 16 , there is a larger surface area possible for cell plate polysilicon layer 30 such that a larger charge can be induced on storage node 26 . The extent or exposing external lateral surfaces of storage node 26 is limited by the ability of storage node 26 to be laid bare and yet to resist physical damage during the remainder of capacitor fabrication.
After the additional etch that removes some of oxide layer 16 surrounding storage node 26 , cell dielectric 28 formation, cell plate polysilicon layer 30 formation, and a superficial insulating layer 34 formation are accomplished. By way of example, in this second embodiment seen in FIG. 7, the means for inducing a charge is in contact with the means for insulating, and the means for insulating contacts at least two surfaces of the means for charge storing in regions above the gate structure.
Third and fourth embodiments of the present inventive method incorporate an additional process step to that of the first and second embodiments of the inventive method. In the third and fourth embodiments of the inventive method, a partial etch into oxide layer 16 is followed by formation of spacers 32 , illustrated in FIG. 8 .
Although it is desirable to maximize the depth of spacers 32 in order to increase the storage node surface area that will be formed on both sides of spacers 32 , spacer depth is dictated by the eventual “bread loafing” of the opening to the concave storage container cell during all required deposition operations in which deposition materials must pass through the opening. Some materials will inevitably deposit so as to narrow the opening, while others will pass through and deposit on the inner walls of the concave storage container cell. With increased depth of the longitudinally vertical extension of the spacers, an exacerbation of the bread loaving effect may take place between the spacers of node, dielectric, or plate materials in the opening to the concave storage container cell before the capacitor structure is completed.
Following spacer formation, an isotropic etch is carried out for the third embodiment of the inventive method to open up the concave storage container cell. For the fourth embodiment, as seen in FIG. 9, an alternative step of an anisotropic etch penetrates oxide layer 16 down to the upper surface of polysilicon plug 20 . This is followed by an isotropic etch in oxide layer 16 to etch out the concave storage container cell.
The fifth, sixth, seventh, and eighth embodiments of the present inventive method are illustrated in part within FIGS. 9 and 10. In the fifth embodiment, an anisotropic dry etch etches through oxide layer 16 to extend downwardly to the top surface of polysilicon plug 20 , as seen in FIG. 9 . In this fifth embodiment, there is a finished storage node-polysilicon plug contact interface wherein polysilicon plug 20 contacts the storage node across an entire upper surface of polysilicon plug 20 , as illustrated in FIG. 10 . In the sixth embodiment, an anisotropic etch etches through oxide layer 16 and partially into polysilicon plug 20 , as seen in FIG. 11 . In both fifth and sixth embodiments of the inventive method, an isotropic etch follows to open the concave storage container cell. In the fifth and sixth embodiments of the inventive method, there is a finished storage node-polysilicon plug contact interface wherein polysilicon plug 20 contacts the storage node across an entire upper surface of polysilicon plug 20 . The interface may include a recessed area at a top surface of the polysilicon plug as illustrated in FIG. 12 .
Formation of doped polysilicon storage layer 24 followed by any of the three above-disclosed methods of removing sacrificial portions of polysilicon layer 24 and hard mask layer 18 is next accomplished. The structure achieved by the sixth embodiment is illustrated in FIG. 12 .
Seventh and eighth embodiments of the inventive method are variations of the fifth and sixth embodiments of the inventive method, respectively, that include the optional removal etch of some of oxide layer 16 that exposes external lateral surfaces of storage node 26 in order to increase the cell plate polysilicon surface area similar to that illustrated in FIG. 7 .
The ninth and tenth embodiments of the present inventive method, illustrated in part in FIG. 8 for the ninth embodiment and FIGS. 8 , 13 , and 14 for the tenth embodiment, include a partially-penetrating anisotropic etch of oxide layer 16 followed by spacer 32 formation. Once again, if the isotropic etch that follows formation of spacer 32 is insufficient to contact polysilicon plug 20 , an additional etch that is anisotropic is carried out to place a contact corridor in the bottom of the concave storage container cell, so as to open up and expose a surface on polysilicon plug 20 .
The tenth embodiment, seen in FIGS. 8, 13 , and 14 , includes a partially-penetrating anisotropic etch of oxide layer 16 followed by formation of spacer 32 , the same as in the ninth embodiment, but then a subsequent anisotropic etch penetrates through the remaining portions of oxide layer 16 to expose a surface on polysilicon plug 20 , and then partially etches into polysilicon plug 20 . There follows an isotropic etch to create the concave storage container cell, the upper surfaces removal by any of the three disclosed methods set forth above, and the formation of cell dielectric 28 and cell plate polysilicon 30 to accomplish the structure illustrated in FIG. 14 .
The eleventh and twelfth embodiments of the present inventive method are variations of the ninth and tenth embodiments of the inventive method that include the optional removal etch of some of oxide layer 16 that exposes external lateral surfaces of storage node 26 in order to increase the cell plate polysilicon surface area similar to that illustrated in FIG. 7 .
The thirteenth through twentieth embodiments of the inventive method are methods of stacked capacitor formation where polysilicon plug 20 between gate stacks 14 has been omitted.
FIG. 15 illustrates a thirteenth embodiment of the present inventive method in which a semiconductor device 10 is being fabricated, from a structure similar to that illustrated in FIG. 1, but without a polysilicon plug 20 . Substrate 12 with active areas (not shown) and two gate stacks 14 form portions of a transistor. Oxide layer 16 is formed over gate stacks 14 and hard mask layer 18 composed of polysilicon, is formed over oxide layer 16 . Photomask 22 is spun on, aligned, exposed and patterned, as was illustrated analogously in FIG. 2 . An anisotropic etch that is selective to photomask 22 is accomplished through hard mask layer 18 and oxide layer 16 so as to etch down to an opening that exposes a surface on substrate 12 . Gate stacks 14 act to align the anisotropic etch, if the anisotropic etch is selective to spacers forming the periphery of gate sacks 14 . An isotropic etch of oxide layer 16 that is selective to hard mask layer 18 and gate stacks 14 significantly undercuts hard mask layer 18 so as to create a concave storage container cell.
A formation of polysilicon storage layer 24 follows, which deposits within the concave storage container cell and upon hard mask layer 18 . The next step is removing of all superficial portions of polysilicon storage layer 24 above hard mask layer 18 . This removing step can be accomplished by any of three methods as disclosed above. To complete the capacitor of the thirteenth embodiment, as seen in FIG. 16, a cell dielectric 28 is formed over storage node 26 and a cell plate polysilicon layer 30 is formed over cell dielectric 28 . The device is finished with formation of superficial insulating layer 34 which may at least partially fill the concave storage container cell so as to be in contact with cell plate polysilicon layer 30 .
Regarding the thirteenth embodiment, because of the uniformity of an isotropic etch, and a large relative depth of the isotropic etch down to substrate 12 , it may occur that a small portion of oxide layer 16 will lie unremoved at the area between gate stacks 14 as illustrated in FIG. 17 . Unremoved oxide layer 16 between gate stacks 14 is removed before forming polysilicon storage layer 24 in order to complete an electrical connection with substrate 12 .
Removal of that portion of oxide layer 16 lying between gate stacks 14 can be accomplished by an anisotropic etch prior to the isotropic etch of the concave storage container cell, where the anisotropic etch penetrates substantially all the way down to substrate 12 . In this way, a substantially uniform isotropic etch occurs in oxide layer 16 . Additionally, with an isotropic etch that is selective to both gate stacks 14 and substrate 12 , substantially vertical walls are formed above substrate 12 between gate stacks 14 within the concave storage container cell. Removal of that portion of oxide layer 16 between gate stacks 14 can also be done by an anisotropic etch after the isotropic etch. This option simply removes that portion of oxide layer 16 that remains between gate stacks 14 .
A process engineer may choose to remove a portion of oxide layer 16 , illustrated analogously in FIG. 7, in order to expose external lateral surfaces of storage node 26 that would further increase the surface area between storage node 26 and cell plate polysilicon 30 , similar to the exposed external lateral portions of storage polysilicon for creation of a fourteenth embodiment.
The fifteenth and sixteenth embodiments of the inventive method are accomplished as optional steps to the thirteenth and fourteenth embodiments of the present inventive method by the step of forming a spacer immediately below the level of hard mask layer 18 that will increase the surface area of the capacitor. A spacer is formed into a concave storage container cell precursor that is followed by an isotropic etch for the fifteenth embodiment, or that is followed by an anisotropic etch to the substrate and an isotropic etch for the sixteenth embodiment. For both embodiments, the isotropic etch opens the concave storage container cell. The fifteenth and sixteenth embodiments of the present inventive method are combinations of the ninth with the thirteenth, and the tenth with the fourteenth embodiments of the inventive method, respectively, in which spacers are formed to increase the surface area of the subsequently formed polysilicon storage layer 24 . The fifteenth and sixteenth embodiments of the inventive method are illustrated by way of analogy in FIG. 8 in which the process is started, and in FIG. 13 in which the penetrating etch down to substrate 12 is accomplished, with the exception that there is no polysilicon plug 20 in the structure realized by the fifteenth and sixteenth embodiments of the inventive method.
In seventeenth, eighteenth, nineteenth, and twentieth embodiments of the present inventive method, described below, a further increase in storage capacity is accomplished in a starting structure in which polysilicon plug 20 is likewise not present. Spacers 32 are formed as in the third embodiment.
In the seventeenth embodiment, an isotropic etch follows formation of spacer 32 as illustrated in FIG. 17 . Following a partially-penetrating dry etch into oxide layer 16 , spacers 32 are formed and an isotropic wet etch is conducted in which hard mask 18 and spacers 32 are undercut, as illustrated in FIG. 17 . The isotropic etch clears out a concave shape to form the concave storage container cell. Undercutting creates a greater surface area for formation of a polysilicon storage layer 24 that forms on the undercut-exposed surface of hard mask 18 .
If the isotropic etch does not remove oxide layer 16 between gate stacks 14 , down to the upper surface of substrate 12 , as illustrated in FIG. 17, an optional etch that is preferably anisotropic is needed to expose substrate 12 . This optional etch can be accomplished while leaving photomask 22 , as seen in FIG. 9, in place or it can be accomplished by using hard mask 18 as the masking medium. Because either photomask 22 or hard mask 18 are in place during both the isotropic concave shape forming etch and the optional anisotropic etch to expose a surface upon substrate 12 , the anisotropic etch is self-aligning aligning to photomask 22 or hard mask 18 such that the hole formed by the anisotropic etch will be centered in the bottom of the concave storage container cell.
Following the optional anisotropic etch to expose substrate 12 , a doped polysilicon storage layer 24 is formed in such a way that the inside of the concave storage container cell is coated, and the upper surface of hard mask layer 18 is incidentally also coated. Removal of both hard mask 18 and that portion of polysilicon storage layer 24 covering hard mask layer 18 can be accomplished by one of the three methods disclosed above.
The eighteenth embodiment includes a single penetrating anisotropic etch of oxide layer 16 that contacts substrate 12 after formation of spacers 32 . There follows an isotropic etch that opens up the concave storage container cell. Formation of polysilicon storage layer 24 and removal of sacrificial portions thereof along with hard mask layer 18 , is followed by formations of cell dielectric 28 and cell plate polysilicon 30 .
The nineteenth and twentieth embodiments of the inventive method reflect the optional external surface area exposure of storage node 26 in the seventeenth and eighteenth embodiments of the inventive method by etching some of oxide layer 16 to lower its topographical profile as illustrated analogously in the exposed external lateral surfaces of storage node 26 in FIG. 7 .
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 illustrated and not restrictive. The scope of the invention is, therefore, indicated by the appended claims and their combination in whole or in part rather than by the foregoing description. All changes that come within the meaning and range of equivalency of the claims are to be embraced within their scope. | The present invention is directed to fabrication of a capacitor formed with a substantially concave shape and having optional folded or convoluted surfaces. The concave shape optimizes surface area within a small volume and thereby enables the capacitor to hold a significant charge so as to assist in increased miniaturization efforts in the microelectronic field. The capacitor is fabricated in microelectronic fashion consistent with a dense DRAM array. Methods of fabrication include stack building with storage nodes that extend above a semiconductor substrate surface. | 7 |
This application is a continuation-in-part of Ser. No. 07/622,586, now U.S. Pat. No. 5,088,555, which was filed on Dec. 3, 1990.
FIELD OF THE INVENTION
This invention relates to the consolidation of subterranean formations and, more particularly, to a method of introducing two consolidating fluids into a zone of an incompetent formation so as to form a silicate cement adjacent to a well penetrating the formation. The method of this invention is especially useful in promoting more uniform fluid injection patterns in a consolidated interval of the formation so as to tolerate high pH's and high temperatures when conducting a steam-flooding or fire-flooding enhanced oil recovery operation.
BACKGROUND OF THE INVENTION
It is well known in the art that wells in sandy, oil-bearing formations are frequently difficult to operate because the sand in the formation is poorly consolidated and tends to flow into the well with the oil. This "sand production" is a serious problem because the sand causes erosion and premature wearing out of the pumping equipment, and is a nuisance to remove from the oil at a later point in the production operation.
In some wells, particularly in the Saskatchewan area of Canada, oil with sand suspended therein must be pumped into large tanks for storage so that sand can settle out. Frequently, the oil can then only be removed from the upper half of the tank because the lower half of the tank is full of sand. This, too, must be removed at some time and pumped out. Moreover, fine sand is not always removed by this method and this causes substantial problems later in production operations which can lead to rejection of sand-bearing oil by the pipeline operator.
Also, removal of oil from tar sand formations is particularly challenging because high temperature steam with high pH is used. A suitable consolidating agent must withstand a similar harsh environment. In order to prevent caving around a wellbore and damage thereto, during the production of oil from a tar sand formation, it is often necessary to consolidate the formation.
Steam or fire stimulation recovery techniques ar used to increase production from viscous oil-bearing formations. In steam stimulation techniques, steam is used to heat a section of the formation adjacent to a wellbore so that production rates are increased through lowered oil viscosities.
In a typical conventional steam stimulation injection cycle, steam is injected into a desired section of a reservoir or formation. A shut-in or soak phase may follow, in which thermal energy diffuses through the formation. A production phase follows in which oil is produced until oil production rates decrease to an uneconomical amount. Subsequently, injection cycles are often used to increase recovery. During the production phase, sand flowing from a subsurface formation may leave therein a cavity which may result in caving of the formation and collapse of the casing.
Caving of the formation and collapsing of the casing is not peculiar to the production of oil from a reservoir by steam stimulation. It may also occur during a water-flooding, fire-flooding, or carbon dioxide stimulation oil recovery operation.
Therefore, what is needed is a method to consolidate a formation so as to prevent caving of an interval near the wellbore which interval requires stability to withstand high pH and high temperatures during a steam stimulation or thermal oil recovery process. Similarly, prevention of caving is also required during a water-flooding or carbon dioxide stimulation oil recovery operation.
SUMMARY OF THE INVENTION
This invention is directed to a method for consolidating sand in an unconsolidated or loosely consolidated oil or hydrocarbonaceous fluid containing formation or reservoir. In the practice of this invention, an aqueous organoammonium silicate, alkali metal or ammonium silicate solution is injected into an interval of the formation where sand consolidation is desired. The aqueous silicate solution enters the interval through perforations made in a cased well penetrating the formation. By use of a mechanical packer, penetration of the fluid into the interval can be controlled. As the aqueous silicate enters the interval, it saturates said interval.
Thereafter, a spacer volume of a water-immiscible hydrocarbonaceous liquid is directed into the interval. Hydrocarbonaceous liquids for use herein comprise parafinnic and aromatic liquids. Paraffinic liquids are preferred. Preferred parafinnic liquids are selected from a member of the group consisting of mineral oils, naphthas, C 5 -C 40 alkanes and mixtures thereof.
After a desired spacer volume of hydrocarbonaceous liquid has been placed into the interval requiring sand consolidation, a water-miscible organic solvent containing an alkylpolysilicate and hydrated calcium chloride is next injected into the interval. Upon coming into contact with the organoammonium silicate, alkali metal or ammonium silicate solution which remains on the sand grains and between the sand grain contact points, alkylpolysilicate and hydrated calcium chloride react with the organoammonium silicate, alkali metal or ammonium silicate to form calcium silicate cement in the interval being treated. The calcium silicate cement which is formed is stable at high pH's and temperatures in excess of about 400° F. These steps can be repeated until the interval has been consolidated to the extent desired.
Once the treated interval has been consolidated to a desired strength, a water-flooding, carbon dioxide stimulation, steam-flooding, or fire-flooding enhanced oil recovery method can be used to product hydrocarbonaceous fluids to the surface. By controlling the concentration and rate of injection of the aqueous silicate and the organic solvent containing the alkylpolysilicate and calcium chloride which are injected into the interval being treated, the consolidation strength of the formation can be tailored as desired.
It is therefore an object of this invention to provide for an in-situ calcium silicate composition for consolidating an interval of a formation which composition is more natural to a formation's environment.
It is another object of this invention to provide for a composition which will ensure an even flow front and a homogeneous consolidation of an interval of a formation requiring treatment.
It is yet another object of this invention to consolidate an unconsolidated or loosely consolidated interval in a formation to prevent caving and damage to an adjacent wellbore.
It is still yet further object of this invention to provide for a a method to obtain a desired consolidation within an interval of a formation which can be reversed by treating the interval with a strong acid.
It is an even still yet further object of this invention to provide for a formation consolidation agent which is resistant to high temperatures and high pH's.
It is yet an even still further object of this invention to provide for a consolidation composition lacking a particulate matter therein which matter might prevent penetration of the composition in an area requiring consolidation, flow alteration, or pore size reduction.
BRIEF DESCRIPTION OF THE DRAWING
The drawing is a schematic representation showing how the composition is injected into the formation so as to consolidate sand grains while maintaining the porosity of the formation.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In the practice of this invention, a shown in the drawing, an aqueous organoammonium silicate, alkali metal or ammonium silicate slug is injected into well 10 where it enters formation 12 via perforations 14. A method for perforating a wellbore is disclosed in U.S. Pat. No. 3,437,143 which issued to Cook on Apr. 8, 1969. This patent is hereby incorporated by reference herein. As the aqueous slug containing the organoammonium silicate, alkali metal or ammonium silicate proceeds through formation 12, it fills the pores in the formation.
As the aqueous organoammonium silicate, alkali metal or ammonium silicate solution proceeds through zone 12, it deposits a film of said aqueous silicate on sand grains therein. This aqueous silicate also fills intersitial spaces between the sand grains. A spacer volume of a water-immiscible hydrocarbonaceous liquid 16 is directed through zone 12 so as to remove excess aqueous silicate from the intersitial spaces while leaving sufficient aqueous silicate adhering filmwise to the sand grains. The hydrocarbonaceous liquid comprises paraffinic and aromatic hydrocarbons.
This spacer volume of water-immiscible hydrocarbonaceous liquid 16 is selected from a member of the group consisting of mineral oils naphthas, C 5 -C 40 alkanes and mixtures thereof. Hydrocarbonaceous liquid used as a spacer volume can be of an industrial grade. A spacer volume of hydrocarbonaceous liquid is used to remove excess aqueous silicate from between the sand grains while allowing a thin silicate film to remain on the surface to obtain a cementing reaction with a subsequently injected water-miscible organic solvent containing an alkylpolysilicate and hydrated calcium chloride.
Afterwards, a water-miscible organic solvent containing an alkylpolysilicate and hydrated calcium chloride mixture therein is injected into formation 12 where it forms in-situ a permeability retentive silicate cement which is stable to temperatures up to and in excess of about 500° F. Once the silicate cement has hardened and formation 12 has bee consolidated to the extent desired, by repeated applications if necessary, an EOR operation is initiated in formation 12.
The cementing reaction which takes place binds sand grains i the formation thereby forming a consolidated porous zone 22. Although the sand grains are consolidated, a cement is formed which results in a substantially high retention of the formation's permeability.
In order to increase the cement s consolidation strength, the concentration of the organoammonium silicate, alkali metal silicate or ammonium silicate contained in an aqueous slug or the alkylpolysilicate and hydrated calcium chloride contained in the organic solvent slug can be increased. Similarly, the flow rates of each of these slugs through the formation can be decreased to obtain better consolidation strength. A decreased flow rate is particularly beneficial for increasing the consolidation strength when the alkylpolysilicate and hydrated calcium chloride slug's flow rate is decreased. As will be understood by those skilled in the art, optimal concentrations and flow rates are formation dependent. Therefore, optimal concentrations and flow rates should be geared to field conditions and requirements.
Injection of aqueous organoammonium silicate, alkali metal or ammonium silicate slug and organic solvent slug 18 containing the alkylpolysilicate and hydrated calcium chloride can be continued until the formation has been consolidated to a strength sufficient to prevent caving and damage to the wellbore. As will be understood by those skilled in the art, the amount of components utilized is formation dependent and may vary from formation to formation. Core samples obtained from the interval to be treated can be tested to determine the required pore size and amount of cement needed. U.S. Pat. No. 4,549,608 which issued to Stowe et al. teaches a method of sand control where clay particles are stabilized along a face of a fracture. This patent is incorporated by reference herein.
After an interval of the formation has been consolidated, that interval or another adjacent to the wellbore can be perforated and an enhanced oil recovery method conducted therein. Steam-flooding processes which can be utilized when enhancing this sand consolidation process described herein are detailed in U.S. Pat. Nos. 4,489,783 and 3,918,521 which issued to Shu and Snavely, respectively. U.S. Pat. No. 4,479,894 that issued to Chen et al. describes a water-flooding process which may be used herein. Fire-flooding processes which can be utilized herein are disclosed in U.S. Pat. Nos. 4,440,227 and 4,669,542 which issued to Holmes and Venkatesan, respectively. These patents are hereby incorporated by reference herein.
A carbon dioxide EOR process which can be used after consolidating the higher permeability zone is disclosed in U.S. Pat. No. 4,513,821 which issued to W. R. Shu on Apr. 30, 1985. This patent is hereby incorporated by reference herein.
Organoammonium silicate, ammonium or alkali metal silicates having a SiO 2 /M 2 O molar ratio of about 0.5 to about 4 are suitable for forming a stable alkali silicate cement. The metal (M) which is utilized herein comprises sodium, potassium, or lithium. Preferably, the SiO 2 /M 2 O molar ratio is in the range of about greater than 2. The concentration of the silicate solution is about 10 to about 60 wt. percent, preferably 20 to about 50 wt. percent. As will be understood by those skilled in the art, the exact concentration should be determined for each application. In general, concentrated silicate solutions are more viscous and form a stronger consolidation due to a higher content of solids.
In those cases where it is not possible to control the viscosity of the silicate solution and preclude entry into a lower permeability zone, a mechanical packer may be used. The silicate cement which is formed can withstand pH's of 7 or more and temperatures up to and in excess of about 400° F. The preferred silicates are sodium, lithium and potassium. Potassium is preferred over sodium silicate because of its lower viscosity. Fumed silica, colloidal silica, or other alkali metal hydroxides can be added to modify the SiO 2 /M 2 O molar ratio of commercial silicate. Colloidal silicate can be used alone or suspended in alkali metal or ammonium silicate as a means of modifying silicate content, pH, and/or SiO 2 content. In a preferred embodiment, two parts of the aqueous silicate is mixed with one part colloidal silicate.
Organoammonium silicates which can be used in an aqueous solution include those that contain C 1 through C 8 alkyl or aryl groups and hetero atoms. Tetramethylammonium silicate is preferred.
Alkylpolysilicate (EPS) contained in the water-miscible organic solvent is the hydrolysis-condensation product of alkylorthosilicate according to the reaction equation below: ##STR1## where n≦2
R=C 1 -C 10
R should be ≦10 carbons for good solubility and high SiO 2 content.
Tetramethyl (TMS) or tetraethylorthosilicates (TEOS) are preferred. Mixed alkylorthosilicate can also be used. It is desirable to obtain an alkylpolysilicate with n>0.5, preferably n greater than 1. As n increases, the SiO 2 content increases, resulting in stronger consolidation. It is desirable to use an alkylpolysilicate with a silica content of 30% or more, preferably about 50%. EPS which is used herein is placed into a water-miscible organic solvent. The preferred solvent is ethanol. Of course, other alcohols can be used. EPS, TMS, TEOS, or other alkylpolysilicates are contained in the solvent in an amount of from about 10 to about 90 weight percent sufficient to react with the silicates contained in the aqueous solution. Although alcohol is the solvent preferred because of its versatility and availability, other water-miscible organic solvents can be utilized. These solvents include methanol and higher alcohols, glycols, ketones, tetrahydrofuran (THF), and dimethyl sulfoxide (DMSO).
Although ethanol is the preferred solvent, higher alcohols also can be utilized, as well as other solvents capable of dissolving alkylpolysilicates. The concentration of alkylpolysilicate should be in the range of about 10 to about 100 wt. percent, preferably 20 to about 80 wt. percent. Of course, enough alkylpolysilicate should be used to complete the reaction with the organoammonium silicate, alkali metal or ammonium silicate.
The calcium salt which can be used herein is one which is soluble in alcohol or the water-miscible organic solvent. Calcium chloride hydrate is preferred. However, chelated calcium forms can also be used. Higher alcohols also can be utilized, as well as other solvents capable of dissolving calcium salts and chelates. The concentration of calcium chloride hydrate should be in the range of about 10 to about 40 wt. percent, preferably 20 to about 30 wt. percent. Of course, enough EPS and calcium chloride solution should be used to complete the reaction with the aqueous silicate.
In another embodiment, calcium chloride can be used alone in the organic solvent to form a silicate cement in combination with EPS. Similarly, a spacer volume of hydrocarbonaceous liquid is used to separate the calcium chloride solution slug from the EPS organic solvent slug.
While hydrated calcium chloride is preferred, cations of other chlorides can be used. Other chlorides that can be used comprise titanium dichloride, zirconium chloride, aluminum chloride hydrate, ferrous chloride, and chromous chloride.
Although the present invention has been described with preferred embodiments, it is to be understood that modifications and variations may be resorted to without departing from the spirit and scope of this invention, as those skilled in the art readily understand. Such variations and modifications are considered to be within the purview and scope of the appended claims. | A sand consolidating method is provided for use in a borehole within an unconsolidated or loosely consolidated oil or gas reservoir which is likely to introduce substantial amounts of sand into the borehole and cause caving. After perforating the borehole's casing at an interval of the formation where sand will be produced, an aqueous silicate solution is injected into said interval. Next, a spacer volume of a water-immiscible hydrocarbonaceous liquid is introduced into the interval. Thereafter, a water-miscible organic solvent containing an alkylpolysilicate and inorganic salt or chelated calcium is injected into the interval. A permeability retentive silicate cement is formed in the interval. Injection of the aqueous silicate and organic solvent is continued until the interval has been consolidated by the silicate cement to an extent sufficient to prevent sand migration and thereby prevent caving. | 4 |
BACKGROUND OF THE INVENTION
The present invention relates generally to fluid infusion systems, and more particularly to an improved apparatus for detecting the formation of bubbles in such systems.
The infusing of fluids such as parenteral fluids and blood into the human body is usually accomplished by means of an administration set and metering apparatus which controls the rate of flow of fluid through the set. Peristaltic-type pumps, which function by repetitively compressing and expanding a section of tubing, have proven particularly attractive for use in such metering apparatus since they do not introduce the possibility of leakage or contamination into the system, while providing positive control of fluid flow through the system. One form of metering apparatus employing a peristaltic-type pump is described in U.S. Pat. No. 4,155,362, which issued to Thurman S. Jess on May 21, 1979, and is assigned to the present assignee. A successful commercial embodiment of this apparatus is currently marketed as the Travenol Model 2M014 infusion pump by Baxter Travenol Laboratories, Inc., of Deerfield, Illinois.
One problem which arises with the use of liquid infusion sets is that dissolved gases in the liquid being infused may be released as bubbles as the liquid is subjected to pressure and/or temperature changes as it passes through the pump of the metering apparatus. These bubbles may coalesce and form larger bubbles or pockets of gas which may be infused along with the liquid into the body, an occurence which may be harmful or even fatal to the patient under certain circumstances.
To prevent gas from being infused it has become common practice to locate a bubble detector downline of the metering apparatus pump to automatically stop the apparatus should gas bubbles be detected. Such sensors typically employ a light source and a light detector positioned on opposite sides of the administration set tubing to monitor the level of light transmitted through the tubing. Operation of the metering apparatus is interrupted and an alarm is sounded when the transmitted light level falls below a predetermined level. To this end, the lens effect of the fluid in the lumen of the tubing may be employed to enhance the difference in transmission levels between fluid and no fluid conditions.
One problem encountered with such bubble detectors is that fluid pressure changes in the tubing of the administration set such as may result from the use of a downline flow restriction, as in the Travenol Model 2M8014 infusion pump may deform the wall of the tubing from its unstressed shape and diminish the lens effect. This has the potential of diminishing the reliability and sensitivity of the bubble detector. The present invention is directed to a bubble detector which is not subject to such variations in effectiveness as a result of changes in fluid pressure.
Accordingly, it is a general object of the present invention to provide a new and improved bubble detector.
It is another object of the present invention to provide a new and improved bubble detector wherein means are provided for preventing deformation of the tubing wall as a result of internal fluid pressure.
It is a further object of the present invention to provide a new and improved bubble detector suitable for use with vinyl tubing or the like subject to deformation from internal fluid pressure.
SUMMARY OF THE INVENTION
The invention is directed to a flow metering apparatus for controlling the flow of fluids through an administration set of the type having transparent tubing subject to deformation from internal fluid pressure. The apparatus includes a bubble detector comprising a light source arranged at one side of the tubing, and a light detector generally arranged at the opposite side of the tubing opposite the light source and defining a light path through the tubing. The detector generates an output signal in response to the intensity of light from the light source transmitted through the tubing, the intensity of the transmitted light being dependent on the presence of fluid within the lumen of the tubing and on the shape of the lumen between the source and the detector. Control circuit means responsive to the output signal are provided for interrupting operation of the flow metering apparatus upon the intensity of the transmitted light falling below a predetermined minimum level. Platen means including at least one forming member engaging the tubing about a substantial portion of its circumference adjacent the light path are provided for preventing deformation of the tubing and consequent changes in the intensity of the transmitted light with fluid pressure changes in the lumen of the tubing.
The invention is further directed to a flow system for infusing fluid from a reservoir into the human body. The system comprises a length of transparent tubing subject to deformation from internal fluid pressure. Metering means operatively engaging the tubing are provided for urging fluid through the tubing at a predetermined rate. The system further includes a light source arranged at one side of the tubing downline of the metering means, and a light detector generally arranged at the opposite side of the tubing opposite the light source and defining a light path through the tubing, the detector generating an output signal in response to the intensity of light from the light source transmitted through the tubing, the intensity of the transmitted light being dependent on the presence of fluid within the lumen of the tubing and on the shape of the lumen between the source and the detector. Control circuit means responsive to the output signal are provided for interrupting operation of the metering means upon the intensity of the transmitted light falling below a predetermined minimum level. Platen means including at least one forming member engaging the tubing about a substantial proportion of the circumference of the tubing adjacent the light path are provided for preventing deformation of the tubing and consequent changes in the intensity of the transmitted light with fluid pressure changes in the lumen of the tubing.
BRIEF DESCRIPTION OF THE DRAWINGS
The features of the present invention which are believed to be novel are set forth with particularity in the appended claims. The invention, together with the further objects and advantages thereof, may best be understood by reference to the following description taken in conjunction with the accompanying drawings, and the several figures of which like reference numerals identify like elements, and in which:
FIG. 1 is a perspective view of a metering apparatus incorporating a bubble detector constructed in accordance with the invention.
FIG. 2 is an enlarged front elevational view of the metering station of the flow metering apparatus partially in section and partially broken away to illustrate the operation thereof.
FIG. 3 is a cross-sectional veiw of the metering station taken along line 3--3 of FIG. 2.
FIG. 4 is an elongated front elevational view of the bubble detector head of the metering station.
FIG. 5 is a cross-sectional view of the bubble detector head taken along line 5--5 of FIG. 4.
FIG. 6 is an exploded perspective view of the bubble detector head showing the principal components thereof.
FIG. 7(A) is a diagramatic depiction of the bubble detector head useful in depicting operation of the bubble detector in the absence of fluid.
FIG. 7(B) is a diagramatic depiction similar to FIG. 7(A) showing operation of the bubble detector with fluid present.
FIG. 8(A) is a simplified diagramatic depiction of a prior art bubble detector head illustrating the effect of deformation of the tubing wall on the operation of the bubble detector.
FIG. 8(B) is a simplified diagramatic depiction of the flow detector head of the invention useful in understanding the operation thereof.
FIG. 9 is a simplified functional block diagram of the control system of the metering apparatus of FIG. 1.
FIG. 10 is a simplified schematic diagram of a preferred detector circuit for use in conjunction with the bubble detector of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the figures, and particularly to FIG. 1, a peristaltic-type flow metering apparatus 10 for use in conjunction with an administration set for controlling the flow of fluid into a vein or artery includes a generally rectangular housing 12 having a handle 13 at one end thereof for convenient carrying. The front surface of the housing includes a control panel 14 which allows the operator to control and monitor the operation of the metering apparatus, and a peristaltic-type flow metering head 15 for compressing a section of tubing 16 of the administration set to effect control of fluid flow therein. A channel 17 is provided above the metering head 15 for maintaining a portion of the tubing segment in convenient view of the operator whereby flow irregularities can be more readily observed.
The administration set, of which tubing segment 16 is a part, and which may be conventional in design and construction, is preferably formed of a plastic material such as vinyl and packaged in a sterile and non-pyrogenic condition. To avoid the danger of contamination, the administration set is normally utilized for one application only, and is disposed of after a single use.
The operating mode of metering apparatus 10 is controlled by means of a push button STOP switch 20, a push button START switch 21, and a push button power ON-OFF switch 22. Each of these push button switches includes an internal indicator lamp which provides a positive indication of the operation of the operating mode of the apparatus. Various abnormal operating conditions are annunciated by means of indicator lights 23 contained on the control panel to the left (as viewed in FIG. 1) of the mode control push buttons.
Control panel 14 further includes a digital display 30 of volume infused, a digital display 31 of volume to be infused, and a digital display 32 of the fluid flow rate. The volume displayed by display 30 is the volume of fluid actually infused, and can be reset to zero by the operator by means of a push button RESET switch 33. The volume to be infused by display 31 is preset by the operator by means of a set of push button switches 34 to indicate a desired volume of fluid to be infused. Similarly, the infusion rate display 32 is preset by the operator by means of a second set of push button switches 35 to indicate the rate at which infusion is to take place.
The operation of the various indicators, control switches and other features of metering apparatus 10 is described in detail in the copending applications of Thurman S. Jess and Norm Shim, Ser. No. 856,863; Norm Shim, Ser. No. 857,018; Norm Shim and Vincent L. Knigge, Ser. No. 856,927; and Thurman S. Jess, Ser. No. 856,926; all filed Dec. 2, 1977.
Referring to FIGS. 2 and 3, the peristaltic metering head 15 includes a rotor 40 having four pressure rollers 41 disposed in equi-spaced relation about its circumference. The rollers are each mounted on a shaft 42 for free rotation, and the shafts are carried on carriages 43 and constrained to radial movement by respective radial slots 44. Each carriage is mounted for reciprocation within a radial recess 45 and spring loaded radially outward by a helical spring 46 disposed within the recess.
The pump also includes a pressure plate 50 having an arcuate working surface 51 which substantially corresponds in shape to the circumference of rotor 40. The working surface brings tubing 16 into compressive engagement with rollers 41 around at least a portion of the rotor circumference corresponding to the spacing between adjacent rollers. The pressure plate may be reciprocated toward and away from rotor 40 to facilitate installation and removal of tubing 16 by rotation of an eccentric cam 52, which is constrained to operate within a vertical slot 53 provided on the pressure plate. Rotation of the cam is accomplished by a shaft 54 and a user-actuable lever 55 operatively connected to the cam. When the lever 55 is in its vertical position, as shown in FIG. 3, the pressure plate is moved sufficiently close to the rotor circumference to cause tubing 16 to be completely occluded by one of the pressure rollers 41.
After passing through metering station 15, tubing 16 extends between a light source 60 and a photodetector 61, which together comprise a bubble detector head 62. This head, combined with asssociated control circuitry forms a bubble detector system which discontinues operation of the metering apparatus and alerts the operator upon formation of a bubble in the tubing.
The tubing next passes through a flow restriction station 63. This station includes a pressure block 66 and a slidably mounted plunger 67 biased against the sidewall of tubing segment 16. The end of plunger 67 which engages the tubing segment includes a generally L-shaped head portion 68 having a wedge-shaped working surface 70 which occludes the tubing and a generally flat control surface 71 which responds to fluid pressure changes. Plunger 67 is slidably received within a mounting block 73, and extends through the center of a helical compression spring 74 which biases head 68 into engagement with the tubing. The occlusion of the tubing by the flow restriction station increases the pressure of the fluid in the tubing at the point of engagement of the rollers 41 of rotor 40 to assist in restoration of the tubing following compression by the pressure rollers for improved metering accuracy.
Plunger 67 can be opened to facilitate loading or unloading of tubing 16 by means of a lever 76. The plunger is locked open by means of a latch member 77 which is pivotally mounted at 78 to pressure plate 50 and biased by a helical spring 79 for operation within a plane perpendicular to the plunger. Latch member 77 is received in a slot 80 on the plunger when the plunger is moved to its full open position.
To insure that plunger 67 will be released when pressure plate 50 is subsequently closed, an actuator pin 82 having a tapered end surface displaces latch member 77 from slot 80 when the pressure plate is returned to its closed position by rotation of knob 55. This prevents inadvertent operation of the system without the back pressure and gravity flow protection provided by the plunger. Also, when the pressure plate is opened, the displacement of latching member 77 prevents the plunger from being latched open.
In accordance with the invention, metering apparatus 10 includes a bubble detector head 62 which renders the bubble detector system of the apparatus immune to variations in fluid pressure in tubing 16. Referring to FIG. 4, the bubble detector head is seen to comprise first and second forming members 90 and 91 disposed on opposite sides of tubing 16. The first form member 90 is secured to housing 12 by a bolt 93, extending through a flange portion 92. Similarly, the second form member 91 is secured to the slidable pressure plate 50 by means of a bolt 94 extending through a flange portion 95 of the base member.
To provide mounting means for light source 60, the first form member 90 is provided with a bore 96 perpendicularly aligned to the axis of tubing 16. To provide a receptacle for photodetector 61, form member 91 is similarly provided with a perpendicularly aligned bore 97. Bores 96 and 97 are each dimensioned with an inside diameter just slightly larger than the outside diameter of light source 96 and photodetector 97, respectively, to provide a fit for these elements sufficiently tight to maintain the elements in alignment.
It will be noted that form members 90 and 91 define inwardly concave mandrel surfaces 98 and 99, respectively, between which tubing 16 is held when the form elements 90 and 91 are in their closed position, as shown in FIGS. 4 and 5. The curvature of these mandrel surfaces is dimensioned to correspond closely to the natural or unstressed curvature of the outside surface of tubing 16 so that when the tubing is engaged to the form members the tubing lumen is maintained in its unstressed cross-sectional shape notwithstanding pressure changes in the fluid contained therein.
To remove the tubing, it is merely necessary to separate form members 90 and 91, as shown in FIG. 6. In metering apparatus 10, this is accomplished automatically upon the operator actuating knob 55 to open metering station 15, since form member 90 is mounted to a stationary housing member, and form member 91 is mounted to the movable pressure plate 50.
To illustrate the benefit of maintaining the cross-section of tubing 16 constant, reference is made to FIGS. 7(A) and 7(B) which illustrate the lens effect upon which the detector depends. In FIG. 7(A) no fluid is present in the lumen of tubing 16, and light from light source 60 diverges as it passes through the transparent walls of the tubing. As a result, only a small portion of the light transmitted through the tubing actually falls upon light detector 61, and the resulting signal produced by that device is small. In contrast, when liquid is present in the lumen of the tubing as shown in FIG. 7(B), the circular cross-section of the fluid mass, as defined by the inner surface of the wall of tubing 16, forms a lens which focuses the light on detector 61. As a result, a greater portion of the transmitted light is actually incident on the detector and the resulting detector output signal is stronger. By comparing the light detector output signals for the conditions shown in FIGS. 7(A) and 7(B), appropriate bubble detector circuitry within metering apparatus 10 determines the presence or absence of fluid in the tubing.
Referring to FIG. 8(A), in prior art bubble detectors no provision was made for maintaining the tubing in constant cross-section. As a result, as the pressure of the fluid in the tubing lumen increased the walls of the tubing became deformed. This caused the light from light source 60 to be only partially focused on light detector 61, so that the output signal developed by that device was weaker than the signal would have been had the distortion not taken place. As a result, the capability of the bubble detector to distinguish between liquid and no liquid conditions was diminished.
As shown in FIG. 8(B), the invention overcomes this deficiency by maintaining tubing 16 in constant cross-section regardless of pressure variations in fluid in the tubing lumen. The light from light source 60 continues to be focused on light detector 61 and an optimum output signal is developed for maximum capability in distinguishing between fluid present and fluid absent conditions.
The output of light detector 61 is applied to appropriate bubble detector circuitry wherein it is utilized to develop a control signal suitable for controlling the operation of the metering apparatus. Referring to FIG. 9, in the present embodiment the output of light detector 61 is applied to a bubble detector circuit 100 wherein a control signal is developed indicative of the presence or absence of fluid in tubing segment 16. This control signal is applied to one input of an AND gate 101, wherein it serves to control the application of control pulses to the motor drive circuit 102 of a stepper motor 103, which is utilized to drive the peristaltic rotor 40 of the apparatus.
Control pulses for drive circuit 102 are obtained from a pulse source in the form of a clock 104. The clock pulses are divided to a lower frequency by a variable-rate divider 105, and applied through AND gate 101 to the motor drive circuit. The division factor of rate divider 105 is selected by the operator to obtain a desired rate. The pulses derived from divider 105 are also applied to a volume register 106 wherein they are counted for use by volume display 30. The divided pulses are also applied to a bi-directional register 107 which supplies an inhibit signal to AND gate 101 upon the desired volume having been infused. The counting state of this register is displayed by display 31.
Referring to FIG. 10, a preferred bubble detector circuit 61 may comprise a multi-vibrator 111 consisting of three NAND gates 112, 113 and 114. A capacitor 115 connected to the output of gate 113 and a potentiometer 116 connected to the output of gate 114 provide an RC time constant which determines the frequency of the multi-vibrator output signal in a manner well known to the art. A diode 117 is connected between the arm of potentiometer 116 and the output of gate 114 to vary the duty cycle of the oscillator output signal. A fixed resistance 118 connected in series with the body of potentiometer 116 provides a desired adjustment range.
The AC signal generated by multi-vibrator 111 is applied through a resistance 119 and transistor 120 to light source 60. The AC signal developed by multi-vibrator 111 is amplified by transistor 120 and utilized to drive the LED, causing the LED to produce a light output which varies at a rate dependent on the output frequency of the multi-vibrator.
The alternating light developed by the LED is converted by phototransistor detector 122 to an output signal indicative of the strength of the transmitted light. The emitter of transistor 123 is connected to ground through a resistor 124, and is connected through respective diodes 125-127 to respective inputs of a threshold trigger device in the form of a dual Schmidt trigger 128. The cathodes of diodes 125-127 are connected to ground by respective parallel combinations of capacitors 130-132 and resistors 133-135. These elements serve in conjunction with the diodes as alternating current detectors, generating a DC signal at the inputs of trigger 128 dependent on the amplitude of the AC signal produced by detector 61. The dual Schmitt trigger 128, which may be a commercially available component such as the type NC14583B Schmitt trigger marketed by Motorola, Inc., of Schaumburg, Ill., produces an output upon reduction of either of its input signals falling below a predetermined threshold level. The input associated with diode 125 functions as an enabling input for both triggers. The outputs of Schmidt triggers 128, which comprise a first control signal, are applied to one input of a logic OR gate 129.
The emitter of transistor 123 is also connected to ground through series-connected resistors 136 and 137. The signal developed at the junction of these two resistors is filtered by a series-connected resistor 138 and a short-connected capacitor 139 and resistor 140 connected to ground. This forms a second control signal, which is applied to the remaining input of OR gate 129. In this way, OR gate 129 is provided with the output signal developed by the dual Schmitt trigger 128, and with the DC control signal developed across capacitor 139, either of which can result in an output from the gate in the event of the occurence of a bubble in tubing 16. The output of Schmitt triggers 128 and the output of OR gate 129 are also connected to the positive unidirectional current source of the system by respective resistors 143 and 144.
Since the output of OR gate 129 is dependent on both the amplitude of the AC signal as rectified and applied to the parallel-connected Schmitt triggers 128, and on the DC signal developed across capacitor 139, the bubble detector utilized in the metering apparatus provides two control channels. The first channel, which utilizes Schmitt triggers 128, establishes a highly precise threshold below which an alarm output is produced. The second channel, which depends only on the input characteristic of gate 129, serves to provide an alarm output in event of failure of resistor 124 in the photodetector bias circuit.
In order for bubble detector 62 to not provide an output, it is necessary that the DC signals applied to the Schmitt triggers as a result of rectification by diodes 126 and 127 be above a predetermined minimum level, which is possible only when there is fluid within tubing segment to provide a lens to direct light from light source 60 to light detector 61.
While a particular embodiment of the invention has been shown and described, it will be obvious to those skilled in the art that changes and modifications may be made therein without departing from the invention in its broader aspects, and, therefore, the aim in the appended claims is to cover all such changes and modifications as fall within the true spirit and scope of the invention. | In a flow metering apparatus a bubble detector for detecting bubble formation in tubing subject to deformation from internal fluid pressure includes a light source and a light detector. The light detector is positioned on the opposite side of the tubing from the light source such that the light transmitted through the tubing to the detector is dependent on the presence of fluid in the tubing and on the shape of the lumen of the tubing. A control circuit responsive to the output of the detector interrupts operation of the metering apparatus when the light transmitted through the tubing falls below a predetermined minimum level. False interruptions resulting from deformation of the tubing by pressure changes in the fluid are prevented by forming members which engage the wall of the tubing adjacent the light source and light detector. | 0 |
CROSS-REFERENCE TO RELATED APPLICATIONS
Continuation of U.S. patent application Ser. No. 12/786,456 filed on May 25, 2010, now U.S. Pat. No. 8,413,722, and incorporated herein by reference in its entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable.
BACKGROUND
This disclosure relates generally to the field of drilling wellbores through subsurface rock formations. More particularly, the disclosure relates to method for removing fluid that has entered the wellbore from subsurface formations outside the wellbore.
Drilling wellbores through subsurface rock formations includes inserting a drill string into the wellbore. The drill string, which is typically assembled by segments (“joints” or “stands”) of pipe threadedly coupled end to end) has a bit at its lower end. The drill string is suspended in a hoist unit that forms part of a drilling “rig.” During drilling, a specialized fluid (“mud”) is pumped from a tank into a passage in the interior of the drill string and is discharged through courses or nozzles on the bit. The mud cools and lubricates the bit and lifts drill cuttings to the surface for treatment and disposal. The mud also typically includes high density particles such as barite (barium sulfate), hematite (iron oxide), or other weighting agents suspended therein to cause the mud to have a selected density. The density is selected to provide sufficient hydrostatic pressure in the wellbore to prevent fluid in the pore spaces of the rock formations from entering the wellbore. The density is also selected to maintain mechanical integrity of the wellbore.
Wellbores drilled through subsurface formations below the bottom of a body of water, particularly if the water is very deep (e.g., on the order of 1,000-3,000 meters or more) may require special equipment for effective drilling. An example drilling system for such water depths is shown in FIG. 1 . The drill string 28 extends from a drilling rig (not shown for clarity) and is disposed in a wellbore 14 being drilled through rock formations 12 below the bottom of a body of water 10 such as a lake or the ocean. A wellhead 16 including a plurality of sealing devices collectively called a “BOP stack” is disposed at the top end of a surface casing 14 A cemented in place to a relatively shallow depth below the mud line. A marine riser 26 extends from the upper part of the wellhead 20 to the drilling rig (not shown). The riser 26 usually has auxiliary lines associated with it known as “choke” lines 24 , and a “kill line” 22 . Fluid may be pumped into such lines from the rig (not shown) toward the wellbore 14 or may be allowed to move from the wellbore 14 toward the surface. Valves 18 , 20 control fluid movement at the lower end of the kill line 22 . Corresponding valves 30 , 32 control fluid movement at the lower end of the choke line 24 .
In the present example, the riser 26 is hydraulically opened to the wellbore 14 below. In order to maintain a hydrostatic pressure in the wellbore annulus 13 that is lower than would be provided if the entire length of the riser 26 were filled with mud, the riser 26 may be partially or totally filled with sea water. See, for example, U.S. Pat. No. 6,454,022 issued to Sangesland et al. As the mud leaves the wellbore annulus 13 (the space between the drill string and the wellbore wall), it is diverted, through suitable valves 34 , 36 to a pump 38 that lifts the mud to the surface through a separate mud return line 40 . Typically, the pump 38 is operated so that the interface between the drilling mud and the water column above in the riser 26 is maintained at a selected level. Maintaining the selected level causes a selected hydrostatic pressure to be maintained in the wellbore 14 .
The issue dealt with by methods according to the present invention is to safely remove from the wellbore 14 any fluid which enters from the rock formations 12 . Such fluid, by reason of its entry, is at a higher pressure than the total hydrostatic pressure exerted by the mud column in the annulus 13 and the column of sea water in the riser 26 . Methods known in the art for dealing with such fluid entry require “shutting in the well”, meaning that the BOP stack is closed to seal against the drill string 28 , and fluid pumping is stopped. Frequently during such operation, the density of the drilling fluid will be increased by adding more dense, powdered material to the mud. See for example U.S. Pat. No. 6,474,422 issued to Schubert et al. for an example of a kick control method.
It is also possible that the pressures necessary to be applied to the mud return pump and its connecting lines may be exceeded if conventional kick control methods are used.
It is desirable to have a method for removing kick fluid from a wellbore that does not require the kick fluid to go through the pump, but maintains well bore pressures at acceptable levels. These pressures must be high enough to keep additional formation fluids from entering the wellbore from one formation, while not exceeding the fracture pressure (pressure that cases wellbore fluids to enter the formation) of other exposed formations, most specifically the formation at the last casing shoe, which is the end of the last installed casing.
SUMMARY
One aspect of the disclosure is a method for removing a fluid influx from a wellbore. The wellbore is drilled using a drill string having an internal passage therethrough. The wellbore has a wellhead disposed proximate a bottom of a body of water disposed thereabove. A fluid outlet of the wellbore is coupled to an inlet of a mud return pump. An outlet of the return pump is coupled to a return line to the water surface. A riser is disposed above the wellhead and extends to the water surface. The riser is substantially or partially filled with a fluid less dense than a fluid pumped through the drill string. The method includes detecting the influx when a rate of the return pump increases. Flow out from the well is diverted from the return pump inlet to a choke line when the influx reaches the wellhead. A choke in the choke line is operated so that a substantially constant bottom hole pressure is maintained while drilling fluid continues to be pumped through the drill string. Fluid flow from the well is rediverted to the return pump inlet when the influx has substantially left the wellbore.
In one example, an interface level in the riser between the less dense fluid and the fluid pumped through the drill string is then increased to increase fluid pressure at the bottom of the well. A method according to one aspect of the invention for removing a fluid influx from a subsea drilling wellbore drilled using a pump to return drilling fluid from the wellbore to the sea surface. The fluid influx is observed when an operating rate of the return pump increases. Drilling fluid continues to be pumped through the drill string and the return pump until the fluid influx reaches the wellhead. The return pumping is performed at a rate such that a flow into the wellbore substantially equals a flow out of the wellbore. An intake to the return pump is hydraulically isolated from the wellbore. Flow out of the wellbore is diverted to a choke line. The choke is operated so that the flow into the wellbore substantially equals a flow out of the wellbore. Flow out of the wellbore back to the intake of the return pump when an end of the influx reaches the wellhead. The less dense fluid is pumped down an auxiliary line proximate a bottom end thereof to proximate a bottom end of the choke line. Influx fluid is displaced from the choke line using the less dense fluid.
In one example, drilling fluid is pumped down the auxiliary line into a lower end of the riser to raise an interface level between drilling fluid and less dense fluid in a riser above the wellhead such that a fluid pressure at the bottom of the well is at least as much as fluid pressure in rock formations penetrated by the wellbore.
Other aspects and advantages of the invention will be apparent from the following description and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an example prior art mud lift drilling system.
FIGS. 2-15 show various elements of a method according to the invention that can be performed using the system shown in FIG. 1 . In the various figures, like components will be identified using like reference numerals.
DETAILED DESCRIPTION
A well control procedure described herein will enable circulating out a fluid influx (“kick”) from a rock formation when drilling in dual gradient mode through a line auxiliary to a drilling riser, such as a choke line. The procedure is dynamic and never exposes the wellbore to a complete column of drilling mud from the bottom of the well to the surface (in the riser). Such a mud column could exert enough hydrostatic pressure to fracture the formations exposed by the wellbore.
FIG. 1 , as explained in the Background section herein, represents drilling under normal conditions, wherein no fluid enters the wellbore from any formation exposed by the wellbore. When drilling is under normal conditions, the drilling system may be configured as shown in FIG. 1 , specifically, the riser 26 and choke and kill (“C&K”) lines are filled with seawater. The C&K lines are isolated from the wellbore 14 by keeping its lower control valves 18 , 20 , 30 , 32 closed. The pump inlet valves 34 , 36 are open and the pump 38 is operated to lift drilling mud to the surface. A pump suction pressure sensor SPP measures annulus discharge pressure, typically proximate the intake of the pump 38 . The pressure sensor SPP as well as other pressure sensors described below may be coupled to a controller (not shown) for automatic or semi-automatic control over various components of the system. Alternatively, measurements made by the sensors may be communicated to the system operator for manual operation. Operation of the pump 38 is typically maintained automatically at a set point pressure as measured by the sensor SPP, which operation keeps the mud/seawater interface in the riser 26 at a constant level. The riser 26 is open to wellbore 14 as explained in the Background section herein, and includes sea water therein above the interface. The sea water may extend all the way to the surface or to a selected depth below the surface.
FIG. 2 shows an example ten barrel volume fluid influx (“kick”) 50 entering the wellbore. Such a kick fills about 100 meters of the wellbore with kick fluid, although the length of the wellbore filled by any particular kick will depend, as is known in the art, on the actual volume of the kick, the diameter of the drill string and the diameter of the wellbore. It can be observed that the pump 38 speed and horsepower output will increase in response in order to move the extra fluid volume resulting from the fluid influx (kick). The system operator may determine from observation of the pump speed and/or power measured by sensors that a kick has entered the well. Generally, the pump speed and/or power measurement increases due to the kick 50 because the pump 38 response to the extra fluid volume. As the kick enters the wellbore it may cause movement of the mud/seawater interface in the riser upward; this will have the effect of increasing the SPP reading (more mud, less water in the riser). However, the control program, having sensed this increase in pressure will speed the pump 38 up and restore the level to what is was (the level only changes an inch or two) prior to the kick, This will then restore SPP back to what it was. Once it is observed that a kick is occurring from the change in pump speed and/or power the SPP setpoint may be changed to increase pressure. This has the effect of slowing the pump 38 so that it supports less of the column of fluid in the mud return line adding pressure to the bottom the well and killing the kick. It should be understood that observing the increase in pump speed is only one technique for observing an influx. It is also possible to include a flow meter at a selected position in the mud return line and observe an increase in flow rate. Other techniques for observing the influx will occur to those skilled in the art.
FIG. 3 shows an initial action in controlling and circulating out the kick 50 . An annular preventer (not shown separately) in the BOP stack 16 is closed around the drill string, thereby isolating the wellbore 14 from the riser 26 . The suction set point pressure may be increased to control the kick 50 . This can be performed by slowing the operating rate of the pump 38 . The pump rate is slowed, and the suction pressure (as measured by the sensor SPP) is increased until the flow rate of mud into well (“flow in”—pumped through the drill string 28 and the rate of flow out of well (“flow out”—through the return line 40 ) are substantially equal. When the flow in and the flow out are substantially equal, no additional fluid is entering well. At such condition, the kick 50 has been stopped or “killed.” It is then necessary to circulate the kick fluid out of the wellbore 14 in a controlled manner. Kick fluid frequently contains gas, in solution and/or as actual bubbles. As the kick fluid moves toward the surface, and hydrostatic pressure is reduced, the gas exsolves from the kick fluid and/or expands in volume. When the flow rates in and out are balanced, the drill string pressure increases, which may be observed by measurements made using a drill string pressure sensor DPP.
FIG. 4 shows the situation where the rig mud pump (the pump that moves mud through the interior of the drill string) rate is slowed, but the rate is sufficient to keep the drill string full of mud. The kick fluid begins moving up wellbore annulus 13 . At this point, the mud return pump 38 is operated so that the intake pressure (measured by the sensor SPP) is increased to maintain a constant drill pipe pressure (as measured by sensor DPP). The mud return pump 38 should be operated to maintain fluid flow out equal to fluid flow in.
FIG. 5 shows the kick fluid moving up the wellbore and beginning to expand in volume. During such time, the operator continues to control the mud return pump 38 speed so to maintain constant drill string pressure (measured by sensor DPP) and to cause flow out to be substantially equal to flow in.
FIG. 6 shows continuing to adjust the mud return pump 38 speed to keep constant drill string pressure. The mud return pump 38 speed is also controlled to maintain flow out matching flow in. At the point shown in FIG. 6 , the kick fluid 50 has reached the BOP stack 16 .
FIG. 7 shows opening the valves 30 , 32 to the choke line 24 . A variable orifice choke 44 coupled to the surface end of the choke line 24 is operated to maintain fluid pressure at the bottom of the wellbore (bottom hole pressure) substantially constant. Bottom hole pressure may be measured by a sensor (not shown) in the drill string, or may be estimated using the density of the drilling mud, and an hydraulic model that describes the flow system including the drill bit, wellbore walls, drill string and rheological properties of the mud.
When the valves 30 , 32 to the choke line 24 are opened, the valves 34 , 36 to the intake side of the mud return pump 38 are closed. Thus, further flow out of the wellbore 14 will move up the choke line 24 . When the pump intake valves 34 , 36 are closed, the mud return pump 38 is stopped. It may be necessary that the flow rate into the well will have to be reduced to avoid excess pressure from friction of the fluid in the smaller choke line 24 .
FIG. 8 shows that the kick fluid 50 is less dense than the mud and seawater, and thus displaces the sea water in the choke line 24 . The surface choke 44 continues to be operated to keep the bottom hole pressure substantially constant. Note that the foregoing is correct for water based drilling fluid. If oil based drilling fluid is used, the oil based fluid will be very close to its original density because any gas will be dissolved in the oil based fluid. Reduction of fluid density will not occur until exsolution of the gas. When this actually takes place varies depending on wellbore conditions.
FIG. 9 shows that while the kick volume at the bottom of the wellbore was ten barrels, the kick will expand substantially as the kick moves up the choke line 24 to the surface. The choke line 24 unit volume in the present example 0.0197 bbl/ft. Thus, in a system in 10,000 feet water depth, the total choke line volume is 197 barrels.
FIG. 10 shows the surface choke 44 being operated to keep bottom hole pressure constant as the kick fluid is discharged through the choke 44 . A typical indication that bottom hole pressure is constant is a constant drill string pressure (as shown by sensor DPP).
FIG. 11 shows restarting the mud return pump 38 . The valves 34 , 36 to the mud return pump 38 inlet are opened, and the valves 30 , 32 to the choke line 24 are also open. The intake pressure set point on the mud return pump 38 , measured by sensor SPP, is set to match the existing pressure at the mud return pump 38 intake The valves 30 , 32 to the choke line 24 are then closed.
FIG. 12 shows connecting one of the other auxiliary lines, e.g., the kill line 22 to the choke line 24 using bypass lines or internal passages the BOP stack 16 . The valves 30 , 32 at the base of the choke line and the kill line 18 , 20 are then opened. Sea water is pumped from the surface down the kill line 22 , back up the choke line 24 . Such pumping displaces the kick fluid 50 from the choke line 24 .
FIG. 13 shows that once kick fluid 50 is fully displaced from the choke line 24 , the well choke pressure (which may be measured by sensor CK) is zero. At this point any connection between the boost line 22 and the choke line 24 may be removed or closed. The wellbore 24 is then returned to regular drilling control by the following procedure, which takes into account the higher fluid pressure in the rock formation from which the kick originated.
FIG. 14 shows pumping mud through the boost line (not shown). The boost line is placed in hydraulic communication with the lower end of the riser 26 . Pumping continues down the boost line until the fluid pressure at the bottom of the riser 26 equals the pressure in the wellbore existing at the BOP stack 16 . This pressure is the existing pressure (measured by the sensor SPP) at the mud return pump 38 intake.
FIG. 15 shows the annular preventer being opened, the choke line 24 valves 30 , 32 and the kill line 22 valves 18 , 20 being closed, and normal drilling resuming with a new fluid level interface in the riser 26 . The new fluid interface level in the riser 26 , being higher than the interface level shown in FIG. 1 , provides a greater bottom hole pressure than with the interface as shown in FIG. 1 . Thus, formations having higher fluid pressure may be safely drilled without fluid entry into the wellbore 14 .
It will be appreciated by those skilled in the art that the foregoing method may also be used when no riser connects the wellhead to the drilling unit. In such examples, the wellhead may have affixed to the top thereof a rotating diverter, rotating BOP or rotating control head that directs fluid from the annular space surrounding the drill string 28 to the pump 38 intake. The intake pressure of the pump SPP will be adjusted for the lack of a column of liquid applied to the wellbore annulus in “riserless” configurations. The principle of operation of the method is substantially the same for the riser version shown and explained with reference to the figures as it is in riserless configurations.
A method according to the invention may enable safe control of fluid influx into a wellbore being drilled without the need to shut in the wellbore and without the need to increase the density of drilling mud to prevent further fluid influx.
While the invention has been described with respect to a limited number of embodiments, those skilled in the art, having benefit of this disclosure, will appreciate that other embodiments can be devised which do not depart from the scope of the invention as disclosed herein. Accordingly, the scope of the invention should be limited only by the attached claims. | A method for removing a fluid influx from a subsea wellbore drilled using a pump to return fluid from the wellbore to the surface. The method includes detecting the influx when a rate of the return pump increases. Flow from the wellbore is diverted from the return pump to a choke line when the influx reaches the wellhead. A choke in the choke line is operated so that a substantially constant bottom hold pressure is maintained while drilling fluid continues to be pumped through the drill sgring. Fluid flow from the wellbore is redirected to the return pump inlet when the influx has substantially left the well. | 4 |
TECHNICAL FIELD
Invention relates to security devices for cabinet drawers and doors. More specifically, the invention relates to pin tumbler cam locks.
BACKGROUND OF THE ART
There are two basic families of cabinet drawer and door locks: deadlocking and latch locking type locks; and, cam type locks. Both families of locks are used on cabinet drawers and doors such as those found on office desks, credenzas and interior cabinetry. In the former family, an elongated bolt moves in a reciprocating manner into and out of locked and unlocked positions, respectively upon actuation of a key. In the latter family, an elongated bolt moves along an arcuate path, between locked and unlocked positions. In the cam family of locks, an angular rotation of 90° is typically sufficient to determine the locked and unlocked positions.
Both families of locks may have their bolts actuated by either pin tumbler cylinder and plug assemblies, or disk tumbler type assemblies. The disk tumbler type assemblies are the least expensive and historically have been used in the cam type of lock. A lock of this type is shown in U.S. Pat. No. 3,863,476 to Patriquin in which a plurality of spring loaded plates in a plug are biased to position a protrusion from the plates into an elongated trough or cavity in an externally threaded lock body. Interference between the protrusions and sidewalls of the lock body trough prevent rotation of the plug. Upon insertion of a key into a key way of the plug, the plates retract and the protrusions are withdrawn from the trough. Thereupon, the plug can rotate within the threaded lock body. The plug is longitudinally restrained within the lock body by a spring loaded clip. The bolt is typically journaled for rotation with and screwed on a longitudinal extension at the rear of the plug. A cam lock of this type is considered a "direct drive" cam lock because the bolt is directly journaled for rotation with the plug. Stated another way, consider a cam lock of the type described in which the lock is received in a desk drawer wherein the bolt at a 12 o'clock position interferes with a downwardly protruding sill or ledge in the desk. By inserting a key into the plug key way the disk tumblers are retracted so as to be free of a trough in the externally threaded cylindrical body. Rotation of the key by 90° to the 3 o'clock position clears the bolt of the desk so that the drawer may be opened. The externally threaded, cylindrical lock body may be provided with a pair of internal troughs angularly spaced at 90° with respect from one another so that the key may be withdrawn while the bolt is in the unlocked, 3 o'clock position. Otherwise, to remove the key, the plug must be counter-rotated back into the 12 o'clock position leaving the bolt in the "locked position" while the drawer is still open. This procedure has the undesirable consequence in that accidentally closing the open desk drawer with the bolt locked into the 12 o'clock position tends to mar the desk cabinetry. By positioning a second trough in the lock body cavity at the 3 o'clock position, this result can be avoided.
Over the years, it has become desirable to provide cam locks with a pin tumbler rather than a disk tumbler system. In the pin tumbler system, the disk plates are replaced with a series of cylindrical pins which reside in bores in the plug. These "bottom pins" have differing lengths corresponding to protrusions and valleys in a mating key. The lock body or cylinder is provided with a corresponding series of spring loaded top pins which can drop down into the bores in the plug into which the lower pins reside. When a key is inserted into the plug key way, the top pins and bottom pins form a shear line at the interface of the plug and cylinder allowing the plug to rotate freely. A particular problem with this type of lock is that the key can only be inserted or removed when the top and bottom pins are in alignment (typically the 12 o'clock position). Thus, a cam lock adapted as a pin tumbler lock will suffer from the "damaged desk" syndrome discussed above unless a means is provided for rotating and locking the bolt in respective 12 o'clock and 3 o'clock positions while permitting continued rotation of the key back to the 12 o'clock position.
For this purpose, the so called "lazy cam" has been developed in which the bolt of a pin tumbler type cam lock is free to rotate about a protrusion extending from a rearward surface of the plug. The lazy cam however is journaled for rotation with the plug and drives a pin or other protrusion on the bolt. An opposite side of the bolt is typically also provided with a forwardly extending pin which cooperates with laterally extending shoulders on the rear of the cylinder so as to limit rotation of the bolt through 90°. The above-described structure permits the plug to rotate through 360° while the bolt only rotates through 90° thus allowing the key to be removed while the bolt remains rotationally contained between the shoulder on the cylinder and a shoulder on the lazy cam. The desk drawer can now be opened and closed with the bolt in the unlocked position with the key removed.
The above-described lazy cam design provides the cam lock with all of the advantages of a pin tumbler design (e.g. ease in re keying, possible master keying with other cabinet drawer and door locks as well as entry way locks) which are difficult to achieve or unattainable with disk tumbler type locks. However, geometric realities prevent the bolt from being positionable anywhere other than the 12 o'clock and 3 o'clock positions described without changing the threaded cylinder body so as to reposition the shoulders thereon which define the arcuate range of movement for the bolt. Alternate positioning for the bolt is desirable as consumers have needs for cam locks having bolts which operate between the 12 o'clock and 3 o'clock positions; the 3 o'clock and 6 o'clock positions; the 6 o'clock and 9 o'clock positions; and, the 9 o'clock and 12 o'clock positions as in drawer locks; left hand door locks; tray locks; and, right hand door locks respectively.
U.S. Pat. No. 4,099,397 to Dauenbaugh in part addresses this problem by providing a cam type lock which will accept either a complete disk tumbler lock, or a complete pin tumbler lock for driving an arcuately moveable bolt. The bolt defines a square aperture therein which can be positioned in either the 12 o'clock, 3 o'clock, 6 o'clock, or 9 o'clock positions on a square protrusion from a driver attached to the back of either the pin tumbler or disk tumbler lock assembly. Dauenbaugh, however, requires the use of a master lock body, separate from the pin tumbler or disk tumbler locks to house the locks, drivers, bolts, etc. undesirably increasing the cost of the cam lock.
A need therefore exists for a low cost, pin tumbler cam lock providing ambidextrous positions for an arcuately moveable bolt.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a pin tumbler, lazy cam type cam lock having an ambidextrous, arcuately moveable bolt.
The invention achieves this object, and other objects and advantages which will become apparent from the description which follows by providing a pin tumbler cam lock having a cylindrical plug and an elongated cylinder defining a longitudinal bore for rotatably receiving the plug. A lazy cam is journaled for rotation with the plug while a selectively positionable bolt rotation limiter can be mounted in one of at least two positions to limit angular motion of a bolt through two different 90° arcuate paths.
In a preferred embodiment of the invention, the bolt rotation limiter has a pin extending therefrom which is received in one of two bores in the lock cylinder. Two pairs of shoulders are defined on the bolt rotation limiter by two diametrically opposed, radially extending arcuate portions. These portions form shoulders which selectively limit the arcuate travel of the bolt.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an isometric, environmental rear view of a cam lock employing the general principals of the invention.
FIG. 2 is an exploded, isometric view similar to FIG. 1.
FIG. 3 is a rear view of a lock configured for use with a right hand cabinet door wherein the bolt rotation limiter is in a first position corresponding to a latched position of the bolt.
FIG. 4 is a rear view, similar to FIG. 3 in which the bolt is rotated a 90° to an unlocked position.
FIG. 5 is a rear view of the lock in a locked position in which the bolt rotation limiter has been repositioned to a second position suitable for use with a left hand cabinet door.
FIG. 6 is a rear view, similar to FIG. 5 with the bolt moved to an unlocked position.
FIG. 7 is an isometric environmental view of a retaining plate for use with the cam lock.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
An ambidextrous vertical inverted handed cam lock for cabinet doors and drawers, in accordance with the principals of the present invention is generally indicated at reference numeral 10 in the figures. The lock is of the pin tumbler type and is an improvement upon the re keyable cam lock shown and described in U.S. Pat. No. 5,038,589 issued to Martin on Aug. 13, 1991 the disclosure of which is incorporated herein by reference.
It is sufficient for the purposes of this disclosure to state that the lock 10 has a cylinder 12 having flat side walls for receipt in a bore in a cabinet door or drawer along with a radially extending rim 14 which in cooperation with a threaded nut (not shown) for engagement with threads 16 secures the lock 10 in the cabinet door or drawer. A plate shown in FIG. 7 has a conventional main aperture 17(a) for receiving the cylinder 12 and preventing rotation of the same when the plate is secured to adjacent cabinetry. Three holes, 17(b), (c) and (d) are provided for receipt of an appropriate wood screw. By placing a screw in hole 17(c), rotation of the nut (not shown) can be prevented.
The cylinder 12 has a longitudinal bore for receipt of a plug 18 having a key way 19 in communication with a plurality of bores for receiving bottom pins. As is well known to those of ordinary skills in the art, the cylinder 12 has a plurality of corresponding bores for receiving spring biased top pins which when the plug 18 is in place as shown in FIG. 2 are further secured by a slide 20. The lock further comprises an arcuately moveable bolt 22 which defines an aperture 24 permitting the bolt to freely rotate on a rearwardly extending portion 26 of the plug 18. The bolt may be of the off set type 22 as shown, or a straight bolt 22' as will be understood by those of ordinary skill in the art. The bolt also has a transverse pin 28 with rearwardly and forwardly extending portions whose purposes will be discussed further herein below.
The rearwardly extending portion 26 of plug 18 is also provided with a laterally disposed flats 32 which journal a conventional lazy cam 34 for rotation with the plug 18. The lazy cam is longitudinally secured to the plug 18 by a conventional boar star washer 36 and screw 38. Interpositioned between the bolt 22 and cylinder 12 is a bolt rotation limiter 50 having a circular inner sidewall 52 sized for receipt about the rearwardly extending portion 26 of the plug 18. The bolt rotation limiter 50 would be free to rotate about the rearwardly extending portion were it not for the presence of a longitudinally directed pin 54 which is fixed to a forwardly directed surface of the bolt rotation limiter 50. The pin 54 is adapted for receipt in either of a left hand longitudinal bore 56 or a right hand longitudinal bore 58 in a rearward surface 60 of the lock cylinder 12. When seated in the appropriate bore 56, 58, radially extending, arcuate protrusions 62, 64, on the bolt rotation limiter define four shoulders 66, 68, 70, and 72 which engage the forwardly extending portion of the pin 28 of the bolt 22. These shoulders act in pairs to limit the arcuate movement of said bolt to not more than approximately 90°. The cam mechanism 34 also has a conventional radially extending, arcuate protrusion defining shoulders 82, 84 which engage the rearwardly extending portion of pin 28 of bolt 22 such that rotation of the plug 18, rotates the lazy cam 34 thereby driving the bolt 22 in an arcuate path about a longitudinal axis 90. The lazy cam 34 permits the plug to rotate through 360° permitting a key (not shown) to be inserted and removed from the plug 18. By subtending an angle of approximately only 90° with respect to the longitudinal axis 90, the shoulders cause 360° rotation of the plug to translate the bolt only through 90°. The radially extending protrusion 62, 64 on the bolt rotation limiter 50 are diametrically opposed and also subtend to angles of approximately 90°. Thus, the rotational distance between opposite shoulders 66,70 or 68,72 is also 90° limiting rotation of the bolt 22 to 90° as well.
By repositioning the bolt rotation limiter 50 from engagement of its pin 54 with bore 56, to bore 58, the vertical orientation of the cylinder 12 and plug 18 can be advantageously maintained while the throw of the bolt 22 is translated through a full 90°. In this way, the lock 10 can ben used as either a left hand door lock, or a right hand door lock as will be seen with respect to FIGS. 3-6. Removal, reorientation and reinsertion of the lazy cam is also necessary to achieve the desired reconfiguration. That is, after the bolt rotation limiter 50 has been repositioned and the cam 34 has been removed from the plug 18, the cam must be rotated through 180° about a line defined by the plane of the lazy cam. Further understanding may be made by reference to FIGS. 3-6.
As shown in FIG. 3, the lock 10 is shown in rear view with the bolt 22 in a locked, right handed position (i.e. the 3 o'clock position) if viewed from the front. The forwardly extending portion of the pin 28 of bolt 22 is trapped between the shoulder 84 of the lazy cam 34 and the shoulder 68 of the bolt rotation limiter 50. By inserting the key and rotating the key, plug and lazy cam through a full 360°, the bolt 22 will assume the unlocked position shown in FIG. 4 while the pin 28 is trapped between the shoulder 82 of the lazy cam 34 and the shoulder 72 of the bolt rotation limiter 50.
To reconfigure the cam lock 10 from a right hand cabinet door lock as shown in FIGS. 3 and 4, to a left hand cabinet door lock as shown in FIGS. 5 and 6 the bolt rotation limiter 50 is repositioned so that its longitudinally directed pin 54 is received in the right hand longitudinal bore 58 in the rear surface 60 of the cylinder 12. The lazy cam 34 has been rotated through 180° about a line defined by the plane of the figure. The bolt 22 is now in the locked 9 o'clock position (as viewed from the front) while the bolt pin 28 is trapped between the shoulder 84 of the lazy cam 34 and the shoulder 66 of the bolt rotation limiter 50. Rotation of the key (not shown) through 360° will position the bolt in the unlocked position shown in FIG. 6 with the bolt pin 28 trapped between shoulder 82 of the lazy cam 34 and shoulder 68 of the bolt rotation limiter 50.
In all of the positions shown in FIGS. 3-6, the key way 19 is in the vertical position with respect to the cylinder 12 thereby locking the plug 18 (and therefore the bolt 22) in the positions shown in solid lines. In either case, the key (not shown) may be removed from the plug.
The above disclosure describes an ambidextrous cam lock which can be used for left hand or right hand cabinet door applications. As will be apparent to those of ordinary skill in the art upon reviewing the above disclosure, the lock 10 may be modified for desk drawer or tray applications by repositioning the bolt 22 without repositioning the lazy cam 34 so that the pin 28 has its forwardly directed portion captured between the shoulders 66, 70. In this manner, the key way 19 remains in the advantageous vertical position. Other modifications and variations of the invention within the ability of those of ordinary skills and are also contemplated. Therefore, the invention is not to be limited by the above disclosure, but is to be determined as scope by the claims which follow. | An ambidextrous vertical inverted handed cam lock for cabinet doors and drawers has a conventional pin tumbler cylinder and plug assembly. An arcuately movable bolt is journaled for rotation about a rearwardly extending portion of the plug. A conventional lazy cam drives the bolt. An arcuately repositionable bolt rotation limiter provides either left hand or right hand throws for the bolt while simultaneously allowing for inverted vertical use. | 4 |
FIELD OF THE INVENTION
[0001] The present invention relates to an examination and imaging system for fired cartridge cases, and more specifically to an examination and imaging system for use by firearms manufacturers to gather fired cartridge case identification data.
BACKGROUND OF THE INVENTION
[0002] It is well known that fired bullets and spent cartridge cases are left with markings from the firearm from which they come. The markings left on spent cartridge cases result from forced contact between the cartridge and metal parts within the firearm, namely the firing pin and breech. Because the breech and firing pin of each individual firearm are slightly different from firearm to firearm, those of each other firearm, markings are left on each fired cartridge case (a kind of “fingerprint”) unique to each firearm. These “fingepripnts” can be and have been used to determine if two or more cartridge cases have been fired from the same firearm (handgun, rifle, or shotgun). For example, an automated process and apparatus for capturing, storing and comparing fired cartridge case images is disclosed in U.S. Pat. No. 5,654,801 and sold by Forensic Technology WAI Inc. as the IBIS® system. However, despite its success, the ability of the IBIS® system to link cartridge cases to a particular identified firearm has been limited to cases where a firearm has been recovered as evidence. Thus, there is a need for a system that obtains information on firearms before sale (and subsequent use in potential crimes) so that firearm information and evidence gathered in criminal and other investigations, such as fired cartridge cases, can be compared against and linked to particular firearms.
[0003] The present invention provides a method of comparing the markings on spent cartridge cases and identifying the particular firearms, by serial number, from which they were fired without possession of the firearm as evidence. In accordance with the present invention, firearm manufacturers will have the ability to gather firearms identification data to be employed subsequently during forensic analysis of spent cartridge cases.
SUMMARY OF THE INVENTION
[0004] In brief, the object of the present invention is to provide firearm manufacturers with a solution for recovering, sorting, marking, and acquiring the images of spent cartridge cases during firearm test-fires and, most preferably, a system that is fully automated.
[0005] It is one object of the present invention to provide fully automated industrial cartridge casing recovery, sorting, marking, and imaging for use by firearm manufactures in an industrial environment. In a preferred embodiment, the system and method includes five sub-systems, which work in the following sequence: a firearm serial number recognition sub-system; a cartridge case recovery sub-system; a cartridge case sorting sub-system; a cartridge case marking sub-system; and an image acquisition sub-system. The firearm serial number recognition sub-system is a hardware and software sub-system that reads the serial number of a firearm and stores it in a database. The cartridge case recovery sub-system is a mechanical sub-system, which recovers the firearm's ejected cartridge cases and transports them to the sorting sub-system. The cartridge case sorting sub-system identifies the orientation of the cartridge cases and reorients them if necessary, the object being to put the cartridge cases into the correct position for marking. The cartridge case marking sub-system stamps a reference numeral related to the firearm serial numbers on the cartridge cases with a stylus. The reference number is encrypted in a 2D matrix (barcode) form on the cartridge cases. The image acquisition sub-system automatically acquires the firing pin and breech face images of a cartridge case after reading the stamped reference number on its side. This sub-system processes many cartridge cases one after another.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] For a more complete understanding of the present invention, and for further advantages thereof, reference is now made to the following description, taken in conjunction with the accompanying drawings, in which:
[0007] FIG. 1 . is a schematic illustration of the Firearm Serial Number Recognition Sub-System of the present invention.
[0008] FIG. 2 is a perspective view of the Cartridge Case Recovery Sub-System of the present invention.
[0009] FIG. 2A is a perspective view of an alternative embodiment of the Cartridge Case Recovery Sub-System of the present invention.
[0010] FIG. 3A is a cross-sectional side view of the Cartridge Case Sorting Sub-System of the present invention.
[0011] FIG. 3B is a cross-sectional view of the Cartridge Case Sorting Sub-System of the present invention.
[0012] FIG. 4 is a top view of the Cartridge Case Marking Sub-System of the present invention.
[0013] FIG. 5A is a perspective view of the image acquisition sub-system of the present invention.
[0014] FIG. 5B is a front view of the image acquisition sub-system of the present invention.
[0015] FIG. 6 is a schematic depiction of the vacuum/blowing device of the present invention.
[0016] FIG. 7A is a perspective view of the pick and place device of the present invention.
[0017] FIG. 7B is a front view of the pick and place device of the present invention.
[0018] FIG. 8 is a perspective view of a portion of the cartridge case recovery subsystem of the present invention.
[0019] FIG. 9 is a perspective view of the cartridge case decelerator device of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0020] The present invention is a novel firearms identification system that provides a solution for recovering, sorting, marking, and acquiring the images of spent cartridge cases during firearm test-fires. In the preferred embodiment of the invention hereinafter described, the system provides a fully automated cartridge case recovery, sorting, marking, and imaging for use by firearm manufacturers in an industrial environment (e.g. a firearms manufacturer's test fire range). The preferred system includes a sequence of five sub-systems as follows: a firearm serial number recognition sub-system; a cartridge case recovery sub-system; a cartridge case sorting sub-system; a cartridge case marking sub-system; and an image acquisition sub-system.
[0021] Referring to FIG. 1 , the firearm serial number recognition sub-system and process shall be described. Prior to the test firing of the firearm 102 , the operator positions the firearm 102 in a firearm holding fixture 120 . The holding fixture 120 is a device designed to hold the firearm in place during a test fire while not obscuring the visibility of the serial number on the firearm. The firearm is positioned in the holding fixture such that its serial number 106 (or other identifying numerals, letters or markings relatively unique to the firearm, hereinafter generally referred to as a serial number) is in front of and visible to serial number recognition device 130 which is designed to automatically read the firearm serial number. In other alternative embodiment, more than one camera could be used to capture the image of the firearm serial number at different locations on the firearm.
[0022] The serial number recognition device 130 consists of a CCD (charge-coupled device) digital camera 108 connected to a computer equipped with high-resolution image grabber technology (a PCI card). A suitable image grabber is a commercially available PCI card from Matrox Inc by the name of Matrox frame Grabber Meteor 2/4. Digital camera 108 is preferably controlled by a computer which signals to the camera to take a picture (image) of the firearm serial number 106 at a preselected time prior to test firing of the firearm. This is done through OCR (Optical Character Recognition) software which instructs the frame grabber card to activate the digital camera to grab an image of the serial number on the firearm positioned in front of the camera. The image of the serial number is electronically transmitted to the computer for further processing and/or stored in the computer's memory or other storage medium (e.g. disk, storage tape, etc.) for later processing. After the image of the serial number is obtained and transmitted to the computer, the image is analyzed and processed by the computer with Optical Character Recognition (OCR) algorithm and software which are designed to read and recognize the serial number of the specific firearm. At this point in the process, the system then preferably sends the image for storage in a database and next sends the serial number (in alphanumerical format) for storage in the same database after an automatic or manual validation. The level of confidence preset in the software controlling the OCR software predefines the automatic or manual validation. The image of the serial number and the serial number itself are then linked to the record of the acquired cartridge case image for the firearm in the database. In an alternative embodiment of the firearm serial number recognition sub-system, the image capture from the CCD digital camera 108 is stored directly in the computer database and associated to the firearm serial number without being processed by the OCR algorithm.
[0023] Referring to FIGS. 2 and 8 , the cartridge case recovery sub-system and process will be described. The cartridge case recovery sub-system is a multi-part system that catches cartridge cases ejected from the firearm as it is test fired. As shown, a chute 203 is positioned adjacent the firearm being test fired. The chute 203 includes a main body 207 and an opening 210 designed to permit fired cartridge cases to readily enter the chute. The opening 210 is positioned in the path of the expected ejection of the spent cartridge case. The main body 207 of the chute is funnel-shaped to allow the ejected cartridge cases to fall toward a vacuuming and blowing device 204 (Venturi) and into pneumatic conveyor 205 .
[0024] FIGS. 2A and 8 depict an alternative embodiment of the cartridge case recovery sub-system. The same reference numerals are used to depict similar components as described above in relation to FIG. 2 . In this alternative embodiment, the orientation of conveyor 205 differs as shown. Further, in the alternative embodiment of the cartridge case recovery subsystem shown in FIGS. 2A and 8 , chute 203 includes a hood portion 209 extending over the firearm held in the firearm holding jig 120 . In this configuration, the chute effectively surrounds the upper part and a lateral side of the firearm and thus the ejection port of the firearm from which the fired casing is ejected.
[0025] Referring to FIG. 6 , the vacuum/blowing device 204 shall be described in greater detail. Vacuum device 204 is a commercially available 1½ inch diameter “venturi” (Line Vac). Compressed air flows through inlet 211 into an annular plenum chamber 213 . The compressed air is then injected into the throat through directed nozzles 215 . These jets of air create a vacuum at the intake 217 which draws the cartridge cases in and accelerates them through a 1¼ diameter antistatic tube 205 (pneumatic conveyor) and transports them to the end of the conveyor 205 where the cases are received by the decelerator/receiving device 206 ( FIGS. 2 and 9 ). The antistatic tube 205 is preferably constructed of rigid plastic tubing and is made of an antistatic material to avoid build up of static electricity that can be dangerous if gunpowder builds up in the tube.
[0026] Referring to FIG. 2 and FIG. 8 (alternative configuration), after the cartridge cases are ejected into the chute 203 , a light curtain device 220 counts the number of cartridge cases that go through. Light curtain devices suitable for counting cartridge cases are commercially available. The light curtain device 220 in the embodiments shown in FIGS. 2 and 8 is a commercially available Banner LS10 light curtain. Light curtain device 220 includes a light source on one side that produces a strobe array of modulated light beams to produce a light screen and receiver cell in the opposite side, creating a “light curtain” between the emitter and receiver. Preferably, the light curtain device 220 is arranged so that the light curtain is located in the middle part of the chute to ensure that all cartridge cases passing through chute 203 are counted. When a cartridge case passing through chute 203 cuts the light curtain, an electrical signal is sent to a Programmable Logic Controller (PLC) (i.e., a computer) that keeps count of cartridge cases that went through the light. Suitable PLCs are commercially available Honeywell and others. The PLC can then validate that all the cartridge cases that went through the chute arrived at the other end of tube 205 by using a second similar light curtain, where they are slowed down in the receiving device 206 (decelerator), then fall into the sorting system. The function of decelerator/receiving device 206 is to catch and reduce the traveling speed of the incoming cartridge cases and to evacuate the air and firing fumes coming from the venturi device 204 . As shown in FIG. 9 , decelerator/receiving device 206 has a triangular shape. The interior walls of the decelerator/receiving device 206 are covered with rubber padding 250 to avoid any extra marking on the cartridge cases. As cartridge cases enter the device with an upward trajectory, they ricochet on a mesh fabric 219 located on the upper wall of the device and then fall by gravity into a bottom opening 221 , while air and firing fumes exhaust through the mesh fabric.
[0027] Referring to FIGS. 3A and 3B , the cartridge case sorting sub-system and process will be described. The test-fired cartridge cases 600 ejected from the firearm travel through the recovery sub-system before falling into a pre-sorting device working as a funnel comprising two parallel plates 301 and 304 and a sliding plate 302 (preferably made of plastic) at the bottom between the two parallel plates. The sliding plate 302 has four openings 309 that match the width and the length of the cartridge cases. Those openings are specially chamfered at the bottom to one side to allow the cartridge cases to slide out when the four openings 306 of the sustaining plate 304 axe properly aligned with the four casings. The top edge of the sliding plate 302 is designed with an angle to facilitate the sliding of the cartridge cases into the four openings. The sliding plate 302 moves horizontally, pushed by a pneumatic piston 305 .
[0028] In the operation of the sorting sub-system shown in FIGS. 3A and 3B , the spent cartridge cases 600 are initially held vertically in slots 309 of sliding plate 302 where there are an equal number of sensors 308 relative to the number of test-fired cartridge cases. The sensors 308 detect and count the cartridge cases. Sensors 308 can be of any suitable type for detecting objects of the nature and for the purposes described herein. Model PTB 46U fiber optic sensors manufactured by Banner have been found to be particularly suitable. The PLC receives a signal from each of the four sensors 308 located beside the cartridge cases openings. When the presence of all four cartridge cases has been detected, the PLC then instructs a solenoid valve to activate pneumatic cylinder 305 , which is operably connected to and moves sliding plate 302 , thus guiding the four cartridge cases to fall by gravity in their respective slots 306 of plate 304 . Thereafter, the released cartridge cases fall through openings 311 in transfer block 307 . After a specified delay, the PLC instructs a solenoid valve to activate a pneumatic cylinder 303 that shifts the transfer block 307 over the openings of the rotating device 312 .
[0029] The rotating device 312 comprises a cylinder with four chambers 314 to hold each of the respective cartridge cases 600 and is mounted to a pneumatic rotary actuator 316 driven by a solenoid valve that is controlled by the PLC and a pneumatic piston 320 for translation displacements. Once the transfer block 307 is positioned above the rotating device, the cartridge cases fall through four openings to reach the rotating device's chambers 314 . At this stage, four vacuum cups 319 that axe mounted on a linear pneumatic slide 321 pick up the primer side up cartridge cases and leave any casings that have not been oriented primer side up. The remaining cartridge cases (i.e., the cases that were not oriented primer side up and therefore not picked up by the vacuum cups) are then rotated 180 degrees so that their primer side is facing up. This rotation of the rotating device 312 is performed by rotary actuator 316 . The vacuum cups 319 then reposition the previously extracted cartridge cases into the empty chambers 314 of the rotating device. At that point, the orientation of all the cartridge cases is the same (primer side up) and pneumatic piston 320 moves laterally the housing block 322 (that holds the rotating device) to align the openings of the rotating device 314 , with openings 318 . In the next step, gate 313 , moved by a pneumatic cylinder 323 that is driven by a solenoid valve, releases the cartridge cases 600 to the cartridge case marking subsystem only when the four sensors 325 confirm to the PLC the presence of four cartridge cases. Sensors 325 can be of the same type as sensors 308 , namely, fiber optic sensors.
[0030] Referring to FIG. 4 , the cartridge case marking sub-system and process will be described. Once all the casings are oriented correctly as described above, they fall into an indexing device 413 where they are held in place by a holding device 418 , preferably working as clamps. Holding device 418 is spring loaded so that spring force is applied by default to hold the cartridge cases in place. The spring holding force is released when necessary by using a single action pneumatic cylinder, driven by a solenoid valve, which is controlled by the PLC. The indexing device 413 , controlled by the PLC, positions the cartridge cases in front of the two marking machines 414 . These marking machines utilize micro punching technology which uses pneumatically accelerated hardened pins to print a reference numeral linked to the serial number of the firearm. This reference number is encoded in a 2D matrix (bar code equivalent). A suitable micro punching system is the PINSTAMP® TMP 1700/400 sold by Telesis which is pneumatically driven and which uses conical tipped pins to permanently indent the surface of the cartridge cases to form a dot matrix 2D code corresponding to the firearm's serial number.
[0031] In the preferred sub-system, two machines are used at the same time to speed up the marking step. Once the cartridge cases have been marked, a vision system 420 with a CCD, (Charge Coupled Device) camera 415 reads the 2D-matrix code to validate if each cartridge case has been clearly marked for marking validation purposes. The vision system 420 uses a commercially available CCD (e.g., SmartSensor Series 600 manufactured by DVT) which includes software to read for validation purposes that the marking of the 2D bar code on the cartridge case has been properly done. After this validation process, the indexing device/table positions the cartridge cases holding device 418 in front of a pick and place device ( FIGS. 7A and 7B ). The cartridge cases are then picked from the storage tray 417 , one at a time, by a pneumatic parallel gripper 701 , moved up the Z axis 702 using a guided linear pneumatic slide and then placed in their assigned position in the storage device/tray 417 . An electrical actuator drives the linear positioning of the NY table. The electrical actuators are driven by solenoid valves and the positioning tables are driven by a motion control drive and controller. As shown in FIG. 4 , cartridge case storage device 417 is preferably designed to hold many cartridge cases at the same time (e.g., 100 cases as shown in FIG. 4 ).
[0032] Referring to FIG. 5 , the cartridge case image acquisition sub-system and process will be described. The cartridge case image acquisition sub-system is a multi-part system that includes an XY table 518 and a motorized Z axis 524 ; a microscope and CCD camera 519 ; an integrated ring light in a microscope holder 520 ; a motor device and vacuum cup to lift and rotate the cartridge cases 600 ; a 2D matrix reading system to read the cartridge case numbers 522 ; and a spent cartridge case storage device 417 that can contain many cartridge cases at the same time (called the carrier media). A suitable ring light 520 is available from Nikon with a Dolan-Jenner power supply.
[0033] The sorted and marked cartridge cases are positioned into a carrier media 417 . This carrier media is placed manually on the motorized XY table 518 under the microscope 519 for the image acquisitions. Preferably, an automated acquisition procedure is then started, controlled by a computer. The bar code reader 523 identifies the current carrier media by reading a bar coded label attached to its side. The NY table moves sequentially to pre-programmed positions that match the cartridge case locations in the carrier device. The XY table's translations to a position under the microscope for image acquisition, the microscope's focus and the light intensity can be accomplished manually, but automated control of these steps via a computer is preferred. A small motor with a vacuum cup 521 lifts and rotates the first cartridge case in front of the digital camera (smart sensor) 522 . That camera 522 , assisted by lighting, reads the reference number represented by a 2D-matrix code engraved on the cartridge case. A suitable light for reading the 2D bar code is one that brings contrast to the 2D matrix code engraved on the cartridge case's surface. A commercially available light suitable for this purpose is an LED illuminator sold under the name NERLITE® S-40. The reference number that has now been read is used to validate that the correct cartridge case is being acquired.
[0034] Preferably, the acquisition of the firing pin and breech face images is done automatically with the help of a ring light 520 . The process of cartridge case breech face and firing pin marks examination has been successfully automated using apparatus as set out in U.S. Pat. No. 5,654,801, which is hereby incorporated by reference. After the first image acquisition (firing pin and breech face), the next cartridge case is positioned under the microscope 519 (preferably automatically via control by a computer) and the acquisition procedure is repeated. The system continues the automatic reference number reading and the image acquisition for all the cartridge cases in the carrier media 417 . Once all the cartridge cases images of the carrier media have been acquired the operator validates the images by verifying that every image corresponds to the quality required by the QA (quality assurance) standards. This can be accomplished by a visual inspection of the images by the operator who validates whether the images appear in focus and the light intensity seems adequate. Preferably this is done using a monitor with multiviewer window capability, such as that employed in the commercially available IBIS system sold by Forensic Technology WAI, Inc. of Canada, to allow a more efficient validation process. The multiviewer is a window generated by a software application displaying multiple acquired images on a monitor. Preferably, the multiviewer process employs a tiling (configurable) format, such as that employed by the IBIS system, enabling the operator to perform a fast quality assurance verification of the images. Any image that does not meet the quality standards is reacquired until quality standards are met.
[0035] After the acquisition and validation procedures are successfully executed, the acquired cartridge cases can then be used in a correlation procedure. The correlation procedure is to compare a discovered or tested-fired cartridge case against the database of images acquired as described above. Any suitable image comparison software can be used to correlate the images. A suitable correlation process is described in U.S. Pat. No. 5,654,801
[0036] Preferably, the carrier media with the cartridge cases is covered with a protective plastic plate for storage after image acquisition. The carrier media are also identified by specific barcode. The barcode stored in the database helps to trace the cartridge cases for later use in investigations or other evidentiary purposes. For example, the test fired cartridge cases may be compared under a comparison microscope with evidence from crime scenes to validate “hits” (i.e., potential matches) indicated by the automated image correlation process.
[0037] Although the present invention has been described with respect to preferred embodiments, various changes, substitutions and modifications of this invention may be suggested to one skilled in the art, and it is intended that the present invention encompass such changes, substitutions and modifications as fall within the scope of the appended claims. | A system and method for identifying, test firing, marking, and imaging firearm cartridge cases and firearms for use by firearm manufactures. The system and method includes five subsystems, which work in the following sequence: a firearm serial number recognition sub-system; a cartridge case recovery sub-system; a cartridge case sorting sub-system; a cartridge case marking sub-system; and an image acquisition sub-system ( 108 ). The firearm serial number recognition sub-system ( 130 ) reads the serial number of a firearm and stores it in a database. The cartridge case recovery sub-system recovers fired cartridge cases and transports them to the sorting sub-system. The cartridge case sorting sub-system identifies the orientation of the cartridge cases and reorients them, if necessary, for marking. The cartridge case marking sub-system stamps the firearm serial numbers on the cartridge cases. The serial number is encrypted in a 2D matrix (barcode) form on the casings. The image acquisition sub-system acquires the firing pin and breech face images of a cartridge case after reading the stamped serial number on its side. | 5 |
BACKGROUND OF THE INVENTION
The present invention relates to a combustor of a gas turbine and, more particularly, to a combustor of a gasturbine which can effectively withstand the vibration and thermal distortion generated during the combustion.
It is a current measure for preventing the pollution of air attributable particularly to lower nitrogen oxide (NOx) content to effect a spray of water, steam or the like into the combustors of gas turbines. This spray lowers the temperature of the combustion gas to effectively suppress the production of NOx in the combustor. On the other hand, however, the lowered temperature of the combustion gas considerably hinders the combustion of the fuel in the combustor. More specifically, the pulsation of the combustion is enhanced due to the lowered combustibility, resulting in a cyclically repeated application of load. This repetitional load is concentrated to the thermally weak portions of the combustor to cause a break down due to a stress concentration.
Generally, in the gas turbines for industrial purposes, compressed air produced by an air compressor is introduced into a combustor where the compressed air is mixed with the fuel and the mixture is burnt to form a combustion gas. This combustion gas is introduced to drive the turbine which in turn drives a load connected thereto. The combustor is mainly constituted by a liner forming a combustion chamber, a transition piece connected to the liner, an outer casing surrounding the liner and the transition piece and a fuel nozzle attached to the outer casing.
The fuel atomized into a liner from the fuel nozzle is burnt under the presence of the air which has been compressed by the air compressor and introduced into the liner through the jacket defined between the outer casing and the combined body of the liner and the transition piece and then through the combustion air port formed in the wall of the liner. The combustion gas produced as the result of the combustion then flows through the liner and introduced into the gas turbine after a rectification performed by the transition piece.
The transition piece is partially cooled by the compression air which flows toward the liner defining the combustion chamber. However, the transition piece has some portions which are in locations relatively inaccessible to the cooling air flow and, hence, the cooling is rather difficult. More specifically, this portion is the radially outer part of the gas outlet of the transition piece closest to the gas turbine. In consequence, this portion of the transition piece is heated excessively and broken due to the stress concentration.
The liner and the transition piece are supported for free thermal expansion and shrinkage. In other words, they are supported rather loosely. Therefore, the vibration caused by the pulsating combustion is transmitted from the liner to the transition piece to generate a vibration of a considerably large amplitude in the transition piece, particularly at the gas outlet side of the latter.
SUMMARY OF THE INVENTION
It is, therefore, an object of the invention to provide an improved construction which permits, in the gas turbine combustor, an efficient cooling of the portion of the transition piece which is relatively inaccessible to the cooling air flow.
It is another object of the invention to provide an improved construction capable of suppressing the vibration of transition piece of the gas turbine combustor.
To these ends, according to the invention, there is provided a combustor of a gas turbine having a plurality of combustor liners, transition pieces connected to respective liners and adapted to rectify the flow of the combustion gas and outer casings enclosing the liners and the transition pieces, wherein the improvement comprises at least one guide plate disposed between adjacent transition pieces and adapted to rectify the flow of air passing through the clearances between adjacent transition pieces.
According to another aspect of the invention, there is provided a gas turbine combustor having the above stated features, wherein the guide plates are disposed in the vicinity of the gas outlets of the transition pieces.
These and other objects, as well as advantageous features of the invention will become more clear from the following description of the preferred embodiments taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view of a part of a conventional gas turbine engine, showing a typical arrangement of the combustor;
FIG. 2 is a schematic illustration of the gas outlet of a transition piece of the gas turbine combustor shown in FIG. 1, as viewed from the side closer to the turbine;
FIG. 3 is a schematic illustration of the gas outlet of a transition piece of a gas turbine combustor constructed in accordance with the invention, as viewed from the side closer to the turbine; and
FIG. 4 is a perspective view showing the construction for mounting guide plates shown in FIG. 3.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring first to FIG. 1 which is a sectional view of a part of a conventional gas turbine engine, reference numerals 1, 2 and 3 denote, respectively, an air compressor, a combustor and a turbine. The combustor 2 is constituted mainly by a plurality of (e.g. 10) liners 4 equispaced in the circumferential direction of the turbine engine, transition pieces 5 connected to the rear ends of respective inner cylinders, outer casings surrounding the inner cylinders and the transition pieces, each outer casing having a cylindrical portion 6a coaxial with corresponding liner 4 and an annular housing 6b to which the rear end of the cylindrical portion 6a is attached, and fuel nozzles 9 attached to the side covers 8 of respective outer casings.
The air compressed by the air compressor 1 is introduced through the outlet 10 of the latter into jackets 11 defined in respective outer casings 6 and makes a turn in the annular housing 6b. The air then flows as indicated by arrows to the inside 13 of each liner through combustion air ports 12 formed in the wall of the liner 4.
Meanwhile, the fuel atomized into the inside of each liner 4 from the associated fuel nozzle 9 is ignited for starting the engine by an ignition plug 14 which is usually provided in one or two of the plurality of liners 4, and is burnt under the presence of the combustion air supplied through the combustion air ports 12. The fuel in the liners which are not provided with the ignition plug is ignited by the flame propagated through cross fire tube 15 which connects the adjacent liners. Once the ignition is made in all liners, the combustion is maintained continuously, and the combustion gas of high temperature flows through the liner 4 and is introduced to the first nozzle of first stage of the gas turbine, after a rectification performed by the transition piece. The gas then is effective in the turbine 3 to thereby drive a load such as a generator (not shown) coupled to the turbine. During the operation of the turbine, the inner surface of each liner 4 is film-cooled by the air which is introduced into the liner through a multiplicity of louver ports 17 formed in the liner, so that the inner surfaces of the liner is not so hot and is maintained at a comparatively low temperature of 600° to 700° C. In contrast to the above, the film cooling is not effected on the transition piece because the latter has no louver ports. In consequence, the wall of the transition piece is heated up to a high temperature which may reach 800°-850° C. or higher. In FIG. 1, a turbine casing is designated at a reference numeral 32.
The reason why the wall of the transition piece is heated to the high temperature will be described in more detail with specific reference to FIG. 2. FIG. 2 schematically shows the gas outlets of some of the transition pieces as viewed from the side closer to the first nozzle 16 of the gas turbine. The combustion gas coming from a plurality of liners is introduced to the nozzle 16 of the first stage of the gas turbine, through the gas outlets 18 of respective transition pieces. On the other hand, the flow 19 of the compressed air outside of the gas outlet 18 collides with the lower surface of each transition piece, i.e. the radially inner surface 20 of the same and then flows through the gaps 21 between adjacent transition pieces 5. In consequence, eddy currents 23 of air are generated on the upper surface, i.e. the radially outer surface 22 of each transition piece. Simultaneously, dead air regions 25 are formed at the corners 24 of the radially outer surface 22 of each transition piece. The central portion of the radially outer surface 22 is maintained at a comparatively low temperature thanks to a large cooling effect provided by the turbulent flow of the air generated by the eddy currents 23, whereas the corners 24 on which the dead air regions 25 are formed are heated to a very high temperature which is, for example, about 850° C. In consequence, the stress is concentrated to the corners 24 of the radially outer surface 22 of each transition piece, resulting in a break down of the transition piece at these corners.
As stated before, the invention aims at providing a combustor of a gas turbine, capable of overcoming the above-described problems of the prior art.
To this end, according to the invention, guide plates for rectifying the flow of air are disposed in the gaps between adjacent transition pieces.
Hereinafter, an embodiment of the gas turbine combustor of the invention will be described with specific reference to FIGS. 3 and 4. In these Figures, reference numerals 5 and 18 denote, respectively, transition pieces and gas outlets of these transition pieces. A T-shaped guide plate 31 is disposed in the gap 21 between each pair of adjacent transition pieces 5. The radial portion 31a of the guide plate 31 is disposed at the intermediate portion of the gap 21 so as to divide the latter into two sections, while the circumferential portion 31b is disposed to overlie the upper corners 24 of each transition piece 5 at a suitable clearance δ from the upper surface of the transition piece 5. This guide plate 31 is welded to a base plate 34 which in turn is fixed to the turbine casing 32 by means of bolts 33, and is received at its both side edge portions by the innersurface of the U-shaped channel section 35a, 36a of support members 35 and 36 which are welded to the wall of the gas outlets of the adjacent transition pieces 5. Therefore, the guide plate 31 connects the adjacent transition pieces 5 to each other. In the illustrated embodiment, the guide plate 31 is formed by folding a web member at the center and then opening both free ends to provide the T-shaped cross-section.
In operation of the gas turbine having the combustor of the invention, the flow 19 of compressed air flowing through each gap 21 between each pair of adjacent transition pieces 5 is rectified to flow along the surface of the guide plate. More specifically, the compressed air flows in the gap 21 along the radial portion 31a of the guide plate 31 and then on the radially outer surface 22 of the transition piece so as to cover the latter, along the circumferential portion 31b of the guide plate.
As a result, the compressed air flows smoothly on the entire area of the radially outer surface 22 of the transition piece including the corners 24 without forming the dead air regions which are inevitably formed in the conventional combustor, so that the cooling effect on the entire area of the radially outer surface is increased to avoid the local temperature rise.
In consequence, the stress concentration to the corners 24 attributable to the generation of dead air regions is eliminated completely. In addition, since the guide plate 31 connects the adjacent transition pieces 5 to each other, the sliding of the transition pieces due to the thermal distortion, as well as the vibration of the same, is effectively suppressed.
An optimum cooling effect will be obtained by suitably adjusting the clearance δ between the radially outer surface 22 of the transition piece 5 and the circumferential portion 31b of the guide plate through changing the position of the latter. The position of the guide plate 31 can be changed by changing the positions of bolts 33 of the base plate 34.
Also, it is possible to rectify the air flow more smoothly, if the transient portion between the radial and circumferential portions 31a, 31b is suitably curved.
From the foregoing description, it will be apparent that various advantages are brought about by the invention.
Firstly, it is possible to obviate the stress concentration to the corners of radially outer surface of the transition piece, thanks to a uniform and efficient cooling of that surface.
Secondly, the guide plate which connects the adjacent transition pieces to each other is effective to suppress the sliding of these pieces caused by the thermal distortion, as well as the undesirable vibration of these pieces attributable to the vibratory combustion taking place in the liners. | A combustor of a gas turbine having a plurality of liners defining combustion chambers, and transition pieces adapted to rectify the flow of the combustion gas discharged from the liners before the combustion gas is introduced to the turbine. A guide plate is disposed in the gap between each pair of adjacent transition pieces near the gas outlets of the latter so as to guide the flow of air to the radially outer surfaces of adjacent transition pieces, thereby to improve the cooling of these surfaces and, at the same time, to mechanically connect the adjacent transition pieces to suppress the vibration of the transition pieces. | 5 |
[0001] This application is continuation of application Ser. No. 10/243,997, which is currently pending and which is a continuation-in-part of application Ser. No. 09/635,108 filed Aug. 9, 2000, now U.S. Pat. No. 6,471,694. The contents of application Ser. Nos. 10/243,997 and 09/635,108 are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention pertains generally to systems and methods for implementing cryoablation procedures. More particularly, the present invention pertains to systems and methods that precool a primary fluid to a sub-cooled, fully saturated liquid state, for use in a cryoablation procedure. The present invention is particularly, but not exclusively, useful as a system and method for cooling the distal tip of a cryoablation catheter during cardiac cryoablation therapy to cure heart arrhythmias. The present invention also relates to the field of methods and apparatus used to generate and control the delivery of cryosurgical refrigeration power to a probe or catheter.
BACKGROUND OF THE INVENTION
[0003] As the word itself indicates, “cryoablation” involves the freezing of material. Of importance here, at least insofar as the present invention is concerned, is the fact that cryoablation has been successfully used in various medical procedures. In this context, it has been determined that cryoablation procedures can be particularly effective for curing heart arrhythmias, such as atrial fibrillation.
[0004] It is believed that at least one-third of all atrial fibrillations originate near the ostia of the pulmonary veins, and that the optimal treatment technique is to treat these focal areas through the creation of circumferential lesions around the ostia of these veins. Heretofore, the standard ablation platform has been radiofrequency energy. Radiofrequency energy, however, is not amenable to safely producing circumferential lesions without the potential for serious complications. Specifically, while ablating the myocardial cells, heating energy also alters the extracellular matrix proteins, causing the matrix to collapse. This may be the center of pulmonary vein stenosis. Moreover, radiofrequency energy is known to damage the lining of the heart, which may account for thromboembolic complications, including stroke. Cryoablation procedures, however, may avoid many of these problems.
[0005] In a medical procedure, cryoablation begins at temperatures below approximately minus twenty degrees Centigrade (−20° C.). For the effective cryoablation of tissue, however, much colder temperatures are preferable. With this goal in mind, various fluid refrigerants (e.g. nitrous oxide N 2 O), which have normal boiling point temperatures as low as around minus eighty eight degrees Centigrade (−88° C.), are worthy of consideration. For purposes of the present invention, the normal boiling point temperature of a fluid is taken to be the temperature at which the fluid boils under one atmosphere of pressure. Temperature alone, however, is not the goal. Specifically, it is also necessary there be a sufficient refrigeration potential for freezing the tissue. In order for a system to attain and maintain a temperature, while providing the necessary refrigeration potential to effect cryoablation of tissue, several physical factors need to be considered. Specifically, these factors involve the thermodynamics of heat transfer.
[0006] It is well known that when a fluid boils (i.e. changes from a liquid state to a gaseous state) a significant amount of heat is transferred to the fluid. With this in mind, consider a liquid that is not boiling, but which is under a condition of pressure and temperature wherein effective evaporation of the liquid ceases. A liquid in such condition is commonly referred to as being “fully saturated”. It will then happen, as the pressure on the saturated liquid is reduced, the liquid tends to boil and extract heat from its surroundings. Initially, the heat that is transferred to the fluid is generally referred to as latent heat. More specifically, this latent heat is the heat that is required to change a fluid from a liquid to a gas, without any change in temperature. For most fluids, this latent heat transfer can be considerable and is subsumed in the notion of wattage. In context, wattage is the refrigeration potential of a system. Stated differently, wattage is the capacity of a system to extract energy at a fixed temperature.
[0007] An important consideration for the design of any refrigeration system is the fact that heat transfer is proportional to the difference in temperatures (ΔT) between the refrigerant and the body that is being cooled. Importantly, heat transfer is also proportional to the amount of surface area of the body being cooled (A) that is in contact with the refrigerant. In addition to the above considerations (i.e. ΔT and A); when the refrigerant is a fluid, the refrigeration potential of the refrigerant fluid is also a function of its mass flow rate. Specifically, the faster a heat-exchanging fluid refrigerant can be replaced (i.e. the higher its mass flow rate), the higher will be the refrigeration potential. This notion, however, has it limits.
[0008] As is well known, the mass flow rate of a fluid results from a pressure differential on the fluid. More specifically, it can be shown that as a pressure differential starts to increase on a refrigerant fluid in a system, the resultant increase in the mass flow rate of the fluid will also increase the refrigeration potential of the system. This increased flow rate, however, creates additional increases in the return pressure that will result in a detrimental increase in temperature. As is also well understood by the skilled artisan, this effect is caused by a phenomenon commonly referred to as “back pressure.” Obviously, an optimal operation occurs with the highest mass flow rate at the lowest possible temperature.
[0009] In light of the above, it is an object of the present invention to provide an open-cycle, or closed-cycle, refrigeration system for cooling the tip of a cryoablation catheter that provides a pre-cooling stage in the system to maximize the refrigeration potential of the refrigerant fluid at the tip of the catheter. Another object of the present invention is to provide a refrigeration system for cooling the tip of a cryoablation catheter that substantially maintains a predetermined pressure at the tip of the catheter to maximize the refrigeration potential of the refrigerant fluid at the tip. Still another object of the present invention is to provide a refrigeration system for cooling the tip of a cryoablation catheter that provides the maximum practical surface area for the tip that will maximize the ablation potential of the refrigerant fluid. Also, it is an object of the present invention to provide a refrigeration system for cooling the tip of a cryoablation catheter that is relatively easy to manufacture, is simple to use, and is comparatively cost effective.
SUMMARY OF THE PREFERRED EMBODIMENTS
[0010] In a cryosurgical system, contaminants such as oil, moisture, and other impurities are often deposited in the impedance tubing or other restriction through which the refrigerant is pumped. In the impedance tubing, the temperature is very low, and the flow diameter is very small. Deposit of these impurities can significantly restrict the flow of the cooling medium, thereby significantly reducing the cooling power.
[0011] A cryosurgical catheter used in a cardiac tissue ablation process should be able to achieve and maintain a low, stable, temperature. Stability is even more preferable in a catheter used in a cardiac signal mapping process. When the working pressure in a cryosurgery system is fixed, the flow rate can vary significantly when contaminants are present, thereby varying the temperature to which the probe and its surrounding tissue can be cooled. For a given cryosurgery system, there is an optimum flow rate at which the lowest temperature can be achieved, with the highest possible cooling power. Therefore, maintaining the refrigerant flow rate at substantially this optimum level is beneficial.
[0012] In either the ablation process or the mapping process, it may be beneficial to monitor the flow rates, pressures, and temperatures, to achieve and maintain the optimum flow rate. Further, these parameters can be used to more safely control the operation of the system.
[0013] A cryosurgical system which is controlled based only upon monitoring of the refrigerant pressure and catheter temperature may be less effective at maintaining the optimum flow rate, especially when contaminants are present in the refrigerant. Further, a system in which only the refrigerant pressure is monitored may not have effective safety control, such as emergency shut down control.
[0014] It may also be more difficult to obtain the necessary performance in a cryosurgery catheter in which only a single compressor is used as a refrigeration source. This is because it can be difficult to control both the low and high side pressures at the most effective levels, with any known compressor. Therefore, it can be beneficial to have separate low side and high side pressure control in a cryosurgical system.
[0015] Finally, it is beneficial to have a system for monitoring various parameters of data in a cryosurgery system over a period of time. Such parameters would include catheter temperature, high side refrigerant pressure, low side refrigerant pressure, and refrigerant flow rate. Continuous historical and instantaneous display of these parameters, and display of their average values over a selected period of time, can be very helpful to the system operator.
[0016] The present invention provides methods and apparatus for controlling the operation of a cryosurical catheter refrigeration system by monitoring pressures, temperature, and/or flow rate, in order to automatically maintain a stable refrigerant flow rate at or near an optimum level for the performance of crysurgical tissue ablation or mapping. Different refrigerant flow rates can be selected as desired for ablation or mapping. Flow rate, pressures, and temperature can be used for automatic shut down control. Refrigerant sources which provide separate high side and low side pressure controls add to the performance of the system. Continuous displays of temperature, high side refrigerant pressure, low side refrigerant pressure, and refrigerant flow rate are provided to the operator on a single display, to enhance system efficiency and safety.
[0017] A refrigeration system (open-cycle, or closed-cycle) for cooling the tip of a cryoablation catheter includes a source for a primary fluid refrigerant, such as nitrous oxide (N 2 O). Initially, the primary fluid is held under pressure (e.g. 750 psia) at ambient temperature (e.g. room temperature). A pressure regulator is connected in fluid communication with the primary fluid source for reducing the pressure on the primary fluid down to a working pressure (e.g. approximately 400 psia). During this pressure reduction to the working pressure, the primary fluid remains at substantially the ambient temperature.
[0018] After pressure on the primary fluid has been reduced to the working pressure, a precooler is used to pre-cool the primary fluid from the ambient temperature. This is done while substantially maintaining the primary fluid at the working pressure. Importantly, at the precooler, the primary fluid is converted into a fully saturated liquid which has been pre-cooled to a sub-cool temperature. As used here, a sub-cool temperature is one that is below the temperature at which, for a given pressure, the fluid becomes fully saturated. For example, when nitrous oxide is to be used, the preferred sub-cool temperature will be equal to approximately minus forty degrees Centigrade (T sc =−40° C.).
[0019] Structurally, the precooler is preferably a closed-cycle refrigeration unit that includes an enclosed secondary fluid (e.g. a freon gas). Additionally, the precooler includes a compressor for increasing the pressure on the secondary fluid to a point where the secondary fluid becomes a liquid. Importantly, for whatever secondary fluid is used, it should have a normal boiling point that is near to the preferred sub-cool temperature of the primary fluid (T sc ). The secondary fluid is then allowed to boil, and to thereby pre-cool the primary fluid in the system to its sub-cool temperature (T sc ). As a closed-cycle unit, the secondary fluid is recycled after it has pre-cooled the primary fluid.
[0020] The cryoablation catheter for the system of the present invention essentially includes a capillary tube that is connected with, and extends coaxially from a supply tube. Together, the connected supply and capillary tubes are positioned in the lumen of a catheter tube and are oriented coaxially with the catheter tube. More specifically, the supply tube and the capillary tube each have a distal end and a proximal end and, in combination, the proximal end of the capillary tube is connected to the distal end of the supply tube to establish a supply line for the catheter.
[0021] For the construction of the cryoablation catheter, the supply tube and the capillary tube are concentrically (coaxially) positioned inside the lumen of the catheter tube. Further, the distal end of the capillary tube (i.e. the distal end of the supply line) is positioned at a closed-in tip section at the distal end of the catheter tube. Thus, in addition to the supply line, this configuration also defines a return line in the lumen of the catheter tube that is located between the inside surface of that catheter tube and the supply line. In particular, the return line extends from the tip section at the distal end of the catheter tube, back to the proximal end of the catheter tube.
[0022] Insofar as the supply line is concerned, it is an important aspect of the present invention that the impedance to fluid flow of the primary refrigerant in the supply line be relatively low through the supply tube, as compared with the impedance presented by the capillary tube. Stated differently, it is desirable for the pressure drop, and consequently the temperature reduction, on the primary refrigerant be minimized as it traverses the supply tube. On the other hand, the pressure drop and temperature reduction on the primary refrigerant should be maximized as the refrigerant traverses the capillary tube. Importantly, the physical dimensions of the supply tube, of the capillary tube, and of the catheter tube can be engineered to satisfy these requirements. It is also desirable to engineer the length of the capillary tube so that gases passing from the tip section, back through the return line do not impermissibly warm the capillary tube. By balancing these considerations, the dimensions of the supply line, the tip section and the return line, can all be predetermined.
[0023] As the fluid refrigerant is transferred from its source to the catheter supply line, it passes through the precooler. During this transfer, a control valve(s) is used to establish a working pressure (p w ) for the refrigerant. Also, a pressure sensor is provided to monitor the working pressure on the primary fluid refrigerant before the refrigerant enters the supply line at the proximal end of the catheter.
[0024] On the return side of the system, an exhaust unit is provided for removing the primary fluid from the tip section of the catheter. For the present invention, this exhaust unit consists of a vacuum pump that is attached in fluid communication with the return line at the proximal end of the catheter tube. A pressure sensor is also provided at this point to determine the pressure in the return line at the proximal end of the catheter tube (p r ).
[0025] In accordance with well known thermodynamic principles, when pressures at specific points in a system are known, fluid pressures at various other points in the system can be determined. For the present invention, because the supply line and return line are contiguous and have known dimensions, because “p w ” (working pressure) and “p r ” (return line pressure) can be determined and, further, because the fluid refrigerant experiences a phase change during the transition from p w to p r , it is possible to calculate pressures on the fluid refrigerant at points between the proximal end of the supply tube (inlet) and the proximal end of the catheter tube (outlet). In particular, it is possible to calculate an outflow pressure (p o ) for the fluid refrigerant as it exits from the distal end of the capillary tube into the tip section of the catheter.
[0026] The outflow pressure (p o ) for the fluid refrigerant can be determined in ways other than as just mentioned above. For one, a pressure sensor can be positioned in the tip section of the catheter near the distal end of the capillary tube to measure the outflow pressure (p o ) directly. Additionally, the system of the present invention can include a temperature sensor that is positioned in the tip section of the catheter to monitor the temperature of the primary fluid refrigerant in the tip section (T t ). Specifically, when this temperature (T t ) is measured as the primary fluid refrigerant is boiling (i.e. as it enters the tip section from the capillary tube), it is possible to directly calculate the outflow pressure (p o ) using well known thermodynamic relationships.
[0027] A computer is used with the system of the present invention to monitor and control the operational conditions of the system. Specifically, the computer is connected to the appropriate sensors that monitor actual values for “p r ” and “p w ”. The values for “p r “and “p w ” can then be used to determine the outflow pressure “p o ” in the tip section of the catheter (for one embodiment of the present invention, “p o ” is also measured directly). Further, the computer is connected to the control valve to manipulate the control valve and vary the working pressure (p w ) on the primary fluid. At the same time, the computer can monitor the temperature in the tip section of the catheter (T t ) to ensure that changes in the working pressure “p w ” result in appropriate changes in “T t ”. Stated differently, the computer can monitor conditions to ensure that an unwanted increase in “back pressure,” that would be caused by an inappropriate increase in “p w ” does not result in an increase in “T t ”. The purpose here is to maintain the outflow pressure (p o ) in the tip section of the catheter at a desired value (e.g. 15 psia).
[0028] In operation, the sub-cooled primary fluid is introduced into the proximal end of the capillary tube at substantially the working pressure (p w ). The primary fluid then traverses the capillary tube for outflow from the distal end of the capillary tube at the outflow pressure (p o ). Importantly, in the capillary tube the fluid refrigerant is subjected to a pressure differential (Δp). In this case, “Δp” is substantially the difference between the working pressure (p w ) on the primary fluid as it enters the proximal end of the capillary tube (e.g. 300 psi), and a substantially ambient pressure (i.e. p o ) as it outflows from the distal end of the capillary tube (e.g. one atmosphere, 15 psi)(Δp=p w −p o ). In particular, as the pre-cooled primary fluid passes through the capillary tube, it transitions from a sub-cool temperature that is equal to approximately minus forty degrees Centigrade (T sc ≅−40° C.), to approximately its normal boiling point temperature. As defined above, the normal boiling point temperature of a fluid is taken to be the temperature at which the fluid boils under one atmosphere of pressures. In the case of nitrous oxide, this will be a cryoablation temperature that is equal to approximately minus eighty-eight degrees Centigrade (T ca ≅−88° C.). The heat that is absorbed by the primary fluid as it boils, cools the tip section of the catheter.
BRIEF DESCRIPTION OF THE DRAWINGS
[0029] The novel features of this invention, as well as the invention itself, both as to its structure and its operation, will be best understood from the accompanying drawings, taken in conjunction with the accompanying description, in which similar reference characters refer to similar parts, and in which:
[0030] FIG. 1 is a schematic of a first embodiment of the apparatus of the present invention, using a pressure bottle as the primary refrigerant source;
[0031] FIG. 2 is a schematic of a second embodiment of the apparatus of the present invention, using a compressor as the primary refrigerant source;
[0032] FIG. 3 is a schematic of a third embodiment of the apparatus of the present invention, using two compressors connected in series as the primary refrigerant source;
[0033] FIG. 4 is a schematic of a first embodiment of a control system apparatus according to the present invention, for use with the apparatus shown in FIG. 1 ;
[0034] FIG. 5 is a schematic of a second embodiment of a control system apparatus according to the present invention, for use with the apparatus shown in FIG. 2 or 3 ;
[0035] FIG. 6 is a schematic of a parameter display for use with the control equipment of the present invention; and
[0036] FIG. 7 is a flow diagram showing one control sequence for use with the control apparatus of the present invention.
[0037] FIG. 8 is a perspective view of the system of the present invention;
[0038] FIG. 9 is a cross-sectional view of the catheter of the present invention as seen along the line 2 - 2 in FIG. 8 ;
[0039] FIG. 10 is a schematic view of the computer and its interaction with system components and sensors for use in the control of a cryoablation procedure;
[0040] FIG. 11 is a schematic view of the interactive components in the console of the present invention;
[0041] FIG. 12 is a pressure-temperature diagram (not to scale) graphing an open-cycle operation for a refrigerant fluid in accordance with the present invention; and
[0042] FIG. 13 is a diagram (not to scale) showing the tendency for changes in temperature response to changes of fluid mass flow rate in a catheter environment as provided by the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0043] According to certain embodiments of the invention, the refrigeration system may be a two stage Joule-Thomson system with a closed loop precool circuit and either an open loop or a closed loop primary circuit. A typical refrigerant for the primary circuit would be R-508b, and a typical refrigerant for the precool circuit would be R-410a. In the ablation mode, the system may be capable of performing tissue ablation at or below minus 70.degree. C. while in contact with the tissue and circulating blood. In the mapping mode, the system may be capable of mapping by stunning the tissue at a temperature between minus 10.degree. C. and minus 18.degree. C. while in contact with the tissue and circulating blood. These performance levels may be achieved while maintaining the catheter tip pressure at or below a sub-diastolic pressure of 14 psia.
[0044] As shown in FIG. 1 , one embodiment of the apparatus 10 of the present invention is an open loop system using a pressure bottle for the refrigerant source. Such a system can include a primary refrigerant supply bottle 200 , a primary refrigerant fluid controller 208 , a catheter 300 , a primary refrigerant recovery bottle 512 , a secondary refrigerant compressor 100 , a precool heat exchanger 114 , and various sensors. In certain embodiments, all but the catheter 300 and the precool heat exchanger 114 may be located in a cooling console housing. The precool heat exchanger 114 is connected to the console by flexible lines 121 , 221 . Pressure of the refrigerant in the primary refrigerant supply bottle 200 is monitored by a primary refrigerant supply pressure sensor 202 . Output of primary refrigerant from the supply bottle 200 is regulated by a pressure regulator 204 , which, in certain embodiments, can receive refrigerant from the bottle 200 at a pressure above 350 psia and regulate it to less than 350 psia. A primary refrigerant relief valve 206 is provided to prevent over pressurization of the primary system downstream of the pressure regulator 204 , for example, above 400 psia. The flow rate of primary refrigerant is controlled by the fluid controller 208 , which can be either a pressure controller or a flow controller. A feedback loop may be provided to control the operation of the fluid controller 208 . The feedback signal for the fluid controller 208 can come from a pressure sensor 310 or a flow sensor 311 , on the effluent side of the catheter 300 , discussed below.
[0045] A primary refrigerant high pressure sensor 210 is provided downstream of the fluid controller 208 , to monitor the primary refrigerant pressure applied to the precool heat exchanger 114 . The high pressure side 212 of the primary loop passes through the primary side of the cooling coil of the precool heat exchanger 114 , then connects to a quick connect fitting 304 on the precool heat exchanger 114 . Similarly, the low side quick connect fitting 304 on the precool heat exchanger 114 is connected to the low pressure side 412 of the primary loop, which passes back through the housing of the precool heat exchanger 114 , without passing through the cooling coil, and then through the flow sensor 311 . The catheter tip pressure sensor 310 monitors catheter effluent pressure in the tip of the catheter 300 . The control system maintains catheter tip pressure at a sub-diastolic level at all times.
[0046] The low pressure side 412 of the primary loop can be connected to the inlet 402 of a vacuum pump 400 . A primary refrigerant low pressure sensor 410 monitors pressure in the low side 412 of the primary loop downstream of the precool heat exchanger 114 . The outlet 404 of the vacuum pump 400 can be connected to the inlet 502 of a recovery pump 500 . A 3 way, solenoid operated, recovery valve 506 is located between the vacuum pump 400 and the recovery pump 500 . The outlet 504 of the recovery pump 500 is connected to the primary refrigerant recovery bottle 512 via a check valve 508 . A primary refrigerant recovery pressure sensor 510 monitors the pressure in the recovery bottle 512 . A 2 way, solenoid operated, bypass valve 406 is located in a bypass loop 407 between the low side 412 of the primary loop upstream of the vacuum pump 400 and the high side 212 of the primary loop downstream of the fluid controller 208 . A solenoid operated bypass loop vent valve 408 is connected to the bypass loop 407 .
[0047] In the catheter 300 , the high pressure primary refrigerant flows through an impedance device such as a capillary tube 306 , then expands into the distal portion of the catheter 300 , where the resultant cooling is applied to surrounding tissues. A catheter tip temperature sensor 307 , such as a thermocouple, monitors the temperature of the distal portion of the catheter 300 . A catheter return line 308 returns the effluent refrigerant from the catheter 300 to the precool heat exchanger 114 . The high and low pressure sides of the catheter 300 are connected to the heat exchanger quick connects 304 by a pair of catheter quick connects 302 . As an alternative to pairs of quick connects 302 , 304 , coaxial quick connects can be used. In either case, the quick connects may carry both refrigerant flow and electrical signals.
[0048] In the precool loop, compressed secondary refrigerant is supplied by a precool compressor 100 . An after cooler 106 can be connected to the outlet 104 of the precool compressor 100 to cool and condense the secondary refrigerant. An oil separator 108 can be connected in the high side 117 of the precool loop, with an oil return line 110 returning oil to the precool compressor 100 . A high pressure precooler pressure sensor 112 senses pressure-in the high side 117 of the precool loop. The high side 117 of the precool loop is connected to an impedance device such as a capillary tube 116 within the housing of the precool heat exchanger 114 . High pressure secondary refrigerant flows through the capillary tube 116 , then expands into the secondary side of the cooling coil of the precool heat exchanger 114 , where it cools the high pressure primary refrigerant. The effluent of the secondary side of the precool heat exchanger 114 returns via the low side 118 of the precool loop to the inlet 102 of the precool compressor 100 . A low pressure precooler pressure sensor 120 senses pressure in the low side 118 of the precool loop.
[0049] Instead of using primary refrigerant supply and return bottles, the apparatus can use one or more primary compressors in a closed loop system. FIG. 2 shows a second embodiment of the apparatus of the present invention, with a single compressor system. This embodiment would be appropriate in applications where the high side and low side pressures can be adequately controlled with a single compressor. In the apparatus 10 ′ of this type of system, the low side 622 of the primary loop conducts the effluent of the catheter 300 to the inlet 602 of a primary refrigerant compressor 600 . The compressor 600 compresses the primary refrigerant, and returns it from the compressor outlet 604 via the high side 612 of the primary loop to the primary side of the precool heat exchanger 114 . A primary refrigerant high pressure sensor 614 is provided in the high side 612 of the primary loop, to monitor the primary refrigerant pressure applied to the precool heat exchanger 114 . A primary refrigerant high pressure flow sensor 312 can be provided in the high side 612 of the primary loop. A primary refrigerant low pressure sensor 610 monitors pressure in the low side 622 of the primary loop downstream of the precool heat exchanger 114 . A primary loop filter 608 can be provided in the low side 622 of the primary loop. A 2way, solenoid operated, primary refrigerant charge valve 626 and a primary refrigerant reservoir 628 can be provided in the low side 622 of the primary loop. A high pressure after-cooler 605 can be provided downstream of the primary refrigerant compressor 600 .
[0050] As further shown in FIG. 2 , a 2 way, solenoid operated, primary loop bypass valve 606 is located in a bypass loop 607 between the low side 622 of the primary loop upstream of the compressor 600 and the high side 612 of the primary loop downstream of the compressor 600 . Opening of the primary loop bypass valve 606 can facilitate startup of the primary compressor 600 . A precool loop filter 101 can be provided in the low side 118 of the precool loop. Further, a 2 way, solenoid operated, precool loop bypass valve 111 is located in a bypass loop 119 between the low side 118 of the precool loop upstream of the compressor 100 and the high side 117 of the precool loop downstream of the compressor 100 . Opening of the precool loop bypass valve 111 can facilitate startup of the precool compressor 100 .
[0051] A purification system 900 can be provided for removing contaminants from the primary refrigerant and the secondary refrigerant. Solenoid operated 3 way purification valves 609 , 611 are provided in the high side and low side, respectively, of the primary loop, for selectively directing the primary refrigerant through the purification system 900 . Similarly, solenoid operated 3 way purification valves 115 , 113 are provided in the high side and low side, respectively, of the precool loop, for selectively directing the secondary refrigerant through the purification system 900 .
[0052] The remainder of the precool loop, the precool heat exchanger 114 , and the catheter 300 are the same as discussed above for the first embodiment.
[0053] In applications where separate low side and high side pressure control is required, but where a closed loop system is desired, a two compressor primary system may be used. FIG. 3 shows a third embodiment of the apparatus of the present invention, with a dual compressor system. In the apparatus 10 ″ of this type of system, the low side 622 of the primary loop conducts the effluent of the catheter 300 to the inlet 616 of a low side primary refrigerant compressor 618 . The low side compressor 618 compresses the primary refrigerant, and provides it via its outlet 620 to the inlet 602 of a high side primary refrigerant compressor 600 . A low pressure after-cooler 623 can be provided downstream of the low side compressor 618 . The high side compressor 600 further compresses the primary refrigerant to a higher pressure and returns it via its outlet 604 and via the high side 612 of the primary loop to the primary side of the precool heat exchanger 114 . A primary refrigerant high pressure sensor 614 is provided in the high side 612 of the primary loop, to monitor the high side primary refrigerant pressure upstream of the precool heat exchanger 114 . A primary refrigerant low pressure sensor 610 monitors pressure in the low side 622 of the primary loop downstream of the precool heat exchanger 114 . A primary refrigerant intermediate pressure sensor 624 monitors pressure between the outlet 620 of the low side compressor 618 and the inlet 602 of the high side compressor 600 . The high side compressor 600 and the low side compressor 618 are separately controlled, using feedback from the catheter tip pressure sensor 310 and/or the flow sensors 311 , 312 .
[0054] As further shown in FIG. 3 , a 3 way, solenoid operated, bypass valve 606 ′ is located in a bypass loop 607 between the low side 622 of the primary loop upstream of the low side compressor 618 and the high side 612 of the primary loop downstream of the high side compressor 600 . A third port is connected between the high side and low side compressors. The precool loop, the precool heat exchanger 114 , and the catheter 300 are the same as discussed above for the first and second embodiments.
[0055] FIG. 4 shows a control diagram which would be suitable for use with the apparatus shown in FIG. 1 . A computerized automatic control system 700 is connected to the various sensors and control devices to sense and control the operation of the system, and to provide safety measures, such as shut down schemes. More specifically, on the sensing side, the low pressure precool sensor 120 inputs low side precool pressure PA, the high pressure precool sensor 112 inputs high side precool pressure PB, the primary supply pressure sensor 202 inputs supply bottle pressure P 1 , the primary recovery pressure sensor 510 inputs recovery bottle pressure P 2 , the high pressure primary sensor 210 inputs high side primary pressure P 3 , the low pressure primary sensor 410 inputs low side primary pressure P 4 , the catheter tip pressure sensor 310 inputs catheter tip pressure P 5 , the temperature sensor 307 inputs catheter tip temperature T, and the flow sensor 311 inputs primary refrigerant flow rate F. Further, on the control side, the control system 700 energizes the normally closed bypass valve 406 to open it, energizes the normally open vent valve 408 to close it, and energizes the recovery valve 506 to connect the vacuum pump outlet 404 to the recovery pump inlet 502 . Finally, the control system 700 provides a pressure set point SPP or flow rate set point SPF to the fluid controller 208 , depending upon whether it is a pressure controller or a flow controller.
[0056] FIG. 5 shows a control diagram which would be suitable for use with the apparatus shown in FIG. 2 or FIG. 3 . A computerized automatic control system 700 is connected to the various sensors and control devices to sense and control the operation of the system, and to provide safety measures, such as shut down schemes. More specifically, on the sensing side, the low pressure precool sensor 120 inputs low side precool pressure PA, the high pressure precool sensor 112 inputs high side precool pressure PB, the high pressure primary sensor 614 inputs high side primary pressure P 3 , the low pressure primary sensor 610 inputs low side primary pressure P 4 , the catheter tip pressure sensor 310 inputs catheter tip pressure P 5 , the temperature sensor 307 inputs catheter tip temperature T, and the flow sensors 311 , 312 input primary refrigerant flow rate F. Further, on the control side, the control system 700 energizes the normally closed primary loop bypass valve 606 , 606 ′ to open it, and the control system 700 energizes the normally closed precool loop bypass valve 111 to open it. The control system 700 also energizes the primary loop purification valves 609 , 611 to selectively purify the primary refrigerant, and the control system 700 energizes the precool loop purification valves 113 , 115 to selectively purify the secondary refrigerant. Finally, the control system 700 provides a minimum high side pressure set point PL 2 to the controller 601 of the primary compressor 600 in the system shown in FIG. 2 . Alternatively, in the system shown in FIG. 3 , the control system 700 provides a minimum high side pressure set point PL 2 B to the controller 601 of the high side primary compressor 600 , and the control system 700 provides a maximum low side pressure set point PL 2 A to the controller 619 of the low side primary compressor 618 .
[0057] A numeric digital display, or a graphical display similar to that shown in FIG. 6 , is provided on the cooling console to assist the operator in monitoring and operating the system. For example, on a single graphical display, graphs can be shown of catheter tip temperature T, high side primary pressure P 3 , low side primary pressure P 4 , and primary flow rate F, all versus time. Further, on the same display, the operator can position a vertical cursor at a selected time, resulting in the tabular display of the instantaneous values of T, P 3 , P 4 , and F, as well as the average, maximum, and minimum values of these parameters.
[0058] The present invention will now be further illustrated by describing a typical operational sequence of the open loop embodiment, showing how the control system 700 operates the remainder of the components to start up the system, to provide the desired refrigeration power, and to provide system safety. The system can be operated in the Mapping Mode, where the cold tip temperature might be maintained at minus 10 C., or in the Ablation Mode, where the cold tip temperature might be maintained at minus 65 C. Paragraphs are keyed to the corresponding blocks in the flow diagram shown in FIG. 7 . Suggested exemplary Pressure Limits used below could be PL 1 =160 psia; PL 2 =400 psia; PL 3 =500 psia; PL 4 =700 psia, PL 5 =600 psia; PL 6 =5 psia; PL 7 =diastolic pressure; PL 8 =375 psia; and PL 9 =5 psia. Temperature limits, flow limits, procedure times, and procedure types are set by the operator according to the procedure being performed.
[0059] Perform self tests (block 802 ) of the control system circuitry and connecting circuitry to the sensors and controllers to insure circuit integrity.
[0060] Read and store supply cylinder pressure P 1 , primary low pressure P 4 , and catheter tip pressure P 5 (block 804 ). At this time, P 4 and P 5 are at atmospheric pressure. If P 1 is less than Pressure Limit PL 2 (block 808 ), display a message to replace the supply cylinder (block 810 ), and prevent further operation. If P 1 is greater than PL 2 , but less than Pressure Limit PL 3 , display a message to replace the supply cylinder soon, but allow operation to continue.
[0061] Read precool charge pressure PB and recovery cylinder pressure P 2 (block 806 ). If PB is less than Pressure Limit PL 1 (block 808 ), display a message to service the precool loop (block 810 ), and prevent further operation. If P 2 is greater than Pressure Limit PL 4 (block 808 ), display a message to replace the recovery cylinder (block 810 ), and prevent further operation. If P 2 is less than PL 4 , but greater than Pressure Limit PL 5 , display a message to replace the recovery cylinder soon, but allow operation to continue.
[0062] Energize the bypass loop vent valve 408 (block 812 ). The vent valve 408 is a normally open two way solenoid valve open to the atmosphere. When energized, the vent valve 408 is closed.
[0063] Start the precool compressor 100 (block 814 ). Display a message to attach the catheter 300 to the console quick connects 304 (block 816 ). Wait for the physician to attach the catheter 300 , press either the Ablation Mode key or the Mapping Mode key, and press the Start key (block 818 ). Read the catheter tip temperature T and the catheter tip pressure P 5 . At this time, T is the patient's body temperature and P 5 is atmospheric pressure.
[0064] Energize the bypass loop valve 406 , while leaving the recovery valve 506 deenergized (block 820 ). The bypass valve 406 is a normally closed 2 way solenoid valve. Energizing the bypass valve 406 opens the bypass loop. The recovery valve 506 is a three way solenoid valve that, when not energized, opens the outlet of the vacuum pump 400 to atmosphere. Start the vacuum pump 400 (block 822 ). These actions will pull a vacuum in the piping between the outlet of the fluid controller 208 and the inlet of the vacuum pump 400 , including the high and low pressure sides of the catheter 300 . Monitor P 3 , P 4 , and P 5 (block 824 ), until all three are less than Pressure Limit PL 6 (block 826 ).
[0065] Energize the recovery valve 506 and the recovery pump 500 (block 828 ). When energized, the recovery valve 506 connects the outlet of the vacuum pump 400 to the inlet of the recovery pump 500 . De-energize the bypass valve 406 , allowing it to close (block 830 ). Send either a pressure set point SPP (if a pressure controller is used) or a flow rate set point SPF (if a flow controller is used) to the fluid controller 208 (block 832 ). Where a pressure controller is used, the pressure set point SPP is at a pressure which will achieve the desired refrigerant flow rate, in the absence of plugs or leaks. The value of the set point is determined according to whether the physician has selected the mapping mode or the ablation mode. These actions start the flow of primary refrigerant through the catheter 300 and maintain the refrigerant flow rate at the desired level.
[0066] Continuously monitor and display procedure time and catheter tip temperature T (block 834 ). Continuously monitor and display all pressures and flow rates F (block 836 ). If catheter tip pressure P 5 exceeds Pressure Limit PL 7 , start the shutdown sequence (block 840 ). Pressure Limit PL 7 is a pressure above which the low pressure side of the catheter 300 is not considered safe.
[0067] If F falls below Flow Limit FL 1 , and catheter tip temperature T is less than Temperature Limit TL 1 , start the shutdown sequence (block 840 ). Flow Limit FL 1 is a minimum flow rate below which it is determined that a leak or a plug has occurred in the catheter 300 . FL 1 can be expressed as a percentage of the flow rate set point SPF. Temperature Limit TL 1 is a temperature limit factored into this decision step to prevent premature shutdowns before the catheter 300 reaches a steady state at the designed level of refrigeration power. So, if catheter tip temperature T has not yet gone below TL 1 , a low flow rate will not cause a shutdown.
[0068] If P 3 exceeds Pressure Limit PL 8 , and F is less than Flow Limit FL 2 , start the shutdown sequence (block 840 ). PL 8 is a maximum safe pressure for the high side of the primary system. Flow Limit FL 2 is a minimum flow rate below which it is determined that a plug has occurred in the catheter 300 , when PL 8 is exceeded. FL 2 can be expressed as a percentage of the flow rate set point SPF.
[0069] If P 4 is less than Pressure Limit PL 9 , and F is less than Flow Limit FL 3 , start the shutdown sequence (block 840 ). PL 9 is a pressure below which it is determined that a plug has occurred in the catheter 300 , when flow is below FL 3 . FL 3 can be expressed as a percentage of the flow rate set point SPF.
[0070] An exemplary shutdown sequence will now be described. Send a signal to the fluid controller 208 to stop the primary refrigerant flow (block 840 ). Energize the bypass valve 406 to open the bypass loop (block 842 ). Shut off the precool compressor 100 (block 844 ). Continue running the vacuum pump 400 to pull a vacuum between the outlet of the fluid controller 208 and the inlet of the vacuum pump 400 (block 846 ). Monitor primary high side pressure P 3 , primary low side pressure P 4 , and catheter tip pressure P 5 (block 848 ) until all three are less than the original primary low side pressure which was read in block 804 at the beginning of the procedure (block 850 ). Then, de-energize the recovery pump 500 , recovery valve 506 , vent valve 408 , bypass valve 406 , and vacuum pump 400 (block 852 ). Display a message suggesting the removal of the catheter 300 , and update a log of all system data (block 854 ).
[0071] Similar operational procedures, safety checks, and shutdown procedures would be used for the closed loop primary system shown in FIG. 2 or FIG. 3 , except that the primary compressor 600 or compressors 600 , 618 would provide the necessary primary refrigerant flow rate in place of the supply and recovery cylinders, the fluid controller, and the vacuum and recovery pumps. As with the open loop system, the closed loop system can be operated in the Mapping Mode, where the cold tip temperature might be maintained at minus 10 C., or in the Ablation Mode, where the cold tip temperature might be maintained at minus 65 C. As a first option to achieve the desired cold tip temperature, the precool bypass valve 111 can be adjusted to control the liquid fraction resulting after expansion of the secondary refrigerant, thereby adjusting the refrigeration capacity. Under this option, primary refrigerant high and low pressures are kept constant. As a second option, or in combination with the first option, primary refrigerant flow rate can be by means of operating controllers 601 , 619 on the primary compressors 600 , 618 to maintain a high pressure set point SPP which will achieve the desired flow rate, resulting in the desired cold tip temperature.
[0072] A Service Mode is possible, for purification of the primary and secondary refrigerants. In the Service Mode, the normally open bypass valves 111 , 606 are energized to close. The primary loop purification valves 609 , 611 are selectively aligned with the purification system 900 to purify the primary refrigerant, or the precool loop purification valves 113 , 115 are selectively aligned with the purification system 900 to purify the secondary refrigerant.
[0073] In either the Mapping Mode or the Ablation Mode, the desired cold tip temperature control option is input into the control system 700 . Further, the type of catheter is input into the control system 700 . The normally closed charge valve 626 is energized as necessary to build up the primary loop charge pressure. If excessive charging is required, the operator is advised. Further, if precool loop charge pressure is below a desired level, the operator is advised.
[0074] When shutdown is required, the primary loop high side purification valve 609 is closed, and the primary loop compressors 600 , 618 continue to run, to draw a vacuum in the catheter 300 . When the desired vacuum is achieved, the primary loop low side purification valve 611 is closed. This isolates the primary loop from the catheter 300 , and the disposable catheter 300 can be removed.
[0075] Referring to FIG. 8 , a system for performing cryoablation procedures is shown and generally designated 910 . As shown, the system 910 includes a cryoablation catheter 912 and a primary fluid source 914 . Preferably, the primary fluid is nitrous oxide (N 2 O) and is held in source 914 at a pressure of around 750 psig. FIG. 8 also shows that the system 910 includes a console 916 and that the console 916 is connected in fluid communication with the primary fluid source 914 via a fluid line 918 . Console 916 is also connected in fluid communication with the catheter 912 via a fluid line 920 . Further, the console 916 is shown to include a precooler 922 , an exhaust unit 924 , and a computer 926 .
[0076] In detail, the components of the catheter 912 will be best appreciated with reference to FIG. 9 . There, it will be seen that the catheter 912 includes a catheter tube 928 that has a closed distal end 930 and an open proximal end 932 . Also included as part of the catheter 912 , are a supply tube 934 that has a distal end 936 and a proximal end 938 , and a capillary tube 940 that has a distal end 942 and a proximal end 944 . As shown, the distal end 936 of supply tube 934 is connected with the proximal end 944 of the capillary tube 940 to establish a supply line 946 . Specifically, supply line 946 is defined by the lumen 948 of supply tube 934 and the lumen 950 of capillary tube 940 . It is an important aspect of the system 910 that the diameter (i.e. cross section) of the supply tube 934 is greater than the diameter (i.e. cross section) of the capillary tube 940 . The consequence of this difference is that the supply tube 934 presents much less impedance to fluid flow than does the capillary tube 940 . In turn, this causes a much greater pressure drop for fluid flow through the capillary tube 940 . As will be seen, this pressure differential is used to advantage for the system 910 .
[0077] Still referring to FIG. 9 , it is seen that the supply line 946 established by the supply tube 934 and capillary tube 940 , is positioned coaxially in the lumen 952 of the catheter tube 928 . Further, the distal end 942 of the capillary tube 940 (i.e. also the distal end of the supply line 946 ) is displaced from the distal end 930 of catheter tube 928 to create an expansion chamber 954 in the tip section 956 of the catheter 912 . Additionally, the placement of the supply line 946 in the lumen 952 establishes a return line 958 in the catheter 912 that is located between the supply line 946 and the wall of the catheter tube 928 .
[0078] Optionally, a sensor 960 can be mounted in expansion chamber 954 (tip section 956 ). This sensor 960 may be either a temperature sensor or a pressure sensor, or it may include both a temperature and pressure sensor. In any event, if used, the sensor 960 can be of a type well known in the art for detecting the desired measurement. Although FIG. 9 shows both a pressure sensor 962 and a valve 964 positioned at the proximal end 938 of the supply tube 934 , this is only exemplary as the sensor 962 and valve 964 may actually be positioned elsewhere. The import here is that a pressure sensor 962 is provided to monitor a working fluid pressure, “p w, ” on a fluid refrigerant (e.g. N 2 O). In turn, this pressure “p w ” is controlled by a valve 964 as it enters the inlet 966 of the supply line 946 . Further, FIG. 9 shows that a pressure sensor 968 is provided to monitor a return pressure “p r ” on the fluid refrigerant as it exits from the outlet 970 of the return line 958 .
[0079] FIG. 10 indicates that the various sensors mentioned above are somehow electronically connected to the computer 926 in console 916 . More specifically, the sensors 960 , 962 and 968 can be connected to computer 926 in any of several ways, all known in the pertinent art. Further, FIG. 10 indicates that the computer 926 is operationally connected with the valve 964 . The consequence of this is that the computer 926 can be used to control operation of the valve 964 , and thus the working pressure “p w ”, in accordance with preprogrammed instructions, using measurements obtained by the sensors 960 , 962 and 968 (individually or collectively).
[0080] A schematic of various components for system 910 is presented in FIG. 11 which indicates that a compressor 972 is incorporated as an integral part of the precooler 922 . More specifically, the compressor 972 is used to compress a secondary fluid refrigerant (e.g. Freon) into its liquid phase for subsequent cooling of the primary refrigerant in the precooler 922 . For purposes of the present invention, the secondary fluid refrigerant will have a normal boiling point that is at a temperature sufficiently low to take the primary fluid refrigerant to a sub-cool condition (i.e. below a temperature where the primary fluid refrigerant will be fully saturated). For the present invention, wherein the primary fluid refrigerant is nitrous oxide, the temperature is preferably around minus forty degrees Centigrade (T sc =−40° C.).
[0081] The operation of system 910 will be best appreciated by cross referencing FIG. 11 with FIG. 12 . During this cross referencing, recognize that the alphabetical points (A, B, C, D and E), shown relative to the curve 974 in FIG. 12 , are correspondingly shown on the schematic for system 910 in FIG. 11 . Further, appreciate that curve 974 , which is plotted for variations of pressure (P) and temperature (T), represents the fully saturated condition for the primary fluid refrigerant (e.g. nitrous oxide). Accordingly, the area 976 represents the liquid phase of the refrigerant, and area 978 represents the gaseous phase of the refrigerant.
[0082] Point A ( FIG. 11 and FIG. 12 ) represents the primary fluid refrigerant as it is drawn from the fluid source 914 , or its back up source 914 ′. Preferably, point A corresponds to ambient temperature (i.e. room temperature) and a pressure greater than around 700 psig. After leaving the fluid source 914 , the pressure on the refrigerant is lowered to a working pressure “p w ” that is around 400 psig. This change is controlled by the regulator valve 964 , is monitored by the sensor 962 , and is represented in FIG. 12 as the change from point A to point B. The condition at point B corresponds to the condition of the primary refrigerant as it enters the precooler 922 .
[0083] In the precooler 922 , the primary refrigerant is cooled to a sub-cool temperature “T sc ” (e.g. −40° C.) that is determined by the boiling point of the secondary refrigerant in the precooler 922 . In FIG. 12 this cooling is represented by the transition from point B to point C. Note that in this transition, as the primary fluid refrigerant passes through the precooler 922 , it changes from a gaseous state (area 978 ) into a liquid state (area 976 ). Point C in FIG. 12 represents the condition of the primary fluid refrigerant as it enters the supply line 946 of cryocatheter 12 at the proximal end 938 of supply tube 934 . Specifically, the pressure on the primary fluid refrigerant at this point C is the working pressure “p w ”, and the temperature is the sub-cool temperature “T sc ”.
[0084] As the primary fluid refrigerant passes through the supply line 946 of catheter 12 , its condition changes from the indications of point C, to those of point D. Specifically, for the present invention, point D is identified by a temperature of around minus eighty eight degrees Centigrade (−88° C.) and an outlet pressure “p o ” that is close to 15 psia. Further, as indicated in FIG. 11 , point D identifies the conditions of the primary fluid refrigerant after it has boiled in the tip section 956 as it is leaving the supply line 946 and entering the return line 958 of the catheter 12 .
[0085] The exhaust unit 924 of the catheter 912 is used to evacuate the primary fluid refrigerant from the expansion chamber 954 of tip section 956 after the primary refrigerant has boiled. During this evacuation, the conditions of the primary refrigerant change from point D to point E. Specifically, the conditions at point E are such that the temperature of the refrigerant is an ambient temperature (i.e. room temperature) and it has a return pressure “p r ”, measured by the sensor 968 , that is slightly less than “p o ”. For the transition from point D to point E, the main purpose of the exhaust unit 924 is to help maintain the outlet pressure “p o ” in the tip section 956 as near to one atmosphere pressure as possible.
[0086] Earlier it was mentioned that the mass flow rate of the primary fluid refrigerant as it passes through the catheter 912 has an effect on the operation of the catheter 912 . Essentially this effect is shown in FIG. 13 . There it will be seen that for relatively low mass flow rates (e.g. below point F on curve 980 shown in FIG. 13 ), increases in the mass flow rate of the refrigerant will cause lower temperatures. Refrigerant flow in this range is said to be “refrigeration limited.” On the other hand, for relatively high mass flow rates (i.e. above point F), increases in the mass flow rate actually cause the temperature of the refrigerant to rise. Flow in this range is said to be “surface area limited.” Because the system 910 is most efficient at the lowest temperature for the refrigerant, operation at point F is preferred. Accordingly, by monitoring the temperature of the refrigerant in the tip section 956 , “T t ”, variations of T t can be used to control the mass flow rate of the refrigerant, to thereby control the refrigeration potential of the catheter 912 .
[0087] In operation, the variables mentioned above (p w , p o , p r , and T t ) can be determined as needed. System 910 then manipulates the regulator valve 964 , in response to whatever variables are being used, to vary the working pressure “p w ” of the primary fluid refrigerant as it enters the supply line 946 . In this way, variations in “p w ” can be used to control “p o ” and, consequently, the refrigeration potential of the catheter 912 .
[0088] While the particular invention as herein shown and disclosed in detail is fully capable of obtaining the objects and providing the advantages herein before stated, it is to be understood that it is merely illustrative of the presently preferred embodiments of the invention and that no limitations are intended to the details of construction or design herein shown other than as described in the appended claims. | An apparatus and method for automatic operation of a refrigeration system to provide refrigeration power to a catheter for tissue ablation or mapping. The primary refrigeration system can be open loop or closed loop, and a precool loop will typically be closed loop. Equipment and procedures are disclosed for bringing the system to the desired operational state, for controlling the operation by controlling refrigerant flow rate, for performing safety checks, and for achieving safe shutdown. The catheter-based system for performing a cryoablation procedure uses a precooler to lower the temperature of a fluid refrigerant to a sub-cool temperature (−40° C.) at a working pressure (400 psi). The sub-cooled fluid is then introduced into a supply line of the catheter. Upon outflow of the primary fluid from the supply line, and into a tip section of the catheter, the fluid refrigerant boils at an outflow pressure of approximately one atmosphere, at a temperature of about −88° C. In operation, the working pressure is computer controlled to obtain an appropriate outflow pressure for the coldest possible temperature in the tip section. | 5 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This is a divisional application of U.S. patent application Ser. No. 10/117,518, filed Apr. 4, 2002, entitled: A Proximity Latch Mechanism Using an Impact Rebound Crash Stop for an Outside Disk Ramp Loading Disk Drive.
TECHNICAL FIELD
[0002] This invention relates to latch mechanisms used in parking read-write heads outside the disk media surface(s).
BACKGROUND ART
[0003] Disk drives are an important data storage technology based on several crucial components including disk media surfaces and read-write heads. When in operation, rotation of disk media surfaces, with respect to the read-write heads, causes each read-write head to float a small distance off the disk media surface it accesses. However, for a variety of reasons, disk media surfaces frequently stop rotating when not in operation for awhile.
[0004] When the disk media surface is not rotating with respect to the read-write head, mechanical vibrations acting upon the disk drive can cause the read-write head to collide with the disk media surface, unless they are separated.
[0005] This separation is often referred to as “parking” the read-write heads. Parking the read-write heads minimizes the possibility of damaging the disk media surfaces and/or the read-write heads due to these mechanical collisions. Often such parking mechanisms include a ramp on which the head slider(s) are “parked” and a latch mechanism. The purpose of the latch mechanism is to minimize the chance that the actuator will accidentally leave the parking ramp outside the disk media surface and potentially damage the disk media surface(s).
[0006] [0006]FIG. 1A illustrates a typical prior art high capacity disk drive 10 including actuator arm 30 with voice coil 32 , actuator axis 40 , suspension or head arms 50 - 58 with slider/head unit 60 placed among the disks.
[0007] [0007]FIG. 1B illustrates a typical prior art high capacity disk drive 10 with actuator 20 , actuator arm 30 with voice coil 32 , actuator axis 40 , head arms 50 - 56 and slider/head units 60 - 66 with the disks removed.
[0008] Since the 1980's, high capacity disk drives 10 have used voice coil actuators 20 - 66 to position their read/write heads over specific tracks. The heads are mounted on head sliders 60 - 66 , which float a small distance off the disk drive surface when in operation. Often there is one head per head slider for a given disk drive surface. There are usually multiple heads in a single disk drive, but for economic reasons, usually only one voice coil actuator.
[0009] Voice coil actuators are further composed of a fixed magnet actuator 20 interacting with a time varying electromagnetic field induced by voice coil 32 to provide a lever action via actuator axis 40 . The lever action acts to move head arms 50 - 56 positioning head slider units 60 - 66 over specific tracks with remarkable speed and accuracy. Actuator arms 30 are often considered to include voice coil 32 , actuator axis 40 , head arms 50 - 56 and head sliders 60 - 66 . Note that actuator arms 30 may have as few as a single head arm 50 . Note also that a single head arm 52 may connect with two head sliders 62 and 64 .
[0010] While there are many forms of mechanical impact upon a disk drive, only rotary shock in actuator 30 's plane of motion can bring the read-write heads into collision with disk media surfaces once the read-write heads are parked. These rotary shocks will be described herein based upon a view defining clockwise and counterclockwise rotations with respect to the disk drive base, with a parking zone located to the right of the disk media surfaces as viewed from above the disk base. As will be apparent to one of skill in the art, it is just as possible for a disk drive to use a parking zone on the left of the disk media surfaces. While this is most certainly possible, the discussion hereafter will focus on a parking zone to the right to clarify the discussion. Such a clarification is not meant to limit the scope of the claims.
[0011] [0011]FIG. 1C illustrates a magnetic latch affixed to an actuator arm 30 of the prior art.
[0012] A magnet is affixed to the tail end of the voice coil 32 region, which when near a second magnet located in either the top yoke or bottom yolk of the fixed magnet region 20 , will tend to attract actuator 30 to a parking site often inside the disk media. Magnetic latches are used with Crash Start Stop (CSS) designs.
[0013] While they have been put into production in several circumstances, they place additional requirements on the voice coil actuators. This kind of latch requires additional actuator torque to exit from the parking zone. Further, these latches require sophisticated actuator speed control. Inside disk parking zones also tend to heat the read-write heads more. The read-write heads tend to suffer more frequent mechanical collisions with the disk surface.
[0014] The outside disk surface approach to parking read-write heads parks the read-write head or heads on a ramp outside the disk surface, removing and/or minimizing the possibility for contact when the disk is not in operation. Latch mechanisms provide at least some assurance that the actuator will remain parked with head sliders on the ramp even after mechanical shocks to the disk drive.
[0015] [0015]FIGS. 2A to 2 C illustrate the operation of a single lever inertial latch as found in the prior art.
[0016] [0016]FIG. 2A illustrates the prior art single level inertial latch mechanism including latch arm 100 pivoting about 102 and including latch hook 104 , mechanically fitting with actuator catch mechanism 106 , as well as latch stop 110 , and crash stop 90 , with the latch mechanism at rest.
[0017] Note that actuator 30 abuts crash stop 90 and that inertial latch arm 100 abuts latch stop 110 when the single-lever inertial latch is at rest. Slider 60 is in position on parking ramp 120 .
[0018] [0018]FIG. 2B illustrates the prior art single level inertial latch during a clockwise acceleration of actuator 30 .
[0019] In a clockwise acceleration, actuator 30 moves away from crash stop 90 and actuator catch mechanism 106 engages with inertial latch catch mechanism 104 .
[0020] [0020]FIG. 2C illustrates the prior art single level inertial latch during a counterclockwise acceleration of the actuator.
[0021] In a counterclockwise acceleration 130 , the latch may fail if the actuator 30 rebounds 132 from its crash stop 90 .
[0022] [0022]FIG. 3A illustrates a prior art example of a dual-lever inertial latch at rest.
[0023] When at rest, a magnet or spring, (which are not shown), biases the small latch arm 142 clockwise, holding the latch 144 - 152 open.
[0024] [0024]FIG. 3B illustrates a prior art example of a dual-lever inertial latch during a clockwise rotational acceleration of actuator 30 .
[0025] [0025]FIG. 3C illustrates a prior art example of a dual-lever inertial latch during a counterclockwise rotational acceleration of actuator 30 .
[0026] The large latch arm 140 rotates in opposite directions during the clockwise and counterclockwise motions of actuator arm 30 of FIGS. 3B and 3C, respectively. Motion of large latch arm 140 in either direction causes the small arm 142 to rotate counterclockwise to the close position. This dual lever action prevents a rebound of actuator arm 30 off the crash stop 90 from escaping the latched condition.
SUMMARY OF THE INVENTION
[0027] The invention includes an impact rebound crash stop pivoting about a pivot 218 between the top and bottom yoke of an actuator magnet assembly 20 . The impact rebound crash stop includes a latch bias tab 210 magnetically attracted to the voice coil magnet 32 when near. The magnet attraction rigidly moves a crash stop 216 about pivot 218 . This motion engages the crash stop 216 with crash stop site 226 , as well as pusher 212 with pusher site 224 . Pusher site 214 and crash stop site 226 are both on the actuator 30 fantail.
[0028] The impact rebound crash stop uses an impact rebound bi-directional inertial latch and is preferably made of at least one plastic with low elastic coefficient and a magnetically attractive latch bias tab 210 . The plastic is preferably essentially rigid.
[0029] The invention further includes a proximity latch for an outside disk, ramp loading disk drive allowing the actuator to stay on the ramp when not in use. The proximity latch includes two small magnets 220 bonded to the top and bottom yoke of the voice coil magnet assembly 20 and the impact rebound crash stop.
[0030] The proximity latch mechanism attracts a magnetically attractive component molded into the actuator fantail. The attraction is toward the crash stop. The two magnets and magnetically attractive component attract each other, but do not make contact.
[0031] The proximity latch, together with the impact rebound crash stop, provide an outside disk ramp loading disk drive with a very reliable, non-contact break free latch while maintaining a high resistance to accidental latch release during rotary shock conditions. The proximity latch mechanism achieves this without using any inertial latch mechanism, eliminating the extra travel allowance required by an impact rebound inertial latch mechanism.
[0032] The invention includes the actuator arm 30 embedding the magnetically attractive component 222 in the actuator fantail. The invention further includes an actuator 20 - 66 containing the proximity latch mechanism with the magnetically attractive component 222 and pusher stop 224 in the actuator fantail and crash stop 210 - 218 mounted through its pivot 218 to the top yoke 224 and bottom yoke 222 of the actuator magnet assembly 20 .
[0033] The invention includes the making of these actuators with their crash stop and proximity latch mechanisms, as well as the making of disk drives using these actuators, and the disk drives themselves.
[0034] The invention includes the method of parking an actuator through the operation of an internal crash stop and the operation of the internal proximity latch. The invention also includes the method of parking a disk drive using the method of parking the actuator.
[0035] These and other advantages of the present invention will become apparent upon reading the following detailed descriptions and studying the various figures of the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0036] [0036]FIG. 1A illustrates a typical prior art high capacity disk drive 10 including actuator arm 30 with voice coil 32 , actuator axis 40 , suspension or head arms 50 - 58 with slider/head unit 60 placed among the disks;
[0037] [0037]FIG. 1B illustrates a typical prior art high capacity disk drive 10 with actuator 20 , actuator arm 30 with voice coil 32 , actuator axis 40 , head arms 50 - 56 and slider/head units 60 - 66 with the disks removed;
[0038] [0038]FIG. 1C illustrates a magnetic latch affixed to an actuator arm 30 of the prior art;
[0039] [0039]FIG. 2A illustrates the prior art single level inertial latch mechanism including latch arm 100 pivoting about 102 and including latch hook 104 , mechanically fitting with actuator catch mechanism 106 , as well as latch stop 110 , and crash stop 90 , with the latch mechanism at rest;
[0040] [0040]FIG. 2B illustrates the prior art single level inertial latch during a clockwise acceleration of actuator 30 ;
[0041] [0041]FIG. 2C illustrates the prior art single level inertial latch during a counterclockwise acceleration of the actuator;
[0042] [0042]FIG. 3A illustrates a prior art example of a dual-lever inertial latch at rest;
[0043] [0043]FIG. 3B illustrates a prior art example of a dual-lever inertial latch during a clockwise rotational acceleration of actuator 30 ;
[0044] [0044]FIG. 3C illustrates a prior art example of a dual-lever inertial latch during a counterclockwise rotational acceleration of actuator 30 ;
[0045] [0045]FIG. 4 illustrates an impact rebound type bi-directional inertial latch;
[0046] [0046]FIG. 5A illustrates the proximity latch mechanism in the open position;
[0047] [0047]FIG. 5B illustrates the proximity latch mechanism in the closed position;
[0048] [0048]FIG. 6A illustrates a side view of the proximity latch mechanism as housed in the voice coil magnet assembly; and
[0049] [0049]FIG. 6B illustrates a perspective view of the proximity latch mechanism.
DETAILED DESCRIPTION OF THE INVENTION
[0050] A proximity latch for an outside disk ramp loading disk drives allows the actuator to stay on the ramp when not in use (see FIGS. 5A to 6 B).
[0051] [0051]FIG. 4 illustrates an impact rebound type bi-directional inertial latch.
[0052] The inertial latch rests in an open position due to a light bias torque applied by the magnetic attraction between the voice coil magnet 32 and the balance steel 200 when there is no externally induced rotational acceleration acting upon actuator arm 30 .
[0053] Actuator arm 30 and the latch assembly 102 - 104 - 202 are rotationally balanced. During clockwise rotational acceleration of the disk drive, the latch 102 - 104 rotates in the counterclockwise direction with respect to the base. This latch motion causes the latch hook 104 to engage the barb 106 on the actuator 30 tail.
[0054] During counterclockwise rotational acceleration of the disk drive, actuator arm 30 rebounds from its crash stop 90 and the latch 202 - 102 - 104 also rebounds in the clockwise direction with respect to the base, due to the actuator tail touching the rebound part 202 of the latch. This latch motion causes the latch hook 104 to engage the barb 104 on the actuator 30 tail.
[0055] [0055]FIG. 5A illustrates the proximity latch mechanism in the open position.
[0056] [0056]FIG. 5B illustrates the proximity latch mechanism in the closed position.
[0057] [0057]FIG. 6A illustrates a side view of the proximity latch mechanism as housed in the voice coil magnet assembly.
[0058] [0058]FIG. 6B illustrates a perspective view of the proximity latch mechanism.
[0059] The proximity latch includes two small magnets 220 bonded to the top yoke 22 and bottom yoke 24 of the actuator assembly 20 and an impact rebound crash stop 216 . The impact rebound crash stop 216 uses an impact rebound bi-directional inertial latch 210 - 218 . The impact rebound bi-directional latch includes pusher 212 , latch pivot 218 and latch bias tab 210 .
[0060] The proximity latch mechanism attracts a magnetically attractive component 222 molded into the actuator fantail toward the two small magnets 220 . The actuator fantail is further formed of a pusher stop 224 and a crash stop site 226 . The attraction is toward the pusher 212 . Note that the small magnets 220 are preferably magnetically aligned so that their North poles point in essentially the same direction.
[0061] The two small magnets 220 and magnetically attractive component 222 attract each other, but do not make contact. However, as the two small magnets 220 and the magnetically attractive component 222 approach each other, pusher stop 224 engages pusher 210 , rotating the proximity latch mechanism 210 - 218 about latch pivot 218 to engage crash stop 216 and crash stop site 226 .
[0062] The magnetically attractive component 222 is preferably made of a magnetically attractive form of steel, preferably number 430.
[0063] Note that the proximity latch mechanism illustrated in FIGS. 5A and 5B does not use an impact rebound inertial latching mechanism. This eliminates the extra travel allowance required in all the designs illustrated by FIGS. 1C to 4 .
[0064] The impact rebound crash stop 216 halts the actuator 30 at a contact point illustrated in FIG. 5B through engagement with crash stop site 226 on actuator arm 30 .
[0065] The magnetic force between the magnetically attractive actuator component 222 and the two non-contact magnets 220 , provide a torque upon the actuator. This magnetic force is preferably between 4.8 and 6.0 Newton-meter{circumflex over ( )}2. This preferred magnetic force supports high rotary shock performance in the clockwise direction. The impact rebound crash stop 216 is used to keep the actuator 30 from rebounding during counterclockwise rotary shocks. The impact rebound crash stop 216 is built into the voice coil magnet assembly as shown in FIG. 6B.
[0066] When the actuator approaches the impact rebound crash stop, the magnetic latching mechanism engages and helps the actuator to move faster into the crash stop. The magnetic latching mechanism includes the magnetic attraction between the two small magnets and magnetically attractive component molded into the actuator. The two small magnets are placed on the top and bottom yokes of the voice coil magnet assembly exactly so that the actuator is maintained at a parking “home” where the impact rebound crash stop is located. As the magnetically attractive component of the actuator slowly approaches the flux generated by these two small magnets, the actuator pushes upon the impact rebound crash stop. The impact rebound crash stop is rotated clockwise until the impact rebound crash stop touches the actuator by its latch arm at the crash stop.
[0067] The proximity latch mechanism helps a disk drive resist relatively high rotary shock in the clockwise direction with respect to the disk drive base. This resistance depends upon the magnetic attractive force between the two small magnets and the magnetically attractive component molded into the actuator.
[0068] The impact rebound crash stop helps increase rotary shock performance in the counterclockwise direction with respect to the disk drive base. The impact response crash stop is preferably made from plastic, preferably from an ultem plastic material. The actuator fan tail is preferably includes a plastic overmold made of vectra.
[0069] The elastic coefficient between the plastic impact response crash stop and the plastic overmold actuator fantail is less than one, preferably about 0.6. The elastic coefficient being less than one contributes to very minimal rebound effect from impact between the actuator fantail and the impact rebound crash stop. The loss of high energy during the impact also significantly reduces the chance of sudden impact rebound motion. This reduction in the chance of sudden impact rebound motion, combined with the reduced energy of any sudden impact rebound motion, both contribute to high rotary shock resistance in the counterclockwise direction with respect to the disk drive base.
[0070] The latch bias tab 210 is molded into the latch mechanism and supports the latch opening its arm automatically when the actuator is controlled to move out in a desirable speed. The latch opens its arm based upon the attractive force generated on the latch bias tab 210 by the voice coil magnet 32 . The latch bias tab 210 is preferably composed of a magnetically attractive steel compound preferably SUS 430 steel.
[0071] The invention secures read-write head parking through rotational shocks of 25,000 to 30,000 radians/sec{circumflex over ( )}2 of up to two milliseconds duration. Note that the contemporary industry standard is support for up to 20,000 radians/sec{circumflex over ( )}2.
[0072] Depending upon the small magnets, the performance can protect read-write head parking under even more severe conditions. The small magnets preferably have magnetic strengths of 48 MGO and are preferably 1.5 millimeters thick and 3 millimeters by 4 millimeters wide.
[0073] The preceding embodiments have been provided by way of example and are not meant to constrain the scope of the following claims. | The invention includes an impact rebound crash stop pivoting about a pivot between the top and bottom yoke of an actuator magnet assembly. The impact rebound crash stop includes a latch bias tab magnetically attracted to the voice coil magnet when it is near. The invention further includes a proximity latch allowing the actuator to stay on the ramp when not in use. The invention includes the operation of actuator arms embedding part of the magnetic proximity latch, actuators, and disk drives using the crash stop and proximity latch. | 6 |
INCORPORATION BY REFERENCE
[0001] The present application incorporates by reference the entire disclosures of U.S. Pat. No. 6,003,606 (entitled “PULLER-THRUSTER DOWNHOLE TOOL”); U.S. Pat. No. 6,347,674 (“ELECTRICALLY SEQUENCED TRACTOR”); U.S. Pat. No. 6,241,031 (“ELECTRO-HYDRAULICALLY CONTROLLED TRACTOR”); U.S. Pat. No. 6,679,341 (“TRACTOR WITH IMPROVED VALVE SYSTEM”); U.S. Pat. No. 6,464,003 (“GRIPPER ASSEMBLY FOR DOWNHOLE TRACTORS”); and U.S. Pat. No. 6,715,559 (“GRIPPER ASSEMBLY FOR DOWNHOLE TRACTORS”). The present application also incorporates by reference the entire disclosures of U.S. Patent Application Publication Nos. 2004/0168828 (“TRACTOR WITH IMPROVED VALVE SYSTEM”); and 2005/0247488 (“ROLLER LINK TOGGLE GRIPPER AND DOWNHOLE TRACTOR”). The present application also incorporates by reference the entire disclosure of U.S. Provisional Patent Application No. 60/781,885, filed Mar. 13, 2006 (“EXPANDABLE RAMP GRIPPER”).
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates generally to tools for conducting operations within passages, and specifically to tools for borehole intervention and/or drilling.
[0004] 2. Description of the Related Art
[0005] U.S. Pat. No. 6,003,606, entitled “Puller-Thruster Downhole Tool,” discloses an innovative self-propelled tool or tractor for drilling, completion, stimulation, and intervention that pulls a drill string and simultaneously thrusts itself and its payload downhole and/or into a casing or borehole formation. The '606 patent discloses a tractor that includes one or more gripper assemblies (e.g., bladders or packerfeet) that grip onto an inner surface of a borehole or casing, and one or more propulsion assemblies that propel the tractor body forward when at least one of the gripper assemblies is gripping the borehole. A valve system directs a fluid (e.g., drilling mud, intervention fluid, hydraulic fluid) to and from the gripper assemblies and propulsion assemblies to power movement of the tractor.
[0006] The '606 patent discloses two basic types of tractor configurations—open loop and closed loop. The open loop system uses an externally provided fluid as a medium of hydraulic communication within the tractor. The open loop consists of a ground surface pump, tubing extending from the pump into a borehole, a tractor within the borehole and connected to the tubing, and an annulus between the exterior of the tractor and an inner surface of the borehole. The fluid is pumped down through the tubing to the tractor, used by the tractor to move and conduct other downhole operations, and then forced back up the borehole through the annulus. The tractor is powered by differential pressure—the difference of the pressure at the point of intake of fluid to the tractor and the pressure of fluid ejected from the tractor into the annulus. In the open loop system, a portion of the fluid is used to power the tractor's movement and another portion of the fluid flows through the tractor for various downhole purposes, such as hole cleaning, sand washing, acidizing, and lubricating of a drill bit (in drilling operations). Both portions of the fluid return to the ground surface through the annulus.
[0007] The '606 patent also discloses a closed loop configuration in which a hydraulic fluid is circulated through the gripper assemblies and propulsion assemblies to power the tractor's movement within the borehole. In particular, FIG. 19 of the '606 patent discloses a downhole motor that powers the recirculation of the hydraulic fluid.
[0008] U.S. Pat. Nos. 6,347,674; 6,241,031; and 6,679,341, as well as U.S. Patent Application Publication No. 2004/0168828, disclose alternative valve systems and methods for directing fluid to and from a downhole tractor's gripper assemblies and propulsion assemblies for moving the tractor.
SUMMARY
[0009] In one aspect, a tool for moving within a passage is provided. The tool comprises an elongated body, at least one gripper assembly engaged with the body, a turbine, and a power transmission assembly. The elongated body has an internal fluid chamber and is configured to be secured to a fluid conduit so that a first fluid flowing through the conduit flows into the internal fluid chamber. The gripper assembly has an actuated position in which the gripper assembly grips onto an inner surface of the passage to substantially limit relative movement between the gripper assembly and the inner surface. The gripper assembly also has a retracted position in which the gripper assembly permits substantially free relative movement between the gripper assembly and the inner surface of the passage. The turbine is configured to receive the first fluid flow through the internal fluid chamber, the turbine having an output shaft configured to rotate as the first fluid flows through the turbine. The power transmission assembly is configured to convert rotation of the output shaft into power for moving the gripper assembly to its actuated position.
[0010] In another aspect, a method of moving a tool within a passage is provided. An elongated body having an internal fluid chamber is provided. The body is secured to a fluid conduit so that a first fluid flowing through the conduit flows into the internal fluid chamber of the body. At least one gripper assembly is provided and engaged with the body. The gripper assembly has an actuated position in which the gripper assembly grips onto an inner surface of the passage to substantially limit relative movement between the gripper assembly and the inner surface, and a retracted position in which the gripper assembly permits substantially free relative movement between the gripper assembly and the inner surface of the passage. A turbine is provided, the turbine configured to receive the first fluid flow through the internal fluid chamber. The turbine has an output shaft configured to rotate as the first fluid flows through the turbine. A power transmission assembly is provided, the power transmission assembly configured to convert rotation of the output shaft into power for moving the gripper assembly to its actuated position. The first fluid is pumped through the conduit into the internal fluid chamber of the body and through the turbine.
[0011] For purposes of summarizing the invention and the advantages achieved over the prior art, certain objects and advantages of the invention have been described herein above. Of course, it is to be understood that not necessarily all such objects or advantages may be achieved in accordance with any particular embodiment of the invention. Thus, for example, those skilled in the art will recognize that the invention may be embodied or carried out in a manner that achieves or optimizes one advantage or group of advantages as taught herein without necessarily achieving other objects or advantages as may be taught or suggested herein.
[0012] All of these embodiments are intended to be within the scope of the invention herein disclosed. These and other embodiments of the present invention will become readily apparent to those skilled in the art from the following detailed description of the preferred embodiments having reference to the attached figures, the invention not being limited to any particular preferred embodiment(s) disclosed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a schematic diagram of a conventional coiled tubing tractor system.
[0014] FIG. 2 is a schematic diagram of a closed loop system for powering a downhole tractor, according to one embodiment of the invention.
[0015] FIG. 3 is a more detailed schematic diagram of the closed loop system of FIG. 2 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0016] FIG. 1 illustrates a conventional coiled tubing tractor or tool for conducting downhole operations such as intervention and drilling. The illustrated system is an open loop configuration. The coiled tubing system 100 typically includes a power supply 102 for powering ground-level equipment, a tubing reel 104 , a tubing guide 106 , and a tubing injector 110 , which are well known in the art. The illustrated system includes a bottom hole drilling assembly 120 for drilling a borehole 132 with a drill bit 130 . However, other types of bottom hole assemblies 120 can alternatively be provided, such as those for intervention operations like hole cleaning, sand washing, acidizing, and the like. As known, coiled tubing 114 is inserted into the borehole 132 , and a fluid (e.g., drilling mud, intervention fluid) is typically pumped through the inner flow channel of the coiled tubing 114 towards the drill bit 130 located at the end of the drill string. Positioned between the drill bit 130 and the coiled tubing 114 is a tool or tractor 112 . The illustrated bottom hole assembly (BHA) 120 includes a number of elements known to those skilled in the art, such as a downhole motor 122 and a Measurement While Drilling (MWD) system 124 . The tractor 112 is preferably connected to the coiled tubing 114 and the bottom hole assembly 120 by connectors 116 and 126 , respectively, as known in the art. In this system, the fluid is pumped through the inner flow channel of the coiled tubing 114 and through the tractor 112 to the drill bit 130 . The fluid and drilling debris return to the surface in the annulus defined between the exterior surface of the tractor 112 and the inner surface of the borehole 132 , and also defined between the exterior surface of coiled tubing 114 and the inner surface of the borehole 132 .
[0017] When operated, the tractor 112 is configured to move within the borehole 132 . This movement allows, for example, the tractor 112 to maintain a pre-selected force on the bottom hole assembly 120 such that the rate of movement or drilling can be controlled. The tractor 112 can be used to move various types of equipment through the borehole 132 . For example, it will be understood that the tractor 112 can be connected with or include, without limitation, a downhole motor (for rotating a drill bit), steering system, instrumentation sub (an instrumented package that controls various aspects of downhole operation, including shock vibration, weight on bit, torque at bit, rate of penetration, downhole motor rpm, and differential pressure across motor), Measurement While Drilling apparatus (an apparatus for measuring gyroscopic data such as azimuth, inclination, and measured depth), drill bit, mechanical and hydraulic disconnect for intervention, jetting tools, production logging tools (including apparatus for measuring and recording, without limitation, temperature, annulus pressure, and various flow rates), drilling logging tools (for measuring and recording, without limitation, resistivity measurements, magnetic resonance (MRI), sonic neutron density, density, fluid identification, and gamma ray measurements), perforation guns, casing collar locators, and torque limiting tools (for drilling).
[0018] A closed loop configuration has relevant differences from an open loop system that operates on differential pressure (the difference in pressure between the bore of the tractor and the exterior of the tractor). With an open system, a restriction in the system is required to produce a pressure difference (decrease) between the interior and exterior of the tractor. Typically, the restriction is an orifice such as a fixed diameter nozzle, and is not capable of being adjusted from the surface. For typical coiled tubing rig operations, the effective means of control is to control the surface pump output flow rate. However, the differential pressure available at the tractor is a quadratic (non-linear) function of the surface pump output flow rate. Thus, doubling the surface pump output flow rate will increase the differential pressure through an in-series fixed orifice by a factor of four. This makes power control of the tractor more difficult as normal operational changes can have non-linear impact on tractor power, requiring additional features to be incorporated into the open loop powered tractor to restrict the amount of pressure delivered to the gripper assemblies, for example. Further, this has a disadvantage in that the normal operating range of the surface pump output flow rate required for various operations may have to be restricted, thus reducing cleaning efficiency during the operation.
[0019] FIG. 2 is a schematic illustration of a turbine-powered pump for circulating hydraulic fluid in a closed loop for powering a downhole tool or tractor, according to one embodiment of the present invention. In this configuration, a first fluid (typically drilling/intervention fluid) that is externally pumped into the coiled tubing typically at the ground surface flows through the tractor and passes through a turbine 150 on its way to the remaining bottom hole assembly (typically secured to the distal end of the tractor). The flow through the turbine 150 produces rotation of the turbine's output shaft, which drives a pump 154 through a gearbox 152 . The pump 154 circulates a second fluid (typically a different type of fluid than the first fluid, such as, for example, hydraulic fluid) in a closed system loop 156 . Box 158 represents a valve system, gripper assemblies, and propulsion assemblies as known in the art. For example, the valve system, gripper assemblies, and propulsion assemblies can be substantially as shown and described in U.S. Pat. Nos. 6,003,606; 6,347,674; 6,241,031; and 6,679,341, as well as U.S. Patent Application Publication No. 2004/0168828. Also, the gripper assemblies can be substantially as shown and described in U.S. Pat. Nos. 6,464,003 and 6,715,559; U.S. Patent Application Publication No. 2005/0247488; and U.S. Provisional App. No. 60/781,885. The second fluid provides hydraulic force for operation of the gripper assemblies and propulsion assemblies, and in some cases the valves.
[0020] FIG. 3 is a more detailed schematic illustration of the closed loop system of FIG. 2 adapted for use with a variation of the Puller-Thruster Downhole Tool (also referred to as the “Puller-Thruster Assembly” or “PTA”) described in U.S. Pat. No. 6,003,606. As the first fluid is pumped through the turbine 150 , the turbine output shaft rotates to power the pump 154 via the gearbox 152 (not shown), and the pump 154 in turn circulates the second fluid through the illustrated valve assembly. The second fluid flows from a supply line 228 through a start/stop valve 160 (also known as an “idler valve”) into the valve system. A six-way control valve 162 shuttles back and forth to direct the fluid to and from an aft gripper assembly 180 (illustrated as a deflated packerfoot) and a forward gripper assembly 182 (illustrated as an inflated packerfoot), and also to and from an aft propulsion assembly 184 and a forward propulsion assembly 186 (each propulsion assembly comprising barrels and internal pistons, as taught in the '606 patent). Valves 164 and 166 (also known as “directional control valves”) control the shuttling and position of the six-way control valve 162 . Packerfeet valves 168 and 170 regulate the flow of fluid into the packerfeet 180 and 182 . A reverser valve 172 controls the direction of tractor movement (i.e., uphole or downhole). The operation of these valves is understood from the teachings of the aforementioned patents incorporated by reference. A sump 157 is preferably provided to store a reservoir of the second fluid. The circulating second fluid returns to the sump 157 via a return line 230 .
[0021] FIG. 3 shows an embodiment of a tool 200 (illustrated as a Puller-Thruster Assembly) positioned within a drilled hole 205 inside a rock formation 212 . The tool 200 includes an elongated body formed of central coaxial cylinders 207 . The aft gripper assembly 180 , aft propulsion assembly 184 , forward gripper assembly 182 , and forward propulsion assembly 186 are engaged on the central coaxial cylinders 207 . The aft propulsion assembly 184 includes annular pistons 218 secured to the cylinders 207 . Similarly, the forward propulsion assembly 186 includes annular pistons 220 secured to the cylinders 207 . The number of pistons can vary (e.g., up to 20 pistons) and depends on the desired thrust and pull loads.
[0022] The tool body defines an internal mud flow passage 224 inside the cylinders 207 . The aft end of the tool body has an inlet 201 connected to coiled tubing 114 via a coiled tubing connector 206 (connection can be threaded or snapped together). While FIG. 3 shows coiled tubing 114 , the tool 200 can also be used with rotary drill rigs instead. The forward end of the tool body is connected to a bottom hole assembly (BHA) 204 . The illustrated tool includes a female coiled tubing connector 208 and stabilizers 210 . The valve control pack 214 is positioned between the forward and aft gripper assemblies and also between the forward and aft propulsion assemblies. Splines 216 can optionally be incorporated between the central coaxial cylinders 207 and the gripper assemblies to prevent the transmission of torque from the BHA 204 to the coiled tubing 114 .
[0023] In use, drilling/intervention fluid flows from the coiled tubing 114 into the inlet 201 of the tool body, and downhole (toward the bottom of the hole) through the mud flow passage 224 . The fluid flows through the turbine 150 , powering the pump 154 . The fluid continues through the passage 224 into the BHA 204 , exiting the BHA 204 through an outlet 203 . The inlet 201 and outlet 203 are also shown in relation to the turbine 150 on the bottom right hand side of FIG. 3 . The drilling/intervention fluid that exits via the outlet 203 then flows uphole to the ground surface through an annulus defined between the tool 200 and the drilled hole 205 .
[0024] The upper right hand side of FIG. 3 includes a cross-sectional view of the inflated packerfoot 182 , taken along line A-A. The illustrated packerfoot 182 includes three inflated sections. Three mud flow return paths 222 are defined between the three inflated sections of the packerfoot. These return paths 222 allow drilling fluid that exits via the outlet 203 to flow back uphole past the inflated packerfoot. It will be understood that the aft packerfoot 180 can be substantially identical to the forward packerfoot 182 . The illustrated packerfoot cross section shows the packerfoot inflated radially beyond the outside diameter 226 of the tool 200 .
[0025] A relevant advantage of using a turbine-powered pump as illustrated is that the system is flow-based, meaning that the downhole tractor can be more easily controlled by the surface pump that pumps fluid down into the coiled tubing toward the turbine. With a flow-based system, any change in the surface pump output volume flow rate linearly changes the power available to the tractor. Since the surface pump output flow rate can be relatively easily adjusted dynamically during tractor operation, the resulting adjustment of the power to the tractor provides enhanced control over the tractor's speed and pulling force. This enhanced control is available over a substantial operating range of surface pump output flow rates. This is convenient for some types of operations. For example, during sand washing it is desirable to provide a maximum amount of fluid into the borehole while the tractor continues its forward movement, usually at near-maximum pulling capacity.
[0026] Another relevant advantage of this system is that the pump 154 is desirably directly powered by the rotating output of the turbine/gearbox combination, without any intermediate steps (e.g., electrical power generation from the turbine output, and use of such electrical power to drive an electric motor that drives the pump). The provision of such intermediate steps would introduce a risk of a loss of efficiency in converting the kinetic energy of the first fluid pumped into the turbine 150 into power for driving the operation of the pump 154 . The disclosed turbine/gearbox combination advantageously provides a highly efficient conversion of the first fluid's kinetic energy.
[0027] Although this invention has been disclosed in the context of certain preferred embodiments and examples, it will be understood by those skilled in the art that the present invention extends beyond the specifically disclosed embodiments to other alternative embodiments and/or uses of the invention and obvious modifications thereof. Thus, it is intended that the scope of the present invention herein disclosed should not be limited by the particular disclosed embodiments described above. | A tool for moving within a passage comprises an elongated body, at least one gripper assembly engaged with the body, a turbine, and a power transmission assembly. The elongated body has an internal fluid chamber and is configured to be secured to a fluid conduit so that a first fluid flowing through the conduit flows into the internal fluid chamber. The gripper assembly has an actuated position in which the gripper assembly grips onto an inner surface of the passage to substantially limit relative movement between the gripper assembly and the inner surface. The gripper assembly also has a retracted position in which the gripper assembly permits substantially free relative movement between the gripper assembly and the inner surface of the passage. The turbine is configured to receive the first fluid flow through the internal fluid chamber, the turbine having an output shaft configured to rotate as the first fluid flows through the turbine. The power transmission assembly is configured to convert rotation of the output shaft into power for moving the gripper assembly to its actuated position. | 4 |
RELATED APPLICATION
[0001] The entire disclosure of DE 10 2005 012 896.3, which was filed Mar. 21, 2005, is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to a vehicle seat, in particular a motor vehicle seat, having a backrest, at least one headrest rod that is slidingly guided in relation to the backrest and locked in an in-use position, and at least one headrest mounted on the headrest rod, wherein the headrest rod is unlockable by the actuation of an actuation element, and the headrest is adjustable in height and removable by way of sliding the headrest rod.
[0003] In a vehicle seat of the type described immediately above, it is known that the height of the headrest can be adjusted by actuating the actuation element. If, in so doing, the headrest is pulled upwards beyond the highest adjustable level, it necessarily comes off its mounting. As the highest adjustable level is usually not known, this may occur totally inadvertently, in particular if, in order to save material, the rods used for supporting the headrest are very short. Reinstallation of the headrest is not only considered an inconvenience, but also involves a safety risk, in particular if the headrest is positioned above the highest adjustable level and just below the level where it will inevitably come off again.
BRIEF SUMMARY OF SOME ASPECTS OF THE INVENTION
[0004] An aspect of the present invention is the provision of improvements to a vehicle seat of the type described above.
[0005] In accordance with one aspect of the present invention, a vehicle seat, in particular a motor vehicle seat, has a backrest, at least one headrest rod that is slidingly guided in relation to the backrest and locked in an in-use position, and at least one headrest mounted on the headrest rod. The headrest rod is unlockable by the actuation of at least one actuation element, and the headrest is adjustable in height and removable by way of sliding the headrest rod. In one example, two different methods of actuating the same actuation element (e.g., a single or certain actuation element) are respectively provided for the adjustment and removal processes. In another example, two different actuation elements are respectively provided for the adjustment and removal processes.
[0006] By providing two different actuation elements or two different methods of actuating the actuation element for the purpose of adjusting and removing the headrest, unintentional removal of the headrest during the adjustment process is avoided because the user must carry out a significantly different actuation in order to remove the headrest. Preferably at least one adjustment notch, more precisely one such notch per each level of adjustment, and at least one, preferably no more than one, stop notch are formed on the headrest rod, with the notches respectively interacting with a locking element of the actuation element to lock the headrest rod in place. When the headrest rod is locked by engagement in an adjustment notch, unlocking is accomplished by way of a first actuation element that is preferably easy for the user to access and that interacts by way of its locking element with the adjustment notch, or by actuating the (single) actuating element in a first particular way. When, on the other hand, the headrest rod is locked by engagement in the stop notch, unlocking is accomplished by way of the second actuation element whose own locking element interacts with the stop notch, or by actuating the (single) actuation element in a second particular way. The second actuation element preferably becomes accessible and/or actuatable when the interlocking with the stop notch occurs. The adjustment notches and stop notches may be formed on different sides of the same headrest rod (e.g., a certain headrest rod) or on different headrest rods, it being preferable in the first case that the actuation elements are actuated in different directions.
[0007] The actuation element is movably located in a space-saving manner, preferably in a receptacle in the head section of a guide bushing in which the headrest rod is mounted. The actuation element is preferably supported and pretensioned (e.g., biased) with respect to the head of the bushing by way of at least one mounting spring. The actuation element is then held in its resting position by way of the mounting spring. The actuation element is then actuated correspondingly, preferably by pushing it against the force of the mounting spring. In the case of a single actuation element, the action element is actuated by two distinctly different methods of actuation, preferably by pressing and turning, or by turning it in two different directions.
[0008] Other aspects and advantages of the present invention will become apparent from the following.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] Hereinafter, the present invention is described in more detail with reference to six exemplary embodiments illustrated in the drawings, in which:
[0010] FIG. 1 shows a vertical cross section through a portion of the first exemplary embodiment in the in-use state;
[0011] FIG. 2 shows a cross-section along the line II-II in FIG. 1 , with an arrow indicating the possible direction of actuation during the adjustment process;
[0012] FIG. 3 shows a cross-section along the line III-III in FIG. 1 , with an arrow that is illustrated in dashed lines indicating the possible direction of actuation when removing the headrest, and dashed lines also illustrate the position of the second actuation element prior to actuation;
[0013] FIG. 4 is a schematic view of a vehicle seat;
[0014] FIG. 5 shows a vertical cross-section through a portion of the second exemplary embodiment in the in-use state;
[0015] FIG. 6 shows a cross-section along the line VI-VI in FIG. 5 , with an arrow indicating the possible direction of actuation during the adjustment process;
[0016] FIG. 7 shows a cross-section along the line VII-VII in FIG. 5 , with an arrow that is illustrated in dashed lines indicating the possible direction of actuation when removing the headrest, and dashed lines also illustrate the position of the second actuation element prior to actuation;
[0017] FIG. 8 shows a vertical cross-section through a portion of the third exemplary embodiment in the in-use state;
[0018] FIG. 9 shows a cross-section along the line IX-IX in FIG. 8 , with an arrow illustrated by a continuous line indicating the possible direction of actuation during the adjustment process, and an arrow illustrated by dashed lines indicating the possible direction of actuation during removal of the headrest;
[0019] FIG. 10 shows a vertical cross-section through a portion of the fourth exemplary embodiment in the in-use state;
[0020] FIG. 11 shows a cross-section along the line XI-XI in FIG. 10 ;
[0021] FIG. 12 shows a cross-section corresponding to FIG. 10 during the adjustment process;
[0022] FIG. 13 shows a cross section along the line XIII-XIII in FIG. 12 , with an arrow indicating the direction of actuation during the adjustment process;
[0023] FIG. 14 shows a cross-section corresponding to FIGS. 10 and 12 during the removal of the headrest;
[0024] FIG. 15 shows a cross-section along the line XV-XV in FIG. 14 , with an arrow illustrated by dashed lines indicating the direction of actuation when removing the headrest;
[0025] FIG. 16 shows a vertical cross-section through a portion of the fifth exemplary embodiment in the in-use state;
[0026] FIG. 17 shows a cross-section along the line XVII-XVII in FIG. 16 , with an arrow indicating the possible direction of actuation during the adjustment process;
[0027] FIG. 18 shows a cross-section corresponding to FIG. 17 , with an arrow illustrated by dashed lines indicating the possible direction of actuation when removing the headrest;
[0028] FIG. 19 shows a vertical cross-section through a portion of the sixth exemplary embodiment in the in-use state;
[0029] FIG. 20 shows a cross-section along the line XX-XX in FIG. 19 , with an arrow indicating the direction of actuation during the adjustment process; and
[0030] FIG. 21 shows a cross section corresponding to FIG. 20 , with an arrow illustrated by dashed lines indicating the direction of actuation when removing the headrest.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0031] In the following, reference is made in greater detail to the drawings, in which like numerals refer to like parts throughout the several views. In all the exemplary embodiments, a vehicle seat 1 of a motor vehicle comprises a headrest 6 mounted on a backrest 3 . The headrest 6 is attached in a known manner to at least one, and in the present case to two metal headrest rods, each of which is mounted in a linearly sliding manner in a plastic guide bushing in the backrest 3 . By these means, the headrest 6 , which is locked in an in-use position, is adjustable in height and can also be fully removed.
[0032] In the first exemplary embodiment, several adjustment notches 12 are arranged equidistantly apart on one side of one of the two headrest rods 10 , and on the other side a stop notch 14 is formed below the lowest adjustment notch 12 . The associated guide bushing 15 comprises a bushing head 17 within which are formed, at various heights and on opposite sides, two open receptacles 19 respectively for an upper, first actuation element 21 , and a lower, second actuation element 23 . Both actuation elements 21 and 23 comprise a locking element 25 aligned perpendicularly to the headrest rod 10 and consisting, for example, of a piece of metal wire or rod. Except for their locking elements 25 , the actuation elements 21 and 23 are made of plastic. The actuation elements 21 and 23 are respectively arranged within the receptacles 19 . For each actuation element 21 and its respective guide bushing 15 , the actuation element 21 is biased by way of a mounting spring 27 , namely by the tendency of the mounting spring 27 to expand, in a manner that urges the actuation element away from a portion of the guide bushing. The locking element 25 is in each case arranged on the side of the headrest rod 10 facing away from the open part of the receptacle 19 and facing towards the closed part of the receptacle 19 .
[0033] When the headrest is in use, the locking element 25 of the first actuation element 21 engages in an adjustment notch 12 , as a result of which the headrest rod 10 , and thus the headrest 6 , is locked in place. While the first actuation element 21 is accessible to the user and flush with the bushing head 17 , the second actuation element 23 is located completely within its receptacle 19 . In order to adjust the headrest 6 , the first actuation element 21 is actuated, i.e. pressed deeper into its receptacle 19 (e.g., moved in a nonrotary direction), so that the locking element 25 is disengaged from the adjustment notch 12 . It is now possible to slide the headrest rod 10 within the guide bushing 15 , thus permitting the height of the headrest 6 to be adjusted. The adjustment notches 12 are preferably beveled downwards so that the headrest rod 10 can be pulled upwards, i.e. further extended, even without actuating the first actuation element 21 .
[0034] In order to remove the headrest 6 , the headrest rod 10 is pulled upwards until the lowest adjustment notch 12 passes by at least the first actuation element 21 and emerges at the top from the bushing head 17 . As soon as the stop notch 14 reaches the second actuation element 23 , the associated mounting spring 27 displaces the second actuation element 23 whose locking element 25 then engages in the stop notch 14 . The headrest rod 10 is thus locked once more. The second actuation element 23 now projects laterally from the bushing head 17 . By actuating, i.e. pressing (e.g., moving in a nonrotary direction), the second actuation element 23 , the locking element 25 is disengaged from the stop notch 14 , and as a result the headrest rod 10 can be pulled further upwards until it finally leaves the guide bushing 15 . The stop notch 14 is preferably beveled upwards so that the headrest rod 10 can be pushed down again, i.e. re-inserted, without actuating the second actuation element 23 .
[0035] Except where stated otherwise below, the second exemplary embodiment is the same as the first exemplary embodiment, for which reason identical and identically acting components bear reference numbers raised by 100. The adjustment notches 112 are in this case formed on a first headrest rod 110 . The first headrest rod 110 is introduced into the guide bushing 115 , in the head 117 of which the first actuation element 121 is mounted with a mounting spring 127 in a receptacle 119 , for locking the first headrest rod 110 by way of its actuation element 125 . On the other hand, the stop notch 114 is formed on a second headrest rod 130 . The second headrest rod 130 is inserted into a guide bushing 115 of identical design to the guide bushing 115 used for the first headrest rod 110 . With the exception of the displacement corresponding to the thickness of the locking element 125 , the second actuation element 123 is identical to the first actuation element 121 , and alternatively the second actuation element 123 can be completely identical to the first actuation element 121 . The second actuation element 123 is arranged and mounted in the same way as the first actuation element 121 , except that the second actuation element 123 is not locking the second headrest rod 130 while the first actuation element 121 is locking the first headrest rod 110 . In both of the first and second exemplary embodiments the mode of functioning, including the mode of actuation, is the same—except for the circumstances determined by the spatially separate arrangement of the actuation elements 121 and 123 .
[0036] Except where stated otherwise below, the third exemplary embodiment is similar in design to the first and second exemplary embodiments, for which reason identical and identically acting components bear reference numbers raised by 200 and 100 respectively. As in the case of the first exemplary embodiment, adjustment notches 212 are formed on one side of the (first) headrest rod 210 and on the opposite side a stop notch 214 is formed. The headrest rod 210 is introduced into the guide bushing 215 . The first actuation element 221 is mounted in a receptacle 219 in the head 217 of the guide bushing 215 ; the first actuation element 221 is accessible to the user. The first actuation element 221 is connected, by way of two parallel-arranged energy-storing elements 233 (e.g., tension springs) that enclose the headrest rod 210 between them, to the second actuation element 223 . The second actuation element 223 is arranged completely inside the receptacle 219 so that the second actuation element 223 is inaccessible to the user. The second actuation element 223 is biased by a mounting spring 227 , namely by the tendency of the mounting spring 227 to expand, in a manner that urges the actuation element away from a portion of the head 217 of the guide bushing 215 . When the headrest is in use, the locking element 225 of the second actuation element 223 locks the headrest rod 210 in place.
[0037] In order to adjust the headrest, the first actuation element 221 is actuated in a first manner, i.e. in the present case it is pressed, as a result of which the motion is transmitted to the second actuation element 223 by the compressed coils of the energy-storing elements 233 , so that the locking element 225 of the second actuation element 223 is disengaged. The headrest rod 210 can now be adjusted in height. In order to remove the headrest, the headrest rod 210 is first pulled upwards until the locking element 225 of the first actuation element 221 engages in the stop notch 214 . By actuating the first actuation element 221 in a second manner, in the present case by pulling (e.g., moving in a nonrotary direction), the locking element 225 is again disengaged and the headrest rod 210 can be pulled further upwards.
[0038] Except where stated otherwise below, the fourth exemplary embodiment is similar in design to the first, second and third exemplary embodiments, for which reason identical and identically acting components bear reference numbers raised by 300, 200 and 100 respectively. As in the first exemplary embodiment, adjustment notches 312 are formed on one side of the (first) headrest rod 310 . On the same side, a stop notch 314 is formed below the lowest adjustment notch 312 . The headrest rod 310 is introduced into the guide bushing 315 . The user-accessible first actuation element 321 is mounted in a receptacle 319 in the head 317 of the guide bushing 315 . The first actuation element 321 is biased by way of a mounting spring 327 , namely by the tendency of the mounting spring 327 to expand, in a manner that urges the actuation element away from a portion of the head 317 of the guide bushing 315 . When the headrest is in use, the locking element 325 of the first actuation element 321 engages in one of the adjustment notches 312 . The second actuation element 323 is mounted within the first actuation element 321 . The second actuation element 323 engages one end of a rocker element 335 . The rocker element 335 is pivotably mounted on the guide bushing 315 . The other end of the rocker element 335 bears a further locking element 325 that is pretensioned by a spring against (e.g., biased toward) the headrest rod 310 .
[0039] In order to adjust the headrest, the first actuation element 321 is actuated, i.e. in the present case it is pressed, causing its locking element 325 to disengage, so that the height of the headrest rod 310 can be adjusted. To remove the headrest, the headrest rod 310 is first pulled upwards until the locking element 325 on the rocker element 335 engages in the stop notch 314 . By actuating the second actuation element 323 , in the present case by pulling it outwards relative to the first actuation element 321 , the rocker element 335 is pivoted and its locking element 325 is again disengaged so that the headrest rod 310 can be pulled further upwards.
[0040] Except where stated otherwise below, the fifth exemplary embodiment is similar in design to the preceding embodiments, for which reason identical and identically acting components bear reference numbers that are in each case raised by 100. The (first) headrest rod 410 is again provided with several adjustment notches 412 . The stop notch 414 is arranged beneath the lowest adjustment notch 412 , and it is offset at an angle of slightly more than 90° with respect to the adjustment notches 412 . The headrest rod 410 is inserted into the guide bushing 415 in the head 417 of which is mounted, in a receptacle 419 , the user-accessible (first) actuation element 421 . The actuation element 421 is biased by way of a first mounting spring 427 , namely by the tendency of the first mounting spring 427 to expand, in a manner that urges the actuation element away from another portion of the head 417 of the guide bushing 415 . The actuation element 421 is also biased by way of a second mounting spring 437 , namely by the tendency of the second mounting spring 437 to expand, in a manner that urges the actuation element away from a portion of the head 417 of the guide bushing 415 . The second mounting spring 437 is arranged perpendicularly to the first mounting spring 427 . When the headrest is in use, the locking element 425 of the actuation element 421 engages in one of the adjustment notches 412 .
[0041] In order to adjust the headrest, the actuation element 421 is actuated in a first manner, i.e. in the present case it is pressed (e.g., moved in a nonrotary direction) against the first mounting spring 427 , thereby causing the locking element 425 to disengage, so that the height of the headrest rod 410 can be adjusted. More specifically, FIG. 17 shows the locking element 425 engaging an adjustment notch 412 , and the arrow indicates how to press the actuation element 421 for disengaging the locking element 425 from the adjustment notch 412 .
[0042] To remove the headrest, the headrest rod 410 is first pulled upwards until an inner edge of the actuation element 421 , which is offset by 90° relative to the locking element 425 , engages in the stop notch 414 . The inner edge of the actuation element 421 , which is offset by 90° relative to the locking element 425 and engages in the stop notch 414 , can be referred to as a locking element portion (e.g., a second locking element) of the actuation element 421 . By actuating the actuation element 421 in a second manner, in the present case by rotating it (e.g., moving it in a rotary direction) around the headrest rod 410 against the force of the second mounting spring 437 , the inner edge of the actuation element 421 (e.g., the second locking element of the actuation element 421 ) is disengaged from the stop notch 414 , so that the headrest rod 410 can be pulled further upwards. More specifically, FIG. 18 shows the inner edge of the actuation element 421 (e.g., the second locking element of the actuation element 421 ) engaged in the stop notch 414 , and the arrow indicates how to rotate the actuation element 421 for disengaging the actuation element 421 (e.g., the second locking element of the actuation element 421 ) from the stop notch 414 .
[0043] Except where stated otherwise below, the sixth exemplary embodiment is similar in design to the preceding exemplary embodiments, and in particular to the fifth exemplary embodiment, for which reason identical and identically acting components bear reference numbers that are in each case raised by 100. The (first) headrest rod 510 is again provided with several adjustment notches 512 . The stop notch 514 is formed slightly offset, for example by 30°, with respect to the adjustment notches 512 , and it is below the lowest adjustment notch 512 . The headrest rod 510 is inserted into the guide bushing 515 in the head 517 of which is mounted, in a receptacle 519 , the user-accessible (first) actuation element 521 . The actuation element 521 is biased by way of a first mounting spring 527 , namely by the tendency of the first mounting spring 527 to expand, in a manner that urges the actuation element away from a portion of the head 517 of the guide bushing 515 . When the headrest is in use, the locking element 525 of the actuation element 521 engages in one of the adjustment notches 512 .
[0044] For the purpose of adjusting the headrest, the actuation element 521 is actuated in a first manner, i.e. in the present case, seen from above, it is rotated counter-clockwise (e.g., moved in a rotary direction) around the headrest rod 510 , thereby causing the locking element 525 to disengage from the respective adjustment notch 512 , so that the height of the headrest rod 510 can be adjusted. More specifically, FIG. 20 shows the actuation element 521 after rotating and disengaging the locking element 525 from an adjustment notch 512 , and the arrow indicates how the actuation element 521 was rotated counter-clockwise, as seen from above, around the headrest rod 510 . During the engagement of the locking element 525 and the adjustment notch 512 , the actuation element 521 had a position similar to its position in FIG. 21 .
[0045] To remove the headrest, the headrest rod 510 is first pulled upwards until the locking element 525 of the actuation element 521 engages in the stop notch 514 . By actuating the actuation element 521 in a second manner, in the present case by rotating it clockwise (e.g., moving it in a rotary manner), as seen from above, around the headrest rod 510 , the locking element 525 disengages from the stop notch 514 so that the headrest rod 510 can be pulled further upwards. More specifically, FIG. 21 shows the actuation element 521 after rotating and disengaging the locking element 525 from the stop notch 514 , and the arrow indicates how the actuation element 521 was rotated clockwise, as seen from above, around the headrest rod 510 . During the engagement of the locking element 525 and the stop notch 514 , the actuation element 521 had a position similar to its position in FIG. 20 .
[0046] It will be understood by those skilled in the art that while the present invention has been discussed above with reference to exemplary embodiments, various additions, modifications and changes can be made thereto without departing from the spirit and scope of the invention as set forth in the following claims. | In a vehicle seat, in particular a motor vehicle seat having a backrest and at least one headrest rod ( 10 ) that is slidingly guided relative to the backrest and is locked in an in-use position and can be unlocked by actuating at least one actuation element ( 21, 23 ), and also having at least one headrest ( 6 ) mounted on the headrest rod ( 10 ), the headrest being adjustable in height and removable by sliding the headrest rod ( 10 ), two different actuation elements ( 21, 23 ) or two different methods of actuating the actuation element are provided for the adjustment and removal processes. | 1 |
BACKGROUND OF THE INVENTION
This application claims priority to provisional U.S. Application Ser. No. 60/297,570, entitled Mechanism For Implementing Virtual Carrier Sense, invented by Matthew J. Sherman, filed Jun. 12, 2001, and incorporated by reference herein.
FIELD OF THE INVENTION
The invention relates to telecommunications. More particularly, the present invention relates to a method and system for providing Quality of Service (QoS) enhancements and for controlling access to a wireless Local Area Network (WLAN) within an IEEE 802.11 service-type environment.
DESCRIPTION OF THE RELATED ART
The IEEE 802.11 standard (Standard 802.11-1999 being the current issue at the time this application was filed, and which is incorporated by reference herein) is a well-established standard for implementing a Media Access Controller (MAC) and Physical Layer controller/interface (PHY) in wireless LANs (WLANs). The 802.11 protocol is based on the well-known technique called Carrier Sense Multiple Access/Collision Avoidance (CSMA/CA). In this protocol, all stations (STAs) must sense the Wireless Medium (WM) of the WLAN before transmitting. A station (STA) is defined as any device that contains an IEEE 802.11 conformant medium access control (MAC) and physical layer (PHY) interface to the wireless medium. When a STA determines that another STA is already transmitting, the STA defers transmission until the WM is determined to be is clear. The 802.11 standard adds a number of variations to the basic CSMA/CA mechanism. For example, the Physical Carrier Sense (called Clear Channel Assessment or CCA) is a mechanism that informs the 802.11 MAC whether the channel is available for access. The 802.11 MAC also includes another form of carrier sense called the Virtual Carrier Sense.
The Virtual Carrier Sense is primarily implemented through a complex mechanism called the Network Allocation Vector (NAV). The NAV can be described conceptually as a counter implemented at each STA that counts down until the time when the medium is clear. The description of the NAV and the rules and exceptions relating to the NAV, as set forth in the 802.11-1999 specification, are complex, difficult to understand, distributed throughout the 802.11 standard and are not found in one section.
For example, when the NAV counter has a non-zero value, the WM is assumed to be occupied, regardless whether the CCA indicates that the WM is idle, and, accordingly, a STA will not transmit. The NAV can be activated (i.e., set) or cleared based on a number of circumstances, and there are exceptions that allow the NAV to be ignored and for transmission to occur.
Another fundamental concept found in the 802.11 standard is the concept of a Basic Service Set (BSS). By definition, a BSS is a set of stations (STAs) that are controlled by a single coordination function. Infrastructure, within the context of the 802.11 standard, is defined to include the distribution system medium (DSM), access point (AP), and portal entities. Infrastructure is also the logical distribution and integration service functions of an extended service set (ESS). An infrastructure contains one or more APs and zero or more portals in addition to the distribution system (DS). An infrastructure BSS assumes that one STA (referred as an AP) has access to network services that are external to the wireless medium, and provides access to all other STA “associated” with AP. The AP and the STA associated with the AP are referred to as a BSS. It is normally assumed that no STA other than the AP has access to an outside network. An Independent BSS (IBSS) is another form of a BSS. It is assumed that no AP exists in an IBSS and that no STA in an IBSS has access to a network outside the IBSS. Accordingly, a BSS or an IBSS can loosely be thought of as being an independent cell in a cellular network.
A key problem associated with the 802.11 e standard is commonly referred to as the Overlapping BSS problem in which participating STAs in separate BSSs can hear each other's transmissions, and thereby cause their respective CCA functions to defer to each other, and their respective NAV functions to be updated by STAs that are not in the appropriate BSS.
There are drawbacks that are generally only apparent when a Point Coordination Function (PCF) operates in the context of an overlapping BSS. One drawback is that Contention Free Period (CFP) parameters sets from PCFs operating in overlapping BSS may overwrite each other, thereby causing system instability. Another drawback is that a CF-End frame (which indicates the end of a CFP for one of the BSSs) resets the NAV in all STAs receiving the CF-End frame, even when the NAV should still be set for the other BSS when the CFP within that BSS has not yet ended.
Yet another drawback is when a CF-End may also reset the NAV in the middle of an existing frame sequence for which the NAV should still be set. For example, consider an adjacent overlapped BSS situation in which a Request to Send (RTS) frame followed by a Clear to Send (CTS) frame followed by Data frame followed by an ACK (Acknowledgement) frame occurs in one BSS. If a STA in the other BSS “hears” only the CTS frame, its NAV should (properly) be set, thereby preventing transmission by the STA during the pending Data and ACK frames, even when the STA cannot hear the data frame. When a CF-End is received from within the BSS of the STA after the (adjacent-BSS) CTS is received, the STA will be allowed to transmit during the pending Data frame on the adjacent BSS.
Still another drawback is that frame sequences may inappropriately ignore the NAV. For example, when the NAV of a STA is set for a CFP frame occurring in its own BSS, as well as on an adjacent-overlapped BSS, and the STA receives a Polling frame, the STA could respond with a Data frame and possibly interfere with transmissions in the adjacent-overlapped BSS.
Further, while each STA maintains an independent NAV, the NAV value maintained by a particular STA may not be the same NAV value maintained by other STAs within the same BSS. Thus, the behavior of a NAV, as defined by the current 802.11 specification for the NAV, can be unpredictable, particularly for a Point Coordination Function (PCF)-based or a Hybrid Coordination Function (HCF)-based protocol. An HCF is a Point Coordination Function (PCF) that incorporates an enhanced version of the original 802.11 PCF with an enhanced version of the original 802.11 Distributed Coordination Function (DCF) in a single coordination function. Consequently, Quality of Service (QoS) performance can be adversely impacted.
Currently, the 802.11 Standards Committee is developing QoS enhancements for the existing 802.11 standard. A large part of the concept of QoS is the guarantee of the time that a frame (packet) will be delivered on a WLAN. Accordingly, reliable and timely transmission across the wireless medium is critical for achieving QoS.
A number of new protocols have been proposed for the QoS version of 802.11 (referred to as 802.11 e). The new protocols include an Enhanced Distributed Coordination Function (EDCF) and a Hybrid Coordination Function (HCF). When a PCF is present, access to the wireless medium is typically divided into two time periods: a Contention Period (CP) and a Contention Free Period (CFP). The proposed HCF that is included in the current 802.11e draft also permits Contention Free Bursts (CFB). Details of the proposed protocols may be found in the current draft of the 802.11 e standard and many related contributions on the 802.11 web site http://grouper.ieee.org/groups/802/11/. The most recent 802.11 e draft, as of the time of the filing of this application, is D2 and is dated November 2001.
What is needed is a way to provide NAV functionality that overcomes the Overlapped BSS Problem in an IEEE 802.11-type environment. Additionally, what is needed is a way to provide Quality of Service (QoS) enhancements and to control access to a wireless Local Area Network (WLAN) within an IEEE 802.11-type environment.
BRIEF SUMMARY OF THE INVENTION
The present invention provides NAV functionality that overcomes the Overlapped BSS Problem in an IEEE 802.11-type environment. Additionally, the present invention provides Quality of Service (QoS) enhancements and controls access to a wireless Local Area Network (WLAN) within an IEEE 802.11-type environment.
The advantages of the present invention are provided by a method and a system for controlling access to a communication medium of at least one network. According to the present invention, a plurality of event counters are maintained in a station coupled to at least one network through the communication medium. Each event counter has a corresponding context and a corresponding state, and can be embodied as a register or as a virtual counter. Each context defines a response for the corresponding event counter to at least one predetermined event. Each state represents a combined effect for the corresponding counter in response to at least one occurrence of a predetermined event defined by the corresponding context. Determination whether to access the communication medium is based on the state of at least two event counters. Subsequently, the station accesses the communication medium.
According to one aspect of the present invention, the communication medium is a wireless communication medium, at least one network operates in accordance with IEEE-802.11, and at least one network includes at least one Basic Service Set (BSS). Further, at least one network can include an Independent Basic Service Set (IBSS).
According to another aspect of the present invention, at least one event counter is an uncommitted event counter that has been configured in accordance with the corresponding context for the counter. Alternatively or additionally, at least one event counter is a dedicated event counter. Moreover, at least one event counter can have a corresponding context in which at least a portion of the context is implicit.
Alternatively or additionally, at least one event counter can have a corresponding context in which at least a portion of the context is explicit.
According to yet another aspect of the present invention, the context corresponding to at least one event counter can include one of information relating to an event causing the counter to be set, information relating to an event causing the counter to be reset, and information relating to a value of the counter that can block access to the communication medium. The information relating to an event causing the counter to be set can include information relating to a predetermined frame type causing the counter to be set. Alternatively or additionally, the context can further include one of at least one parameter relating to a Contention Free Period (CFP), and information relating to an amount of time that has elapsed since the counter was last updated. Alternatively or additionally, the context corresponding to at least one event counter can include one of information relating to a start of a Contention Free Period (CFP) in a Basic Service Set (BSS) of at least one network, information relating to an end of a CFP in the BSS, information relating to an arrival of a predetermined frame type, information relating to a non-arrival of a predetermined frame type by a predetermined time, information relating to an arrival of a frame containing a duration value, an arrival of a frame containing a transmission suppression command, and information relating to an arrival of a beacon frame containing at least one CFP parameter. Alternatively or additionally, the context corresponding to at least one event counter can include one of information relating to receipt of a duration value, information relating to an arrival of a predetermined frame type, and information relating to a non-arrival of a predetermined frame type by a predetermined time. Alternatively or additionally, the context corresponding to at least one event counter can include information relating to a sequence of received frames.
According to still another aspect of the present invention at least two Basic Service Sets (BSSs) are coupled to the communication medium such that at least one BSS is an outside BSS with respect to a first BSS. When the plurality of event counters are maintained in the first BSS, at least one event counter corresponds to a each outside BSS. The context of each event counter corresponding to an outside BSS defines a response of the event counter to at least one predetermined event occurring in the outside BSS. The state of each event counter corresponding to an outside BSS represents a combined effect for the event counter in response to at least one occurrence of a predetermined event in the outside BSS that is defined by the corresponding context for the outside BSS. Determination whether to access the communication medium is based on the state of at least one event counter corresponding to an outside BSS.
When at least one of the event counters is a Contention Free Bursts (CFB) counter, the context of the CFB counter defines a response of the CFB counter to at least one predetermined CFB-related event. The state of the CFB counter represents a combined effect for the CFB counter to at least one occurrence of a predetermined CFB-related event that is defined by the context corresponding to the CFB counter. Determination whether to access the communication medium is based on the state of at least one CFB counter.
When at least one of the event counters is a Transmission Suppression (TxSup) counter, the context of the TxSup counter defines a response of the TxSup counter to at least one predetermined event during a TxSup time interval, which can be defined on a periodic and/or an aperiodic basis. The state of the TxSup counter represents a combined effect for the TxSup counter in response to at least one occurrence of a predetermined event during the TxSup time interval that is defined by the context corresponding to the TxSup counter. Determination whether to access the communication medium is further based on the state of at least one TxSup counter. The context corresponding to a TxSup counter is received from a Management Action Frame that can include one of multicast addressing and broadcast addressing. When a Management Action Frame is received that contains information relating to event information associated with a Transmission Suppression (TxSup) time interval, it is determined whether an event counter is being maintained for the TxSup time interval. The event counter is updated based on event information received with the Management Action Frame when a TxSup counter is being maintained for the TxSup time interval. An event counter corresponding to the TxSup time interval is created when no TxSup counter is being maintained for the TxSup time interval. In the event that a plurality of TxSup counters are being maintained for corresponding TxSup time intervals and a TxSup counter for the TxSup time interval associated with the received event information cannot be created, a least-recently updated TxSup counter is selected. The selected TxSup counter is then allocated to the TxSup time interval associated with the received event information.
When at least two Basic Service Sets (BSSs) are coupled to the communication medium, such that at least one BSS is an outside BSS with respect to a first BSS, and Basic Service Set Identification (BSSID) information is received within the first BSS identifying an outside BSS; a determination is made whether an event counter is being maintained for the outside BSS identified by the received BSSID information. When an event counter is being maintained for the outside BSS identified by the received BSSID information, the event counter is updated based on event information received with the BSSID information. When no event counter is being maintained for the outside BSS, an event counter is created corresponding to the outside BSS identified by the received BSSID. Alternatively, a least-recently updated event counter corresponding to an outside BSS is selected when a plurality of event counters are being maintained for outside BSSs and when an event counter for the outside BSS identified by the received BSSID cannot be created. The selected event counter is then allocated to the outside BSS identified by the received BSSID. As yet another alternative, an event counter corresponding to an outside BSS can be selected based on a strength of a received Beacon signal for the outside BSS when a plurality of event counters are being maintained for outside BSSs and when an event counter for the outside BSS identified by the received BSSID cannot be created. Similarly, the selected event counter is then allocated to the outside BSS identified by the received BSSID.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is illustrated by way of example and not by limitation in FIG. 1 , which shows a block diagram of an exemplary embodiment of a state machine implementing a NAV system according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a NAV system in which each STA uses more than one event counter for providing NAV functions. Each event counter of the NAV system provides flexible use, has an associated context and, depending upon the context, has a varying limited capability to block transmissions from a STA maintaining the NAV system counter. The context associated with an event counter includes a set of parameters that are maintained by a STA and that are used for determining the events that cause the counter to be set (i.e., to contain a non-zero value) or reset (i.e., to contain a zero value), and when the value of the counter can block transmission by the STA. For example, the context of a first event counter defines the events that set or reset the first counter based on the specific frame types that have or have not been received. The context of a second event counter defines events that all or some of which, can be the same or be different from the events defined by the context of the first counter.
There are many different realizations possible for the NAV system of the present invention. For example, one exemplary embodiment of a NAV system of to the present invention is a single event counter having associated registers. Another exemplary embodiment of the NAV system of the present invention is a virtual NAV counter that is realized in software by a list of events that is used for determining the behavior of the virtual NAV counter. Each event in the list has an associated pointer to a record containing all of the information describing the event that is being accounted for.
The number of event counters used can vary depending on the number of overlapping BSSs and the number of events that a particular STA is intended to accommodate. If, for example, six overlapping BSSs are to be accommodated, eight counters would be required. Seven of the counters would, in particular, be configured as CFP counters (one for the BSS of the STA and six for overlapping BSSs). The eighth counter would be configured as a Duration counter. The single CFP counter for the BSS of the STA could be configured as a dedicated counter or an uncommitted event counter that as been assigned. Each of the six CFP counters for the overlapping BSSs could be configured as either dedicated or uncommitted (i.e., assignable) counters. In the situation in which a counter is configured as an uncommitted counter, events that are unrelated to events associated with an overlapping BSS can be accommodated.
As mentioned, an event counter can be dedicated or uncommitted (i.e., assignable). Additionally, the context of a counter can be explicit or implicit. When an event counter is configured as a dedicated counter, such as a dedicated CFP counter for the BSS of a STA or a dedicated Duration counter, the context is implicit. When the BSS of a STA and any overlapping BSSs do not use an HCF, the context for a particular event counter includes an identification of each event causing the counter to be set and the Frame Type causing the counter to be set. For example, when the counter is a Duration counter, the context includes information indicating whether an RTS frame causes the Duration counter to be set. Additional context information includes the Basic Service Set Identification (BSSID) corresponding to the counter. When an event counter is configured as a CFP counter, the context includes CFP parameters. When the BSS of a STA and any overlapping BSSs use an HCF, additional context information is required, such as the MAC address of the STA currently holding a transmission opportunity from the HCF.
The rules governing the CFP NAV system of the present invention are as follows. Each STA maintains a single CFP NAV counter corresponding to the BSS of the STA. Each CFP NAV counter, whether dedicated or assignable, is set at the start of a CFP for the corresponding BSSID for the particular CFP NAV counter. CFP parameter values for each respective BSSID are received from a Beacon frame or a Probe Response frame broadcast by the BSS associated with the counter. When a BSSID is received and no CFP NAV counter has been assigned, and the STA has sufficient resources for creating a new CFP NAV counter, the STA sets up a new CFP NAV counter for the new BSSID. When a new BSSID is identified by a STA, but the STA has no available CFP NAV counters nor sufficient resources for creating a new CFP NAV counter, the STA assigns and overwrites the least-recently updated CFP NAV counter to the newly-identified BSSID, except when the least-recently updated CFP NAV counter is the dedicated CFP NAV counter for BSS of the STA. Information relating to how recently a CFP NAV counter has been updated is contained in the context for the counter. Alternatively or additionally, a digital signal processing (DSP)-type filter may be used in a well-known manner for filtering received Beacon signal strength so that only CFP NAV counters corresponding to the strongest beacons are maintained.
Each CFP NAV counter maintained by a STA is automatically set (i.e., recurring set) for the beginning of every CFP. For compliance with the existing IEEE 802.11 standard, the CFP NAV for the BSS of the STA must be updated prior to the first transmission from the STA. Also, a STA originating an RTS frame, for example, does not set the CFP NAV for the BSS, nor does a reply CTS frame cause the CFP NAV for the BSS of the STA to be set. Rather, RTS and CTS frames set the duration NAV based on the duration value contained in their MAC headers. When a CF-End frame for a particular BSSID is received by a STA, the CFP NAV counter corresponding to the BSSID of the received CF-End frame is reset.
The single Duration NAV counter that each STA maintains for the BSS of the STA is set to a nonrecurring value. In particular, the Duration NAV counter is set to a received duration value when the received duration value is greater than the current value of the Duration NAV counter. The second largest received duration value is also tracked because if an event occurs that resets the current value on the Duration NAV counter, the counter should be set back to the next largest duration value rather than to zero. The Duration NAV counter is not set or reset by the start or end of any CFP, nor is the Duration NAV counter set when the STA is a source or a destination STA. For compliance with IEEE 802.11, the Duration NAV of the present invention is set for an ACK frame plus SIFS (short interframe space) in response to a PS-Poll frame. Additionally, the Duration NAV counter is automatically reset when it expires, and is reset when a RTS (request to send) frame with no subsequent CTS (clear to send) frame occurs and no frame starts after the CTS time. The Duration NAV, however, is reset to the next smallest valid duration value rather than to zero.
A STA ignores all of the NAV counters that are maintained by the STA in order to respond with an ACK frame or to a Polling frame. A STA responds only with an ACK frame or a Null frame when the Duration NAV counter is set or a CFP NAV counter for a BSS other than the BSS of the STA is set. When a STA responds with an ACK frame and has data to respond with, but the NAV counter is suppressing transmission by the STA, the More Data field bit of the ACK frame is set. A STA does not respond or transmit for any other frame when any NAV counter is set.
Note that the final implementation of 802.11 e may chose not to respond to a polling frame when the Duration NAV counter is set or a CFP NAV counter for a BSS other than the BSS of the STA is set. Or, the final implantation may simply chose to respond with a Null data frame with the More Data field bit set when the Duration NAV counter is set or a CFP NAV counter for a BSS other than the BSS of the STA is set. Or, the standard may ultimately chose to respond to a poll with an actual data frame (when data is available) when the Duration NAV counter is set or a CFP NAV counter for a BSS other than the BSS of the STA is set. While these three potential behaviors are mutually exclusive, there is rationale for and against each behavior. The present invention described herein enables each of the possible behaviors by separating the function of tracking a STA's own CFP NAV from the other causes setting the NAV.
FIG. 1 shows a block diagram of an exemplary embodiment of a state machine 100 implementing a NAV system according to the present invention. State machine 100 includes CPF NAV counters 101 0 through 101 N−1 , Duration NAV counter 101 N , set bits 102 0 through 102 N−1 counter contexts 103 0 – 103 N , and gating 104 . Counter contexts 103 0 – 103 N are respectively associated with CPF NAV counters 101 0 through 101 N−1 and Duration NAV counter 101 N . For exemplary implementation shown, CFP Counters are used for counting the time to the next CFP, as well. The SET bit is used for differentiating between two counts. That is, when the SET bit is zero, the counter is counting the time until the beginning of the CFP. Logic 104 prevents the effects of this counting from setting the NAV. When the SET bit is one, the counter is counting the time until the end of the CFP on that counter, and logic 104 permits the NAV to be set during this part of the operation. For clarity, the details of how to reset and set the various counters, which depends on the context of each particular NAV counter, are not shown. Also, details of logic 104 that is required on the Full and Other NAV outputs is also not shown for simplicity.
To implement the QoS enhancements set forth in the 802.11 e draft for the HFC, the present invention provides additional NAV usage rules, as follows. The CFP NAV counter corresponding to the BSS of a STA is ignored when the STA responds to a RTS frame (Respond CTS), a Probe (Respond Probe Response) frame, and a contention control (CC) (Respond RR as appropriate). A Contention Free Bursts (CFB) NAV counter is created and maintained that operates with an non-recurring set and is set by a received Duration value. The CFB NAV counter is also set from the value in the Duration field in a QoS Poll frame from the Hybrid Coordinator (HC), which supervises the HCF. The CFB NAV counter is reset for the occurrence of a new QoS poll from the HC, and is set to the value of a Duration field from a poll frame, even when the value of the Duration field from the poll frame is less than the current value of the CFB NAV counter. The CFB NAV counter is reset when a CF-End frame is received from the BSS of the STA. The CFB NAV counter is ignored when the STA responds to a RTS frame, a Probe frame and a CC frame.
The generalized NAV counter approach of the present invention also provides a Transmission Suppression (TxSup) NAV counter capability that can be customized to the environment of each STA for suppressing transmissions from a STA on a periodic or aperiodic basis during a TxSup time interval. This aspect of the present invention provides controlled access to the medium. Such a capability does not exist in the current 802.11 e draft of 802.11-1999 standard. A Management Action Frame is used to load the context for each TxSup NAV counter used. Multicast and broadcast addressing are allowed for the Management Action Frame. The context of a TxSup NAV counter can use the same parameters as are used for the context of a CFP NAV counter, and can use the same response rules as used for the CFP NAV counters are also used. Each TxSup NAV counter takes precedent over CFP NAV counters, except for the CFP NAV counter corresponding to the BSS of the STA. When no unassigned NAV counters are available when a STA creates a TxSup NAV counter, the least-recently updated CFP NAV is replaced with the new TxSup NAV counter. When multiple TxSup NAV counters are used, a STA replaces the least-recently updated TxSup NAV counter.
As previously mentioned, an exemplary embodiment of a virtual NAV system according to the present invention can be an event-driven state machine implemented in software in which each bit in a single NAV register represents the state of each of the individual NAV counters of the NAV system. A full NAV Mask is used for defining valid NAV counters, that is, a mask is used for determining which of the NAV counters are in use. Other NAV Masks are used for excluding the BSS CFP NAV counter and the CFB NAV counter of the STA. Separate masks are used for producing the Full NAV and Other NAV outputs, such as shown in the Figure. The full context is required for realizing all three modes of operation that are described the IEEE 802.11-1999, 802.11e (HFC), and TxSup extension standards. Each NAV counter has a context that includes a NAV Type, the Frame Type of last set; the Time that the NAV counter was last set; the CF Period, the CF Length, and the BSSID. The NAV Type can be, for example, a Duration NAV-type, a CFB NAV-type, a CFP NAV-type and a TxSup NAV-type. The Frame Type will be null when the NAV counter is not set by the last frame type or when the NAV counter is a CFP NAV counter. The CF Period will be null when the NAV counter is a Duration NAV counter or a CFB NAV counter. The CF Length will be null when the NAV counter is a Duration NAV counter or a CFB NAV counter. The BSSID will be null when the NAV counter is a Duration NAV counter or a TxSup NAV counter.
A time-ordered list of pending events is maintained by the software implementation. Preferably, at least sixteen time-ordered events are supported. Alternatively, any number of events can be supported that provides sufficient NAV functionality. Each event also has an associated context that describes how the event should be interpreted when the event occurs. The Event Context includes the Time of Event, the NAV Number (i.e., the particular bit of NAV that is affected, the Type of event, such as a set or a reset, Qualifiers, and RTS Auto Reset. RTS Auto Reset is canceled when a CTS or a start of response frame is detected.
As events occur, the events are removed from the time-ordered list. Removal of an event from the time-ordered list may accordingly cause another event to be added to the list, based on the context of the counters and event list. Other events, such as receiving particular frames, may cause the pending list to be modified.
A timer is set for an event that is expected to occur next in the time-ordered event list. When the timer expires, either the event is implemented and/or the next event is scheduled for recurring events (implementing, for example, the same functionality of the SET bit as previously described). When a frame is received, the present invention determines whether there is a potential NAV impact and, if so, the event is processed based on the NAV system rules of the present invention.
The 802.11 Management Information Base (MIB) could be modified so that the current state and the full context of the NAV counter system according to the present invention in each STA could be accessible for supporting other Overlapped BSS mechanisms.
While the invention has been described with respect to specific examples including presently preferred modes of carrying out the invention, those skilled in the art will appreciate that there are numerous variations and permutations of the above described systems and techniques that fall within the spirit and scope of the invention as set forth in the appended claims. | A method and a system for controlling access to a communication medium of at least one network uses a plurality of event counters that are maintained in a station coupled to at least one network through the communication medium. Each event counter has a corresponding context and a corresponding state. Each context defines a response for the corresponding event counter to at least one predetermined event. Each state represents a combined effect for the corresponding counter in response to at least one occurrence of a predetermined event defined by the corresponding context. Determination whether to access the communication medium is based on the state of at least two event counters. | 7 |
CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of U.S. patent application Ser. No. 12/363,117 filed Jan. 30, 2009, which is a continuation-in-part of U.S. patent application Ser. No. 12/025,249 filed Feb. 4, 2008 now abandoned, which are both incorporated by reference in its entirety.
BACKGROUND
1. Field of the Invention
Embodiments of the present invention generally relate to adjustable applicators. More particularly the invention relates to applicators that can be adjusted as per user's convenience for application of a cosmetic or a care product.
Applicators of the present invention can be employed in application of various products, such as for viscous cosmetics, for coloring strands of hair, and for dental flossing or for applying pharmaceuticals or cleaning agents.
2. Description of the Related Art
Various applicators for applying a substance are known. There are certain application areas where there is a requirement of curving the applicator as per user's convenience. Some such areas include application of mascara or in the cleaning of dental interstices. Majority of the existing applicators for such usages are pre-curved at a certain angle. For example U.S. Pat. No. 4,326,548 to Wagner discloses an oral hygiene tool comprising of a pen barrel shaped holder that carries a curved dental pick. Another example is that of U.S. Pat. No. 6,082,999 to Tcherny et. Al. which discloses a reusable flexible interdental device that has advantages of a toothpick and an interdental brush and also provides flexibility in two mutually perpendicular directions. However, the flexibility achieved is not controllable by the user. Therefore, there exists a need for a personal oral hygiene tool which can be used as per convenience by the user.
Also, mascara, an important make-up accessory used to darken and define eyelashes to accentuate the eyes, is difficult to apply because of the target area of application. The eyelashes offer a very small application area, while being soft, flexible, delicate and in close proximity to very sensitive eye tissue. Therefore, a mascara product would be liked by the consumers when a right kind of applicator is provided to them for easy application as the overall consumer experience depends on both the product and on the applicator used to apply it.
Mascara applicators such as twisted wire mascara brushes, curved mascara brushes and adjustable mascara applicators are known in the art. Curved mascara brushes permit contact of the brush with more eyelashes along a correspondingly curved eyelid. However, the rigid curved brush is a more difficult instrument to learn to use in the confines of the eye area, particularly the corners of the eye where a straight brush works better. Another drawback of pre-curved brush is that it is not readily adjustable to conform to a particular user's eyelid curvature. In addition, the curvature of the upper and lower eyelids is rarely the same and a brush curved to fit the upper lid will not properly fit the lower lid.
Adjustable mascara brushes are known in the prior art. It is known to provide adjustment of the angle of the brush or applicator relative to the applicator wand or handle as in U.S. Pat. No. 4,428,388 to Cassai et al. and the amount of brush exposed as in U.S. Pat. No. 4,598,723 to Cole.
U.S. Pat. No. 5,137,038 to Kingsford discloses an adjustable mascara applicator which can be adjusted by a user from straight to curved by the help of an extendable rod which is slidably disposed in the applicator wand. This rod may be straight to straighten a precurved applicator or curved so as to impart curvature to a straight applicator.
U.S. Pat. No. 6,309,125 to Andrea Peters discloses an adjustable mascara applicator that includes a brush attached to a bendable wand which is characterized by recovery memory in which it automatically assumes a predetermined bend angle in the absence of bending force.
While International Patent application WO 2007/117091A1 to Amorepacific Corporation, discloses an adjustable mascara brush that includes a brush stick provided in a cap, a brush provided at the end of the brush stick and an elevating bar which is connected to the brush stick in a manner of screw wherein the brush gets straightened when the elevating bar is lowered and the brush gets curved when the elevating bar is elevated up.
Although many of these prior art adjustable applicators are relevant with respect to the present invention, most of them use an additional component i.e. a rod that is either pre-bent or has a recovery memory. Moreover, none of the designs propose a mechanism by which the applicator element could be straightened or curved to varying degrees without the usage of additional component.
Therefore, there exists a need for an applicator that provides ease-of-use as well as is modifiable to adapt to the shape requirement of the user.
Further, there may also be a requirement by the user to lift and curl the eyelashes, which generally requires a different instrument such as a curler. However, it would be desirable that a single applicator is able to apply and lift and curl the lashes. Therefore, there is a need for an applicator that provides added function of lifting and curling the eyelashes.
SUMMARY
The present invention generally is an adjustable applicator employed for application of a cosmetic or a care product such as for application of mascara, coloring strands of hair, for dental flossing or for applying pharmaceuticals or cleaning agents. The use of adjustable applicator of the present invention for removal of make up products is also contemplated.
According to an embodiment of the invention, there is provided an applicator which employs an inventive mechanism to enable angular deformation of the applicator element to varying degrees of deformation.
In accordance with an embodiment of the invention, the adjustable applicator of the invention comprises of an applicator element and a filament. In the applicator element is provided a bore that houses the filament. Further, the filament is arranged to be movable inside the bore of the applicator element.
According to an embodiment of the invention the bore in the applicator element may be either centrally or non-centrally aligned.
According to yet another embodiment of the invention, the applicator element may be molded as a single piece from an elastically deformable material. The applicator element may be produced from an elastomer or any other elastic material allowing compression and expansion of the applicator element.
According to an embodiment of the invention, the filament may be made out of a material selected from a polymeric material and metals.
According to an embodiment of the invention, the filament is so arranged as to cause progressive modification in the shape of the applicator element. The filament facilitates adjustment of the angular deformation of the applicator element.
According to an embodiment of the invention the applicator element further comprises a biasing member arranged so as to assist the material memory of the applicator.
According to yet another embodiment of the invention, one end of the filament is connected to the distal end of the applicator element and the other end of the filament is attached to a clasping means such that when force is applied on the clasping means it causes tension along the axis of the filament which results in angular deformation of the applicator element. Further, the force applied to the clasping means is directly proportional to the deformation angle of the applicator element achieved. The filament may alternatively be connected by way of a locking arrangement with the distal end of the applicator element thereby guiding the movement of the applicator. For example, when the filament is in a stretched state it causes the applicator to be bent while when it is in relaxed state it guides the applicator to come back to its straight position.
According to an embodiment of the invention the clasping means may be provided at the proximal end of the filament itself. Alternatively, the filament may be engaged with another element having clasping or any other suitable means for application of force. Further, the mode of application of force on the clasping means could be manual, mechanical, magnetic, electrical or any other suitable mode.
According to an embodiment of the invention the applicator element may have a substantially circular outside cross-section, but the case in which the deformable applicator element has a cross-section of different shape, such as polygonal, is also contemplated by this invention.
According to yet another embodiment of the invention, the filament may be fixed tautly at both the ends of the applicator element such that the angular deformation in the applicator element is caused by application of force along the axis of the applicator.
Independently or in combination with the above, exemplary embodiments of the invention provide a device for packaging and dispensing a substance, for example, a cosmetic, comprising an applicator as defined above. The device may comprise a receptacle and an adjustable applicator. The adjustable applicator in such a device may comprise a gripping member, a stem having a cavity and an applicator element wherein the stem may be connected to the applicator element at one end and to the gripping member at another end. The said device may also include a wiper member. The gripping member may comprise a cap for closing the receptacle and a manipulating means for adjusting the angular deformation of the applicator element. The said manipulating means could be connected to a movable member present inside the cap in such a way that its rotational movement with respect to the cap is restricted while translational movement is allowed and said movable member is connected to the filament in the applicator element.
According to another embodiment of the invention the movable member of the packaging device may be connected to the filament via another filament that passes through the cavity inside the stem and hooks up the filament of the applicator. In such a case, the force provided by the manipulating means effects synchronous movement of both the filament in the stem as well as the filament in the applicator with respect to the gripping member thereby adjusting the angular deformation of the applicator element.
According to yet another embodiment of the invention, the adjustable applicator may comprise a stem connected to the applicator element at one end and a gripping member provided at another end of the stem. The stem may be hollow from inside. The gripping member may comprise a handle member and a manipulating means for adjusting the angular deformation of the applicator element. The said manipulating means could be connected to a movable member present inside the handle in such a way that its rotational movement with respect to the handle is restricted while translational movement is allowed and said movable member is directly connected to the filament that passes through the cavity in the stem to the applicator element. In a further embodiment, the movable member may also be connected to the filament via a separate filament that passes through the cavity inside the stem and hooks up the filament of the applicator member. In such a case, the force provided by the manipulating means effects synchronous movement of both the filament in the stem as well as the filament in the applicator with respect to the handle for adjusting the angular deformation of the applicator element.
According to an embodiment of the invention, there is provided an adjustable applicator wherein the user has more control over the curved angle achieved in the applicator. Further, a constant rigidity of the applicator is provided as no additional component is inserted or withdrawn to achieve the straight or curved shape.
According to another embodiment of the invention, the applicator element is capable of being used for application of a care product such as a dental floss or in a cosmetic product such as mascara. Further, the adjustable applicator could also be used for removal of a cosmetic product such as mascara.
According to yet another embodiment of the invention there is provided an applicator which employs an inventive mechanism to enable radially-angular deformation of the applicator element to varying degrees of deformation. The radially angular deformation being defined herein as the angular deformation occurring on the radial axis of the applicator element. Further, the deformation may be regular or irregular. Alternatively, the deformation in the applicator may follow a helical path.
According to yet another embodiment of the invention the adjustable applicator comprises an applicator element and a filament. In the applicator element is provided a bore that houses the filament such that the filament is arranged to be movable inside the bore of the applicator element. The bore in the applicator element may be either centrally or non-centrally aligned. The applicator element may be molded as a single piece from an elastically deformable material. The applicator element may be produced from an elastomer or any other elastic material allowing radially-angular deformation of the applicator element.
According to an embodiment of the invention, the filament may be made out of a material selected from a polymeric material and metals.
According to an embodiment of the invention, the filament is so arranged as to cause progressive modification in the shape of the applicator element, there occurs a progressive decrease or increase in the angle of deformation of the applicator element. The filament facilitates adjustment of the radially-angular deformation of the applicator element. The radially-angular deformation may be distributed evenly throughout the applicator element i.e. the angular gap is maintained evenly in the body of the applicator element. As an exemplary embodiment the radially-angular deformation in the applicator element may be such that there occurs twisting of the body of the applicator element. Alternatively, the angular deformation may be irregular or uneven in the body of the applicator element. When the applicator element is a mascara brush, the angular deformation in the applicator element helps in lifting and curling of the eyelashes.
According to an embodiment of the invention the applicator element further comprises a biasing member arranged so as to assist the material memory of the applicator.
According to yet another embodiment of the invention, one end of the filament is connected to the distal end of the applicator element and the other end of the filament is attached to a clasping means such that when force is applied on the clasping means it causes tension along the radial axis of the filament which results in angular deformation of the applicator element. Further, the force applied to the clasping means is directly proportional to the deformation angle of the applicator element achieved. The filament may alternatively be connected by way of a locking arrangement with the distal end of the applicator element thereby guiding the movement of the applicator. For example, when the filament is in a stretched state it causes the applicator to be angularly deformed while when it is in relaxed state it guides the applicator to come back to its straight position.
According to an embodiment of the invention the clasping means may be provided at the proximal end of the filament itself. Alternatively, the filament may be engaged with another element having clasping or any other suitable means for application of force. Further, the mode of application of force on the clasping means could be manual, mechanical, magnetic, electrical or any other suitable mode.
According to an embodiment of the invention the applicator element may have a substantially circular outside cross-section, but the case in which the deformable applicator element has a cross-section of different shape, such as polygonal, is also contemplated by this invention.
According to yet another embodiment of the invention, the filament may be fixed tautly at both the ends of the applicator element such that the angular deformation in the applicator element is caused by application of force along the axis of the applicator.
Independently or in combination with the above, exemplary embodiments of the invention provide a device for packaging and dispensing a substance, for example, a cosmetic, comprising an applicator as defined above. The device may comprise a receptacle and an adjustable applicator. The adjustable applicator in such a device may comprise a gripping member, a stem having a cavity and an applicator element wherein the stem may be connected to the applicator element at one end and to the gripping member at another end. The said device may also include a wiper member. The gripping member may comprise a cap for closing the receptacle and a manipulating means for adjusting the angular deformation of the applicator element. The said manipulating means could be connected to an inner rod present inside the cap in such a way that its rotational movement with respect to the cap is allowed and said inner rod is further connected to the filament in the applicator element.
According to yet another embodiment of the invention, the adjustable applicator may comprise a stem connected to the applicator element at one end and a gripping member provided at another end of the stem. The stem may be hollow from inside. The gripping member may comprise a handle member and a manipulating means for adjusting the angular deformation of the applicator element. The said manipulating means could be connected to an inner rod present inside the handle in such a way that its rotational movement with respect to the handle is allowed and said inner rod may be in the form of a filament that passes through the cavity in the stem and connects to the applicator element. In a further embodiment, the inner rod may be connected to the applicator filament and hooks up the filament of the applicator member. In such a case, the force provided by the manipulating means effects synchronous movement of both the inner rod in the stem as well as the filament in the applicator with respect to the handle for adjusting the angular deformation of the applicator element.
According to an embodiment of the invention, there is provided an adjustable applicator wherein the user has more control over the angular deformation achieved in the applicator. Further, a constant rigidity of the applicator is provided as no additional component is inserted or withdrawn to achieve the straight or angularly deformed shape.
These and further aspects which will be apparent to the expert of the art are attained by an adjustable applicator in accordance with the main claim.
BRIEF DESCRIPTION OF THE DRAWINGS
So that the manner in which the above recited features of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings. It is to be noted, however, that the appended drawings illustrate only typical embodiments of this invention and are therefore not to be considered limiting of its scope, for the invention may admit to other equally effective embodiments.
FIG. 1 illustrates an isometric view of the applicator according to an embodiment of the invention;
FIG. 2 is a cross sectional view of the applicator taken along the line A-A of FIG. 1
FIG. 3 is a cross sectional view of the applicator in curved position taken along the line A-A of FIG. 1 ;
FIG. 4 illustrates an isometric view of the device comprising the adjustable applicator according to one embodiment of the present invention;
FIG. 5 illustrates an exploded view of the device of FIG. 4 ;
FIG. 6 is an isometric view of the adjustable applicator according to one embodiment of the present invention;
FIG. 7 illustrates a cross-sectional view of the device of FIG. 4 ;
FIG. 8 is cross sectional view of the device of FIG. 6 ;
FIG. 9 is cross sectional view of the device of FIG. 6 when the applicator is in curved position; line A-A of FIG. 3 ;
FIG. 10 is an isometric view of an adjustable applicator according to another embodiment of the present invention;
FIG. 11 is an isometric view of the device containing the adjustable applicator of FIG. 10 ;
FIG. 12 represents a cross-sectional view of the adjustable applicator of FIG. 10 ;
FIG. 13 represents a cross-sectional view of the device of FIG. 11 ;
FIG. 14 a illustrates the isometric views of the adjustable applicator of FIG. 10 ;
FIG. 14 b is an isometric view of the adjustable applicator of FIG. 10 showing the applicator as seen upon 180 degree radially-angular deformation;
FIG. 14 c is an isometric view of the adjustable applicator of FIG. 10 showing the applicator as seen upon 360 degree radially-angular deformation;
FIG. 15 a is a front view of the adjustable applicator of FIG. 10 ;
FIG. 15 b is a front view of the adjustable applicator of FIG. 10 showing the applicator as seen upon 180 degree radially-angular deformation;
FIG. 15 c is an isometric view of the adjustable applicator of FIG. 10 showing the applicator as seen upon 360 degree radially-angular deformation;
FIG. 16 a is a top view of the adjustable applicator of FIG. 10 ;
FIG. 16 b is a top view of the adjustable applicator of FIG. 10 showing the applicator as seen upon 180 degree radially-angular deformation;
FIG. 16 c is a top view of the adjustable applicator of FIG. 10 showing the applicator as seen upon 360 degree radially-angular deformation;
FIG. 17 a is an isometric view of an adjustable applicator according to another embodiment of the invention;
FIG. 17 b is an isometric view of the adjustable applicator of FIG. 17 a showing the applicator as seen upon 180 degree radially-angular deformation;
FIG. 17 c is an isometric view of the adjustable applicator of FIG. 17 a showing the applicator as seen upon 360 degree radially-angular deformation;
FIG. 18 a is a front view of the adjustable applicator of FIG. 17 a;
FIG. 18 b is a front view of the adjustable applicator of FIG. 17 a showing the applicator as seen upon 180 degree radially-angular deformation;
FIG. 18 c is an isometric view of the adjustable applicator of FIG. 17 a showing the applicator as seen upon 360 degree radially-angular deformation;
FIG. 19 a is a top view of the adjustable applicator of FIG. 17 a;
FIG. 19 b is a top view of the adjustable applicator of FIG. 17 a showing the applicator as seen upon 180 degree radially-angular deformation;
FIG. 19 c is a top view of the adjustable applicator of FIG. 17 a showing the applicator as seen upon 360 degree radially-angular deformation;
To facilitate understanding, identical reference numerals have been used, where possible, to designate identical elements that are common to the figures. It is to be noted, however, that the appended drawings illustrate only typical embodiments of this invention and are therefore not to be considered limiting of its scope, for the invention may admit to other equally effective embodiments.
DETAILED DESCRIPTION
The adjustable applicator according to one embodiment of the present invention is shown in FIGS. 1 to 3 .
FIG. 1 is one embodiment of the present invention showing the adjustable applicator 100 . The adjustable applicator 100 of the invention comprises of an applicator element 101 and a filament 102 . In the applicator element 101 is a bore 104 housing the filament 102 . The bore 104 may either be centrally or non-centrally aligned. The filament 102 is arranged to be movable inside the bore 104 of the applicator element 101 . The applicator element 101 may be produced from an elastomer or any other elastic material allowing compression and expansion of the applicator. Further, the filament 102 may be made out of a material selected from a polymeric material and metals. The filament 102 is so arranged as to cause progressive angular deformation of the applicator element 101 .
As shown in FIGS. 2 and 3 , one end of the filament 102 is connected at a distal end 103 of the applicator 100 and the other end of the filament 102 is attached to a clasping means 105 such that when force is applied on the clasping means 105 it causes tension along the axis of the filament 102 , which results in angular deformation of the applicator element 101 as is illustrated in FIG. 3 . Further, the force applied on the filament 102 is directly proportional to the deformation angle of the applicator element 101 achieved. The mode of application of force on the clasping means 105 could be manual, mechanical, magnetic, electrical or any other suitable mode to cause tension along the axis of the filament 102 . Moreover, the applicator element 101 may have a substantially circular outside cross-section, but the case in which the deformable applicator element 101 has a cross-section of different shape, such as polygonal, is also contemplated by this invention. Further, the applicator element may further comprise of a biasing member arranged so as to assist the material memory of the applicator element.
A device 200 for packaging and dispensing a substance comprising the said applicator is illustrated by FIGS. 4 and 5 . The device 200 comprises a gripping means 201 and a receptacle 202 containing the substance. As shown in FIG. 6 , the gripping means 201 further comprises a handle 203 , a stem 204 and an applicator 205 . The proximal end of the stem 204 is connected to the handle 203 while its distal end is connected to the applicator 205 . The handle 203 acts as a manipulating means for adjusting the deformation of the applicator 205 . The handle 203 further comprises a cap 206 and a casing 207 that houses a movable member 208 . FIGS. 6 to 8 illustrate the gripping means 201 in further details and the arrangement of various parts of the device 200 . As shown in FIGS. 7 to 9 , one end of the casing 207 has ledges 209 which mate with complimentary ledges 210 in the cap 206 , thereby restricting movement of the cap 206 along its longitudinal axis and at the same time allowing rotational movement of the cap 206 with respect to the casing 207 . However, any lock and key arrangement between the casing and cap could be used for restricting axial movement of the cap with respect to the casing. The movable member 208 is hollow from inside and is so arranged with the cap 206 that its rotational movement with respect to the cap 206 is restricted. The casing 207 has threads 216 in its inner surface just above its centre towards its proximal end that mate with the threads in the movable member 208 , thereby allowing movement of the movable member 208 along its axis. Further, below the centre point of casing 207 is present an annular ridge 217 through which it cooperates with the stem 204 . Also present are threads 219 at distal end of the casing 207 which cooperate with the threads 220 in the neck of the receptacle 202 helping in fastening and unfastening of the gripping member 201 with respect to the receptacle 202 . The stem 204 houses a separate filament 213 . However, there may be present one filament that extends through the stem and the applicator element. At the proximal end of the movable member 208 is provided a feature for example a groove 212 to hold one end of the filament 213 . The filament 213 has a groove 214 at its distal end which engages the applicator filament 215 . The applicator 205 is hollow from inside and houses the applicator filament 215 . Also, one end of the applicator filament 215 is fitted inside the applicator 205 . The applicator filament 215 is adjusted with the groove 214 such that it is off-centered and provides a favorable and consistent plane along which angular deformation of the applicator occurs. However, the groove 214 may also be centrally aligned. Further, in such an arrangement, the force exerted via the gripping means 201 effects synchronous movement of both the filament 213 in the stem as well as the applicator filament 215 with respect to the applicator 205 to cause the desired angular deformation of the applicator 205 . The said device 200 may also include a wiper member 218 .
FIG. 9 illustrates the applicator 205 in its angularly deformed state. The rotation of the cap 206 with respect to the casing 207 results in the axial displacement of the movable member 208 thereby displacing the filament 213 and the applicator filament 215 along with it. The displacement in the applicator filament 215 causes the applicator 205 to angularly deform.
During use, the user rotates the cap 206 with respect to the casing 207 of the gripping means to cause the applicator 205 to be suitably deformed along a desired axis. Also, the user can control the magnitude of deformation during use.
FIG. 10 is another embodiment of the present invention showing a device 350 containing an adjustable applicator 300 . The device 350 for packaging and dispensing a substance comprising the said adjustable applicator 300 is illustrated by FIGS. 11 to 13 . The device 350 comprises a gripping means 301 and a receptacle 302 containing the substance. As shown in FIGS. 10 to 13 , the gripping means 301 further comprises a handle 303 , a stem 304 and an applicator element 305 . In the applicator element 305 is a bore housing an applicator filament 306 . The bore may either be centrally or non-centrally aligned. The applicator filament 306 is arranged to be movable inside the bore of the applicator element 305 . The applicator element 305 may comprise of bristles, discs or flocked applicator element or any suitable applicator suitable for cosmetic use. Further, the applicator element 305 may be produced from an elastomer or any other elastic material allowing compression and expansion of the applicator. Further, the applicator filament 306 may be made out of a material selected from a polymeric material and metals. The applicator filament 306 is so arranged as to cause progressive angular deformation of the applicator element 305 . Further, the applicator element 305 may house a biasing means. Furthermore, the proximal end of the stem 304 is connected to the handle 303 while its distal end is connected to the applicator element 305 . The handle 303 acts as a manipulating means for adjusting the angular deformation of the applicator element 305 . As shown in FIGS. 11 to 13 , the handle 303 of the gripping member 301 further comprises an actuator means 303 a which causes the radially-angular deformation in the applicator element 305 . The radially-angular deformation being defined herein as the angular deformation occurring on the radial axis of the applicator element. The handle 303 further houses an inner rod 307 such that the inner rod 307 is connected to the actuating means 303 a . As seen in FIG. 11 , the protrusion in the proximal end of the inner rod 307 sits inside the hollow of the actuating means 303 a while the distal end of the inner rod 307 is engaged with the applicator filament 306 . Further, the inner rod 307 is encased in the stem 304 of the gripping means 301 . Further, the applicator element 305 has a free end 305 a and a fixed end 305 b such that the fixed end 305 b is fixed to the stem 304 of the gripping means 301 . As shown in the drawings the applicator filament 306 is housed in the applicator element 305 while the inner rod 307 is housed in the stem 304 , however, there may be present one filament that extends through the stem and the applicator element. The distal end of the inner rod 307 is provided a feature for example a groove to hold one end of the applicator filament 306 . The applicator element 305 is hollow from inside and houses the applicator filament 306 . Also, one end of the applicator filament 306 is fitted inside the applicator element 305 . The bore inside the applicator element 305 provides a favorable and consistent plane along which angular deformation of the applicator element 305 occurs. Further, in such an arrangement, the force exerted via the gripping means 301 effects synchronous movement of both the inner rod 307 in the stem 304 as well as the applicator filament 306 with respect to the applicator element 305 to cause the desired angular deformation of the applicator element 305 . The said device 350 may also include a wiper member 308 . Also present are threads at distal end of the handle 303 which cooperate with the threads in the neck of the receptacle 302 helping in fastening and unfastening of the gripping member 301 with respect to the receptacle 302 .
During use, the user rotates the actuating means 303 a with respect to the handle 303 of the gripping means 301 to cause the applicator 305 to be suitably angularly deformed at a desired degree. Also, the user can control the magnitude or degree of angular deformation during use.
FIGS. 14 a , 14 b and 14 c illustrate the isometric view of the applicator 305 in its normal state, deformed state with an angular deformation of 180 degrees and deformed state with angular deformation of 360 degrees respectively. The rotation of the actuating means 303 a with respect to the handle 303 results in the synchronous rotation of the inner rod 307 thereby angularly deforming the applicator filament 306 which inn turn causes the applicator 305 to angularly deform. The degree of angular deformation of the applicator filament 306 and hence the applicator 305 depends on the similar force applied to the actuating means 303 a . As an exemplary embodiment, when the actuating means 303 a is rotated to a less extent, the degree of angular deformation is less in the applicator 305 and if the degree of rotation is high then the degree of angular deformation is higher in the applicator. As represented by FIG. 14 b , the degree of angular deformation in the applicator 305 is 180 degrees while in FIG. 14 c , the degree of deformation of applicator 305 is 360 degrees.
FIGS. 15 a , 15 b and 15 c illustrate the front view of the applicator 305 in its normal state, deformed state with an angular deformation of 180 degrees and deformed state with angular deformation of 360 degrees respectively. While FIGS. 16 a , 16 b and 16 c illustrate the top view of the applicator 305 in its normal state, deformed state with an angular deformation of 180 degrees and deformed state with angular deformation of 360 degrees respectively.
As an exemplary embodiment of the invention, the applicator element 305 may comprise of bristles. FIGS. 17 a , 17 b and 17 c illustrate the isometric view of the applicator 405 in its normal state, deformed state with an angular deformation of 180 degrees and deformed state with angular deformation of 360 degrees respectively. FIGS. 18 a , 18 b and 18 c illustrate the front view of the applicator 405 in its normal state, deformed state with an angular deformation of 180 degrees and deformed state with angular deformation of 360 degrees respectively. While FIGS. 19 a , 19 b and 19 c illustrate the top view of the applicator 405 in its normal state, deformed state with an angular deformation of 180 degrees and deformed state with angular deformation of 360 degrees respectively.
The materials suitable for forming the receptacle 202 , 302 and the filament 213 could be polyprolpylene while the cap 203 , the casing 207 , the movable member 208 , the actuating means 303 a and the inner rod 307 could be formed of acrylonitrile butadiene styrene or any other suitable polymeric material. The material of applicator filament 215 , 306 could be any polymeric material as nylon or could be a suitable metal. The stem 204 , 304 may be formed of polyacetal or any other suitable polymeric material. The material for forming wiper 216 , 308 could be low-density polyethylene. The aforementioned materials for forming various parts of the device of the present invention are an example, however other suitable materials may also be used.
Depending upon the substance being used in the receptacle, a variety of sizes and shapes of the applicator can be utilized. The applicator 205 , 305 , 405 may be constructed of a porous or non-porous rubber, fabric mesh, felt material, foamed polymers, sponge material, Hydrel™, TPE or any other suitable material. Also, the applicator could have any suitable shape depending on the kind of application required. It could have a shape other than cylindrical such as ovular, tapered or any other suitable shape.
Although the above description and drawings show the device being cylindrical, the shapes and profile cross section thereof are not limited to the same.
These and further aspects which will be apparent to the expert of the art are attained by an adjustable applicator in accordance with the main claim.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. | An adjustable applicator employed for application of a cosmetic or a care product such as for application of mascara, coloring strands of hair, for dental flossing or for applying pharmaceuticals or cleaning agents is provided. In one embodiment, an adjustable applicator includes an applicator element having a bore, a filament wherein the filament is housed inside the bore of the applicator element and a clasping means wherein the applicator element angularly deforms when a force is applied on the clasping means such that the angular deformation occurs on the radial axis of the applicator element. Also disclosed is a device for packaging and dispensing a substance that includes an adjustable applicator. | 0 |
BACKGROUND
U.S. Pat. No. 3,581,733 describes a system for continuously monitoring blood pressure within blood vessels and the heart. The system includes a catheter joined to a connecting tube leading to a pressure transducer that converts physical pressure signals into an electrical impulse which is then fed to a recording machine, such as an oscilloscope. As pressure readings can be seriously affected if blood should coagulate in any part of the pressure monitoring system, this patent describes continuously forcing a very slow flow of a physiological salt solution (normal saline would be an example) into the patient. This very slow flow rate is sufficient to prevent blood from backing up into the catheter and connecting tube, but is so slow that it does not cause any significant error in blood pressure reading.
Immediately after connecting the system to the patient and periodically through pressure monitoring, it becomes necessary to flush a larger amount of parenteral liquid into the patient, particularly to insure that the catheter or needle is completely free of blood. U.S. Pat. No. 3,581,733 does this flushing by a valve 18. Another type flushing valve is described in Pat. No. 3,675,891. The set up of the valve of this latter patent is described in the attached instructions for the valve made under U.S. Pat. No. 3,675,891. This flushing valve has an elongated stem that must be pulled to actuate the valve. If the valve is not physically anchored to a rigid IV pole, transducer, etc., this operation requires two hands; i.e., one to hold the valve and one to pull the stem. Should the stem ever break off during the pulling action, the valve would be rendered useless. In addition, the valve of U.S. Pat. No. 3,675,891 includes a very large number of complicated parts including special sealing gaskets, etc.
SUMMARY OF THE INVENTION
The present invention overcomes the problems described above and provides a flushing valve with a restrictor in an elastically distortable tube. The resistor combines with the tube to form a slow flow rate passage and the tube is distortable, such as by squeezing, to temporarily form a flush passage with a much faster flow rate. An assembly method for the valve is described in which a pair of hollow connectors are joined to the elastically distortable tube and moved into abutting contact with the flow restrictor.
THE DRAWINGS
FIG. 1 is an elevational view of a blood pressure monitoring system which includes the medical flushing valve;
FIG. 2 is an enlarged view of the flushing valve;
FIG. 3 is a sectional view taken along line 3--3 of FIG. 2 showing the valve in its unsqueezed condition or it normal slow flow rate;
FIG. 4 is a view similar to FIG. 3, but showing the valve squeezed into its temporary fast flush condition;
FIG. 5 is an enlarged view, partially in section, taken along line 5--5 of FIG. 2;
FIG. 6 is an end view taken along line 6--6 of FIG. 5;
FIG. 7 is a perspective view of a hollow connector of the valve;
FIG. 8 is a sectional view taken along line 8--8 of FIG. 5;
FIG. 9 is a sectional view taken along line 9--9 of FIG. 5 showing the position of the tube during assembly; and
FIG. 10 is a sectional view similar to FIG. 9, but showing the position of the tube after assembly.
DETAILED DESCRIPTION
In FIG. 1, a sytem is shown for continuously monitoring blood pressure. This system has a hollow member 1, such as a needle or catheter, inserted into a patient's vein or artery. Usually blood pressure is continuously monitored from an artery because this gives a more accurate and dynamic reading of the heart function. Hydraulic pressure from the patient's artery is transmitted through a connecting tube 2 which can have ports or stopcocks, such as 3 and 4, for bleeding off blood samples or injecting medication into the patient. Tube 2 connects to a rigid T-connector 5 which is shown attached to a rigid arm 6 of a transducer pressure dome 7. It is understood that the term T-connector is used in its broad sense to also include an angled Y-connector. The transducer dome 7 includes a bleed valve 8 for use in eliminating all air from the system prior to use. It is important that no air bubbles be in the system because this can affect the hydraulic liquid pressure wave generated by the patient's heartbeat.
The pressure dome 7 of the transducer can include a diaphragm (not shown) which can respond to liquid pressure vibrations and engage electrical means inside a transducer body 9 to convert hydraulic liquid pressure surges into electrical impulses. Such electrical impulses are fed through a line 10 to an instrument 11 for reading the pressure fluctuations in a patient's cardiovascular system. Instrument 11 can be an oscilloscope, an electronically activated stylus, etc. If desired, the instrument 11 can have other monitoring functions, such as at 12 and 13, to monitor pulse rate, etc. in addition to blood pressure fluctuations at each heartbeat.
As explained above, the blood pressure monitoring for each heartbeat involves a liquid filled line between the patient and a diaphragm in the transducer dome. Since there is no liquid flow across the diaphragm of the transducer, there is no continuous blood flow out of the patient. This is why in U.S. Pat. No. 3,581,733 it is necessary to very slowly force a small volume of parenteral liquid, such as normal saline, into the patient to prevent blood from backing up into the catheter and connecting tube 2 where it could coagulate over an extended period of time. Coagulated blood portions in the system can materially affect the accuracy of a pressure monitoring because such coagulated blood forms a restriction in the hydraulic pressure system. This very slow infusion of parenteral liquid (such as at 3 cc/hour) into the patient is from a container 15 supported on a pole structure 16. Preferably, container 15 is of the collapsible bag type with a pressure cuff 17 that includes a squeeze bulb 18 and pressure gauge 19. The parenteral liquid flows from container 15 through a drip chamber 20 and a connecting tube 21 to a valve shown generally at 22 which is joined by flexible tube segment 23 to the rigid T-connector 5. Flow through connecting tube 21 can be controlled by conventional roller clamp 24.
The structure of the valve shown generally at 22 and the method of assembling this valve is the subject matter of the present invention. Related co-pending co-owned applications filed on the same day as the present application are "Method of Flushing A Medical Liquid," filed Apr. 24, 1979, Ser. No. 32,830; "System For Flushng A Medical Liquid," filed Apr. 24, 1979, Ser. No. 32,831; and "Protector Housing For Squeezable Valve" (Design), filed Apr. 24, 1979; Ser. No. 32,971.
In FIG. 2, the enlarged view of the valve illustrates a protector housing that includes a base 25 connected to ends 26 and 27, which in turn are connected to a top 28 that has a narrow central section 29. Within the protector housing is an elastically distortable squeeze tube of rubber-like material, such as silicone. Preferably, this squeeze tube 30 is generally transparent, or at least translucent to aid in detecting any air bubbles in the valve.
As shown in FIG. 3, the top wall has a longitudinal bracing rib 32 which extends through its longitudinal length to strengthen narrow portion 29 of the top. Bottom wall 25 has a limit lug such as cradle 33, with a concave surface, for preventing excess distortion of squeeze tube 30. Preferably, squeeze tube 30 has a generally triangular cross-sectional shape.
In FIG. 3, the valve is shown in its normal continuous slow flow rate position with the squeeze tube 30 sealingly engaging the periphery of a fixed size rigid glass flow restrictor 40 that has a bore 41 with a diameter of 0.001 to 0.004 inch. A diameter of 0.002 inch works very well and the restrictor can be made of glass tubing, such as is used for glass thermometers.
When it becomes necessary to fast flush the system of FIG. 1 with the parenteral liquid, the elastically distortable tube 30 is manually pinched through side openings of the protector housing. This causes the tube 30 to temporarily distort and create a flushing passage 42 around restrictor 40. When this is done, cradle 33 prevents undue flexure in the valve which might dislocate the restrictor. Release of the squeeze tube 30 causes it to immediately resume the FIG. 3 configuration and the predetermined slow flow rate resumed.
Perhaps the valve structure can best be understood by referring to the enlarged sectional view in FIG. 5. Here the housing's end wall 26 is integrally formed with a stationary hollow connector 45 which is joined to flexible tube segment 23. End wall 27 of the protector housing is joined to a tubular retainer 46 that has a bayonet type locking channel 47. This bayonet type lock can also be seen in FIG. 2. Fitting within tubular retainer 46 is a longitudinally movable hollow connector 48 which has a bayonet type lug 49 which engages slot 47 of retainer 46. Movable connector 48 has an internally tapered outer end and retaining ears 50 for connecting with connecting tube 21 leading from the parenteral liquid source.
As liquid is delivered from the pressurizied parenteral liquid source in the system shown in FIG. 1, it flows to the left as shown by the flow arrows in FIG. 5. The liquid enters a hollow filter assembly 51 that is inside connector 48. After the liquid exits through sides of the filter as shown by the arrow, it travels to the flow restrictor 40 and the pressure forces the liquid through the restricted passage 41. The elastic tube 30 tightly seals against the external periphery of glass tube 40 and prevents any other passage of liqud other than through restricted passage 41. To firmly hold ends of the tube 30 in place, compression shrink bands 52 and 53 can be used, if desired.
When it is desired to fast flush the system of FIG. 1, the elastically distortable tube 30 is laterally squeezed between thumb and forefinger causing an upper portion of tube 30 to lift off the periphery of glass tube 40 creating a flush passage. Thus, the liquid can flow through lateral passage 55 of connector 48, and go around restrictor 40 and enter the passage of connector 45 through its lateral passage 56.
It is important that air bubbles be eliminated from the system as they can interfere with the hydraulic pressure waves being transmitted from the patient to the transducer. For this reason, it is important that the hollow connectors 45 and 48 abuttingly engage ends of the restrictor 40 so no undue pockets are formed which could trap air bubbles. It has also been found that in cutting the glass flow restrictions 40, their length sometimes varies. To accept variable lengths of the restrictor 40, as well as eliminating any undue pockets to trap air bubbles, a special assembly method has been developed.
During assembly, the restrictor 40 is inserted into the squeeze tube and an end of tube 30 inserted on connector 45 which is fixedly joined to the protector housing. The squeeze tube has a configuration as shown in FIG. 8 at the area of assembly to connector 45. Next the right end portion of squeeze tube 30 is angularly twisted as shown in FIG. 9 and a tapered end of movable connector 48 inserted into a right end of tube 30. Lug 49 is then inserted into an entrance 60 of the bayonet type slot of the housing's retainer 46. Preferably, retainer 46 has diametrically opposed entrances 60 and 61 that are of different sizes which match with different sized lugs on diametrically opposed sides of connector 48. Thus, the connector 48 will always be oriented in the proper position so that its lateral port 55 is always at an upper part of the valve to correspond with the lateral port 56 of connector 45.
Once the connector 48 and tube 30 that has been temporarily twisted at one end with a torquing force have been assembled, lug 49 is tightened in the bayonet slot 47. The squeeze tube 30 also has a certain degree of elasticity that tends to untwist and tighten the connector 48. Thus, the bayonet type lock compressively urges the connectors 45 and 48 into compressive engagement with ends of the glass restrictor 40. If glass restrictor 40 varies slightly in length from one restrictor to the next, the bayonet structure can tolerate such variances. After the valve is assembled, the tube 30 resumes a shape generally shown at FIG. 10.
It has been found that the flushing valve of the present invention works very well when the flow restrictor is of glass, the squeeze tube is of silicone rubber, and the protective housing and hollow adapters are made of a rigid thermoplastic material.
In the above description, a specific example has been used to illustrate the invention. However, it is understood by those skilled in the art that certain modifications can be made to this example without departing from the spirit and scope of the invention. | A valve for an arterial monitoring set which continuously supplies a small flow of parenteral liquid, such as normal saline, into a patient's artery while arterial pressure is being continuously monitored. The valve has a flow restrictor providing a normally slow continuous flow rate and an elastically distortable tube which is manually squeezable to provide a fast flush rate. The valve is convenient for one hand operation. A method for assembling the valve by twisting the tube is also disclosed. | 0 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority from U.S. provisional application Ser. No. 60/191,464, filed Mar. 23, 2000.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH
This invention was made with Government support in the form of Grant No. USPHS 30206, from the United States Department of Health and Human Services, National Institutes of Health. The United States Government may have certain rights in this invention.
BACKGROUND OF THE INVENTION
1. Technical Field
The present invention relates to mutants of the tegument protein of human cytomegalovirus (CMV) known as CMVpp65. The mutants desirably do not exhibit the protein kinase activity which is associated with the native pp65 protein but retain its desirable immunologic target characteristics.
2. Description of the Background Art
The CMV genome is relatively large (about 235 k base pairs) and has the capacity to encode more than two hundred proteins. CMV is composed of a nuclear complex of double-stranded DNA surrounded by capsid proteins having structural or enzymatic functions, and an external glycopeptide- and glycolipid-containing membrane envelope. CMV is a member of the herpes virus family and has been associated with a number of clinical syndromes.
Human cytomegalovirus is not only a significant cause of morbidity in persons undergoing immunosuppressive therapy, but remains the major infectious cause of congenital malformations and mental retardation (26, 38, 53) (see the appended list of References for the identification of references cited throughout this specification). Although improved antiviral chemotherapy is becoming available for management of CMV infection, the large number of congenital infections (approximately 35,000 newborns per years in the U.S. (9)) underscores the need for an effective CMV vaccine (37), especially one which can be used safely in healthy persons. Attenuated and recombinant live virus vaccine approaches have been proposed, but safe use of these types of vaccines in healthy populations remains to be shown. Subunit vaccines are attractive because they have the potential to boost the immune system against certain viral proteins without risking viral infection or viral recombination.
CMV infection is widespread and persistent, and can become reactivated and clinically evident in the immunosuppressed patient. Because human cytomegalovirus is relatively common, yet is associated with extremely serious health conditions, a considerable effort has been made to study the biology of the virus with the aims of improving diagnosis of the disease as well as developing preventative and therapeutic strategies.
It would be highly desirable to deliver an effective vaccine derived from CMV that would impart immunity persons at risk of CMV disease such as a bone marrow transplant (BMT) recipient, a solid organ recipient, a heart patient, an AIDS patient or a woman of child-bearing years. No such vaccine presently is commercially available, however.
Cell-mediated immunity (CMI) plays an essential role in recovery from acute CMV infection and in the control of persistent CMV infection. The generation of cytotoxic T lymphocytes (CTL) is a most important factor in limiting CMV disease. Several proteins encoded by CMV are known to be recognized by the cellular immune system and elicit CTL. Borysiewicz et al. (2) first described the role of specific CMV proteins in CTL induction. The non-virion, immediate early proteins of CMV (CMV-IE), as well as the envelope glycoprotein, CMVgB, activate CTL function, however, the internal matrix proteins of the virus, CMVpp65 and CMVpp150, are more prevalent immune targets. CMVpp65 is the immunodominant protein: 70-90% of all CMV-specific CTL recognize this protein.
CMVpp65 is not essential for virus replication, therefore it may function to facilitate host cell changes important to virus spread. CMVpp65 has emerged as the primary target of CMV-specific CTL. Because it is a structural virus protein, it is available as an immune target immediately after infection, in the absence of virus replication. Thus, CMVpp65 is a preferred target for the cellular immune system.
CMVpp65 is known to interact with the cellular polo-like kinase-1 that is present at high levels during cellular mitosis (15). It contains redundant nuclear localization signals (17, 43) and becomes associated with nuclear lamina and condensed chromosomes during infection (8, 42). Thus, CMVpp65 clearly has nuclear and chromosomal trafficking ability that could represent an unknown risk if the protein were expressed in normal cells.
CMVpp65 also has been reported to have endogenous serine/threonine phosphotransferase activity (2, 3, 31, 32, 35, 41), however, it lacks several of the recognizable protein kinase (PK) consensus domains (21) (see FIG. 1 ). The kinase activity of CMVpp65 remains incompletely understood, but certain consensus sequences conserved threonine/serine/tyrosine PK catalytic domain are found within the 173 amino acid carboxy-terminal region of CMVpp65 (45). Only three subdomains align properly with these conserved residues of the catalytic domain (21) but two other subdomains are present. These CMVpp65 motifs consist of the catalytic subdomain I (amino acids 422-427; EXEXXE; SEQ. ID NO: 1), subdomain II (amino acid 436; K), and subdomain VIB (amino acids 543-545; RDL. See FIG. 1 . The sequences not in precise alignment are subdomain VIII (amino acids 463-465; APE, upstream from subdomain VIB and subdomain XI (carboxyl terminal amino acid 460; R).
PK activity plays an important role in the regulation of normal and transformed cell growth (7, 11, 25) and is important in viral regulation of cellular functions (29) and in regulation of virus transcription, DNA synthesis, and virion assembly (18, 36, 47, 51, 52). Because Protein kinases play an important role in the regulation of both normal and malignant cell growth (46), DNA vaccines (13, 34) that depend on the expression of intact CMVpp65 also could pose problems associated with introduction of PK activity into normal cells. The growth effects of increased kinase activity in healthy cells could limit the use of intact CMVpp65 as a vaccine, especially in children and women of child-bearing age. Therefore, new CMVpp65-derived sequences which could be used in DNA vaccines, yet which lack the undesired activities of the native protein would be highly useful.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagram illustrating the protein kinase (PK) domains of CMVpp65, with expression vectors. Putative PK domains (Roman numerals), peptide sequences (upper case letters with mutated amino acid in bold type) and nucleotide sequences (lower case letters) for the targeted amino acids in domains II and VIII are shown. The expression plasmids, made in pQE9 vector under the control of CMV promoter (CMVp), are shown for the native CMVpp65 (pQE9pp65n), for CMVpp65 with PK domain II mutation (pQE9pp65mII), for CMVpp65 with PK domain VIII mutation (pQE9pp65mVIII), for CMVpp65 with PK domains II and VIII mutations (pQE9pp65mII/VIII), and for CMVpp65 with carboxy-terminal truncation (pQE9pp65mTTH).
FIG. 2 provides a dot-blot protein kinase assay of CMVpp65 and its mutants immunoprecipitated from cell lysates of pQE9 transformed bacteria alone (upper row) or with MRC-5 cell lysates (lower row). CMVpp65mTTH and CMVpp150 were used as negative controls.
FIG. 3 is a western blot illustrating the expression of CMVpp65 and its mutants purified from cells transfected with the pQE9 expression system and probed with mAb 28-103.
FIG. 4 shows a 12.5% polyacrylamide gel of the indicated autophosphorylated recombinant proteins separated from phosphorylated casein.
FIG. 5 is a membrane blot containing phosphorylated products, probed with antibodies specific to phosphorylated serine and threonine residues.
FIG. 6 is a bar graph showing the results of a chromium release assay using human T lymphocyte clone 3.3F4 effector cells and HLA-matched or -mismatched target cells infected with recombinant vaccinia virus.
FIG. 7 is a schematic illustration of CMVpp65, pcDNAintpp65n, pcDNAintpp65mII and pcDNAint.
FIG. 8 presents data showing the percent specific 51 Cr release from peptide-loaded T2 cells by spleen cells from CMVpp65 immunized mice after one in vitro stimulations (8A), two in vitro stimulations (8B) and from HLA-mismatched target cells (8C).
FIG. 9 shows the same results as FIG. 8A except mice were immunized with a kinase-deficient CMVpp65 DNA vaccine.
FIG. 10 presents chromium release assay results showing the ability of a CTL clone to lyse the indicated different target cell lines, each loaded with a CMV peptide.
SUMMARY OF THE INVENTION
Accordingly, the present invention provides a cytomegalovirus pp65 protein which lacks protein kinase activity and which elicits a CTL response against cells infected with cytomegalovirus. Preferred embodiments of this protein contain the K436N mutation and in particular pcDNAintpp65mII. Further embodiments of the invention provide a DNA encoding such cytomegalovirus pp65 proteins.
The invention also provides vaccine compositions which comprise the cytomegalovirus pp65 proteins described above and the pharmaceutically acceptable carrier. Further embodiments of the invention provide a cellular vaccine composition which comprises antigen presenting cells that have been treated in vitro so as to present epitopes of a cytomegalovirus pp65 protein which lacks protein kinase activity and which elicits a CTL response against cells infected with cytomegalovirus and a pharmaceutically acceptable carrier. These DNA vaccines may further comprise an adjuvant. In addition, the invention provides a eukaryotic virus vector which comprises the DNAs described above.
The invention further provides a DNA vaccine composition which comprises a DNA which encodes a cytomegalovirus pp65 protein which lacks protein kinase activity and which elicits a CTL response against cells infected with cytomegalovirus and a pharmaceutical acceptable carrier.
The invention further provides a method of enhancing immunity to cytomegalovirus which comprises administering any of the vaccine compositions described above.
The invention further provides a diagnostic reagent for detecting the presence of active versus quiescent cytomegalovirus infections which comprises pp65mII transfected target antigen presenting cells.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention provides mutants of CMVpp65 which exhibit substantially no protein kinase activity but retain the immunological activity of the native sequence whereby they are capable of eliciting an antibody response and/or a CTL response against CMV in a suitable host. These mutants may differ in primary sequence from native CMVpp65 by one or more amino acid residues. One preferred embodiment comprises a mutant form of CMVpp65 that contains a point mutation that preserves native immunologically important epitopes but eliminates protein kinase activity.
The invention provides methods to augment the immune response of a host who is naive to CMV or to a patient latently infected with CMV and at risk for reactivation of CMV infection, wherein T cells are removed from a donor individual and treated in vitro with a mutant CMVpp65 DNA of the present invention that has been transfected into an HLA-matched antigen presenting cell. The resulting CMV-reactive CTL are infused into a recipient to provide protection from CMV disease.
The above methods also can be used to confer immunity against a CMV infection in a previously uninfected individual such as, for example, a woman of child-bearing years to prevent maternal-infant or maternal-fetus transmission of CMV. The methods can be used to vaccinate children to reduce the spread of CMV infection in, for example, day care centers. Vaccines may take any form known in the art, such as protein vaccines, DNA vaccines or recombinant live virus vaccines containing a DNA of this invention.
Adjuvants may form part of vaccine compositions. Any adjuvant known in the art which is suitable may be used. Examples include Freund's adjuvant, alum or any known adjuvant suitable for use with a protein vaccine. For in vivo use in humans, such adjuvants are not preferred. A DNA adjuvant may be used with a protein vaccine in humans, if desired. Genetic adjuvants may be used to enhance the effect of DNA immunization, for example genes encoding GM-CSF or IL-2. These genes may be inserted into the modified vector to enhance CTL activity. Carriers may be used with the vaccine compositions, including any pharmaceutically acceptable carrier known in the art. Exemplary carriers may include sterile water, saline solutions, liposomes or solutions containing cyclo-dextrin. Liposomes and cyclo-dextrin may be used to enhance uptake of the DNA by the antigen presenting cells.
Any suitable vector may be used in DNA vaccine compositions according to the invention. For example, pMG vector (Invitrogen) has been developed with two different promoters, one of which is the elongation factor 1α/HTLV hybrid. This is a strong promoter suitable for use with the DNA vaccines of this invention. The selection of hygromycin (bacteria) or Zeocin (mammalian) yields stable transfectants in two weeks.
The peptides of the mutant protein of the present invention may be administered to previously infected or uninfected patients, or in vitro to T cells, in the form of a protein vaccine or a polynucleotide (DNA-based) vaccine, or as a component of a recombinant viral vaccine. Suitable gene transfer vectors, such as a plasmid or an engineered viral vector that contains DNA encoding the CMVpp65 protein or a fragment thereof under the control of appropriate expression regulatory sequences may be administered to the patient or to T cells in culture for later administration to the patient. Therefore, the present invention provides a vaccinia, canarypox or other eukaryotic virus vector containing a DNA sequence encoding the immunologically active protein. The vector infects an antigen presenting cell which in turn presents antigen that will be recognized by CTL of patients having a latent (inactive) CMV infection.
A DNA vaccine permits direct and efficient expression of the protein of interest (pp65mII), that can be transfected easily in vitro or in vivo into an antigen presenting cell and trigger a cytotoxic T cell response. To accomplish this, a plasmid which has a promoter with high expression levels (e.g., the CMV IE promoter as used in pcDNAintpp65mII) is used. Preferably, the promoter also has an intron (e.g., intron A of the CMV IE gene as used in pcDNAintpp65mII) which stabilizes the expression of the DNA due to the presence of transcriptional enhancers. Finally, the preferred DNA vaccines have a polyadenylation termination sequence (e.g., bovine growth hormone poly A sequence as used in pcDNAintpp65mII). The vaccine sequence exemplified below (pcDNAintpp65mII) was derived from pcDNA3.1+ (Invitrogen), but for a safer vaccine, the ampicillin gene is preferably removed because it confers resistance to penicillin and is replaced with the kanamycin gene. In addition, the viral SV40 ori and pA preferably are removed to improve safety by diminishing the likelihood of integration into the host genome.
In regard to recombinant virus vectors, it is possible to use recombinant viruses that encode the CMV pp65mII gene to enhance the immunological response. Poxvirus recombinants such as recombinant vaccinia, modified vaccinia virus Ankara (MVA), and canarypox may be used for this type of recombinant viral vaccine production. Attenuated recombinant virus vaccine strains can be produced with multiple virus epitopes and with soluble cytokine factors that further augment the immune response. In vivo immunization of CMV seronegative subjects may be done with a DNAintpp65mII priming followed by a recombinant virus (e.g., vaccinia-pp65mII or MVApp65mII) boost to elicit specific CTL proliferation. The in vitro expansion of specific CTL may be done with matched-HLA stably transfected with pcDNAintpp65mII cell lines such as EBV-transformed B cells, such as LCL, and stimulators such as anti-CD3 antibody.
The invention also relates to diagnostic reagents for detection of the presence of active versus quiescent CMV infections. A human cell line, A293, stably transfected with pcDNAintpp65mII has been established and expresses the pp65mII protein. These cells can be used in a diagnostic assay to detect the presence of antibody to CMV in plasma and thus determine the CMV serology status by immunofluorescence or any suitable method. The specific CTL response can be assayed ex vivo using a cytokine-based assay, such as an IFN-γ elispot assay or FACS intracellular IFN-γ assay, whereby the T cells are stimulated in vitro for a period of time, with matched-HLA transfected/not transfected pp65mII LCL and the number of cytokine positive cells are determined. The IFN-γ positive CD8+ cells are CTL that have been stimulated by the expression of the mutant peptide expressed in the LCL; the IFN-γ positive CD4+ cells are the T helper CD4 cells that have been stimulated to induce a TH1 pathway and generate more CTL.
Because the native PK activity of CMVpp65 may be harmful if expressed in healthy cells, vaccine methods using CMVpp65 which lacks this potentially harmful activity were created. To reduce or eliminate the PK activity of CMVpp65, expression plasmids were constructed in the pQE9 vector using site-specific mutations within the CMVpp65 protein, including mutations within the putative PK domains II and VIII at amino-acid locations 436 and 465. In addition, a complete carboxy-terminal truncation was created in pQE9pp65mTTH that represented a deletion of all the putative PK domains of CMVpp65 (aa398-552). A plasmid containing CMVppl150 served as an additional negative control to check for background PK activity of the expression system. See FIG. 1 and Example 1. The plasmids containing mutated CMVpp65 were compared to plasmid pQE9pp65n, containing the native CMVpp65, for kinase activity and protein expression. The bacterial expression system used here allowed PK activity to be tested without possible contamination of mammalian cellular kinases. Other suitable plasmids are well known in the art. Other suitable plasmids are continuously being developed as better expression vectors for in gene therapy or vaccine research. The mutant pp65 gene may be inserted in any of these vectors as seems fit. Therefore, any suitable plasmid is contemplated for use with this invention.
The choice of CMVpp65 sequences to mutagenize was based on available sequences that conformed to the conserved catalytic subdomains of known threonine/serine PKs (Hanks 1991) and yet did not overlap with known CMVpp65-specific CTL epitopes. CMVpp65 contains the conserved PK subdomains I, II, VIB, VIII, and XI. CTL epitopes overlap in domains I and in various parts of the CMVpp65 carboxy terminal sequence (50). Therefore, only domains II and VIII were selected for modification. Subdomain II contains lysine 436 that corresponds to the invariant lysine present in several PKs that is known to interact with ATP analogs that inhibit PK (27). In addition, mutating the lysine in domain II suppresses the PK activity of other typical protein kinases, such as the insulin receptor, the EGF receptor, and viral proteins, such as P130 gag-fps of the Fujinami sarcoma virus and P37 mos the transforming gene product of Moloney murine leukemia virus (5, 23, 24, 49). Subdomain VIII, although out of sequence order compared to VI b, contains the triplet Ala-Pro-Glu that lies near the PK catalytic site and that has been linked to a nearby autophosphorylation site (22). Therefore, lysine 436 and glutamic acid 465 were selected for mutagenesis.
The expression products of the plasmids containing the mutated sequences were first tested for protein kinase activity by dot blot using the exogenous substrate, casein. As shown in FIG. 2 (upper row), the (native protein) CMVpp65n possesses intrinsic protein kinase activity, resulting in phosphorylation of the exogenous substrate casein. The mutant CMVpp65mII, containing the K436N mutation, showed no detectable kinase activity. The mutant CMVpp65mVIII showed approximately the same ability to phosphorylate casein as the native sequence, although there was a slight reduction in detectable phosphorylation. The combined mutant CMVpp65mII/VIII, with both K436N and E465K mutations demonstrated phosphorylation levels similar to the single mutant CMVpp65mII. The negative controls, CMVpp65mTTH and CMVpp150, showed the level of background casein phosphorylation in the assay.
The CMVp65mII mutant remained recognizable by a specific monoclonal antibody, as shown in western blot experiments. See FIG. 3 . In addition, the CMVpp65mII protein localized to the nucleus of infected cells, as indicated by monoclonal antibody staining (data not shown), suggesting that the mutation did not significantly affected the normal trafficking of this protein. However, because the humoral immune response to CMVpp65 is not considered the most important element in the immune response to infection to viruses, it was more important to determine the effect of this mutation on CTL recognition and activation (cellular immunity). Therefore, cells infected with vaccinia-CMVpp65mII were tested for recognition as targets by a CTL clone derived from natural human infection.
Cells expressing native sequence (CMVpp65n), the mutated sequence (CMVpp65mII), wild type vaccinia virus (no sequence) or an HLA-mismatched control cells expressing the mutated sequence were all tested by chromium release assay for lysis by a human CD8 + CTL clone specific for a CMVpp65 HLA A2 epitope. This CD8 + CTL clone, 3.3F4 described in (10) the disclosures of which are hereby incorporated by reference, was obtained from a healthy CMV-seropositive human volunteer who had mounted a successful immune response to CMV, and is specifically reactive to HLA autologous targets expressing native CMVpp65. Cytolytic function against cells expressing the mutant was similar to that directed toward the native CMVpp65.
The mutant CMVpp56 proteins therefore are demonstrated to retain the immunological characteristics shown to be important in immune function in the human response to CMV infection, particularly cell-mediated immunity. The in vitro chromium release assays discussed above are well-recognized in the art to successfully correspond to in vivo function of the same cells. Therefore, HLA specific recognition of cells expressing the native protein by the human T lymphocyte clone 3.3F4 clearly demonstrates an equivalent cell-mediated immune response which is predictive of in vivo recognition, activation and cytolysis.
Further, data show CTL activation by CMVpp65 in a well-accepted animal model used for prediction of human vaccine responses. The HLA-A2.1 transgenic mouse model is accepted for use where no animal model is available to study the immunologic responses to a particular human virus. See Vitiello et al., J. Exp. Med. 173:1007, 1991. The cytotoxic response in HLA-A2.1 transgenic mice is shown to recognize the same epitopes as the ones presented in, human cells in HCV (Wentworth et al., Int. Immunol., 1996), influenza (Man et al., Int. Immunol., 1995) or HIV (Ishioka et al., J. Immunol., 1999). The data therefore, clearly demonstrate the feasibility of this approach for modifying the immune systems of human patients to protect both healthy and immunocompromised persons from CMV disease.
The following examples are provided as illustrations of methods of the invention and are not intended to be limiting in any way.
EXAMPLES
Example 1
DNA Constructions and Generation of Recombinant Vaccinia Virus
The CMVpp65 gene, cloned into the BamHI and EcoRI restriction sites of pBluescript II KS DNA (35) was used to create the constructs. CMV nucleotide coordinates were used as published (4). Mutations of the CMVpp65 DNA were made using a Quikchange™ site-directed mutagenesis kit (Stratagene, San Diego, Calif.) using the following pairs of mutagenic primers developed using the published PK domain characteristics (22, 28). 5′ GCGGGCCGC AAC CGCAAATCAGCATCC 3′ and 5′ GGATGCTGATTTGC GGT TGCGGCCCGC 3′ (nt:1270-1296; SEQ. ID NOS:2 and 3) were used to mutate the indicated lysine into asparagine in the putative PK domain II (mII) of CMVpp65 (the K436N mutation). 5′ GAGTCCACCGTCGCGCCC AAA GAGGACACCGACGAG 3′ and 5′ CTCGTCGGTGTCCTC TTT GGGGGCGACGGTGGACTC 3′ (nt:1345-1377; SEQ ID NOS:4 and 5) were used to mutate the indicated glutamic acid into lysine in the putative PK domain VIII (mVIII) (the E465K mutation). The codon for the presumed functional amino acid K436 or E465 of CMVpp65 is shown underlined. Another mutant plasmid which contains both mII and MVIII (pp65mII/VIII) was also generated. The mutations were confirmed by DNA sequencing. A negative control lacking the putative CMVpp65 phosphokinase domain was created in pBluescript II KS (pp65mTTH) by digesting the CMVpp65 gene with Tth111I and NSiI (New England Biolabs, Beverly, Mass.) to delete the nucleotides which encode CMVpp65 (amino acids 398-552). Overhanging sequences were removed with mung bean nuclease (New England Biolabs, Beverly, Mass.) and the ends re-ligated using T4 DNA ligase (Life Technologies, Inc., Gaithersburg, Md.).
To express the proteins in a bacterial system, the CMVpp65 DNA was removed from pBluescript using Sal I—Bam HI digestion and inserted downstream from the CMV promoter in the pQE9 vector (Qiagen, Valencia, Calif.). The pQE9 CMVpp65 expression plasmid was used to transform E. coli strain M15, which contains the repressor pREP4 plasmid, and the proteins were expressed following the manufacturer's protocol (Qiagen, Valencia, Calif.).
The mTTH modification of CMVpp65 was created to establish a kinase-deficient CMVpp65 control by inserting the Tth111I and NSiI truncations into the pQE9 plasmid. As shown in FIG. 1, the plasmid containing the native CMVpp65 was designated pQE9pp65n, the K436N subdomain II mutant was pQE9pp65mII, the E465K subdomain VIII mutant was pQE9pp65mVIII, the combined K436N/E465K mutant was pQE9pp65mII/VIII, and the truncation control was pQE9pp65mTTH. pQE9 pp150 was used as a negative plasmid control. The CMVpp65 mutant sequences were subcloned into transfer vector pSC11 and then transfected using LIPOFECTAMINE (Life Technologies, Inc., Gaithersburg, Md.) into CV-1 cells that had been simultaneously infected with wild-type WR strain vaccinia virus using the method of Elroy-Stein and Moss (12). Recombinant virus was cloned and correct insertion was confirmed by PCR and DNA sequencing.
The efficiency of protein expression in the constructs was verified by western blot. The proteins were purified from cells transfected with the indicated pQE9 vector, separated using 12.5% SDS-PAGE, transferred to a nitrocellulose membrane and probed with mAb 28-103 specific for the detection of the pp65 protein (see Britt et al., J. Clin. Microbiol. 28:1229-1235, 1990), followed by ABC peroxidase staining using a VECTASTAIN ABC kit (Vector Laboratories, Inc., Burlingame, Calif.). All the proteins of the constructs bearing the intact carboxy-terminus of CMVpp65 were detected by the mAb, including the mutant CMVpp65. The level of expression was qualitatively similar in all constructs, suggesting that the mutations did not alter protein expression. In addition, mutation did not appear to significantly affect the immune recognition of the proteins.
Example 2
Immunoprecipitation of Recombinant CMVpp65
The CMVpp65 native and mutant proteins were expressed in the pQE9 bacterial system according to a Qiagen™ protocol. Cell pellets were extracted and subjected to immunoprecipitation as described by Michelson et al. (32) with modifications. Briefly, the bacterial pellets were frozen and thawed three times and incubated in lysis buffer (20 mM Tris/HCl pH 8.0, 300 mM NaCl, 10% glycerol, 2 mM EDTA, 0.5% Nonidet P-40) in the presence of protease inhibitor (5 μg/ml aprotinin and 5 μg/ml leupeptin) for 20 minutes at 4° C. The cell lysates were incubated with mouse IgG to remove non-specific proteins, sonicated and then clarified by centrifugation at 15,000×g for 5 minutes at 4° C. The CMVpp65 protein was immunoprecipitated with mAb28-103, specific for CMVpp65. Protein extract (200 μg) was mixed with 10 μl mAb28-103 unpurified ascites in 500 μl buffer A (10 mM Tris-HCl, pH 7.4, 150 mM NaCl, 2 mM EDTA, 1% NP-40, with 5 μg/ml aprotinin and 5 μg/ml leupeptin (32)) and incubated at 4° C. for 90 minutes with agitation. When relevant, 100 μg MRC-5 cell lysate in 1% SDS was added to the mixture to check whether cellular kinases co-immunoprecipitated with the CVMpp65 protein. The immune complex was captured with 100 μl 50% protein A-Sepharose 4 Fast Flow beads (Amersham Pharmacia Biotech, Piscataway, N.J.) co-incubated with the extract at 4° C. for 45 minutes and then washed three times by centrifugation with buffer A.
Example 3
Protein Kinase Assays
The immunoprecipitated native and mutant CMVpp65 proteins, still bound to the sepharose beads, were tested for protein kinase (PK) activity. pQE9pplS0 was also processed in the same way, as a negative control. Casein kinase II (Promega, Madison, Wis.) enzyme was used as a positive control. Dot blot PK assays were performed according to the methods of Glover and Allis (20). Briefly, 100 μl samples to be assayed were immobilized on a nitrocellulose membrane (Hybond ECL, Amersham Pharmacia Biotech, Piscataway, N.J.) by vacuum filtration using a commercial dot blot manifold (Minifold, Schleicher & Schuell, Inc.). Dephosphorylated bovine casein (Sigma Chemical Co, St Louis, Mo.) (100 μl 1 mg/ml) was added to each well as substrate, followed by incubation at room temperature for 30 minutes with 100 μl reaction mix (25 mM Tris pH 8.5, 100 mM NaCl, 10 mM MgCl 2 , 1 mM dithiothreitol, 0.1 μM [γ- 32 P]ATP). At the end of the incubation, free radioactive ATP was removed by washing the membrane 10 times in PBS at 37° C. followed by incubation at 37° C. in a shaking bath containing 100 ml stripping solution (4 M guanidine hydrochloride, 1% SDS, 0.1% Tween-20, 0.5% β-mercaptoethanol) for 30 minutes, with a final wash in distilled water. Incorporation of [ 32 P]-ATP into protein was visualized by autoradiography. See FIG. 2 . Mutant CMVpp65mII showed no kinase activity. To quantitate the amount of phosphokinase activity, serial dilutions of casein kinase II (Promega, Madison, Wis.) were assayed, and a standard curve was established using a PhosphorImager 445 SI (Molecular Dynamics, Sunnyvale, Calif.). The data were plotted and fitted to a linear curve from which CMVpp65-PK units were derived. One unit was defined as the amount of kinase needed to transfer 1 picomole of phosphate per minute at 37° C. using casein as substrate. Any values below 1.0 were considered negative.
Because native CMVpp65 undergoes autophosphorylation (3), the signals detected by PK assay using CMVpp65 are actually the combined results of both casein and CMVpp65 phosphorylation. To separate the two activities, a protein kinase assay was performed in solution according to the method described by Roby et al. (41) and then analyzed by SDS-PAGE. Immunoprecipitated recombinant proteins, including CMVpp65n, CMVpp65mII, CMVpp65mVIII, CMVpp65mII/VIII, CMVpp65TTH and CMVpp150, were used in protein kinase reactions in solution and then separated by 12.5% SDS-PAGE. Typically, 50 μl sample and 50 μl casein substrate (1 mg/ml) were added to 100 μl of a twofold-concentrated reaction mix as described above. The reaction was incubated at 37° C. for 30 minutes and terminated by adding 20 μl 100 μM EDTA, and then heated in boiling water for 3 minutes, releasing the CMVpp65 protein from the Sepharose beads, and sedimented at 15,000×g for 1 minute. The phosphorylated proteins were precipitated with 10% trichloroacetic acid, washed in acetone, and resuspended in loading buffer to be analyzed by 12.5% SDS-PAGE. Phosphorylation of the separated proteins on the gel was visualized by autoradiography using X-OMAT™ AR5 film (Kodak, Rochester, N.Y.).
Since the immunoprecipitation step may copurify other kinases from human-derived cells as well as the specific CMVpp65 protein (16), the bacterial lysate was mixed with 100 μg of MRC-5 cell lysate. The results are shown in FIG. 2 (lower row). No increase in phosphate signal was detected in any of the samples, including the negative controls. The CMVpp65mII remained negative, suggesting that it did not bind cellular kinases. To quantify the phosphokinase activities among the various mutants, with or without the addition of human-derived cell lysate, serial dilutions of casein kinase II were used to standardize the activity as units per assay (standardization data not shown).
The CKII positive control had 10 U PK activity, the CMVpp65n had 10.3 U, CMVpp65mVIII had 7.8 U, and CMVpp65mII, CMVpp65mII/VIII, CMVpp65mTTH and CMVppl150 had no activity. When the MRC-5 cell lysate was added to the reaction, CMVpp65n and CMVpp65mVIII had an activity equivalent to 10.4 U and 7.0 U respectively, whereas the other reactions remained negative. These results show that no detectable cellular kinases were coimmunoprecipitated from the system containing human-derived cell lysates using the mAb 28-103 to precipitate the CMVpp65 specific kinase.
The efficiency of the protein expression in the constructs was verified by western blot as shown in FIG. 3 . Proteins expressed from the constructs bearing the intact carboxy-terminus of CMVpp65 are shown in this western blot. The CMVpp65 mutations are detected by mAb 28-103. The level of expression appears to be similar in all constructs, suggesting that the mutations did not alter protein expression. To perform the blot, a 1 ml culture of bacterial cells containing the expressed proteins in pQE9 were lysed in 100 μl lysis buffer, sonicated on ice three times for 30 seconds and sedimented at 15,000×g for 5 minutes. The protein concentration of the supernatants was measured and 100 μg protein was subjected to 12.5% SDS-PAGE, transferred to a nitrocellulose membrane and incubated with mAb 28-103 followed by staining with peroxidase. See FIG. 3 .
As shown in FIG. 4, CMVpp65 and casein were phosphorylated by CMVpp65n and CMVpp65mVIII. CMVpp65mII, containing the substitution at K436N, showed not only complete loss of phosphorylation of casein but also absence of autophosphorylation. The same absence of autophosphorylation was observed with CMVpp65mII/VIII, as well as the negative controls CMVpp65mTTH and CMVpp150.
To further characterize which residues were phosphorylated, an SDS-PAGE membrane blot containing the phosphorylated products was incubated with specific monoclonal antibodies directed to the phosphorylated residues of serine and threonine. The PK assay was performed according to the same methods of the dot blot assay described above, except that unlabeled ATP (30 mM) was used in the sample reaction. Phosphorylation was detected by incubating the membrane with specific anti-phosphoserine or anti-phosphothreonine antibodies (2 μg/ml), (Sigma Chemical Co., St. Louis, Mo.) and revealed by immunoperoxidase staining using a VECTASTAIN ABC Kit (Vector Laboratories, Inc., Burlingame, Calif.) (40). The results (FIG. 5) showed that autophosphorylation (without casein as substrate) and casein phosphorylation were revealed using anti-phosphothreonine antibody only with the CMVpp65n and CMVpp65mVIII reactions, but not with CMVpp65mII and CMVpp65m II/VIII or with the negative control CMVpp65mTTH and CMVpp150. No serine phosphorylation was detected in any of the immunoprecipitated CMVpp65 protein (data not shown). See FIG. 5 .
Example 4
Chromium Release Assay
To investigate whether the mutation of the PK domains in CMVpp65 interferes with epitope presentation on a target cell surface for recognition by CTL, chromium release assays were performed. A human CD8+ CTL clone 3.3F4, with specificity for CMVpp65 HLA A2 epitope (10) was used as the effector in a chromium release assay using HLA-type (LCL-A2) matched or mismatched (LCL-A11) EBV-transformed B lymphocyte targets. All target cells were infected with vac-pp65n, vac-pp65mII or wild-type vaccinia virus (vac-wt) overnight at MOI=5, then incubated for four hours with 200 μCi 51 Cr (ICN Pharmaceuticals Inc., Costa Mesa, Calif.). The MHC-mismatched control LCL-All also was infected with vac-pp65mII. The cells were assayed using the methods of McLaughlin-Taylor et al. (30). Spontaneous release (without effector) and maximum release (lysed in 2% SDS) of radioactivity were determined for each target. Specific cytotoxicity was expressed as (effector cpm—spontaneous release cpm)/(maximum release cpm—spontaneous release cpm)×100.
As shown in FIG. 6, clone 3.3F4 recognized cells presenting the CMVpp65mlI epitope as efficiently as cells expressing the CMVpp65n (native) epitope. There was no significant difference in cytolytic effect at any of the various effector-to-target (E:T) ratios. This suggests that the point mutation of the invariant lysine K436N, which eliminates PK activity, does not negatively affect the HLA-restricted presentation of CMVpp65 CTL epitope.
Example 5
CMVpp65 DNA Immunization of Transgenic HLA A*0201 Mice
Transgenic HLA A#0201 mice were immunized with CMVpp65 DNA to test for CTL activity in response to the immunogen. The transgenic mice have been described previously by Benmohammed et al., Hum. Immunol. 61:764-778, 2000 and Vitiello et al., J. Exp. Med. 173:1007, 1991. The known CMV epitope, NLVPMVATV (SEQ ID NO:6; Peninsula Laboratories, Inc. San Carlos, Calif.; 95% pure) was used in a specific chromium release assay to demonstrate the efficacy of the DNA vaccine administered to the mice. The mice express human HLA antigens, therefore this mouse model permits the study of the immunologic response to human CMV as presented in the context of a normal human HLA molecule and to evaluate the protection a vaccine will elicit in humans. The specific epitope of SEQ ID NO: 6 is known to elicit human CD8+ T cell activity in HLA A*0201 CMV-seropositve individuals.
The CMVpp65 gene was inserted into the pBluescriptII KS+ vector and was modified as follows. The CMV intron A of the immediate-early gene (823bp) was inserted in front of the pp65 gene at the Spe1/BamH1 site using PCR with the following primers:
Forward: 5′ - GAATTCACTAGT GTAAGTACCGCC - 3′
(SEQ ID NO: 7).
EcoR1 Spe1
Reverse: 5′ - GACT GGATC CCTGCAGAAAAGACCC - 3′
(SEQ ID NO: 8).
BamH1
The intronA/CMVpp65 gene, still in pBluescript (see FIG. 7 ), was mutagenized as described in Example 1 using the Quickchange™ site-directed mutagenesis kit (Strategene, San Diego, Calif.). The intronA/CMVpp65 mutant II gene (pcDNAintpp65mII), the expression product of which exhibits no phosphokinase activity, was removed from pBluescript with the Spe1 and EcoR1 site of the pcDNA 3.1+ vector (Invitrogen, San Diego, Calif.). The control plasmids, including the intronA/CMVpp65 native (pcDNAintpp65n) and the intron A alone (pcDNAint), were inserted in the pcDNA3.1+ vector as well. All plasmids' DNA were transformed in DH5α competent cells, grown in terrific broth (Gibco-BRL Life technologies, Grand Island, N.Y.) and isolated using the Qiagen Maxi kit (Qiagen, Valencia, Calif.).
The intronA/CMVpp65n and intronA/CMVpp65mII DNA were removed from pBluescript, inserted into the pSC11 vector at the SpeI and KpnI site, and transfected into CV1 cells as described above in Example 1. The CV1 cells were simultaneously infected with WR strain vaccinia and the recombinant plasmid and were plaque purified three times to ensure clonality and purity. To titer the vaccinia virus in the ovaries, CV1 cells were plated at a density of 1.25×10 5 cells per well in a 24 well plate. The ovaries were collected, dissected free of fat tissue, weighed and frozen at −80° C. until ready for processing. They were homogenized with a TEFLON homogenizer on ice, sonicated three times for 30 seconds, resuspended in 100 μl of medium and diluted serially. An aliquot was added to the CV-1 cells, incubated overnight and stained with crystal violet the next day.
Transgenic HLA-A2.1 mice were constructed by microinjection of a chimeric molecule containing the α2 domains of the HLA-A*0201 gene and the α3 domain of murine H-2K b into fertilized eggs from C57Bl/6 mice as described previously (Hogan, et al., 1986. Manipulating the Mouse Embryo-Laboratory Manual Cold Spring Harbor Laboratory. Cold Spring Harbor, N.Y.; Vitiello et al., J. Exp. Med. 173:1007, 1991). The HLA-A*0201 expression was verified by FACS using mAb BB7.2, Parham et al., Hum. Immunol. 3:277-99, 1981; Benmohammed et al., Hum. Immunol. 61: 764-779, 2000, and by PCR according to a modified protocol described by Krausa et al., Tissue Antigens 45:223-231, 1995. The transgenic mice were called TgA2/K b for the chimeric MHC molecule.
Six to eight week old TgA2K b mice were inoculated intra-muscularly every 4 weeks with 50 μg Qiagen column purified DNA in 50 μl sterile PBS in each thigh. The mice were immunized with pcDNAintpp65n, pcDNAintpp65mII and pcDNAint as control plasmid. The spleens were collected 4 weeks after the last immunization. When applicable, the mice were challenged on day 7 after the last inoculation, IP, with 5×10 6 pfu of recombinant vaccinia expressing pp65n and the ovaries were collected 5 days later to titer vaccinia. The spleens were collected as well to check for the presence of specific CMVpp65 CTL.
Blood samples were collected prior to each injection during the immunization process and the sera isolated and frozen at −20° C. The sera were diluted at 1/50 and 1/100 and incubated with MRC-5 cells previously infected with Toledo CMV strain for 3 days. The presence of the pp65 protein was revealed with a biotinylated antimouse IgG and immunoperoxidase labeling (Vector Laboratories, Inc., Burlingame, Calif.). When the sera were positive for pp65 Ab, they were subjected to an ELISA for quantitation.
Example 6
Detection of Specific CTL Activation Elicited by CMVpp65 DNA Vaccine
Three days before the harvest of effector cells from immunized TgA2Kb mice, blasts cells were prepared from syngeneic spleen cells (1 spleen for 3 immunized mice) and cultured at a concentration of 1×10 6 cells/ml in complete RPMI (10% heat-inactivated FBS, 50 units/ml Pen/Strep, 10 mM Hepes, 2 mM L-glutamine, 5× −5 M β-mercaptoethanol,) and stimulated with 25 μg/ml LPS (Sigma, St Louis, Mo.) and 7 μg/ml dextran sulfate (Sigma, St Louis, Mo.). The cells were subjected to in vitro stimulation (IVS) as follows. Stimulated blast cells (targets), resuspended at a concentration of 25×10 6 cells/0.2 ml serum-free RPMI with 100 μM CMVpp65peptide 495 (SEQ ID NO:6) and 3 μg/ml of β2-microglobulin, were incubated at 37° C. for 4 hours with regular mixing to load the targets with peptide. The cells then were irradiated at 3000 RADS using a Isomedix Model 19 Gammator (Nuclear Canada, Parsippany, N.J.) and plated in a 24 well plate (1×10 6 blasts per well) in complete RPMI supplemented with 10% rat T-stim culture supplement (Becton-Dickinson, Franklin Lakes, N.J.). Each well also contained 3×10 6 immunized spleen cells. A second IVS procedure was done 7 days later using the same protocol.
T2 cells (ATCC CRL-1992), LCL-A2 cells (human EBV transformed cell), EL4A2 cells (mouse H-2b cell stably transfected with the A2 gene) presenting the HLA-A*0201 allele and LCL-A3 cells (control HLA cell line) were used as targets. For chromium release assay (HLA-specific, antigen-specific cytolysis assay), the target cells were incubated with 200 μCi 51 Cr with or without peptide (100 μM) and β2-microglobulin (3 μg/ml) for 1 hour at 37° C. They were washed and mixed at a effector:target (E/T) ratio of 100:1 to 10:1 in a 96-well bottom plate with effector cells (immunized spleen cells). The effectors and targets were co-incubated for 4 hours and an aliquot was counted using a Topcount TM counter (Packard Instrument Co, Downers Grove, Ill.). Specific CTL clones (e.g. 19M3) were maintained in culture by weekly stimulation with peptide loaded blasts in complete RPMI with 10% rat stim or 20 units/ml of rhIL-2.
Four mice were immunized with pcDNAintpp65n and two mice with pcDNAint (controls). One out of four mice generated specific CTL which recognized and lysed peptide pp65 495 loaded T2 cells after one in vitro stimulation (20% lysis), and two after a second in vitro stimulation (39% and 44% lysis). The effector cells from mice immunized with control DNA did not lyse the target cells, showing that the assay was specific. The other control HLA-mismatch LCLA3 target cells were not lysed by either responsive CTL cells M2 and M4. The results show that construct, pcDNAintpp65n, which expresses the native gene of CMVpp65, elicits CTL activity in the transgenic mouse model. More importantly, the CTL generated specifically recognize the minimal cytotoxic epitope of pp65 for the HLA A*0201, NLVPMVATV (SEQ. ID NO:6), presented by the human cell line T2. See FIG. 8 for results.
Example 7
Kinase Deficient CMVpp65 DNA Vaccine Elicits Specific Cellular Immunity
The methods of Example 6 were repeated, except that the mice were vaccinated with pcDNApp65mII gene inserted in the same mammalian expression vector as pcDNApp65n. Two out of 3 mice responded to pcDNApp65mII DNA immunization with almost 90% specific lysis of the target T2 cell loaded with the epitope of SEQ ID NO:6. See FIG. 9 . The mutated CMV protein therefore is at least equivalent to the native sequence in its ability to elicit a CTL response.
Example 8
A CTL Clone Generated from Mutant CMVpp65 Immunization Specifically Recognizes only HLA Compatible Targets
A CTL clone (19M3) generated by the mutant pp65 immunization and weekly stimulation with SEQ ID NO:6 loaded blasts was grown in culture and used to lyse the following target cell lines: T2, LCLA2, EL4A2 and LCLA3 (HLA mismatch). Only the HLA A*0201 expressing cells were lysed. See FIG. 10 . These results demonstrate that the mutant CMVpp65 protein elicits specific CTL activity and performs the functions necessary for successful vaccination.
Two CTL clones were not able to lyse HCMV-infected fibroblasts, however fibroblasts infected with the Towne strain of CMV at an MOI of 5 were lysed at 30% and peptide loaded T2 cells at 85% by the CTL clones. See FIG. 10 and Table I. The serum from immunized mice were tested for specific antibody response to the pp65 protein by immunohistochemistry on CMV-infected MRC-5 cells (infected for 3 days at MOI:02). The mice in each immunization group, pp65n or pp65mII, which developed cytolytic activity to the pp65 protein, responded with antibody production.
Example 9
Elispot Assay for CMV Diagnosis
Sterile microtiter plates are coated with 100 μl per well rat anti-mouse IFN-γ (2 μg/ml) in 50 mM sterile filtered carbonate buffer, pH 9.6 (21 μl/10.5 ml) with overnight incubation. The plates then are washed twice with RPMIc and blocked for 1-3 hours. The medium is replaced and 2× or 3× serial dilutions of effector cells (from 1×10 6 to 1.25×10 5 in 100 μl) irradiated feeder/target cells (2.5×10 5 cells plus/minus peptide or transfected with pp65mII in 50 μl or 5×10 6 c/ml). Stimulation factors (conA, peptides, pp65) are added, plus rat stim. Cell lines such as T2 (loaded or not loaded with peptides) also may be used. After 8-24 hours incubation, the plate is washed with DIH 2 O cycle P03M8 to remove the cells, then with 1× PBS plus 0.05% Tween-20 (PBST) with cycle P03M8 and blotted. Biotinylated anti-IFN-γ (100 μl/well; 1.25 μg/ml in PBST; Pharmingen, San Diego) was incubated in the wells overnight at 4° C. The bound antibody is detected with an alkaline phosphatase streptavidin according to known methods.
TABLE I
Cytolytic Response to CMVpp65 DNA Immunization with a Vaccinia Challenge (recvacpp65n).
Response after
Response after
Ex vivo
One In Vitro
Two In Vitro
Response
Stimulation
Stimulations
Vaccinia Titer
E/T Ratio
10
30
100
10
30
100
10
100
100
per Ovary
DNApp65mII
M2
1.8
4
9.2
7.8
15.2
45.6
ND
ND
ND
3.4 × 10 4
M4
1.5
1.6
4.4
0.2
8.3
16.7
ND
ND
ND
3.9 × 10 4
M4(2)
1.1
0.3
3.4
3.97
1.81
13.24
22
51.2
81.7
5
M3
−1.3
−3.7
−3.4
0.2
−2.2
−1.1
ND
ND
ND
9.5 × 10 4
M3(2)
1.9
0.3
0.4
−3.9
3.31
0.12
1.3
8.9
24
4 × 10 6
M1
−2.1
−1.3
2.9
−1.8
−0.6
1.9
ND
ND
ND
1.25 × 10 5
DNApp65n
M3
−1.4
0.2
−2.7
2.3
2.83
18.17
8.49
12.17
28.09
2.75 × 10 4
M1
3.2
0
4.3
−0.7
−1.43
−2.2
−2.63
0.59
5.92
6 × 10 4
M2
−3
−1.1
1.2
−1.6
0.47
−4.9
5.46
6.38
3.55
1.4 × 10 5
M4
−2.2
−2.4
−2.6
0.24
−3.2
−2.6
0.59
−1.97
0.53
5
pcDNAint
C1
−0.6
−1
1.9
−2.7
−4.14
−2.35
−6.12
−2.57
−1.78
2 × 10 4
C2
−1.2
−0.7
−1.7
−2.02
−0.45
−0.33
1.64
2.96
12.11
2.3 × 10 4
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12
1
6
PRT
Human cytomegalovirus
MISC_FEATURE
(2)..(2)
Xaa = any amino acid
1
Glu Xaa Glu Xaa Xaa Glu
1 5
2
27
DNA
Artificial Sequence
mutagenic primer for CMVpp65
2
gcgggccgca accgcaaatc agcatcc 27
3
27
DNA
Artificial Sequence
mutagenic primer for CMVpp65
3
ggatgctgat ttgcggttgc ggcccgc 27
4
36
DNA
Artificial Sequence
mutagenic primer for CMVpp65
4
gagtccaccg tcgcgcccaa agaggacacc gacgag 36
5
36
DNA
Artificial Sequence
mutagenic primer for CMVpp65
5
ctcgtcggtg tcctctttgg gggcgacggt ggactc 36
6
9
PRT
Human cytomegalovirus
6
Asn Leu Val Pro Met Val Ala Thr Val
1 5
7
24
DNA
Artificial Sequence
PCR primer for CMVpp65
7
gaattcacta gtgtaagtac cgcc 24
8
25
DNA
Artificial Sequence
PCR primer for CMVpp65
8
gactggatcc ctgcagaaaa gaccc 25
9
7
PRT
Human cytomegalovirus
9
Ala Gly Arg Lys Arg Lys Ser
1 5
10
19
PRT
Human cytomegalovirus
10
Ala Pro Glu Glu Asp Thr Asp Glu Asp Ser Asp Asn Glu Ile His Asn
1 5 10 15
Pro Ala Val
11
7
PRT
Artificial Sequence
Mutated PK domain II of CMVpp65
11
Ala Gly Arg Asn Arg Lys Ser
1 5
12
19
PRT
Artificial Sequence
Mutated PK domain VIII of CMVpp65
12
Ala Pro Lys Glu Asp Thr Asp Glu Asp Ser Asp Asn Glu Ile His Asn
1 5 10 15
Pro Ala Val | This invention relates to mutated CMVpp65, a viral structural protein which activates cell mediated immunity in humans infected with CMV. The mutations remove undesirable protein kinase activity naturally present in the protein and make it suitable for the production of both DNA and protein vaccines. Therefore, the invention provides proteins and DNAs, as well as vaccines comprising the proteins and DNAs, including cellular vaccines and vectors. Other embodiments of the invention relate to methods of enhancing immune response and vaccinating against CMV, including gene therapy methods and vectors. | 2 |
[0001] Pursuant to 35 U.S.C. §119, the benefit of priority from provisional applications 60/936,015 and 60/975,540, with filing dates of Jun. 1, 2007 and Sep. 27, 2007 respectively, is claimed for this non-provisional application.
ORIGIN OF THE INVENTION
[0002] This invention was made in part by employees of the United States Government and may be manufactured and used by or for the Government of the United States of America for governmental purposes without the payment of any royalties thereon or therefor.
BACKGROUND OF THE INVENTION
[0003] 1. Field of the Invention
[0004] This invention relates to electrospinning. More specifically, the invention is a method and system for aligning fibers for the controlled placement thereof during an electrospinning process using an elliptical electric field to guide fiber deposition.
[0005] 2. Description of the Related Art
[0006] Electrospinning is a polymer manufacturing process that has been revived over the past decade in order to produce micro and nano fibers as well as resulting fiber groups (or mats as they are known) with properties that can be tailored to specific applications by controlling fiber diameter and mat porosity. The individual fibers are formed by applying a high electrostatic field to a polymer solution that carries a charge sufficient to attract the solution to a grounded source. Parameters that determine fiber formation include solution viscosity, polymer/solvent interaction, surface tension, applied voltage, distance between the spinneret and collector, and the conductivity of the solution.
[0007] Typically, only non-woven mats can be produced during this process due to splaying of the fibers and jet instability of the polymer expelled from the spinneret. These non-woven mats can be used as scaffolds for tissue engineering, wound dressings, clothing, filters, and membranes. While non-woven mats have proven to be useful for a variety of applications, controlling fiber alignment in the mat is a desirable characteristic to expand the applications of electrospun materials. Particularly for the case of tissue engineering scaffolds, the control of fiber distribution, fiber alignment, and porosity of the scaffold are crucial for the success of any scaffold. Current manufacturing techniques are limited by erratic polymer whipping that often produces dense nanofiber mats, which cannot support cell infiltration or cell alignment.
SUMMARY OF THE INVENTION
[0008] Accordingly, it is an object of the present invention to provide a method and system for aligning fibers produced during an electrospinning process.
[0009] Another object of the present invention is to provide a method and system for controlling fiber alignment and/or fiber placement during fiber deposition on a collector by means of electrospinning.
[0010] Other objects and advantages of the present invention will become more obvious hereinafter in the specification and drawings.
[0011] In accordance with the present invention, a method and system are provided for aligning fibers in an electrospinning process. A jet of a fiberizable material is directed towards an uncharged collector from a dispensing location (e.g., an electrically charged spinneret) that is spaced apart from the collector. While the fiberizable material is directed towards the collector, an elliptical electric field is generated via the electrically charged dispenser and an oppositely-charged control location. The term “elliptical” as used herein includes elliptical and all dipole field-like shapes, including both symmetric and unsymmetric, and including both spherical and ovoid. The field is generated such that it (i) spans between the dispensing location and the control location comprising an oppositely-charged electrode that is within line-of-sight of the dispensing location, and (ii) impinges upon at least a portion of the collector.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1 is a schematic view of a system for producing aligned electrospun fibers in accordance with an embodiment of the present invention;
[0013] FIG. 2 is a view of a portion of the system in FIG. 1 illustrating position for the fiberizable material dispenser and the electrode in accordance with an embodiment of the present invention; and
[0014] FIG. 3 is a schematic view of a system for producing aligned electrospun fibers in accordance with another embodiment of the present invention.
[0015] FIGS. 4A and 4B illustrate example fiber distributions in accordance with an embodiment of the present invention.
[0016] FIG. 5 illustrates an example set-up for dual dispensing and control locations in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0017] Referring now to the drawings and more particularly to FIG. 1 , an electrospinning system for fabricating a mat of aligned fibers in accordance with the present invention is shown and is referenced generally by numeral 10 . For simplicity of discussion, system 10 will be described for its use in producing a single-ply mat with aligned single fibers or fiber bundles that are substantially parallel to one another. However, as will be explained further below, the present invention can also be used to produce a multiple-ply mat where fiber orientation between adjacent plies is different to thereby create a porous multi-ply mat. Such multi-ply porous mats could be used in a variety of industries/applications without departing from the scope of the present invention as would be understood by one of ordinary skill in the art.
[0018] In general, system 10 includes a dispenser 12 capable of discharging a fiberizable material 14 therefrom in jet stream form (as indicated by arrow 14 A) that will be deposited as a single fiber or fiber bundles (not shown) on a collector 16 . Dispenser 12 is typically a spinneret through which fiberizable material 14 is pumped as is well known in the art of electrospinning. The type and construction of dispenser 12 will dictate whether a single fiber or fiber bundles are deposited on collector 16 . Fiberizable material 14 is any viscous solution that will form a fiber after being discharged from dispenser 12 and deposited on collector 16 . Typically, material 14 includes a polymeric material and can include disparate material fillers mixed therein to give the resulting fiber desired properties. Examples of suitable fillers are ceramic particles, metal particles, nanotubes and nanoparticles. Suitable collectors 16 include a static plate, a wire mesh, a moving-conveyor-type collector, or a rotating drum/mandrel fabricated in a variety of shapes and configurations, the choice of which is not a limitation of the present invention. For the illustrated example, collector 16 will be rotated about its longitudinal axis 16 A as indicated by rotational arrow 16 B. In the present invention, collector 16 is maintained in an electrical uncharged state (e.g., floating or coupled to an electric ground potential 18 as illustrated). The fiber deposition surface of collector 16 can be electrically conductive (e.g., copper or aluminum), semi-conductive, or non-conductive without departing from the scope of the present invention.
[0019] Dispenser 12 is positioned such that its dispensing aperture 12 A faces collector 16 a short distance therefrom as would be understood in the electrospinning art. For example, if dispenser 12 is a spinneret, aperture 12 A represents the exit opening of the spinneret. In the present invention, the portion of dispenser 12 defining aperture 12 A should be electrically conductive. A voltage source 20 is coupled to dispenser 12 such that an electric charge is generated at the portion of dispenser 12 defining aperture 12 A.
[0020] Positioned near collector 16 and within the line-of-sight of aperture 12 A is an electrode 22 . More specifically, a tip 22 A of electrode 22 is positioned within line-of-sight of aperture 12 A as is readily seen in FIG. 2 where dashed line 24 indicates the line-of-sight communication between aperture 12 A and electrode tip 22 A. A voltage source 26 is coupled to electrode 22 such that an electric charge is generated at electrode tip 22 A. The charge is opposite in polarity to that of the charge on the portion of dispenser 12 defining aperture 12 A. That is, if the charge is positive at aperture 12 A (as indicated), the charge should be negative at electrode tip 22 A (as illustrated). Similarly, if the charge is negative at aperture 12 A, the charge should be positive at electrode tip 22 A. The magnitude of the voltages applied to dispenser 12 and electrode 22 can be the same or different without departing from the scope of the present invention.
[0021] The opposite-polarity charges at dispenser aperture 12 A and electrode tip 22 A cause an electric field of controllable geometry and magnitude to be generated therebetween as represented by dashed lines 30 . In general, if the geometric shape of dispenser 12 at aperture 12 A and electrode tip 22 A are substantially the same, electric field 30 will be spherical and uniform. Typically, aperture 12 A and electrode tip 22 A will be circular, and they can be the same or different in terms of their size. Since aperture 12 A and electrode tip 22 A are in line-of-sight of one another, some portion of electric field 30 will impinge upon the surface of collector 16 . This will be true whether electrode tip 22 A is positioned centrally with respect to collector 16 (as illustrated), or at any position along collector 16 . The magnitude of the electric field is determined by the voltages 20 and 26 .
[0022] In operation, dispenser 12 and electrode 22 are positioned with respect to collector 16 as described above. Opposite-polarity voltages are applied to dispenser 12 and electrode 22 in order to establish electric field 30 with at least a portion of collector 16 being disposed in electric field 30 . Fiberizable material 14 is pumped from dispenser 12 such that a jet stream 14 A thereof is subject to electric field 30 . A pulsed electric field, generated for example by pulsing the voltages applied to dispenser 12 and electrode 22 , may also be used.
[0023] By judicious placement of dispenser 12 and electrode 22 , the orientation of the field lines of electric field 30 can be predetermined for a particular application. For example, FIG. 3 illustrates an electrode 22 placement that will cause the electric field lines of field 30 and, therefore fiber orientation, to be angled with respect to longitudinal axis 16 A of collector 16 . While FIG. 2 and FIG. 3 illustrate two different orientations, other orientations of the dispenser 12 , collector 16 , and electrode 22 can be used so long as an elliptical electric field is generated.
[0024] The advantages of the present invention are numerous. The electrospinning process has been improved to provide for the fabrication of aligned-fiber mats. The generation of an elliptical electric field and placement of an uncharged collector therein will align fibers as they are deposited on the collector. A broad range of fiber diameters can be produced by modifying the viscosity of the fiberizable material 14 . In tests of the present invention, polymer fibers in the order of 10 μm in diameter were deposited with uniform spacing ranging between 25-30 μm. In other tests, nano-sized polymer fibers on the order of 500 nm to 1 μm in diameter were deposited with uniform spacing ranging between 7-10 μm. Thus, the present invention will provide for predictability in fiber alignment and spacing so that fiber mats can be designed for use in a variety of industries/applications.
[0025] The present invention is further illustrated by the following examples.
Example 1
[0026] A 10 wt % polymer solution was prepared by dissolving colorless polyimide CP2 [(2,2-bis(3-aminophenyl) hexafluoropropane+1,3-bis(3-aminophenoxy)benzene)] ([η]=1.2 dL/g) in chloroform. CP2 was electrospun using a 10 mL syringe fitted with an 18 gauge blunt end needle. A syringe pump was used to deliver a constant flow rate of 2 ml/hr. A rotating collector (approximately 2400 rpm) was positioned 5-20 cm from the tip of the needle. The collector was grounded and a Kapton® film was placed around the barrel of the collector to create an insulative surface. An alligator clip was used to attach a high voltage power supply to the needle to distribute a positive voltage to the polymer solution. An electrode (stainless steel needle) was positioned at an angle 90° directly above the top of the rotating collector using a plexi-glass mounting bracket. An alligator clip was used to attach the high voltage power supply to the electrode to generate a negative voltage equal and opposite to the positive voltage. Mat images were obtained using a Kodak® 14N camera fitted with a 105 mm Nikon® macro lens. The equipotential lines and field strengths were modeled using Matlab® software.
[0027] Several experimental trials were performed in order to determine the effect of the electric field on fiber orientation and distribution. For each trial, CP2 was collected for a period of approximately one second at four different distances; 5 cm, 10 cm, 15 cm and 20 cm with applied voltages of +/−5 kV, +/−10 kV, +/−15 kV and +/−20 kV at each distance. This was accomplished by pulsing the power supplies on and off in an attempt to create a single rotational uptake of fibers. This technique allowed the examination of fiber orientation and overall mat width; however, exact fiber distribution was not determined due to the inability to collect precisely one uptake of the fibers, hence, only a general assessment of fiber distribution could be ascertained from the data. The fiber density decreased with increasing distance and decreasing field strength. The relationship appeared to be fairly linear with the total fiber mat widths being approximately 0.5 cm, 0.6 cm, 0.8 cm and 1.0 cm for collection distances of 5 cm, 10 cm, 15 cm and 20 cm, respectively, at +/−10 kV. The fiber diameter and morphology were not significantly affected as the field strength varied.
Example 2
[0028] CP2 ([η]=1.2 dL/g) was dissolved in chloroform (10 wt %) at room temperature and allowed to stir for a minimum of 2 hours prior to use. Polyglycolic acid (PGA) was dissolved in hexafluoroisopropanol (HFIP) under low heat and allowed to stir overnight until all particles were dissolved.
[0029] CP2 was electrospun using a 10 mL syringe and an 18 gauge blunt end needle. A constant flow rate of 2 ml/hr was obtained using a syringe pump. A rotating collector (approximately 2400 rpm) was positioned 13-17 cm from the tip of the needle. The collector was grounded and Kapton® polymer film was placed around the barrel of the collector to create an insulative surface. An alligator clip was used to attach the high voltage power supply to the needle to distribute a positive voltage of 10 kV to the polymer solution. PGA was electrospun using a 10 mL syringe and a 22 gauge blunt end needle at a constant flow rate of 1.5 ml/hr. The rotating collector was positioned 10-17 cm from the tip of the needle and a positive voltage of 15 kV was applied to the polymer solution. For each polymer, an auxiliary electrode (stainless steel needle) was positioned at an angle 90° directly above the top of the rotating collector using a plexi-glass mounting bracket. An alligator clip was used to attach the high voltage power supply to the auxiliary electrode to generate a negative voltage equal and opposite to the positive voltage.
[0030] Fibers and mats were coated with 4-8 nm of Au/Pd using a sputter coater. Images were obtained using a scanning electron microscope and a high resolution scanning electron microscope. Image processing and analysis of fiber diameter and degree of alignment were performed.
[0031] High speed videos were captured at 2000 frames/sec and data was processed and post-processed. High speed video imaging was used to capture the fiber from jet initiation through collection on the rotating mandrel. Jet exit images illustrated the stability of the fiber as it overcame surface tension and was drawn into the electric field. The fiber continued along the field line path and was pulled straight to the rotating mandrel. Jet whipping and bending instability that are typical characteristics of electrospinning were not observed. The fiber continued to follow the straight electric field path after a period of 5 minutes. In order to verify the influence of the control electrode on controlling fiber placement and alignment, the location of the control electrode was repositioned to a location offset from the spinneret. The fiber was directed to the rotating mandrel only at the location of the control electrode.
[0032] In order to determine the effect of the electric field on the fiber alignment and distribution over time, each polymer was collected for a period of 30 seconds. Fibers that were electrospun from CP2 were on the order of 10 μm in diameter. The spacing between fibers was fairly uniform and ranged from approximately 25-30 μm. Nanofibers were observed for the PGA polymer. The PGA fibers were approximately 500 nm-1 μm in diameter with spacing between fibers in the range of 7-10 μm.
[0033] Pseudo-woven mats were generated by electrospinning multiple layers in a 0°/90° lay-up. This was achieved by electrospinning the first layer onto a Kapton® film attached to the collector, removing the polymer film, rotating it 90°, reattaching it to the collector and electrospinning the second layer on top of the first, resulting in the second layer lying 90° relative to the first layer. Fibers were collected for one minute in each direction. A high degree of alignment was observed in this configuration. In order to assess the quality of a thicker pseudo-woven mat, the lay-up procedure was repeated 15 times in each direction (0°/90°) for a period of 30-60 seconds for each orientation, generating a total of 30 layers. The average fiber diameter for the CP2 pseudo-woven mat was 9.9±3.3 μm and the PGA mat had an average fiber diameter of 0.91±0.4 μm. The distribution in fiber diameter is illustrated in FIGS. 4A (PGA (average 0.91±0.4 μm)) and 4 B (CP2 (average 9.9±3.3 μm)). PGA exhibited a much narrower Gaussian fiber diameter distribution while the CP2 polymer had a much broader range of fiber diameters. The degree of alignment was determined for each material by measuring the angle of the long axis of the fiber relative to the plane of the collector at deposition for each 0°/90° orientation. The data obtained for both polymers indicated excellent alignment with CP2 having an average degree of alignment of 89.7°±1.7° and PGA with 89.5°±4.8°.
EXAMPLE 3
[0034] CP2 was electrospun using two 10 mL syringes and 18 gauge blunt end needles 50 and 52 using the set-up generally illustrated in FIG. 5 . A constant flow rate of 2 ml/hr at each syringe was obtained using a dual syringe pump. A rotating collector 54 (approximately 2400 rpm) was positioned 13-17 cm from the tip of the needles. The collector was grounded and Mylar® film was placed around the barrel of the collector to create an insulative surface. Alligator clips were used to attach the high voltage power supply to the needles to distribute a positive voltage of 10 kV to the polymer solutions. Alligator clips were used to attach the high voltage power supply to the control electrodes 56 and 58 to generate a negative voltage equal and opposite to the positive voltage. Two distinct fiber mats were generated using the dual syringe and dual control electrodes. The fibers produced were highly aligned for each syringe/control electrode location.
[0035] The present invention is further discussed in Lisa A. Carnell et al., Aligned Mats from Electrospun Single Fibers, Macromolecules (accepted 2008), the contents of which are incorporated by reference herein in their entirety.
[0036] Although the invention has been described relative to specific embodiments thereof, there are numerous variations and modifications that will be readily apparent to those skilled in the art in light of the above teachings. For example, the present invention can be extended to the fabrication of multiple-ply fiber mats with fiber orientation between the plies being pre-determined. One method of accomplishing this is to attach a polymer film to the collector and deposit aligned fibers thereon as described above. The resulting polymer film/fiber mat can be removed from the collector and then re-positioned on the collector so that the next ply of aligned fibers are deposited on the first ply at a pre-determined orientation with respect thereto. This process can be repeated as frequently as desired until the desired mat thickness is achieved. Since fiber spacing and alignment are readily controlled by the present invention, the porosity of the final mat structure can also be controlled.
[0037] The present invention could also incorporate mobile versions (e.g., via mobile or motorized mountings in one or more directions such as rotation and/or translation) of dispenser 12 and/or electrode 22 and/or collector 16 to permit the movement thereof before or during fiber deposition. Still further, the present invention can be extended to use multiple dispensers 12 and/or electrodes 22 and/or collectors 16 , where one or more of each can be mobile as previously described. The multiple dispensers 12 and/or electrodes 22 may be electrically connected or separate and may be of the same or different physical form, material and charge magnitude. The multiple dispensers 12 may direct the same or different fiberizable materials. Additionally, one or more of the dispenser 12 and electrode 22 combinations may produce pulsed electric fields. Further, the numbers of dispensers 12 , collectors 16 , and electrodes 22 are not required to be equal, and a system can be configured to have each element (dispenser 12 , collector 16 and electrode 22 ) communicating with one or more other elements (dispenser 12 , collector 16 and electrode 22 ). Numerous configurations of each of dispensers 12 , collectors 16 and electrodes 22 , can be utilized (such as stacked, rotating, etc.), with such configuration(s) not being limitation of the present invention as long as the appropriate elliptical electric field is generated.
[0038] Further, the collector could comprise one or more fiber deposition surfaces located thereon. In an alternate embodiment, the collector can be attached (via clamping, gluing, taping or other suitable means) to the electrode, in which case it would then carry the same charge as the electrode.
[0039] It is therefore to be understood that, within the scope of the appended claims, the invention may be practiced other than as specifically described. | A method and system are provided for aligning fibers in an electrospinning process. A jet of a fiberizable material is directed towards an uncharged collector from a dispensing location that is spaced apart from the collector. While the fiberizable material is directed towards the collector, an elliptical electric field is generated via the electrically charged dispenser and an oppositely-charged control location. The field spans between the dispensing location and the control location that is within line-of-sight of the dispensing location, and impinges upon at least a portion of the collector. Various combinations of numbers and geometries of dispensers, collectors, and electrodes can be used. | 3 |
RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. provisional application, Ser. No. 61/880,372 filed on Sep. 20, 2013.
FIELD OF INVENTION
[0002] The present invention relates to devices and apparatus for the treatment of stenosis, and particularly the use of catheter devices in combination with an expandable device for the treatment of stenosis.
BACKGROUND OF THE INVENTION
[0003] Disc herniation and degenerative disorders of the lumbar spine are prevalent, deteriorate the quality of life, and are a major health care concern of the general population.
[0004] Lumbar spinal stenosis is defined as the narrowing of the spinal canal in the lumbar region. This is as a consequence of several pathologic conditions, the most common of which is chronic degenerative spondylosis. Other common causes of stenosis include disc herniation, facet hypertrophy, or congenital causes. Absolute stenosis has been defined as a decrease in the midsagittal lumbar canal diameter of less than 10 mm on MRI.
[0005] Although there are different ways of describing stenosis, generally the stenosis of the spinal canal can occur centrally or laterally. Patients often present with a combination of symptoms from both central and lateral stenosis.
[0006] Lateral stenosis can be further classified into three distinct zones: the lateral recess, foraminal zone, and extraforaminal zone.
[0007] Lateral recess stenosis is caused by overgrowth of the superior articular facet, and ligamentum or capsular redundancy or hypertrophy. Foraminal stenosis may be due to a foraminal disk protrusion, posterior osteophyte formation, ligamentum or capsular hypertrophy, or loss of vertical height from degenerative collapse of the disk. The extraforaminal zone, which is defined as the area lateral to the intervertebral foramen, is most often affected by far-lateral disk and osteophyte pathology.
[0008] Spinal nerves (also referred to as “nerve roots”) originate from the spinal cord, remain within the central portion of the spinal canal, and then exit through the foramen or neuroforamen. The neuroforamen primarily contains the nerve root exiting from each corresponding intervertebral level. It also contains the dorsal root ganglion (DRG), a structure that contains the cell bodies of the afferent sensory neurons. DRG has a variety of sensory receptors that are activated by mechanical, thermal, chemical, and noxious stimuli. If DRG is impinged within the foramen, in lateral stenosis cases, it can be quite painful, and it can become a major source of pain generation.
[0009] Spinal stenosis is treated conservatively initially with therapy modalities and medications. Epidural injections with local anesthetics and steroids may be used next. However, these injections may relieve pain for a limited period of time only. More importantly, injections typically do not influence or improve the functional outcome of patient condition. The majority of patients report little substantial improvement in symptoms with repeated treatment.
[0010] Decompression surgery is considered only after conservative treatments have failed. Currently, there are 2 surgical approaches to decompress the lateral portion of the canal: medial (or “inside-out”), and lateral (or “outside-in”, or “transforaminal”). Each has its advantages and disadvantages. The advantage of the medial approach includes surgeon familiarity through a laminotomy. The disadvantage of medial approach is significant bone resection required to get to the foramen, which is located more laterally, and possible dural tear. This excess bone resection may lead to an iatrogenic instability of the spinal segment if it is extensive. Also, trying to reach under the facet to decompress the foraminal zone can result in possible injury to the nerve root injury due to the deep and lateral position of the nerve root within the foramen. The advantage of transforaminal approach includes less or no bone resection, less risk of dural tear, faster recovery due to less muscle dissection, less risk of possible epidural scar formation. The disadvantages of transforaminal approach include technically demanding approach, and difficulty in visualizing the content of foramen from the lateral side.
[0011] Balloon dilation is currently used in various parts of the body including esophagus, urethra, coronary arteries, and peripheral arteries. Additionally, balloons have been used to create a void within vertebral body to restore the height of fractured vertebrae and allow for filling of the void with cement or bone graft to stabilize a vertebral fracture, commonly referred to as Kyphoplasty.
[0012] Balloons have also been used to aid in separating tissues or vital structures away from a targeted area to be addressed surgically in various parts of the body, including abdominal surgery.
[0013] However, the prior art devices or techniques have not addressed the performing a less invasive open or percutaneous decompression of the lateral stenosis through the use of balloons.
[0014] The use of balloons in the neuroforamen has been discussed in the prior art, but has not addressed the main problem of having adequate control of the balloon device and the method to specifically localize and target a specific point within the neuroforamen.
SUMMARY OF THE INVENTION
[0015] The present invention is directed towards the use of systems and devices that employ catheter devices in combination with expandable structures, e.g. balloons, to treat stenosis. The balloons are utilized to perform foraminal decompression, which allows for non-surgical or less invasive surgical treatment of lateral spinal stenosis by modifying the underlying pathophysiology.
[0016] In one embodiment of the present invention, the expandable structure of the present invention is positioned within the foramen of the spine, with the structure used for decompression of spinal stenosis. The present invention may be used for decompression of lateral spine stenosis. For example, the present invention may be used for decompression in the lateral recess zone, the foraminal zone, or the far lateral (or extraforaminal zone of the spinal canal.
[0017] The methods of the present invention include using the systems and methods used for treating stenosis. The methods can be used for treating spinal stenosis.
[0018] The methods of the present invention include advancing the catheter and inflatable member into the spinal area near where the stenosis occurs. The inflatable member will be advanced, partially inflated, with the steps repeated until proper positioning of the inflatable member to address the stenosis.
[0019] The inflatable members used in the present invention can be of varying sizes, shapes, and materials.
[0020] The inflatable members of the present invention provide selective control of the location of the inflatable member into the spinal area.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] FIG. 1 is an anatomic view of a human spine, showing the different regions of vertebrae.
[0022] FIG. 2 is an anatomic ipsilateral view of the lower back region of the spine, showing the lumbar vertebrae L2 to L5, the sacral vertebrae S1 to S5, and the coccygeal vertebrae.
[0023] FIG. 3 is an anatomic posterior view of the lower back region of the spine, showing the lumbar vertebrae L2 to L5.
[0024] FIG. 4 is an anatomic distal view of the view of the spine shown in FIG. 3 .
[0025] FIG. 5A is an anatomic superior view of a vertebral body, taken along line 5 A- 5 A of FIG. 3 , depicting the central canal, foraminal zone, and the extraforaminal zone of the vertebral body.
[0026] FIG. 5B is an anatomic superior view of a vertebral body, taken along line 5 A- 5 A of FIG. 3 , but showing spinal stenosis affecting the region.
[0027] FIG. 6A is a partially cut-away view of the spinal region as shown in FIG. 3 .
[0028] FIG. 6B is a partially cut-away view of the spinal region as shown in FIG. 3 , but showing spinal stenosis in the region.
[0029] FIG. 7A is a partial view of a delivery device 10 of the present invention being used in the present invention, with a generally spherical inflatable member being used within the delivery device.
[0030] FIG. 7B is a partial view of a delivery device as shown in FIG. 7A , with the exception that the inflatable member has a generally barbell shape.
[0031] FIG. 8 is partial cut-away perspective view of a delivery device of the present invention, with the inflatable member being inflated and a guide wire within the inflatable member.
[0032] FIG. 9 is a partially cut-away view of the delivery system of the present invention, demonstrating a radiopaque marker on the inflatable member.
[0033] FIG. 10 is a partially cut-away view of the delivery system of the present invention, demonstrating an echogenic marker on the inflatable member in combination with an ultrasound imaging machine.
[0034] FIG. 11 depicts a patient lying on an operating table, with the patient's back exposed, which demonstrates an initial step in performing a procedure according to the present invention.
[0035] FIG. 12 depicts an incision in the area depicted in FIG. 11 .
[0036] FIG. 13 depicts the area around the incision being resected to allow access to the area of the spine where insertion of a delivery system according to the present invention will take place.
[0037] FIG. 14 is a partially cut-away view of the spinal region as shown in FIG. 6A showing the first position of the delivery system near the spinal region.
[0038] FIG. 15 depicts a further step in advancing the delivery system into the spinal area.
[0039] FIG. 16 depicts another further step in advancing the delivery system in to the spinal area to be treated, with the inflatable member being slightly expanded.
[0040] FIG. 17 depicts another further step in advancing the delivery system into the spinal area to be treated.
[0041] FIG. 18 depicts the delivery system being positioned as desired within the spinal area.
[0042] FIG. 19 depicts the delivery of a medicament or other solution to the treated area.
[0043] FIG. 20 demonstrates the spinal stenosis being treated, with the inflatable member being retained in place.
[0044] FIGS. 21-29 demonstrate a similar process as described above, with the exception that the delivery device will enter the spinal area from a different position.
[0045] FIG. 30 depicts a perspective partially cut-away view of an alternate delivery device of the present invention.
[0046] FIG. 31 depicts the device of FIG. 30 with the inflatable member in an inflated position.
[0047] FIGS. 32-39 demonstrate a similar process as the process described in FIGS. 21-29 , using a delivery device as shown in FIG. 30 .
[0048] FIG. 40 demonstrates a process similar to the processes described in FIGS. 21-39 , with the delivery system being housed in a portable device.
[0049] FIG. 41 demonstrates a further step in the process shown in FIG. 40 , wherein a guide wire is inserted into the spinal area.
[0050] FIG. 42 demonstrates a further step in the process of FIG. 41 , wherein a catheter is inserted into the spinal area.
[0051] FIG. 43 demonstrates a further step in the process of FIG. 42 , wherein the guide wire is retracted from the spinal area.
[0052] FIG. 44 demonstrates a further step in the process of FIG. 43 , wherein an inflatable member is deployed in the spinal area.
[0053] FIG. 45 demonstrates the spinal stenosis being treated, with the inflatable member being removed from the spinal area.
[0054] FIG. 46 demonstrates an alternate delivery method of the delivery system, wherein the inflatable member is delivered alongside of the guide wire.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0055] Although the disclosure hereof is detailed and exact to enable those skilled in the art to practice the invention, the physical embodiments herein disclosed merely exemplify the invention, which may be embodied in other specific structure. While the preferred embodiment has been described, the details may be changed without departing from the invention. While the present invention pertains to systems, devices, and surgical techniques applicable at virtually all spinal levels, the invention is well suited for achieving dynamic stabilization of transverse processes of adjacent lumbar vertebrae. It should be appreciated, however, the systems, device, and methods so described are not limited in their application to the spine, and could be employed for use in treating different types of stenosis throughout the body.
[0056] The spine (see FIG. 1 ) is a complex interconnecting network of nerves, joints, muscles, tendons and ligaments. The spine is made up of small bones, called vertebrae, which are named according to the region of the body they occupy. The vertebrae in the head and neck region are called the cervical vertebrae (designated C1 to C7). The vertebrae in the neck and upper back region are called the thoracic vertebrae (designated T1 to T12). The vertebrae in the lower back region are called the lumbar vertebrae (numbered L1 to L5). The vertebrae in the pelvic region are called the sacral vertebrae (numbered S1 to S5).
[0057] The vertebrae protect and support the spinal cord. They also bear the majority of the weight put upon the spine. As can be seen in FIG. 4A , vertebrae, like all bones, have an outer shell called cortical bone (the vertebral body) that is hard and strong. The inside is made of a soft, spongy type of bone, called cancellous bone. The bony plates or processes of the vertebrae that extend rearward and laterally from the vertebral body provide a bony protection for the spinal cord and emerging nerves. The vertebrae also protect the thecal sac as shown in FIGS. 2 and 3 . The thecal sac contains the nerve roots for the spinal cord. The spinal cord ends around L1-L2 vertebrae, with the thecal sac continuing downwardly from there.
[0058] The configuration of the vertebrae differ somewhat, but each (like vertebrae in general) includes a vertebral body (see FIG. 5A ), which is the anterior, massive part of bone that gives strength to the vertebral column and supports body weight. The vertebral canal is posterior to the vertebral body and is formed by the right and left pedicles and lamina. The pedicles are short, stout processes that join the vertebral arch to the vertebral body. The pedicles project posteriorly to meet two broad flat plates of bone, called the lamina. The arrangement can also be viewed in FIG. 4 .
[0059] Other processes arise from the vertebral arch. For example, two superior articular processes (“SAP”) project upward from vertebral arch and provide an area for adjacent vertebrae to fit together with one another. Three other processes—the spinous process and two transverse processes—project from the vertebral arch and afford attachments for back muscles, forming levers that help the muscles move the vertebrae.
[0060] FIG. 2 shows the S1 sacral vertebra and the adjacent fourth and fifth lumbar vertebrae L4 and L5, respectively, in a lateral view (while in anatomic association). The sacral and lumbar vertebrae are in the lower back, also called the “small of the back.” FIG. 3 shows the fourth and fifth lumbar vertebrae L4 and L5 from a different, more posterior, perspective.
[0061] As previously described, between each vertebra is a soft, gel-like “cushion,” called an intervertebral disc (see FIG. 2 ). These flat, round cushions act like shock absorbers by helping absorb pressure and keep the bones from rubbing against each other. The intervertebral disc also binds adjacent vertebrae together. The intervertebral discs can bend and rotate a bit but do not slide. Along with the invertebral discs, the vertebrae also provide protection for the spinal cord and thecal sac by forming the vertebral foramen ( FIG. 5A ). The foramen may be depicted with three zones, the foraminal zone, the central canal, and the extraforaminal zone. Stenosis may occur in any of these zones of the foramen, and it is intended that the methods and systems of the present invention would address stenosis in any of these areas.
[0062] FIG. 5A shows a vertebra with a normal vertebral foramen. The vertebral foramen provides an open spinal canal for the spinal cord and the thecal sac to reside. FIG. 5B shows a vertebra with abnormal narrowing of the vertebral foramen, e.g. showing spinal stenosis. As previously explained, when spinal stenosis occurs, the spinous process overgrows into the vertebral foramen, thereby impinging on the spinal cord and/or the thecal sac and the related spinal nerves. The impingement into the vertebral foramen causes nerve root compression and spinal stenosis, with resulting pain, and discomfort.
[0063] As previously discussed, each vertebra also has two other sets of joints (see FIGS. 2 and 3 ). For a given vertebra (e.g., L4), one pair of facet joints faces upward (called the superior articular process, SAP) and the other pair of facet joints faces downward (called the inferior articular process, IAP). The inferior and superior processes mate, allowing motion (articulation), and link vertebrae together. Facet joints are positioned at each level to provide the needed limits to motion, especially to rotation and to prevent forward slipping (spondylolisthesis) of that vertebra over the one below.
[0064] FIGS. 6A and 6B provide another perspective to demonstrate the anatomy shown and described in FIGS. 5A and 5B . The partially cut-away view in FIG. 6A shows the thecal sac sitting within the vertebral foramen, being protected by the vertebral body, as described above. However, as shown in FIG. 6B , an impingement of the thecal sac is shown. The disc is pushing into the thecal sac, while the vertebral facet pushes forward into the thecal sac. Such an impingement is often a condition of facet hypertrophy, or an enlargement or degenerative change in the facet joint. These degenerative changes in the spinous process and the spine in general can adversely affect the ability of each spinal segment to bear weight, accommodate movement, and provide support. When one segment deteriorates to the point of instability, it can lead to localized pain and difficulties.
[0065] Facet joint fixation procedures have been used for the treatment of pain and the effects of degenerative changes in the lower back. In one conventional procedure for achieving facet joint fixation, the surgeon works on the spine from the back (posterior). The surgeon passes screws from the spinous process through the lamina and across the mid-point of one or more facet joints.
II. Representative System of a Delivery Device Used in Treating Stenosis
[0066] The present invention is directed towards a system for treating and addressing conditions caused by stenosis of the joints and is particularly useful for treatment of spinal stenosis. The system will provide relief of the vertebral column and the discs from impinging on the spinal cord and/or thecal sac located in the vertebral foramen.
[0067] As shown in FIG. 8 , the system 10 generally comprises a catheter 12 that houses an expandable member 14 , 14 ′, e.g. a balloon. As will be discussed in further detail, the catheter will generally be introduced into the vertebral foramen by way of a working cannula 15 . The system may also include a guide wire 16 to assist in directing the catheter into the vertebral foramen. Preferably the guide wire 16 is attached to the working cannula 14 at the proximal end 18 by a screw fitting 20 or other common arrangement that will allow the guide wire to be attached or removed as necessary.
[0068] FIGS. 7A and 7B demonstrate different shaped expandable members 14 , 14 ′ that may be used in the system. In FIG. 7A , a spherical expandable member 14 is shown, while a dumbbell-shaped expandable member 14 ′ is shown in FIG. 7B . The dumbbell-shaped expandable member 14 ′ may be designed so that the middle section 22 is less expandable than the distal 24 and proximal portions 26 (see FIG. 8 ). In certain situations, as discussed below, such an arrangement will provide for the expandable member 14 ′ to act as anchor between the medial and lateral sides of a vertebral facet joint. The expandable member 14 ′ may be made of differing materials that allow the distal 24 and proximal portions 26 to expand quicker than the central portion 22 of the expandable member 14 ′.
[0069] To assist in proper positioning of the expandable member 14 , 14 ′, a marker 28 may be located on the end or tip of the expandable member. For example, a radiopaque marker (demonstrated in FIG. 9 ) may be used to visualize the expandable member 14 , 14 ′ position during fluoroscopy. Alternatively, an echogenic marker (demonstrated in FIG. 10 ) could be used in combination with an ultrasound device for ultrasonic guidance of the expandable member 14 , 14 ′.
[0070] To assist in the treatment of stenosis, the catheter 12 is also designed so that the pressure within the expandable member 14 , 14 ′ can be measured, so that proper positioning of the expandable member 14 , 14 ′ when deployed will occur. The volume may also be measure, for example with the use of a dyed fluid being injected into the expandable member.
[0071] The system is also designed so that various solutions, treatments, and substances can be injected into the treated area. For example, anesthetics, steroids, growth factors, stem cell material, or other medicinal materials, may be injected through the system into the treated foraminal space.
[0072] As will be discussed below, the system 10 is designed so that the expandable members can be advance into the vertebral foramen to address the stenosis and, eventually, removed from the foramen once the stenosis has been addressed.
III. Representative Methods for the Treatment of Stenosis
[0073] The present invention includes methods for the treatment of stenosis. As generally discussed above, stenosis is caused by an impingement into a foramen, thereby constricting the thecal sac, nerves, or spinal cord that may be located within the foramen. The methods generally are directed towards the use of expandable members 14 , 14 ′ such as balloons that are inserted into the foramen. The expandable members are inflated in a step-like process to treat the impingement.
[0074] As demonstrated below, the methods of the present invention can be used for the treatment of spinal stenosis. Spinal stenosis may be caused by the overgrowth of the superior articular facet, ligamentum, capsular redundancy, hypertrophy, or a combination of these. As described below, there are two main ways of addressing the spinal stenosis according to the present invention: 1) a mid-line approach that would generally be performed during a laminotomy, or 2) a percutaneous approach.
[0075] Furthermore, the methods described below address issues and problems of the prior art, namely having adequate control of the inflatable members 14 , 14 ′ used in the methods. The described methods are capable of being directed to specifically localize and target a specific point within the neuroforamen. As will be discussed, the present invention allows for control of the inflation of the discussed inflatable members 14 , 14 ′, including control of variables such a pressure and volume for the inflatable members, which allows for precise treatment of the stenosis.
[0076] As shown in FIG. 11 , a patient will be positioned to provide access to the patient's back, such as for a laminotomy. A cut will be made along the length of the spine ( FIG. 12 ), and the area will be resected to provide access to the spinal area ( FIG. 13 ). The expandable member will then be inserted into the resected area, posteriorly to anteriorly until a desired placement and position is found so that the expandable member 14 can be properly inflated.
[0077] FIG. 14 shows an initial positioning of the catheter 12 as it is introduced posteriorly through the laminotomy site. The tip 30 of the catheter 12 is positioned at the beginning of the subarticular zone. The catheter 12 will be slowly moved forwardly in a posterior to anterior direction, further into the foramen ( FIG. 15 ), wherein the expandable member 14 is slowly inflated ( FIG. 16 ). As previously discussed, the positioning of the expandable member 14 will be monitored by the use of a marker, such as a fluoroscopic or echogenic marker.
[0078] Once the catheter 12 and the expandable member 14 are determined to be in a safe position, the catheter 12 may be further inserted into the foramen, with the expandable member being further inflated ( FIGS. 17 and 18 ). The process of insertion and inflation will be repeated until the surgeon has determined that the expandable member is properly positioned. Further, if it is determined that the expandable 14 member may not be properly inflated or positioned after any particular step, the catheter 12 can be retracted and/or the expandable member 14 can be partially deflated to reposition the catheter 12 and the expandable member 14 . In this manner, the stepped process will do minimal agitation or discomfort to the patient while carrying out the process.
[0079] If necessary, a medicinal or therapeutic material such as anesthetics, steroids, growth factors, stem cell material, or other materials, may be injected through the system into the treated foraminal space, as demonstrated in FIG. 19 . As shown, the materials are injected using the same catheter 12 as that which delivered the expandable member 14 . However, it may be possible that a second catheter dedicated to the delivery of these materials may also be employed.
[0080] Once treatment and process has been carried out, the expandable member 14 and the catheter 12 can be removed, as shown in FIG. 20 . The impingement on the thecal sac and/or the spinal cord has been removed/minimized, thereby treating the stenosis.
[0081] The process described can also be carried out from different angles and positions within the vertebral region. For example, FIGS. 21-29 depict another embodiment of the process of the present invention, wherein the stenosis is approached percutaneously. As shown in FIG. 21 , an incision is made laterally from where the vertebral area where the stenosis is located. The catheter 12 and the expandable member 14 ′ will then be inserted laterally to medially, as demonstrated in FIG. 22 .
[0082] As with the previously described method, the catheter will be positioned in a safe area at the initial steps of the process. In this instance, the catheter 12 will be positioned near the superior articular process, in an area referred to as Kambin's triangle (i.e. the Safe Triangle) (also see FIG. 4 ).
[0083] Once properly positioned, the catheter 12 can be advanced medially, as shown in FIG. 24 . If the further position is determined acceptable, the expandable member 14 ′ can be slowly inflated (FIG. 25 ). Monitoring of the position of the catheter 12 and expandable member 14 ′ can be carried out by the use of a marker, such as a fluoroscopic or echogenic marker 28 , as previously described.
[0084] The steps of insertion and inflation can be repeated (see FIGS. 26 and 27 ) as many times as necessary until the expandable member 14 ′ is properly positioned. The process of insertion and inflation will be repeated until the surgeon has determined that the expandable member 14 ′ is properly positioned. And, as previously discussed, if it is determined that the expandable member 14 ′ may not be properly inflated or positioned after any particular step, the catheter 12 can be retracted and/or the expandable member 14 ′ can be partially deflated to reposition the catheter 12 and the expandable member 14 ′. In this manner, the stepped process will do minimal agitation or discomfort to the patient while carrying out the process.
[0085] If necessary, a medicinal or therapeutic material such as anesthetics, steroids, growth factors, stem cell material, or other materials, may be injected through the system into the treated foraminal space, as demonstrated in FIG. 28 . As shown, the materials are injected using the same catheter 12 as that which delivered the expandable member 14 ′. However, it may be possible that a second catheter dedicated to the delivery of these materials may also be employed.
[0086] Once treatment and process has been carried out, the expandable member 14 ′ and the catheter 12 can be removed, as shown in FIG. 29 . The impingement on the thecal sac and/or the spinal cord has been removed/minimized, thereby treating the stenosis.
[0087] As shown in FIGS. 26-28 , the expandable member 14 ′ is of a dumbbell-shape, as previously discussed as one possible shape for the expandable member. The expandable member will act as an anchor between the medial and lateral sides of the facet joint, thereby minimizing the risk of the expandable member 14 ′ being displaced into the medial canal, thereby potentially avoiding the risk of dural injury, or displacing laterally, thereby preventing dislodging of the balloon (expandable member 14 ′) laterally and out of the foramen.
[0088] As appreciated and understood with such procedures as described herein, there are different layers, e.g. skin and fascia (deep thick layer underneath the skin), that need to be navigated when performing such a procedure. Likewise, the present devices and procedures are used around sensitive nerves and the foramen. The devices and methods of the present invention are designed to be used in such differing areas of the body. For example, to penetrate the skin and the fascia, a sharp device may be desired to penetrate these layers, while a more blunt device may be desirous when navigating around the nerves and the foramen. The delivery device and system 100 shown in FIG. 30 contemplates such considerations.
[0089] The delivery device 100 of FIG. 30 generally comprises a catheter 102 . The delivery device 100 comprises a pair of stylets 104 and 106 that will be used to for navigation of the delivery device through the various layers discusses above. The delivery device also houses an inflatable member 108 , and preferably a guide wire 110 to assist in properly positioning the inflatable member in place.
[0090] As shown in FIG. 31 , the stylets 104 and 106 of the delivery device 100 are telescopingly arranged with one another. The interior stylet 106 has a blunt end 112 , which is beneficial when navigating around the foramen and nerves located in the spinal area. The blunt end 112 of the interior stylet 106 will also minimize any damage, e.g. puncturing, of the inflatable member 108 . The inflatable member 108 shown in Figure is dumb-bell shaped, but, as discussed above, a spherical or other shaped balloon may be used, as noted with inflatable members 14 , 14 ′.
[0091] The exterior stylet 104 has an angled or sharpened end 114 , which assists in piercing or penetrating the skin and the fascia. For example, the beveled end 114 of the exterior stylet 104 may have an angle (greater than 0°), e.g. 20° or 30°, that will provide the sharpened edge. To protect the inflatable member 108 from being damaged by the exterior stylet 104 , the inflatable member 108 is preferably located within the interior stylet 106 , thereby providing a barrier between the exterior stylet 104 and the inflatable member 108 .
[0092] FIG. 32 demonstrates a step in the insertion of the delivery device into a patient. The patient will be initially prepped, as shown previously in FIGS. 21 and 22 . Once prepped, the catheter 102 will be positioned in a safe area. The catheter 102 will be positioned near the superior articular process, in an area referred to as Kambin's triangle (i.e. the Safe Triangle) (also see FIG. 4 ). The sharpened end 114 of the exterior stylet 104 will be used to penetrate the skin and the fascia.
[0093] Once properly positioned and the exterior stylet 104 has properly and sufficiently pierced and penetrated the skin and the fascia, the interior stylet 106 will be extended, as shown in FIG. 33 , with the exterior stylet 104 being maintained at the initial position shown in FIG. 32 . Once properly positioned in an acceptable position, the inflatable member 108 will then be further extended outwardly from the blunt 112 end of the interior stylet 106 ( FIG. 34 ), and the inflation process can commence, with the process being monitored, as previously described. The guide wire 110 will be used in properly navigating the inflatable member into the proper positioning.
[0094] As previously described above, the steps of insertion and inflation can be repeated as many times as necessary (see FIGS. 35 and 36 ). The process of insertion and inflation will be repeated until the surgeon has determined that the expandable member 108 is properly positioned. And, as previously discussed, if it is determined that the expandable member 108 may not be properly inflated or positioned after any particular step, the catheter 102 can be retracted and/or the expandable member 108 can be partially deflated to reposition the catheter 102 and the expandable member 108 . In this manner, the stepped process will do minimal agitation or discomfort to the patient while carrying out the process. Once properly positioned, the guide wire 110 is withdrawn from the device ( FIG. 35 ). As previously noted with respect to FIG. 8 , the guide wire 110 may be removed by unscrewing the guide wire from the delivery device.
[0095] If necessary, a medicinal or therapeutic material such as anesthetics, steroids, growth factors, stem cell material, or other materials, may be injected through the system into the treated foraminal space, as demonstrated in FIG. 37 . As shown, the materials are injected using the same catheter 102 as that which delivered the expandable member. However, it may be possible that a second catheter dedicated to the delivery of these materials may also be employed.
[0096] Once treatment and process has been carried out, the expandable member 108 and the catheter 102 can be removed, as shown in FIG. 38 , with the inflatable member 108 being retracted into the interior stylet 106 . The interior stylet 106 is then telescoped inside of the exterior stylet 104 , and the catheter 102 can be removed. The impingement on the thecal sac and/or the spinal cord has been removed/minimized, thereby treating the stenosis.
[0097] The system and device can delivered in a similar fashion as described in the methods above, but with the delivery system being positioned within a portable housing 40 . The portable housing is preferably designed so that it can be hand held. As shown in FIG. 40 , the portable housing 40 allows deployment of a catheter, in the similar fashion as described above. The portable housing preferably has a switch or control device 42 that assists in delivery of the guide wire 16 and/or the inflatable member 14 ′ (see FIG. 43 ). The control device 42 may comprise further devices so that the individual parts of the system, e.g. the guide wire 16 or the inflatable member 14 ′ could be individually controlled. The control device can be used to monitor the volume, e.g. mm 3 , of the inflatable member 14 ′, so that the inflatable member 14 ′ will be properly inflated.
[0098] FIG. 40 shows the catheter 12 being properly positioned in the spinal area, as described above. Once the catheter is positioned, the guide wire 16 can be introduced into the spinal area, as demonstrated in FIG. 41 . Once the guide wire 16 is positioned, the cannula 15 that will deliver the inflatable member 14 ′ is introduced into the spinal area ( FIG. 42 ).
[0099] As an alternate step to the processes discussed above, the guide wire 16 is then removed from the spinal area ( FIG. 43 ), prior to the deployment of the inflatable member 14 ′ ( FIG. 44 ). It is understood, as described above, that the inflatable member can be deployed and retracted as necessary so that the device can be properly positioned to treat the stenosis (see FIG. 45 ).
[0100] It should be understood that either expandable member shape, or other shapes, could be used with either of the processes described. Provided that an expandable member was inserted and progressed as described, it is understood that the process will be covered by the present disclosure. For example, FIG. 46 demonstrates a delivery step that could be used in any of the above procedures. The inflatable member 14 ′ is delivered over the guide wire 16 , but is used with a portable housing 40 , as shown in FIG. 40 .
[0101] The foregoing is considered as illustrative only of the principles of the invention. Furthermore, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described. While the preferred embodiment has been described, the details may be changed without departing from the invention. | Catheter system, devices and methods for diagnosing and treating lateral stenosis causing back pain and or leg pain. The devices comprise a tubular part for insertion into a working cannula to self-position itself safely within the foramen, and minimize the risk of displacement medially or laterally, to prevent nerve or dura injury. An expandable membrane is configured to maintain the catheter device within the foramen. Expansion of this membrane would decompress the nerve within the foramen by opening the foraminal canal as the membrane expands. | 0 |
BACKGROUND OF THE INVENTION
The present invention relates to an automatic deployment and retrieval tethering system. In particular, the present invention relates to a system for automatically winding and unwinding cable, for example, fiber optic or electrical cable or a combination of both, from a moving vehicle. The moving vehicle might be, for example, a remotely controlled robot.
The invention relates to a cable deployment and retrieval system for a moving object, for example a robot having a tether or umbilical cord. Some robots do not use radio control, for example, because of interference, and require an umbilical cord to be attached to the robot to transmit or receive information or data, for providing control and possibly power, if the robot does not include its own power source. The problem with such umbilical cords or tethers is deploying the cable so that the cable does not become tangled when the robot moves in different directions. The cable deployment system must be able to deploy the cable as the robot moves forward and retract the cable as it reverses. In addition, the system must be able to allow the robot to go around corners without placing excess tension on the cable and must allow the robot to turn, sometimes in very tight quarters, without snagging the cable. There may be situations where even though the robot is not moving forward or backward, the cable must either be retracted or deployed, depending upon the turn that the robot is making. Additionally, the robot must be able to drive over the cable without snagging the cable and while still allowing cable to be extended or retracted.
There have been various attempts in the prior art to provide cable deployment systems. However, all of the prior art devices, as far as applicant is aware, suffer from various drawbacks.
U.S. Pat. No. 4,736,826 to white et al. is exemplary of efforts made in the prior art. In that patent, the tethering system uses a cable feed drive motor that deploys and retrieves cable. The system is wholly dependent on receiving encoded signals originating from the direction of rotation of the drive wheels of the robot vehicle itself.
Because in the device of the White et al. reference the cable feed drive motor is dependent on wheel rotation, and not on actual vehicle movement, if there is any slippage between the wheels and the ground, so that the wheels spin or in trying to stop, slip, the signal that would be sent through the encoders to the cable reel motor would reflect the rotation or non-rotation of the wheels, but not the actual movement of the vehicle. This would cause an incorrect amount of cable to be deployed or retracted by the cable reel motor relative to the actual vehicle movement, resulting in damage to the cable or the robot.
Another disadvantage of the device of the White et al. reference relates to when a robot is pivoted around its own center point. For example, if the drive wheels in the White et al. device would rotate in opposite directions with the same rotational speed, the robot would basically pivot around its own center point, and the encoder signals coming from the opposite drive wheels would vector each other out, and no cable would exit from the vehicle. However, as the exit point of the cable is above the pivot wheel, which is at some radial distance away from the exampled pivot turning center of the robot, the cable would have to be deployed at the same circumferential speed as the pivoting robot's cable exit point. However, vectorially the drive wheel encoders would cancel each other out, the cable would not deploy and the cable already deployed would go into extreme tension and break, or stop the robot from pivoting.
Other systems are also known in the prior art for deploying cable from a moving vehicle. In some, tension is sensed in the deployed cable. However, these systems typically employ a dancer arm, tension control arm or tension rollers to sense the tension in the deployed cable. The problem with these systems is that they typically operate in only one direction. For example, U.S. Pat. No. 4,666,102 to Colbaugh et al., shows an apparatus for automatically dispensing and taking up a flexible communications cable such as an optical fiber which includes a motor driven reel which is mounted on a vehicle. The fiber passes through a pivotably mounted tension control arm whose angular position is detected to control the motor. Depending on the position of the tension control arm, the reel may be rotated in one direction to relieve fiber tension or it may be rotated in the opposite direction to take-up slack, or it may remain quiescent.
The problem with the device of the Colbaugh et al. reference is that if the mobile vehicle makes a pivot turn, for example, such that the instantaneous direction of cable exit is at an angle with respect to the tension control arm, the tension control arm cannot respond properly since it can only pivot along one axis. Such a system will result in increased tension in the cable which cannot, be detected properly by the tension control arm, with subsequent damage to the cable and/or vehicle.
In U.S. Pat. No. 4,583,700 to Tschurbanoff, a cable winding system for electrically powered mine vehicles is disclosed. This system utilizes a pivotable extension arm having guide rollers thereon. Again, as in the device of Colbaugh et al., this system is incapable of sensing tension in all directions and is only capable of substantially sensing the tension in a direction collinear with the extension arm.
U.S. Pat. No. 4,692,063 to Conti describes a system for measuring the tension in a cable during underground placement in for example, a furrow formed by a tractor deploying the cable. The system measures the pressure of a hydraulic fluid supplied to a capstan motor to determine the tension in the cable which can be monitored so that if the tension increases the tractor can be stopped. If the tension increases without exceeding a trip point, the tractor can be slowed down to reduce the tension in the cable. The system of the Conti reference is for use in a forward direction only (i.e. unwinding) and further, is incapable of sensing tension in a 360° arc around a cable exit point. Furthermore, the system of that reference is designed for large tractor size cable laying devices and not for mobile vehicles such as robots which perform very complex tasks including pivoting about an axis, rapid changes of direction and forward and reverse motions.
Another example of a unidirectional cable unwinding system is shown in U.S. Pat. No. 4,744,696 to Vidler. This device utilizes a slack loop formed in the cable during paying out and the amount of the cable in the slack loop is monitored to determine the tension in the cable.
SUMMARY OF THE INVENTION
It is accordingly an object of the present invention to provide an automatic deployment and retrieval tethering system, i.e. an automatic cable deployment and retrieval system.
It is still a further object to provide an automatic cable deployment and retrieval system which can be used with mobile vehicles.
It is yet still a further object of the invention to provide such an automatic cable deployment and retrieval system which can be used for mobile vehicles such as remotely controlled robots which employ a tether system for providing power, control and/or communications.
It is yet still a further object of the invention to provide such an automatic cable deployment and retrieval system which can be used with varying types of cable, for example, electrical cable, power cable, control cable, communication cable, fiber optic cable etc. The cable may carry electrical signals or power through metallic conductors or may comprise a fiber optic cable or a combination of both.
It is yet still another object of the invention to provide an autonomous automatic cable deployment and retrieval system which can be used interchangeably with different mobile vehicles or robots, i.e., a device which can be substantially "bolted on" to a variety of mobile vehicles.
It is yet still a further object of the invention to provide such an automatic cable deployment and retrieval system which is unitized, self-contained, self-regulating, self-programming and automatic.
It is yet still another object of the invention to provide such an automatic cable deployment and retrieval system which can be attached to any robotic vehicle, permitting continuous two way transmission of voice, video, data, power and command through all speeds, directions, motions, turns, including pivot turns, of the vehicle to which it is attached.
It is yet still a further object of the invention to provide such an automatic cable deployment and retrieval system which uses a novel system for measuring the strain in the deployed cable to control cable deployment or retrieval. In particular, it is an object of the invention to provide a strain gauge for sensing cable tension for controlling the deployment or retrieval of the cable.
It is yet still a further object of the invention to provide such an automatic cable deployment and retrieval system which allows deployment and retrieval of fiber optic, metallic, or a combination cable, through all motion modes, with zero or pre-defined lay-down tension and smooth level wind storage onto or off of a self-contained cable reel which is attachable to the device.
It is yet still a further object of the invention to provide such an automatic cable deployment and retrieval system whose control is independent of the rotation of or direction of rotation of the drive wheels or other movement causing member of the vehicle itself.
It iS yet still a further object of the invention to provide such an automatic cable deployment and retrieval system which is completely autonomous and independent of any signals from the drive mechanism of the vehicle, or the vehicle itself, as it senses a need to deploy or retrieve cable or remain dormant, based on a self-contained cable strain sensor which itself accounts for the actual relative direction, motion and speed between the vehicle to which the cable deployment and retrieval system is attached and the deployed cable itself.
It is yet still a further object of the invention to provide a much simpler cable deployment and retrieval system than provided in the prior art. Using strain gauge sensors, it is possible to obtain such a device.
It is yet still a further object of the invention to provide such an automatic cable deployment and retrieval system which eliminates the need for all speed and direction circuitry or mechanical linkages between the robot or robot drive motor and the cable deployment and retrieval system.
It is yet still a further object of the invention to eliminate all gearing, chain drives, optical encoders and encoder mounts between the vehicle wheels or drive system and the cable deployment and retrieval system.
It is yet still a further object of the invention to provide an automatic cable deployment and retrieval system which will retract cable when the vehicle reverses itself but, in addition, due to the action of a strain gauge sensor, will also retract the cable when it returns directly, in a forward direction, to its monitoring station.
It is yet still a further object of the invention to provide an automatic cable deployment and retrieval system which allows the vehicle to which it is attached to reverse itself or simply turn around to head back to its monitoring station with proper deployment and retrieval of the cable in such a situation.
It is yet still another object of the invention to provide an automatic cable deployment and retrieval system which includes sensor means for allowing 360° sensitivity to the tension in the cable where it exits the automatic cable deployment and retrieval system.
It is still yet a further object of the invention to provide an automatic cable deployment and retrieval system which uses a sensor which senses the cable strain pressure on its surface in any direction such that the system can deploy or retract cable regardless of whether the vehicle is moving forward, backward, sideways or pivot turning.
It is still yet another object of the invention to provide an automatic cable deployment and retrieval system which is flexible enough to be used with different width cable reels and varying thickness cables.
The above and other objects of the invention are achieved by an apparatus adapted to be mounted on a mobile vehicle for deploying and retrieving cable from the vehicle into the vehicle environment comprising: a frame for mounting to the vehicle; means on the frame adapted to receive a cable storage reel having cable wound thereon for rotatable motion, the cable on the reel having a first end near the center of the reel, a wound portion of cable on the reel and an unwound portion of cable that extends from the reel; means for coupling the first end of the cable to the vehicle; means for feeding the cable comprising the unwound portion on and off the cable storage reel; means including a cable exit area for guiding the unwound portion of cable from the vehicle into the environment in any direction defined by a 360° arc around the cable exit area; means for sensing the tension in the unwound portion of cable in any direction defined by the 360° arc around the cable exit area; and means coupled to the sensing means receiving a signal from the sensing means related to the tension in the unwound cable for controlling said feeding means so as to maintain a preset tension or no tension in the unwound cable. The ability to sense cable tension in an arc of 360° about the cable exit opening allows the device to be used to deploy cable connected to vehicles which have varying speeds, turn in any direction including pivot turns, go around obstacles and corners and reverse direction.
In accordance with the invention, the means for sensing preferably comprises a strain gauge for generating a signal related to the amount of tension in the cable.
Preferably, the means for feeding cable on and off the cable storage reel comprises a drive means comprising a drive motor for driving the cable storage reel in rotation and a pair of drive rollers for receiving the cable from the storage reel between surfaces of the rollers, at least one of the rollers being driven by a drive roller motor.
In accordance with a preferred embodiment, the means for controlling comprises circuit means electrically coupled to the strain gauge for controlling the rotation of the drive means and for controlling the rotation of the drive rollers so as to maintain the preset tension or no tension in the unwound cable.
Further in accordance with a preferred embodiment, the means for sensing further comprises a member having an exit opening for the cable, the opening have a perimeter, the cable being provided through the opening so that it can come into contact with the perimeter of the opening over 360° of the perimeter of the opening, the cable thereby exerting a force on the perimeter of the opening related to the tension in the cable, the strain gauge being coupled to the member having the exit opening and providing a signal related to the force applied and thereby to the tension in the cable.
In the preferred embodiment, the member having the exit opening comprises a tubular conduit, the tubular conduit being coupled to the strain gauge. The tubular conduit moves when the cable applies a force thereto, thereby flexing the strain gauge and generating a signal related to the tension in the cable. Minute forces in the cable can be detected and amplified with suitable electronic amplification circuitry to control cable deployment.
Preferably, a means for limiting movement of the tubular conduit is provided. The means for limiting movement in the preferred embodiment comprises a plate having an opening larger than an outside diameter of the tubular conduit with the tubular conduit extending through the plate opening, and thereby defining a clearance between an inner surface of the plate opening and the tubular conduit.
In accordance with the preferred embodiment, a fixed mounting support is mounted to the frame, the strain gauge being coupled between the mounting support and the tubular conduit. A rigid bracket is fastened to the mounting support and extends downwardly adjacent the strain gauge and tubular conduit and is fastened to the plate having the opening larger than the outside diameter of the tubular conduit, thereby securing the plate in position around the tubular conduit.
Further in accordance with the invention, a means for coupling the first end of the cable which is at the center of the cable reel to the vehicle comprises a rotating joint for providing communication between the cable wound on the reel and the vehicle. Preferably, a hinged conduit supporting the rotating joint and for guiding the cable connected to the rotating joint to the vehicle is provided. The rotating joint may comprise, for example, a means for providing electrical and/or fiber optic communication with the cable on the cable reel, e.g., an electrical/fiber optic rotating joint.
In accordance with the preferred embodiment of the invention, means for guiding the cable onto the cable reel so as to achieve a level wind of the cable on the cable reel is provided. The means may comprise a flaking loop which reciprocally moves across the width of the cable reel.
Preferably, the traverse and starting point of the flaking loop which is reciprocally movable across the width of the cable reel is adjustable to accommodate different width cable reels. Provision is made for maintaining the starting point of the flaking loop traverse at a fixed point.
In accordance with a preferred embodiment of the invention, the cable reel drive means is turned on only to retrieve cable and is not turned on when cable is deployed. When cable is deployed, the cable reel turns freely only against the braking action provided by the reducing gear transmissions forming a part of the apparatus.
Further in accordance with the preferred embodiment, the roller drive motor is bi-directional so as to turn in a first direction to deploy cable and to turn in a second opposite direction to retrieve cable, with the cable reel drive means being controlled so as to maintain a prescribed tension in the cable between the cable reel and the drive rollers during cable retrieval.
In accordance with a further aspect of the invention, a method is provided for deploying and retrieving cable from a mobile vehicle into the vehicle environment comprising mounting a cable storage reel for rotatable motion on a frame coupled to the vehicle, the cable having a first end near the center of the reel, a wound portion of cable on the reel and an unwound portion of cable that extends from the reel, coupling the first end of the cable to the vehicle, feeding cable comprising the unwound portion on and off the cable storage reel, guiding the unwound cable from the vehicle from a cable exit area into the vehicle environment in any direction defined by a 360° arc around the cable exit area, sensing the tension in the unwound cable in any direction defined by the 360° arc around the cable exit area, and receiving a signal related to the tension in the unwound cable and bi-directionally controlling the feeding of cable so as to maintain a preset tension or no tension in the unwound cable.
In addition to robots as commonly envisioned, the invention may be applied to any type of unmanned autonomous vehicle, such as Bobcats, backhoes, diggers, ground moving equipment, etc., which may be used in any hazardous environment such as waste dumps sites, radiation or chemically polluted sites, explosive removal and for use also with manned vehicles for automatically deploying cable along roads, fields, beaches, etc.
Other objects, features and advantages of the present invention will become apparent from the following description of the invention which refers to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be described in greater detail in the following detailed description with reference to the drawings in which:
FIG. 1 is a perspective 3/4 view of the front of the automatic cable deployment and retrieval system;
FIG. 2 is a plan view of the front of the automatic cable deployment and retrieval system;
FIG. 3 is a top plan view of the automatic cable deployment and retrieval system;
FIG. 4 is a side view of the automatic cable deployment and retrieval system according to the present invention corresponding to a view looking from the left in FIG. 1 or FIG. 2;
FIG. 5 shows the automatic cable deployment and retrieval system according to the present invention mounted to a wheeled robot, showing an exemplary use of the invention;
FIG. 6 shows the automatic cable deployment and retrieval system according to the present invention utilized on a "walking" type of robot;
FIG. 7 is a detailed front view of the automatic cable deployment and retrieval system according to the present invention, showing details of the internal mechanism in phantom and corresponding to FIG. 2;
FIG. 8 is a top view of the automatic cable deployment and retrieval system according to the present invention, showing the details of the mechanism in a phantom view corresponding to FIG. 3;
FIG. 9 is a right side phantom view of the automatic cable deployment and retrieval system according to the present invention taken along line 9--9 of FIG. 7, corresponding to the side opposite the side shown in FIG. 4, i.e. corresponding to a view looking from the right in FIG. 2;
FIG. 10 is a rear plan view of the automatic cable deployment and retrieval system according to the present invention with the hinged back cover opened, corresponding to the back side opposite the side shown in FIG. 2;
FIG. 11 is a top view of the support for the cable strain sensing assembly used in the automatic cable deployment and retrieval system of the present invention;
FIG. 12 is a side view of the cable reel hinged conduit assembly and the cable strain sensor assembly used in the present invention and corresponding to a view along line 12--12 of FIG. 8;
FIG. 13 is an electronic block diagram of the circuitry receiving signals from the cable strain sensor assembly and for controlling the reel drive motor (driving the cable reel) and roller drive motors which drive rollers from which the cable is deployed and/or retrieved;
FIG. 14 is a plan view of the cable reel attaching gear plate;
FIG. 15 is a perspective view of the cable strain sensor assembly of the cable deployment and retrieval system showing details of the deployed cable exit tube as well as the strain gauge assembly and the manner of attaching the strain gauge assembly to the device frame;.
FIG. 16 is a plan view of a cam follower employed in the invention for achieving reciprocating movement of the cable reel flaker assembly which achieves level wind of the cable on the cable reel;
FIG. 17 is a detailed perspective view of a level wind camshaft worm thread used to achieve a reciprocating movement of the cable reel flaker assembly for obtaining level wind of the cable on the cable reel;
FIG. 18 illustrates a detail of the cable strain sensing apparatus;
FIG. 19 shows a cable reel illustratively used with the invention; and
FIG. 20 shows a fiber optic/electrical rotating joint useful in the invention.
DETAILED DESCRIPTION OF THE INVENTION
With reference now to the drawings, FIG. 1 shows a perspective view of the automatic cable deployment and retrieval system according to the present invention, generally designated 1. The device 1 includes a main housing 10, a subsidiary hinged housing 12 hinged at the hinge 14, a cable deployment retrieval exit bracket 16 which also serves as a strain sensor motion limiting device (to be described below), a hinged conduit 18 for supporting a fiber optic/electrical rotating joint 20 and for leading wires from the rotating joint 20 into the housing 10 for providing control, communications and/or power to the vehicle upon which the system is disposed, and a removable cable reel 22 upon which the deployed cable 24 is wound. The free deployed end of the cable 24 is coupled to a monitoring control and/or power station for the mobile vehicle to which the system 1 is fastened.
In addition, projecting from the housing 10 is a loading knob 26 for relatively moving pinch rollers, to be described later, so that the cable can be loaded into the device for deployment. Also provided is a tension adjusting knob 28 which will be described hereinafter, as well as a switch 30 having two positions, "null" and "run", and two potentiometers 32A and 32B for adjustment of the null point, and whose function will be described in greater detail below. Also provided is a main power circuit breaker 31.
FIG. 5 shows the automatic cable deployment and retrieval system according to the present invention mounted to a wheeled robot 2, and FIG. 6 shows the device according to the present invention attached to a "walking" type of robot 3 equipped with a robot arm holding a television camera. The present invention is not limited to use with remotely controlled robots. It may be used with any vehicle requiring a tether for control, communications and/or power or for any other purpose. For example, it is equally applicable to a manned vehicle which is provided with electrical power from a remote source or is provided with communication cables or for deploying cable.
With reference now to the detailed drawing FIGS. 7-18, which show details of the automatic cable deployment and retrieval system according to the present invention, cable reel 22 is removably supported on a gear plate 34. Gear plate 34 includes three equally spaced keyhole slots 36 (FIG. 14) which receive grooved studs 38 (FIG. 8) which are mounted to the back of cable reel 22 flange 22A. To mount the cable reel 22 on the plate 34, the grooved studs 38 on the cable reel flange 22A are inserted first through the respective large diameter portions 36B of the keyhole openings 36 and rotated slightly in a counterclockwise direction to allow the grooved studs to slide into the respective small width portions 36A of the keyholes. A manually releasable spring clip 40 is attached to the back side of the gear plate 34, to lock the cable reel in position once the studs 38 are located within the smaller sections 36A of the keyholes 36. Gear plate 34, as shown in more detail in FIG. 9, is coupled to a shaft 42 which is driven by a main drive motor 44 through a reducing gear transmission 46. Transmission 46 is provided to achieve the required speed range for the cable reel 22.
On the front flange 22B, three equally spaced ball studs 48 (FIG. 8) are provided, which releasably engage with a rotating joint fastening plate 50. The rotating joint fastening plate is secured to the rotating part of a rotating joint 20, which may be a fiber optic/electrical rotating joint.
FIG. 20 shows a perspective view of a typical rotating joint 20, showing the rear of the joint which is attachable to rotating fastening plate 50 which releasably engages the cable reel. The joint 20 includes a stationary outer main housing 20A which is coupled to the brackets 55. See FIG. 8. Stationary fiber optic/electrical cables 52 exits from the stationary housing and is fed into conduit 18. The center 20B of the rotatable joint is rotatable about an axis 20C. This portion includes a central fiber optic cable with connector 20D and various electrical conductors with connectors 20E. These are coupled to the fiber optic and/or electrical cable 24 on the cable reel 22, as will be explained below.
The purpose of the rotating joint is to allow communication of electrical signals on the electric conductors and light signals on the fiber optic conductors in the cable 24 wound on the reel 22, which is rotating, with the stationary conductors and fiber optic conductors 52 threaded through the conduit 18. The electrical/fiber optic conductors 52 are guided through the conduit 18 into the housing 10 of the deployment system and then connected to the vehicle itself. The cables 52 may be used for a number of purposes, including power for the vehicle upon which the invention is disposed, for control signals for the vehicle or communications, for example, for television, radio or camera signals. In addition, the cable deployment and retrieval device of the present invention may be powered from the cables 52 or it may receive power from the robotic vehicle itself on which it is mounted or from its own power source such as batteries, e.g., rechargeable batteries.
FIG. 19 shows an illustrative cable reel which can be used with the invention. The cable 24 is wound on the cable reel 22. Only a small portion of the cable 24 near the end which is first wound on the cable reel is shown in FIG. 19, for clarity. The cable 24, when wound on the reel 22, is first inserted through a hole 23 located on the inner drum part 22C of the cable reel. The cable is threaded through the hollow center portion 22D of the drum and extends out. Pigtail and fiber optic connectors, as necessary, are provided for connection to the rotating part of rotating joint 20, which is coupled to the studs 48 via snap sockets 58 on plate 50.
The automatic cable deployment and retrieval system according to the invention is illustratively mounted to the vehicle by bolts placed through holes 53 in a relatively thick plate 51 located at the bottom of housing 10.
The rotating joint 20 is commercially available from companies such as ElectroTech Corp. of Blackburn Va. and others, and generally includes a number of pigtail leads and a fiber optic connector on both the rotating and stationary sides which are coupled to the respective portion of the rotating cable 24 at the center of the reel and stationary cable 52.
Conduit 18 is fastened at the reel end to a fastening bracket 55 which in turn is fastened to the stationary housing of the rotating joint 20. The other end of conduit 18 is mounted to a hinge 54 which is attached in turn to a further straight portion of conduit 56 which is secured to the device frame 10.
Rotating joint 20 rotatable fastening plate 50 at the reel includes three ball stud sockets 58 which releasably engage with the ball studs 48 mounted on the flange 22B. Thus, after the reel 22 containing wound cable 24 is installed on the gear 34, conduit 18, which has been moved on its hinge 54 away from the reel area, is moved toward the reel 22. The reel 22 is rotated slightly to line up the ball studs 48 with the ball stud sockets 58, thereby securing the rotating joint to the reel 22 and providing bearing support for the outer flange of the reel 22B. Prior to snapping the sockets 5 onto the studs 48, the necessary electrical and fiber optic connections between the rotating joint 20 and the wound end of cable 24 extending from the center of the reel 22 is made in the area 60. Thus, electrical and light connections are made between the cable 24 on the reel 22 and the cable or cables 52 which are attached to the mobile vehicle.
Turning now particularly to FIGS. 7 and 8, hinged housing 12 covers two drive rollers 62 and 64. The unwound portion of cable 24 for deployment is fed from the reel 22 through a reciprocating flaker assembly 66, then through a cable centralizer 68 and then through the pinch space 70 between the two rollers 62 and 64. Cable 24 is then fed downwardly through a hole 72 in a sensor mounting block 74 and then through a cylindrical conduit 76 to the ground (FIGS. 11, 12, 15 and 18) for deployment. The deployed end is typically coupled to the mobile vehicle's monitoring, control and/or power station.
As shown in FIG. 7, housing 12 is hinged at 14 for internal access and is releasably fastened to the main mounting frame 10 of the device by ball stud snap fasteners received in sockets 78.
Turning again to the drive rollers 62 and 64, drive roller 64 is secured via splines 80 on a rotating shaft 82 which is driven by a roller drive motor 84 through a gear reducing transmission 86.
Idler drive roller 62 is supported for pivoting movement to allow the cable 24 to be initially loaded between the roller 62 and 64. Roller 62 is rotatably supported via a bearing 87 on a shaft 88 and secured to the shaft 88 via set screws 90. Shaft 88 is fixedly attached to a pivoting lever arm 92 via set screws 94. Pivoting lever arm 92 pivots about a pivot point provided by a shaft 96. Lever arm 92 is securely attached to the pivot shaft 96 via set screws 98. Shaft 96 is a part of a load lever arm 104 having a 90° bend and is supported in a bearing 100 provided in a bearing support 102 mounted to the device frame 10. Arm 104 is bent at a right angle from shaft 96 to project upwardly through elongated slot 107 in housing 10. A knob 26 is attached to the projecting end of the arm 104. One end of a tension spring 108 is secured to the load lever arm 104 and the other end of the spring is secured to a screw 110 received through a hole in housing 10 by a tension adjusting knob 28.
When it is desired to deploy cable, the cable is first manually threaded through the loop of reciprocating cable guide (or flaker arm) assembly 66, through the cable centralizer 68, and then down between the rollers 62 and 64. To do this, the knob 26 is moved to the right in slot 107, thereby pivoting roller 62 about the pivot shaft 96 against the tension of the spring 108. This creates a gap between two rollers 62 and 64 at pinch point 70 and the cable may be inserted there-between, and then down through the hole 72 in the sensing support block 74. The cable is further threaded through the strain gauge movement limiting tube 76 to the ground. A description of the function of the tube 76 will be provided later.
The function of the cable centralizer 68 is to locate the cable approximately along the center plane P (FIG. 8) of the two rollers 62 and 64. The centralizer 68 has a downwardly projecting first portion 68A and an upwardly projecting portion 68B which is coupled to the first portion 68A to form a loop. At its top, the portion 68B traverses horizontally in a portion 68C toward the portion 68A to form an open loop to enable easy threading of cable 24 therethrough. The portion 68C clears the portion 68A by approximately the diameter of cable 24.
The centralizer is mounted in a stationary adjustable fashion to the device frame 10 via two nuts 69 as shown in FIG. 8. Adjustment of the cable centralizer 68 to the center plane of the two rollers 62 and 64 is provided by adjusting and locking the two nuts 69 which secure the cable centralizer to the support frame. The desired location of the centralizer 68 with respect to the center plane of the rollers 62 and 64 as well as the desired distance away from the rollers can thus be obtained.
In contrast to the cable centralizer 68, the flaker assembly 66 is a moving element which allows the cable 24 to be deployed from or wound on the cable reel 22 in proper alignment, i.e. it "flakes" the cable onto the reel 22 in a "level wind" fashion. In order to accomplish this function, it must move back and forth across the width W of the cable reel 22 (FIG. 8).
To obtain such a reciprocating motion, a gear 116 (see FIG. 7) is provided which is driven by the reel plate gear 34. In the preferred embodiment, the gear ratio between plate gear 34 and gear 116 is approximately 2 1/2 to 1 so that one revolution of the gear 34 turns the gear 116 2 1/2 times. Gear 116 drives a gear reducing transmission 118. The gear ratio of the gear reducing transmission 118 is determined by the size of the cable being wound on the reel 22 to provide the proper rate of flaker assembly 66 traverse across the width W of the reel 22 for a given reel speed. As is known to those of skill in the art, to obtain a level wind on reel 22, given a certain reel speed, the cable must be moved across the reel so that the cable is laid down in a level wind fashion across the width of the reel. Thus, the output speed of the gear reducing transmission 118 can be determined by a knowledge of the diameter of the cable being wound on the reel 22. For example, if the cable 24 has a diameter of 1/4 inch, flaker assembly 66 must move 1/4 inch for each rotation of cable reel 22. In the embodiment shown, a fixed ratio transmission 118 is provided which transmission can be changed to accommodate different thickness cables. The reducing transmission 118 could be made variable, however, and preferably continuously variable (e.g., a continuously variable belt drive) to allow greater flexibility for different size cables.
The output of the gear reducing transmission 118, as shown more particularly in FIG. 9, is attached to a coupler 120. The coupler 120 is fastened to the output of the gear reducing transmission 118 by a suitable set screw 122. Coupler 120 is provided with a slotted keyed end 124 which receives a level wind screw camshaft 126 provided with a flat end 128. See FIG. 17. The level wind camshaft 126 has a two-direction continuous thread, including a connected continuous right-hand and left-hand thread. Thus, the left and right hand threads are connected to each other at the ends so that a cam follower can continuously reciprocate back and forth as the camshaft turns in one direction. A pivotal cam follower 130 rotatably mounted in a support block 132 rides on the level wind camshaft 126. Cam follower 130 follows the thread in the camshaft 126 across the length of the camshaft. Upon reaching an end, the cam follower 130 is pivoted by the reversing thread thereby to follow the reversed thread back on the return trip along the camshaft 126. The two positions of the cam follower 130 are shown in bold lines and the phantom lines 130A in FIG. 16. Thus, cam follower 130 moves back and forth along camshaft 126 as the camshaft 126 rotates, providing a reciprocating movement to the support 132. The support 132 is L-shaped and is fastened to a descending (see FIG. 10) flaker eccentric lever arm 134 via a shoulder screw 136 and bushing 138. Lever arm 134 is secured slidably to the shoulder bolt 136 in a slot 140. Lever arm 134 pivots about a pivot point provided by an L-shaped pivot pin 142 which is adjustably fixedly attached to the support frame at 144 via suitable nuts 143. The purpose of providing adjustable pivot pin 142 will be described shortly. At the other end of lever arm 134, a further slot 144 is provided into which another shoulder bolt 146 is received. Shoulder bolt 146 is secured to flaker arm assembly rod 148. A spring 150 is provided between pivot arm 142 and lever arm 134 to provide tension to the lever arm 134. FIG. 10 shows the back cover opened on hinge 11 which provides access to the internal mechanism.
Flaker assembly rod 148 is slidably secured in a first bushing 152 secured to bushing bracket 182 and slidably in a second bushing 154 to provide sufficient support. As shown, the flaker arm assembly 66 includes two supporting rods, 148 and 148A. Rod 148A is also supported in a bushing 157. These two supporting guide rods are necessary to prevent rotation of the flaker arm assembly 66. As shown in FIG. 9, the flaker arm assembly 66 is bent upwardly in a first portion 66A along the perimeter of the reel 22, and then downwardly in a second portion 66B and then across the first portion via a horizontal portion 66C to form an open loop through which cable 24 is guided. The portion 66C clears the first portion by the approximate diameter of the cable 24 (similar to centralizer 68). Rod 148a is welded or otherwise fixed to the bent portion of the flaker arm assembly at 160.
Bushing 152 in which the flaker arm rod 148 slides is illustratively supported on a bracket 182 mounted to the device frame.
The flaker arm 66 achieves its reciprocating motion as follows: transmission 118 rotates the coupling 120 as reel 22 turns. Coupling 120 rotates the level wind camshaft 126. Cam follower 130 follows the threads in the camshaft 126 back and forth across the camshaft 126 as it rotates. This causes the lever arm 134 to pivot about the pivot pin 142 defining arcuate motion Z at end 172 (FIG.8).
As shown particularly in FIG. 17, level wind camshaft 126 is supported both axially and longitudinally by a thrust adjusting bolt 162 which is threaded into a supporting bracket 164. A suitable thrust load is obtained by adjusting the thumb screw 162 and locking with a nut 166. Thumb screw 162 is provided with a bearing hole 168 which receives a cut down bearing surface 170 of the level wind camshaft 126.
As the cam follower 130 follows the threads back and forth across the camshaft 126, lever arm 134 pivots about the pivot pin 142. The slots 140 and 144 in lever arm 134 are provided because the lever arm 134 describes the arcuate path Z. In addition, the slots 140 and 144 are provided for allowing adjustment for the amount of travel of the flaker assembly 66 across the width W of the reel 22. As the end 172 of the lever arm 134 describes a reciprocating arcuate path Z, flaker assembly arm 66 reciprocates across the width W of the reel 22, guiding the cable 24 uniformly back and forth across the reel 22 to accomplish the level wind.
In order to vary the width W for different width reels, the pivot point 142 can be adjusted by rotating it as shown in phantom in FIG. 10. In FIG. 10, the pivot 142 has been shown in phantom in two additional positions 142A and 142B. In position 142A, the width W across which the flaker assembly 166 traverses has been increased because the length B (between the pivot pin and flaker assembly) has been increased with respect to the length A (between the camshaft 126 and the pivot pin). If a lesser width W is required, the pivot pin 142 would be rotated to the position shown in phantom at 142B, in which case the dimension B has been decreased with respect to the dimension A and therefore the amount of traverse W has been decreased. A suitable clearance hole 145 in the lever arm 134 to receive the pivot pin 142 at an angle as shown at 142A and 142B must be provided. Spring 150 provides suitable tension to the lever arm 134 to maintain a fixed pivot point despite the clearance in the hole 145 provided in the lever arm 134 for the pivot pin 142.
Slots 140 and 144 are necessary not only because the ends 172 and 171 of lever arm 134 describe arcuate paths, but also to allow for the variation in pivot point determined by pivot pin 142. If greater adjustment is necessary than can be obtained by the slots 140 and 144, new holes can be drilled in lever arm 134 for the new pivot point.
Although the width W should be adjustable, the starting point (FIG. 8), i.e, the location of the inner surface of flange 22A of reel 22, must not vary. In order to achieve a variable width W but maintain a fixed starting point Y at the inner surface of the flange 22A, pivot point 142 is also adjustable inwardly and outwardly on bracket 164 via two nuts 143. By loosening the nuts 143 and adjusting the distance of the pivot point from the bracket 164, the location of the starting point Y at which the flaker assembly 66 begins its traverse across the reel 22 may be maintained.
Although a mechanical arrangement for achieving reciprocating movement of the flaker assembly 66 has been described, it will be evident to those of skill in the art that electronic control of the flaker assembly 66 can be provided. For example, an encoder coupled to plate gear 34 can provide pulses to indicate revolutions or portions of revolutions of the reel 22. A motor can be provided driving the flaker assembly 66 incrementally or continuously back and forth across the width W of the reel 22 and which receives control signals from the encoder so that for each reel revolution, the flaker assembly 66 moves the desired amount. The flaker assembly 66 may be driven in discrete increments or continuously using this method, as would be known to those of skill in the art. Such an electronic control may be preferable because it would allow easier programming for different reel widths and cable diameters. A microprocessor could be employed to provide control and simplified programming for different reels widths and cable diameters.
Directly below the pinch point 70 of the rollers 62 and 64, a sensing block mounting support 74 is provided which is secured to the device frame with three bolts 190 (See FIGS. 7 and 11). The sensing block mounting support 74 is a relatively thick piece of metal which is necessary to prevent flexing. Coupled to the support block 74 is downwardly depending protective bracket 16 which is also secured to the block 74 with three bolts 192. The support block 74 includes an aperture therein 72 through which cable 24 traverses. At the bottom of the bracket 16, a horizontally disposed bracket 194 is provided. See FIGS. 12 and 15. Bracket 194 is provided with an aperture 196 which has a diameter somewhat greater than the outer diameter of a tubular conduit 76, also through which cable 24 traverses. See FIGS. 12, 15 and 18. A section of metal 200, made of, for example, aluminum, connects the tubular conduit 76 with the support block 74. The metal rod 200 is suitably fastened to the support block 74 via set screws 202 and to conduit 76 via stud screws 77 welded to conduit 76 and fastened to rod 200 with suitable nuts.
Rod 200 incorporates strain gauge elements 204 at a reduced thickness portion 205 of the rod 200 where flexing is designed to occur. The rod 200 and integral strain gauge elements 204 together comprises a strain gauge and may be a type model number N2A-06-T012R-350 manufactured by Micro Measurements of Raleigh N.C. and available from their catalog TC-116-3. The strain gauge elements 204 may comprise, for example, resistance elements coupled into two balanced bridges, as well known to those of skill in the art. The two balanced bridges provide two resistance signals X and Y, each of which have a defined balance point. The balance point can be set by adjusting a variable resistance in each bridge. The adjusted balance point defines a "null" point, to be described later. When the strain increases on the rod 200 due to tension in cable 24, the resistance of the strain gauge elements in the balanced bridges changes, due to the strain, thereby upsetting the balance. This change in the resistance can be detected and is indicative of the amount of strain present in the rod 200 and the tension in the cable. This resistance signal can be used to control the deployment or retrieval of the cable 24.
The way in which the strain is measured is as follows:
Clearance hole 196 (see FIGS. 12, 15 and 18) is provided somewhat larger than the outside diameter of conduit 76 in order to protect the strain gauge rod 200 from breakage due to overbending or shock. The maximum amount that the strain gauge rod 200 can bend is limited by the clearance between the inner circumference of the hole 196 and the outer surface of the tubular conduit 76.
The invention allows for the deployment and retrieval of cable, no matter what direction the vehicle to which the cable deployment and retrieval system is attached moves, because of its use of strain sensing for measuring the amount of tension in the deployed cable 24. In the present invention, the cable 24, as it is being deployed, will contact an edge of the exit hole 206 of the tubular conduit 76. An example of this contact is illustrated at 197 in FIG. 18. When the cable touches the edge of the exit hole 206, it imparts a strain to the conduit 76 and thus to the rod 200, which strain cause a resistance change in strain gauge elements 204. This change in resistance is measurable by the sensitive circuitry coupled to the strain gauge elements 204. The change in resistance is small, corresponding to only millivolt voltage drops, but is measurable by the strain gauge amplifier circuitry, to be described.
The stress in rod 200 is detected by the strain gauge elements 204 provided at the reduced thickness portion 205 of rod 200. If a strain greater than a reference amount of strain is detected, this means that additional cable must be deployed, i.e., there is greater than desired tension in the cable which must be reduced by playing out more cable. Conversely, if an amount of strain below the reference amount is detected, this means the cable is loose, and therefore the cable must be retrieved to increase the amount of tension in the cable.
The present invention provides significant advantages over the prior art. In the prior art, the cable feed drive motor is dependent on wheel rotation, and not on actual vehicle movement. If there is any slippage between the wheels and ground, and the wheels spin, or in trying to stop slip, the signal that would be sent to the cable reel motor would reflect the rotation or non rotation of the wheels, but not the actual movement of the vehicle. This would cause an incorrect amount of cable to be deployed or retracted by the cable reel motor, relative to the actual vehicle movement, resulting in damage to the cable or the robot.
In the present invention, the cable deployment is autonomous and independent of any signals from the drive mechanism of the vehicle, or the vehicle itself, as it senses the need to deploy, retrieve or remain dormant based upon the amount of strain, as detected by the strain gauge, in the cable. Thus, the present invention deploys and retrieves cable without requiring any direct feedback from any mechanism which governs the direction, motion and speed of the vehicle. The present invention uses only the described strain gauge sensor to determine whether the cable should be deployed or retrieved. The system of the invention always seeks to maintain a defined value of tension (or no tension) in the cable. The system allows cable to be deployed and retrieved by sensing the strain in the cable in any direction (an arc of 360°) about exit hole 206 which results from any change in relative direction, motion and speed between the vehicle to which the device is attached and the deployed cable itself. These latter factors are all accounted for by sensing the cable tension and maintaining the desired cable tension.
The desired tension may be a minute quantity, as the strain gauge system of the invention can be adjusted for and is sensitive to very minute quantities of tension.
The arrangement of the exit hole 206 of tubular conduit 76 at a distance from the strain gauge elements 204 enables very small forces applied by cable 24 to be measured. The leverage provided by the conduit 76 and the strain gauge rod 200 magnifies these minute forces present at exit hole 206, increasing the flexing motion at strain gauge elements 204 and thus enabling high sensitivity to the forces applied by cable 24.
The present invention thus provides a much simplified and much more reliable method of deploying cable from a mobile vehicle.
The present invention, using a strain gauge sensor, is completely autonomous, self contained, self regulating and much simpler than prior art systems. It eliminates the need for all speed and direction circuitry or mechanical linkages between the robot or robot drive motor and the cable deployment and retrieval system. It eliminates all gearing, chain drives, encoders and encoder mounts between the rotating drive system and the cable deployment and retrieval system. It is equally effective in deploying and retrieving metallic, fiber optic or dual component cable.
In the present invention, cable 24 will be retracted when the vehicle reverses itself. In addition, due to the action of the strain gauge, it will also retract the cable when it returns directly, in a forward direction, to the monitoring station for the robot. This is because the null point established in the strain gauge circuitry is adjusted to sense the difference in strain induced voltage when the cable is in deployment mode (null point voltage positive) as opposed to when the cable is in retrieval mode, (null point voltage negative). As a result, whether the robot reverses itself or simply turns around to head back to its monitoring station, the 360° sensitivity of the circular strain gauge cable exit hole 206 senses the lower cable strain pressure on its surface in any direction, and will cause the circuitry to go into retrieval mode to pick up cable. The system is such that it can deploy or retract cable regardless of whether the vehicle is moving forward, backward, sideways or pivot turning. The system is completely adaptable to any change in conditions. For example, if the system is retrieving cable but a snag in the cable occurs, or the robot itself drives over the cable, the cable tension will increase, perhaps momentarily, and the system will shift from retrieving cable to playing out cable, as the conditions demand.
FIG. 13 shows a block diagram of the electronic control circuitry of the present invention. The resistance signals from the two balanced bridges of the strain gauge circuit are shown at 250 as X and Y. Generally, one of the strain gauge resistances is disposed in a longitudinal direction along the strain gauge rod 200 and the other resistance for the other balanced bridge is disposed at an angle to the longitudinal direction. The two signals X and Y are supplied to strain gauge amplifiers and filters 252. Amplifier/filters 252 incorporate null adjustments 254 which are coupled to potentiometers 32A and 32B. See FIG. 1. A switch 30 (see FIG. 1) is provided which can be switched between "null" and "run" positions. Prior to use, the switch is flipped to the null position, at which a null reference level is determined when the cable 24 touches the bottom inner edge of the tubular conduit 76 with the desired reference tension. The null point determines the reference point above which point greater strain is detected and below which point a lesser strain is detected. For example, if the cable 24 presses against the tubular conduit 76 with greater force, a greater strain will be detected by the strain gauge elements 204. If the cable presses against the conduit 76 with a lesser force, or does not touch it at all, a lesser or no strain will be detected by the strain gauge elements 204. Once the null point has been set, the switch 30 is placed back into the "run" position, in which case the device is ready for use.
The outputs of the strain gauge amplifier/filters 254 are fed to a summing amplifier 256 which generate the absolute value of each of the input signals and adds the signals together to produce a force magnitude signal 258. The output of the summing amplifier 256 is provided to a force threshold amplifier 260, preferably at which a threshold value above the null point is set to provide an amount of tension, as minute as necessary, in the cable at all times. Preferably the system control circuitry is set up so that the system is biased toward take-up, i.e., the system is biased so that the reel 22 and rollers 62 and 64 (see below) will turn to take-up cable 24 whenever the magnitude of the force detected is below the threshold value (but above null) set in the force threshold amplifier 260. Thus, if the force threshold is set slightly above the null point, as long as the tension detected is below the force threshold but above the null point, the rollers 62 and 64 and reel 22 will turn to take-up cable and thus maintain the threshold tension in the cable at exit hole 206. The roller drive motor 84 will stop when the threshold is reached. The reel drive motor will also stop when the threshold is reached. As explained below, the reel motor 44 maintains a preset tension in cable 24 between the reel 22 and the roller 62 and 64 during take-up of the cable.
The output of the force threshold amplifier 200 is provided to under/over comparator 262 and to an error amplifier 264. The comparator 262 output is coupled to a current regulator 266 whose output is coupled to a reel motor driver 268 which controls the reel motor 44. The reel motor 44 provides current feedback via line 270 to the current regulator 266 to maintain the reel motor speed at the required rate.
Preferably, the reel motor 44 is operated such that it turns in only one direction, i.e., so as to retrieve cable 24. When cable is being retrieved, the reel motor 44 is turned on by the current regulator 266 in response to the threshold amplifier 260 so long as the tension in the cable 24 is below the force threshold set by the force threshold amplifier 260. The reel motor 44 will seek to maintain a degree of tension in cable 24 between the reel 22 and the roller 62 and 64 during take-up of the cable.
To deploy cable, the reel motor is turned off and the turning drive rollers 62 and 64 only pull cable 24 off the reel 24. The reel 22 will, of course, turn against the braking action provided by the transmissions 46, gear 116 and transmission 118. This braking action will prevent overshoot of the reel when the drive rollers stop or reverse direction.
The output of the force threshold amplifier 260 is also fed to error amplifier 264. The error amplifier 264 provides a positive or negative error signal, dependent on the tension in the cable 24, which is fed to a pulse width modulator speed regulator 272 which drives a roller motor driver circuit 274. Driver 274, in turn, drives the roller motor 84. Current feedback 276 and voltage feedback 278 are provided. The voltage feedback 278 provides stability and damps out oscillations. The current feedback 276 maintains the speed of the roller drive motor 84 at the required rate, dependent on the sensed strain in the cable at the exit hole 206. If the strain increases, the sensed roller drive motor current will increase, thereby causing the speed regulator 272 to drive the roller drive motor faster to pay out cable until the tension in the cable is driven back to the force threshold. Once the force threshold is achieved, the speed regulator maintains the current drawn by the roller motor at the required level to maintain the threshold.
Conversely, if the strain in the cable 24 at exit hole 206 decreases as sensed by the strain gauge, the current regulator 266 will cause the reel motor 44 to turn on to take-up cable 24. The current feedback 270 will regulate the current regulator 266 so as to drive the reel motor against a defined torque which is created by the tension in the cable between the reel 22 and the drive rollers 62 and 64. The current regulator maintains a preset tension in the cable between these points to prevent any slack between these points in the cable. At the same time, the error amplifier 264 will determine that the tension is below the force threshold, and it will reverse the roller motor 84 to cause it also to take-up cable. The speed at which the roller motor 84 turns will be determined by the current feedback circuit 276. The desired roller motor drive current will be that current which causes the tension in the cable 24 to increase toward and maintain the force threshold amount of tension.
As is evident from the above, in the preferred embodiment, the spool motor turns in only one direction so as to take-up cable. The roller motor 84 must be able to turn in both directions so as to take-up cable and so as to play out cable. As would be obvious to persons of skill in the art, the invention could be operated so that the reel motor 44 also turns in both directions. In the preferred embodiment, the invention uses DC motors for the roller and reel motors, but as would be obvious to persons of skill in the art, other type motors, for example, AC motors, could be used with suitable control circuitry. For example, AC motors may be used if power is obtained remotely for the device from an AC network, or AC motors could be used even if batteries supply power if suitable DC to AC conversion circuitry is employed, as known to those of skill in the art. In the preferred embodiment of the invention, the reel motor 44 and drive roller motor 84 are reversible, variable speed motors (although motor 44 is operated in only one direction in the preferred embodiment).
Additionally, as described, certain purely mechanical mechanisms described herein, e.g. the level wind flaker assembly driving mechanism, could be substituted by electronic circuits receiving signals proportional to reel 22 speed and an electric motor controlled by these circuits so as to traverse the required distance for each reel revolution.
Although the present invention has been described in relation to particular embodiments thereof, many other variations and modifications and other uses will become apparent to those skilled in the art. Therefore, the present invention should be limited not by the specific disclosure herein, but only by the appended claims. | A system for a mobile vehicle such as a remotely controlled robot, for deploying and retrieving cable into the environment external to the vehicle. The system includes a frame, a cable reel mounting device for a cable storage reel having cable wound thereon for rotatable motion. A rotatable electric/fiber optic joint is provided for coupling one end of the cable to the vehicle. The device has a mechanism for feeding the cable on and off the cable storage reel and for guiding the unwound cable from the vehicle. A sensor senses the tension in the cable in any direction in an arc of 360° as the cable exits a cable exit opening. An electronic circuit receives a signal from the sensor related to the tension in the cable for controlling the feeding of cable so as to maintain a preset tension or no tension in the cable. Preferably, the tension sensor is a strain gauge. The system can be attached to any mobile vehicle, e.g. a robot, requiring a cable for control, power and/or communication. It can allow two way transmission of voice, data, video, power and commands through all speeds, directions, motions and turns, including pivot turns, of the vehicle. The system can be used for deploying and retracting fiber optic, metallic or combination cables. | 7 |
CROSS-REFERENCE TO RELATED U.S. APPLICATIONS
[0001] Not applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not applicable.
NAMES OF PARTIES TO A JOINT RESEARCH AGREEMENT
[0003] Not applicable.
REFERENCE TO AN APPENDIX SUBMITTED ON COMPACT DISC
[0004] Not applicable.
BACKGROUND OF THE INVENTION
[0005] 1. Field of the Invention
[0006] The present invention concerns a method and device for dynamically treading fruit or even vegetables.
[0007] In particular, the invention is advantageously applicable to the bursting of grapes, beginning right with the crop of de-stemmed grapes or in whole bunches, for the elaboration of white, rosé or red wines.
[0008] 2. Description of Related Art Including Information Disclosed Under 37 CFR 1.97 and 37 CFR 1.98.
[0009] In a vinification process at the end of which the grapes is transformed into wine, treading is the operation which consists of pressing or crushing the grapes to burst them open and to release their components in order to obtain a grape must which is in contact with the skins.
[0010] The invention is also applicable to the bursting of apples for cider production or of other fruit or even vegetables, for use in an ulterior process of producing juices or concentrates of these.
[0011] The objective is to achieve, through the present innovation, the bursting of fruit or even of certain vegetables, in order to increase exchanges between the liquid and solid phases within the whole grape must obtained in this manner which will be reused later, for instance in a maceration process.
[0012] With respect to vinification, the treading method and machine according to the invention consist of bursting the grape berries to obtain a grape must then intended for maceration, without crushing neither the pips nor the possibly present grape stalks or other plant debris (leaves, stems, . . . ), the crushing of which could release and diffuse substances undesirable for good vinification (release of oils or polyphenolic compounds in uncontrolled quantities).
[0013] Especially on the oenological level, what is sought is the largest contact area possible between the juice and the skin of the grapes, during the maceration process.
[0014] Crushing the grape berries will have these effects:
establishing contact with the grape must, of the yeast present on the outside surface of the skin of the berries, in the case of spontaneous vinification; good maceration or exchange by dissolution of polyphenols (coloring matter, tannins, . . . ) residing primarily on the inner surface of the grape skin, during red wine production; reducing the risk of having residual reducing sugars at the end of alcoholic fermentation.
[0018] This process of obtaining fermentative must from grapes can also be applied to other fruit containing seeds or pits, or even to vegetables.
[0019] In order to obtain a quality grape must and to extract, during the maceration phase, the maximum of polyphenolic compounds, it is necessary that the following conditions be met:
all berries without exception grape must be crushed; the grape berries must not only be crushed to release the juice and seeds, but the skin grape must also be completely spread out so as to present the largest exchange surfaces possible for both its sides, inside and outside; if the skin folds over itself after bursting, the grape juice must be able to infiltrate and circulate freely over the entire surface of the inside and outside of the skin It is in effect necessary to extract from the skin surface all compounds that are indispensable to vinification such as yeast and polyphenols (coloring matter, tannins, . . . ); under no circumstances must the pips or pieces of stalks or vegetable debris be crushed or their integrity is impaired in order to avoid the release of substances that are undesirable for the quality of the grape must.
[0024] Mechanical wine-presses have been available commercially for many years. They have superseded the age-old operation of treading by hand or foot which consisted of crushing, between the fingers or with the feet, the grape bunches brought in by manual harvest. For the most part they are being built, based on the principle of crushing berries between two more or less notched rolls rotating in opposite directions to each other. The differences between the solutions proposed by the manufacturers have to do with the geometry of the rolls or their notching, but the principle remains basically the same.
[0025] The rolls are made of food materials (rubber, polyurethane) and particularly not of hard materials (steel, stainless steel for example) to limit the effects of crushing seeds, plant or other organic debris.
[0026] Most of these systems allow adjusting the distance between the rolls, to increase or reduce the crushing of the grape berries, but also to adapt to the size of the grapes (which varies for different vine-stocks) or to the flow of fruit to be processed.
[0027] In consideration of their principle of mechanical crushing of the berries (rolling mill system, calendering), these wine-presses do indeed let these berries be crushed in order to release the juice, pulp and seeds But their major disadvantage remains that the berry opens only over a small surface, sufficient to evacuate its content through the wine-press. In effect, by passing through the wine-press the berry is progressively crushed. The pressure thereby generated inside the fruit makes the skin split open, generally where it is attached to the pedicel. After the exit of the grape components and the passage through the wine-press, the grape skin collapses on itself and, during the maceration process, limits the exchange surface between the juice and the inside wall of the berry skin This fact induces a longer maceration process (in order to extract as much as possible of the active components located at the inside of the skin turned back on itself), and of less quality in oenological terms.
[0028] Considering the design of these wine-presses, a fixed distance separates the two rolls of the wine-press during the treading. This distance may or may not be adjustable to adapt it to the average size of the berries and the intensity of the desired treading. So it is this distance which defines the minimum size of the grape that will be pressed between the rolls. Grapes and objects of smaller size than the distance between the rolls can therefore pass undamaged, while all other objects are being systematically pressed between the rolls.
[0029] Now, in a grape harvest, the size of the grapes is not constant, but depends on the vine-plant, and also on the degree of ripeness of the grapes. Thus, there will always be a not insignificant proportion of grapes with a diameter smaller than the distance between the two rolls, grapes which will therefore not be crushed and which will be unable to participate efficiently in the maceration process. Therefore, if one wants to subject almost all grapes to treading, one is obliged to reduce the distance between the rolls, at the cost of having to risk crushing or breaking down, in their entirety, seeds or plant material such as grape stalks.
[0030] In this case, the disadvantage of this type of equipment is that the output is linked to the distance between the rolls, for a given roll length. A significant increase of this output can therefore lead to degrading the treading quality.
[0031] On the other hand, one knows, for example in the elaboration of fruit juices, how to achieve the separation of liquid and solid matters of fruit, using centrifugation methods and machines.
[0032] However, for the application of these methods and machines, it is indispensable to first perform a grinding operation of all parts of the fruit, consequently including fruit pits or seeds, so as to then be able to extract the liquid parts of the grape must resulting from this grinding operation, by centrifugation, through a filter rotating at high speed.
[0033] In the FR-1.595.035 document a grape treader is described. According to this document, crushing of the berries is achieved by using a rotary beater with radial blades, so that this crushing operation is obtained through the beating action exerted directly on the berries by said blades. The rotary beater is not used to impart any kinetic energy to the berries but to make them burst through successive strokes by these blades, along a tunnel. There is no effect of centrifugal acceleration in a single level of fruit.
[0034] In the U.S. Pat. No. 4,957,043 document, a fruit disintegration device is described which includes a chamber with an inlet opening and an outfeed canal, this chamber containing a drive rotor to accelerate the speed of the fruit around a circular trajectory and then to discharge the fruit through said tangential outfeed channel into a separation chamber where the fruit is crushed on a fixed wall away from the rotor.
[0035] According to this document, the fruit is poured into a chamber in which a vertical rotor consisting of a part with a U profile is mounted so that it rotates around a horizontal axis. The fruit dumped by an infeed device is introduced between the longitudinal blades of this U-shaped rotor, and, under the effect of centrifugal force the fruit is ejected one by one into a channel leading to a separation chamber in which a fixed wall is installed facing the exit of the channel and against which the fruit propelled by kinetic energy is crushed. It would seem that a single fruit is ejected into the connecting channel whenever one of the open ends of the rotor appears opposite the entrance of said channel
[0036] Such a device cannot be contemplated, nor is it applicable, on a practical level, to the treading of small fruit such as grapes or other berries, if one considers that the passage of the latter, one by one, from the chamber of acquisition of kinetic energy towards the separation chamber over a connecting channel would require an excessively long time, which is completely incompatible with the treading of grapes coming in from the harvest. On the other hand, a portion of the kinetic energy imparted by the rotor is dissipated during the passage of the fruit through the connecting channel The performance of this device would be clearly insufficient for applying it to grape treading. Finally, the fruit finds itself projected at a right angle to the fixed crushing plane, since such a process does not permit a development of the fruit skin which is indispensable for maceration in the wine-making process. This orthogonal projection of the grapes leads in fact to grapes crushing on themselves to release their components with, as a result, an effect that is identical to that obtained by traditional treading by means of machines with rollers, which is to say the folding of the grape skin on itself instead of being developed in the grape must.
[0037] As previously indicated, the invention is essentially and advantageously usable for achieving the separation of the liquid and solid phases of juicy fruit, in particular of fruit in the form of berries, such as grapes. However, we do not exclude the application of the invention to treading of certain vegetables, by means of adaptations of the treaders, depending on the nature of the vegetables to be processed. Under these conditions, the word “fruit”, or even the word “berry” should be considered as equivalent to the term “vegetable” in the description which follows and in the claims.
[0038] The aim of the present invention is precisely to remedy the aforementioned disadvantages of treading devices with rollers and its goal is to make available to professionals interested in the utilization of this type of equipment, a dynamic wine-press allowing complete crushing of the fruit, berries or vegetables passing through it, and to release their liquid and solid matter, in order to constitute a high-quality grape must, as a preamble to ulterior operations of maceration or fermentation.
BRIEF SUMMARY OF THE INVENTION
[0039] According to the invention, this objective has been achieved, thanks to:
[0040] - A process according to which the fruit is dumped into a treading enclosure and received on a rotary ejector, the fruit being endowed with kinetic energy under the effect of the centrifugal force communicated by the rotation of said rotary ejector and projected against a fixed bursting wall, at a determined speed so that the contact of the fruit with said fixed bursting wall occurs in the form of a shock or impact causing the bursting of the fruit, this process being remarkable in that the fruit is received on a rotary ejector mounted so it rotates around a vertical axis, and is projected, under the effect of the centrifugal force resulting from the rotation of this rotary ejector, against a fixed bursting wall surrounding said rotary ejector or positioned opposite the peripheral edge of projection of the latter.
A dynamic wine-press including a treading enclosure featuring, looking in the direction of the trajectory of the fruit in the treader, an upstream opening for dumping the fruit, and a downstream opening for evacuating the grape must resulting from the treading of the fruit, featuring also a rotary ejector capable of imparting kinetic energy to the fruit transported on said rotary ejector, and to project said fruit against a bursting wall, this treader being remarkable in that the rotary ejector is mounted in rotation around a vertical axis, and a fixed bursting wall is positioned around said rotary ejector or facing the peripheral edge of projection of the latter, the rotation of which causes the fruit to be projected, under the effect of the centrifugal force imparted to it by this rotation, against said fixed bursting wall, in the form of shocks or impacts provoking the bursting of the fruit.
[0042] According to another characteristic arrangement, the fruit is projected tangentially to the internal surface of impact of the fixed bursting wall.
[0043] According to a preferred embodiment, the fruit is projected tangentially to the curved surface of the fixed bursting wall which is cylindrical, tapered, or polygonal.
[0044] According to an advantageous embodiment, the rotary ejector is constituted by a rotating plate positioned horizontally, preferably circular and/or flat.
[0045] According to a preferred embodiment, the ejection edge of the fixed bursting wall is circular.
[0046] According to another preferred embodiment, the fixed bursting wall is rigid.
[0047] According to another characteristic arrangement, the upper surface of the rotary plate is provided with angularly spaced guiding fins and extending from the central part of the plate to the periphery of the latter.
[0048] Advantageously, said guiding fins have a curved (concave) shape.
[0049] According to another implementation, the rotary ejector is constituted by an inverted truncated cone.
[0050] According to another characteristic arrangement, the internal wall of the truncated cone is equipped with angularly spaced guiding fins extending from the low part of said truncated cone to the peripheral edge of projection of the latter.
[0051] According to another characteristic arrangement, the fixed bursting wall positioned around the rotary plate or facing the peripheral edge of projection of the inverted truncated cone presents a truncated conical shape.
[0052] According to another characteristic arrangement, a space is provided between the peripheral edge of projection of the rotary ejector and the fixed crushing wall.
[0053] According to an advantageous embodiment, a circular skirt is positioned below and in the continuity of the fixed bursting wall, this circular skirt being equipped on the inside with angularly spaced braking fins.
[0054] According to another characteristic arrangement of the treading method and the dynamic wine-press of the invention, means that are known as such make it possible to regulate the kinetic energy or the ejection speed of the fruit exiting the rotary ejector so as to allow the bursting of the fruit, but without bursting the seeds or other plant debris harder than the constituents of said fruit being treaded.
[0055] The method and the dynamic treader according to the invention provide in particular the following advantages:
bursting the berries without crushing the seeds or the stalks or other plant debris which, when crushed, could release undesirable substances and diffuse them in the liquid phase; obtention of a quality grape must that is free of undesirable substances; bursting of all berries dumped into the treader, regardless of their size; obtention of a grape must in which the juice is in contact, under optimal conditions, with the internal and exterior surfaces of the skin of the fruit. a strong flow with excellent yield.
BRIEF DESCRIPTION OF THE DRAWINGS
[0061] The aims, characteristics and advantages mentioned above and still more will become clearer from the description below and the attached drawings in which:
[0062] FIG. 1 is a perspective view of a first example of embodiment of the treader;
[0063] FIG. 2 is a perspective view showing the treader in opened position for cleaning the centrifugal rotary plate and the treading chamber;
[0064] FIG. 3 is an axial section view of the treader;
[0065] FIG. 4 is a perspective view of the rotary plate;
[0066] FIG. 5 is an analog view to FIG. 3 showing the treader in operation;
[0067] FIG. 6 is a plan view and section view along line 6 - 6 of FIG. 5 ;
[0068] FIG. 7 is an analog view to FIG. 3 , viewed perpendicularly, illustrating the treader in operation;
[0069] FIG. 8 is a plain view and section view along line 8 - 8 of FIG. 7 ;
[0070] FIG. 9 is a schematic view of an example of embodiment of the treader with the rotary ejector in the shape of a truncated cone.
[0071] Reference is made to said drawings to describe interesting, although by no means limiting examples of implementation of the treading method and of embodiment of the dynamic treader according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0072] In the description below as well as in the claims the terms “upstream” and “ downstream” refer to the direction of passage of the fruit and grape must through the treader.
[0073] According to the invention, separation of liquid and solid matters of the fruit is achieved through the transfer of kinetic energy between said fruit and a fixed bursting wall.
[0074] The dynamic treader according to the invention includes a treading enclosure 11 , featuring, while looking in the direction of travel of fruit in the treader, an upstream infeed opening 13 for the fruit and a downstream outfeed opening 14 of the grape must resulting from the treading of the fruit, featuring also a rotary ejector 12 , 12 ′ for imparting kinetic energy to the fruit dumped into said treading enclosure 11 , and for projecting said fruit against a fixed bursting wall 10 , 10 ′, and, according to a first characteristic arrangement, this treader is remarkable in that the rotary ejector is mounted so it rotates around a vertical axis 18 and a fixed bursting wall is positioned around said rotary ejector or facing the peripheral edge of projection of the latter, the rotation of which enables the fruit to be projected, under the effect of the centrifugal force imparted to it by this rotation, against said fixed bursting wall, in the form of shocks or impacts causing the bursting of the fruit.
[0075] According to the example of embodiment shown in FIGS. 1 to 8 , the dynamic treader for the bursting of fruit, in particular of grapes, includes a treading enclosure 11 featuring an upstream infeed opening 13 for the fruit and a downstream opening 14 for the evacuation of the grape must resulting from the treading of said fruit, while looking in the direction of the travel of the fruit inside the treader.
[0076] Inside the treading enclosure 11 is mounted a rotary ejector 12 capable of imparting kinetic energy to the fruit F dumped on said rotary ejector and of projecting it against the fixed bursting wall 10 positioned around said rotary ejector 12 .
[0077] According to this implementation, the rotary ejector is constituted by a rotating plate 12 , onto which the fruit F falls, for example in the central part, dumped into the treading enclosure 11 . This plate 12 is mounted so it rotates around a vertical axis 18 and it is positioned horizontally. It presents, preferably, a circular shape. Means of propulsion known as such permit the motorized drive in rotation of the ejection plate 12 at high speed, this speed being determined and adjustable to allow projecting the fruit, under the effect of kinetic energy imparted to it and of centrifugal force, against the bursting wall 10 positioned around the rotary plate. In this manner, contact of fruit F with said fixed bursting wall 10 takes place in the form of shocks or impacts leading to its bursting, without however causing the seeds or other undesirable components to burst.
[0078] The ejection plate 12 may have a flat shape and it is, for example, installed in the bottom of the treading enclosure.
[0079] A ring-shaped space is provided between the ejection edge 12 b of the rotating plate 12 and the bursting wall 10 positioned around the latter. This ring-shaped space may have a width in the order of 30 to 40 mm, this dimension being given only as a non-limiting example.
[0080] The ejection plate 12 may be advantageously equipped, on its upper face, with a plurality of angularly spaced guide fins 15 extending from the central part 12 a of said plate to its periphery. Advantageously these guide fins 15 have a curved concave shape, looking in the direction of rotation of plate 12 . They may be of various height, depending on the dimensions of the treader, they themselves being dependent on the nature of the produce to be processed, for example a height in the order of 60 mm for treading of grapes with the berries presenting a diameter between 5 and 30 mm, depending on the vine-plants and their maturity.
[0081] The fins 15 may be made of rigid materials, of stainless steel for example, or of elastic or viscoelastic materials, for example polyurethane or food-grade rubber. These fins may be formed directly of the same material as the ejector properly speaking, or they may be attached on the latter.
[0082] According to the example of embodiment shown in FIG. 9 , the rotary ejector presents the shape of an inverted truncated cone 12 ′. The lateral wall of this truncated cone may present an angle of inclination A between 0° and 90° and, for example an angle of inclination in the order of 30°. The upper edge 12 b′ of the great basis of this inverted truncated cone constitutes the peripheral edge of ejection of this rotary ejector 12 ′.
[0083] A fixed bursting wall 10 ′ is positioned around the upper ejection edge 12 b′ of the inverted truncated cone 12 ′. A ring-shaped space E′ is provided between said upper ejection edge 12 b′ and said fixed bursting wall 10 ′. The drive in rotation of the rotary ejector (plate 12 or truncated cone 12 ′) may be provided, in a manner known as such, by any appropriate motorization.
[0084] For example, as far as the ejection plate 12 is concerned, these means may include an electrical motor 16 and an appropriate transmission system 17 for the rotary drive of a vertical shaft 18 on which said plate may be attached, at a speed which may be constant or adjustable by means of any appropriate speed regulating system, preferably in a range between 800 and 2000 rpm.
[0085] The fixed bursting wall 10 is positioned around the rotary plate 12 . This wall may be constituted by the lateral wall of the treader enclosure 11 . Advantageously, this wall 10 is in the form of a truncated cone the upper part of which is closed by a horizontal wall 19 in which the upper opening 13 for infeed of the fruit is made and which is positioned upstream of plate 12 , preferably near its central part 12 a. This opening communicates with the outfeed opening 20 of a hopper 21 or other feeding apparatus.
[0086] According to an advantageous characteristic disposition of the invention, the fruit F is projected tangentially to the impact surface of the bursting wall 10 or 10 ′.
[0087] The fixed bursting wall 10 or 10 ′ and more exactly the inside impact surface of this wall against which the fruit F is projected may have a circular, tapered or polygonal shape (constituted by a plurality of facets).
[0088] The frame 22 of the treader may be constituted by an upper portion 22 a which is integral with the walls of the treader enclosure 11 , and by a lower portion 22 b on which said upper portion 22 a is mounted, with a tipping capability, by means of any appropriate system of articulation. In this way, it is possible to swing the upper portion 22 a around in order to open the treader and thus to have access to the rotary plate and the treading chamber for cleaning and maintenance purposes.
[0089] The rotary plate 12 is positioned above the large base of the conical bursting wall 10 , which delimits the outfeed opening 14 . A circular skirt 23 is positioned below and in the continuity of the fixed bursting wall 10 . This circular skirt is equipped, on the inside, in the low part, with regularly spaced fins 24 . The lower end of the circular skirt 23 delimits an opening that can be connected to a vat or tank for ulterior processing of said grape must, depending on the nature of the latter and the products to be elaborated from it.
[0090] The operation of the dynamic treader according to the invention can easily be understood by referring, for example, to the preferred and advantageous embodiment shown in FIGS. 1 to 8 . The grape berries or the fruit F are brought up in a receiving trough connected at its end to the infeed opening of the treader via an infeed device constituted by the hopper 21 .
[0091] At the exit from the hopper 21 , the grape berries which have a relative speed of almost zero are dumped onto the rotary plate 12 at the level of its central part 12 a . High speed rotation imparts to the berries progressive acceleration generated by the centrifugal force which projects them towards the outer edge of said plate. They acquire, in this way, as they leave the plate 12 , a speed V which is a function of the rotary speed of the plate, and hence kinetic energy which is a function of this same speed V and the mass of the berries or fruit. When they leave the plate 12 , under the effect of the centrifugal force, the berries or fruit possess the kinetic energy necessary to burst open upon contact with the fixed wall 10 .
[0092] The liquid and solid phases containing the different constituents of the grape berries having thus been separated flow down by gravity along said fixed wall 10 .
[0093] The rotational speed of the plate 12 is preferably constant, but should this be necessary, it can be adapted to other types of fruit or berries, and/or regulated depending on the desired output, and the level of ripeness of the fruit.
[0094] After their separation resulting from their being projected at high speed against the bursting wall 10 , the constituents of the berries are slowed down by friction on said wall. They then flow by simple gravity along the circular skirt 23 positioned below and in continuation of the bursting wall 10 , while the fins 24 positioned on the inside, in the low part of said circular skirt 23 serve to definitely halt the rotation of the separated constituents and to channel their flow in a vertical orientation in the axis of the treader.
[0095] As indicated before, the treader may, according to a preferred embodiment of the innovation process, feature a device for varying the rotational speed of the rotary ejector (plate 12 or inverted truncated cone 12 ′) in order to adapt this speed to the fruit to be processed, to its degree of ripeness, or even to the product flow passing through the treader. Different shapes of rotors (rotary plates) or of acceleration blade profiles may be used, depending on the intensity of treading desired or on the type of product to be processed.
[0096] Operation of the embodiment shown in FIG. 9 is essentially identical to that of the device shown in FIGS. 1 to 8 which has just been described.
[0097] In this case, the berries dumped into the truncated ejector 12 ′ are propelled in the direction of the lateral wall of the ejector and are drawn in an upward movement in the direction of the peripheral edge of projection 12 b′ , under the effect of the centrifugal force and find themselves ejected against the fixed wall 10 ′ positioned opposite said peripheral edge of projection, which leads to their bursting.
[0098] Preferably, the internal wall of the truncated ejector is provided with angularly spaced guide fins which extend from the low part 12 a′ to the peripheral edge of projection 12 b′ of said truncated ejector. | Dynamic crusher for treading fruit, particularly grapes, with a treading chamber having, when considering the direction of the path followed by the fruit in the crusher, an upstream fruit-introduction opening, a downstream discharge opening for discharging the must that results from the treading, a rotary ejector that allows kinetic energy to be imparted to the fruit introduced into the treading chamber, and allows the fruit to be cast against a fixed fruit-bursting wall, wherein the rotary ejector is mounted such that it can rotate about a vertical axis and a fixed fruit-bursting wall is positioned around the rotary ejector or facing the peripheral edge thereof against which fruit is cast, rotation of which allows the fruit to be cast, under the effect of centrifugal force, against the fixed fruit-bursting wall, causing the fruit to burst. A method for dynamically treading fruit using such a crusher is also disclosed. | 1 |
FIELD OF THE INVENTION
An improved and efficient process for the preparation of 2-[3-cyano-4-(2-methylpropoxy)phenyl]-4-methylthiazole-5-carboxylic acid (febuxostat) that is substantially free from amide by-product is provided.
BACKGROUND OF THE INVENTION
Febuxostat is a non-purine xanthine oxidase inhibitor known from U.S. Pat. No. 5,614,520. It is chemically designated as 2-[3-cyano-4-(2-methylpropoxy)phenyl]-4-methylthiazole-5-carboxylic acid having the structure as represented by Formula I.
Febuxostat is marketed in the United States under the brand name Uloric® and in Europe under the brand name Adenuric® for the chronic management of hyperuricemia in patients with gout. It works by non-competitively blocking the channel leading to the active site on xanthine oxidase. Xanthine oxidase is needed to successively oxidate both hypoxanthine and xanthine to uric acid. Hence, febuxostat inhibits xanthine oxidase, therefore, reducing production of uric acid.
Processes for the preparation of febuxostat and intermediates thereof are disclosed in U.S. Pat. No. 5,614,520; Japanese Patent Nos. JP 2834971; JP 3202607; JP 2706037, JP 10139770 and JP 3169735.
U.S. Pat. No. 5,614,520 discloses preparation of febuxostat by hydrolysis of its corresponding ester using sodium hydroxide. It has been observed that when hydrolysis is carried out with sodium hydroxide, the cyano moiety also gets hydrolyzed along with ester leading to the generation of amide by-product, a very potential impurity in febuxostat API. The structure of the amide by-product is as shown below:
JP 2834971 describes preparation of febuxostat ester via formylation of a 4-hydroxyphenyl substituted thiazole intermediate in the presence of an organic acid, preferably with trifluoroacetic acid, and JP 3202607 describes preparation of febuxostat ester via formylation of a 4-hydroxyphenyl substituted thiazole intermediate in the presence of polyphosphoric acid. The work-up procedure for the isolation of product is tedious requiring a number of steps.
The processes described in U.S. Pat. No. 5,614,520, JP 2706037, JP 10139770 and JP 3169735 involve the use of toxic metal cyanides for the preparation of febuxostat. The use of metal cyanides is hazardous to health and is not recommended for an industrial scale preparation.
Accordingly, there is a need for a process to synthesize febuxostat that is substantially free of the amide by-product. The process should avoid long work-up procedures and allow easy isolation of final product and also avoid the use of toxic metal cyanides.
SUMMARY OF THE INVENTION
The present invention provides an improved and efficient manufacturing method of 2-[3-cyano-4-(2-methylpropoxy)phenyl]-4-methylthiazole-5-carboxylic acid (febuxostat) that addresses many of the drawbacks of the prior art processes. Thus, it is suitable for commercial-scale production. The process of the present invention does not involve the use of hazardous cyanides. Also, the process makes use of methanesulfonic acid for formylation, which allows easy isolation of the formylated product. In addition, the febuxostat so synthesized is substantially free from the amide by-product. The control of the formation of amide by-product was a challenge. The inventors of this patent application found that this amide by-product could be controlled by selecting appropriate base and solvent for the hydrolysis step.
Accordingly, the first aspect of the present invention provides a process for the preparation of febuxostat of Formula I
comprising the steps of:
(i) reacting 4-hydroxy thiobenzamide of Formula II
with a compound of Formula III (wherein X is halogen and R is alkyl or arylalkyl)
to give a compound of Formula IV;
(ii) formylation of the compound of Formula IV with hexamethylene tetramine in presence of an acid to give a compound of Formula V;
(iii) reaction of the compound of Formula V with hydroxylamine hydrochloride to give a compound of Formula VI;
(iv) alkylation of the compound of Formula VI with isobutyl halide of Formula VII (wherein X is halogen)
to give a compound Formula VIII; and
(v) hydrolysis of the compound of Formula VIII with a base selected from oxide and hydroxide of barium to give febuxostat of Formula I.
In a second aspect, the present invention provides a process for the preparation of febuxostat of Formula I
comprising hydrolysis of the compound of Formula VIII (wherein R is ethyl)
with barium hydroxide octahydrate.
Other objects, features, advantages and aspects of the present invention will become apparent to those of ordinary skill in the art from the following detailed description.
DETAILED DESCRIPTION OF THE INVENTION
Definitions
The following definitions apply to terms as used herein:
The term “alkyl”, unless otherwise specified, refers to a monoradical branched or unbranched saturated hydrocarbon chain having from 1 to 20 carbon atoms. This term can be exemplified by groups such as methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, sec-butyl, t-butyl, n-pentyl, isopentyl, neopentyl, n-hexyl, n-decyl, tetradecyl, and the like.
The term “arylalkyl”, unless otherwise specified, refers to alkyl-aryl linked through an alkyl portion (wherein alkyl is as defined above) and the alkyl portion contains 1-6 carbon atoms and aryl is as defined below. Examples of arylalkyl groups include benzyl, ethylphenyl, propylphenyl, naphthylmethyl, and the like.
The term “halogen” or “halo” or “halide” refers to fluorine, chlorine, bromine or iodine.
The term “substantially free from amide by-product” refers to limit of amide by-product in febuxostat of Formula I as less than or equal to 0.07%.
Various embodiments and variants of the present invention are described hereinafter.
The reaction of a compound of Formula II with a compound of Formula III (wherein X is halo and R is alkyl or arylalkyl) to give a compound of Formula IV can be carried out in a solvent, for example, ethanol, methanol, denatured spirit (DNS), 2-propanol, 2-methyl-2-propanol or the mixture(s) thereof, at a temperature of about 0° C. to about 250° C. for about 15 minutes to about several days depending on type of reactant and solvent selected.
In a particular embodiment, the reaction of compound of Formula II with a compound of Formula III (wherein X is Cl and R is ethyl) to give a compound of Formula IV is carried out in denatured spirit (DNS) at a temperature of about 60° C. to about 65° C. for a time period of about 2.5 hours.
The formylation of the compound of Formula IV with hexamethylene tetramine to give a compound of Formula V can be carried out in presence of an acid selected from methanesulfonic acid, trifluoroacetic acid, polyphosphoric acid, ethane sulphonic acid, trifluoromethane sulphonic acid, p-toluene sulphonic acid, acetic acid, formic acid, propionic acid, or mixture(s) thereof, optionally in the presence of a solvent, for example, benzene, toluene, dichloromethane, dichloroethane, chloroform, carbon tetrachloride, ethyl acetate, methanol, ethanol, propanol, 2-propanol, diethylether, tetrahydrofuran, dioxane, 1,2-dimethoxyethane, dimethylformamide, dimethyl sulfoxide, or mixture(s) thereof, at a temperature of about 0° C. to about 250° C. for about 15 minutes to about several days depending on type of reactant, solvent and acid selected. After completion of the reaction, the reaction mixture may be cooled. The isolation of product can be carried out by addition of a solvent, for example, water and then optional extraction in a different solvent, for example, ethyl acetate. In a particular embodiment, the formylation of compound of Formula IV (wherein R is ethyl) is carried out with methanesulfonic acid at a temperature of about 20° C. to about 100° C. for a time period of about 10 hours to about 14 hours.
In a particular embodiment, the formylation of compound of Formula IV is carried out by adding hexamethylene tetramine to a solution of hydroxy phenyl thiazole ethyl ester in methanesulfonic acid over an interval of about 30 minutes. The reaction mixture may be heated at a temperature of about 70° C. to about 80° C. for a period of about 10 hours to about 12 hours. The reaction mixture may be cooled to about 30° C. Isolation of the product may be carried out by adding water, cooling to about 0° C. to about 5° C. and stirring for about another 1 hour.
The conversion of the compound of Formula V to a compound of Formula VI can be carried out with hydroxylamine hydrochloride, wherein formyl group reacts with hydroxylamine initially to form oxime and then a cyano group. The reaction can be carried out in a solvent, for example, formic acid, acetic acid, dichloromethane, dichloroethane, chloroform, carbon tetrachloride, methanol, ethanol, 1-propanol, 2-propanol, toluene, benzene, pyridine, ethyl acetate, diethylether, tetrahydrofuran, dioxane, 1,2-methoxyethane, dimethylformamide, dimethyl sulfoxide, or mixture(s) thereof, in the presence of a base, for example, sodium formate, potassium formate, sodium acetate, triethylamine, potassium carbonate, caesium carbonate, sodium carbonate, sodium bicarbonate, pyridine or mixture(s) thereof at a temperature of about 0° C. to about 250° C. for about 15 minutes to about several days depending on type of reactant, solvent and base selected.
In a particular embodiment, the reaction of compound of Formula V (wherein R is ethyl) with hydroxylamine hydrochloride to give a compound of Formula VI is carried out using sodium formate as base and formic acid as solvent at a temperature of about 25° C. to about 125° C. for a time period of about 7 hours to about 12 hours.
The alkylation of the compound of Formula VI with isobutyl halide of Formula VII to give a compound of Formula VIII can be carried out in the presence of a base, for example, potassium carbonate, sodium carbonate, caesium carbonate, sodium bicarbonate, sodium hydride, a sodium ethoxide, sodium methoxide, potassium tert-butoxide, triethylamine or pyridine, optionally in the presence of an additive agent, for example, potassium iodide, sodium iodide or dimethylaminopyridine (DMAP), in a solvent, for example, dimethylformamide, dimethylacetamide, ethyl methyl ketone, acetone, methyl isopropyl ketone, methyl isobutyl ketone, methyl n-butyl ketone, methyl t-butyl ketone, methyl isoamyl ketone, dimethyl sulfoxide, hexamethylphosphoric triamide, tetrahydrofuran, dioxane, dimethoxyethane, diethylene glycol, dimethyl ether, dichloromethane, dichloroethane, chloroform, carbon tetrachloride, toluene, ethyl acetate, or mixture(s) thereof. The temperature of the reaction mixture may vary from about 0° C. to about 250° C. and the time interval for carrying out the reaction may vary from about 15 minutes to about several days depending upon the solvent, additive agent, base and reactants involved. In a particular embodiment, the isobutyl halide is isobutyl bromide, the solvent is dimethylformamide, the temperature for carrying out the reaction is about 70° C. to about 80° C. and the time interval is about 7 hours to about 8 hours.
The hydrolysis of the compound of Formula VIII to give febuxostat of Formula I can be carried out in the presence of a base, for example, alkali or alkaline earth metal oxides and hydroxides selected from barium hydroxide octahydrate, barium oxide, potassium hydroxide, magnesium hydroxide, lithium hydroxide or calcium hydroxide in a solvent, for example, tetrahydrofuran (THF), water, ethanol, methanol, denatured spirit, 1-propanol, 2-propanol, 1-butanol, dimethylformamide (DMF), dimethylacetamide (DMA), ethyl methyl ketone, acetone, methyl isopropyl ketone, methyl isobutyl ketone, methyl n-butyl ketone, methyl t-butyl ketone, methyl isoamyl ketone, dimethyl sulfoxide, dichloromethane, dichloroethane, chloroform, carbon tetrachloride, toluene, ethyl acetate or mixture(s) thereof at a temperature of about 0° C. to about 250° C. for about 15 minutes to about several days depending on type of reactant, solvent and base selected. In a particular embodiment, hydrolysis of compound of Formula VIII is carried out with barium hydroxide octahydrate, barium oxide or lithium hydroxide monohydrate in a solvent selected from tetrahydrofuran, ethanol, water, 2-propanol, methanol, denatured spirit, or mixture(s) thereof. In another particular embodiment, the hydrolysis of compound of Formula VIII (wherein R is ethyl) to give febuxostat of Formula I is carried out with barium hydroxide octahydrate in tetrahydrofuran, ethanol, methanol, denatured spirit and water. The temperature of the reaction may be about 55° C. to about 70° C., more particularly about 60° C. to about 65° C. The time interval for carrying out the reaction may be from about 30 minutes to about 3 hours, more particularly about 90 minutes to about 120 minutes. Upon completion of reaction, the temperature of the reaction mixture may be cooled down to about 40° C. to about 55° C. Dilution of the reaction mixture may be carried out with a solvent such as ethyl acetate and water. pH of the reaction mixture may be adjusted to 0.5-0.8 with an acid such as 6N HCl. The organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layer may be treated with activated carbon, filtered and concentrated. The residue thus obtained may be dissolved in a solvent selected from dichloromethane, dichloroethane, chloroform or carbon tetrachloride, methanol, ethanol, 2-propanol, 1-propanol, 2-methyl-2-propanol, or mixture(s) thereof. The solution may be cooled to about 0° C. to about 10° C., more particularly to about 0° C. to about 5° C., stirred for about 1 hour, filtered, washed with a pre-cooled mixture of methanol and dichloromethane and dried under reduced pressure to febuxostat.
The hydrolysis process of the present invention uses barium hydroxide octahydrate and thereby provides febuxostat of very high chemical purity with very less amount of amide by-product as compared to conventional hydrolyzing agents. The experimental observations are tabulated in Table 1 as below.
TABLE 1
Amide
by-
Isolated product
product
Amide
in the
HPLC
by-
Base Used
Solvent used
reaction
purity
product
NaOH (1.7 mole
Mixture of THF
0.34%
99.80%
0.15%
eqv) (As per patent
and absolute
U.S Pat. No. 5,614,520)
alcohol
NaOH solution (1.7
THF
0.27%
99.85%
0.15%
mole eqv)
Ba(OH) 2 •8H 2 O
Mixture of THF
0.21%
99.90%
0.10%
solution (0.6 mol
and IPA
eqv)
Ba(OH) 2 •8H 2 O
Mixture of THF
0.158%
99.93%
0.07%
solution (0.6 mol
and absolute
eqv)
alcohol
Ba(OH) 2 •8H 2 O
Mixture of THF
0.14%
99.87%
0.07%
solution (0.6 mol
and DNS
eqv)
BaO solution (0.6 mol
Mixture of THF
0.12%
99.89%
0.06%
eqv)
and absolute
alcohol
BaO solution (1 mol
Mixture of THF
0.25%
—
—
eqv)
and methanol
It has also been observed that the formation of amide by-product increases with time in case of hydrolysis with conventional hydrolyzing agents such as sodium hydroxide, whereas in case of the hydrolysis with barium hydroxide octahydrate, the amide by-product does not increase with time as shown below in Table 2.
TABLE 2
Formation of Amide by-
product in the reaction
Amide by-
Base Used
Solvent used
Reaction Time
product
NaOH Solution (1.7
Mixture of THF and
45 min
0.24%
mole equivalent)
absolute alcohol
2 hrs
0.38%
3 hrs
0.53%
4 hrs
0.62%
5 hrs
0.79%
NaOH (1.7 mole
Mixture of THF and
1 hr
0.44%
equivalent)
absolute alcohol
2 hrs
0.50%
3 hrs
0.68%
4 hrs
0.84%
5 hrs
0.95%
Ba(OH) 2 •8H 2 O (0.6
Mixture of THF and
6 hrs
<0.10%
mole equivalent)
absolute alcohol
7 hrs
0.10%
8 hrs
0.10%
22 hrs
0.16%
In the present invention, reactants may interact with each other by different means, for example, dissolving to give a solution, slurrying to form a suspension or making colloids to give an emulsion.
In the present invention, isolation of the product may be accomplished by, among other things, extraction, concentration, precipitation, crystallization, filtration or centrifugation.
Washing of the obtained residue may be carried out using the solvents in which the product is sparingly soluble and by selecting a temperature that allows dissolving of impurities only and not the desired product. The solvents for washing may include, but are not limited to, water, ethyl acetate, acetone, methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl-l-propanol, 1-pentanol, ethylene glycol, propylene glycol, diethyl ether, ethyl methyl ether, tert-butyl methyl ether, tetrahydrofuran or 1,4-dioxane, methyl acetate, propyl acetate, butyl acetate, methyl ethyl ketone, methyl isobutyl ketone, benzene, toluene, xylene, N,N-dimethylformamide or N,N-dimethylacetamide, acetonitrile, propionitrile, dimethyl sulfoxide, diethyl sulphoxide, or mixture(s) thereof.
Extraction of the product is a method to separate compounds based on their relative solubilities in two different immiscible liquids, usually water and an organic solvent, and may be carried out using a separatory funnel. The extraction process in the present invention may employ non-aqueous systems also depending upon the type of product. Extraction process may be single stage or a multistage continuous process.
Separation and concentration method of the organic compound should be such that allows minimum product decomposition and maximum product quality. The methods for concentration employed in the present invention may involve any of the conventional methods known in the art, for example, common distillation, distillation under reduced pressure, through reverse osmosis membrane, prevaporation through a membrane, hydrophilic ultrafiltration membrane, or a combination thereof.
Drying may be accomplished by any suitable method of drying such as drying under reduced pressure, vacuum tray drying, air drying or a combination thereof. Drying may be carried out at a temperature of about 45° C. to about 70° C. for about 10 hours to about 2 days.
Filtration may be accomplished by any of the methods known in the art, for example, by using büchner funnel, belt filter, rotary vacuum-drum filter, crossflow filters, screen filter. Filtration may also be accompanied by filter aids, for example, diatomaceous earth, kieselguhr, wood cellulose, perlite, etc. or a combination thereof.
Purification or refinement may be accomplished by combining suitable means, such as processing by extraction, chromatography separation, activated carbon, florisil, etc., and recrystallization.
In the foregoing section, embodiments are described by way of examples to illustrate the processes of invention. However, these are not intended in any way to limit the scope of the present invention. Several variants of the examples would be evident to persons ordinarily skilled in the art which are within the scope of the present invention.
Non-limiting examples of the present invention are as follows.
EXAMPLES
Example 1
Synthesis of Ethyl 2-(4-Hydroxyphenyl)-4-Methyl-5-Thiazol Carboxylate
A mixture of 4-hydroxy thiobenzamide (100 g, 0.653 mol) and ethyl 2-chloroacetoacetate (118.3 g, 0.719 mol) in denatured spirit (DNS) (500 mL) was heated at about 60° C. to 65° C. for about 2.5 hours. The reaction mixture was cooled to about 0° C. to 5° C. and stirred for about 1 hour at the same temperature. The solid obtained was filtered, washed with denatured spirit and dried to obtain the title compound. (Yield: 156 g, 90.7%)
Example 2
Synthesis of Ethyl-2-(3-Formyl-4-Hydroxyphenyl)-4-Methyl-5-Thiazole Carboxylate
Hexamethylene tetramine (134 g, 0.971 mol) was added to a solution of ethyl 2-(4-hydroxyphenyl)-4-methyl-5-thiazol carboxylate (100 g, 0.38 mol) in methanesulfonic acid (500 mL) slowly over a period of about 30 minutes. The reaction mixture was heated to about 75° C. and stirred for about 10 hours. After completion of reaction, the reaction mixture was cooled to about 30° C. and water was added to it. The reaction mixture was further cooled to about 0° C. and stirred for about 1 hour. The solid thus obtained was filtered, washed with water and dried to give the title compound. (Yield: 80 g, 72.3%)
Example 3
Synthesis of ethyl-2-(3-cyano-4-hydroxyphenyl)-4-methyl-5-thiazole carboxylate
Hydroxylamine hydrochloride (35.82 g, 0.515 mol) and sodium formate (46.73 g, 0.687 mol) were added to a solution of ethyl-2-(3-formyl-4-hydroxyphenyl)-4-methyl-5-thiazole carboxylate (100 g, 0.343 mol) in formic acid (anhydrous, 300 mL) and the reaction mixture was heated to a temperature of about 100° C. for about 8 hours. After completion of reaction, the reaction mixture was cooled to about 40° C. and water was added to it. The reaction mixture was cooled to about 25° C. and stirred for about 1 hour. The solid obtained was filtered, washed with water and dried. The solid was then dissolved in acetone at about 50° C. and water was added slowly over a period of about 30 minutes. The mixture was cooled to about 25° C. and again stirred for about 1 hour. The solid thus obtained was filtered, washed with acetone:water (1:1) mixture and dried to obtain the title product. (Yield: 85 g, 85.9%)
Example 4
Synthesis of Ethyl-2-(3-Cyano-4-Isobutyloxyphenyl)-4-Methyl-5-Thiazole Carboxylate
Potassium carbonate (300 g, 2.17 mol) and isobutyl bromide (142.7 g, 1.041 mol) were added to a solution of ethyl-2-(3-cyano-4-hydroxyphenyl)-4-methyl-5-thiazole carboxylate (100 g, 0.347 mol) in dimethylformamide (300 mL), and the reaction mixture was heated at a temperature of about 75° C. for about 8 hours. After completion of reaction, the reaction mixture was cooled to about 40° C. and water was added. The reaction mixture was further cooled to about 0° C. and stirred for about 1 hour. The solid thus obtained was filtered, washed with water and dried to give title compound. (Yield: 111g, 92.9%)
Example 5
Synthesis of 2[3-Cyano-4-(2-Methylpropoxy)Phenyl]-4-Methylthiazole-5-Carboxylic Acid (Febuxostat)
Aqueous barium hydroxide octahydrate solution (prepared by dissolving 55 g, 0.174 mol of barium hydroxide octahydrate in 350 mL water) was added to a solution of ethyl-2-(3-cyano-4-isobutyloxyphenyl)-4-methyl-5-thiazole carboxylate (100 g, 0.29 mol) in tetrahydrofuran (1000 mL) and denatured spirit (300 mL). The reaction mixture was stirred at a temperature of about 60° C. for about 90 minutes to about 120 minutes. After completion of reaction, the mixture was cooled to a temperature of about 45° C. and diluted with ethyl acetate and water. The pH of the reaction mixture was adjusted to 0.5-0.8 with 6N HCl at about 35° C. The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The combined organic layer was treated with activated carbon (10 g) and filtered through hyflobed. The hyflobed was washed with ethyl acetate. The combined filtrate was concentrated at a temperature of about 45° C. under reduced pressure. The residue thus obtained was dissolved in a mixture of dichloromethane (400 mL) and methanol (1000 mL) and the solution was cooled to about 0° C., stirred for about 1 hour. The solid thus obtained was filtered, washed with a precooled mixture of methanol and methylene chloride, dried under reduced pressure to give febuxostat. (Yield: 81 g, 88%)
HPLC purity: 99.93%
Amide by-product: 0.07%. | An improved and efficient process for the preparation of 2-[3-cyano-4-(2-methylpropoxy)phenyl]-4-methylthiazole-5-carboxylic acid (febuxostat) that is substantially free from amide by-product is provided. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
The present application is the U.S. counterpart of WO 2007/135335 and claims priority to French application no. 0651863 filed on May 22, 2006 and French application no. 0655440 filed on Dec. 12, 2006, the entire contents of each of which are hereby incorporated herein by reference.
BACKGROUND
1. Field
The present invention relates to sheets, particularly sheets of fragile material of the glass type, equipped for being fixed to supports or to be joined together using joining elements.
2. Description of the Related Art
Such sheets are intended in particular for producing walls or fixtures and fittings, of a facade element or an internal arrangement, which are made up of substrates, particularly transparent substrates, for example glass substrates.
To these ends, these sheets have therefore to have holes at the fixing and/or connecting points. They may be reinforced, particularly using thermal or chemical tempering, in order to obtain the required mechanical strength (and the required thermal resistance if necessary). The holes have therefore to be made before the heat treatment operation.
Document DE 195 42 040 discloses a sheet of glass which, at its edge face, has a peripheral slot, this slot being intended to accept a joint, it being possible for the joint to be forcibly inserted into the slot or bonded or extruded into said slot.
The main disadvantage with this type of sheet lies, in particular, in the fact that the connection between the slot and its joint requires the use of an external agent or an external action.
In the case of adhesive bonding, the adhesive chosen needs to be applied beforehand to the faces of the joint and/or of the slot that are to be bonded together, then the faces of the joint and/or of the slot are brought into contact, the assembly not actually being mechanically secure until after a given curing time has elapsed.
This adhesive-bonding technique is dependent upon the time taken for the adhesive to cure, and upon the integrity of the adhesive over time, it being possible for the mechanical connection between the joint and its slot to deteriorate over time as a result in particular of aging of the adhesive (under the action of UV radiation for example) or as a result of inappropriate mechanical or chemical demands, of the detergent or solvent type, etc., on the joint.
German utility model DE 203 02 370 describes a connecting system for glass sheets, this connecting system allowing connection to be made using a joining element collaborating through retaining shapes made on the edges of the sheets of glass. These dovetail retaining shapes are inappropriate if, as is often the case, the sheet has to undergo a heat treatment in order to improve its mechanical properties, this typically being a tempering operation. Stress concentrations are then created in the angular parts and there is a risk that these stresses will be released, destroying the sheet of glass.
When the joint or connecting system is “force fitted” into the slot without any special retaining appendages, insertion is governed by the mechanical properties of the material of which the joint or connecting system is made, particularly the elastic deformation properties. Provided that the joint or connecting system is not mechanically stressed, it will remain in place in its slot, but if, as a result of aging of the material, mechanical stresses that are inappropriate in terms of their direction and/or in terms of their intensity are applied, a gap may open and cause the joint or connecting system to escape from its slot. In addition, it is found that “force-fitting” a part of the joint or connecting system type is not the optimum way of inserting such a component when the latter is supposed to be able to transmit loads.
SUMMARY
The present invention proposes a connecting system allowing at least one cavity, preferably positioned on a surface portion situated on the edge or edge face of a substrate to be secured to a support member without displaying the disadvantages of the prior art.
To these ends, the connecting system designed to secure at least one cavity having curved and retaining walls and positioned on a surface portion located on the edge of a glass substrate and a support member, characterized in that it comprises a shoe equipped with at least one appendage projecting from at least one of the faces of said shoe, said appendage having a profile that complements the profile made on the surface portion situated on the edge of said substrate.
In some preferred embodiments of the invention, recourse may also possibly be had to one and/or another of the following arrangements:
the shoe is T-shaped the shoe is L-shaped the shoe is U-shaped the shoe is made of plastic, preferably of Nylon-6,6, the shoe is made from a pultrusion of plastic fibers and reinforcing fibers, the shoe is produced by molding or injection molding a plastic, the appendage has projecting parts of convex profile that complement the profile of the concave faces made in said cavity, the appendage has parts capable of flexing elastically or even plastically inwards so as to allow said appendage to be fitted into the corresponding cavity of said substrate, collaboration between the shoe and the cavity is designed in such a way as to ensure that said connecting means is automatically locked into the cavity, a wetting agent is interposed at the interface between the side wall of the cavity and the connecting means in order to improve the surface condition.
Within the meaning of the invention, an “edge” is defined as being the long narrow face of a large sized element.
The present invention also relates to a sheet of mineral or organic glass comprising, on at least one of its faces, preferably at its edge, a cavity intended to accept at least one connecting system as defined hereinabove. It also relates to a sheet such as this equipped with its connecting means of which there may be one or more. It also relates to a sheet which has been equipped with its one or more connecting means and in which the or each connecting means allows for connection with a support member, it being possible for this support to be another sheet.
As indicated hereinabove, the fragile material of which these sheets is made is generally tempered glass, or, more generally, a glass substrate which can undergo a heat treatment or chemical treatment, particularly a tempering, a toughening, an annealing, a bending operation, or alternatively, a glass which is mechanically strengthened, after the cavities have been made.
The present invention also relates to an assembled assembly or assembly for assembly comprising at least one sheet of fragile material of the glass type as defined hereinabove.
In particular, an assembly such as this constitutes a part of fixtures and fittings, a partition or wall of a piece of furniture, of a room, of a shower cubicle, a shelf, for example a refrigerator shelf, shop furniture, display cabinets, doors, shop windows.
An assembly such as this may constitute a double glazing or even a triple glazing, each of the substrates forming this assembly being assembled and joined together by joining elements.
BRIEF DESCRIPTION OF THE DRAWINGS
In order to provide a better illustration of the subject matter of the present invention, various particular embodiments thereof will be described hereinbelow by way of nonlimiting indication with reference to the attached drawings in which:
FIG. 1 is a perspective view of a connecting system according to the invention, produced in an L-shape,
FIG. 2 is a perspective view of a connecting system according to the invention, produced in a T-shape,
FIG. 3 is a perspective view of an alternative form of embodiment of a T-shaped embodiment,
FIG. 4 is a perspective view illustrating the joining-together of two substrates using a connecting system according to the invention,
FIG. 5 is a perspective view illustrating the joining-together of two substrates using the connecting system according to FIG. 2 ,
FIG. 6 is a view in cross section illustrating the joining-together of a substrate and a connecting system according to the invention, this system of joining having the property of allowing for axial expansion between the substrate and the connecting system,
FIG. 7 is a view in cross section of an alternative form of embodiment of an alternative form of embodiment of a connecting system according to the invention.
DETAILED DESCRIPTION
FIGS. 4 and 5 depict monolithic glass panes 1 and 2 which are provided on at least one surface portion, and near their edge 3 , with at least one slot which was made before the glass pane was tempered, parallel to the main faces thereof and along the edge.
In a conventional way, solid angles of intersection between the edge-forming face and the two main faces of the glass pane are removed in the customary way, for example by chamfering.
The cross section of the slot is rectangular in a first part near these remaining surfaces, then is of rounded shape in a second part that forms the bottom of the slot. However, its bottom will be very well rounded, in order to prevent any stress raisers in the corners and minimize the effect of the cutting of the slot.
A series of cutters with appropriate profiles and tooth shapes (roughing cutter, semi-finishing cutter, finishing cutter) is used to produce a blind cavity inside this slot. Of course, the cross section of the cavities may vary, these being circular or oblong in particular, according to the intended application.
In an alternative way of producing the slot, this slot is obtained using abrasive disks or grinding wheels. These abrasive tools are of course rotationally driven and positioned on a pivotable or inclinable head. Thus, by inclining the tool with respect to the normal to the side or edge of the glass substrate and by combining this movement with a feed movement, a slot or the desired profile can be obtained, after a number of machining passes.
The cavity is delimited by a flat bottom perpendicular to the main faces of the sheet of glass, and by a side wall connected to the bottom by a region of curved and retaining profile, particularly of concave shape, with the concave face facing towards the inside of the cavity and exhibiting axial symmetry, followed by a short oblong region, and then opening onto the remaining surfaces via a frustoconical region that widens towards the outside. This region thus constitutes, together with the parts adjacent to the regions, a catching or retaining bead the purpose of which is explained later on.
If necessary, the slot may also have a cross section with undercut, if the corresponding manufacturing possibilities are available and the total thickness of the sheet is sufficient.
The slot made on the edge 3 of each substrate is intended to accept a connecting system 4 obtained by molding a plastic such as PVDF (poly(vinylidene fluoride)) or Nylon-6,6, for example, or by an operation of pultrusion of reinforcing fibers (glass fibers) and plastic fibers.
As can best be seen in FIGS. 3 , 4 and 5 , the connecting system 4 comprises a projecting appendage 5 connected to a more or less flat shoe 6 . This connecting system 4 is either one-piece or made up of several elements. It is elastically or even plastically deformable so as to allow it to be inserted into the slot.
The external face of the appendage 5 is connected to the bottom by a curved region the shape of which allows it to hug that of the concave region of the slot. The curved region is extended by a low wall which is intended to bear against the oblong region delimiting the slot, ending, after a step inwards, in another oblong region.
Depending on the application, and particularly in the application at which this example is aimed, it may be important to make the hole and its insert invisible from the side facing the user. To do this, a wetting agent is interposed at the interface between the internal side wall of the slot and the external wall of the connecting system 4 in order to improve the surface condition, this wetting agent being silicone for example, or a wetting agent that has this property.
According to a preferred embodiment (depicted in FIGS. 1 and 2 for example), the connecting system 4 has a shoe-shaped part of parallelepipedal overall shape, at least one of the faces of which has a projecting appendage 5 . Depending on the number of appendages, it is possible for example to have L-shaped, T-shaped, U-shaped, Y-shaped, etc. connecting systems or, more generally, connecting systems with any cross section produced from a succession of simple or straight shapes as listed above and having, on at least one of their faces, at least one appendage 5 allowing for connection to the edge of a substrate. It is also possible, as in the alternative form depicted in FIG. 4 , to have a connecting system 4 of U-shaped overall cross section in which the lateral parts of the U are provided with appendages 5 for securing to the edges of the substrates and in which the central part of the U allows another substrate or wall or partition to be mounted by force-fitting or the like.
The part forming the appendage 5 has projecting parts 7 of convex profile that complement the profile of the concave faces made in the slot.
These convex parts 7 are produced as one piece with the shoe and are elastically deformable.
Furthermore, it is also possible to conceive of prefabricating the shoe separately from the convex parts 7 and assembling them later (by clipping, bonding, fusing). That would possibly have the advantage that the shoe and the convex parts could be made of different materials (and in particular also have different hardnesses).
In order to mount the connecting system 4 in the slot in the sheet 1 (the glazing or the like), all that is required is for the appendage to be “forced” into the slot in the correct position. The convex parts 7 are then elastically deformed.
As an alternative (not depicted in the figures), this connecting system may collaborate with a rod or any other type of similar component designed to allow it to collaborate with another connecting system intended to collaborate with another cavity of another sheet in order in this way to form elements (fixtures and fittings or the like).
As an alternative, such as the connecting system depicted in FIG. 3 for example, the system is in the form of a plate or sole designed to be connected to the ground or to any other bearing structure via holes 8 through which fasteners can be inserted, or alternatively, the connecting system may in general consist of any transmission allowing a sheet of fragile material to be connected to a support. Thus, this transmission may involve a ball joint, possibly extended by a rod, an articulation, a box, etc.
According to yet another alternative form of embodiment illustrated in FIG. 6 , the assembly between a substrate 1 and a connecting system 4 (possibly secured to another substrate 2 ) may be performed by providing or allowing an expansion clearance between the connecting system 4 and the substrate 1 . In order to do this, the slot produced in the edge 3 of the substrate 1 is designed to have a characteristic dimension (in this instance a depth in particular) significantly larger than the characteristic dimension of the appendage 5 so as to allow an axial movement by j 1 of the appendage 5 in the slot in one direction or the other. This axial movement of the system 4 and of its appendage 5 with respect to the substrate 1 may be the result of thermal expansion phenomena or of mechanical play resulting from the assembly of the substrates 1 , 2 .
It will be readily appreciated that this clearance j 1 can also be allowed not between the connecting system 4 and the substrate 1 or 2 but more generally with a transmission constituting an intermediate part or intermediate collection of parts between a connecting system and at least one substrate.
According to yet another alternative form of embodiment shown in FIG. 7 , it can be seen that the appendage 5 ′ of the connecting system 4 is asymmetric. This asymmetric profile is particularly well suited to facilitating assembly between a substrate 1 or 2 and a connecting system 4 not by nesting the connecting system 4 via one of its ends in the slot made in the edge of the glazing and then sliding the appendage 5 along the slot but by positioning the appendage 5 ′ facing the slot in its final position and then performing a slight rotational movement to allow the appendage 5 ′ to engage in the slot. This way of mounting the connecting system 4 bearing its asymmetric appendage 5 ′ in the slot 3 is similar to the way in which two sheets of laminate flooring are clipped together, the two parts locking together once the substrate 1 and the connecting system are positioned in the same plane (this is the assembly shown in FIG. 7 ).
The sheets of glass which have undergone a heat treatment or chemical treatment (for example a tempering operation) are prepared as follows: to begin with, the sheets are cut from non-tempered glass; the cavities are machined at the required locations (generally at least at one surface portion of the edge of said sheet), the heat treatment or chemical treatment is then performed (in this example, it is a tempering operation) on the sheets. The concave region of the side walls delimiting the cavities spreads the stresses which arise within the glass during the tempering. In particular, the profile of this concave region in terms of the choice of radius of curvature makes it possible to ensure that tempering can be performed without causing the glass to break in this region, thus avoiding having to scrap sheets.
Next, the connecting systems are introduced into the cavities. As has already been stated, this insertion of the joining elements is very easy because of the elasticity or even the plasticity thereof. The sheets may be delivered already equipped with their joining elements.
In general, the connecting system makes it possible to perform assembly between a frame or a bearing structure in general, and a sheet.
Thus, for example, the connecting system can be used to assemble multiple glazing. This may be triple glazing (of course, a variant for double glazing can be readily deduced from the aforementioned one), in which case the joining element is a triple one, having a central element and two lateral elements collaborating respectively with that same number of cavities made in the edges of the glazings. The choice of material of which to make the connecting system is made in such a way as to give the assembly the required mechanical strength once it has been assembled and, if necessary, to afford sealing if the multiple glazing is assembled incorporating a gas between the glazings. If need be, the joining elements are sealed against atmospheric pressure since the space between the glazings may be kept at a reduced pressure.
The invention as described hereinabove offers numerous advantages:
the connection is relatively insensitive to manufacturing tolerances, the connection can be disconnected and is able to withstand relatively high mechanical loads.
Of course the embodiment described hereinabove is not in any way limiting and may give rise to any desirable modifications without thereby departing from the scope of the invention. | A connecting system configured to secure at least one cavity including curved and retaining walls and positioned on a surface portion located on an edge of a substrate made of a fragile material of glass type and a support member. The connecting system includes a shoe including at least one appendage projecting from at least one of faces of the shoe, the appendage having a profile that complements the profile made on the surface portion situated on the edge of the substrate. | 4 |
RIGHTS OF THE GOVERNMENT
The invention described herein may be manufactured and used by or for the Government of the United States for all governmental purposes without the payment of any royalty.
BACKGROUND OF THE INVENTION
The present invention relates generally to methods for bonding dissimilar materials, and more particularly to a method for bonding plastic to metal utilizing a chemical milling process.
In certain fabrication processes wherein a plastic member is placed in contact with a metallic member, injection molding or similar processes have been used to form the plastic member onto the metallic member. If substantial adhesion between the plastic and metallic members is desired, the metallic member may first be conditioned by such processes as roughening or knurling the surface interfacing the plastic member, or flame or plasma spraying a porous coating thereon, or attaching fastening objects thereto. Certain end uses for products formed of a plastic member bonded to a metallic member may, however, require a reproducible and substantially stronger bond at the interface than is obtainable using adhesives and conventional surface preparation techniques.
The present invention substantially solves or reduces in critical importance deficiencies in the prior art as just described by providing a method for bonding plastic to a metallic member. In accordance with teachings of the invention, cavities are formed in the surface of the metallic member by etching using masking and etching techniques and allowing the etchant to undercut the surface to provide an interlock with a plastic member subsequently applied to the metallic surface by spraying, injection molding or the like or by heating/pressing the plastic member to the metallic member.
It is therefore a principal object of the invention to provide a method for bonding plastic to metal.
It is a further object of the invention to provide a method for bonding dissimilar materials, particularly plastic to metal, utilizing masking and etching techniques.
These and other objects of the invention will become apparent as the detailed description of representative embodiments proceeds.
SUMMARY OF THE INVENTION
In accordance with the foregoing principles and objects of the invention, a method for bonding plastic to a metallic member is described which comprises the steps of forming a preselected pattern of etched cavities in the metallic surface to be bonded, which cavities at least in part increase in width with depth of etching, and subsequently applying a plastic layer to the metallic surface so that a portion of the applied plastic layer fills the cavities and forms an interlock with the metallic surface.
DESCRIPTION OF THE DRAWINGS
The invention will be clearly understood from the following detailed description of representative embodiments thereof read in conjunction with the accompanying drawings wherein:
FIGS. 1-6 show schematic cross sections of intermediate structures obtained in the practice of representative processes comprising the invention and in obtaining the representative bond structure illustrated in FIG. 7; and
FIG. 7 is a schematic cross section of a representative plastic to metal bond structure made in accordance with the invention.
DETAILED DESCRIPTION
The method for bonding plastic to a metallic member in accordance with the invention is illustrated in FIGS. 1-6 which show schematic cross sections of intermediate structures obtained utilizing representative etching processes in the practice of the invention and in obtaining the representative plastic to metal bond structure illustrated in schematic cross section in FIG. 7. The process sequences represented by FIGS. 1-7 are examples of methods usable in the practice of the invention and of a representative structure of a bond between plastic and metal obtainable according to the invention. The specific intermediate and final structures shown being, however, only representative, it is understood that variations to the methods described and ultimate bond configurations obtainable may be envisioned by one with skill in the field of the invention within the scope of the appended claims guided by these teachings.
Referring first to FIGS. 1 and 5 together, shown therein are schematic cross sections of intermediate structures obtained utilizing a typical chemical etching or milling process to form the cavities desired to effect the plastic to metal bond according to an embodiment of the invention. As suggested in FIG. 1, a metallic member 11 to which plastic is to be bonded may first be suitably conditioned on a surface 13 thereof by any suitable conventional process in preparation for performing a corresponding chemical milling treatment of surface 13. As will be appreciated by further reading hereof, substantially any metal or alloy may be bonded to plastic utilizing the method of the invention, so long as a surface 13 of metallic member 11 to be bonded may be chemically milled using suitable etchant. Accordingly, as used herein, "metallic member" is intended to include both metals and alloys, including iron, steel, aluminum, magnesium, copper, tin, zinc, titanium, zirconium, uranium, lead, nickel, antimony, beryllium, cadmium, cerium, chromium, cobalt, gold, silver, hafnium, indium, iridium, molybdenum, palladium, platinum, rhenium, rhodium, tantalum, tungsten and vanadium and other alloys thereof as well as a few non-metals, such as glass, for which chemical milling is suitable. Onto surface 13 is overlaid mask 14 or other etch resistant coating defining a pattern 15 of exposed areas corresponding to the desired pattern of etched cavities in surface 13 at which a plastic to metal bond is intended. Any desired pattern may be defined in mask 14 depending on the characteristics of the plastic to metal bond to be made, such as the expanse of the bonded interface, degree of adhesion desired, intended use of the bonded product and the like. The exposed pattern 15 in surface 13 is then etched using a suitable etchant 17 for selected period of time, with or without an applied electrical current, to produce the intermediate structure illustrated in FIG. 5 (mask 14 removed) wherein small pits or cavities 19 in the desired pattern 15 are defined on metallic member 11. Any suitable etchant 17 may be used depending on the material comprising metallic member 11. Typical etchants may therefore include ferric chloride, various acids, bases or electrolytes.
Referring now collectively to FIGS. 2-5, metallic member 11 may in accordance with an alternative etching process contemplated herein first be suitably conditioned on surface 13' thereof for receiving layer 21 of photoresist material. Layer 21 of photoresist may include any well known brand commercially available for the purpose contemplated herein. Onto layer 21 is overlaid a photographic mask 23 having the desired pattern 25 therein corresponding to the regions in surface 13' of metallic member 11 at which a plastic to metal bond is intended. Photoresist layer 21 with mask 23 overlaid is then exposed to (usually ultraviolet) radiation 27 to selectively harden a (unmasked) portion of photoresist layer 21 defining the ultimate desired pattern of cavities for effecting the intended bond. Mask 23 is then removed and layer 21 is chemically treated to remove that portion thereof defining the desired pattern of cavities on surface 13', as suggested by the intermediate structure depicted in FIG. 3 showing layer 21 with the desired pattern 25 therein which corresponds to the ultimate desired pattern of cavities 19 in metallic member 11. The underlying surface 13' of metallic member 11 is then etched using a suitable etchant 17' to produce the intermediate structure including cavities 19 illustrated in FIG. 5 in manner corresponding to the process described above in relation FIG. 1.
In addition to any of the etching processes suggested above, any of numerous alternate processes well known to one skilled in the art, including silk screening, stamping, printing, spraying or other methods, may be used to deposit an appropriate pattern of masking material exposing the metallic surface only in areas to be etched.
In accordance with a governing principle of the invention and significant departure from prior art procedures, a chemical etching (or milling) step as just described is performed in manner and degree to intentionally cause undercutting of the unetched portion of surface 13 as suggested in FIG. 5, that is, to provide cavities 19 which at least in part increase in width with depth of etching. In prior art chemical etching or related processes, care is normally taken to avoid the undercutting desired in the practice of this invention. Each cavity 19 may be therefore characterized by the somewhat tear drop shaped cross section suggested in FIG. 5. The purpose of deliberately inducing undercutting according to the invention is to produce a reproducible surface which interlocks with a subsquently applied plastic layer or coating to produce a bond of predictably high bond strength.
Accordingly, once the structure for metallic member 11 as suggested in FIG. 5 is obtained by any of the etching methods mentioned above, a selected plastic or polymer layer 29 is then applied to metallic member 11. Representative materials for plastic or polymer layer 29 attachable according to the invention include polyethylene, nylon, polyether sulfone, ABS, polystyrene, vinyls, acrylics, phenols and other like materials including polyolefins, styrene polymers, styrene copolymers, vinyl polymers or copolymers, polyesters, polyethers, polyamines, polyamides, polyimides, polyurethanes, elastomers, vinylidene polymers, epoxies, phthalate polymers, ionomers, cellulosics, silicones, and other thermoplastics and thermoset plastics. Layer 29 may be applied by any of numerous techniques known in the applicable art such as spraying, sputtering, injection molding, etc, or may be cured in place on metallic member 11, or may be applied as a sheet or bulk plastic material as suggested in FIG. 6 and subjected to heat and/or pressure using appropriate means 31 to obtain the bond suggested in the final structure depicted in FIG. 7. It is noted that the bond between metallic member 11 and plastic layer 29 is substantially mechanical in nature characterized by an interlock between cavities 19 and portions 33 of layer 29 which are formed within cavities 19, in addition to such adhesive or abhesive bond which may otherwise form at the interface of metallic member 11 and plastic layer 29.
In the examples described in relation to FIGS. 1-7 above, the interlock of layer 29 with metallic member 11 is characteristic of the selected pattern of chemically milled pits or cavities, which pattern is not considered limiting of the invention herein. Other interlocking configurations contemplated herein include small spaced holes which increase in diameter with depth, and various patterns of lines, grids, herring bone shapes and the like which may have specific advantages in given applications.
The invention therefore provides an improved method for bonding plastic to a metallic member. It is understood that modifications to the invention as described may be made as might occur to one with skill in the field of the invention within the scope of the appended claims. All embodiments contemplated hereunder which achieve the objects of the invention have therefore not been shown in complete detail. Other embodiments may be developed without departing from the spirit of the invention or from the scope of the appended claims. | A method for bonding plastic to a metallic member is described which comprises the steps of forming a preselected pattern of etched cavities in the metallic surface to be bonded, which cavities at least in part increase in width with depth of etching, and subsequently applying a plastic layer to the metallic surface so that a portion of the applied plastic layer fills the cavities and form an interlock with the metallic surface. | 1 |
OBJECT OF THE INVENTION
The present invention relates to a termination of those employed for finishing the free extremity of a tape, generally manufactured on a basis of nylon or similar, whereby a substantial reduction is achieved in costs for the fastening of the termination to the tape, as well as a possibility of regulation in position for said termination.
The invention is applicable within the sphere of backpacks, handbags, cyclists' helmets, etc., in which tapes of the type mentioned above are used, as harnesses, means of fastening, means of closing, etc.
BACKGROUND OF THE INVENTION
The tapes for the applications mentioned above or others similar, come in a fabric structure, participating generally as base material in the constitution thereof nylon thread or other synthetic similar products, with or without the admixture of natural products, and as common denominator all of them require their free end to be finished in a termination which, as well as finishing the tape decoratively, impedes the fraying thereof and especially permits its coupling with other parts of the object on which it is fitted.
One of the commonly adopted solutions for implementing this termination, generally of plastic material, consists in providing said termination with a housing for the extremity of the tape, into which the latter is introduced and is subsequently fixed with the collaboration of a stitching process, which has to be sufficiently robust to endow the termination with a certain resistance to pulling. This solution has a fundamental problem in the cost of the stitching operation which has a considerable impact on the cost of the end product. Even in some cases, such as life jackets and in infants' chairs, it is necessary to position the entire finished product on the stitching table, since the tape stitching process takes place at the end of the production cycle. This, doubtless, augments even more the manufacturing cost.
Another solution consists in fastening the termination to the tape by means of the employment of rivets or similar, in which case the plastic piece is usually in the material form of two parts which adapt to the respective faces of the tape and which are finally fastened with one or more rivets, which also makes necessary the employment of machines for implanting the rivets in question, both in the case mentioned and in a further solution existing in this respect consisting in folding back the end of the tape on itself configuring a hem which is fixed with the rivets mentioned.
Another problem inherent to any of the solutions indicated above, lies in the fact that the termination is rigidly fixed to the end of the tape, there being no possibility of adjusting the effective length of said tape, in such a manner that in order to achieve the adjustment mentioned it is necessary to provide the tape, together with the termination mentioned, with another auxiliary mechanism which permits such adjustment.
DESCRIPTION OF THE INVENTION
The termination which is proposed by the invention overcomes in a fully satisfactory manner the problems outlined above, in the different aspects mentioned, constituting a structurally simple solution, very easy to assemble, which acts simultaneously as a means of adjusting the effective length of the tape, adjustment which can not only be implemented in manufacture but also throughout the period during which the tape is employed by the user thereof.
To this end and in more specific form, the termination which is proposed is implemented by means of a plastic piece which configures a type of clamp, of width in accordance with that of the tape for which it is intended, clamp in which participate two bodies, noticeably flat, connected to each other to form a unit by means of an intervening articulating hinge, obtained on a basis of weakened sectors in the region of union between the two bodies, each one of which configures a type of shallow cup, each of these incorporating also, in the bottom of each, a slot through which the tape passes, parallel and relatively close to said hinge, the slots of one and the other body being noticeably different in width and being provided with toothed edges, the teeth of which are directed towards the inside of the clamp, in such a manner that the teeth of one body are slightly offset with respect to those of the other in order to define in the tape a slight inflection in its path which enhances the gripping effect.
As a complement to the structure described one of the two bodies incorporates on its side edges respective claws, saw-tooth in outline, intended for insertion in internal and complementary recesses of the other body, when the coupling between the two takes place, with the interposition of the tape, said claws acting as a means of locking for the clamp in the closed position, which permit a straightforward assembly thereof on the tape and which guarantee perfect stability of the termination with respect thereto.
Moreover, each of the bodies mentioned presents, in correspondence with its edge opposite the hinge, an internal rim, in such a manner that these rims exercise in turn a pinching effect on the tape.
In accordance with this construction the end of the tape rests against the inside face of one of the bodies, emerges to the outside through the corresponding slot, passes behind the hinge towards the slot of the second body, penetrates inside said second body and is perfectly fastened when the clamp is closed especially through the effect of the complementary teeth, whilst by performing the closure of said clamp by means of a male-female coupling which permits the subsequent opening thereof, the user may at any time adjust at will the effective length of the tape, up to the point where the termination may even not be closed in manufacture leaving it at the option of the user to position it directly at the location on the tape which he prefers and in this eventuality cut off the segment of tape in excess.
DESCRIPTION OF THE DRAWINGS
In order to complete the description being made and for the purpose of assisting in a better understanding of the characteristics of the invention, in accordance with a preferred example of embodiment thereof, and forming an integral part of said description, a set of drawings is attached in which by way of illustration and not restrictively, the following has been shown:
FIG. 1 . Shown is a view in perspective of a tape finishing termination for implementation in accordance with the object of the present invention, which is shown in the open position.
FIG. 2 . Shown, also in a perspective view, is the termination of the previous figure duly coupled to the end of a tape.
FIG. 3 . Shown is a detail in side elevation and in cross section of the assembly illustrated in the previous figure, according to the cut A-B of said figure.
FIG. 4 . Shown, finally, is a detail in cross section of the assembly illustrated in FIG. 2, at the level of one of the interlocking points between the two bodies of the clamp, in accordance with the cut C-D of said figure.
PREFERRED EMBODIMENT OF THE INVENTION
In the light of these figures, it can be seen how the finishing termination for tapes which is proposed by the invention is structured by means of a single piece ( 1 ), preferentially injected in plastic material, in which piece are defined two bodies ( 2 ) and ( 3 ), noticeably flat, which are shaped in the form of respective cups joined to each other by means of an articulating hinge ( 4 ) which converts them into a kind of clamp capable of adopting the open position shown in FIG. 1 or the closed position shown in FIG. 2, which position being established in a stable fashion, after the insertion of the tape ( 5 ), thanks to the presence in one of the bodies ( 3 ), specifically on its side edges, prepared for fitting inside the body ( 2 ), of a pair of side claws ( 6 ) , saw-tooth in shape, which after elastic deformation fit into recesses ( 7 ) implemented in the other body ( 2 ), which permits the closure of the clamp to be performed by simply pressing on one body ( 3 ) with respect to the other ( 2 ).
The body ( 2 ) comes with a wide slot ( 8 ), parallel and relatively close to the edge thereof in which the hinge ( 4 ) is mounted, slot ( 8 ) delimited by each toothed edge ( 9 ), with its teeth pointing towards the inside of the cup, whilst on the body ( 3 ) is established in turn another slot ( 8 ′), noticeably narrower that the previous one, facing the latter in the closed position and equally delimited by teeth ( 9 ′) similar to those previously mentioned.
In accordance with this construction and starting from the open position shown in FIG. 1, the tape ( 5 ) is able to pass easily through the slot ( 8 ), from the inside of the body ( 2 ), coming out on the outside, passing over the hinge ( 4 ) and being housed inside the other body ( 3 ), through the slot ( 8 ′) of the latter, and from this situation the clamp defined by the two bodies is capable of being closed and of maintaining said closure stable, thanks to the male-female coupling which can be seen especially in the detail of FIG. 4, closed position in which the teeth ( 9 - 9 ′) bite into the end, folded-back segment of the tape ( 5 ), as is also shown in FIG. 3, preventing the occurrence of longitudinal displacement of the tape with respect to the termination in the event of pulling forces that may be applied to these elements.
It only remains to point out finally that both bodies ( 2 - 3 ) each incorporate on their free edge opposite the hinge ( 4 ) rims ( 10 - 10 ′), which in the closed position operate facing each other to determine a supplementary clamping zone for the tape ( 5 ), as may also be observed in the cross section of FIG. 3, there being also on the inside face of the two bodies ( 2 ) and ( 3 ) small conical protuberances ( 11 ) which collaborate likewise in said fastening, and said bodies also being provided with broad hollows ( 12 ) which, as well as having a favourable impact on the appearance of the termination, lighten the material thereof in those areas where it proves non-operational. | Applicable to tapes like those employed in backpacks, handbags, cyclists' helmets and similar goods, it is constituted by means of a piece ( 1 ) injected in plastic in which are defined two bodies ( 2 - 3 ) connected by means of a hinge ( 4 ), these bodies coming with respective slots ( 8 - 8′ ) for the passage of the tape to which the termination has to be coupled, and one of said bodies ( 3 ) having side claws ( 6 ) which, through elastic, deformation of said body, can couple into complementary recesses ( 7 ) in the other body ( 2 ), in order to stabilise the clamp formed by the termination in the closed position upon the tape. | 8 |
CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of copending application Ser. No. 09/906,974 (filed Jul. 17, 2001), entitled “MANUFACTURING PROCESS FOR ALPHA-OLEFINS”, which claims priority under 35 U.S.C. §119 from U.S. Prov. Appl. Ser. No. 60/218,888 (filed Jul. 18, 2000), which is incorporated by reference herein for all purposes as if fully set forth. This application further claims priority under 35 U.S.C. §119 from U.S. Prov. Appl. Ser. No. 60/222,786 (filed Aug. 3, 2000), which is also incorporated by reference herein for all purposes as if fully set forth.
FIELD OF THE INVENTION
A continuous manufacturing process for α-olefins using certain iron containing ethylene oligomerization catalysts together with alkylaluminum cocatalysts, in which using a low ratio of Al:Fe in the process results in a lowered formation of undesired polyethylene waxes and polymer.
TECHNICAL BACKGROUND
α-Olefins are important items of commerce, billions of kilograms being manufactured yearly. They are useful as monomers for (co)polymerizations and as chemical intermediates for the manufacture of many other materials, for example detergents and surfactants. Presently most α-olefins are made by the catalyzed oligomerization of ethylene by various catalysts, especially certain nickel complexes or aluminum alkyls, see for instance U.S. Pat. No. 4,020,121 and I. Kroschwitz, et al., Ed., Kirk - Othmer Encyclopedia of Chemical Technology, 4 th Ed., Vol. 17, John Wiley & Sons, New York, p. 839-858.
Recently, as reported in U.S. Pat. No. 5,955,555 and U.S. Pat. No. 6,103,946, both of which are hereby incorporated by reference herein for all purposes as if fully set forth, it has been found that iron complexes of certain tridentate ligands are excellent catalysts for the production of α-olefins from ethylene. Among the options for using such catalysts are those in which the iron complexes are used in conjunction with a cocatalyst, particularly an alkylaluminum cocatalyst such as an alkylaluminoxane.
It has recently been found, particularly in continuous processes using such iron complexes, that high molar ratios of Al:Fe lead to the undesirable formation of polyethylene waxes and polymers, which tend to foul the oligomerization apparatus. It has now been found that lower Al:Fe ratios diminish the formation of these undesirable polyethylenes, while not otherwise significantly deleteriously affecting the process.
SUMMARY OF THE INVENTION
This invention concerns a continous process for the production of a linear α-olefin product, comprising the step of contacting, in a continuous reactor, process ingredients comprising an ethylene oligomerization catalyst composition, ethylene and a cocatalyst, wherein:
(a) the ethylene oligomerization catalyst composition comprises an iron complex of a compound of the formula
wherein:
R 1 , R 2 and R 3 are each independently hydrogen, hydrocarbyl, substituted hydrocarbyl or an inert functional group, provided that any two of R 1 , R 2 and R 3 vicinal to one another taken together may form a ring;
R 4 and R 5 are each independently hydrogen, hydrocarbyl, substituted hydrocarbyl or an inert functional group;
R 6 and R 7 are each independently a substituted aryl having a first ring atom bound to the imino nitrogen, provided that
in R 6 , a second ring atom adjacent to said first ring atom is bound to a halogen, a primary carbon group, a secondary carbon group or a tertiary carbon group; and further provided that
in R 6 , when said second ring atom is bound to a halogen or a primary carbon group, none, one or two of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a halogen or a primary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom; or
in R 6 , when said second ring atom is bound to a secondary carbon group, none, one or two of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a halogen, a primary carbon group or a secondary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom; or
in R 6 , when said second ring atom is bound to a tertiary carbon group, none or one of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a tertiary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom;
(b) the cocatalyst comprises an alkyl aluminum compound; and
(c) the molar ratio of Al in the cocatalyst to Fe in the ethylene oligomerization catalyst is about 2000 or less.
This invention further concerns an improved continous process for the production of a linear α-olefin product, the process comprising the step of contacting, in a continuous reactor, process ingredients comprising an ethylene oligomerization catalyst composition, ethylene and a cocatalyst, wherein:
(a) the ethylene oligomerization catalyst composition comprises an iron complex of a compound of the formula
wherein:
R 1 , R 2 and R 3 are each independently hydrogen, hydrocarbyl, substituted hydrocarbyl or an inert functional group, provided that any two of R 1 , R 2 and R 3 vicinal to one another taken together may form a ring;
R 4 and R 5 are each independently hydrogen, hydrocarbyl, substituted hydrocarbyl or an inert functional group;
R 6 and R 7 are each independently a substituted aryl having a first ring atom bound to the imino nitrogen, provided that
in R 6 , a second ring atom adjacent to said first ring atom is bound to a halogen, a primary carbon group, a secondary carbon group or a tertiary carbon group; and further provided that
in R 6 , when said second ring atom is bound to a halogen or a primary carbon group, none, one or two of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a halogen or a primary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom; or
in R 6 , when said second ring atom is bound to a secondary carbon group, none, one or two of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a halogen, a primary carbon group or a secondary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom; or
in R 6 , when said second ring atom is bound to a tertiary carbon group, none or one of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a tertiary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom; and
(b) the cocatalyst comprises an alkyl aluminum compound;
wherein the improvement comprises reducing the formation of polyethylene waxes and polymers in the linear α-olefin product by contacting the process ingredients at a molar ratio of Al in the cocatalyst to Fe in the ethylene oligomerization catalyst of less than about 2000.
This invention also concerns a method for reducing the formation of polyethylene waxes and polymers in a continous process for the production of a linear α-olefin product, said continuous process comprising the step of contacting, in a continuous reactor, process ingredients comprising an ethylene oligomerization catalyst composition, ethylene and a cocatalyst, wherein:
(a) the ethylene oligomerization catalyst composition comprises an iron complex of a compound of the formula
wherein:
R 1 , R 2 and R 3 are each independently hydrogen, hydrocarbyl, substituted hydrocarbyl or an inert functional group, provided that any two of R 1 , R 2 and R 3 vicinal to one another taken together may form a ring;
R 4 and R 5 are each independently hydrogen, hydrocarbyl, substituted hydrocarbyl or an inert functional group;
R 6 and R 7 are each independently a substituted aryl having a first ring atom bound to the imino nitrogen, provided that:
in R 6 , a second ring atom adjacent to said first ring atom is bound to a halogen, a primary carbon group, a secondary carbon group or a tertiary carbon group; and further provided that
in R 6 , when said second ring atom is bound to a halogen or a primary carbon group, none, one or two of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a halogen or a primary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom; or
in R 6 , when said second ring atom is bound to a secondary carbon group, none, one or two of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a halogen, a primary carbon group or a secondary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom; or
in R 6 , when said second ring atom is bound to a tertiary carbon group, none or one of the other ring atoms in R 6 and R 7 adjacent to said first ring atom are bound to a tertiary carbon group, with the remainder of the ring atoms adjacent to said first ring atom being bound to a hydrogen atom; and
(b) the cocatalyst comprises an alkyl aluminum compound;
said method for reducing comprising the step of contacting said process ingredients in amounts such that the molar ratio of Al in the cocatalyst to Fe in the ethylene oligomerization catalyst is about 2000 or less.
These and other features and advantages of the present invention will be more readily understood by those of ordinary skill in the art from a reading of the following detailed description. It is to be appreciated that certain features of the invention which are, for clarity, described below in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the invention which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any subcombination.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Herein, certain terms are used. Some of them are:
A “hydrocarbyl group” is a univalent group containing only carbon and hydrogen. As examples of hydrocarbyls may be mentioned unsubstituted alkyls, cycloalkyls and aryls. If not otherwise stated, it is preferred that hydrocarbyl groups (and alkyl groups) herein contain 1 to about 30 carbon atoms.
By “substituted hydrocarbyl” herein is meant a hydrocarbyl group that contains one or more substituent groups which are inert under the process conditions to which the compound containing these groups is subjected (e.g., an inert functional group, see below). The substituent groups also do not substantially detrimentally interfere with the oligomerization process or operation of the oligomerization catalyst system. If not otherwise stated, it is preferred that substituted hydrocarbyl groups herein contain 1 to about 30 carbon atoms. Included in the meaning of “substituted” are rings containing one or more heteroatoms, such as nitrogen, oxygen and/or sulfur, and the free valence of the substituted hydrocarbyl may be to the heteroatom. In a substituted hydrocarbyl, all of the hydrogens may be substituted, as in trifluoromethyl.
By “(inert) functional group” herein is meant a group, other than hydrocarbyl or substituted hydrocarbyl, which is inert under the process conditions to which the compound containing the group is subjected. The functional groups also do not substantially deleteriously interfere with any process described herein that the compound in which they are present may take part in. Examples of functional groups include halo (fluoro, chloro, bromo and iodo), and ether such as —OR 50 wherein R 50 is hydrocarbyl or substituted hydrocarbyl. In cases in which the functional group may be near a transition metal (Fe) atom, the functional group alone should not coordinate to the metal atom (Fe) more strongly than the groups in those compounds that are shown as coordinating to the metal atom, that is they should not displace the desired coordinating group.
By a “cocatalyst” or a “catalyst activator” is meant one or more compounds that react with a transition metal compound to form an activated catalyst species. One such catalyst activator is an “alkyl aluminum compound” which, herein, is meant a compound in which at least one alkyl group is bound to an aluminum atom. Other groups such as, for example, alkoxide, hydride and halogen may also be bound to aluminum atoms in the compound.
By a “linear α-olefin product” is meant a composition predominantly comprising a compound (or mixture of compounds) of the formula H(CH 2 CH 2 ) q CH═CH 2 wherein q is an integer of 1 to about 18. In most cases, the linear α-olefin product of the present process will be a mixture of compounds having differing values of q of from 1 to 18, with a minor amount of compounds having q values of more than 18. Preferably less than 50 weight percent, and more preferably less than 20 weight percent, of the product will have q values over 18. The product may further contain small amounts (preferably less than 30 weight percent, more preferably less than 10 weight percent, and especially preferably less than 2 weight percent) of other types of compounds such as alkanes, branched alkenes, dienes and/or internal olefins.
By a “primary carbon group” herein is meant a group of the formula —CH 2 —, wherein the free valence — is to any other atom, and the bond represented by the solid line is to a ring atom of a substituted aryl to which the primary carbon group is attached. Thus the free valence — may be bonded to a hydrogen atom, a halogen atom, a carbon atom, an oxygen atom, a sulfur atom, etc. In other words, the free valence — may be to hydrogen, hydrocarbyl, substituted hydrocarbyl or a functional group. Examples of primary carbon groups include —CH 3 , —CH 2 CH (CH 3 ) 2 , —CH 2 Cl, —CH 2 C 6 H 5 , —OCH 3 and —CH 2 OCH 3 .
By a “secondary carbon group” is meant the group
wherein the bond represented by the solid line is to a ring atom of a substituted aryl to which the secondary carbon group is attached, and both free bonds represented by the dashed lines are to an atom or atoms other than hydrogen. These atoms or groups may be the same or different. In other words the free valences represented by the dashed lines may be hydrocarbyl, substituted hydrocarbyl or inert functional groups. Examples of secondary carbon groups include —CH(CH 3 ) 2 , —CHCl 2 , —CH(C 6 H 5 ) 2 , cyclohexyl, —CH(CH 3 ) OCH 3 , and —CH═CCH 3 .
By a “tertiary carbon group” is meant a group of the formula
wherein the bond represented by the solid line is to a ring atom of a substituted aryl to which the tertiary carbon group is attached, and the three free bonds represented by the dashed lines are to an atom or atoms other than hydrogen. In other words, the bonds represented by the dashed lines are to hydrocarbyl, substituted hydrocarbyl or inert functional groups. Examples of tetiary carbon groups include —C(CH 3 ) 3 , —C(C 6 H 5 ) 3 , —CCl 3 , —CF 3 , —C(CH 3 ) 2 OCH 3 , —C≡CH, —C(CH 3 ) 2 CH═CH 2 , aryl and substituted aryl such as phenyl and 1-adamantyl.
By “aryl” is meant a monovalent aromatic group in which the free valence is to the carbon atom of an aromatic ring. An aryl may have one or more aromatic rings which may be fused, connected by single bonds or other groups.
By “substituted aryl” is meant a monovalent aromatic group substituted as set forth in the above definition of “substituted hydrocarbyl”. Similar to an aryl, a substituted aryl may have one or more aromatic rings which may be fused, connected by single bonds or other groups; however, when the substituted aryl has a heteroaromatic ring, the free valence in the substituted aryl group can be to a heteroatom (such as nitrogen) of the heteroaromatic ring instead of a carbon.
By a “first ring atom in R 6 and R 7 bound to an imino nitrogen atom” is meant the ring atom in these groups bound to an imino nitrogen shown in (I), for example
the atoms shown in the 1-position in the rings in (II) and (III) are the first ring atoms bound to an imino carbon atom (other groups which may be substituted on the aryl groups are not shown). Ring atoms adjacent to the first ring atoms are shown, for example, in (IV) and (V), where the open valencies to these adjacent atoms are shown by dashed lines (the 2,6-positions in (IV) and the 2,5-positions in (V)).
In one preferred compound (I) R 6 is
wherein:
R 8 is a halogen, a primary carbon group, a secondary carbon group or a tertiary carbon group; and
R 9 , R 10 , R 11 , R 14 , R 15 , R 16 and R 17 are each independently hydrogen, hydrocarbyl, substituted hydrocarbyl or a functional group; provided that:
when R 8 is a halogen or primary carbon group none, one or two of R 2 , R 13 and R 17 are a halogen or a primary carbon group, with the remainder of R 12 , R 13 and R 17 being hydrogen; or
when R 8 is a secondary carbon group, none or one of R 12 , R 13 and R 17 is a halogen, a primary carbon group or a secondary carbon group, with the remainder of R 12 , R 13 and R 17 being hydrogen; or
when R 8 is a tertiary carbon group, none or one of R 12 , R 13 and R 17 is tertiary carbon group, with the remainder of R 12 , R 13 , and R 17 being hydrogen; and further provided that any two of R 8 , R 9 , R 10 , R 11 , R 12 , R 13 , R 14 , R 15 , R 16 and R 17 vicinal to one another, taken together may form a ring.
In the above formulas (VI) and (VII), R 8 corresponds to the second ring atom adjacent to the first ring atom bound to the imino nitrogen, and R 12 , R 13 and R 17 correspond to the other ring atoms adjacent to the first ring atom.
In compounds (I) containing (VI) and (VII), it is particularly preferred that:
if R 8 is a primary carbon group, R 13 is a primary carbon group, and R 12 and R 17 are hydrogen; or
if R 8 is a secondary carbon group, R 13 is a primary carbon group or a secondary carbon group, more preferably a secondary carbon group, and R 12 and R 17 are hydrogen; or
if R 8 is a tertiary carbon group (more preferably a trihalo tertiary carbon group such as a trihalomethyl), R 13 is a tertiary carbon group (more preferably a trihalotertiary group such as a trihalomethyl), and R 12 and R 17 are hydrogen; or
if R 8 is a halogen, R 13 is a halogen, and R 12 and R 17 are hydrogen.
In all specific preferred compounds (I) in which (VI) and (VII) appear, it is preferred that R 1 , R 2 and R 3 are hydrogen; and/or R 4 and R 5 are methyl. It is further preferred that:
R 9 , R 10 , R 11 , R 12 , R 14 , R 15 , R 16 and R 17 are all hydrogen; R 13 is methyl; and R 8 is a primary carbon group, more preferably methyl; or
R 9 , R 10 , R 11 , R 12 , R 14 , R 15 , R 16 and R 17 are all hydrogen; R 13 is ethyl; and R 8 is a primary carbon group, more preferably ethyl; or
R 9 , R 10 , R 11 , R 12 , R 14 , R 15 , R 16 and R 17 are all hydrogen; R 13 is isopropyl; and R 8 is a primary carbon group, more preferably isopropyl; or
R 9 , R 10 , R 11 , R 12 , R 13 , R 15 , R 16 and R 17 are all hydrogen; R 13 propyl; and R 8 is a primary carbon group, more preferably n-propyl; or
R 9 , R 10 , R 11 , R 12 , R 14 , R 15 , R 16 and R 17 are all hydrogen; R 13 is chloro; and R 8 is a halogen, more preferably chloro; or
R 9 , R 10 , R 11 , R 12 , R 14 , R 15 , R 16 and R 17 are all hydrogen; R 13 is trihalomethyl, more preferably trifluoromethyl; and R 8 is a trihalomethyl, more preferably trifluoromethyl.
In another preferred embodiment of (I), R 6 and R 7 are, respectively
wherein
R 18 is a halogen, a primary carbon group, a secondary carbon group or a tertiary carbon group; and
R 19 , R 20 , R 23 and R 24 are each independently hydrogen, hydrocarbyl, substituted hydrocarbyl or a functional group;
Provided that:
when R 18 is a halogen or primary carbon group none, one or two of R 21 , R 22 and R 25 are a halogen or a primary carbon group, with the remainder of R 21 , R 22 and R 25 being hydrogen; or
when R 18 is a secondary carbon group, none or one of R 21 , R 22 and R 25 is a halogen, a primary carbon group or a secondary carbon group, with the remainder of R 21 , R 22 and R 25 being hydrogen;
when R 18 is a tertiary carbon group, none or one of R 21 , R 22 and R 25 is a tertiary carbon group, with the remainder of of R 21 , R 22 and R 25 being hydrogen;
and further provided that any two of R 18 , R 19 , R 20 , R 21 , R 22 , R 23 , R 24 and R 25 vicinal to one another, taken together may form a ring.
In the above formulas (VIII) and (IX), R 18 corresponds to the second ring atom adjacent to the first ring atom bound to the imino nitrogen, and R 21 , R 22 and R 25 correspond to the other ring atoms adjacent to the first ring atom.
In compounds (I) containing (VIII) and (IX), it is particularly preferred that:
if R 18 is a primary carbon group, R 22 is a primary carbon group, and R 21 and R 25 are hydrogen; or
if R 18 is a secondary carbon group, R 22 is a primary carbon group or a secondary carbon group, more preferably a secondary carbon group, and R 21 and R 25 are hydrogen; or
if R 18 is a tertiary carbon group (more preferably a trihalo tertiary carbon group such as a trihalomethyl), R 22 is a tertiary carbon group (more preferably a trihalotertiary group such as a trihalomethyl), and R 21 and R 25 are hydrogen; or
if R 18 is a halogen, R 22 is a halogen, and R 21 and R 25 are hydrogen.
In all specific preferred compounds (I) in which (VIII) and (IX) appear, it is preferred that R 1 , R 2 and R 3 are hydrogen; and/or R 4 and R 5 are methyl. It is further preferred that:
R 19 , R 20 , R 21 , R 23 and R 24 are all hydrogen; R 22 is methyl; and R 18 is a primary carbon group, more preferably methyl; or
R 19 , R 20 , R 21 , R 23 and R 24 are all hydrogen; R 22 is ethyl; and R 18 is a primary carbon group, more preferably ethyl; or
R 19 , R 20 , R 21 , R 23 and R 24 are all hydrogen; R 22 is isopropyl; and R 18 is a primary carbon group, more preferably isopropyl; or
R 19 , R 20 , R 21 , R 23 and R 24 are all hydrogen; R 22 is n-propyl; and R 18 is a primary carbon group, more preferably n-propyl; or
R 19 , R 20 , R 21 , R 23 and R 24 are all hydrogen; R 22 is chloro or bromo; and R 18 is a halogen, more preferably chloro or bromo.
Compound (I) and its iron complexes (the oligomerization catalyst) may be prepared by a variety of methods, see for instance previously incorporated U.S. Pat. No. 5,955,555 and U.S. Pat. No. 6,103,946, as well as U.S. Pat. No. 6,232,259 and WO00/08034, both of which are also incorporated by reference herein for all purposes as if fully set forth.
It is preferred herein to react an iron complex of (I), such as a complex of (I) with FeCl 2 , with the cocatalyst (e.g., the alkylaluminum compound), preferably an aluminoxane such as methylaluminoxane, to form an active ethylene oligomerization species. The molar ratio of aluminum (as alkylaluminum compound) to iron (as a complex) in the oligomerization preferably is about 2000 or less. A more preferred upper limit is about 1500 or less, still more preferably about 1000 or less, and especially about 700 or less; and as a lower limit is about 5 or more, more preferably about 10 or more, still more preferably about 100 or more, even more preferably about 300 or more, and especially about 500 or more. For clarity, any combination of the aforementioned upper and lower limits may be used to define a preferred range herein such as, for example, from about 5 to about 1500, from about 5 to about 1000, from about 100 to about 1000, from about 500 to about 700, and other other such combination.
Another preferred range in accordance with the present invention is from about 5 to about 300. Within this range, a more preferred lower limit is about 10 or more, more preferably about 20 or more, still more preferably about 30 or more, and especially about 50 or more; and a more preferred upper limit about 200 or less, still more preferably about 150 or less, and especially about 100 or less. Again for clarity, any combination of the aforementioned upper and lower limits may be used to define a preferred range herein.
It should be noted that the above ranges refer to steady state operating conditions. Under certain circumstances, it may be beneficial to start the reaction under higher Al:Fe ratios then, in the course of the process stabilizing, lower the Al:Fe ratio to the desired steady state level. For example, the reaction could be started at above any of the upper ratio limits mentioned above, then reduced to the desired level at or above any of the lower ratio limits mentioned above.
Preferred alkylaluminum compounds include one or more of R 51 3 Al, R 51 AlCl 2 , R 51 2 AlCl, and “R 51 AlO” (alkylaluminoxanes), wherein R 51 is alkyl containing 1 to 25 carbon atoms, preferably 1 to 4 carbon atoms. Specific alkylaluminum compounds include methylaluminoxane (which is an oligomer with the general formula (MeAlO) n ), (C 2 H 5 ) 2 AlCl, C 2 H 5 AlCl 2 , (C 2 H 5 ) 3 Al and ((CH 3 ) 2 CHCH 2 ) 3 Al. A preferred alkylaluminum compound is an aluminoxane, especially methyl aluminoxane.
The conditions for the oligomerization described in previously incorporated U.S. Pat. No. 6,103,946 and parent application Ser. No. 09/906,974 (filed Jul. 17, 2001), entitled “MANUFACTURING PROCESS FOR ALPHA-OLEFINS”, may otherwise be followed.
For example, the oligomerization reaction may be run at a wide range of temperatures generally ranging from about −100° C to about +300° C., preferably about 0° C. to about 200° C., and more preferably about 20° C. to about 100° C. Pressures may also vary widely, ranging from an ethylene pressure (gauge) of from about 0 kPa to about 35 MPa, more preferably from about 500 kPa to about 15 MPa.
The process may be run in gas or liquid phase, but is typically run in liquid phase, preferably using an aprotic organic liquid. The process ingredients and products may or may not be soluble in these liquids, but obviously these liquids should not prevent the oligomerization from ocurring. Suitable liquids include alkanes, alkenes, cycloalkanes, selected halogenated hydrocarbons and aromatic hydrocarbons. Specific useful liquids include hexane, toluene, benzene and the α-olefins themselves.
The ethylene oligomerizations herein may also initially be carried out in the solid state by, for instance, supporting and active catalyst and/or aluminum compound on a substrate such as silica or alumina. Alternatively a solution of the catalyst precursor may be exposed to a support having an alkylaluminum compound on its surface. These “heterogeneous” catalysts may be used to catalyze oligomerization in the gas phase or the liquid phase. By “gas phase” is meant that the ethylene is transported to contact with the catalyst particle while the ethylene is in the gas phase. In general, the oligomerization may be run as a continuous gas phase, solution or slurry processes.
It is particularly preferred to run the oligomerization as “essentially single phase liquid full”, which means that at least 95 volume percent of the reactor volume is occupied by a liquid that is a single phase. Small amounts of the reactor volume may be taken up by gas, for example ethylene may be added to the reactor as a gas, which dissolves rapidly under the process conditions. Nevertheless, some small amount of dissolving ethylene gas may be present. Not counted in the reactor volume is any solid resulting from fouling of the reactor. See, for example, previously incorporated parent application Ser. No. 09/906,974 (filed Jul. 17, 2001), entitled “MANUFACTURING PROCESS FOR ALPHA-OLEFINS”.
These molar ratios of Al:Fe described herein are based on the process ingredients, that is, the ingredients comprising the reactor feed; therefore, it is preferred at such low molar Al:Fe ratios to purify the process ingredients so that the alkylaluminum compounds are not “used up” reacting with moisture or other impurities.
Using the oligomerization catalysts described herein a mixture of α-olefins is obtained. A measure of the molecular weights of the olefins obtained is factor K from the Schulz-Flory theory (see for instance B. Elvers, et al., Ed. Ullmann's Encyclopedia of Industrial Chemistry, Vol. A13, VCH Verlagsgesellschaft mbH, Weinheim, 1989, p. 243-247 and 275-276). This is defined as:
K=n (C n+2 olefin)/ n (C n olefin)
wherein n(C n olefin) is the number of moles of olefin containing n carbon atoms, and n(C n+2 olefin) is the number of moles of olefin containing n+2 carbon atoms, or in other words the next higher oligomer of C n olefin. From this can be determined the weight (mass) fractions of the various olefins in the resulting oligomeric reaction product mixture. The K factor is preferred to be in the range of about 0.65 to about 0.8 to make the α-olefins of the most commercial interest. This factor can be varied to some extent, see for instance previously incorporated U.S. Pat. No. 6,103,946 and parent application Ser. No. 09/906,974 (filed Jul. 17, 2001), entitled “MANUFACTURING PROCESS FOR ALPHA-OLEFINS”. | A manufacturing process for α-olefins using certain iron containing ethylene oligomerization catalysts together with alkylaluminum cocatalysts, in which using a low ratio of Al:Fe in the process results in a lowered formation of undesired polyethylene waxes and polymer. This results in less fouling of the process lines and vessels in the manufacturing plant. | 2 |
FIELD OF THE INVENTION
[0001] This invention relates to measurement instruments, and more particularly, to a method and relative device for sensing modulus and phase or a real part and an imaginary part of the electrical impedance of biologic tissues.
BACKGROUND OF THE INVENTION
[0002] Measurements of electrical impedance of the human body (bioimpedance) have been studied, in bioengineering, since 1960s. These measurements include forcing an alternating current (AC) through the body (usually at a frequency higher than 10 kHz to reduce interference with the electrical activity of nervous and muscular tissues), and sensing the voltage drop between two points.
[0003] Water and body fluids (blood, intra and extra cellular fluid, for example) provide the conductive medium. Several measures and studies have been conducted by applying this technique in different parts or regions of the body and using different frequencies to target different biological information (See for example, Deok-Won Kim, Detection of physiological events by impedance , Yonsei Medical Journal, 30(1), 1989). In numerous applications only the absolute value of the bioimpedance is to be determined because it is easier to calculate and provides much information. In other applications, both modulus and phase of the complex bioimpedance are measured.
[0004] It may be a relatively difficult to determine precise and reliable mathematical models of bioimpedance, particularly in the thoracic region. The main factors influencing electrical impedance in the chest are: the blood present in the heart and in the aorta; and the pleural fluids and the pulmonary circulation. Heart pumping, causing a varying spatial distribution of blood in the heart-aorta region, and respiration cause non-negligible variations of thoracic bioimpedance (i.e. the impedance of biologic tissues). From these variations it may even be possible to determine heart rate, breath rate, and evaluate cardiac output (volume of blood pumped by the heart for unity of time).
[0005] The measurements may be carried out using two or four electrodes, as schematically shown in FIG. 1 . When using two electrodes, the measured impedance is the sum of the bioimpedance Zbody and of the contact impedance Ze at the electrodes. Generally, the impedance Ze disturbs the measurement of the impedance Zbody. Using a more refined four electrode setup, it may be possible to measure the impedance Zbody as a ratio between the measured voltage drop and the current forced through the body tissues with increased precision, because the measurement is no longer affected by the contact impedance Ze.
[0006] There is an increasing interest about methods of carrying out these measurements, because it is generally a non-invasive technique and may be correlated to a vast range of physiological parameters. Thus it may be seen as having a strong potential in many medical fields. Furthermore, simplicity of measurements, integratability, reduced size, and low cost of the equipment, may make the technique of measuring thoracic bioimpedance particularly suitable to be implemented in wearable or implantable health monitoring systems.
[0007] Generally, the voltage V Z (t) sensed on the electrodes is an AC signal that is modulated by the bioimpedance Z(t);
[0000] V Z ( t )= Z ( t ) I 0 sin(ω t )
[0000] With an AM demodulator it may be possible to obtain a base-band signal representing the modulus |Z(t)| of the impedance. The phase of Z(t) may be evaluated, for example, by measuring the delay between the input current and output voltage or with a phase and quadrature demodulation.
[0008] A block diagram of a typical circuit for measuring the impedance of a biologic tissue is illustrated in FIG. 2 . An AC voltage generated by an oscillator is used to control a voltage-to-current converter that delivers a current Iz that is injected through the biologic tissue using two or four electrodes. The voltage on the biologic tissue is sensed, amplified, and AM demodulated for obtaining a base-band signal. The DC component Z 0 and the AC component deltaZ of the obtained base-band signal are extracted using a low-pass filter LPF and a high-pass filter HPF and converted into digital form by an analog-to-digital converter ADC. This type of system is characterized by the presence of an instrumentation amplifier (INA) upstream the AM demodulator.
[0009] A drawback of such a signal processing path is the fact that the INA operates on the modulated input signal. For this reason, the known architecture of FIG. 2 requires either an INA of sufficiently large bandwidth and thus having a large current consumption, or the use of a relatively low frequency of the current that is injected in the body tissues for carrying out the measurement. This is a limitation, because INAs, especially low power consumption and low cost devices, usually have a relatively narrow bandwidth.
[0010] U.S. patent application publication No. 2009/234,262 discloses a device for measuring the impedance of a biologic tissue having a differential amplifier connected to the electrodes and an AM demodulator of the differentially amplified signal. This prior device has the same drawbacks of the prior device of FIG. 2 .
[0011] Another known measurement system is depicted in FIG. 3 , as disclosed in Rafael González-Landaeta, Oscar Casas, and Ramon Pallás-Areny, Heart rate detection from plantar bioimpedance measurements, IEEE Transactions on Biomedical Engineering, 55(3):1163-1167, 2008. AM demodulation is performed upstream the INA to increase the CMRR. The circuitry is fully differential and a differential stage with coupled amplifiers is used as first stage of the voltage drop on the electrodes. A high pass filter HPF and amplifier stage is used for extracting the AC components of the signal, deltaZ, that in many applications (for example thoracic bioimpedance measurement), including important physiological information.
[0012] By resuming, in the cited prior devices, there is an input amplification stage for amplifying (and, eventually, filtering) the signals collected on the electrodes and, downstream, a demodulation circuit for extracting the base-band components thereof.
[0013] U.S. Pat. No. 4,909,261 discloses a device for measuring impedances of biologic tissues has two pairs of electrodes coupled through transformers to a circuit. The circuit applies a same AC voltage to the electrodes. The device also includes as many differential AM demodulators, each coupled to a respective pair of electrodes through a respective transformer. A circuit combines the AC and DC components of the two AM demodulated signals for measuring the impedance of the biologic tissue.
[0014] Each AM signal to be differentially demodulated is collected on the same pair of electrodes used to force current throughout a respective portion of the biologic tissue. Therefore, this prior device combines two demodulated AM signals not pertaining to the same portion of biologic tissue. Moreover, the presence of transformers may not make it suited for wearable applications.
[0015] A device that does not require any differential amplifier of the sensed voltage on the electrodes is disclosed in prior Italian patent application No. VA2010A000017, the applicant of which is the same as the present applicant. The device includes two single-ended AM demodulators respectively of the voltages towards ground of two electrodes, a differential amplifier of the base-band demodulated single-ended voltages, and a filter for extracting the DC and the AC components of the differential base-band voltage. An output circuit is adapted to generate an output signal representative of the impedance corresponding to the DC component of the base-band voltage.
SUMMARY OF THE INVENTION
[0016] Studies carried out by the applicant have led to the recognition that it is possible to realize a device implementing a related method of measuring electrical impedance of biologic tissues, particularly adapted for wearable applications. The device embeds at least a differential amplitude modulation (AM) demodulator of the voltage present on the electrodes. The differential AM demodulator generates a base-band signal, that eventually may be amplified with a low cost amplifier, from which an output circuit may generate output signals of the device representing the impedance of the biologic tissue between the electrodes.
[0017] According to an embodiment adapted to estimate the real part and the imaginary part of bioimpedances, the device includes a second differential AM demodulator, one demodulating the differential voltage on the electrodes with a carrier in phase with the current injected throughout the biologic tissue by the electrodes. The device also includes the other AM demodulator demodulating the same differential voltage with a second carrier in quadrature in respect to the first carrier. Preferably, the first and second carriers are square-wave oscillating signals, and the output circuit of the device generates signals representative of the real part and of the imaginary part of the impedance in the complex domain by processing the signals generated by the two AM demodulators according to two parametric polynomial functions.
[0018] According to a particular embodiment of the method of measuring impedance of biologic tissues, the parameters of the two parametric polynomial functions are adjusted using values stored in a look-up table using as entry value either:
the phase difference between the voltage on the electrodes and the current forced throughout the biologic tissue, or the ratio between the demodulated signals generated by the two differential AM demodulators.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] FIG. 1 illustrates two architectures for measuring the impedance of a biologic tissue in accordance with the prior art.
[0022] FIG. 2 is a schematic diagram of an architecture for measuring the impedance of a biologic tissue in accordance with the prior art.
[0023] FIG. 3 is a schematic diagram of an architecture disclosed in Rafael González-Landaeta, Oscar Cases, and Ramon Pallás-Areny, Heart rate detection from plantar bioimpedance measurements , IEEE Transactions on Biomedical Engineering, 55(3):1163-1167, 2008 for measuring impedance of biologic tissues in accordance with the prior art.
[0024] FIG. 4 is a schematic diagram of a device for measuring impedance of biologic tissues having a differential AM demodulator directly connected to the electrodes in accordance with the present invention.
[0025] FIG. 5 is a device generating an electrocardiogram (ECG), having a channel for sensing the impedance of biologic tissues using a square-wave AM demodulating carrier in accordance with the present invention.
[0026] FIG. 6 is a more detailed schematic diagram of another architecture of the device that uses a square-wave AM demodulating carrier for sensing the AC and the DC components of the real part of the impedance in the complex domain in accordance with the present invention.
[0027] FIG. 7 is a graph of the voltage on the electrodes vs. the phase of the impedance in the complex domain when a resynchronization technique is implemented and when it is not implemented.
[0028] FIG. 8 is a graph of a test case of the error in estimating the modulus of the impedance vs. the phase thereof with and without using a compensation technique.
[0029] FIG. 9 is a graph of the ratio between an impedance modulus Z 0 estimated by injecting a sinusoidal current with the electrodes and by using a demodulating square-wave and the effective modulus M of the impedance of a biologic tissue for various phase angles of the impedance in the complex domain, with and without applying a resynchronization technique.
[0030] FIG. 10 is a schematic diagram of an embodiment of a device for measuring impedance of biologic tissues having two differential AM demodulators directly connected to the electrodes in accordance with the present invention.
[0031] FIG. 11 is a schematic diagram of a two-channel architecture of a device that uses square-wave AM demodulating carriers in quadrature for generating signals representing the real part and the imaginary part of the impedance in the complex domain in accordance with the present invention.
[0032] FIGS. 12 a and 12 b are graphs of percentage error on the estimation of the real part and of the imaginary part vs. the phase of the impedance in the complex domain.
[0033] FIG. 13 a is a graph of the corrected and the uncorrected ratio between the estimations of the real part and of the imaginary part vs. the phase of the impedance in the complex domain.
[0034] FIG. 13 b is a graph of the error on the estimations of the real part and of the imaginary part vs. the phase of the impedance in the complex domain.
[0035] FIG. 14 is a graph of the error on the estimations of the real part and of the imaginary part and of the evaluated modulus of the impedance vs. the phase of the impedance in the complex domain when a compensation technique is implemented.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0036] An embodiment of a device for measuring the impedance of biologic tissues is illustrated in FIG. 4 . The circuit blocks in common with the prior devices of FIGS. 2 and 3 are identified by the same labels.
[0037] The applicant found that it is not necessary to amplify the voltage on the electrodes that inject a current throughout a biologic tissue, and thus, that it is possible to connect directly the AM differential demodulator directly to the electrodes as shown in FIG. 4 . The demodulated base-band signal is, in most practical cases, adapted to be amplified and processed for generating signals representing with a sufficient accuracy the modulus and the phase of the impedance in the complex domain. The so AM demodulated base-band differential signal may be supplied in input to an INA, that generates an amplified replica thereof.
[0038] Differently from the known device of FIG. 2 , the INA amplifies always a base-band signal, thus it has a large gain and a relatively good CMRR in the base-band range of frequencies. Therefore it is possible to use a low cost and low power consumption INA.
[0039] According to an embodiment, the voltage generator VOLTAGE GENERATOR generates a sinusoidal voltage, to force a sinusoidal current throughout the electrodes. According to a more preferred embodiment, throughout the electrodes, a square-wave current is forced and the AM demodulated base-band signal is obtained by demodulation using a square-wave demodulating carrier. Therefore, in this particular case the block VOLTAGE GENERATOR generates a square-wave voltage that is converted into a square-wave current injected throughout the biologic tissue. In this embodiment the realization of the differential AM demodulator is simplified and the resulting AM demodulated base-band signal may be processed, as will be shown hereinafter, to generate signals that represent accurate estimations of the modulus and the phase (or of the real part and of the imaginary part) of the impedance.
[0040] In a four electrode configuration, as the architecture shown in FIG. 4 , it is optionally possible to connect an ECG front-end to measure also the electrocardiogram of a patient. An architecture of a device for measuring the impedance of biologic tissues and for generating an ECG of a patient is illustrated in FIG. 5 . The blocks X include two pairs of switches controlled in phase opposition by the control phases φ 1 and φ 2 , as shown in FIG. 5 . The function of each block is resumed in the following table:
[0000]
INPUT STAGE
Instrumentation Amplifier stage
OS
Output stage with chopping spike filter
PGA
Programmable Gain Amplifier
≈
Analog Filter
x1
Voltage buffer
X
Chopper switches
[0041] The frequency spectra on the right side of FIG. 5 highlights that the output of the channel at the top of the figure is the sum of a base-band signal representing the ECG of the patient and of a modulated signal at the switching frequency f of the square-waves φ 1 and φ 2 , that represent the impedance of the biologic tissue between the electrodes. The channel at the bottom of the figure outputs the sum of a base-band signal representing the impedance of the biologic tissue between the electrodes and of a modulated signal at the switching frequency f of the square-waves φ 1 and φ 2 , that represent the ECG of the patient. Low-pass filters (not shown in the figure) extract the base-band signals representing the ECG and the impedance from the output signals of the two channels.
[0042] Injecting a square-wave current throughout the biologic tissue greatly simplifies the architecture of the differential AM demodulator and also of the AM modulator. Moreover, using a differential AM demodulator immediately downstream from the electrodes without interposing any signal processing stage between the demodulator and the electrodes, allows to use an amplification stage INPUT STAGE with a reduced bandwidth, because it has to amplify a base-band signal.
[0043] A more detailed representation of an architecture of a device for measuring electrical impedance of biologic tissues is illustrated in FIG. 6 . Given that the current injected throughout the biologic tissue is a square-wave, the AM demodulator immediately downstream the electrodes may be easily realized with two pairs of switches controlled in phase opposition by the control phases φ 1 and φ 2 . In the embodiment of FIG. 6 , the amplifier INA generates signals that represent the AC (ReM AC) and the DC (ReM DC) components of the real part ReM of the impedance in the complex domain. A digital circuit DIGITAL PART processes the signals ReM AC and ReM DC and generates signals representing the modulus and the phase of the impedance of the biologic tissue under test.
[0044] In some applications, the parameter of interest is the modulus of the bioimpedance, that may be roughly approximated with the real part of the impedance in the complex domain, that is greater than the imaginary part. According to a more accurate method of estimating the modulus of the bioimpedance, the demodulating carrier is resynchronized with the sensed voltage on the electrodes using the technique disclosed in Italian patent application No. VA2010A000078 in the name of the applicant of the present application. Both the above mentioned methods may be relatively easily implemented with the devices disclosed herein.
[0045] In particular, the method disclosed in the Italian patent application No. VA2010A000078 may be implemented in the device of FIG. 10 , even if this prior method has been disclosed only for AC currents injected throughout the tissue, and allows accurate estimation of the modulus of the bioimpedance. For illustrative purposes, the graph of FIG. 7 compares, obtained in a test case, the voltages sensed on the electrodes and the mean values thereof (that estimate the modulus of the bioimpedance) when a square-wave current is injected in a biologic tissue with and without applying the resynchronization technique disclosed in the cited prior Italian patent application, assuming that the correct value of the modulus of the bioimpedance is 100. It is evident that the resynchronization technique relevantly improves the accuracy of the estimations given by the mean values of the sensed voltages. The graph in FIG. 8 illustrates the corresponding percentage error vs. the phase of the bioimpedance without implementing the cited prior resynchronization technique and implementing it with different resynchronization steps.
[0046] It is also possible to estimate the impedance of biologic tissues by forcing an AC sinusoidal current therethrough, and by demodulating the voltage on the electrodes with a square-wave carrier. In this case, only the main harmonic of the square-wave demodulating carrier contributes in generating the base-band AM demodulated signal. For this reason, the graph of the ratio between the amplitude Z 0 of the base-band signal and the modulus M of the bioimpedance is as shown in FIG. 9 , as a function of the phase difference between the voltage on the electrodes and the square-wave demodulating carrier.
[0047] Therefore, the modulus M of the bioimpedance may be obtained by multiplying the amplitude Z 0 of the base-band signal by a correction factor k:
[0000] M=k*Z 0.
[0048] The values of the correction factor k for various phase angles may be heuristically estimated with tests and stored in a look-up table. With this technique, when the phase angle of the bioimpedance is known, for example, by using a resynchronization technique as disclosed in Italian patent application No. VA2010A000078, it may be possible to determine the value of the correction factor k, and thus obtain the modulus of the bioimpedance.
[0049] Another architecture of the device with two demodulation channels for determining in-phase and quadrature components of the bioimpedance in the complex domain is shown in FIG. 10 . The blocks with the same name of those of FIG. 5 have the same function. Taking into consideration what has been stated for the architecture of FIG. 5 , the functioning of the architecture of FIG. 10 will be immediately evident and for this reason this last architecture will not be further described.
[0050] An architecture similar to that of FIG. 6 for the device of FIG. 10 is illustrated in FIG. 11 . Differently from the embodiment depicted in FIG. 6 , the voltage on the electrodes is AM demodulated with a square-wave carrier in phase (φ=0°) and in quadrature (φ=90°) to generate signals that represent the AC and DC components of the real part V ReM and of the imaginary part V ImM of the bioimpedance in the complex domain.
[0051] Exemplary graphs of percentage error vs. the phase of the bioimpedance in the complex domain for the real part ReM and for the Imaginary part ImM thereof are illustrated in FIGS. 12 a and 12 b.
[0052] According to an innovative aspect, the signals V ReM and V ImM are processed by the block DIGITAL PART for generating signals representing in a very accurate fashion the effective modulus and phase of the bioimpedance. This is done substantially by calculating the effective real ReC and imaginary ImC parts of the bioimpedance using the following parametric equations:
[0000]
ReC=b
R
*V
ReM
+c
R
*V
ImM
[0000]
IMC=b
I
*V
ImM
+c
I
*V
ImM
2
[0000] wherein b R , c R , b I and c I are fixed parameters.
[0053] According to an embodiment, the impedance is assumed capacitive-resistive, and the parameters b R , c R , b I and c I are about equal to 0.0606, −0.02, 0.093 and 0.0000056, respectively. As a general rule, the values of the parameters b R , c R , b I and c I depend on the working frequency and may be heuristically determined with tests depending on the application and stored in a look-up table in function of the values of the signals V ReM and V ImM .
[0054] According to another embodiment, the parameters c R and c I are null, and the values of the parameters b R and b I are adjusted according to the following procedure:
[0055] preliminarily filling-in a look-up table of heuristically determined values of the parameters b R and b I as a function of phase differences between the square wave input current and the corresponding differential voltage; sensing the phase difference between the square wave input current and the corresponding differential voltage; and updating the values of the parameters b R and b I with the values stored in the look-up table corresponding to the sensed phase difference.
[0056] Substantially, according to this embodiment, the phase of the bioimpedance is used as an indicator that allows adjustment of the values of the parameters b R and b I . Exemplary percentage error characteristics vs. the phase of the bioimpedance on the estimated real part ReC and imaginary part ImC of the bioimpedance, and the estimated modulus M of the bioimpedance obtained using the above method are compared in the graph of FIG. 14 .
[0057] The phase of the bioimpedance may not be used as the indicator that allows adjustment of the parameters b R and b I . Instead, any quantity tied to the phase with a bijective law may be used.
[0058] Referring to the graph in FIG. 13 a , it is possible to notice that the ratio V ImM /V ReM is bijectively tied to the phase of the bioimpedance, i.e. by knowing the ratio V ImM /V ReM it is possible to determine the phase of the bioimpedance, and thus to adjust the values of the parameters b R and b I to estimate the effective ratio Im/Re between the imaginary part and the real part of the bioimpedance. The percentage error in approximating the effective real part and imaginary part with the values V ImM and V ReM is shown in the graph of FIG. 13 b.
[0059] Accordingly, the real part and the imaginary part of the bioimpedance are calculated with the following parametric equations:
[0000]
ReC=b
R
*V
ReM
+C
R
*V
ImM
[0000]
ImC=b
I
*V
ImM
+c
I
*V
ImM
2
[0000] being c R and c I null, wherein the values of the parameters b R and b I are adjusted according to the following procedure: preliminarily filling-in a look-up table of heuristically determined values of the parameters b R and b I in function of ratios between the demodulated signals first V ReM and second V ImM ; calculating the ratio between the demodulated signals first V ReM and second V ImM ; and updating the values of the parameters b R and b I with the values stored in the look-up table in correspondence of the calculated ratio. | A device for measuring an electrical impedance of biologic tissue may include electrodes configured to contact the biologic tissue and generate a differential voltage thereon. The device may include a first circuit coupled to the electrodes and configured to force an oscillating input signal therethrough, and a differential amplitude modulation (AM) demodulator coupled to the plurality of electrodes. The differential AM demodulator may be configured to demodulate the differential voltage, and generate a base-band signal representative of the demodulated differential voltage. The device may further include an output circuit downstream from the differential AM demodulator and may be configured to generate an output signal representative of the electrical impedance as a function of the base-band signal. | 6 |
CROSS-REFERENCE TO RELATED APPLICATION
This is a divisional of U.S. application Ser. No. 297,354 filed Jan. 17, 1989, now abandoned which is a divisional of U.S. application Ser. No. 920,536 filed Oct. 20, 1986, now U.S. Pat. No. 4,822,801, which is a continuation-in-part of U.S. application Ser. No. 770,897 filed Aug. 30, 1985, now abandoned, which is a continuation-in-part of U.S. application Ser. No. 633,153 filed Jul. 20, 1984, now abandoned, and which claims priority to Irish Application 1666/85 filed Feb. 7, 1985.
BACKGROUND OF THE INVENTION
U.S. Pat. No. 4,341,784 discloses certain substituted 7-(3-amino-1-pyrrolidinyl)-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acids having the general formula: ##STR1## The compounds are disclosed to have antibacterial activity.
The Journal of Medicinal Chemistry, 23, 1358 (1980) discloses certain substituted quinoline-3-carboxylic acids having the structural formula ##STR2## wherein ##STR3## may be pyrrolidinyl. See also U.S. Pat. No. 4,146,719. The compounds are disclosed to have antibacterial activity.
European Patent Application 81 10 6747, Publication Number 047,005, published Mar. 10, 1982, discloses certain benzoxazine derivatives having the structural formula ##STR4## wherein A is halogen and B may be a cyclic amine substituent such as pyrrolidine, or piperidine.
Certain 7-heterocyclic substituted 1,8-naphthyridines are disclosed in Eur. J. Med. Chem.-Chimica Therapeutica, 29, 27 (1977). U.S. Pat. Nos. 3,753,993 and 3,907,808 disclose certain 7-pyridylquinolones.
The references teach that these compounds possess antibacterial activity.
SUMMARY OF THE INVENTION
The invention in a first generic chemical compound aspect are compounds having the structural formula I and II ##STR5## wherein Z is ##STR6## Y is NH 2 , NHR, NRR', OR, or OH wherein R and R' are each independently an alkyl of from one to six carbon atoms or a cycloalkyl of from three to six carbon atoms; X is CH, CF, CCl, CBr, COR, COH, CCF 3 , or N; n is 1, 2, 3, or 4; n' is 1, 2, 3, or 4 wherein n+n' is a total of 2, 3, 4, or 5, and n" is 0, 1, or 2; R 1 is hydrogen, alkyl having from one to six carbon atoms or a cation; R 2 is alkyl having from one to four carbon atoms, vinyl, haloalkyl, or hydroxyalkyl having from two to four carbon atoms, or cycloalkyl having three to six carbon atoms; R 3 is hydrogen, alkyl having from one to four carbon atoms or cycloalkyl having three to six carbon atoms; R 4 is hydrogen, alkyl from one to four carbon atoms, hydroxyalkyl having two to four carbon atoms, trifluoroethyl or R 7 CO-- wherein R 7 is alkyl having from one to four carbon atoms, or alkoxy having from one to four carbon atoms; R 5 is hydrogen, or alkyl having from one to three carbon atoms; R 6 is hydrogen or alkyl having from one to three carbon atoms; and the pharmaceutically acceptable acid addition or base salts thereof.
The preferred compounds of this invention are those wherein Z is ##STR7## Also preferred compounds of this invention are those wherein Z is ##STR8##
Other preferred compounds of this invention are those wherein R 1 is hydrogen or a pharmaceutically acceptable base salt such as a metal or amine salt.
Other preferred compounds of this invention are those wherein R 2 is ethyl, vinyl, 2-fluoroethyl, or cyclopropyl.
The most preferred compounds are those wherein X is N, CF, or CCl, Z is ##STR9## R 1 is hydrogen, R 2 is ethyl, vinyl, 2-fluoroethyl or cyclopropyl; n" is 0 or 1 and R 3 is hydrogen, methyl, ethyl, 1- or 2-propyl, Y is NH 2 or a pharmaceutically acceptable acid addition or base salt thereof.
Particularly preferred species of the invention are the compounds having the names:
8-amino-9-fluoro-3-methyl-10[(3-cyclopropylaminomethyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-(3-amino-1-pyrrolidinyl)-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid hydrochloride;
8-amino-9-fluoro-3-methyl-10-[3-(aminomethyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-[3-[(propylamino)methyl]-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-[3-[(2-hydroxyethyl)amino)methyl]-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-[3-[(2-propylamino)methyl]-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-[3-[(2,2,2-trifluoroethyl)amino]methyl]-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-[3-[(ethylamino)methyl]- 1-pyrrolidinyl]7oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-[2,7-diazaspiro[4.4]non-2-yl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-[7-(7-methyl-2,7-diazaspiro[4.4]non-2-yl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
8-amino-9-fluoro-3-methyl-10-[7-(7-ethyl-2,7-diazaspiro[4.4]non-2-yl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-(3-amino-1-pyrrolidinyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid hydrochloride;
1-ethyl-5-amino-6,8-difluoro-7-[3-(ethylamino)methyl-1-pyrrolidinyl)]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[3-(aminomethyl)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[3-(propylaminomethyl)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[3-(2-propylaminomethyl)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[3-(cyclopropylaminomethyl)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[2,7-diazaspiro[4.4]non-2-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[7-(7-methyl-2,7-diazaspiro[4.4]non-2-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[7-(7-ethyl-2,7-diazaspiro[4.4]non-2-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[3-[[(2-hydroxyethyl)amino]methyl]-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
1-ethyl-5-amino-6,8-difluoro-7-[3-[[(2,2,2-trifluoroethyl)amino]methyl]-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid;
5-amino-7-(3-amino-1-pyrrolidinyl)-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid;
5-amino-7-(3-amino-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid;
5-amino-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-7-[3-[(methylamino)methyl]-1-pyrollidinyl]-4-oxo-3-quinolinecarboxylic acid;
5-amino-7-(3-amino-1-pyrrolidinyl)-8-bromo-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid; and
5-amino-7-(3-amino-1-pyrrolidinyl)-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid.
The following process for preparing compounds of the formula ##STR10## wherein R 1 , R 2 , X, and Z are as defined for formula I which comprises reacting a compound having the following structural formula ##STR11## with an amine corresponding to the group Z wherein Z is the compound having the structural formula ##STR12## wherein all of the above terms are as defined in formulae I and II and L is a leaving group which is preferably fluorine or chlorine.
This invention also includes novel intermediates. In a second generic chemical aspect are compounds having the structural formula VII ##STR13## wherein X is CH, N, CF, CCl, CBr, CCF 3 , COH, or COR; Y is NH 2 , NHR, NRR', OR or OH wherein R and R" are each independently an alkyl of from one to six carbon atoms or a cycloalkyl of from three to six carbon atoms; R 1 is as defined above and the pharmaceutically acceptable acid addition or base salts thereof. The preferred compounds are those wherein X is CCl, CBr, or CF and Y is NH 2 , NHR, or NRR'.
Particularly preferred species of the invention are compounds having the names:
5-amino-8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid;
5-amino-8-bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid; and
5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid.
The invention also includes a pharmaceutical composition which comprises an antibacterially effective amount of a compound having structural formula I and the pharmaceutically acceptable salts thereof in combination with a pharmaceutically acceptable carrier.
The invention further includes a method for treating bacterial infections in a mammal which comprises administering an antibacterially effective amount of the above defined pharmaceutical composition to a mammal in need thereof.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The compounds of the invention having the structural formula III or IIIa may be readily prepared by treating a corresponding compound having the structural formula IV or V with the desired cyclic amine VIa or VIb. For purposes of this reaction, the alkylamine substituent of compound VIa or VIb may, if desired, be protected by a group which renders it substantially inert to the reaction conditions. Thus, for example, protecting groups such as the following may be utilized: carboxylic acyl groups such as formyl, acetyl, trifluoroacetyl; alkoxycarbonyl groups such as ethoxycarbonyl, t-butoxycarbonyl, β,β,β-trichloroethoxycarbonyl, β-iodoethoxycarbonyl; aryloxycarbonyl groups such as benzyloxycarbonyl, p-methoxybenzyloxycarbonyl, phenoxycarbonyl; silyl groups such as trimethylsilyl; and groups such as trityl, tetrahydropyranyl, vinyloxycarbonyl, o-nitrophenylsulfenyl, diphenylphosphinyl, p-toluenesulfonyl, and benzyl, may all be utilized. The protecting group may be removed, after the reaction between compound IV or V and compound VIa or VIb if desired, by procedures known to those skilled in the art. For example, the ethoxycarbonyl group may be removed by acid or base hydrolysis and the trityl group may be removed by hydrogenolysis.
The reaction between the compound of structural formula IV or V and a suitably protected compound of formula VIa or VIb, may be performed with or without a solvent, preferably at elevated temperature for a sufficient time so that the reaction is substantially complete. The reaction is preferably carried out in the presence of an acid acceptor such as an alkali metal or alkaline earth metal carbonate or bicarbonate, a tertiary amine such as triethylamine, pyridine, or picoline. Alternatively an excess of the compound of formula VI may be utilized as the acid acceptor.
Convenient solvents for this reaction are nonreactive solvents such as acetonitrile, tetrahydrofuran, ethanol, chloroform, dimethylsulfoxide, dimethylformamide, pyridine, picoline, water, and the like. Solvent mixtures may also be utilized.
Convenient reaction temperatures are in the range of from about 20° to about 150° C.; higher temperatures usually require shorter reaction times.
The removal of the protecting group R 4 may be accomplished either before or after isolating the product, III. Alternatively, the protecting group R 4 need not be removed.
Some of the starting compounds having structural formulae IV and V are known in the art or, if new, may be prepared from known starting materials by standard procedures or by variations thereof. Thus the following compounds are disclosed in the noted references: ##STR14##
Other starting compounds having structural formula IV wherein Y is NRR' and R and/or R' are not hydrogen may be prepared from the known 5-amino quinolines or naphthyridines by an alkylation sequence shown below wherein L is a leaving group as previously defined. ##STR15##
The 5-amino group is preferably acylated by trifluoroacetic acid anhydride although other acyl moieties may be employed. The alkylation of R proceeds with the presence of sodium hydride or other nonnucleophilic bases. Removal of the acyl activating group is accomplished with acid or base hydrolysis such as 2N hydrochloric acid in acetic acid. A second alkylation, if desired, with R'L, again in the presence of base such as, for example, potassium carbonate provides compounds of formula IV where both R and R' are not hydrogen.
Alternatively, the 5-alkylamino compounds of formula II may be prepared from the nitro or amino acids IV through reductive amination procedures as illustrated in the following scheme. ##STR16## Using appropriate control of the aldehyde (RCHO) equivalents mono and disubstituted amines may be obtained. The substituted amino acids may be converted to the desired compounds of formula II by methods described in the references cited in the Background of the Invention.
The compounds of formula IV wherein Y is OR may be prepared from the polysubstituted acids or esters by displacement of an ortho leaving group with OR as shown: ##STR17##
Other compounds of formula IV wherein X is CH, CCl, CBr, COR, COH, CCF 3 or N are made by the sequence shown below according to the general methods in the references cited in the background of the invention. ##STR18##
The general pathway to the compounds of formula IV is illustrated with 2-nitro-3,4,5,6-tetrafluorobenzoyl chloride. This starting material is treated with n-butyl lithium and malonic half acid ester to form 2-nitro-3,4,5,6-tetrafluoro-β-oxo-benzene propanoic acid ethyl ester. This product can be converted to 5-nitro-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid ethyl ester by a three step reaction. The starting material is first treated with triethylorthoformate and subsequently with cyclopropyl amine in t-butyl alcohol. The product is ring closed with potassium t-butoxide to form 5-nitro-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid ethyl ester. This product is hydrogenated to form the corresponding 5-amino compound. This is then hydrolyzed to form 1-cyclopropyl-5-amino-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinoline carboxylic acid. Alternatively compounds of the formula IV may be prepared by a series of reactions illustrated with 3,4,5,6-tetrafluoroanthranilic acid. The acid is reacted with acetic anhydride and acetic acid to form 2-acetylamino-3,4,5,6-tetrafluorobenzoic acid. This compound is reacted with oxalyl chloride and dichloromethane in the presence of N,N-dimethylformamide catalyst to form 2-acetylamino-3,4,5,6-tetrafluorobenzoyl chloride. This product is treated with n-butyl lithium and malonic half acid ester to form 2-acetylamino-3,4,5,6-tetrafluoro-β-oxobenzenepropanoic acid ethyl ester.
This product can be converted to 5-acetylamino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid ethyl ester by a three step reaction. The 2-acetylamino-3,4,5,6-tetrafluoro-β-oxobenzene-propanoic acid ethylester is first treated with triethylorthoformate and acetic anhydride. After removal of the solvent the residue is treated with a solution of cyclopropylamine in t-butanol. After the reaction is complete a solution of potassium t-butoxide in t-butanol is added. The resulting product is 5-acetylamino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid ethyl ester. The ester is hydrolyzed to form 1-cyclopropyl-5-amino-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid.
The compounds of the invention having structural formula VIa or VIb are either known compounds or they may be prepared from known starting materials by standard procedures or by variations thereof. For example, 3-pyrrolidinemethanamines having the structural formula D ##STR19## may be readily prepared from the known starting material methyl 5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxylate, A, [J. Org. Chem., 26, 1519 (1961)] by the following reaction sequence. ##STR20##
The compound wherein R 3 is hydrogen, namely 3-pyrrolidinemethanamine, has been reported in J. Org. Chem., 26, 4955 (1961).
Thus compound A may be converted to the corresponding amide B by treatment with R 3 NH 2 ; for example, a saturated solution of ethylamine in an alkanol such as methyl alcohol may be utilized. The diamide B may next be reduced to produce the corresponding diamine C. This reduction may be carried out using lithium aluminum hydride, for example, in a convenient solvent such as tetrahydrofuran. Compound C may next be debenzylated, for example using hydrogen and 20% palladium on carbon catalyst to produce the diamine D. Alternatively, when R=H in C, the primary amine function may be protected with a group R 4 as defined, hereinabove. For example, the primary amine function may be acylated with an acyl halide such as acetyl chloride by well known procedures. The primary amine function of C may also be converted to a carbamate ester such as the ethyl ester by treatment with ethyl chloroformate in the presence of a strong base such as 1,8-diazabicyclo[5.4.0]undec-7-ene in a convenient solvent such as methylene chloride. The benzyl group may next be removed, for example as described above for compound C, thereby producing compound D where R is --CO 2 Et, which after conversion to a compound of the type VIa or VIb may be reacted with a compound having the structural formula IV or V to thereby produce a corresponding compound having the structural formula I or Ia. The --CO 2 Et group may be removed by standard procedures.
Likewise spiroamino compounds represented by structural formula VIb may be readily prepared from the known starting material 3-ethoxycarbonyl-5-oxo-3-pyrrolidineacetic acid ethyl ester [J. Org. Chem. 46, 2757 (1981)] by the following reaction sequence. ##STR21##
The compound 2,7-diazaspiro[4.4]nonane where R 3 is H is described in the above reference. Thus compound E may be converted to the corresponding amide F by treatment with R 3 NH 2 , for example, methyl amine in water followed by benzylation which may be carried out with sodium hydride and benzyl chloride to give G. Reduction to the diamine H may be accomplished with lithium aluminum hydride. Subsequent debenzylation, for example, with hydrogen and 20% palladium on carbon catalyst produces the diamine J.
The compounds of the invention display antibacterial activity when tested by the microtitration dilution method as described in Heifetz, et al, Antimicr. Agents & Chemoth., 6, 124 (1974), which is incorporated herein by reference.
The compounds of the invention are capable of forming both pharmaceutically acceptable acid addition and/or base salts. Base salts are formed with metals or amines, such as alkali and alkaline earth metals or organic amines. Examples of metals used as cations are sodium, potassium, magnesium, calcium, and the like. Examples of suitable amines are N,N'-dibenzylethylenediamine, chloroprocaine, choline, diethanolamine, ethylenediamine, N-methylglucamine, and procaine.
Pharmaceutically acceptable acid addition salts are formed with organic and inorganic acids.
Examples of suitable acids for salt formation are hydrochloric, sulfuric, phosphoric, acetic, citric, oxalic, malonic, salicyclic, malic, gluconic, fumaric, succinic, ascorbic, maleic, methanesulfonic, and the like. The salts are prepared by contacting the free base form with a sufficient amount of the desired acid to produce either a mono or di, etc salt in the conventional manner. The free base forms may be regenerated by treating the salt form with a base. For example, dilute solutions of aqueous base may be utilized. Dilute aqueous soldium hydroxide, potassium carbonate, ammonia, and sodium bicarbonate solutions are suitable for this purpose. The free base forms differ from their respective salt forms somewhat in certain physical properties such as solubility in polar solvents, but the salts are otherwise equivalent to their respective free base forms for purposes of the invention. Use of excess base where R' is hydrogen gives the corresponding basic salt.
The compounds of the invention can exist in unsolvated as well as solvated forms, including hydrated forms. In general, the solvated forms, including hydrated forms and the like are equivalent to the unsolvated forms for purposes of the invention.
The alkyl groups contemplated by the invention comprise both straight and branched carbon chains of from one to about six carbon atoms. Representative of such groups are methyl, ethyl, propyl, isopropyl, and the like.
The cycloalkyl groups contemplated by the invention comprise those having three to six carbon atoms such as cyclopropyl, cyclobutyl, cyclopentyl, and cyclohexyl.
The alkoxy groups contemplated by the invention comprise both straight and branched carbon chains of from one to about six carbon atoms unless otherwise specified. Representative of such groups are methoxy, ethoxy, propoxy, i-propoxy, t-butoxy, hexoxy, and the like.
The term, haloalkyl, is intended to include halogen substituted straight and branched carbon chains of from two to four carbon atoms. Those skilled in the art will recognize that the halogen substitutent may not be present on the α-carbon atom of the chain. Representative of such groups are β-fluoroethyl, β-chloroethyl, β,β-dichloroethyl, β-chloropropyl, β-chloro-2-propyl, -iodobutyl, and the like.
The term halogen is intended to include fluorine, chlorine, bromine, and iodine unless otherwise specified.
Certain compounds of the invention may exist in optically active forms. The pure D isomer, pure L isomer as well as mixtures thereof; including the racemic mixtures, are contemplated by the invention. Additional asymmetric carbon atoms may be present in a substitutent such as an alkyl group. All such isomers as well as mixtures thereof are intended to be included in the invention.
The compounds of the invention can be prepared and administered in a wide variety of oral and parenteral dosage forms. It will be obvious to those skilled in the art that the following dosage forms may comprise as the active component, either a compound of formula I or a corresponding pharmaceutically acceptable salt of a compound of formula I.
For preparing pharmaceutical compositions from the compounds described by this invention, inert, pharmaceutically acceptable carriers can be either solid or liquid. Solid form preparations include powders, tablets, dispersible granules, capsules, cachets, and suppositories. A solid carrier can be one or more substances which may also act as diluents, flavoring agents, solubilizers, lubricants, suspending agents, binders, or tablet disintegrating agents; it can also be an encapsulating material. In powders, the carrier is a finely divided solid which is in admixture with the finely divided active compound. In the tablet the active compound is mixed with carrier having the necessary binding properties in suitable proportions and compacted in the shape and size desired. The powders and tablets preferably contain from 5 or 10 to about 70 percent of the active ingredient. Suitable solid carriers are magnesium carbonate, magnesium sterate, talc, sugar, lactose, pectin, dextrin, starch, gelatin, tragacanth, methyl cellulose, sodium carboxymethyl cellulose, a low melting wax, cocoa butter, and the like. The term "preparation" is intended to include the formulation of the active compound with encapsulating material as carrier providing a capsule in which the active component (with or without other carriers) is surrounded by carrier, which is thus in association with it. Similarly, cachets are included. Tablets, powders, cachets, and capsules can be used as solid dosage forms suitable for oral administration.
Liquid form preparations include solutions, suspensions and emulsions. As an example may be mentioned water or water-propylene glycol solutions for parenteral injection. Such solutions are prepared so as to be acceptable to biological systems (isotonicity, pH, etc). Liquid preparations can also be formulated in solution in aqueous polyethylene glycol solution. Aqueous solutions suitable for oral use can be prepared by dissolving the active component in water and adding suitable colorants, flavors, stabilizing, and thickening agents as desired. Aqueous suspension suitable for oral use can be made by dispersing the finely divided active component in water with viscous material, i.e., natural or synthetic gums, resins, methyl cellulose, sodium carboxymethyl cellulose, and other well-known suspending agents.
Preferably, the pharmaceutical preparation is in unit dosage form. In such form, the preparation is subdivided into unit doses containing appropriate quantities of the active component. The unit dosage form can be a packaged preparation, the package containing discrete quantities of preparation, for example, packeted tablets, capsules, and powders in vials or ampules. The unit dosage form can also be a capsule, cachet, or tablet itself or it can be the appropriate number of any of these packaged forms.
The quantity of active compound in a unit dose of preparation may be varied or adjusted from 1 mg to 100 mg according to the particular application and the potency of the active ingredient.
In therapeutic use as agents for treating bacterial infections the compounds utilized in the pharmaceutical method of this invention are administered at the initial dosage of about 3 mg to about 40 mg per kilogram daily. A daily dose range of about 6 mg to about 14 mg per kilogram is preferred. The dosages, however, may be varied depending upon the requirements of the patient, the severity of the condition being treated, and the compound being employed. Determination of the proper dosage for a particular situation is within the skill of the art. Generally, treatment is initiated with smaller dosages which are less than the optimum dose of the compound. Thereafter, the dosage is increased by small increments until the optimum effect under the circumstances is reached. For convenience, the total daily dosage may be divided and administered in portions during the day if desired.
The following nonlimiting examples illustrate the inventors' preferred methods for preparing the compounds of the invention.
PREPARATION OF STARTING MATERIALS
Example A
1-Ethenyl-6,7,8-trifluoro-1,8-dihydro-4-oxo-3-quinolinecarboxylic acid
6,7,8-Trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid ethyl ester was treated with dibromo ethane to afford the 1-ethenyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid ester, mp 134-135° C. Subsequent hydrolysis with hydrochloric acid gave 1-ethenyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, mp 186-187° C.
Example B
6,7,8-Trifluoro-1-(2-fluoroethyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid
In identical fashion, 6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid ethyl ester was converted to 6,7,8-trifluoro-1-(2-fluoroethyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, mp 207-211° C.
Example C
N-Methyl-3-pyrrolidinemethanamine
N-Methyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide
A mixture of 100 g (0.43 mole) of methyl 5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxylate [J. Org. Chem., 26, 1519 (1961)], 500 ml methanol and 100 g (3.2 mole) of methylamine was heated at 100° C. in a pressure reactor for 16 hours. The reaction mixture was cooled and the ammonia and methanol were removed under pressure. The residue was taken up in dichloromethane and washed 3×100 ml 1N sodium hydroxide. The organic layer was dried over magnesium sulfate and the solvent removed at reduced pressure to give 88.3 g of N-methyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide as a white solid, mp 82.5-83.0° C.
______________________________________Analysis calculated for C.sub.13 H.sub.16 N.sub.2 O.sub.2 :______________________________________ C, 67.22; H, 6.94; N, 12.06Found C, 66.98; H, 6.69; N, 12.02.______________________________________
This material was used in the next step.
N-Methyl-1-(phenylmethyl)-3-pyrrolidinemethanamine
To a suspension of 37.4 g (1.00 mole) lithium aluminum hydride in 1000 ml tetrahydrofuran, was added a solution of 88.3 g (0.380 mole) of N-methyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide in tetrafuran dropwise under nitrogen. The reaction was then refluxed overnight. The reaction flask was cooled in an ice bath and 37.4 ml of water 37.4 ml of 15% sodium hydroxide and 112.2 ml of water were added. The precipitated solids were filtered and washed with hot ethanol. The combined filtrates were concentrated, then dissolved in dichloromethane, filtered, dried over magnesium sulfate, and the solvent evaporated under reduced pressure to give 68.7 g of N-methyl-1-(phenylmethyl)-3-pyrrolidinemethanamine as an oil. This material was used without further purification in the step.
N-Methyl-3-pyrrolidinemethanamine
A mixture of 67.3 g (0.32 mole) of N-methyl-1-(phenylmethyl)-3-pyrrolidinemethanamine, 3 g of 20% palladium on carbon, and 600 ml of methanol was shaken in an atmosphere of hydrogen at about 4.5×10 5 Pa and at room temperature for 18 hours. Another 3 g of 20% palladium on carbon was added and the hydrogenation continued for 6.5 hours. Another 3.0 g of 20% palladium on charcoal was added and the hydrogenation continued for another 4.5 hours. The catalyst was filtered and the filtrate evaporated under reduced pressure. The residue was distilled under vacuum (72-76° C, 10.5 mm Hg) to give 8.32 g N-methyl-3-pyrrolidinemethanamine.
Example D
N-Ethyl-3-pyrrolidinemethanamine
N-Ethyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide
A mixture of 200 g (0.86 mole) of methyl-5-oxo-1-(phenylmethyl)pyrrolidinecarboxylate (J. Org. Chem., 26, 1519 (1961)], 1000 ml methanol and 200 g (4.4 mole) of ethylamine was heated at 100° C. in a pressure reactor for 17.2 hours. The reaction mixture was cooled and the excess ethylamine and methanol were removed under reduced pressure. The residue was taken up in dichloromethane and washed 3×150 ml 1N sodium hydroxide. The organic layer was dried over magnesium sulfate and the solvent removed at reduced pressure to give 104.6 g of N-ethyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide as a white solid, mp 97-99° C.
This materials was used in the next step.
N-Ethyl-1-(phenylmethyl)-3-pyrrolidinemethanamine
To a suspension of 108.8 g (2.86 mole) lithium aluminum hydride in 800 ml tetrahydrofuran, was added a solution of 194.5 g (0.79 mole) of N-ethyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide in 600 ml tetrahydrofuran dropwise under nitrogen. The reaction was then refluxed four hours. The reaction flask was cooled in an ice bath and 108 ml of water, 108 ml of 15% sodium hydroxide, and 324 ml of water were added. The precipitated solids were filtered and washed with hot ethanol. The combined filtrates were concentrated, then dissolved in dichloromethane, filtered, dried over magnesium sulfate, and the solvent evaporated under reduced pressure to give 151.9 g of N-ethyl-1-(phenylmethyl)-3-pyrrolidinemethanamine as an oil.
This material was used without further purification in the next step.
N-Ethyl-3-pyrrolidinemethanamine
A mixture of 151.6 g (0.69 mole) of N-ethyl-1-(phenylmethyl)-3-pyrrolidinemethanamine, 5 g of 20% palladium on carbon, and 1100 ml of ethanol was shaken in an atmosphere of hydrogen at about 4.5×10 5 Pa and at room temperature for 21.6 hours. Another 5 g of 20% palladium on carbon was added and the hydrogenation continued for 24 hours. The catalyst was filtered and the filtrate evaporated under reduced pressure. The residue was distilled under vacuum (88-91° C., 11.5 mm Hg) to give 66.0 g N-ethyl-3-pyrrolidinemethanamine.
Example E
N-(2,2,2-Trifluoroethyl)-3-pyrrolidinemethanamine
5-Oxo-1-(phenylmethyl)-N-(2,2,2-trifluoroethyl)-3-pyrrolidine carboxamide
A mixture of 21.9 g (0.10 mole) methyl 5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxylate in 150 ml tetrahydrofuran, was cooled to 0° C. in an ice bath under nitrogen and 24.3 g (0.15 mole) carbonyl diimidazole was added. The reaction was stirred at 0° C. for 30 minutes, then at room temperature for 30 minutes. A solution of 13.6 g (0.10 mole) of 2,2,2-trifluoroethylamine hydrochloride, 15.2 g (0.10 mole) 1,8-diazabicyclo[5.4.0]undec-7-ene and 100 ml tetrahydrofuran was added. The reaction was stirred at room temperature overnight. The solvent was removed at reduced pressure. The residue was taken up in dichloromethane and washed 3×150 ml saturated sodium bicarbonate. The organic layer was dried over magnesium sulfate and the solvent removed under reduced pressure. The product was purified by column chromatography on silica with ethyl acetate to give 8.50 g of 5-oxo-1-(phenylmethyl)-N-(2,2,2-trifluoroethyl)-3-pyrrolidinecarboxamide, mp 110-112° C.
This material was used in the next step.
1-(Phenylmethyl)-N-(2,2,2-trifluoroethyl)-3-pyrrolidinemethanamine
A mixture of 8.50 g (28.3 mole) of 5-oxo-1-(phenylmethyl)-N-(2,2,2-trifluoroethyl)-3-pyrrolidinecarboxamide in 100 ml tetrahydrofuran was added dropwise to 3.22 g (84.9 mmole) of lithium aluminum hydride in 50 ml tetrahydrofuran. The reaction was refluxed two hours, then stirred at room temperature overnight. The reaction was cooled in an ice bath and 3.2 ml of water, 3.2 ml of 15% sodium hydroxide, and 9.6 ml of water were added. The precipitated salts were filtered and washed with hot ethanol. The combined filtrates were concentrated under reduced pressure. The residue was taken up in dichloromethane, filtered, and dried over magnesium sulfate. The solvent was removed at reduced pressure to give 7.15 g of 1-(phenylmethyl)-N-(2,2,2-trifluoroethyl)-3-pyrrolidinemethanamine.
This material was used without further purification in the next step.
N-(2,2,2-Trifluoroethyl)-3-pyrrolidinemethanamine
A mixture of 7.15 g (26.3 mmole) 1-(phenylmethyl)-N-(2,2,2-trifluoroethyl)-3-pyrrolidinemethanamine 100 ml of methanol and 0.7 g of 20% palladium on carbon was shaken in an atmosphere of hydrogen at about 4.5×10 5 Pa and at room temperature for 24 hours. The catalyst was filtered and the filtrate evaporated under reduced pressure. The residue was distilled under vacuum (63-65° C., 2.8 mm Hg) to give 2.55 g of N-(2,2,2-trifluoroethyl)-3-pyrrolidinemethanamine.
Example F
N-Propyl-3-pyrrolidinemethanamine
5-Oxo-1-(phenylmethyl)-N-propyl-3-pyrrolidinecarboxamide
To a solution of 10.9 g (50 mmole) of 5-oxo-1-phenylmethyl)-3-pyrrolidinecarboxylic acid in 150 ml of acetonitrile was added 9.73 g (60 mmole) of 1,1'-carbonyldiimidazole. The reaction was heated to 60° C. for one hour, cooled to room temperature and treated with 4.13 g (70 mmole) of n-propylamine. After stirring for two hours, the solvent was removed in vacuo and the residue partitioned between ether and water. The organic layer was washed with water, 1N hydrochloric acid, dried over magnesium sulfate, filtered, and evaporated in vacuo to give 12.0 g of 5-oxo-1-(phenylmethyl)-N-propyl-3-pyrrolidinecarboxamide, mp 86-87° C.
1-(Phenylmethyl)-N-propyl-3-pyrrolidinemethanamine
To a suspension of 8.2 g (0.2 mole) of lithium aluminum hydride in 150 ml of dry tetrahydrofuran was added portionwise, 12.0 g (45.6 mmole) of solid 5-oxo-1-(phenylmethyl)-N-propyl-3-pyrrolidinecarboxamide. When the addition was complete, the reaction mixture was stirred at room temperature for 18 hours and then at reflux for two hours. After cooling to room temperature, the mixture was treated dropwise, successively, with 8 ml of water, 8 ml of 15% aqueous sodium hydroxide and 24 ml of water, titrating the final addition to produce a granular precipitate. The solid was removed by filtration, washed with tetrahydrofuran and the filtrate evaporated in vacuo to give 9.6 g of 1-(phenylmethyl)-N-propyl-3-pyrrolidinemethanamine, as a heavy syrup.
This material was used for the next step without further purification.
N-Propyl-3-pyrrolidinemethanamine
A mixture of 14.0 g (60.0 mmole) of 1-(phenylmethyl)-N-propyl-3-pyrrolidinemethanamine, 1.0 g of 20% palladium on carbon and 140 ml of methanol was shaken in an atmosphere of hydrogen at about 4.5×10 5 Pa and room temperature for 24 hours. The catalyst was removed by filtering through Celite, the filtrate concentrated and distilled in vacuo to give 7.1 g of N-propyl-3-pyrrolidinemethanamine, bp 49-50° C./0.25 mm.
Example G
N-Cyclopropyl-3-pyrrolidinemethanamine
5-Oxo-1-(phenylmethyl)-N-cyclopropyl-3-pyrrolidinecarboxamide
To a solution of 16.4 g (75 mmole) of 5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxylic acid in 150 ml of acetonitrile was added 13.8 g (85 mmole) of 1,1'-carbonyldiimidazole. The reaction was heated to 60° C. for one hour, cooled to room temperature and treated with 4.85 g (85 mmole) of cyclopropylamine. The reaction was stirred at room temperature for 18 hours, the solvent removed in vacuo and the residue partitioned between chloroform and water. The organic layer was washed with water, 1N hydrochloric acid, dried over magnesium sulfate, filtered, and evaporated in vacuo to give 18.3 g of 5-oxo-1-(phenylmethyl)-N-cyclopropyl-3-pyrrolidinecarboxamide, mp 94-96° C.
1-(Phenylmethyl)-N-cyclopropyl-3-pyrrolidine methanamine
To a suspension of 8.2 g (0.20 mole) of lithium aluminum hydride in 150 ml of dry tetrahydrofuran was added portionwise 18.0 g (70.0 mmole) of solid 5-oxo-1-(phenylmethyl)-N-cyclopropyl-3-pyrrolidinecarboxamide. When the addition was complete, the reaction mixture was stirred at room temperature for 18 hours and then at reflux for two hours. After cooling to room temperature, the mixture was treated dropwise, successively, with 8 ml of water, 8 ml of 15% aqueous sodium hydroxide and 24 ml of water, titrating the final addition to produce a granular precipitate. The solid was removed by filtration, washed with tetrahydrofuran and the filtrate evaporated in vacuo to give 16.0 g of 1-(phenylmethyl)-N-cyclopropyl-3-pyrrolidinemethanamine, as a heavy oil. This was used for the next step without further purification.
N-Cyclopropyl-3-pyrrolidinemethanamine
A mixture of 13.6 g (59.0 mmol) of 1-(phenylmethyl)-N-cyclopropyl-3-pyrrolidinemethanamine, 0.5 g of 20% palladium on carbon and 140 ml of methanol was shaken in an atmosphere of hydrogen at about 4.5×10 5 Pa and room temperature for 24 hours. The catalyst was removed by filtering through Celite, the filtrate concentrated and distilled in vacuo to give 6.3 g of N-cyclopropyl-3-pyrrolidinemethanamine, bp 88-90°/13 mm.
Example H
N-(2-Propyl)-3-pyrrolidinemethanamine
5-Oxo-1-(phenylmethyl)-N-(2-propyl)-3-pyrrolidinecarboxamide
To a solution of 16.4 g (75.0 mmole) of 5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxylic acid in 150 ml of acetonitrile was added 13.8 g (85.0 mmole) of 1,1-'carbonyldiimidazole. The reaction was heated to 60° C. for one hour, cooled to room temperature and treated with 5.0 g (85 mmole) of isopropylamine. The reaction was stirred at room temperature for 18 hours, the solvent removed in vacuo and the residue partitioned between chloroform and water. The organic layer was washed with water, 1N hydrochloric acid, dried over magnesium sulfate, and evaporated in vacuo to give 18.6 g of 5-oxo-1-(phenylmethyl)-N-(2-propyl)-3-pyrrolidinecarboxamide, mp 122-124° C.
1-(Phenylmethyl)-N-(2-propyl)-3-pyrrolidinemethanamine
To a suspension of 8.2 g (0.2 mole) of lithium aluminum hydride in 150 ml of dry tetrahydrofuran was added portionwise, 18.3 g (70.0 mmole) of solid 5-oxo-1-phenylmethyl)-N-(2-propyl)-3-pyrrolidinecarboxamide. When the addition was complete, the reaction mixture was stirred at room temperature for 18 hours and then refluxed for two hours. After cooling to room temperature, the mixture was treated dropwise, successively, with 8 ml of water, 8 ml of 15% aqueous sodium hydroxide and 24 ml of water, titrating the final addition to produce a granular precipitate. The solid was removed by filtration, washed with tetrahydrofuran and the filtrate evaporated in vacuo to give 15.6 g of 1-(phenylmethyl)-N-(2-propyl)-3-pyrrolidinemethanamine as a heavy syrup.
This materials was used for the next step without further purification.
N-(2-Propyl)-3-pyrrolidinemethanamine
A mixture of 13.4 g (58.0 mmol) of 1-phenylmethyl-N-(2-propyl)-3-pyrrolidinemethanamine, 1.0 g of 20% palladium on carbon and 130 ml of methanol was shaken in an atmosphere of hydrogen at about 4.5×10 5 Pa and room temperature for 24 hours. The catalyst was removed by filtration through Celite; the filtrate concentrated and distilled in vacuo to give 6.3 g of N-(2-propyl)-3-pyrrolidinemethanamine, bp 58-60° C./3.5 mm.
Example I
1,1-Dimethylethyl(3-pyrrolidinyl)carbamate
1,1-Dimethylethyl[1-(phenylmethyl)-3-pyrrolidinyl]carbamate
A solution of 77.0 g (0.44 mole) of 3-amino-1-(phenylmethyl)pyrrolidine [J. Med. Chem., 24, 1229 (1981)], 440 ml (0.44 mole) 1.0N sodium hydroxide and 600 ml of tertiarybutyl alcohol was treated dropwise with 98.2 g (0.45 mole) of di-tertiarybutyl dicarbomate. The reaction was stirred at room temperature for 18 hours and the solvent removed in vacuo. The residue was partitioned between ether and water. The aqueous layers were reextracted with ether, the combined ether layers were washed with water, dried (MgSO 4 ), filtered, and evaporated on a steam bath replacing the ether with petroleum ether. The crystals which formed were removed by filtration, washed with ether/petroleum ether (1:1), and dried in vacuo to give 84.8 g of 1,1-dimethylethyl[1-(phenylmethyl)-3-pyrrolidinyl]carbamate, mp 114-115° C. A second crop (16.7 g) was obtained by concentrating the filtrate.
1,1-Dimethylethyl(3-pyrrolidinyl)carbamate
A mixture of 101.5 g (0.37 mole) of 1,1-dimethylethyl[1-(phenylmethyl)-3-pyrrolidinyl]carbamate, 5.0 g of 20% palladium on carbon and 1 liter of tetrahydrofuran was shaken in an atmosphere of hydrogen at about 50 psi and room temperature for 24 hours. The catalyst was removed by filtering through Celite, and the filtrate was concentrated in vacuo to give 6.8 g of 1,1-dimethylethyl (3-pyrrolidinyl)carbamate which solidified upon standing and was of sufficient purity to be used as is for the ensuing steps.
Example J
2-[(3-Pyrrolidinylmethyl)amino]ethanol
N-(2-Hydroxyethyl)-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide
A mixture of 46.7 g (0.2 mole) of methyl 5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxylate [J. Org. Chem., 26, 1519 (1961)], 36.7 g (0.6 mole) of 2-aminoethanol and 500 ml methanol was refluxed overnight. The reaction was cooled to room temperature and the solvent removed at reduced pressure. The residue was taken up in dichloromethane and extracted 3×100 ml 1N sodium hydroxide. The aqueous layer was taken to pH 5, extracted 3×150 ml dichloromethane, then taken to pH 8 and again extracted 3×150 ml dichloromethane. The aqueous layer was concentrated at reduced pressure and the resulting slurry stirred in dichloromethane. The salts were filtered off. The combined organic layers were dried over magnesium sulfate, the solvent removed at reduced pressure to yield 47.9 g of N-(2-hydroxyethyl)-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide as an oil. This was used in the next step without further purification.
2-[[[1-(Phenylmethyl)-3-pyrrolidinyl]methyl]amino]ethanol
A mixture of 46.6 g (0.18 mole) of N-(2-hydroxyethyl)-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide in 200 ml of tetrahydrofuran was added dropwise to a slurry of 20.25 g (0.534 mole) of lithium aluminum hydride in 150 ml tetrahydrofuran. The reaction was refluxed three hours, then cooled in an ice bath. The work up consisted of sequential addition of 20 ml water, 20 ml 15% sodium hydroxide then 60 ml water. The reaction was filtered and the precipitate washed with ethanol. The filtrate was concentrated at reduced pressure, the residue taken up in dichloromethane, dried over magnesium sulfate, and the solvent removed at reduced pressure to give 32.31 g of 2-[[[1-(phenylmethyl)-3-pyrrolidinyl]methyl]amino]ethanol as an oil. This material was used in the next step without further purification.
2-[(3-Pyrrolidinylmethyl)amino]ethanol
A mixture of 32.3 g of 2-[[[1-(phenylmethyl)-3-pyrrolidinyl]methyl]amino]ethanol, 330 ml of methanol and 3 g of 20% palladium on charcoal was shaken in an atmosphere of hydrogen at about 4.5×10 5 Pa and at room temperature for 18 hours. The solvents were then removed at reduced pressure. The residue was distilled under vacuum (bp 129-131° C., 1.5 mm Hg) to give 11.43 g of 2-[(3-pyrrolidinylmethyl)amino]ethanol.
Example K
2-Methyl-2,7-diazaspiro[4.4]nonane Dihydrochloride
2-Methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione
A solution of 20.3 g (0.084 mole) 3-ethoxycarbonyl-5-oxo-3-pyrrolidineacetic acid, ethyl ester [J. Org. Chem., 46, 2757 (1981)] in 40 ml of 40% aqueous methylamine was stirred at room temperature overnight, then placed in an oil bath and gradually heated to 220° C. over 30 minutes allowing volatiles to distill from the open flask. The crude product was crystallized from ethanol to afford 12.6 g of 2-methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione, mp 201-204° C.
______________________________________Analysis calculated for C.sub.8 H.sub.10 N.sub.2 O.sub.3 :______________________________________ C, 52.74; H, 5.53; N, 15.38Found C, 52.87; H, 5.60; N, 15.25.______________________________________
7-Benzyl-2-methyl-2,7-diazaspiro[4.4)nonane-1,3,8-trione
A solution of 1.82 g (10 mmol) of 2-methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione in 20 ml N,N-dimethylformamide was added gradually under a nitrogen atmosphere to 0.05 g (10.4 mmol) of 50% oil suspension of sodium hydride which had been previously washed twice with toluene and covered with 10 ml N,N-dimethylformamide. After stirring one hour there was added 1.40 g (11 mmol) of benzyl chloride and stirring was continued overnight at room temperature. After concentrating to a small volume in vacuo, the residue was diluted with 40 ml water and extracted twice with dichloromethane. The combined organic phase was washed with water, dried over magnesium sulfate, and evaporated to give a solid. Crystallization from toluene:hexane to afford 1.74 g of 7-benzyl-2-methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione, mp 157-158° C.
______________________________________Analysis calculated for C.sub.15 H.sub.16 N.sub.2 O.sub.3 :______________________________________ C, 66.16; H, 5.92; N, 10.27Found C, 66.45; H, 5.79; N, 10.09.______________________________________
7-Phenylmethyl-2-methyl-2,7-diazaspiro[4.4]nonane Dihydrochloride
A solution of 1.36 g (5.0 mmol) 7-phenylmethyl-2-methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione in 50 ml tetrahydrofuran was added dropwise to a suspension of 0.95 g (25 mmol) lithium aluminum hydride in 30 ml tetrahydrofuran. The mixture was stirred overnight at room temperature, refluxed one hour, cooled, and treated dropwise with 0.95 ml water, 0.95 ml 15% sodium hydroxide solution, and 2.8 ml water. After removal of the inorganic solids by filtration, the filtrate was concentrated in vacuo to give a syrup which was dissolved in isopropanol and treated with excess 6N hydrogen chloride in isopropanol. Crystallization afforded 0.97 g of the title compound, mp 233-234° C.
______________________________________Analysis calculated for C.sub.15 H.sub.24 N.sub.2 Cl.sub.2 :______________________________________ C, 59.40; H, 7.98; N, 9.24; Cl, 23.38Found C, 59.37; H, 7.98; N, 9.03; Cl, 23.09.______________________________________
2-Methyl-2,7-diazaspiro[4.4]nonane Dihydrochloride
A solution of 7-benzyl-2-methyl-2,7-diazaspiro ]4.4]nonane dihydrochloride in 150 ml of methanol with 1.0 g 20% palladium on carbon catalyst was hydrogenated at 4.5×10 5 Pa for two days. After filtration, the filtrate was concentrated to a thick syrup which crystallized on addition of acetonitrile to give 11.5 g of 2-methyl-2,7-diazaspiro[4.4]nonane dihydrochloride, softened at 164° C. and melted at 168-170 ° C.
______________________________________Analysis calculated for C.sub.8 H.sub.18 N.sub.2 Cl.sub.2 :______________________________________ C, 45.08; H, 8.51; N, 13.15; Cl, 33.27Found C, 45.24; H, 8.77; N, 13.18; Cl, 33.26.______________________________________
Example L
2-Ethyl-2,7-diazaspiro[4.4]nonane Dihydrochloride
2-Ethyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione
A suspension of 24.3 g (0.10 mmole) 3-ethoxycarbonyl-5-oxo-3-pyrrolidineacetic acid, ethyl ester in an excess of 2N sodium hydroxide, was stirred three hours at room temperature, acidified with dilute hydrochloric acid, and evaporated to dryness in vacuo. The product, 3-carboxy-5-oxo-3-pyrrolidineacetic acid, was taken up in isopropyl alcohol, separated from insoluble sodium chloride by filtration, concentrated to a syrup and dissolved in 100 ml 70% ethylamine. The solution was gradually heated in an oil bath up to 230° C. allowing volatiles to distill and then maintained at 230-240° C. for ten minutes. After cooling, the product was crystallized from isopropyl alcohol to afford 10.1 g of 2-ethyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione, mp 168-169° C.
______________________________________Analysis calculated for C.sub.9 H.sub.12 N.sub.2 O.sub.3 :______________________________________ C, 55.09; H, 6.17; N, 14.28Found C, 55.03; H, 5.84; N, 14.01.______________________________________
2-Ethyl-7-benzyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione
A suspension of sodium hydride (2.20 g of 60% oil suspension (0.055 mole) washed with toluene) in 50 ml N,N-dimethylformamide was treated gradually with a solution of 10.0 g (0.051 mole) 2-ethyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione in 100 ml N,N-dimethylformamide. After stirring 15 minutes, there was added dropwise 6.4 ml (0.055 mole) benzyl chloride and the mixture was stirred overnight, concentrated in vacuo and shaken with water-methylene chloride. The organic layers were dried, evaporated, and the product crystallized from toluene-hexane to afford 11.1 g of the title compound, mp 125-126.5° C.
______________________________________Analysis calculated for C.sub.16 H.sub.18 N.sub.2 O.sub.3 :______________________________________ C, 67.11; H, 6.34; N, 9.79Found C, 67.41; H, 6.33; N, 9.79.______________________________________
2-Benzyl-7-ethyl-2,7-diazaspiro[4.4]nonane Dihydrochloride
A solution of 11.0 g (0.038 mole) 2-ethyl-7-benzyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione in 100 ml tetrahydrofuran was added dropwise to a suspension of 6.00 g (0.158 mole) lithium aluminum hydride in 250 ml tetrahydrofuran. After stirring overnight, the mixture was refluxed one hour, cooled, and treated dropwise with 6 ml water, 6 ml 15% sodium hydroxide, and 18 ml water. Inorganic solids were separated by filtration and the filtrate was concentrated, taken up in ether, dried with magnesium sulfate, and reevaporated. The resulting syrup was dissolved in isopropyl alcohol and treated with excess hydrogen chloride in isopropyl alcohol to afford 9.63 g of the title compound, mp 196-198° C. (dec).
______________________________________Analysis calculated for C.sub.16 H.sub.26 N.sub.2 Cl.sub.2 :______________________________________ C, 60.56; H, 8.26; N, 8.83; Cl, 22.35Found C, 60.51; H, 8.08; N, 8.69; Cl, 22.26.______________________________________
2-Ethyl-2,7-diazaspiro[4.4]nonane Dihydrochloride
A solution of 9.5 g (0.03 mole) 2-benzyl-7-ethyl-2,7-diazaspiro[4.4]nonane dihydrochloride in 100 ml methanol was hydrogenated with 1.0 g 20% palladium on carbon catalyst at 4.5×10 5 Pa for 22 hours. After filtration, the solution was concentrated to a syrup and crystallized from acetonitrile to afford 6.7 g of the title compound, mp 168-172° C.
______________________________________Analysis calculated for C.sub.9 H.sub.20 N.sub.2 Cl.sub.2 :______________________________________ C, 47.58; H, 8.86; N, 12.33; Cl, 31.21Found C, 47.70; H, 8.58; N, 12.39; Cl, 30.92.______________________________________
Example M
1-Cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid
2,3,4,5-Tetrafluorobenzoylacetic Acid, Ethyl Ester
To 25.2 g (0.117 mol) of sodium 2,3,4,5-tetrafluorobenzoate, prepared as a dry powder from 2,3,4,5-tetrafluorobenzoic acid [J. Org. Chem., 29, 2381 (1961)] and aqueous sodium hydroxide with concentration to dryness, was added 400 ml of dry ether and the suspension was cooled to 0° C. Slowly, 25 ml (≈2.5 equivalents) of oxalyl chloride in 50 ml of ether was added and the mixture brought to room temperature where it was maintained for 2.0 hours. It was filtered and concentrated to remove low boiling impurities. The residue was dissolved in 100 ml of ether and placed in an addition funnel.
Meanwhile, 2.9 g (0.119 mol) of magnesium turnings were treated with 100 ml of absolute ethanol and 0.3 ml of carbon tetrachloride. To this mixture was added 18.6 ml (0.12 mol) of diethyl malonate in 75 ml of ether at a rate to keep the temperature just below reflux. When addition was complete, the reaction was refluxed for two hours. At -20° C., the etheral acid chloride was slowly added. When addition was complete, the reaction was brought to 0° C. over 18 hours. The mixture was poured into dilute hydrochloric acid and was extracted into dichloromethane which was dried (MgSO 4 ) and concentrated. The residue was then treated with 340 mg of p-toluenesulfonic acid in 600 ml of water at 100° C. for two hours with rapid stirring. The oil was extracted into dichloromethane, dried (MgSO 4 ) and concentrated. The residue was purified by column chromatography (silica gel, using toluene:hexane:ether, 4:5:1), to give 18.5 g of a reddish oil. This material was triturated with pentane to give 10.2 g of 2,3,4,5-tetrafluorobenzoylacetic acid, ethyl ester, mp 49-51° C.
(2,3,4,5-Tetrafluorobenzoyl)-3-cyclopropylaminoacrylic Acid, Ethyl Ester
To 10.2 g (38.5 mmol) of the 2-(2,3,4,5-tetrafluorobenzoylacetic acid, ethyl ester was added 8.4 g (57.0 mmol) of triethylorthoformate and 9.3 g (91.5 mmol) of acetic anhydride. The mixture was heated to 150° C. for two hours and was then placed under high vacuum at 75-85° C. for one hour. The residue dissolved, without purification, in 100 ml of isopropyl alcohol and treated with 2.4 ml of cyclopropylamine. The reaction was allowed to stand overnight. It was concentrated and purified by column chromatography (silica gel 70-200, using hexane:chloroform:isopropyl alcohol, 80:15:5). The product off the column was recrystallized from pentane to give 6.16 g of 2-(2,3,4,5-tetrafluorobenzoyl)-3-cyclopropylaminoacrylic acid, ethyl ester, mp 63-64° C.
1-Cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid
To 2.0 g (6.0 mmol) of the 2-(2,3,4,5-tetrafluorobenzoyl)-3-cyclopropylaminoacrylic acid, ethyl ester in 60 ml of dry dioxane was added 0.29 g of sodium hydride 50% dispersion) that was prewashed with pentane. The sodium hydride was delivered in 10 ml of dry tetrahydrofuran at 0° C. When evolution of hydrogen began to slow, the mixture was refluxed for two hours. It was concentrated, and the residue taken up in dichloromethane, which was water extracted, dried (MgSO 4 ), and concentrated. The residue was purified by column chromatography (silica gel 70-200 mesh, using chloroform:hexane:isopropanol, 4:5:1) to give 0.95 g of the 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, ethyl ester, mp 168-169° C. This material was dissolved in acetic acid at 100° C. and was treated with 10 ml of 0.5N hydrochloric acid for 2.5 hours. The mixture was cooled and water added. The solids were then collected to give 0.7 g of 1-cyclopropyl-1,4-dihydro-4-oxo-6,7,8-trifluoro-3-quinolinecarboxylic acid, mp 226-228° C.
Example N
7-Chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic Acid
4-[6-(Cyclopropylamino)-3-nitro-2-pyridinyl]-1-piperazinecarboxylic Acid, Ethyl Ester
A solution of 126.0 g (0.4 mole) of 4-(6-chloro-3-nitro-2-pyridinyl)-1-piperazinecarboxylic acid, ethyl ester (prepared as described in European Patent Publication No. 9425), 76.1 g (0.5 mole) of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), 28.6 g (0.5 mole) of cyclopropylamine and 500 ml of absolute ethanol was stirred at room temperature for 48 hours. The solution was then heated at reflux for four hours and concentrated in vacuo. The residue was partitioned between chloroform and water. The chloroform layer was dried over magnesium sulfate and concentrated in vacuo. The residue was triturated with ether to give 64.0 g of the title compound, mp 100-103° C.
4-[6-(Acetylcyclopropylamino)-3-nitro-2-pyridinyl]-1-piperazinecarboxylic Acid, Ethyl Ester
A solution of 64.0 g (0.19 mole) of 4-[6-(cyclopropylamino)-3-nitro-2-pyridinyl]-1-piperazinecarboxylic acid, ethyl ester, 115 ml of acetic anhydride and 115 ml of acetic acid was heated on a steam bath for 36 hours. The solvents were removed in vacuo, the residue was triturated with a mixture of ethanol and toluene which was also evaporated in vacuo to give 68.3 g of the title compound, mp 90-93° C.
4-[6-(Acetylcyclopropylamino)-3-amino-2-pyridinyl]-1-piperazinecarboxylic Acid, Ethyl Ester
A mixture of 17.0 g (45 mmole) of 4-[6-(acetylcyclopropylamino)-3-nitro-2-pyridinyl-1-piperazine carboxylic acid, ethyl ester, 1.5 g of Raney nickel and 180 ml of absolute ethanol was shaken in an atmosphere of hydrogen at about 50 psi and room temperature for approximately 24 hours. The catalyst was removed by filtering through Celite and the solvent removed in vacuo to give 15.2 g of the title compound, mp 149-150° C.
2-[4-(Ethoxycarbonyl)-1-piperazinyl]-6-(acetylcyclopropylamino)-3-pyridinediazonium Tetrafluoroborate
A solution of 20.8 g (60 mmole) of 4-(6-acetylcyclopropylamino)-3-amino-2-pyridinyl]-1-piperazine carboxylic acid, ethyl ester, 44 ml of ethanol and 27 ml of 48% tetrafluoroboric acid was cooled to 0° C. and treated dropwise with a solution of 4.56 g (66 mmol) of sodium nitrite in 8 ml of water under a nitrogen atmosphere keeping the temperature 0-5° C. After the addition was complete, the reaction was stirred at 0-5° C. for one hour and treated with 150 ml of anhydrous ether keeping the temperature below 10° C. The solid was removed by filtration, the precipitate was washed with ethanol/ether (1:1), ether and dried in vacuo to give 24.5 g of the title compound, mp 100-105° C. (dec).
4-[6-(Acetylcyclopropylamino)-3-fluoro-2-pyridinyl]-1-piperazinecarboxylic Acid, Ethyl Ester
To 800 ml of refluxing toluene was added in portions, as a solid, 46.2 g (0.1 mole) of 2-[4-(ethoxycarbonyl)-1-piperazinyl]-6-acetylcyclopropylamino)-3-pyridinediazonium tetrafluoroborate. After the addition was complete, the reaction was refluxed for ten minutes and the toluene was decanted from the insoluble precipitate. The toluene was evaporated in vacuo and the residue was partitioned between chloroform and water. The chloroform layer was washed with 5% aqueous sodium bicarbonate, water, dried over magnesium sulfate, and evaporated in vacuo to give 13.7 g of the title compound, as a viscous oil. An additional 10.2 g could be obtained by partitioning the original toluene insoluble material in chloroform and water. The organic layer was washed with 5% aqueous sodium bicarbonate, dried over magnesium sulfate, evaporated in vacuo and the residue was chromatographed on silica gel eluting with chloroform/ethyl acetate (6:4). This fraction was also a viscous oil which did not crystallize upon standing. Both fractions were of sufficient purity to be used as is in the ensuing steps.
4-[6-(Cyclopropylamino)-3-fluoro-2-pyridinyl]-1-piperazinecarboxylic Acid, Ethyl Ester
A solution of 21.9 g (63 mmole) of 4-[6-(acetylcyclopropylamino)-3-fluoro-2-pyridinyl]-1-piperazinecarboxylic acid, ethyl ester, 170 ml of 15% hydrochloric acid and 235 ml of methanol was refluxed for one hour and allowed to stir at room temperature for 18 hours. The methanol was removed in vacuo and the aqueous acid was made basic with 1.0N sodium hydroxide to pH 10.5. The mixture was extracted with chloroform, the chloroform layer washed with water, dried over magnesium sulfate, and evaporated in vacuo to give 17.6 g of the title compound, mp 68-70° C.
1-Cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-1,8-naphthyridine-3-carboxylic Acid
Route A
[[Cyclopropyl[6-[4-(ethoxycarbonyl)-1-piperazinyl]-5-fluoro-2-pyridinyl]amino]methylene]propanedioic Acid, Diethyl Ester
A solution of 3.8 g (12.3 mmole) of 4-[6-(cyclopropylamino)-3-fluoro-2-pyridinyl]-1-piperazine carboxylic acid, ethyl ester, 2.7 g (12.3 mmole) of diethyl(ethoxymethylene)malonate and 50 ml of xylene was refluxed for 24 hours. The solvent was removed in vacuo and the residue was chromatographed over silica gel eluting with chloroform/ethyl acetate (80/20) to give 2.3 g of the title compound as a viscous oil which was used without further purification.
Ethyl 1-Cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-4-(ethoxycarbonyl)-1-piperazinyl]-1,8-naphthyridine-3-carboxylate
A solution of 2.3 g (4.8 mmole) of [[cyclopropyl[6-[4-(ethoxycarbonyl)-1-piperazinyl]-5-fluoro-2-pyridinyl]amino]methylene]propanedioic acid, diethyl ester, in 15 ml of acetic anhydride was treated dropwise with 5 ml of 98% sulfuric acid keeping the temperature 55-60° C. When the addition was complete, the reaction was stirred for one hour and poured onto 50 g of ice. The aqueous suspension was extracted with chloroform, the chloroform layer washed with water, dried over magnesium sulfate, filtered, and evaporated in vacuo. The residue was triturated with several portions of ethanol/toluene which were also removed in vacuo to give 0.4 g of the title compound, mp 184-186° C. An additional 0.5 g of product could be obtained by concentrating the original aqueous fraction, mp 184-186° C.
1-Cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-1,8-naphthyridine-3-carboxylic Acid
A suspension of 0.7 g (1.6 mmole) of ethyl 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-[4-(ethoxycarbonyl)-1-piperazinyl]-1,8-naphthyridine-3-carboxylate, 6 ml of 10% aqueous sodium hydroxide and 2 ml of ethanol was refluxed for three hours. The reaction was filtered through a fiber glass pad to clarify and acidified to pH 1.5 with 6.0M hydrochloric acid and lyophilized. The residue was dissolved in 10 ml of ammonium hydroxide and the solution concentrated in vacuo. The precipitate which formed was removed by filtration, washed with aqueous ethanol, ether, and dried in vacuo to give 0.04 g, mp 274-276° C.
Route B
4-[6-[Cyclopropyl(2,2-dimethyl-4,6-dioxo-1,3-dioxan 5-ylidine)amino]-3-fluoro-2-pyridinyl]-1-piperazinecarboxylic Acid, Ethyl Ester
A solution of 17.6 g (57 mmole) of 4-[6-(cyclopropylamino)-3-fluoro-2-pyridinyl]-1-piperazine carboxylic acid, ethyl ester, 11.6 g (63 mmole) of 5-(methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione and 250 ml of methanol was stirred at room temperature for four hours. The solid was removed by filtration, washed with methanol, ether and dried in vacuo to give 17.6 g of the title compound, mp 177-178° C.
1-Cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-[4-(ethoxycarbonyl)-1-piperazinyl]-1,8-naphthyridine-3-carboxylic Acid
A solution of 17.0 g (37.0 mmole) of 4-[6-(cyclopropyl-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)amino]-3-fluoro-2-pyridinyl]-1-piperazinecarboxylic acid, ethyl ester in 125 ml of acetic anhydride was treated dropwise with 35 ml of 98% sulfuric acid keeping the temperature 50-60° C. When the addition was complete, the reaction was stirred for two hours and poured onto 600 g of ice. The mixture was stirred for one hour and the resulting precipitate was removed by filtration, washed with water, and dried in vacuo to give 10.2 g of the title compound, mp 277-279° C.
1-Cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl-1,8-naphthyridine-3-carboxylic Acid
A solution of 10.2 g (25 mmole) of 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-[4-(ethoxy carbonyl)-1-piperazinyl]-1,8-naphthyridine-3-carboxylic acid, 100 ml of 10% aqueous sodium hydroxide and 40 ml of ethanol was refluxed for three hours. The solution was concentrated to 125 ml and acidified to pH 7.3 with glacial acetic acid. The resulting precipitate was removed by filtration, washed with 50% aqueous ethanol, ether and dried in vacuo to give 7.2 g of the title compound, mp 274-276° C.
1-Cyclopropyl-6-fluoro-1,4-dihydro-7-hydroxy-4-oxo-1,8-naphthyridine-3-carboxylic Acid
To a solution of 2 ml of 70% nitric acid in 10 ml of 98% sulfuric acid was added in portions 1.0 g (3.0 mmole) of 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-1,8-naphthyridine-3carboxylic acid, keeping the temperature between 25-30° C. The resulting solution was stirred at room temperature for 18 hours and poured onto 40 g of ice. The mixture was stirred at room temperature for 24 hours, concentrated in vacuo, the pH adjusted to 12 with aqueous sodium hydroxide, and filtered through a fiber glass pad. The filtrate was acidified to pH 3.5 with 6.0M hydrochloric acid, the resulting precipitate removed by filtration, washed with water then ether and dried in vacuo to give 0.23 g of the title compound, mp 325-327° C.
7-Chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic Acid
A suspension of 0.19 g (0.72 mmole) of 1-cyclopropyl-6-fluoro-1,4-dihydro-7-hydroxy-4-oxo-1,8-naphthyridine-3-carboxylic acid in 2 ml of phosphorus oxychloride was heated at reflux for one-half hour. The resulting solution was cooled to room temperature and the solvent was removed in vacuo. The residue was triturated with ice water and the resulting solid was removed by filtration, washed with water, then ether, and dried in vacuo to give 0.11 g of the title compound, mp 209-212° C.
Example O
2-Nitro-3,4,5,6-tetrafluorobenzoyl Chloride
A solution of 6.7 g (28 mmoles) of 2-nitro-3,4,5,6-tetrafluorobenzoic acid [Tetrahedron, 23, 4719, (1967)], 3.8 g (30 mmoles) of oxalyl chloride and 50 ml of dichloromethane was treated with four drops of N,N-dimethylformamide and stirred at room temperature overnight. The solvent was removed and the residue was used as is without further purification.
Example P
2-Nitro-3,4,5,6-tetrafluoro-β-oxobenzenepropanoic Acid, Ethyl Ester
To a solution of 7.5 g (56.8 mmoles) of malonic half acid ester in 125 ml of dry tetrahydrofuran was added 20 mg of 2,2'-bipyridyl. The reaction mixture was cooled to -30° C. and treated dropwise with 24 ml (57.6 mmoles) of 2.4N n-butyl lithium. The reaction was then allowed to warm to -5° C. where a second equivalent, 24 ml (57.6 mmoles), of 2.4N n-butyl lithium was added until a light pink color persisted for 15 minutes. The reaction mixture was then cooled to -75° C. and treated dropwise with a solution of 7.2 g (28 mmoles) of 2-nitro-3,4,5,6-tetrafluorobenzoyl chloride in 15 ml of tetrahydrofuran. The reaction was stirred at -75° C. for one hour, warmed to -35° C., and quenched by pouring onto a solution of 28 ml of concentrated hydrochloric acid in 50 ml of ice water. The reaction was extracted with dichloromethane (3×200 ml), the organic layer was washed with 5% aqueous sodium bicarbonate (2×100 ml), and with 1.0M hydrochloric acid (1×100 ml), dried (MgSO 4 ), and evaporated in vacuo to give 7.3 g of the title compound which was used for the ensuing step without further purification.
Example Q
Ethyl 1-Cyclopropyl-5-nitro-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate
A solution of 6.8 g (22 mmoles) of 2-nitro-3,4,5,6-tetrafluoro-β-oxobenzenepropanoic acid, ethyl ester, 4.9 g (33 mmoles) of triethylorthoformate and 50 ml of acetic anhydride was heated at reflux for two hours. The solvent was removed in vacuo and then in high vacuo at 80° C. for 1.5 hours. The residue was dissolved in 25 ml of t-butanol and treated with 1.43 g (25 mmoles) of cyclopropylamine. The mixture was heated at 45° C. for four hours, cooled to room temperature and treated dropwise with a solution of 2.47 g (25 mmoles) of potassium t-butoxide in 25 ml of t-butanol. The reaction was heated at 60° C. for six hours and the solvent was removed in vacuo. The residue was dissolved in chloroform, washed with water, dried (MgSO 4 ), and evaporated in vacuo. The residue was chromatographed over silica gel eluting with chloroform/ethyl acetate (80/20) to give 1.9 g of the title compound as an oil which was used without further purification.
Example R
Ethyl 5-Amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate
A suspension of 1.9 g (5.3 mmoles) of ethyl 1-cyclopropyl-5-nitro-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate, 0.5 g of Raney nickel and 100 ml of ethanol was shaken in a hydrogen atmosphere at pressures of 42.5-50 psi and temperatures of 24-26.5° C. for ten hours. The mixture was filtered through Celite and some insoluble product was dissolved in tetrahydrofuran with filtration. The combined filtrates were evaporated in vacuo and the residue was chromatographed on silica gel to give 600 mg of the title compound, mp 223-225° C.
Example S
5-Amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid
A solution of 0.5 g (1.5 mmoles) of ethyl 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate, 5 ml of 6.0M hydrochloric acid and 5 ml of ethanol was heated at reflux for two hours. The solvent was removed in vacuo to give 430 mg of the title compound, mp 269-271° C.
Example T
3-Chloro-2,4,5-trifluoro-6-nitrobenzoic Acid
To a solution of 42.1 g (200 mmol) of 3-chloro-2,4,5-trifluorobenzoic acid (E.P.O. 0 183 129) in 100 ml of sulfuric acid was added concentrated nitric acid (50 ml) dropwise such that the reaction temperature stayed below 40° C. The reaction mixture was heated at 60° C. for 18 hours, then poured cautiously onto 500 g of ice water. The aqueous solution was extracted with ether, and the ether extracts were washed with water, dried over magnesium sulfate, and concentrated to give 26.5 g of 3-chloro-2,4,5-trilfuoro-6-nitrobenzoic acid.
Example U
3-Chloro-2,4,5-trifluoro-6-nitrobenzoyl Chloride
To a suspension of 25.6 g (100 mmol) of 3-chloro-2,4,5-trifluoro-6-nitrobenzoic acid in 75 ml of dichloromethane was added 14.0 g (110 mmol) of oxalyl chloride. This mixture was treated with four drops of dry N,N-dimethylformamide, and the rapidly bubbling solution was stirred overnight at room temperature. The mixture was concentrated to give 27.0 g of the title compound which was used without purification in the next step.
Example V
Ethyl (3-Chloro-2,4,5-trifluoro-6-nitro)-β-oxophenylpropanoate
To 26.4 g (200 mmol) of malonic half ethyl ester in 500 ml of dry tetrahydrofuran at -35° C. was added 91 ml of n-butyllithium (2.2M, 200 mmol) dropwise. A catalytic amount of bipyridyl (10 mg) was added, and the suspension was warmed to -5° C. Another equivalent of n-butyllithium (91 ml, 200 mmol) was added until the indicator turned pink. The mixture was cooled to -78° C., and a solution of 27 g of 3-chloro-2,4,5-trifluoro-6-nitrobenzoyl chloride in 50 ml of tetrahydrofuran was added dropwise. The reaction mixture was kept at -78° C. for one hour, then warmed to -35° C. and poured into a mixture of ice water (400 ml) and concentrated hydrochloric acid (17 ml). The solution was extracted with dichloromethane; the extracts were combined and washed with 5% sodium bicarbonate, 2M hydrochloric acid, and water. The dichloromethane was dried over magnesium sulfate and concentrated to give 27.4 g of the title compound.
Example W
Ethyl 2-(3-Chloro-2,4,5-trifluoro-6-nitrobenzoyl)-3-ethoxyacrylate
To 27.4 g (84.1 mmol) of the ethyl (3-chloro-2,4,5-trifluoro-6-nitro)-β-oxophenyl propanoate was added 18.7 g (126 mmol) of triethyl orthoformate and 100 ml of acetic anhydride. The mixture was refluxed for two hours, then cooled to 80° C., and concentrated to give 31.5 g of the title compound.
Example Y
Ethyl 8-Chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-nitro-4-oxo-3-quinolinecarboxylate
The ethyl 2-(3-chloro-2,4,5-trifluoro-6-nitrobenzoyl)-3-ethoxyacrylate prepared in the previous step was dissolved in 200 ml of t-butanol and treated with 5.0 g (88 mmol) of cyclopropylamine. The reaction mixture was warmed to 45° C. and stirred for three hours at that temperature. The solution was then cooled to room temperature and treated with a slurry of 9.4 g (84 mmol) of potassium t-butoxide in 50 ml of t-butanol. The mixture was stirred at 60° C. for five hours; the suspension was filtered, and the solid was washed with water and ether to give 21.7 g of the title compound.
Example Z
Ethyl 5-Amino-8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate
A suspension of 21.7 g (58.2 mmol) of ethyl 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-nitro-4-oxo-3-quinolinecarboxylate in 300 ml of ethanol and 300 ml of tetrahydrofuran was catalytically reduced using 3 g of Raney nickel in a hydrogen atmosphere of 50 psi. After twelve hours the mixture was diluted with dichloromethane and the catalyst was removed by filtration. The filtrate was concentrated to give 17.2 g of the title compound.
Example AA
5-Amino-8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid
A suspension of 17.2 g (50.2 mmol) of ethyl 5-amino-8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate in 100 ml of 6M hydrochloric acid was refluxed for three hours. The mixture was cooled to room temperature, and the solids were filtered, washed with water and ether, and dried to give 14.2 g of the title compound.
Using the same sequence of reactions the following compounds could be prepared:
5-amino-8-bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid;
5-amino-1-cyclopropyl-6,7-difluoro-8-trifluoro-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid;
5-amino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid;
5-amino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-hydroxy-4-oxo-3-quinolinecarboxylic acid;
5,8-diamino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid;
5-amino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid; and
5-amino-7-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid.
Example BB
1-Cyclopropyl-6,7,8-trifluoro-1,4-dihydro-5-(methylamino)-4-oxo-3-quinolinecarboxylic Acid
A solution of 5.9 g (20 mmol) of 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, 20 ml of trifluoroacetic anhydride, and 100 ml of trifluoro acetic acid was stirred at room temperature overnight. The solution was evaporated to dryness and the residue was triturated with water and filtered to give 7.55 g of 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-5-[(trifluoroacetyl)amino]-3-quinolinecarboxylic acid, mp 188° C.
A solution of 5.53 g (14.0 mmol) of the trifluoroacetyl intermediate above, 55 ml of DMF and 1.42 g (30.9 mmol) of 50% sodium hydride was stirred at 50-55° C. for 35 minutes. To this mixture was added 2.8 ml (45 mmol) of iodomethane with continued stirring at 50-55° C. for two hours and for three hours at room temperature. The reaction mixture was evaporated and the residue was triturated with water and filtered. The solid was dissolved with 60 ml of acetic acid and 30 ml of 6N HCl was added and the solution was heated under reflux for two hours. The solution was concentrated and the residual oil was treated with isopropanol to give 3.0 g of the title compound, mp 205-207° C.
In a similar manner, the following compounds were prepared: 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-(methylamino)-4-oxo-3-quinolinecarboxylic acid; 8-bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-(methylamino)-4-oxo-3-quinolinecarboxylic acid; and 1-cyclopropyl-6,7-difluoro-8-trifluoromethyl-1,4-dihydro-5-(methylamino)-4-oxo-3-quinolinecarboxylic acid.
Example CC
1-Cyclopropyl-6,7,8-trifluoro-1,4-dihydro-5-dimethylamino-4-oxo-3-quinolinecarboxylic Acid
2-(Dimethylamino)-3,4,5,6-tetrafluorobenzoic Acid
A solution of 10.0 g (41.8 mmol) of 2-nitro-3,4,5,6-tetrafluorobenzoic acid, 10 ml of 37% formaldehyde solution, 1.5 g of Raney nickel and 100 ml of ethanol was hydrogenated until TLC indicated absence of starting material. The reaction mixture was filtered and evaporated to an oil which was recrystallized with ethyl acetate-hexane to give 2.15 g of the title compound, mp 110-112° C. An additional 2.28 g, mp 90-100° C. was isolated from the filtrate.
2-(Dimethylamino)-3,4,5,6-tetrafluorobenzoyl Chloride
To a suspension of 4.22 g (17.8 mmol) of 2-(dimethylamino)-3,4,5,6-tetrafluorobenzoic acid and 85 ml of dichloromethane, added 1.7 ml (19.5 mmol) of oxalyl chloride. After the bubbling subsided, five drops of DMF were added and the solution was stirred at room temperature for 21 hours. The solution was evaporated to 4.8 g of an oil which was used in the next step without purification.
2-(Dimethylamino)-3,4,5,6-tetrafluoro-β-oxobenzenepropanoic Acid, Ethyl Ester
To a solution of 4.76 g (36 mmol) of malonic acid monoethyl ester and 75 ml of THF at -35° C. was added 25 ml (40 mmol) of 1.5N n-butyl lithium solution. The remaining 25 ml (40 mmol) of 1.5N butyllithium solution was added at 0° . After cooling to -78° C., a solution of the 4.8 g of 2-(dimethylamino)-3,4,5,6-tetrafluorobenzoyl chloride in 50 ml of THF was added to the dilithio malonate over a 15 minute period. The reaction mixture was stirred for 1.75 hours while the temperature came up to -30° C. The reaction mixture was poured into ice, water, and 50 ml of 1N HCl. The mixture was extracted with ether and the ether extract was washed with H 2 O, 5% NaHCO 3 , and HCl. After drying over MgSO 4 the ether solution was concentrated to 4.4 g of oil product. NMR spectra indicated the desired product.
2-(Dimethylamino)-α-(ethoxymethylene)-3,4,5,6-tetrafluoro-β-oxobenzenepropanoic Acid, Ethyl Ester
A solution of 4.4 g (14.3 mmol) of the crude ketoester, 3.57 ml (21.5 mmol) of triethylortho formate, and 25 ml of acetic anhydride was heated under reflux for two hours. The solution was evaporated to 5.2 g of oil which was used in the next step without purification.
α-[(Cyclopropylamino)methylene]-2-(dimethylamino)-3,4,5,6-tetrafluoro-β-oxobenzenepropanoic Acid, Ethyl Ester
To a solution of 5.2 g (14.3 mmol) of the above crude product in 50 ml of t-butanol was added 1.2 ml (17 mmol) of cyclopropylamine. The reaction solution was stirred for 18 hours at room temperature. The reaction mixture was filtered to give 0.12 g of the title compound, mp 122-124° C. TLC of the filtrate showed it to be the same as the solid.
5-(Dimethylamino)-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid
To the above filtrate was added 1.7 g (15 mmol) of potassium t-butoxide and the mixture was stirred at room temperature for 1.5 hours. TLC showed no change in reactants. An additional 1.7 g (15 mmol) of potassium t-butoxide was added and the reaction mixture was heated at 50-55° C. for two hours. After TLC indicated the reaction was complete, the solution was evaporated to 4 g of an oil. This oil was heated with 100 l 6N HCl for three hours on the steam bath. The solution was evaporated and the residue was recrystallized from isopropanol to give 0.3 g of the title compound, mp 160-163° C. An additional 1.0 g of solid was added from the filtrate.
Following the same sequence, the following compounds were prepared: 8-chloro-1-cyclopropyl-6,7difluoro-1,4-dihydro-5-dimethylamino-4-oxo-3-quinolinecarboxylic acid, and 8-bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-dimethylamino-4-oxo-3-quinolinecarboxylic acid.
Example DD
1-Cyclopropyl-6,7,8-trifluoro-1,4-dihydro-5-methoxy-4-oxo-3-quinolinecarboxylic Acid
To 22.4 g (100 mmol) of the 2-methoxy-3,4,5,6-tetrafluorobenzoic acid prepared as in [J. Fluorine Chem., 28, 361 (1985)] was added 400 ml of tetrahydrofuran, 1 ml of dimethylformamide, and 13 ml of oxalylchloride. The acid chloride mixture was concentrated, diluted with 100 ml of tetrahydrofuran, and added to a solution of the dilithio anion of malonic acid monoethylester (200 mmol) in 800 ml of tetrahydrofuran at -70° C. The reaction was stirred for one hour at -30° C., poured over ice and dilute hydrochloric acid and taken into dichloromethane. The product was isolated by an extraction at pH 7, followed by drying the dichloromethane (MgSO 4 ) and concentration. The crude product was then treated neat with 2.5 equivalents of triethylorthoformate and 2.8 equivalents of acetic anhydride at 150° C. for two hours. The mixture was concentrated and at room temperature a slight excess of cyclopropylamine (6.0 g) was added in 150 ml of t-butanol. The mixture was stirred overnight. To this mixture was added 11.3 g of potassium t-butoxide and the temperature brought to 50° C. The mixture was concentrated after 18 hours and the residue treated with 100 ml of acetic acid and 100 ml of 4N hydrochloric acid. From this mixture after four hours at 100° C., 12.7 g of the title compound precipitated.
In a similar manner, the following compounds were prepared: 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-methoxy-4-oxo-3-quinolinecarboxylic acid; 8-bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-methoxy-4-oxo-3-quinolinecarboxylic acid; 1-cyclopropyl-6,7-difluoro-8-trifluoromethyl-5-methoxy-4-oxo-3-quinolinecarboxylic acid; and 1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-methoxy-4-oxo-3-quinolinecarboxylic acid.
Example EE
1-Cyclopropyl-6,7,8-trifluoro-1,4-dihydro-5-hydroxy-4-oxo-3-quinolinecarboxylic Acid
To 1.5 g of 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-5-methoxy-4-oxo-3-quinolinecarboxylic acid was added 25 ml of hydrogen bromide in acetic acid (32%). The mixture was stirred at room temperature for 16 hours and concentrated to dryness. The residue was triturated with water:ethanol and filtered to give 1.15 g of the title compound.
In a similar manner the following compounds were prepared: 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-hydroxy-4-oxo-3-quinolinecarboxylic acid; 8-bromo-1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-hydroxy-4-oxo-3-quinolinecarboxylic acid; 1-cyclopropyl-6,7-difluoro-8-trifluoromethyl-5-hydroxy-4-oxo-3-quinolinecarboxylic acid and 1-cyclopropyl-6,7-difluoro-1,4-dihydro-5-hydroxy-4-oxo-3-quinolinecarboxylic acid.
Example 1
1-Ethyl-5-amino-6,8-difluoro-7-[3-(t-butoxycarbonylamino)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid
A suspension of 3.02 g (10 mmole) of 1-ethyl-5-amino-6,7,8-trifluoro-4-oxo-1,4-dihydro quinoline-3-carboxylic acid, 2.79 g (15 mmole) of 3-(t-butoxycarbonylamino)pyrrolidine, 3.0 g (30 mmole) of triethylamine and 100 ml of acetonitrile is refluxed for 18 hours. The reaction mixture is cooled to room temperature and the precipitate is removed by filtration, washed with acetonitrile, ether, and dried in vacuo to give 1-ethyl-5-amino-6,8-difluoro-7-[3-(t-butoxycarbonylamino)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.
Example 2
1-Ethyl-5-amino-6,8-difluoro-7-(3-amino-1-pyrrolidinyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid Hydrochloride
A near solution of 4.5 g (10 mmole) of 1-ethyl-5-amino-6,8-difluoro-7-[3-(t-butoxycarbonylamino)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid, 10 ml of 6.0M hydrochloric acid and 100 ml of glacial acetic acid is heated at 60° C. for four hours and then stirred at room temperature for 18 hours. The solvent is removed in vacuo, the residue triturated with ethanol/ether (1:1), filtered, washed with ether, and dried in vacuo to give the title compound.
Example 3
1-Ethyl-5-amino-6,8-difluoro-7-[3-(ethylamino)methyl-1-pyrrolidinyl)]-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid
A suspension of 3.02 g (10 mmole) of 1-ethyl-5-amino-6,7,8-trifluoro-4-oxo-1,4-dihydro quinoline-3-carboxylic acid, 1.93 g (15 mmole) of N-ethyl-3-pyrrolidinemethanamine, 3.0 g (30 mmole) of triethylamine and 100 ml of acetonitrile is refluxed for 18 hours. The reaction mixture is cooled to room temperature and the precipitate is removed by filtration, washed with acetonitrile, ether, and dried in vacuo to give 1-ethyl-5-amino-6,8-difluoro-7-[3-(ethylamino)methyl-1-pyrrolidinyl)]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.
The following compounds may be prepared from 1-ethyl-5-amino-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid and the desired amine or protected amine using the method above: 1-ethyl-5-amino-6,8-difluoro-7-[3-(aminomethyl)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid; 1-ethyl-5-amino-6,8-difluoro-7-[3-(propylaminomethyl)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid; 1-ethyl-5-amino-6,8-difluoro-7-[3-(2-propylaminomethyl)-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid; 1-ethyl-5-amino-6,8-difluoro-7-[3-(cyclopropylaminomethyl)-1pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid; 1-ethyl-5-amino-6,8-difluoro-7-[2,7-diazaspiro [4.4]non-2-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid; 1-ethyl-5-amino-6,8-difluoro-7-[7-methyl-2,7-diazaspiro[4.4]non-2-yl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid; 1-ethyl-5-amino-6,8-difluoro-7-[7-ethyl-2,7-diazaspiro[4.4]non-2-yl]-4 -oxo-1,4-dihydroquinoline-3-carboxylic acid; 1-ethyl-5-amino-6,8-difluoro-7-[3-[[(2-hydroxyethyl)amino]methyl]-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid; and 1-ethyl-5-amino-6,8-difluoro-7-[3-[[(2,2,2-trifluoroethyl)amino]methyl]-1-pyrrolidinyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.
Example 4
8-Amino-9-fluoro-3-methyl-10-[(3-t-butoxycarbonylamino)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic Acid
A solution of 2.9 g (10 mmole) of 8-amino-9,10-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid, 2.8 g (15 mmole) of 3-(t-butoxycarbonylamino)pyrrolidine, 3.03 g (30 mmole) of triethylamine and 100 ml of N,N-dimethylformamide is heated at 100° C. for four hours. The solvent is removed in vacuo and the residue is triturated with water. The aqueous slurry is adjusted to pH 7.2 with 1.0M hydrochloric acid and the precipitate is removed by filtration, washed with water, and dried in vacuo to give the 8-amino-9-fluoro-3-methyl-10-[(3-t-butoxycarbonylamino)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid.
Example 5
8-Amino-9-fluoro-3-methyl-10-(3-amino-1-pyrrolidinyl)-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic Acid, Hydrochloride
A suspension of 4.63 g (10.0 mmole) of 8-amino-9-fluoro-3-methyl-10-[(3-t-butoxycarbonyl amino)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid 5 ml of 6.0M hydrochloric acid and 50 ml of glacial acetic acid is heated at 60° C. for four hours. The solvent is removed in vacuo and the residue is triturated with ethanol/ether (1:1). The precipitate is removed by filtration, washed with ether, and dried in vacuo to give 8-amino-9-fluoro-3-methyl-10-(3-amino-1-pyrrolidinyl)-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid, hydrochloride.
Example 6
8-Amino-9-fluoro-3-methyl-10-[(3-cyclopropylaminomethyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic Acid
A mixture of 2.96 g (10 mmole) of 8-amino-9,10-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid, 2.1 g (15 mmole) of N-cyclopropyl-3-pyrrolidinemethanamine, 3.03 g (30 mmole) of triethylamine and 100 ml of N,N-dimethylformamide is heated at 100° C. for four hours. The solvent is removed in vacuo and the residue triturated with water. The aqueous suspension is adjusted to pH 7.2 with 1.0M hydrochloric acid. The solid is removed by filtration, washed with water, and dried in vacuo to give 8-amino-9-fluoro-3-methyl-10-[(3-cyclopropylaminomethyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid.
The following compounds may be prepared from 8-amino-9,10-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid and the desired amine or protected amine using the above method: 8-amino-9-fluoro-3-methyl-10-[3-(aminomethyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid; 8-amino-9-fluoro-3-methyl-10-[3-[(propylamino)methyl)-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid; 8-amino-9-fluoro-3-methyl-10-[3-[(2-hydroxyethyl)amino)methyl]-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid; 8-amino-9-fluoro-3-methyl-10-[3-[(2-propylamino)methyl]-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid; 8-amino-9-fluoro-3-methyl-10-[3-[(2,2,2-trifluoroethyl)amino]methyl]-1-pyrrolidinyl] -7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid; 8-amino-9-fluoro-3-methyl-10-[3-[(ethylamino)methyl]-1-pyrrolidinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid; 8-amino-9-fluoro-3-methyl-10-[2,7-diazaspiro[4.4]non-2-yl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid; 8-amino-9-fluoro-3-methyl-10-[7-(7-methyl)-2,7-diazaspiro[4.4]non-2-yl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid; and 8-amino-9-fluoro-3-methyl-10-[7-(7-ethyl)-2,7-diazaspiro[4.4]non-2-yl]-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de][1,4]benzoxazine-6-carboxylic acid.
Example 7
5-Amino-1-cyclopropyl-6,8-difluoro-7-[(3-ethylaminomethyl)-1-pyrrolidinyl]-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid
A solution of 0.43 g (1.5 mmoles) of 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, 0.61 g (6.0 mmoles) of triethylamine, 0.77 g (6.0 mmoles) 3-(ethylaminomethyl)pyrrolidine and 25 ml of acetonitrile was heated at reflux for two hours. The solvent was removed in vacuo and the residue was dissolved in water and filtered through a fiber glass pad to remove a trace of insoluble material. The filtrate was adjusted to pH 7.0 and the resulting precipitate removed by filtration, washed with water, and dried in vacuo to give 200 mg of the title compound, mp 250-252° C.
Example 8
5-Amino-7-(3-amino-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic Acid
To 1.57 g (5 mmol) of 5-amino-8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinoline carboxylic acid in 20 ml of acetonitrile was added 0.93 g (5 mmol) of 3-[(t-butoxycarbonyl)amino]pyrrolidine and 1.0 g (10 mmol) of triethylamine. The mixture was refluxed for three hours, cooled, and filtered. The solids were washed with acetonitrile and ether, then dissolved in 10 ml of acetic acid and 2 ml of 3N hydrochloric acid. The mixture was heated at 100° C. for four hours, concentrated, and triturated with 2-propanol. The solid that formed was filtered and washed with ether to give 1.2 g of the title compound.
The following compounds were also prepared by a similar procedure: 5-amino-8-chloro-1-cyclopropyl-7-[3-[(ethylamino)methyl]-1-pyrrolidinyl]-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid; 5-amino-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-7-[3-[(methylamino)methyl]-1-pyrrolidinyl]-4-oxo-3quinolinecarboxylic acid; 5-amino-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-7-[3-[(dimethylamino) methyl]-1-pyrrolidinyl]-4-oxo-3-quinolinecarboxylic acid; 5-amino-7-[3-(aminomethyl)-3-methyl-1-pyrrolidinyl]-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid; 5-amino-8-bromo-1-cyclopropyl-7-[3-[(ethylamino)methyl]-1-pyrrolidinyl]-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid; 5-amino-8-bromo-1-cyclopropyl-6-fluoro-1,4-dihydro-7-[3-[(methylamino)methyl]-1-pyrrolidinyl]-4-oxo-3-quinolinecarboxylic acid; 5-amino-8-bromo-1-cyclopropyl-6-fluoro-1,4-dihydro-7-[3-[(dimethylamino)methyl]-1-pyrrolidinyl]-4-oxo-3-quinolinecarboxylic acid; 5-amino-7-(3 -amino-1-pyrrolidinyl)-8-bromo-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid; 5-amino-7-(3-amino-1-pyrrolidinyl)-1-cyclopropyl-6-fluoro-8-trifluoromethyl-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-6-fluoro-8-trifluoromethyl-1,4-dihydro-7-[3-[(methylamino) methyl]-1-pyrrolidinyl]-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-7-[3-[(ethylamino) methyl]-1-pyrrolidinyl]-6-fluoro-8-trifluoromethyl-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-6-fluoro-8-trifluoromethyl-1,4-dihydro-7-[3-[(dimethylamino)methyl]-1-pyrrolidinyl]-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-7-[3-[(ethylamino)methyl]-1-pyrrolidinyl]-6-fluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-6-fluoro-1,4-dihydro-7-[3-[(methylamino)methyl]-1-pyrrolidinyl]-8-methoxy-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-6-fluoro-1,4-dihydro-7-[3-[(dimethylamino)methyl]-1-pyrrolidinyl]-8-methoxy-4-oxo-3quinolinecarboxylic acid; 5-amino-7-(3-amino-1-pyrrolidinyl)-1-cyclopropyl-6-fluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-7-[3-[(ethylamino)methyl]-1-pyrrolidinyl]-6-fluoro-1,4-dihydro-8-hydroxy-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-6-fluoro-1,4-dihydro-8-hydroxy-7-[3-[(methylamino) methyl]-1-pyrrolidinyl]-4-oxo-3-quinolinecarboxylic acid; 5-amino-1-cyclopropyl-6-fluoro-1,4-dihydro-8-hydroxy-7-[3-[(dimethylamino)methyl]-1-pyrrolidinyl]-4-oxo-3-quinolinecarboxylic acid; 5-amino-7-(3-amino-1-pyrrolidinyl)-1-cyclopropyl-6-fluoro-1,4-dihydro-8-hydroxy-4-oxo- 3-quinolinecarboxylic acid; 7-(3-amino-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-5-methoxy-4-oxo-3-quinolinecarboxylic acid; 7-(3-amino-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-5-hydroxy-4-oxo-3quinolinecarboxylic acid; 7-(3-amino-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-5-methylamino-4-oxo-3-quinolinecarboxylic acid; 7-(3-amino-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-5-dimethylamino-4-oxo-3-quinolinecarboxylic acid; 8-chloro-1-cyclopropyl-7-[3-[(dimethylamino) methyl]-1-pyrrolidinyl]-6-fluoro-1,4-dihydro-5-methoxy-4-oxo-3-quinolinecarboxylic acid; 8-chloro-1-cyclopropyl-7-[3-[(dimethylamino)methyl]-1-pyrrolidinyl]-6-fluoro-1,4-dihydro-5-hydroxy-4-oxo-3-quinolinecarboxylic acid. | Novel naphthyridine-, quinoline- and benzoxazinecarboxylic acids as antibacterial agents are described as well as methods for their manufacture, formulation, and use in treating bacterial infections including the description of certain novel intermediates used in the manufacture of the antibacterial agents. | 2 |
RELATED APPLICATIONS
[0001] This application is related to U.S. patent application Ser. No. 10/446,006, filed May 22, 2003 and U.S. patent application Ser. No. 10/871,557, filed Jun. 18, 2004.
FIELD OF THE INVENTION
[0002] This invention relates to the protection of property against high winds and, in particular, to a flexible protective barrier device for securing property against the force of winds, rain and from impact of foreign objects carried by localized atmospheric over-pressure.
BACKGROUND OF THE INVENTION
[0003] As is known by one skilled in the art of protecting buildings and the like from damage caused by missile-like objects that are occasioned by the heavy winds of hurricanes, tornadoes, or explosive over-pressures, there are commercially available variations of hurricane protective devices, often called shutters, that fasten immediately over the frangible area to be protected. These devices are typically expensive to purchase cumbersome, made from stiff, heavy material such as steel and aircraft quality aluminum alloy or occasionally reinforced plastic. Many need to be manually connected and then removed and stored at each threat of inclement weather. Many require unsightly and difficult-to-mount reinforcing bars at multiple locations. Further, these known shutters are usually opaque, preventing light from entering a shuttered area and preventing an inhabitant from seeing out. Likewise, it is desirable that police be able to see into buildings to check for inhabitants and to prevent looting which can be a problem in such circumstances.
[0004] Missiles, even small not potentially damaging missiles, striking these heretofore known shutters create a loud, often frightening bang that is disturbing to inhabitants being protected. Standardized testing requiring these protective devices to meet certain standards of strength and integrity has been introduced for various utilizations and locales. In order to qualify for use where testing requirements apply, the strength and integrity characteristics of these protective devices must be predictable and must be sufficient to meet mandated standards.
[0005] Additionally, it is beneficial to qualify for these standards even in situations in which standards do not apply. As a result of these standards, many undesirable aspects of the previously known shutters have been acerbated. They have become more cumbersome, more bulky, heavier, more expensive, more difficult to store, and remain generally opaque and noisy when impacted.
[0006] To incorporate sufficient strength to meet said requirements, weight and bulk become a problem over six feet in span. The useable span (usually height) of the heretofore known shutters that meet said standards may be limited to eight feet or less. This makes protecting large windows, for example, or groupings of windows, with the heretofore known devices cumbersome, expensive and impractical. Devices that are intended to be deployed in a roll down manner either manually, automatically, or simply by motor drive, have been difficult to strengthen sufficiently to pass the test requirements and require unsightly reinforcing bars every few feet.
[0007] Prior to the introduction of said standards, an ordinary consumer had very little useful knowledge of the strength and integrity of said shutters. It is believed shutters of the pre-standard era were very weak such that all would fail the present standardized testing. As the hurricane conditions can be very violent and destructive, the standards are not intended to require strength and integrity sufficient to protect in all circumstances. The standards simply provide a benchmark as to strength and integrity. The strength and integrity of the shutters can now be measured by standardized tests.
[0008] There are many patents that teach the utilization of knitted or woven fabric such as netting, tarpaulins, drop cloths, blankets, sheets wrapping and the like for anchoring down recreational vehicles, nurseries, loose soil and the like. But none of these are intended for, nor are capable of withstanding the forces of the missile-like objects that are carried by the wind in hurricanes or explosive over-pressures.
[0009] Some protection devices have internal stiffness and rigidity that resists deflection, or bending. In rigid protection devices, it is stiffness that stops the missile short of the frangible surface being protected.
[0010] Other protection devices use fabric or netting material to cover a unit to be protected. Typically, the device completely covers the unit, and edges of the fabric are fastened to the ground. Examples of fabric employing devices are shown in the following patents: U.S. Pat. No. 3,862,876 issued to Graves, U.S. Pat. No. 4,283,888 and U.S. Pat. No. 4,397,122 issued to Cros, U.S. Pat. No. 4,858,395 issued to McQuirk, U.S. Pat. No. 3,949,527 issued to Double et al., U.S. Pat. No. 3,805,816 issued to Nolte, U.S. Pat. No. 5,522,184 issued to Oviedo-Reyes, U.S. Pat. No. 4,590,714 issued to Walker and U.S. Pat. No. 5,522,184 issued to Pineda. U.S. Pat. No. 5,522,184, for example, provides a netting that fits flush over the roof of a building and uses a complicated anchoring system to tie down the netting.
[0011] Typical of known flexible, fabric-employing protection devices is the characteristic of substantial rain and wind-permeability. For example, U.S. Pat. No. 5,579,794, issued to Sporta, discloses a wind-permeable perforate sheet that extends downwardly and outwardly from the top of the object to be protected at an acute angle so as to surround a substantial portion of each of the sides with an inclined wind-permeable planar surface.
[0012] U.S. Pat. No. 6,325,085 to Gower illustrates a barrier similar to the instant invention to be deployed inside a building or over individual windows. U.S. Pat. No. 6,176,050 to Gower teaches the use of the barrier material of this invention deployed over multi-story buildings. Both patents are incorporated herein by reference.
[0013] Thus, what is lacking in the art is an improved flexible protective barrier constructed from a mesh material with substantial rain and impact resistance that can be easily stored and deployed in combination with a flexible, inflatable, reinforcing cushion for protecting the frangible portion of a structure not only from objects carried by the wind but also from the force of the wind itself.
SUMMARY OF THE INVENTION
[0014] Therefore, it is an objective of this invention to teach the use of a flexible barrier synthetic textile that is able to satisfy stringent testing requirements. When used with a building, for example, the top edge of the fabric may be anchored to the eave of the roof and the bottom of the fabric may be attached to anchors imbedded in the foundation, ground or cement, so as to present a curtain adequately displaced from and in front of the structure of the building to be protected.
[0015] Knitted, woven or extruded material can be used if the material itself meets the criteria described later herein. The device provides a barrier that is substantially impermeable to rain and wind. Although air travels through the barrier, the barrier is approximately 95% closed, and the velocity of wind passing through the device is greatly reduced. For example, the velocity of a 100 mph wind is reduced by approximately 97% by passing through the wind abatement system of the present invention. The wind abatement system of the present invention substantially reduces the force of wind passing through the device and also provides a barrier against wind-borne missiles having diameters of approximately 3/16 inch in diameter or larger. Also, rain drops striking the barrier are reduced in velocity and dispersed into a mist which reduces the water damage to the structure.
[0016] Alternatively the material can be termed to be solid wherein the fabric is coated or the interstices of the fabric are filled by either close weaving, or use of a coating.
[0017] The inflatable cushion(s) between the fabric and the building provide displacement and pneumatic dissipation of the force of impact of debris on the fabric. This pneumatic plenum allows the flexible barrier system to be in direct contact with the structure being protected.
[0018] Another objective of this invention is to teach the use of very large areas with spans covering greater than 25 feet. Thus most window groupings, from a single window up to several stories of a building, could be readily protected. This invention is light in weight, easy to use, does not require reinforcing bars, can be constructed in varying degrees of transparency, can be weather tight, is economical, and is capable is dissipating far greater forces without damage than conventional stiff devices. Missiles striking this barrier make very little sound. Additionally, this invention is suitable to be configured with the necessary motor and mounting devices for automatic deployment.
[0019] Another objective of the invention is to permit the adaptation of the invention to meet a particular enclosure or object. For instance, the inflatable cushion(s) may be placed over a window, preferably a wind rated window, to provide the necessary spacing. Alternatively the inflatable cushion(s) may be placed over the mullions of a window thereby transferring wind loading directly to the inflatable cushion and thus to the structure of the mullion. Further, the inflatable cushion(s) may be placed along the edge of the window or on the structure abutting window. Similarly, the inflatable cushion(s) may be placed adjacent an object, such as a tiled wall, painting, statue, sculpture, or the like, to prevent wind, rain, and debris from impacting the object.
[0020] It is a further objective of this invention to teach a wind barrier that does not rely on rigidity but rather is very flexible, which gives several positive features including allowing for ease of storage as by deflating and rolling or folding. The fabric material in this barrier system is displaced from the structure being protected and this displacement is a function of the depth of the inflatable cushion. An impacting missile stretches the barrier until it decelerates to a stop or is deflected. The fabric material has a predetermined tensile strength and stretch that makes it suitable for this application. The known strength and stretch, together with the speed, weight and size of the impacting missile, all of which are given in test requirements, permit design calculation to ascertain barrier deflection at impact. The cushion is capable of a deflection, due to compression, commensurate with the stretch of the fabric to prevent rupture.
[0021] Thus greater energy from a missile can be safely dissipated than is possible with the prior art structures, and the energy which can be safely dissipated is calculable. In simple terms, the missile is slowed to a stop by elasticity as the barrier stretches and compression as the cushion deforms. The greater the impact, the greater the stretch and compression. Thus the building is not subjected to an abrupt harsh blow as the energy transfer is much gentler and less destructive that with the rigid devices.
[0022] It is yet another objective of this invention to teach the use of a screen-like fabric with interstices that permit the light to pass through and that is reasonably transparent, if desired. If transparency is not desirable, the fabric can be made sufficiently dense to minimize or eliminate the interstices. To assure a long life the material of the fabric preferably would be resistant to the ultra violet radiation, and to biological and chemical degradation such as are ordinarily found outdoors. This invention contemplates either coating the material or utilizing material with inherent resistance to withstand these elements. A synthetic material such as polypropylene has been found to be acceptable. Another example is a coated material of vinyl coated polyester. The coating may fill interstices to make a solid material. The fabrics may use natural or synthetic fibers and blends of fibers or blends of yarns, e.g., an open weave with steel reinforcing strands there through or Kevlar or other ballistic yarns. Materials intended to be used outdoors in trampolines, for example, are more likely candidates for use in this invention. Black colored polypropylene is most resistant to degradation from ultra violet radiation. Other colors and vinyl coated polyester are sufficiently resistant, particularity if the barrier is not intended to be stored in direct sunlight when not in use.
[0023] These same materials may be used to form the walls of the inflatable plenums or cushions. The cushions may be coated or laminated on the outside or inside surfaces to form air tight cells. The cushions may be made of extruded polymeric films. The desired amount of deformation, in the cushion, is a function of the elasticity of the material and the inflation pressure. The plenums may also be thin walled structures inserted into a sleeve of the barrier material which provides the requisite strength.
[0024] The preferred embodiment of the fabric allows air passage through it, albeit at substantially reduced rate. In one embodiment, upwind pressure of 1″ of mercury, which roughly translates into a 100 mph wind, forces air through at 250 cfm or approximately 3 mph. The amount of air passage depends on the interstice size and percentage of openness. If a weather tight and transparent barrier is desired, the polypropylene material may be laminated with a flexible clear plastic skin.
[0025] It is of importance that the material affords sufficient impact protection to meet the regulatory agencies' requirements in order for this to be a viable alternative to other hurricane protective mechanisms. While stiff structures, such as panels of metal, are easily tested for impact requirement and have certain defined standards, fabrics on the other hand, are flexible and react differently from stiff structures. Hence the testing thereof is not easily quantified as the stiffer materials.
[0026] However, certain imperial relationships exist so that correlation can be made to compare the two mediums. Typically, the current impact test of certain locales requires a wood 2×4 stud be shot at the barrier exerting a total force of approximately 351 foot pounds, or 61.3 psi, over its frontal (impacting) surface. This impact and resultant force relate to the Mullen Burst test commonly used by manufacturers to measure the bursting strength of their fabrics. Thus the impact test heretofore used on rigid devices will work equally well on this flexible device.
[0027] The preferred embodiment of this invention would use a textile of the type typically used in trampolines which would burst at least 675 psi or a total of 2,531.25 pounds over the same 3.75 square inch frontal surface of the nominal 2×4 test missile wherein stretch characteristics of the material are known. The strength and stretch characteristics of the material are also known. The strength of this fabric is more than eleven (11) times the 351 foot pounds of strength required to withstand the above-described 2×4 missile test as presently required by said regulatory agencies. Stronger fabrics are available. Others are available in various strengths, colors and patterns.
[0028] The use of flexible fabric distanced out from the frangible area as a protective barrier allows extended deceleration. When the strength and stretch properties of the fabric are known and allowed for, as well as, these same properties in the inflated cushion, the extended deceleration becomes controlled. By mounting the protective barrier material some distance from the frangible surface, i.e., the thickness of the inflated cushion, a distance that is calculable, the missile can be decelerated to a stop prior to contacting the frangible surface. And the pounds per square inch of impact force are spread throughout the inner surface of the cushion. In other words, in any situation where the missile must stop prior to impacting the frangible surface being protected, it is desirable to decelerate the missile through an extended, controlled deceleration. This invention does precisely that. Since the use of a flexible material as a protective barrier affords an extended deceleration, very strong impacts can be withstood.
[0029] A further objective of this invention is to teach a barrier made from fabric to protect the frangible portions of a building and the like from the force of wind, or over pressure, and impact from water or other liquids and wind-borne debris by displacing the barrier out from and in front of the frangible area with inflatable cushions. The barrier is mounted on the building by attaching two opposing edges to anchors located so as to position the barrier as described. For example, one edge of the fabric can be anchored to the overhang of the roof or other high structure and the opposite edge of the span to the ground or low structure. The lower anchors can be attached to the foundation of the building or the ground by embedding in cement or other ground attachment such as tie downs or stakes and the like and providing grommets, rings or other attachments in the fabric to accept a clamp, cable, rope, and the like.
[0030] Another objective of this invention is to teach an inflatable structure placed between any opening in a structure and may be spaced from the structure a greater distance than the thickness of the cushion to allow for some deceleration before the cushion is compressed.
[0031] Still another objective of this invention is to teach the use of a retainer for deploying and securing the two opposing edges of a wind barrier material to retainer channels located so as to form a structure envelope about the openings with the barrier spanning the opening.
[0032] The curtain-like barrier of this invention is characterized as a barrier with strength and simplicity that is unattainable with the heretofore known barriers. Impact by a missile does not cause a large bang, and is not disturbing. It is easy to install, requires low maintenance and has low acquisition cost. There is much flexibility with storage. It can either be left in place or rolled much as a shade, or slid out of the way much as a curtain, so as not to interfere with the aesthetics of the building. It can also be fully removed and stored out of the way, or swung up to form a canopy when not in use as a protective barrier. It is preferable but not essential, that the material selected to be used in the netting fabric of this invention be inherently resistant to elements encountered in the outdoors or can be coated with coatings that afford resistance to these elements. The inflatable cushions can be separate from the netting or attached by interweaving, fasteners or pockets in the netting. The cushions may be stored with the netting or removed for storage elsewhere.
[0033] Another objective of this invention is to teach the use of valves in the inflatable cushions whereby they can be deflated for storage and inflated once the barrier is in place on the building.
[0034] Other objectives and advantages of this invention will become apparent from the following description taken in conjunction with the accompanying drawings wherein are set forth, by the way of illustration and example, certain embodiments of this invention. The drawings constitute a part of this specification and include exemplary embodiments of the present invention and illustrate various objects and features thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
[0035] FIG. 1 is a partial view in perspective and schematic illustrating this invention partially deployed and attached to a building;
[0036] FIG. 2 is a partial cross section and side view illustrating the protective barrier and inflated cushion in place;
[0037] FIG. 3 is a perspective of the barrier showing holders for the cushions;
[0038] FIG. 4 is a detailed showing of a mechanism for attaching the retainers to the barrier;
[0039] FIG. 5 is a detailed view of another mechanism for attaching the retainers to the barrier;
[0040] FIG. 6 is a diagrammatic and schematic view illustrating the channel;
[0041] FIG. 7 is a perspective of a protective barrier for individual openings or small groups of openings; and
[0042] FIG. 8 is a perspective of a single window with an inflatable barrier in place.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0043] This barrier 10 is made up of a flexible material 11 that has known qualities of strength, stretch and deformation and is sufficiently strong to withstand applicable impact testing and one or more inflatable plenums or cushions 12 . The barrier 10 does not derive its strength from stiffness or rigidity but rather from its bursting strength and stretch, with the latter acting like a spring to gradually decelerate any impacting missile. Wind speed may become a significant factor in larger spans.
[0044] There are many desirable characteristics of this barrier 10 , such a resistance to weathering, light weight, ease of installation, deployment and storage, economy. Additionally, there are several methods of deploying and storing this barrier. While this invention is shown in its preferred embodiment as being utilized to protect the windows and overhang roof, shown in FIG. 2 , of a structure, it is to be understood that this item has utility for other items requiring protection and is applicable to other types of structures, as shown in FIG. 8 . Where appropriate, the barrier and inflatable plenums can be deployed horizontally, as well as, the vertical as shown in FIGS. 1-2 .
[0045] Reference is now made to FIGS. 1-6 which partially show a building structure 100 including windows 110 intended to be protected from the onslaught of winds and debris typically occasioned during a hurricane. According to this invention the top of a curtain panel or material 11 , made from a textile woven of a suitable fiber, (other weaves or knits may be used) is attached to roof 16 and the bottom thereof is attached to the foundation 200 . A suitable material is polypropylene formed in a monofilament and woven into geotextile (style 20458) manufactured by Synthetic Industries of Gainesville, Ga. The fabric is woven in a basket (plain) weave as in the preferred embodiment in interstices are substantially equal to 0.6 millimeters which approximates the interstices of commercially available residential window screening.
[0046] The selection of interstices size and configuration is dependent on the amount of transparency and air passage desired and the limitation that the maximum size must be sufficiently small to prevent objects that are potentially damaging on impact from passing there through. The above-mentioned regulations, set in place by Miami-Dade County, Florida, have determined that the smallest diameter missile (wind blown debris) with which they are concerned is 3/16 inch in diameter. Therefore to satisfy the Dade County Regulations the interstices must be small enough to prevent 3/16 inch diameter missiles from passing there through. Other regulations may set other minimum missile diameter sizes, and the interstice size would vary accordingly if new standards were to be met. The parameters of the test and the fabric are fully discussed in U.S. Pat. No. 6,176,050.
[0047] The cushions 12 have conventional inflation-deflation valves 116 , such as those used in tires or sports equipment. The valves may include a safety valve which will open when a pre-selected internal pressure is exceeded. This will prevent rupture of the cushion. The inflation pressure of the cushions 12 can be adjusted to compensate for the impact pressure of the debris or test missile. A higher inflation pressure would decrease the amount of deflection of the material. In this manner, the improved barrier 10 would not require the spacing necessary with the material, per se. For example, a cushion having a depth of 2 feet may be used in spans from 8 feet to 40 feet and beyond. This permits attachment of the bottom of the barrier to the protected structure, as shown in FIG. 8 , rather than being displaced away from the building.
[0048] The top of the barrier 10 is secured to the roof 101 , facia 102 , or under the eave 103 . The bottom of the barrier would be secured to the foundation 200 of the building by fasteners 119 . The longitudinal sides 13 , 14 of the barrier are mounted in retainers 104 , 105 . The retainers 104 , 105 , as shown in FIG. 6 , are elongated box-shaped metal sections permanently attached to the building. The retainers may be installed in sections or as a seamless whole. The top of the retainers 104 , 105 have a flared opening 106 , 107 to facilitate the feeding of the barrier 10 into the retainers as the barrier 10 is unrolled into position.
[0049] The base 108 of the retainers is bolted or otherwise fixed to the structure 100 . The top wall 114 is parallel to the base. The outer wall 109 has a height that provides the spacing of the material 11 from the building 100 to permit the inflatable cushions to be deployed. The outer wall 109 of the opposite retainers 104 , 105 enclose the longitudinal edges of the barrier to prevent wind entry between the barrier and the building. The inner wall 110 has a longitudinal groove 111 through which the longitudinal selvage edge of the material 11 slides. The groove 111 terminates in an enlarged channel 112 of a size and shape to permit the pins 113 to move.
[0050] The pins 113 , shown in FIGS. 4 and 5 , are tapered from the central position toward each end. The pins may be attached to the longitudinal selvage by tabs 120 or hemmed into the selvage. As the barrier is deployed each pin enters the flared end of the retainers and slides down the channel. Since the slot is narrower than the diameter of the pins, the pins are captured in the channels. Other arrangements can include a cable attached to the longitudinal edges of the material.
[0051] Once the minimum space between the barrier and the structure being protected is established, the fabric must be anchored in a suitable manner so as to absorb the loads without being torn from its support. While various hardware devices may be used to anchor the fabric in place, general criteria include stainless steel bolts with 0.5 inch diameter and 1,000 lbs. max. bolt loading; 0.375 inch diameter and 625 lbs. max. bolt loading; with minimum pull-out force for steel 20× bolt loading; concrete 3,000 psi, spaced to achieve 1,100 lbs./linear foot; wood 2,400 lbs/linear inch of engaged thread; ground 8 inch helix ground anchor with 9,900 lbs. holding force in class 5 soil. These criteria are merely exemplary and not limiting. Other anchoring hardware may be used to install protective barrier of this invention.
[0052] As shown in FIGS. 1 and 2 the protective barrier 10 may be unrolled from a spindle 15 that is attached to the roof 101 or the eaves 103 of the roof by suitable threaded bolts or screws. The spindle attaching method allows for ease of installation as the installer can wrap the material around the spindle as necessary to adjust the material to the span and then attach the spindle to the building. Additionally, the use of a spindle 15 allows the edge if the barrier to be securely fastened overhead in a simple and economical method. Other methods are available in appropriate situations. The lower edge is fastened by anchors 118 set in recesses formed into the foundation to bury or partially bury eyebolts.
[0053] The material 11 may also be fabricated with a top and bottom selvage or hem or can utilize a reinforcing tape such as “Polytape” that is made from a polypropylene material. The selvage or tape may include commercially available grommets or rings to accept the tie-down hardware. The side margins may also have a selvage or other reinforcement with either grommets or ties for fastening to anchors placed in the wall of the structure.
[0054] The material, as shown in FIG. 3 , may have one or more belts 117 for containing the cushions in alignment with the material 11 . The belts may be of the same material or an elastic fabric. The belts 117 may be formed as loops with intermediate portions attached to the barrier by interweaving, adhesives or other fasteners. The loops would accommodate the width of the cushions. Alternatively or in addition, pockets may be fashioned in the top and bottom to enclose the ends of the cushions. The cushions or plenums may be completely surrounded by the fabric, as shown in FIG. 7 .
[0055] The multiple story installation may be deployed simply by attaching the upper edge of the barrier to the bolts on the building and feeding the barrier into the top of the retainers then allowing the barrier to fall toward the ground. Once the lower edge becomes free, it can then be attached to a set of lower fasteners located at the corresponding vertical height on the building or the ground. The barrier can be winced down by a hand crank or motorized winch (not shown) attached by a line to the bottom selvage of the barrier. Thin metal, polymeric or wooden battens 115 may be placed across the width of the barrier at spaced intervals to control deployment evenly. Once the barrier is in place, the cushions 12 are inflated to the desired pressure. To store the barrier, the cushions are deflated and either removed or rolled up with the material 11 .
[0056] The inflatable wind barrier may be deployed for individual openings such as windows and doors rather than covering major surfaces of a building, as shown in FIG. 8 . FIG. 7 illustrates a plenum 12 encompassed by the material 11 . The material 11 has flaps 131 , 132 extending outwardly from the sleeve 130 . Each flap terminates in a selvage 135 , as shown. Grommets 133 are attached through the selvage 135 providing apertures 134 to connect to anchors along the periphery of the opening. Top and bottom flaps may also be provided. Other attachment devices, such as hooks, may be used in place of the grommets.
[0057] The cushions or plenums 12 may be inflated by pumps supplying high volume low pressure inflation, HVLP, for example home vacuum cleaners through a valve. The valve may include a means for sealing of the opening similar to a tire valve, inflatable dinghy valve, or conventional air cushion valve.
[0058] FIG. 8 illustrates a single frangible opening, such as a window 201 , in a larger structure. The structure has a set of fasteners 202 mounted about the periphery of the window. Connected to these fasteners are the edges of the barrier material 11 . The edges may have selvages and grommets 203 as mentioned above. Plenums 204 are located between the barrier and the window and are held in place by the fabric of the barrier. The plenums provide the spacing necessary for the fabric to decelerate debris, such as solids and liquids, before striking the frangible portion of the window. However, even if the frangible portion is broken, the barrier remains intact providing protection to the interior of the structure.
[0059] The inflatable cushion(s) permit adaptation of the barrier to meet the design of a particular enclosure or object. For instance, the inflatable cushion(s) may be placed directly over a window, preferably a wind rated window, to provide the necessary spacing of the fabric from the glass. Alternatively the inflatable cushion(s) may be placed over the mullions of a window thereby transferring wind loading directly to the inflatable cushion and thus to the structure of the mullion. Further, the inflatable cushion(s) may be placed along the edge of the window which is stronger than the center, or on the structure abutting window such as the frame or actual structure abutting the window. Similarly, the inflatable cushion(s) may be placed adjacent an object, such as a tiled wall, painting, statue, sculpture, or the like, to prevent wind, rain, and debris from impacting the object.
[0060] Although this invention has been shown and described with respect to detailed embodiments thereof, it will be appreciated and understood by those skilled in the art that various changes in form and detail thereof may be made without departing from the spirit and scope of the claimed invention. | A flexible hurricane shutter or barrier to protect buildings from over pressure has inflatable cushions held in place by a fabric material capable of withstanding winds in excess of 100 mph. The barrier can be stored on site in a rolled fashion. Retainers are mounted on a building to guide and secure the longitudinal edges of the fabric to permit ease of deployment. The retainers may be spaced apart over one side of a building and the barrier may be deployed over an entire surface of a multi-story building by raising and lowering the fabric. Inflatable cushions are held between the fabric and the building. The inflated cushions reinforce the material and distribute the force of impact throughout the surface of the cushions and act as spacers to both hold the fabric off the structure and focus the forces onto stranger portions of the structure. | 4 |
BACKGROUND OF THE INVENTION
This invention relates generally to a rotary finishing tool, and more particularly, to a rotary finishing tool for removing rough, burred or sharp edges from a workpiece. The workpiece generally includes a core material and a plurality of laminate members affixed to at least two surfaces of the core material.
Conventionally extra laminate material is removed from an edge of the laminated workpiece prior to hand finishing. Hand filing is generally required to finish the edge so as to remove burrs, knicks and any sharp edges on the workpiece. Hand filing a workpiece to a finished edge is labor intensive and expensive but necessary in order to finish the workpiece to the specifications generally demanded and expected, particularly for custom work. Furthermore, hand filing is something of an art and an unskilled worker can easily ruin an expensive workpiece during the final stages of preparation.
Prior tools have provided for preparing mitered joints, U.S. Pat. No. 3,955,607; beveled edges, U.S. Pat. Nos. 3,893,372 and 3,241,453; or tools using a ball or spherical cutter, U.S. Pats. No. 4,504,178 and 4,279,554. Prior tools have also provided cutting tool gauges, U.S. Pat. No. 4,156,990; and trimming laminate plastic sheets, U.S. Pat. Nos. 3,981,226; 3,721,157; and 4,044,805.
The rotary finishing tool of the present invention solves these and other problems in a manner not disclosed in the known prior art.
SUMMARY OF THE INVENTION
In the present invention power means are provided for operating the rotary finishing tool. The rotary finishing tool includes a housing for the power means. A finishing bit is operatively associated with the power means. The finishing bit generally includes at least one radius cutting surface for finishing an edge of a workpiece. Guide means are provided for guiding the rotary finishing tool along the edge of the workpiece. The guide means includes a base member and a guide member. The base member is operatively associated with the power means housing for telescoping axial movement. The guide member defines a plane substantially perpendicular to the rotational axis of the finishing bit. The guide member further defines a plane substantially parallel to the rotational axis of the finishing bit. The guide member provides proper orientation between the rotary finishing tool and the workpiece such that the finishing bit removes substantially all sharp, burred or rough edges from the edge of the workpiece. Adjustment means are provided for axially adjusting the finishing bit relative to the guide member and the workpiece. The adjustment means takes advantage of the telescoping relationship between the power means housing and gude means.
It is an aspect of the present invention that a rotary finishing tool is provided that alleviates the need for hand filing to finish a laminated workpiece.
It is another aspect of the present invention that a rotary finishing tool is provided with an adjustment means providing for ease of adjustment in order that the tool can be used on different laminates having different thicknesses.
It is another aspect of the present invention that a rotary finishing tool is provided that is easy to use and, because it is easy to use, can reduce the amount of labor required to accomplish the labor intensive task of finishing the workpiece edge.
It is another aspect of the present invention that a rotary finishing tool is provided that includes a non-spherical finishing bit.
It is another aspect of the present invention that a rotary finishing tool is provided that includes a removable finishing bit. The finishing bit can be removed when dulled and replaced with a new finishing bit or the finishing bit can be sharpened and replaced.
It is another aspect of the present invention that a rotary finishing tool is provided with a finishing bit including at least one radius cutting surface. Furthermore, only the cutting edge of the finishing bit contacts the workpiece.
It is another aspect of the present invention that a rotary finishing tool is provided in which the power means is an air motor.
It is another aspect of the present invention that a rotary finishing tool is provided with a guide means including a guide member for guiding the rotary finishing tool along the edge of the workpiece. The guide member may include low friction shims providing minimum friction between the guide member and the workpiece.
BRIEF DESCRIPTION OF THE DRAWINGS
Further features and characteristics of the present invention can be seen from the figures and descriptions below in which:
FIG. 1 is an elevation of an embodiment of the present invention,
FIG. 2 is a sectional view taken along line 2--2 in FIG. 1,
FIG. 3 is a sectional view taken along line 3--3 in FIG. 2,
FIG. 4 is a sectional view taken along line 4--4 in FIG. 1, and
FIG. 5 is a detailed elevation of a finishing bit and workpiece.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now by characters of reference to the drawings and first to FIG. 1 it will be understood that a rotary finishing tool or tool generally indicated by reference character 10 includes a power means 12, a guide means 14, and an axial adjustment means. In the preferred embodiment the power means 12 includes a pneumatic motor also referred to as an air motor. The adjustment means generally includes a cam means and further includes a cam ring 16 and a cam surface 17. The tool 10 uses a finishing bit 18 driven by the air motor 12. The finishing bit is preferably a carbide bit. The tool 10 further includes a power means housing 20, for example, a generally cylindrical body that serves as an air motor housing. The air motor housing 20 is associated with a base member 46 in a telescoping axial relationship.
The air motor 12 includes a compressed air inlet 22 for the compressed air necessary to operate the tool 10. An adjustment screw 24 provides for pressure regulation of the compressed air supplied to operate the tool 10. A typical compressed air fitting 23 illustrates one possible connection between the tool 10 and a compressed air line from a compressed air source.
Typically, the air motor 12 operates in response to depression of a push button 26. A lever assembly 28 includes a lever arm 30 that pivots on a hinge 32. One hand operation of the lever assembly is normally sufficient to control compressed air to the air motor 12 and operate the tool 10.
The air motor housing 20 includes a shoulder means 38. The cam means forming a part of the axial adjustment means is operatively associated with the shoulder means 38. The cam ring 16 is free to rotate about the air motor housing 20 when not fixed in place by a retaining means. In the preferred embodiment a cam ring set screw 44 is the retaining means.
A finishing bit chuck 42 attached to an output shaft 40 of the air motor 12 releasably operatively carries the finishing bit 18 for rotation about its axis by the air motor 12. The base member 46 associated with the guide means 14 generally conceals the lower portion of the air motor 12 including the output shaft 40 and chuck 42. The base member 46 will preferably be a generally cylindrical base member. The air motor housing 20 fits within the cylindrical base member 46 and can move at least axially within base member 46 in a generally telescoping fashion.
An upper end portion 47 of the base member 46 includes additional structure forming part of the adjustment means. The additional structure is a base member flange 48 formed on the upper end portion 47. The base member flange 48 carries a projection or pin 50 in a pin aperture 51 and another retaining means or base member set screw 52. The base member set screw 52 acts as a set screw to fix the cylindrical base member 46 relative to the air motor housing 20.
The base member 14 includes a notch 54. The notch receives a guide member 56 as generally shown in FIG. 2.
The finishing bit 18 extends at least partially through a guide member aperture 62 defined by the guide member 56.
The guide member includes one guide member portion, a horizontal guide member 58 and another guide member portion, a vertical guide member 60. The horizontal guide member 58 defines a plane generally perpendicular to the rotational axis of the finishing bit. The vertical guide member 60 defines a plane generally parallel to the rotational axis of the finishing bit.
In a preferred embodiment the horizontal guide member 58 includes a shim 64 and the vertical guide member 60 includes another shim 66. The shims 64, 66 are preferrably plastic to allow the guide member arrangement to slide easily over a workpiece 78.
The finishing bit 18 includes a shank member 67 that is received by the chuck 42. The finishing bit further includes a body 68 and at least one cutting flute 69 with a radius cutting edge 70. The finishing bit 18 tapers off to a generally blunt end 71.
As an illustration of one preferred embodiment of the rotary finishing tool the operation of the tool will now be described. Reference is made to FIGS. 2, 4 and 5. The tool 10 is generally intended for removing rough, burred or sharp edges from an edge 76 of the workpiece 78. The workpiece 78 generally includes a core material 80 an upper laminate member 82 and at least one side laminate member 84.
It should be noted that the end 71 of the finishing bit 18 does not contact the workpiece during the finishing process. Only the cutting edge 70 contacts the workpiece 78.
Assembly of the workpiece 78 will be only briefly described. Typically the workpiece, for example a laminated counter top, is assembled by applying the side laminate member to an edge of the core material 80. The top edge of the side member is trimmed flush with the top surface of the core material 80. The edge left by the trimming step is rough, burred and often includes sharp sections. The upper laminate member 82 is applied to the top surface of the core material 80 and the edge of the upper laminate member 82 is trimmed flush with the side laminate member 84. This trimmed edge is often rough and burred with sharp sections. The workpiece edge 76 must be finished before the workpiece 78 can be considered complete. Typically, the rough edge is hand filed, a long and labor intensive task. The present invention reduces the time required, labor involved and provides a better, more uniform finished edge.
Further reference is now made to FIG. 5 illustrating the finishing bit 18 and comparing an unfinished contour 88 and a plurality of finished contours 90 on the workpiece edge 76. The plurality of finished contours are further identified on FIG. 5 with letters "A" through "F". It will be understood that the finishing bit 18 is infinitely adjustable and that only six contours have been illustrated for convenience and clarity.
The finishing bit 18 can be adjusted vertically along its rotational axis with respect to the workpiece 78. Vertical adjustment of the finishing bit 18 can be accomplished with the adjustment means as will now be described.
For the purpose of the description it will be presumed that the finishing bit 18 is in a position (not shown) that would provide finished contour "C" and it is desired to position the finishing bit 18 to provide one of the other finished contours "A", "B" or "D" through "F". It will be necessary to move air motor housing 20 telescopically with respect to the base member 46.
The first step requires loosening either the cam ring set screw 44, this is the set screw bearing against the air motor housing 20, or the base member set screw 52, this is the set screw bearing against a portion of the air motor housing 20 telescopically received within the base member 46. It is thought to be easier to loosen both set screws 44, 52 so that adjustment of the air motor housing 20 and the air motor 12 within the base member 46 can be accomplished using only telescoping movement. The extent of telescopic engagement between the air motor housing 20 and the base member 46 depends upon the portion of the cam surface 17 in contact with the pin 50.
Therefore, vertical adjustment of the finishing bit 18 is accomplished by changing the relationship between the cam surface 17 and the pin 50. This is accomplished by rotating the cam ring 16 about air motor housing 20.
Presuming that both set screws 44, 52 are loosened for purposes of illustration, rotation of the cam ring 16 to the left, with respect to the drawing FIG. 1, will telescope the air motor housing 20 out of the base member 46 as the cam surface 17 rides on the pin 50 forcing the cam ring 16 upward. The cam ring 16 pushes against the cam ring shoulder 38 thereby telescoping the air motor housing 20 out of the base member 46. In this manner the finishing bit 18 is raised to provide a shallower finished contour, for example, contour "A" or "B". This position of the finishing bit 18 may be more suitable for finishing a workpiece having relatively thinner laminate members.
Rotating the cam ring 16 to the right opens a gap between the cam surface 17 and the pin 50. The cam ring is rotated the desired amount and the air motor 12 is telescoped further into the cylindrical base member 46 until the pin 50 again contacts the cam surface 17. In this manner, the finishing bit 18 is lowered to povide a deeper finished contour, for example, contour "D", "E" "E" or "F". This position of the finishing bit 18 (the finishing bit is actually shown at contour "F" in FIG. 5) may be more suitable for finishing a workpiece having relatively thicker laminate members.
Once finishing bit 18 has been adjusted it is just a matter of placing tool 10 on the workpiece 78 as illustrated, for example, in FIG. 2, depressing the handle 30 against push button 26, and sliding the tool 10 along the edge 76 of the workpiece 78, to obtain the desired finished contour 90. The tool 10 operates properly when it is held against the workpiece 78 in a generally upright position. Tilting the tool 10 will separate the finishing bit 18 from the workpiece 78. When tilted the tool 10 pivots on either or both the horizontal guide member 58 or the vertical guide member 60, such that the finishing bit 18 is pulled or drawn away from the workpiece 78. Therefore, it is practically impossible to use the tool 10 improperly and gouge or dig into the workpiece 78 with the finishing bit 18.
In the preferred embodiment the dimensional relationship between the finishing bit 18 and the guide member 56 is critical. This is due in part to the lack of contact between the finishing bit 18 and the workpiece 78 except at the cutting edge 70. No end or bearing guide is required for the finishing bit 18 even though the finishing bit is not a spherical finishing bit.
In a preferred embodiment the following dimensions have been established. There is a dimension of 0.125" ("t")from the finishing bit end 71 to the start of the radius of the cutting edge 70. The thickness of the finishing bit end 71 is 0.125"+/-0.001" ("u") and the radius of the cutting edge 70 is 0.156" ("v"). The finishing bit body 68 has a diameter of 0.375" ("w") and the finishing bit 18 has a 0.250" ("x") diameter shank 67. The outside diameter of the cylindrical base member is 1.750" ("y") and the dimension from the outside edge of the cylindrical base member to the vertical surface of the shim 66 is 0.951"+/-0" ("z").
From the foregoing description these skilled in the art will appreciate that all of the aspects of the present invention are realized. The use of a pneumatic motor or air motor as a power means has eliminated the need for hand filing to finish a laminated workpiece. Eliminating hand filing reduces the amount of labor required in an otherwise very labor intensive task. The rotary finishing tool includes an adjustment means that utilizes a cam means for providing axial adjustment of the finishing bit to provide a rotary finishing tool that can be used on different thickness laminates. The adjustment means allows the rotary finishing tool to be used to finish either standard thickness laminate or non-standard or custom laminates. The rotary finishing tool provides a guide means having a guide member including shims made of a low friction material such as plastic that reduce friction between the guide member and the workpiece thereby reducing the effort required to operate the rotary finishing tool. The finishing bit is removable. A non-spherical finshing bit is used yet only the radius cutting edge contacts the workpiece.
One preferred embodiment of the rotary finishing tool 10 has been shown and described, however, it will be understood that many variations are possible. For example, the adjustment means might use a fastener arrangement other than set screws while still using the described cam ring and pin arrangement. The cross-sections of the base member and telescoping portion of the air motor housing do not have to be cylindrical. An electric or hydraulic motor may be used for the power means.
It will be further understood that the preferred embodiment of the rotary finishing tool has been described and illustrated herein and that the invention is not restricted to the illustrated adjusting means or air motor.
Other modifications may be made to the embodiment illustrated and described without departing from the spirit of the invention. It is not intended that the scope of this invention be limited to a particular embodiment. Rather, the scope of the invention is to be determined by the following claims and their equivalents. | A rotary finishing tool for finishing a laminated workpiece by removing rough, burred or sharp edges from the workpiece. The hand operated tool includes an air motor that moves in a telescopic fashion within a base member to provide for axial adjustment of a finishing bit in order to finish the edges of a laminated workpiece. The base member carries a guide member for properly locating the finishing bit with respect to an unfinished edge of the workpiece. The shape of the finishing bit allows axial, telescopic adjustment of the finishing bit. The finishing bit radius cutting edge is the only part of the finishing bit to contact the workpiece due in part to the close tolerances maintained when machining the finishing bit and manufacturing and assemblying the rotary finishing tool. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit under 35 U.S.C. §119(e) of U.S. Provisional Patent Application No. 60/658,481, filed on Mar. 4, 2005, entitled Encoding and Compressing the Access Point Database, which is herein incorporated by reference in its entirety.
[0002] This application is a continuation-in-part of and claims the benefit under 35 U.S.C. §120 of co-pending U.S. patent application Ser. No. 11/261,848, filed on Oct. 28, 2005, entitled Location Beacon Database, which is herein incorporated by reference in its entirety.
[0003] This application is related to the following U.S. patent applications, filed on Feb. 22, 2006:
[0004] U.S. patent application No. TBA, entitled Continuous Data Optimization of Moved Access Points in Positioning Systems;
[0005] U.S. patent application No. TBA, entitled Continuous Data Optimization by Filtering and Positioning Systems; and
[0006] U.S. patent application No. TBA, entitled Continuous Data Optimization of New Access Points in Positioning Systems.
[0007] This application is related to the following U.S. patent applications, filed on Oct. 28, 2005:
[0008] U.S. patent application Ser. No. 11/261,898, entitled Server for Updating Location Beacon Database;
[0009] U.S. patent application Ser. No. 11/261,987, entitled Method and System for Building a Location Beacon Database; and
[0010] U.S. patent application Ser. No. 11/261,988, entitled Location-Based Services that Choose Location Algorithms Based on Number of Detected Access Points Within Range of User Device.
BACKGROUND
[0011] 1. Field of the Invention
[0012] The invention generally relates to location-based services and, more specifically, to methods and systems of encoding and compression of a location beacon database.
[0013] 2. Discussion of Related Art
[0014] Internet applications and services have historically been designed around the assumption that the user is stationary or they ignore the concept of physical location altogether. But location is an integral contextual element to how information, entertainment and communication services are delivered. In recent years the number of mobile computing devices has increased dramatically creating the need for more advanced mobile and wireless services. Mobile email, walkie-talkie services, multi-player gaming and call following are examples of how new applications are emerging on mobile devices. In addition, users are beginning to demand/seek applications that not only utilize their current location but also share that location information with others. Parents wish to keep track of their children, supervisors need to track the location of the company's delivery vehicles, and a business traveler looks to find the nearest pharmacy to pick up a prescription. All of these examples require the individual to know their own current location or that of someone else. To date, we all rely on asking for directions, calling someone to ask their whereabouts or having workers check-in from time to time with their position.
[0015] Location-based services are an emerging area of mobile applications that leverages the ability of new devices to calculate their current geographic position and report that to a user or to a service. Some examples of these services include local weather, traffic updates, driving directions, child trackers, buddy finders and urban concierge services. These new location sensitive devices rely on a variety of technologies that all use the same general concept. Using radio signals coming from known reference points, these devices can mathematically calculate the user's position relative to these reference points. Each of these approaches has its strengths and weaknesses based on the radio technology and the positioning techniques they employ.
[0016] The Global Positioning System (GPS) operated by the US Government leverages dozens of orbiting satellites as reference points. These satellites broadcast radio signals that are picked up by GPS receivers. The receivers measure the time it took for that signal to reach to the receiver. After receiving signals from three or more GPS satellites the receiver can triangulate its position on the globe. For the system to work effectively, the radio signals must reach the received with little or no interference. Weather, buildings or structures and foliage can cause interference because the receivers require a clear line-of-sight to three or more satellites. Interference can also be caused by a phenomenon known as multi-path. The radio signals from the satellites bounce off physical structures causing multiple signals from the same satellite to reach a receiver at different times. Since the receiver's calculation is based on the time the signal took to reach the receiver, multi-path signals confuse the receiver and cause substantial errors.
[0017] Cell tower triangulation is another method used by wireless and cellular carriers to determine a user or device's location. The wireless network and the handheld device communicate with each other to share signal information that the network can use to calculate the location of the device. This approach was originally seen as a superior model to GPS since these signals do not require direct line of site and can penetrate buildings better. Unfortunately these approaches have proven to be suboptimal due to the heterogeneous nature of the cellular tower hardware along with the issues of multi-path signals and the lack of uniformity in the positioning of cellular towers.
[0018] Assisted GPS is a newer model that combines both GPS and cellular tower techniques to produce a more accurate and reliable location calculation for mobile users. In this model, the wireless network attempts to help GPS improve its signal reception by transmitting information about the clock offsets of the GPS satellites and the general location of the user based on the location of the connected cell tower. These techniques can help GPS receivers deal with weaker signals that one experiences indoors and helps the receiver obtain a ‘fix’ on the closest satellites quicker providing a faster “first reading”. These systems have been plagued by slow response times and poor accuracy—greater than 100 meters in downtown areas.
[0019] There have been some more recent alternative models developed to try and address the known issues with GPS, A-GPS and cell tower positioning. One of them, known as TV-GPS, utilizes signals from television broadcast towers. (See, e.g., Muthukrishnan, Maria Lijding, Paul Havinga, Towards Smart Surroundings: Enabling Techniques and Technologies for Localization, Lecture Notes in Computer Science, Volume 3479, January 2Hazas, M., Scott, J., Krumm, J.: Location-Aware Computing Comes of Age. IEEE Computer, 37(2):95-97, February 2004 005, Pa005, Pages 350-362.) The concept relies on the fact that most metropolitan areas have 3 or more TV broadcast towers. A proprietary hardware chip receives TV signals from these various towers and uses the known positions of these towers as reference points. The challenges facing this model are the cost of the new hardware receiver and the limitations of using such a small set of reference points. For example, if a user is outside the perimeter of towers, the system has a difficult time providing reasonable accuracy. The classic example is a user along the shoreline. Since there are no TV towers out in the ocean, there is no way to provide reference symmetry among the reference points resulting in a calculated positioning well inland of the user.
[0020] The rapid growth of 802.11 for wireless data networking has been widely documented. The majority of mobile devices, including laptop computers, now include 802.11 devices as a standard configuration. Handset manufacturers are also beginning to include 802.11 in their cellular phone devices. At the same time, consumers, businesses and public entities have deployed Wireless Local Area Networks using 802.11 in large numbers. By some estimates, over 10 million 802.11 “access points” have been deployed by the end of 2004. In metropolitan areas of the world, 802.11 radio signals propagate through almost every geographic area.
[0021] Microsoft Corporation and Intel Corporation (via a research group known as PlaceLab) have deployed a Wi-Fi Location system using the access point locations acquired from amateur scanners (known as “wardrivers”) who submit their Wi-Fi scan data to public community web sites. (See, e.g., LaMarca, A., et. al., Place Lab: Device Positioning Using Radio Beacons in the Wild.) Examples include WiGLE, Wi-FiMaps.com, Netstumbler.com and NodeDB. Both Microsoft and Intel have developed their own client software that utilizes this public wardriving data as reference locations. Because individuals voluntarily supply the data the systems suffer a number of performance and reliability problems. First, the data across the databases are not contemporaneous; some of the data is new while other portions are 3-4 years old. The age of the access point location is important since over time access points can be moved or taken offline. Second, the data is acquired using a variety of hardware and software configurations. Every 802.11 radio and antenna has different signal reception characteristics affecting the representation of the strength of the signal. Each scanning software implementation scans for Wi-Fi signals in different ways during different time intervals. Third, the user-supplied data suffers from arterial bias. Because the data is self-reported by individuals who are not following designed scanning routes, the data tends to aggregate around heavy traffic areas. Arterial bias causes a resulting location pull towards main arteries regardless of where the user is currently located causing substantial accuracy errors. Fourth, these databases include the calculated position of scanned access points rather than the raw scanning data obtained by the 802.11 hardware. Each of these databases calculates the access point location differently and each with a rudimentary weighted average formula. The result is that many access points are indicated as being located far from their actual locations including some access points being incorrectly indicated as if they were located in bodies of water.
[0022] There have been a number of commercial offerings of Wi-Fi location systems targeted at indoor positioning. (See, e.g., Kavitha Muthukrishnan, Maria Lijding, Paul Havinga, Towards Smart Surroundings: Enabling Techniques and Technologies for Localization, Lecture Notes in Computer Science, Volume 3479, January 2Hazas, M., Scott, J., Krumm, J.: Location-Aware Computing Comes of Age. IEEE Computer, 37(2):95-97, February 2004 005, Pa005, Pages 350-362.) These systems are designed to address asset and people tracking within a controlled environment like a corporate campus, a hospital facility or a shipping yard. The classic example is having a system that can monitor the exact location of the crash cart within the hospital so that when there is a cardiac arrest the hospital staff doesn't waste time locating the device. The accuracy requirements for these use cases are very demanding typically calling for 1-3 meter accuracy. These systems use a variety of techniques to fine tune their accuracy including conducting detailed site surveys of every square foot of the campus to measure radio signal propagation. They also require a constant network connection so that the access point and the client radio can exchange synchronization information similar to how A-GPS works. While these systems are becoming more reliable for these indoor use cases, they are ineffective in any wide-area deployment. It is impossible to conduct the kind of detailed site survey required across an entire city and there is no way to rely on a constant communication channel with 802.11 access points across an entire metropolitan area to the extent required by these systems. Most importantly, outdoor radio propagation is fundamentally different than indoor radio propagation rendering these indoor positioning techniques almost useless in a wide-area scenario.
[0023] There are numerous 802.11 location scanning clients available that record the presence of 802.11 signals along with a GPS location reading. These software applications are operated manually and produce a log file of the readings. Examples of these applications are Netstumber, Kismet and Wi-FiFoFum. Some hobbyists use these applications to mark the locations of 802.11 access point signals they detect and share them with each other. The management of this data and the sharing of the information is all done manually. These applications do not perform any calculation as to the physical location of the access point, they merely mark the location from which the access point was detected.
[0024] Performance and reliability of the underlying positioning system are the key drivers to the successful deployment of any location based service. Performance refers to the accuracy levels that the system achieves for that given use case. Reliability refers to the percentage of time that the desired performance levels are achieved.
Performance Reliability Local Search/Advertising <100 meters 85% of the time E911 <150 meters 95% of the time Turn-by-turn driving directions 10-20 meters 95% of the time Gaming <50 meters 90% of the time Friend finders <500 meters 80% of the time Fleet management <10 meters 95% of the time Indoor asset tracking <3 meters 95% of the time
SUMMARY
[0025] The invention provides a method for encoding and compression of a location beacon database.
[0026] Under one aspect of the invention, a location-based services system has a reference database of Wi-Fi access points in a target area. Each access point in the target area is identified by a corresponding fixed size MAC address, and each Wi-Fi access point is positioned at a corresponding geographical location. The MAC addresses and geographical locations of the access points are encoded to facilitate storage and/or transmission of the database contents to Wi-Fi enabled devices using the system. The encoding comprises the acts of: (a) storing as an entry of the database a reset address entry, said reset address entry including a fixed-size MAC address and marker information to indicate that the entry has a complete MAC address for a corresponding access point; (b) for each access point in at least a subset of access points in the target area, encoding a mathematical difference between (i) the MAC address of a corresponding access point and (ii) one of the other MAC addresses represented in the database, and storing said encoding, as delta information, in a corresponding delta address entry of the database, said delta address entry further including marker information to indicate that the entry has delta information from which a complete MAC address for a corresponding access point can be reconstituted; and (c) for each entry in the database, including information to represent the geographical location of the corresponding access point.
[0027] Under another aspect of the invention, multiple reset address entries are stored. Each reset address defining a boundary of a set of MAC addresses that are delta encoded.
[0028] Under another aspect of the invention, the delta information is encoded into a selected one of multiple delta address formats. Each delta format has a corresponding storage size different than the storage sizes of the other delta formats and different than the fixed size. Each delta format has an unique marker information to distinguish itself from the other delta formats.
[0029] Under another aspect of the invention, the information to represent geographical location includes cluster identification information to identify a cluster having a known corresponding longitude and latitude, and further includes a longitude offset value and latitude offset value. The longitude offset value encodes the distance from the access point longitude to the known longitude of the identified cluster. The latitude offset value represents the distance from the access point latitude to the identified cluster latitude.
[0030] Under another aspect of the invention, a location-based services system has a reference database of Wi-Fi access points in a target area. Each access point in the target area is identified by a corresponding fixed size MAC address, and each Wi-Fi access point is positioned at a corresponding geographical location. The MAC addresses and geographical locations of the access points are encoded to facilitate storage and/or transmission of the database contents to Wi-Fi enabled devices using the system. The encoding comprises the acts of: (a) storing cluster identification information to identify a cluster having a known corresponding longitude and latitude; (b) for each access point in at least a subset of access points in the target area, storing a longitude offset value and latitude offset value, the longitude offset value encoding the distance from the access point longitude to the known longitude of the identified cluster, and a latitude offset value to represent the distance from the access point latitude to the identified cluster latitude; and (c) for each entry in the database, including information to represent the MAC address of the corresponding access point.
[0031] Under another aspect of the invention, a Wi-Fi enabled device has first logic to determine the MAC addresses of Wi-Fi access points in the vicinity of the Wi-Fi enabled device by exchanging Wi-Fi messages with Wi-Fi access points in the vicinity of the Wi-Fi enabled device. The device has second logic to query a reference database of Wi-Fi access points. Using the MAC addresses determined by the first logic, the second logic retrieves from the database information representing at least the physical location for each MAC address-identified Wi-Fi access point in the database. The device has third logic, using the queried physical location information from the second logic, to calculate the position of the Wi-Fi enabled device. The reference database includes a reset entry having a complete MAC address for at least one Wi-Fi access point and includes a plurality of delta entries. Each delta entry has a mathematical encoding representing a difference between the MAC address of a corresponding Wi-Fi access point and another MAC address represented in the database. Each entry in the database further includes information representing the physical location of a corresponding Wi-Fi access point.
BRIEF DESCRIPTION OF DRAWINGS
[0032] In the drawings,
[0033] FIG. 1 depicts certain embodiments of a Wi-Fi positioning system;
[0034] FIG. 2 depicts a scheme for delta-encoding MAC addresses according to certain embodiments of the invention;
[0035] FIG. 3 depicts a relationship between an entry point table and a MAC address delta table according to certain embodiments of the invention; and
[0036] FIG. 4 depicts a relationship between a cluster reference location information record and an access point location record according to certain embodiments of the invention.
DETAILED DESCRIPTION
[0037] Embodiments of the present invention provide methods for encoding and compression of a location beacon database, such as a 802.11 Wi-Fi access point database, for use in a Wi-Fi Positioning System. The access point database may contain millions of access points with corresponding locations of the points. This presents a challenge for any device centric model where the database is wirelessly downloaded and kept locally on the mobile device. However, it is desirable to have an access point database on the mobile device. By leveraging the device centric model, users do not require a continuous network connection. Removing the network requirement allows the database to be usable in more application scenarios. Under certain embodiments, a data encoding and compression technique significantly reduces the data storage requirements for the access point database, making it easier to distribute the database or segments of the database to Wi-Fi enabled devices.
[0038] An uncompressed MAC address occupies 6 bytes. As explained in further detail below, access point locations having a resolution of 1 meter occupy 7 bytes. Thus, a single uncompressed data record having an access point MAC address and an associated location can occupy 13 bytes. The techniques of certain embodiments of the invention take advantage of delta encoding and data clustering to reduce a single access point record down to 7-8 bytes. This enables the database to occupy a smaller amount of memory on the mobile device and reduces the amount of bandwidth and time required to transfer the database or a portion thereof.
[0039] Embodiments of the present invention build on techniques, systems and methods disclosed in earlier filed applications, including but not limited to U.S. patent application Ser. No. 11/261,988, filed on Oct. 28, 2005, entitled Location-Based Services that Choose Location Algorithms Based on Number of Detected Access Points Within Range of User Device, the contents of which are hereby incorporated by reference in its entirety. Those applications taught specific ways to gather high quality location data for Wi-Fi access points so that such data may be used in location based services to determine the geographic position of a Wi-Fi-enabled device utilizing such services. In the present case, new techniques are disclosed for compressing and encoding the access point database. The present techniques, however, are not limited to systems and methods disclosed in the incorporated patent applications. Instead those applications disclose but one framework or context in which the present techniques may be implemented. Thus, while reference to such systems and applications may be helpful, it is not believed necessary to understand the present embodiments or inventions.
[0040] FIG. 1 depicts a portion of an embodiment of a Wi-Fi positioning system (WPS). The positioning system includes positioning software [ 103 ] that resides on a computing device [ 101 ]. Throughout a particular coverage area there are fixed wireless access points [ 102 ] that broadcast information using control/common channel broadcast signals. The client device monitors the broadcast signal or requests its transmission via a probe request. Each access point contains a unique hardware identifier known as a MAC address. The client positioning software receives signal beacons from the 802.11 access points in range and calculates the geographic location of the computing device using characteristics from the signal beacons. Those characteristics include the unique identifier of the 802.11 access point, known as the MAC address, and the strengths of the signal reaching the client device. The client software compares the observed 802.11 access points with those in its access point database [ 104 ], which may or may not reside on the device as well. If the access point database is located on the device, it may be in an encoded and compressed format. In such an embodiment, a decoding and decompression method may be used to read the access point database, as described in detail below. The access point database contains the calculated geographic locations or power profile of all the access points the gathering system has collected. The power profile is a collection of readings that represent the power of the signal from various locations. Using these known locations, the client software calculates the relative position of the user device [ 101 ] and determines its geographic coordinates in the form of latitude and longitude readings. Those readings are then fed to location-based applications such as friend finders, local search web sites, fleet management systems and E911 services.
Encoding and Compression Scheme for the Access Point Database
[0041] Under aspects of certain embodiments, a data encoding and compression technique significantly reduces the data storage requirements for the access point database, making it easier to efficiently distribute the database or segments of the database to mobile users and to store the database or database segments on a mobile device. As mentioned above and described in greater detail below, the technique takes advantage of delta encoding and data clustering to reduce a single access point record down to 7-8 bytes. This enables the database to occupy a smaller amount of memory on the mobile device and reduces the amount of bandwidth and time required to transfer the database or a portion thereof.
[0042] The database is used to look up access point data by MAC address. One data item is the access point's location (latitude and longitude), but other data items may be included. Under the general approach of the technique, a device looks up a MAC address in a compressed table. If the MAC address is present, the device returns access point data associated with the MAC address entry. This data may be, for example, the location of the access point assigned the MAC address, or this data may be a table index of the MAC address entry. In embodiments using a table index, the table index is used to retrieve the associated data (such as location) from another table. The implementation may cache the associated data results of some number of recently looked up MAC addresses, and return those immediately without having to re-access the database. The data encoding and compression approaches are summarized in the following sections.
[0043] Embodiments of the present invention may be implemented, for example, in software logic running on a computer or computing device platform. Likewise, embodiments may be implemented in hardware-encoded logic.
MAC Data Encoding and Compression
[0044] Access points are uniquely identified by a 48-bit MAC address (e.g. 00:0C:41:F3:CA:65). These addresses are assigned to each device at the time of manufacture, and are guaranteed unique. With a binary, uncompressed encoding, the MAC address can be stored in 6 bytes.
[0045] Under an embodiment of the invention, the MAC address table is significantly compressed with delta-encoding of MAC addresses. This is accomplished by sorting the MAC table, and storing only the differences between successive entries. If the differences (deltas) are small, they can be stored using less than 6 bytes. The scheme is summarized in FIG. 2 .
[0046] In the scheme depicted in FIG. 2 , the deltas are encoded into one, two or three bytes. Under certain embodiments, the most-significant (left-most) bits of the first byte indicate the length of the delta code. Using a Huffman-like coding method, a most-significant bit of 0 would indicate a delta coding length of one byte, with the remaining 7 bits used to encode the delta value of 1 to 128. If the most significant bits of the first byte are (1,0), the delta is encoded in 14 bits representing a value of 129 to 16512, using the remaining 6 bits in the first byte and 8 in the second byte. If the most significant bits of the first byte are (1,1,0), the delta value is encoded in 21 bits over three bytes for a delta range of 16513 to 2113664. If the delta will not fit in a three-byte value (i.e., the difference from the respective MAC address and immediately prior MAC address in the database is greater than 2113664), the delta is not encoded and the complete MAC address is coded (this is the fourth case [ 204 ] on the diagram) indicated by a most-significant bit pattern of (1,1,1). Such a MAC address is referred to as a “reset MAC address”. Thus, the bit patterns act as markers to indicate whether a complete MAC address or delta follows. Note that the delta of zero never has to be coded, since MAC addresses will not occur more than once in the table. With a 54 k entry test database, this approach compressed the MAC table to approximately 98 k bytes, or about 1.8 bytes per MAC address.
[0047] In the embodiments described above, the addition of new access points to the MAC address table requires resorting and recalculation of the deltas. In addition, this may result in generation of new and/or different reset MAC addresses.
[0048] The delta-encoding technique described above may also be accomplished relative to a reset MAC address rather than the preceding MAC address or MAC address delta. In such an embodiment, all MAC addresses following a reset MAC address are delta encoded by storing the difference between the MAC address being encoded and the nearest preceding reset MAC address. Thus, successive delta entries are not dependent on one another. In these embodiments, addition of new delta encoded access point MAC addresses does not require resorting and recalculation of all other delta entries in the delta table.
[0049] Under certain embodiments, MAC lookups are processed by scanning the table from the beginning. The scanning technique keeps a current MAC value, and iterates through the table decoding the deltas and adding them to the running MAC value. When a match is reached, the scanning stops and a table index (i.e., what location the MAC address occurred in the table) or the desired data is returned. Note that the scanning terminates with “not found” when a table MAC address is reached that is higher than the search MAC address (since the table is ordered).
[0050] While the above lookup technique is simple, a sequential scan of a large table (millions of MAC addresses) can take significant time. One optional optimization is to keep a side “entry point” table that contains the indexes of entries in the delta table where the full MAC address is coded (i.e., the reset MAC address). FIG. 3 graphically depicts the relationship between the entry point table and the delta table.
[0051] With this optimization, the lookup routine in certain embodiments can use the entry point table [ 301 ] to binary search the MAC addresses in the delta table [ 302 ]. When a delta table region is identified (i.e., the search MAC is located between two entry points), the region can be sequentially scanned. This approach speeds up the look up by a factor of N on average, where N is the number of reset MAC addresses in the entry point table. In the 54 k entry test MAC database, there were approximately 1,900 reset MAC address entry points.
[0052] Note that there is a pathological case where the MAC table is efficiently delta encoded and has few or no reset MAC address entries, or has large ranges that have no reset MAC address entries. These cases may be dealt with during table compression, by forcing the creation of a reset MAC address entry (even if not needed) if a large number of addresses have been compressed before a naturally occurring reset MAC address is encountered.
Latitude/Longitude Database Encoding and Compression
[0053] In some embodiments, an access point's location is represented by a latitude, longitude, and altitude (distance above sea level). At least one embodiment omits altitude by assuming the location is at or near ground level. The longitude defines an east/west location, and covers 360 degrees (−180 to 179). The latitude defines the north/south location, and covers 180 degrees (−90 to 89).
[0054] The representation of latitude and longitude depend on the required resolution. The circumference of the earth is approximately 40,000 km. The number of discrete longitude positions for a given resolution may be calculated by dividing 40,000 km by the resolution desired. The number of bits (based on a power of 2) required to represent the longitude may then be determined from the number of discrete longitudes. The table below shows the relationship between the desired resolution, number of discrete longitudes, and bits required to represent the longitude.
Resolution Discrete Longitudes Bits to Represent 1 m 40,000,000 26 3 m 13,333,333 24 10 m 4,000,000 22 30 m 1,333,333 21 100 m 400,000 19
[0055] Note that the representation of latitude (north/south) requires one less bit to represent, since the latitude only spans half of the earth circumference. Given this, the combined latitude and longitude resolution may be coded as found in the table below.
Resolution Bits (lat + Lon) Bytes 1 m 51 7 3 m 47 6 10 m 43 6 30 m 41 6 100 m 37 5
[0056] The location data is more difficult to compress, since it is not regularized or correlated. In order to further the compression ratio, at least one embodiment takes advantage of the clustering that happens around countries and population centers.
[0057] The generalized approach defines a cluster scheme, where each location is stored as a cluster ID, latitude offset, and longitude offset, rather than an absolute latitude and longitude value. The offsets define the location of the MAC addresses relative to a cluster reference location, for example, the center of the cluster. The offsets may be defined as distances from the location of a given access point to the reference location. A separate cluster table defines the cluster reference locations latitude and longitude values of each cluster. This cluster table may be downloaded to the mobile device for use in later decoding the location information.
[0058] FIG. 4 shows the relationship between the cluster reference location information [ 400 ] and the access point location information [ 407 ] for at least one embodiment. For example, the cluster reference location information [ 400 ] comprises a longitude [ 401 ] occupying 26 bits, at a 1 m resolution, and a latitude [ 402 ] occupying 25 bits, also at a 1 m resolution. A cluster ID [ 404 ], occupying a variable number of bits (shown as X), is associated with the longitude [ 401 ] and latitude [ 402 ] as shown by arrow [ 403 ].
[0059] The cluster ID [ 404 ] is also associated with the access point location information [ 407 ] for access points within the cluster. The access point information [ 407 ] also comprises a longitude offset [ 405 ], occupying a variable number of bits (shown as Y), and a latitude offset [ 406 ], occupying a variable number of bits (shown as Z). The clustering technique described above allows the cluster ID [ 404 ], longitude offset [ 405 ], and latitude offset [ 406 ] information to be stored in less than the total number of bits that would be required to store the access point location as an absolute longitude and latitude.
[0060] Thus, in order to retrieve the access point's location, the access point location information [ 407 ] is read. The cluster ID [ 404 ] is then used to retrieve the cluster reference location information [ 400 ] via the relationship [ 403 ]. The longitude offset [ 405 ] is applied to the longitude [ 401 ] to produce the longitude of the access point location. Similarly, the latitude offset [ 406 ] is applied to the latitude [ 402 ] to produce the latitude of the access point location.
[0061] For example, the continental US can be enclosed in a box about 5000 km by 3000 km. This can be encoded to 3 m resolution with 21 bits for the longitude, and 20 bits for the latitude, for a total of 41 bits—close to fitting in 5 bytes (vs. 6). One way to take advantage of this is to have two MAC/location databases: one for the US (using 5 bytes for the location), and one for the rest of the world. This technique could be used for other major population areas (e.g. Europe, Australia, etc.)
[0062] Certain embodiments may designate the clusters before the access point data are gathered. For example, the technique may select a particular geographic region as a cluster, for example a country, state, or city. Thus, all access points found within the geographic region would be assigned to the pre-determined cluster. In this embodiment, the technique then generates a cluster reference location, for example by calculating the center location of the cluster or the center location of all access points found within the geographic region.
[0063] Other embodiments may determine the clusters based on the data obtained. Under these embodiments, the technique reduces the size required to store the data by looking for “clumps” of access points near each other. Each clump may then be designated as a cluster, and a cluster reference location may be calculated as above. The ideal size and number of clusters may be determined by varying the size, number, and cluster reference locations of the clusters and comparing the data storage requirements for each combination.
[0064] The compression routines described above may occur in a regional data pack builder of a Wi-Fi location system and may be initiated on a periodic basis to build out data files for the entire database or sub-regions. The routines may be run in batch mode, and each region may be defined by entering boundary coordinates for each region. In certain embodiments, the compression routines will create a data file for each designated region. The resulting files may then be transferred to a data update portion of the location system's server so that remote clients (such as mobile devices) can connect to the server and download the latest compressed files for their region.
[0065] The client applications (such as mobile devices) may be configured to check the server on a periodic basis for new data files for their region. If the client locates a new data file, it downloads the new data file and replaces the older one.
[0066] Thus, under an embodiment of the invention, in order to return the location of a detected access point, the client application would first locate the block to search for the MAC address in the delta table given the entry point table. This returns the start offset and start index of the delta block in the delta table. The application then walks down the delta table (starting at the offset previously retrieved) until it finds the MAC address. Once found, a table index is retuned for the MAC address corresponding to the access point's entry in the coordinates table. The client application then extracts the latitude and longitude delta from the coordinates table. Finally, the client application calculates the latitude and longitude by applying the delta to the cluster reference location.
EXAMPLE OF INTENDED USE
[0067] A traveling salesman wants to find the nearest ATM machine so that he can pick up some money before heading to the airport. He pulls out of his pocket his Wi-Fi enabled Smartphone and runs his favorite mapping application. He selects “find nearest ATM” in the application. The mapping application makes a position request to the Wi-Fi Positioning System (WPS) component resident on the device. The WPS software begins scanning for nearby 802.11 access points and builds a list of them as the signals return.
[0068] The WPS then tries to compare those access point MAC addresses against those in the local database. The WPS uses the compression and encoding scheme to search the compressed data file resident on the device. For each observed access point it checks the data file for a location. Once it has the location for the observed access points found in the compressed data file, the WPS calculates the Smartphone's location and returns that latitude and longitude data back to the mapping application. The mapping application calculates the distance from the salesman's current location to the nearest ATM machine and provides simple directions for how to get there.
[0069] It will be appreciated that the scope of the present invention is not limited to the above described embodiments, but rather is defined by the appended claims, and these claims will encompass modifications of and improvements to what has been described. For example, although the reset MAC addresses may be created dynamically as described above, the reset MAC addresses may also be chosen before encoding the delta table. | A method of delta-encoding and compressing a table containing 6-byte MAC addresses is provided. The MAC addresses are sorted, a first MAC address is stored, and only the binary differences between succeeding MAC addresses are stored. A method of reading a delta-encoded and compressed MAC address table is provided. A first unencoded MAC address is read. The remaining MAC addresses are generated by successively adding stored binary differences to the result of the previous addition. A method of encoding and compressing a location table is provided. A reference latitude and longitude is selected and stored. The offsets from the reference latitude and longitude are stored for the remaining locations. A method of reading an encoded location table is provided. A stored reference latitude and longitude is read. Stored offsets are read and applied to the reference latitude and longitude to generate a set of latitude and longitude locations. | 7 |
RELATED APPLICATIONS
This is a continuation-in-part application of U.S. application, Ser. No. 971,629, filed Dec. 20, 1978, now abandoned, which is a continuation of U.S. application, Ser. No. 851,338, filed Nov. 14, 1977, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a device for housing a chip-carrying package and connecting the package to a PCB.
2. Prior Art
Representative prior art include U.S. Pat. Nos. 3,877,064 and 3,940,786, the latter being a CIP of the former. The teachings of both patents relate to surface to surface connectors for connecting leadless integrated circuit packages to a PCB. The connectors include a housing of insulating material having a central compartment. A number of contact-carrying conductive spring members are positioned about the perimeter of the compartment. A chip-carrying package is placed in the compartment with the contacts on the upper portion of the spring members contacting the electrically conductive pads on the package. The contacts on the lower portion of the spring members contact the traces on the PCB to complete the electrical path from the clip.
SUMMARY OF THE PRESENT INVENTION
Various electronic instruments, such as computers and the like, require structurally different devices for connecting semi-conductor chip packages to a PCB. In addition to the housing and package geometry, other characteristics which often require many days and months of experimental work include spring member force-deflection capability, contact reliability with respect to mechanical and thermal shock, vibration, corrosion, chip package cooling and inductance effects.
The present invention provides a housing of insulating material, a cover having integral biasing means, packaging centering means and S-shaped contact carrying spring members positioned in the housing around a package-receiving, central compartment.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the preferred embodiment of the present invention;
FIG. 2 is a cross-sectional view of the preferred embodiment taken along lines 2--2 of FIG. 1;
FIG. 3 is a view depicting one method of securing the spring members in the housing; and
FIG. 4 is a view depicting another method of securing the spring members in the housing.
DESCRIPTION OF THE INVENTION
Surface to surface connector 10, constructed in accordance with the present invention, is illustrated perspective in FIG. 1.
Its components or parts include the square frame 12, cover 14 and spring members 16.
Frame 12 consists of four side walls 18 integrally joined by corner posts 20 and a floor 22 which can be seen in FIG. 2. The walls and floor define a upwardly opened, package-receiving compartment 24.
The outside vertical surfaces of the side walls are characterized by a recess 26 extending across the upper portion and a plurality of vertically elongated cells 28 extending along the length of each wall between the corner posts. The cells extend downwardly from the recess through the base of each wall as shown clearly in FIG. 2. The vertical sections of the walls between the cells, hereinafter referred to as partitions 30, are notched near the lower ends. These notches, designated by reference numeral 32, receive inner and outer retaining members 34 and 36 respectively.
Top surface 38 of the side walls are flat.
The interior vertical surfaces of side walls 18 include a horizontal ledge 40 located just below the top surface. The ledge extends completely around the perimeter of compartment 24. A plurality of windows 42 are positioned through the ledge to give access to each cell 28. The wall below the ledge has a beveled portion 44 inbetween two vertical sections. The beveled portion represents increasing wall thickness while also providing greater cell depth.
The junction between walls 18 and floor 22 is represented by groove 46. This groove receives the downturned edges 48 of a metal plate 50. Plate 50 provides means for attaching connector 10 to PCB 52 by means of bolt 54 extending through the PCB and threadably received by the plate as shown in FIG. 1.
As chip orientation is a critical necessity and always difficult due to size, orientation features must be present. So that the connector may be properly orientated on the PCB, pegs of various geometric configurations are provided in the bases of corner posts 20. As seen in FIG. 1, one corner post has a cylindrical peg 56 and another corner post has a diamond-shaped peg 58. The three elements consisting of the two corner pegs and clamping screw serve to orient the connection on the P.C. board. In addition, alignment of the lower dimple 98, with respect to contact pad 112 of the P.C. board is critical. The requirement is met by having a round peg fit closely into a round hole which becomes the zero reference point for the pad. The diamond shaped pin engages another corresponding hole in the P.C. board. The large diameter of the diamond pin fits closely into the mating hole and rotational stability and alignment is achieved. The combination of a round peg and a diamond-shaped peg allows a reasonable tolerance or distance between pegs and between holes without loss of locational and alignment accuracy.
Orientation of the chip-carrying package 60 (partially shown in FIG. 2) in connector 10 is accomplished by providing protuberances 62 at three of the four interior corners. Three of the four edges (not shown) of the package have complementary recesses to receive the protuberances. The fourth interior corner of the package has a thruster clip 64 which cams package 60 against the other three corners so as to provide lateral restraint thereof. The biasing force of the thruster clip is a preloaded cantilever arm. Other conventional biasing means may also be used.
Two corner posts carry means to latch cover 14. These latches, indicated by reference numeral 66, are of resilient material and have a pair of ears 68 which provide downwardly facing shoulders 70. The ears are beveled so that the cover, in being closed over the frame 12, cams the latches out of the way. Once the cover is past, the latches rebound with the shoulders on top of the cover holding it in place.
The corner posts opposite the latches carry hinge means 72. These hinges have a U-shaped portion 74 with inwardly projecting ears 76 on the outside or free leg. The hinge loop 74 is designed to allow cover 14 to be pivoted until it is parallel to the substrate before spring fingers 84 contact package 60. The cover is thrust vertically downward until latches 66 are engaged simultaneously on all four corners. This procedure allows simultaneous loading of the four spring fingers 80 on package 60. Since package 60 is very often fabricated from ceramic, which is a brittle material and is relatively weak in tension and bending, it is important to avoid unequal loads.
Cover 14 has a central opening 78 and four hold down springs 80 symmetrically disposed about the opening. Each spring is L-shaped with the free end 82 having an upset portion as indicated by reference numeral 84.
A flap 86 depends from four sides of the cover acting as stiffeners. These flaps are received in recesses 26 when the cover is closed onto the frame.
Preferably the frame is molded from thermoplastic polyester, a plastic material marketed by General Electric Company under the tradename of Valor.
The cover 80 is made from high carbon steel, heat-treated to a spring temper.
Spring members 16 generally resemble a squarish letter "S". The upper portion 88 has a coined and dimpled area which provides the upper contact 90. The free end 92 is turned down and in to provide a smooth rubbing surface against the inner wall 94 of the cell.
The lower portion 96 carries the lower contact 98 formed by placing an outwardly projecting dimple in the horizontal section.
The free end of the lower portion is formed into a tail 100. The tail is L-shaped with a short vertical section 102 and a short horizontal section 104.
Preferably the spring members are stamped and formed from a coplanar strip of berylium copper alloy. They may be heat-treated and plated with gold over nickel, or tin-lead.
Retaining members 34 have a generally concave section 106 extending along the length thereof. The surface of the concave section has slots 108 spaced at intervals corresponding to cell intervals along the sides of the frame.
Retaining members 36 have a rounded edge 110. Retaining members 34 and 36 are assembled to a strip of spring members 16 equal to the number of cells 28 per side.
The spring members 16 are loaded into cells 28 so that the upper contacts 90 are pushing up through windows 42 and tails 100 pointing outwardly, as shown in FIG. 2. One or both retaining members may be fixed to the frame by an adhesive, ultrasonic welding or by an interference fit.
Connector 10 may be secured to a PCB via bolt 54. The lower contacts 98, which extend slightly below the base of the frame, engage circuit paths 112 on the board.
Upon placing package 60 in the frame, the circuit traces 114 thereon engage the spring members upper contacts 90. The encapsulated chip 116 extends down in the frame's compartment 24.
Contact pressure on the spring members is maintined by hold down springs 80 on cover 14. The central opening 78 in the cover provides access to the chip for cooling.
As FIG. 2 shows, a portion of tail 100 is testing probe accessible in that retaining number 34 is set back in notches 32.
With reference now to FIG. 4, another method to retain spring members 216 in the housing is shown. The method employs a one piece retaining member indicated generally by reference numeral 120. Each member or retaining means, is an elongated bar having a complex shape of steps, grooves, bevels and openings.
The very upper or top surface 122 has a series of grooves 124 cutting across the surface normal to the bar's long axis. The grooves receive the upper wall of notches 32.
The lower half of inwardly facing wall 130 has a series of niches 132 corresponding in number and spacing to the cells. Openings 134 extend from the rear wall of the niches to outwardly facing wall 136.
The outwardly facing wall, above the openings, is beveled inwardly as shown by reference numeral 138. A step 140 leads up to the upper or top surface 120. The base 142 of the bar is flat across.
As shown in FIG. 4, spring members 216 are loaded into retaining means 120 by inserting tails 100 through openings 134. The vertical sections 102 bears against the back wall of niches 132.
As will be noticed, spring member 16 shown in FIGS. 1 through 3 has been changed structurally to accommodate retaining means 120.
The changes include the direct attachment of tail 100 to the spring section which carries lower contact 98. This section is designated by reference numeral 144.
Upper portion 88 has been altered by increasing the contact from a dimple, reference numeral 90, to an elongated triangular shaped contact, indicated generally by reference numeral 146. Whereas this particular change does not relate to retaining means 120, the enlarged contact area facilitates manufacture.
The foregoing detailed description has been given for clearness of understanding only, and no unnecessary limitations should be understood therefrom, as some modifications will be obvious to those skilled in the art. | The present invention relates to a connector for connecting a semi-conductor chip carrier to a printed circuit board (PCB). More particularly, the invention comprises an insulating housing and a plurality of contact-bearing spring members positioned around the periphery of a central compartment in the housing. The spring member connects the leads on the chip package to traces on the PCB. | 7 |
BACKGROUND OF THE INVENTION
There are many instances in which it is required to apply a compression force across a large area. For example, it is often desired to produce such a force on a gate by drawing the bottom portion of the swinging or free side of the gate toward the top portion of the hinged side of the gate. When applied in this manner, the compressive force prevents the gate from sagging so that it will continue to close properly, etc.
Many devices have been proposed in the past to produce such a compressive force. In general, most of them comprise a cable, wire, or line of some sort which is fixed near one corner of the gate. There is also usually provided a device fixed to the gate at the diagonally opposite corner by means of which the cable can be tensioned, thereby causing a compression force to be exerted on the gate itself.
In most cases, the amount of force which can be exerted has been dependent upon the manner in which the cable is attached to the devices mounted on the gate. For example, if the end of the cable is merely threaded through one of the devices and then coiled around itself, any strong tensile force will normally overcome the strength of the coil and cause the cable to be loosened, thereby defeating the entire purpose of the device. On the other hand, some devices have employed clamps or crimped sleeves to hold the cable in place. While the use of crimped sleeves is quite satisfactory from the standpoint of strength and economy, it will quickly be realized that it is only possible to use such a structure at one end of the cable since the manufacturer cannot determine what length of cable will need to be employed by the consumer.
When a cable clamp is used so that the resultant strength is sufficient to produce the desired result, the product becomes heavier and more expensive due to the clamp's relatively high bulk and cost.
In addition, after a period of time, the cable may stretch and cause the gate to sag again, thereby necessitating disconnection of the clamping means which, at times, may be impossible.
In other words, the art has not previously presented a low cost, efficient, lightweight structure which will produce a compressive force on a large area, such as a gate, and have sufficient strength to accomplish the task under all conditions.
SUMMARY OF THE INVENTION
The present invention relates to such a device in which a cable or wire may be clamped to itself by a crimped tube or similar device on one end and locked in an adjustable position at the opposite end by means of friction which the cable will exert against itself.
In the preferred embodiment, the locking device comprises a very simple, lightweight, and inexpensive plate having a plurality of eyelets formed therein through which the cable can be threaded. Suitable location of the eyelets and proper threading of the cable will cause the cable to overlap or adjoin itself so that the tension exerted on the cable, to cause the compressive force in the object or gate being maintained, will create sufficient friction between the adjoined sections of the cable to hold it in place. Additionally, if the eyelets are formed so as to be just slightly larger than the diameter of the cable, the cable will grip the edges of the eyelets in a manner which also prevents the cable from slipping out of the plate. If the apertures or eyelets are positioned along a generally straight line and the cable is threaded, first, through the first and last eyelets, the natural tendency of a wire to extend in a straight line will cause it to push the portions of the wire in intermediate eyelets in directions substantially perpendicular to the general line of extension of the wire. This pushes the wire portions in the intermediate eyelets tightly against their respective aperture edges, thus causing the wire to frictionally engage itself, as well as to have the aperture edges "bite" into the wire.
Thus, a very inexpensive, lightweight, pre-drilled plate may be employed to adjust the length of the cable to as short a dimension as possible prior to the time that tension is applied to the cable by a suitable means such as a turnbuckle. In other words, rather than employing a stronger, heavier, and more expensive apparatus, such as a bigger clamp, as might be obvious when structural strength is to be increased, the present invention moves in exactly the opposite direction and employs a small device which causes the cable itself to do all of the clamping work.
Also, in employing the preferred embodiment of this invention, it may be desirable to provide elements which provide a suitable structure for holding the cable, turnbuckle, etc., away from the gate itself in order to prevent interference therewith. Accordingly, in some applications, corner clamps, which can be suitably fastened to gate cross supports such as two by fours, may be provided with raised sections thereon for receipt of the cable and/or a hook from a turnbuckle.
This expedient allows an individual homeowner to install the compression device very quickly and easily. It also prevents an inadvertent jam-up of the parts against the gate which might release at a later time, possibly undoing the installation entirely and at least reducing the tension exerted through the cable.
The invention, together with its objects, advantages, alternative modes, embodiments, etc., will be readily understood by those skilled in the art upon reviewing the following detailed description, taken together with the accompanying drawing which illustrates what is presently considered to be the preferred embodiment of the best mode contemplated for utilizing the invention which is defined in the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 comprises an elevation of a gate structure employing an apparatus in accordance with the present invention to produce a compressive force in the gate and thereby prevent it from sagging;
FIG. 2 comprises a side elevation of a portion of the structure shown in FIG. 1, as seen along the line II--II thereof, but with the tensioning device 21 reversed 180°, as though being seen from the opposite side;
FIG. 3 comprises a side view of an end clamp which may be utilized to fasten a device formed in accordance with the present invention to a gate or other structure; and
FIGS. 4 and 5 comprise isometric illustrations of two different locking devices which may be employed to utilize the present invention.
DETAILED DESCRIPTION
As shown in FIG. 1, a device formed in accordance with the present invention can be utilized to provide a compressive force on any planar structure, such as a gate 11 having two strengthening cross members 13 and 15. As shown, the device employed may, in the preferred embodiment illustrated, comprise a pair of clamps 17 and 19 which are interconnected by a tensioning device 21 to draw the clamps toward one another. If desired, each clamp may be suitably fastened to the edges of its related cross member by any suitable means such as nails, screws, etc., which may pass through apertures 23 therein. Each of the clamps may be provided with a raised central portion or element 25 having an aperture 27 therein.
As shown in FIGS. 1 and 2, the hook 31 of a turnbuckle 33 may be installed through the aperture 27 of bracket 17. The raised central portion 25 of the bracket allows the hook to be quickly and easily passed through the aperture 27 in such a manner that it will not bind against the support member 13. Such binding could cause, in some cases, the tensioning device to be released or lose some of its tension if the hook became jarred by vibration of the gate closing over a period of time.
It will be noted that in the depiction of FIG. 1, the righthand side of the gate is the hinged side thereof and the lefthand side is the free side thereof. Thus, the tension device 21 is employed to pull or compress the lower, free side of the gate toward the upper, hinged side thereof. Realizing that this device can be employed on any large planar surface, it may commonly be employed on a gate so as to prevent the free side of the gate from sagging and/or binding against its latch post to hinder opening or closing of the gate.
Through the aperture 27 in the bracket 19, a cable, wire, cord, or similar element 41 may be passed and brought through a 180° bend so as to adjoin itself within a sleeve 43. The sleeve may then be crimped in any suitable manner to prevent relative movement between the adjoined portions of the cable 41.
In order to facilitate the ability of the average homeowner or gate construction worker to install a device formed in accordance with the present invention, there may be provided a rather simple lightweight, plate-like element 51, having eyelets 53, through which the free end of cable 41 may be threaded. This device allows the cable to be gripped by the free end of the turnbuckle 33, while preventing release of tension in the cable.
A comparison of FIGS. 1 and 4 will reveal that the element 41 may be threaded through the apertures or eyelets 53 in the plate 51 in such a manner that the cable may be gripped by the edges of the eyelets 53 to prevent relative movement. This feature may be facilitated if the eyelets are provided to be only slightly larger in diameter than the cable.
With particular reference to FIG. 4, it can be seen that cable 41 may be threaded in a first direction through a first aperture 53 and in an opposite, second direction in a fourth or last aperture 53. An end loop may then be formed in the cable which may be passed through the eye bolt of turn buckle 33 as shown in FIG. 1. Then, the cable may be brought back and threaded through an intermediate aperture 53 in the first direction and another intermediate aperture 53 in the second or opposite direction. Due to the natural tendency of a wire to extend in a straight line when it is under tension, if the apertures 53 are located in a generally straight line, that portion of the wire between the first and last apertures 53 will tend to push the portions of the wire threaded through one or more intermediate apertures out of the way.
Thus, the portion of the wire or cable extending between the end apertures will tightly engage that portion of the wire threaded through any intermediate apertures in frictional contact and will push the latter portions of the wire against the edges of the second and third apertures 53 to cause the aperture edges to "bite" into the wire and aid in holding it in place. This relationship is shown in FIG. 1; it will be realized by those skilled in the art that the biasing force exerted by the portion of the wire extending between the end apertures is substantially perpendicular to a straight line passing through the apertures. In other words, the biasing force is substantially perpendicular to the general direction of extension of the wire 41.
In any event, it is preferred that the eyelets 53 be provided in a suitable relationship so that threading of the cable through the eyelets will cause the various portions of the cable to be adjoined or overlapped. The friction which results from such adjoining will further prevent the cable from slipping out of the plate.
In use, a person installing the tensioning device 21 can mount the clamps 17 and 19 in the manner illustrated and then install the hook 31 of turnbuckle 33 in the clamp 17. Preferably the cable will have been threaded through the aperture 27 in clamp 19 and crimped within the sleeve 43 during the manufacture thereof. If this has been accomplished, the installer may then thread the cable 41 through the eyelets of plate 51 in the manner illustrated in FIG. 4, leaving a sufficient loop for attachment to the free end of the turnbuckle. Of course, the installer must leave as little slack as possible in the cable 41 when he has completed this step in order to achieve his desired result. Then, when he turns the body of the turnbuckle 33, he will be able to draw sufficient tension in the cable 41 to takeup and/or prevent sagging of the gate 11. When this has been accomplished, the installer can then cut the free end of the cable 41 close to the plate 51.
A careful study of FIG. 4 shows that the particular location of the eyelets in the plate is not critical, so long as there is sufficient or overlapping of the sections of the cable to create friction sufficient to prevent slipping of the cable. Of course, as set forth previously, if the apertures 53 are aligned along a generally straight line, the tendency of the wire 41 to straighten itself under tension will increase the force tending to fix the wire against movement relative to the plate 51.
An alternate plate embodiment can be seen from FIG. 5, wherein like elements have been provided with substantially the same identification numerals, followed by the letter "a". The eyelets 53a define a polygonal configuration in this embodiment which causes the cable to be adjoined in overlapping relationship. Those skilled in the art will thus realize that a wide variety of eyelet locations may be employed. In any event, the eyelets are preferably located to create sufficient friction between the adjoined portions of the cable so that the cable cannot slip.
Those skilled in the art will now realize that the present invention may be employed in a very simple, low cost device and that a wide variety of embodiments may be used within the scope of the invention of the following claims, many of which may not even physically resemble those embodiments illustrated and described here. | The illustrated embodiment discloses a compressive force application device, which might be used on a gate to prevent sagging thereof, including a plate having eyelets therein through which the tensioning cord or cable may be threaded so that it adjoins itself; thus, the threaded relationship is maintained by the cable's frictional contact with itself. | 5 |
This application claims priority on provisional application Serial No. 60/074,336 filed on Feb. 6, 1998, the entire contents of which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a pump enable system and method; and more particularly, a pump enable system and method for variable-displacement piston pumps.
2. Description of Related Art
FIG. 1 schematically illustrates a well-known variable-displacement piston pump 10 such as Vickers Incorporated's Model No. PVE19R930CVPC. The piston pump 10 includes a pump 12 having a plurality of pistons (not shown). The pump 12 is connected between a suction line 14 and a pressure line 16 , and is driven by an engine 18 . Oil leaking in the pump 12 is drained via a drain line 20 .
As is well-known, a swash plate 22 (also known as a wobble plate), connected to the pistons in the pump 12 , controls the displacement of the pistons; and thus, the flow rate of the pump 12 . More specifically, the position of the swash plate 22 determines the displacement of the pistons in the pump 12 . A servo piston 24 controls the movement of the swash plate 22 based on hydraulic pressure (i.e., fluid) supplied thereto.
As shown in FIG. 1, a pressure compensation valve 26 and a flow compensation valve 28 cooperatively regulate the supply of hydraulic pressure generated by the pump 12 to the servo piston 24 based on the hydraulic pressure in a load sense line 30 . The load sense line 30 , for instance, is connected to a directional control valve (not shown), which when placed in a state requiring hydraulic pressure supplies hydraulic pressure to the load sense line 30 . Both the pressure and flow compensation valves 26 and 28 are two-state valves.
When a load is placed on the pump 12 , the pressure compensation valve 26 and the flow compensation valve 28 are both placed in a first state as shown in FIG. 1 . In this first state, the hydraulic pressure generated by the pump 12 is not supplied to the servo piston 24 , and the servo piston 24 is connected with the drain line 20 to remove hydraulic pressure therefrom. As a result, the servo piston 24 retracts and the swash plate 22 moves to an inclined position, which increases the displacement of the pistons in the pump 12 and increases the flow rate of the pump 12 .
When no load is placed on the pump 12 , the pressure compensation valve 26 and the flow compensation valve 28 both attain a second state. While not shown as being in the second state, FIG. 1 does illustrate the second states of the pressure and flow compensation valves 26 and 28 . In this second state, the hydraulic pressure generated by the pump 12 is supplied to the servo piston 24 . As a result, the servo piston 24 extends and moves the swash plate 22 to a more vertical position, which reduces the piston displacement in the pump 12 and decreases the flow rate of the piston pump 12 . When fully stroked, the servo piston 24 moves the swash plate 22 to a position which reduces the hydraulic pressure generated by the pump 12 to a stand-by pressure.
Whether the pressure and flow compensation valves 26 and 28 are placed in the first or second state depends on the hydraulic pressure in the load sense line 30 and the pressure line 16 . Namely, the hydraulic pressure generated by pump 12 is supplied to first control inputs 40 and 44 of the pressure compensation valve 26 and the flow compensation valve 28 , respectively, and the hydraulic pressure in the load sense line 30 is supplied to a second control input 42 of the pressure compensation valve 26 . First and second springs 45 and 46 bias the pressure and flow compensation valves 26 and 28 , respectively, to the right in FIG. 1 .
When no load is placed on the load sense line 30 , the hydraulic pressure generated by the pump 12 causes the pressure and flow compensation valves 26 and 28 to move to the left in FIG. 1 (i.e., the second state). However, when a load is placed on the load sense line 30 , the hydraulic pressure applied to the second control input 42 of the pressure compensation valve 26 causes the pressure compensation valve 26 to move to the right (i.e., the first state). As a result, the hydraulic pressure applied to the first control input 44 of the flow compensation valve 28 is exhausted to the drain line 20 via the pressure compensation valve 26 , and the flow compensation valve 28 moves to the right (i.e., the first state).
The hydraulic pressure generated by the pump 12 and supplied via the pressure line 16 typically powers hydraulically operated machinery. As discussed above, the variable-displacement piston pumps 10 can be connected to a directional control valve. The directional control valve applies hydraulic pressure to the load sense line 30 depending on the need for hydraulic pressure from the variable-displacement piston pump 10 . Unfortunately, if the directional control valve sticks in an open state for operating machinery connected thereto when an operator wants the directional control valve closed, the variable-displacement piston pump 10 continues to supply hydraulic pressure.
As such, it is desirable, such as in emergency conditions, to immediately stop operation of that machinery. Often this is accomplished by removing the supply of hydraulic pressure necessary to operate the machinery. FIG. 1 illustrates a conventional dump system for removing the supply of hydraulic pressure.
As shown in FIG. 1, a dump valve 32 is connected between the pressure line 16 and a reservoir 34 . In a closed state, the dump valve 32 prevents hydraulic pressure from flowing to the reservoir 34 from the pressure line 16 . However, in an open state, as shown in FIG. 1, the dump valve 32 permits hydraulic pressure to flow to the reservoir 34 , which substantially eliminates hydraulic pressure in the pressure line 16 . By placing the dump valve 32 in the open state, operation of machinery utilizing the hydraulic pressure in the pressure line 16 can be brought to a halt.
FIG. 2 schematically illustrates another well-known variable-displacement piston pump 110 such as Parker Hannifin Corporations Model No. PAVC65X29948. The piston pump 110 includes a pump 112 having a plurality of pistons (not shown). The pump 112 is connected between a suction line 114 and a pressure line 116 , and is driven by an engine 118 . Oil leaking in the pump 112 is drained via a drain line 120 .
As is well-known, a swash plate 122 , connected to the pistons in the pump 112 , controls the displacement of the pistons; and thus, the flow rate of the pump 112 . More specifically, the position of the swash plate 122 determines the displacement of the pistons in the pump 112 . A servo piston 124 controls the movement of the swash plate 122 based on hydraulic pressure (i.e., fluid) supplied thereto.
As shown in FIG. 2, a differential adjustment valve 126 regulates the supply of hydraulic pressure generated by the pump 112 to the servo piston 124 based on the hydraulic pressure in a load sense line 130 . The load sense line 130 , for instance, is connected to a directional control valve (not shown), which when placed in a state requiring hydraulic pressure supplies hydraulic pressure to the load sense line 130 .
The differential adjustment valve 126 is a two-state valve. When no load is placed on the pump 110 , the differential adjustment valve 126 is placed in a first state. While FIG. 2 does not illustrate the differential adjustment valve 126 in the first state, FIG. 2 does illustrate the first state. Specifically, because no hydraulic pressure is supplied to the control input 140 of the differential adjustment valve 126 by the load sense line 130 , a spring 142 biases the differential adjustment valve 126 down in FIG. 2 (i.e., biases the differential adjustment valve 126 towards the first state). This connects the servo piston 124 to the drain line 120 , and hydraulic pressure at the servo piston 124 exhausts via the drain line 120 . As a result, the servo piston 124 retracts and moves the swash plate 122 to a more vertical position, which reduces the piston displacement in the pump 112 and decreases the flow rate of the pump 112 . When fully retracted, the servo piston 124 moves the swash plate 122 to a position which reduces the hydraulic pressure generated by the pump 112 to a stand-by pressure.
When a load is placed on the pump 110 , the differential adjustment valve 126 is placed in a second state as shown in FIG. 2 . Namely, when a load is placed on the pump 110 , hydraulic pressure is applied to the control input 142 of the differential adjustment valve 126 by the load sense line 130 . This hydraulic pressure causes the differential adjustment valve 126 to move up in FIG. 2 (i.e., move towards the second state). In this second state, the pressure line 116 is connected to the servo piston 124 , and hydraulic pressure is supplied to the servo piston 124 . As a result, the servo piston 124 extends and the swash plate 122 moves to an inclined position, which increases the displacement of the pistons in the pump 112 and increases the flow rate of the pump 112 .
The hydraulic pressure generated by the pump 112 and supplied via the pressure line 116 typically powers hydraulically operated machinery in the same manner discussed above with respect to the variable-displacement piston pump 10 of FIG. 1 . As such it is desirable, such as in emergency conditions, to immediately stop operation of that machinery
As shown in FIG. 2, a dump valve 132 is connected between the pressure line 116 and a reservoir 134 . In a closed state, the dump valve 132 prevents hydraulic pressure from flowing to the reservoir 134 from the pressure line 116 . However, in an open state, as shown in FIG. 2, the dump valve 132 permits hydraulic pressure to flow to the reservoir 134 , which substantially eliminates hydraulic pressure in the pressure line 116 . By placing the dump valve 132 in the open state, operation of machinery utilizing the hydraulic pressure in the pressure line 116 can be brought to a halt.
In the dump systems of FIGS. 1 and 2, the immediate elimination of hydraulic pressure in the pressure line 116 causes a significant shock or jolt. Furthermore, this immediate elimination of hydraulic pressure defeats the benefits provided by systems incorporating a ramp down feature. Systems incorporating a ramp down feature include hydraulic elements which gradually reduce their demand for hydraulic pressure such that the hydraulic pressure supplied by the variable-displacement piston pump 10 or 110 , in response to this demand, gradually decreases. Consequently, machinery operating based on the hydraulic pressure supplied by the variable-displacement piston pump 10 or 110 gradually comes to a halt.
SUMMARY OF THE INVENTION
The pump enable system according to the present invention comprises: a variable-displacement piston pump having a displacement control device, said displacement control device controlling displacement of pistons in said pump based on a position thereof, and position control system for controlling a position of said displacement control device based on a load on said pump; and an over-ride system for selectively over-riding said position control system such that said displacement control device assumes a position which reduces displacement of said pistons in said pump.
The method of enabling a variable-displacement piston pump according to the present invention, in which said pump includes a displacement control device controlling displacement of pistons in said pump based on a position thereof and position control system for controlling a position of said displacement control device based on a load on said pump, comprises: selectively over-riding said position control system such that said displacement control device assumes a position which reduces displacement of said pistons in said pump.
By controlling the displacement control device, as opposed to exhausting hydraulic pressure supplied by the pump, the pump enable system and method according to the present invention significantly reduces the pressure supplied by the variable-displacement pump without causing a shock or jolt.
In at least one embodiment of the pump enable system and method according to the present invention, over-riding the position control system is delayed to prevent defeating the ramp down feature.
Other objects, features, and characteristics of the present invention; methods, operation, and functions of the related elements of the structure; combination of parts; and economies of manufacture will become apparent from the following detailed description of the preferred embodiments and accompanying drawings, all of which form a part of this specification, wherein like reference numerals designate corresponding parts in the various figures.
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 schematically illustrates a prior art variable-displacement piston pump with a dump system;
FIG. 2 schematically illustrates another prior art variable-displacement piston pump with a dump system;
FIG. 3 schematically illustrates a first embodiment of the pump enable system according to the present invention in a first state;
FIG. 4 schematically illustrates a first embodiment of the pump enable system according to the present invention in a second state;
FIG. 5 schematically illustrates a second embodiment of the pump enables system according to the present invention in a first state;
FIG. 6 schematically illustrates a second embodiment of the pump enable system according to the present invention in a second state; and
FIG. 7 illustrates a control circuit for the solenoid valve in the pump enable system according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 3 schematically illustrates a first embodiment of the pump enable system according to the present invention in a first state. As shown in FIG. 3, the pump enable system according to the first embodiment includes the variable-displacement piston pump 10 discussed in detail above with respect to FIG. 1 . Accordingly, the description of this variable-displacement piston pump will not be repeated.
As further shown in FIG. 3, the housing 50 of the variable-displacement piston pump 10 has been modified to include a solenoid valve 52 . The solenoid valve 52 is connected between the first control input 40 of the pressure compensation valve 26 and the servo piston 24 . The solenoid valve 52 has a closed state which prevents hydraulic pressure from flowing to the servo piston 24 from the first control input 40 , and an open state which allows hydraulic pressure to flow from the first control input 40 to the servo piston 24 . The solenoid valve 52 assumes either the open or closed state based on a received control signal.
When the solenoid valve 52 is placed in the closed state as shown in FIG. 3, the variable-displacement piston pump 10 operates in the conventional manner. When, however, the solenoid valve 52 is placed in the open state as shown in FIG. 4, the hydraulic pressure at the first control input 40 of the pressure compensation valve 26 (i.e., the hydraulic pressure generated by the pump 12 ) flows to the servo piston 24 via the solenoid valve 52 .
Even if the servo piston 24 is connected with the drain line 20 via the pressure and flow compensation valves 26 and 28 as shown in FIG. 2, this connection to the drain line 20 can not sufficiently exhaust the hydraulic pressure being supplied via the solenoid valve 52 to prevent the servo piston 24 from extending. As a result, the servo piston 52 extends and the swash plate 22 moves and reduces the displacement of the pistons in the pump 12 . This causes a reduction in the flow rate of the pump 12 . Specifically, the swash plate 22 reduces the displacement of the pistons in the pump 12 such that the pump 12 can not generate hydraulic pressure above 150 PSI. Hydraulic pressure below 150 PSI is insufficient to operate machinery, but the shock or jolt experienced in prior art pump enable systems is substantially eliminated.
Furthermore, when de-energized, the solenoid valve 52 is in the open state. Unless the solenoid valve 52 is energized, the variable-displacement piston pump 10 does not generate a hydraulic pressure above 150 PSI. Accordingly, even if, for example, the directional control valve to which the variable-displacement piston pump 10 is connected sticks in the open state, undesired operation of machinery does not occur.
As an alternative embodiment, the solenoid valve 52 is connected externally to the variable-displacement piston pump 10 .
FIG. 5 schematically illustrates another embodiment of the pump enable system according to the present invention in a first state. As shown in FIG. 5, the pump enable system according to this embodiment includes the variable-displacement piston pump 110 discussed in detail above with respect to FIG. 2 . Accordingly, the description of this variable-displacement piston pump 110 will not be repeated.
As further shown in FIG. 5, a solenoid valve 152 , external to the housing 150 of the variable-displacement piston pump 110 , is connected to the variable-displacement piston pump 110 . Specifically, the solenoid valve 152 is connected between the servo piston 124 and the drain line 120 . The solenoid valve 152 has a closed state which prevents hydraulic pressure from flowing to the drain line 120 from the servo piston 124 , and an open state which allows hydraulic pressure to flow from the servo piston 124 to the drain line 120 . The solenoid valve 152 assumes either the open or closed state based on a received control signal.
When the solenoid valve 152 is placed in the closed state as shown in FIG. 5, the variable-displacement piston pump 110 operates in the conventional manner. When, however, the solenoid valve 152 is placed in the open state as shown in FIG. 6, the hydraulic pressure at the servo piston 124 flows to the drain line 120 via the solenoid valve 152 .
The hydraulic pressure at the servo piston 124 exhausts to the drain line 120 via the solenoid valve 152 regardless of the state of the differential adjustment valve 126 . For instance, as shown in FIG. 6, even if the differential adjustment valve 126 is in the second state for supplying hydraulic pressure to the servo piston 124 , when the solenoid valve 152 is in the open state, hydraulic pressure exhausts from the servo piston 124 to the drain line 120 .
As a result, the servo piston 124 retracts and the swash plate 122 moves to reduce the displacement of the pistons in the pump 112 . This causes a reduction in the flow rate of the pump 112 . Specifically, the swash plate 122 reduces the displacement of the pistons in the pump 112 such that the pump 112 can not generate hydraulic pressure above 150 PSI. Hydraulic pressure below 150 PSI is insufficient to operate machinery, but the shock or jolt experienced in prior art pump enable systems is substantially eliminated.
Furthermore, when de-energized, the solenoid valve 152 is in the open state. Unless the solenoid valve 152 is energized, the variable-displacement piston pump 110 does not generate a hydraulic pressure above 150 PSI. Accordingly, even if, for example, the directional control valve to which the variable-displacement piston pump 110 is connected sticks in the open state, undesired operation of machinery does not occur.
As an alternative embodiment, the housing 150 of the variable-displacement piston pump 110 is modified to include the solenoid valve 152 .
FIG. 7 illustrates a control circuit for the solenoid valve 52 or 152 in the pump enable system according to the present invention. As shown, a motion signal from a function controller or switch is supplied to both a motion alarm 200 and delay timer 202 . The delay timer 202 also receives a 12 volt power supply, and outputs the control signal to the solenoid valve 52 or 152 .
The delay timer 202 includes an internal timer circuit 204 and a switching relay 206 . The switching relay 206 includes a coil 208 and a switch 210 . The coil 208 receives an output signal from the internal timer circuit 204 . The switch 210 is connected between the 12 volt power supply and the solenoid valve 52 or 152 . When the coil 208 is de-energized, the switch 210 is open, and when the coil 208 is energized, the switch 210 closes and provides a control signal to energize the solenoid valve 52 or 152 .
When the motion alarm 200 receives a motion signal, the motion alarm 200 outputs an alarm. When the internal timer circuit 204 receives the motion signal, the internal timer circuit 204 counts to a predetermined period of time, and then energizes the coil 208 . Accordingly, the switch 210 closes and energizes the solenoid valve 52 or 152 .
When the motion signal is discontinued, the motion alarm 200 stops issuing the alarm and the internal timer circuit 204 de-energizes the coil 208 a predetermined period of time after the motion signal is discontinued. Once the coil is de-energized, the switch 210 opens and the solenoid valve 52 or 152 is de-energized.
Because of the delay timer 202 , the solenoid valve 52 or 152 is energized or de-energized a predetermined period of time after the motion signal is issued or discontinued. This delay allows systems incorporating a ramp down feature and the pump enable system according to the present invention to enjoy the features of the ramp down system. Namely, the ramp down begins when the motion signal is discontinued, but the solenoid valve 52 or 152 is not de-energized until a predetermined period of time thereafter. Consequently, machinery operating based on the hydraulic pressure supplied by the variable-displacement piston pump 10 or 110 gradually comes to a halt.
The invention being thus described, it will be obvious that the same may be varied in many ways. 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 intended to be included within the scope of the following claims. | A pump enable system includes a variable-displacement piston pump having a displacement control device. The displacement control device controls displacement of pistons in the pump based on a position thereof, and a position control system in the pump controls a position of the displacement control device based on a load on the pump. An over-ride system selectively over-rides the position control system such that the displacement control device assumes a position which reduces displacement of the pistons in the pump. | 5 |
BACKGROUND AND SUMMARY OF THE INVENTION
The present invention relates to molding. More particularly, the invention relates to molding or fascia trim, especially for automotive vehicles, having an insert with markings or indicia thereon and exhibiting three-dimensional characteristics.
Moldings for automotive vehicles are commonly used, for example, as body side moldings to protect the sides of vehicles from nicks, scratches and dents, of the type inflicted in parking lots by the careless. Moldings are also used as fascia trim and can serve aesthetic purposes to enhance the lines of vehicles. Some vehicle manufacturers provide moldings with bright work to simulate a bright metallic appearance which is pleasing to the eye. In fact, a variety of shapes and configurations of moldings have been developed through the years in efforts to improve the aesthetic characteristics of the molding and to improve the aesthetic appeal of the vehicle to which the moldings are attached.
It is also quite popular to provide the sides of vehicles with some form of emblem or indicia, such as a trademark, tradename, insignia, logo, design or the like. Conventionally, such emblems are secured to vehicles by pressure sensitive adhesives or with fasteners which require drilling holes in the body panels. These conventional techniques result in an emblem which protrudes from the body of the vehicle, detracting from the aerodynamic appearance. Also adhesively secured emblems are subject to theft. Emblems attached to the body with fasteners secured through holes in the body panels increase the likelihood of body rust at the holes. These disadvantages are overcome by the present invention which incorporates an emblem into a molding.
The present invention provides a new and improved molding strip and method of making the same in which an indicia bearing insert is positioned within an aperture in the molding strip. A transparent plastic overlayer is injected over the insert, sealing the insert in place and forming an exposed surface which is smooth and continuous with the exposed surface of the molding strip. The indicia are viewable through the transparent overlayer and may be formed as three-dimensional raised indicia to exhibit aesthetic three-dimensional characteristics.
In accordance with the inventive method, the molding strip is cut, stamped or formed with an aperture into which the indicia bearing insert is positioned. Plastic material is injected into the aperture so that it overlays or encapsulates the insert and bonds to the insert to produce an integrally formed molding strip. The molding strip may be extruded and then placed in a mold or formed in a mold. Thereafter plastic material forming the overlayer is injected through passageways drilled or formed in the molding strip adjacent the insert receiving aperture and communicating with the mold cavity space proximate the insert. The injected plastic material substantially fills the mold cavity space proximate the insert and forms a good mechanical bond to hold the insert in place within the aperture. The injected plastic material also fuses with the insert and molding strip. If desired, the molding strip can be provided with a decorative metallized film layer. The injected plastic material serves to encapsulate and protect the edges of the metallized film exposed as a result of forming the aperture. This prevents the metallized film edges from deteriorating or oxidizing due to exposure to the elements. The plastic injected material forms a smooth and continuous surface integral with the surface of the molding strip, which avoids accumulation of dirt, road salt and the like from such as occurs in crevices or recessed logos on conventional emblems or moldings.
For a more complete understanding of the invention, its objects and advantages, reference may be had to the following specification and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevation view of a portion of a vehicle including a molding strip in accordance with the present invention;
FIG. 2 is an enlarged partial plan view illustrating the molding strip insert of the invention;
FIG. 3 is a similar enlarged partial plan view showing the aperture in the molding strip prior to insertion of the insert;
FIG. 4 is a similar partial plan view illustrating the insert positioned in the aperture prior to injection of the overlayer material; and
FIG. 6 is a cross-sectional view taken along the line 5--5 of FIG. 2, illustrating the molding strip with insert and injected overlayer in greater detail.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, an automotive body side molding is illustrated generally at 10. Molding 10 is secured to the fender panels and door panels of the automotive vehicle generally in the position shown. Although the molding strip 10 has been illustrated as a protective body side molding for the vehicle, it will be appreciated that the present invention can be employed in molding strips for other purposes. For example, the present invention can be a bumper fascia 11 illustrated in FIG. 1 on bumper 13.
Molding strip 10 includes an emblem or indicia 14, which may be a logo, trademark, tradename, insignia, design or the like. An analogous emblem 15 is illustrated on bumper fascia 11. Indicia 14 are shown in greater detail in FIG. 2. As illustrated, indicia 14 may include one or more letters 16 (or logos, designs and so forth). If desired, molding strip 10 may be in the form of a substrate 18 having a metallized film 20 secured or bonded thereon. Metallized films can be used to stimulate a bright metallic appearance which is pleasing to the eye. For illustration purposes, a portion of metallized film 20 is shown cut away in FIG. 2 to reveal the underlying substrate 18. Substrate 18 can comprise polyvinylchloride or any other conventional material suitable for the intended use of molding strip 10. Indicia 14 further includes a clear or tinted transparent plastic overlayer 22 which fully covers the letters 16 and presents an outwardly facing or exposed surface which is smooth and continuous with the outwardly facing exposed surface of molding strip 10. Overlayer 22 can be, for example, a clear or tinted polyvinylchloride material. Optionally, overlayer 22 can comprise a clear polymer material which exhibits lens magnification properties to make the indicia appear larger than actual size. As will be more fully explained below, letters 16 are integrally formed on or secured to an insert member 24 which is positioned within an aperture formed in the molding strip. To give a three-dimensional appearance, letters 16 may be raised above the surface of the insert member. Insert member 24 can be fabricated from polyvinylchloride or other suitable material. Letters 16 can be painted or can comprise a laminate such as brushed aluminized polyester film, for example.
Referring to FIGS. 3, 4 and 5, the method of making a molding strip of the invention will now be described. FIG. 3 depicts molding strip 10 into which an aperture 26 is formed. Molding strip may be extruded or injection molded and may include a metallized film layer 20 and underlying substrate 18 as discussed above. Aperture 26 may be formed during molding or it may be stamped or cut after formation of the molding strip. However formed, aperture 26 demarks the termination of metallized film layer 20 if such layer is present. In the presently preferred embodiment no special treatment of this terminating edge of film layer 20 is required to prevent oxidation or corrosion of the metallized film because of the encapsulating and protective effects of the overlayer 22. While the aperture 26 has been depicted as an elongated slot having rounded ends, other shapes are equally possible.
Referring to FIG. 4, the next step in manufacturing the molding strip is to position insert member 24 into aperture 26. Insert member 24 is of a similar size and shape to aperture 26. The outwardly facing portion of insert member 24 is somewhat smaller in circumferential size so that there is a gap 28 defined between substrate 18 and the insert member 24.
FIG. 5 depicts the insert member 24 in greater detail. As seen, insert member 24 has a lower portion 30 which conforms closely to the size and shape of aperture 26. The upper portion 32 is of a reduced circumferential size to create the gap 28. Of course, it will be appreciated by those skilled in the art that gap 28, while preferred as increasing the surface of insert member 24 for bonding, is not necessary. Letters 16 can be raised letters as shown.
FIG. 5 also illustrates the makeup of molding strip 10 in greater detail. Molding strip 10 includes substrate 18 upon which a metallized film layer 20 is provided. In practice, the metallized film layer itself comprises a plastic substrate upon which a thin metallized layer or foil layer is secured. As metallized film is conventional, the precise details of the film have been omitted from the drawings to simplify them. Deposited or bonded on top of metallized film layer 20 is a clear or tinted transparent plastic cover layer 34. This layer may be added during the initial fabrication of the molding strip stock, or it may be applied later or concurrently with the application of the metallized film. It will, of course, be understood that in certain applications where the appearance provided by the metallized film is not desired, the metalized film can be omitted.
Substrate 18 is provided with one or more conduits 36 adjacent aperture 26. Conduits 36 communicate with the region directly above the insert member 24. These conduits provide ports through which plastic material may be injected to fill the space immediately above the insert member 24 and thereby create overlayer 22. Conduits 36 may be formed in substrate 18 during fabrication of the molding strip stock or they may be drilled or otherwise formed after stamping to create aperture 26.
One suitable way of forming overlayer 22 is to place the molding strip 10 (or a portion of molding strip 10 adjacent aperture 26) in a mold which provides a mold cavity surface which conforms to the desired exterior configuration of the overlayer. In the presently preferred embodiment, the overlayer is generally flush with, or smooth and continuous with, the exterior surface of molding strip 10 defined by cover layer 34. Once the molding strip is in place, plastic material is injected through conduits 36 so that it fills the space above the insert member 24 and below the mold cavity surface. The plastic material is allowed to cure or harden, whereupon the molding strip may be removed from the mold to produce the finished molding strip. The gap 28 defined between the upper portion 32 and the substrate 18 at aperture 26 provides a surface for good bonding to hold insert member 24 in place. Conduits 36, which are preferably angled as shown, also provide a strong mechanical bond, preventing the overlayer 22 from removal. Overlayer 22 also bonds to overlayer 34 and encapsulates or covers and protects the edge 38 of metallized film 20, so that it will not be exposed to the atmosphere and oxidize.
The resulting molding strip is relatively impervious to attack from the elements and presents no protrusions or crevices which might accumulate dirt and road salt. The indica, encapsulated integrally in the molding strip, is highly aesthetic in appearance and durable. Moreover, the molding strip so manufactured is simple and economical to produce in mass production quantities and does not present the problems associated with conventional emblem mounting techniques such as failing adhesive or rusting at the fastener holes.
While the invention has been described in its presently preferred embodiment, it will be understood that the invention is capable of certain modification and change without departing from the spirit of the invention as set forth in the appended claims.
The molding of the present invention is described as molding for an automotive vehicle, a use to which it is particularly well adapted. However, it will be appreciated that the molding of the present invention is well suited for other uses and such uses are contemplated to be within the broad scope of this invention. | A molding strip having an integrally formed insert with indicia is disclosed. The molding strip includes an elongated plastic strip having an aperture formed therein. An insert is positioned in the aperture. Indicia, such as trademarks, tradenames, insignias, logos, designs or the like, are formed on the insert. A transparent overlayer is injected onto the insert for integrally bonding and securing the insert with the elongated strip. The overlayer enables the indicia to exhibit aesthetic three-dimensional characteristics when viewed by an observer. Also disclosed is a method for manufacturing the present invention. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
The present application is a divisional of U.S. application Ser. No. 09/878,802 entitled AQUEOUS SUSPENSIONS OF PENTABROMOBENZYL ACRYLATE, filed Jun. 11, 2001, now U.S. Pat. No. 6,872,332 which claims foreign priority on Israeli Application No. 136725, filed on Jun. 12, 2000, the disclosures of which are incorporated herein by reference.
FIELD OF THE INVENTION
This invention relates to novel compositions of matter that are aqueous suspensions of pentabromobenzyl acrylate (PBBMA) and to a process for making them.
BACKGROUND OF THE INVENTION
Pentabromobenzyl acrylate (PBBMA) is an acrylic monomer, which is useful in many applications, especially but not exclusively, in the field of fire retardants for plastic compositions. It can be polymerized easily by known techniques such as bulk polymerization, solution polymerization etc., or by mechanical compounding or extrusion. In mechanical compounding or extrusion, it may be grafted onto existing polymer backbones, or added to unsaturated loci on polymers.
All these properties render PBBMA a particularly useful tool in the hands of experienced compounders. However, it has been impossible, so far, to carry out aqueous manipulations with PBBMA, in spite of their desirability, because, on the one hand, PBBMA is insoluble in water, and on the other hand, because of its high bromine content, it has a high specific gravity, about 2.7, —and therefore does not lend itself to the preparation and use of aqueous suspensions.
It is a purpose of this invention to provide stable dispersions or suspensions of PBBMA, which are new compositions of matter. Dispersions and suspensions are to be considered synonyms, as used herein.
It is another purpose of this invention to provide such dispersions or suspensions that are aqueous dispersions or suspensions.
It is a further purpose of this invention to provide a process for preparing such suspensions.
It is a further purpose of this invention to provide suspensions of PBBMA for particular applications in industry.
It is a still further purpose of this invention to provide suspensions of PBBMA together with additional compounds, such as synergists for increasing the fire-retarding efficiency of compositions obtained from PBBMA.
It is a still further purpose of this invention to provide processes comprising the polymerization and/or copolymerization of PBBMA for the production of particular products.
Other purposes and advantages of the invention will appear as the description proceeds.
SUMMARY OF THE INVENTION
The suspension of PBBMA, according to the invention, is characterized in that it comprises PBBMA in the form of finely ground particles, having a size smaller than 50 μm and preferably smaller than 10 μm and more preferably from 0.3 μm to 10 μm, and contains suspending agents chosen from among xanthene gums, anionic or nonionic purified, sodium modified montmorilonite, naphthalene sulfonic acid-formaldehyde condensate sodium salt, sodium or calcium or ammonium salts of sulfonated lignin, acrylic acids/acrylic acids ester copolymer neutralized—sodium polycarboxyl, and wetting agents chosen from among alkyl ether, alkylaryl ether, fatty acid diester and sorbitan monoester types, polyoxyethylene (POE) compounds. The POE compounds are preferably chosen from among:
POE allyl ethers N—5; 10; 20;
POE lauryl ethers N—5; 10; 20;
POE acetylphenyl ethers N—3; 5; 10; 20;
POE nonylphenyl ethers N—3; 4; 5; 6; 7; 10; 12; 15; 20;
POE dinonylphenyl ethers N—5; 10; 20;
POE oleate—N—9, 18, 36;
Sorbitan monooleate N—3; 5; 10; 20.
Alkyl naphthalene sulfonates or their sodium salts.
N is the number of ethylene oxide units.
Said suspension is typically, though not necessarily, an aqueous one.
The suspension according to the invention may also include nonionic or anionic surface active agents or wetting agents, which can be chosen by persons skilled in the art. For example, nonionic agents may be polyoxyethylene (POE) alkyl ether type, preferably NP-6 (Nonylphenol ethoxylate, 6 ethyleneoxide units). Anionic agents may be free acids or organic phosphate esters or the dioctyl ester of sodium sulfosuccinic acid. It may, also, include other additives which function both as dispersing agents and suspending agents commonly used by skilled persons like sodium or calcium or ammonium salts of sulfonated lignin, acrylic acids/acrylic acids ester copolymer neutralized—sodium polycarboxyl, preferably naphthalene sulfonic acid—formaldehyde condensate sodium salt. The suspension according to the invention may also include defoaming or antifoaming agents, which can be chosen by persons skilled in the art. For example, emulsion of mineral oils or emulsion of natural oils or preferably emulsion of silicon oils like AF-52™.
The invention further comprises a method of preparing a suspension of PBBMA, which comprises grinding the PBBMA together with wetting agent and preferably also dispersing agent to the desired particle size adding it to the suspending medium, consisting of water containing suspension stabilizing agents, with slow stirring, preferably at 40 to 400 rpm. Grinding is preferably carried out with simultaneous cooling. The order of the addition of the wetting agents, the dispersing agents and the suspending agents is important.
Preserving or stabilizing agents such as Formaldehyde, and preferably a mixture of methyl and propyl hydroxy benzoates, can also be added to the suspension.
Typical size distributions of PBBMA both before grinding and as they are when present in suspensions according to the invention, are listed hereinafter. “D” indicates the diameter of the particles in μm and S.A. indicates the surface area in square meters per gram. “v” designates volume and 0.25 means 25% by volume.
D(v, 0.1)
D(v, 0.5)
D(v, 0.9)
Specific S.A.
PBBMA before
2.40
19.34
58.20
0.3623
grinding
PBBMA in
0.36
1.54
6.62
2.2554
Suspension
In an embodiment of the process of the invention, wherein suspensions of PBBMA and additional compounds—such as fire-retardant synergists, e.g. fire-retardant antimony oxide (AO), the process comprises preparing a suspension of the additional compound in a way similar to the preparation of the PBBMA suspension, and then mixing the two suspensions, preferably by adding the suspension of the additional compound to a slowly stirred suspension of PBBMA, and continuing stirring until a homogeneous, mixed suspension is obtained.
The suspensions, in particular the aqueous suspensions, of the invention are stable. When stored at room temperature, they are stable for at least two weeks and preferably at least one month. Their stability may be higher, e.g. three months or more. If they have to be stored at high temperature, they should pass the “Tropical Storage Test”, at 54° C., viz. be stable under such Test for at least one week.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The following examples are intended to illustrate the invention, but are not binding or limitative.
EXAMPLE 1
Preparation of a Suspension of PBBMA
A glass bead wet mill equipped with cooling jacket and continuous feed by a peristaltic pump, was utilized for grinding. PBBMA (750 gr) was mixed with water (240 ml), NP-6 (Nonylphenol ethoxylate) (1 ml) and Darvan#1 (Naphtalenesulfonic acid formaldehyde condensate, sodium salt) (30 gr). The mixture was fed into the grinding beads mill over a period of 25 min. The resulting slurry was stirred gently, mechanical blade stirrer, 40-60 rpm, and 10 ml of 1.5% Rhodopol 23, Xanthan Gum (CAS No 11138-66-2) in water with preserving agents, 1% Methyl Paraben,methyl-4-hydroxybenzoate, CAS No 99-76-3 and 0.5% Propyl Paraben, propyl-4-hydroxybenzoate, CAS No 94-13-3, were added.
EXAMPLE 2
Preparation of a PBBMA-AO Suspension
A suspension of Antimony Oxide was prepared as follows. To a 3-liter round bottom flask, fitted with a mechanical stirrer, were added water (240 ml), NP-6 (1 ml) (Nonylphenol ethoxylate), and Darvan #1 (Naphtalenesulfonic acid formaldehyde condensate, sodium salt) (30 g). Finely ground antimony oxide, Ultrafine grade with typical average particle size of 0.2 μm-0.4 μm. (AO, 750 g) was slowly added under fast stirring, 400-600 rpm. The stirrer was slowed, 50-150 rpm and a 1.5% solution of Rhodopol 23 Xanthan Gum (CAS No 11138-66-2) with preserving agents—1% Methyl Paraben,methyl-4-hydroxybenzoate, (CAS No 99-76-3) and 0.5% Propyl Paraben, propyl-4-hydroxybenzoate, (CAS No 94-13-3) were added (115 ml).
The mixed PBBMA-AO suspension was prepared as follows. To a slowly stirred, 40 rpm, suspension of PBBMA (750 ml) at 25° C.-30° C., obtained as described in Example 1, was added the AO suspension (250 ml) as described above. After five minutes, stirring was stopped, yielding a homogeneous mixture.
EXAMPLE 3
Preparation of a PBBMA-Styrene-Butylacrylate Terpolymer Latex
In a 0.5 L 4 necked round bottom flask fitted with mechanical stirrer, reflux condenser, thermometer, dropping funnel and Nitrogen inlet were charged 1.4 gr SDS (Sodium Dodecyl Sulfate) and 100 mL of water. The flask was immersed in an oil bath and heated to 70° C. with continuous stirring, 250 rpm, Nitrogen was introduced under the surface of the liquid. After 1 hr. the nitrogen inlet was raised above the surface of the liquid and 0.15 gr of K 2 S 2 O 8 were added. 5 min. later a solution of 15 gr Styrene and 15 gr Butylacrylate was added dropwise over 30 min. The emulsion pre-polymerization was continued for another 90 min. after which 6 gr of a PBBMA suspension (˜60% solids) were added dropwise over 70 min. The polymerization was continued overnight.
A stable latex (stable for more than two month) was obtained.
The terpolymer isolated from this emulsion was characterized. The bromine content was 7% and the glass transition temperature was 18.8° C.
EXAMPLE 4
Preparation of a PBBMA-Styrene-Acrylonitrile Terpolymer
In a 0.5 L 4 necked round bottom flask fitted with mechanical stirrer, reflux condenser, thermometer, dropping funnel and Nitrogen inlet were charged 1.4 gr SDS (Sodium Dodecyl Sulfate) and 100 mL of water. The flask was immersed in an oil bath and heated to 70° C. with continuous stirring, 250 rpm, Nitrogen was introduced under the surface of the liquid. After 1 hr. the nitrogen inlet was raised above the surface of the liquid and 0.15 gr of K 2 S 2 O 8 were added. 5 min. later a solution of 18.2 gr Styrene and 5.8 gr Acylonitrile was added dropwise over 30 min. The emulsion pre-polymerization was continued for another 20 min. after which 8.5 gr of a PBBMA suspension (˜60% solids) were added dropwise over 40 min. A second portion of 0.15 gr of K 2 S 2 O 8 was added 3 hr. after the addition of the suspension was finished. The polymerization was continued overnight.
A stable latex (stable for at least one month) was obtained.
The terpolymer isolated from this emulsion was characterized. The bromine content was 12.5%, the nitrogen content was 5% and the glass transition temperature was 107° C. The molecular weight depends on the polymerization conditions. In this particular case a Weight Average Molecular Weight, Mw, of 1.2*10 6 and Number Average Molecular Weight, Mn, of 422,000, was determined (in Dimethylformamide solution, calibrated with Polystyrene standards).
The suspensions of the invention are useful for a number of applications, and the way in which they are used and the resulting products, are also part of the invention.
Fire Retardants are commonly used in carpet-backings However, the fire retardants of the prior art are not bound to the carpet, and are susceptible to removal by dry cleaning. According to the invention, the aqueous suspension of PBBMA is applied to the reverse side of the carpets and is polymerized by heating at temperatures above 130° C. This results in a coating of PBBMA polymer which is bound to the carpet.
In the prior art, fire retardants are used in the textile industry. However, they generally produce light scattering, because they are used in powder form. According to the invention, the aqueous solution of PBBMA, optionally with complementary components, is applied to textile materials and penetrates into the fibers, and then polymerization is effected by heating at temperatures above 130° C., thus polymerizing PBBMA and binding the resulting polymers to the fibers. Addition of free radical initiating catalysts, the conventional polymerization catalysts such as organic peroxides, e.g., benzoylperoxide, or other free radical producing catalysts, e.g., azobisisobutyronitrile, will shorten polymerization time.
The PBBMA suspensions of the invention can be used to copolymerize PBBMA with other monomers or grafted to polymers, in order to produce adhesives which are also fire-retardants or other types of surface modifiers and binding promoters.
Likewise, the suspensions of the invention can be used to copolymerize PBBMA with other (meth)acrylate derivatives, such as butyl acrylate, methyl methacrylate or other monomers, to produce transparent plastics of predetermined refraction indices.
Double layered particles can also be produced, according to the invention, by adding another monomer, e.g. another (meth)acrylic derivative, to the PBBMA suspensions under polymerization conditions, to produce very stable latexes. An example of such other monomers can be, for instance, aliphatic (meth)acrylates or hydroxyethyl acrylate.
The novel products obtained according to the invention, and the processes for their production, are also part of the invention.
While examples of the invention have been described for purposes of illustration, it will be apparent that many modifications, variations and adaptations can be carried out by persons skilled in the art, without exceeding the scope of the claims. | Pentabromobenzyl acrylate (PBBMA), a useful flame retardant insoluble in water, is provided as an aqueous fluid for industrial applications. The fluid is an easy to handle, stable suspension of finely ground PBBMA in water. | 3 |
The Government of the United States of America has rights in this invention pursuant to contract agreement No. 49-2862 entered into with Sandia National Laboratories on behalf of the U.S. Department of Energy.
RELATED PATENTS AND APPLICATIONS
This application is related to U.S. Pat. Nos.:
4,105,829, issued: Aug. 8, 1978;
4,169,816, issued: Oct. 2, 1979;
4,197,169, issued: Apr. 8, 1980; and
4,259,417, issued: Mar. 31, 1981;
and U.S. patent applications:
U.S. Ser. No. 178,993, filed: Aug. 18, 1980;
U.S. Ser. No. 204,852, filed: Nov. 7, 1980;
U.S. Ser. No. 144,679, filed: Apr. 28, 1980;
U.S. Ser. No. 165,412, filed: July 3, 1980;
U.S. Ser. No. 160,143, filed: June 16, 1980;
U.S. Ser. No. 122,193, filed: Feb. 19, 1980;
U.S. Ser. No. 122,706, filed: Feb. 19, 1980; and
U.S. Ser. No. 97,194, filed: Nov. 26, 1979.
Inasmuch as many of the teachings expressed in the above-identified patents and applications may be useful in understanding the present invention, it is desired to incorporate these teachings in this disclosure by way of reference.
FIELD OF THE INVENTION
This invention relates to electrochemical cells, and more particularly to an improved cell construction which can be useful in vehicular battery systems.
BACKGROUND OF THE INVENTION
In recent times, the use of light weight battery materials and cost efficient battery constructions have been of prime interest to the automotive and battery industries. In particular, cost-effective battery designs are of paramount importance for electric vehicular systems. For electric vehicles and other bulk energy storage applications, cost justification of a battery system is highly sensitive to the initial battery cost and to the life-cycle cost. The present invention seeks to provide a new electrochemical cell construction which reduces the initial costs and extends operating life for a battery system through the utilization of new manufacturing techniques, new weight-reducing materials and new integration of components.
A new cell design and construction has resulted from the achievement of the above objectives, which design and construction features amongst other novelties:
1. An integral separator and spacer to reduce space, parts and cost.
2. A reduction in gas entrapment with the use of the new separator-spacer design.
3. An integral conductive/non-conductive (dielectric) coextruded plastic electrode which is both light weight and inexpensive to manufacture.
4. Reduction and/or elimination of parasitic shunt currents.
5. Male/female stacking and integration of parts and conduits to provide ease and compactness of assembly.
6. A two-piece interleaved bipolar battery assembly which is more compact, light weight, leakproof, easy to assemble and low cost.
7. A safer battery design and construction which reduces the possibility of spilling corrosive materials should compartments housing these materials rupture.
The subject invention is useful in the manufacture, construction and assembly of many different kinds of electrochemical cells, and the invention should be interpreted as not being limited to a specific system.
It is of particular interest for use in a circulating zinc-bromine battery, constructed in accordance with the teachings advanced in the afore-mentioned U.S. patent to: Agustin F. Venero, entitled: Metal Halogen Batteries and Method of Operating Same, U.S. Pat. No. 4,105,829, issued: Aug. 8, 1978, and assigned to the present assignee.
The above-mentioned battery system is of particular interest because of its low cost and availability of reactants, its high cell voltage and its high degree of reversibility.
DISCUSSION OF THE PRIOR ART
To the best our knowledge and belief, the various novelties presented and described herein, are completely new within the art of electrochemical system design and construction. The skilled practitioner will gain a particular appreciation of the unique ideas and concepts advanced herein.
SUMMARY OF THE INVENTION
This invention relates to an electrochemical construction comprising a stack of cells each comprised of an integral separator and spacer disposed between adjacent electrodes each comprised of a composite plastic sheet having a coextruded electrically conductive mid-portion and electrically non-conductive top and bottom side portions. The separator-spacer and the sheet electrodes are assembled by male and female connections, which are hollow and form fluid conduits for the cells. The electrochemical construction may be comprised of more than one stack of cells.
The integral separator-spacer comprises a microporous sheet, which provides ionic communication between adjacent compartments of each cell. A web surface on each side of the microporous sheet is covered with projections for maintaining a spaced compartmental distance between said separator-spacer and said adjacent electrodes. The projections on one web surface are directly opposite corresponding projections on the other web surface of the sheet in order to provide a greater structural integrity to the sheet in its capacity to maintain a spaced distance between electrodes. The projections can be pebble or rod-shaped or a combination of pebble and rod-shapes.
The separator-spacer has a non-porous border substantially surrounding the microporous sheet, which microporous sheet can be ion-selective.
The electrodes have narrow non-conductive top and bottom side portion strips with respect to their larger conductive mid-portions. The electrodes can be made monopolar or bipolar, but can be specifically bipolar in order to operate in a zinc-bromine system, for example. The non-conductivve side strips can be made of polypropylene, polyethylene, or copolymers thereof, while the conductive mid-portion comprises a carbon-containing polyolefin. More specifically, the conductive mid-portion comprises by weight 100 parts polyolefin, 25 parts carbon, 5 parts each pitch fiber and glass fiber and 1 part fumed silica powder. The extruded material can be hot formed and can be dimpled.
The electrical construction can be provided with a protective current in order to reduce or eliminate parasitic shunt currents in common electrolyte system of this type.
The zinc-bromine electrochemical system of the invention also featues a leak and impact resistant construction comprising:
a first inner compartment for storing a bromine-rich phase;
a second compartment substantially surrounding said first inner compartment and containing a first electrolyte for circulation through said cell;
a third compartment substantially surrounding both said second and first compartments and containing a second electrolyte for circulation through said cell; and
an outer casing substantially surrounding said first, second and third compartments.
The first electrolyte is generally the catholyte for the system, while the second electrolyte is generally the anolyte. The bromine-rich phase is a non-aqueous phase which separates from the aqueous catholyte and contains bromine complexing agents.
The compartment and casing materials are generally comprised of chemically inert, impact resistant plastics.
It is an object of the present invention to provide a cost efficient electrochemical construction;
It is another object of this invention to provide an electrochemical construction which is light weight and compact;
It is a further object of the invention to provide a new electrochemical system having a high voltage and cyclic-life.
These and other objects of this invention will be better understood and will become more apparent with reference to the following detailed description considered in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of a typical circulating zinc-bromine system which can benefit from the inventive construction shown in the following FIGS. 2 through 7.
FIG. 2 is a partially cutaway prospective view of a zinc-bromine system constructed in accordance with this invention;
FIG. 3 is an exploded perspective view of the two-sheet stack construction of a portion of a stack of cells of the electrochemical system of this invention;
FIG. 4 is a front view of the coextruded sheet electrode of the inventive construction shown in FIG. 3;
FIG. 4a is a side view of the sheet electrode of FIG. 4;
FIG. 5 is a perspective view of the electrode being extruded;
FIGS. 5a, 5b and 5c are respective top, front and side views of the coextrusion die used to fabricate the sheet electrode shown in FIGS. 3, 4, and 4a;
FIG. 6 is a front view of the integral separator-spacer illustrated in the inventive construction of FIG. 3;
FIG. 6a is a side view of the integral separator-spacer depicted in FIG. 6;
FIGS. 7a through 7d are illustrative of various designs for the projections depicted on the web surfaces of the separator-spacer shown in FIGS. 6 and 6a; and
FIGS. 7aa through 7dd are side views of the projections depicted in respective FIGS. 7a through 7d.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, a schematic diagram of a typical circulating, bipolar zinc-bromine system is shown. This system can benefit from the inventive construction which will be hereinafter described with reference to FIGS. 2 through 7. The zinc-bromine system of FIG. 1 comprises two electrolytes which are circulated through separate compartments 8, 9 respectively, of the cell 10. An anolyte which is generally stored in reservoir 11 is pumped via pump 12 through compartment 8 and loop 13, generally referred to as the anode loop. A catholyte which is generally stored in reservoir 14, is pumped via pump 15 through compartment 9 and loop 16, generally referred to as the cathode loop.
The zinc-bromine system is also a two phase system, in that the catholyte has bromine complexing agents and is comprised of a first aqueous phase and a second, non-aqueous, bromine-rich phase. The bromine-rich (complexed) phase tends to separate at the bromine active electrode 17 from the aqueous catholyte. This non-aqueous phase is stored in the reservoir 14, as illustrated schematically by shaded portion 14a.
A separator 18 delinates and defines the boundary between the anolyte and cathode compartments 8 and 9, respectively. The separator 18 is a membrane which prevents or binders movement of anions such as the bromide and tribromide ions from cathode compartment 9 to the anode compartment 8. In a bipolar design, the zinc active electrode 19 and the bromine active electrode 17 are opposite sides of the same electrode structure.
Further description of the zinc-bromine system can be obtained with reference to afore-mentioned U.S. Pat. No. 4,105,829; issued Aug. 8, 1978.
The zinc-bromine system can be made more practicable by integrating and improving various components of FIG. 1, as will be hereinafter explained with respect to the inventive construction shown in FIGS. 2 through 7. Where applicable within the description, like components may have similar numerical designations for the sake of brevity.
Now referring to FIG. 2, an improved electrochemical system is shown in a schematic perspective view. The improved system utilizes an integrated two-leaved separator-spacer and electrode forming a portion of a stack of cells, as depicted in the exploded view of FIG. 3.
The electrochemical system of FIG. 2, comprises a battery stack 25 which in turn is comprised of a plurality of cells 10, each having two plates, as shown in FIG. 3. One plate, according to the invention, is an integral separator-spacer 28 and the other plate is an electrode sheet 29. The separator-spacer has two functions combined in a single sheet. The first purpose is that of the separator 18 in FIG. 1, i.e. to provide fluid communication between compartments as a membrane. A more detailed description of this function can be obtained from the above-mentioned U.S. Pat. No. 4,105,829; issued Aug. 8, 1978; and also from U.S. Pat. No. 4,259,417; issued Mar. 31, 1981 for an "Ionic Barrier," to inventors: R. J. Bellows and P. G. Grimes.
The second function of sheet 28 is to space the sheet 28 from the adjacent electrode sheets 29 so as to create respective anolyte and catholyte compartments 8 and 9 (FIG. 1). The separator-spacer sheet 28 has a microporous mid-portion surface 30 which is recessed from the non-porous surface 31 of the sides, as shown in more detail in FIGS. 6 and 6a. When the separator-spacer sheets 28 are pressed between electrode sheets 29, the stack structure 25 is formed, as shown in FIG. 2. The projections 32 on the microporous mid-portion surfaces are designed to maintain a spaced compartmental distance between the separator-spacer surface 30 and the flat conductive surfaces 33 of adjacent electrode sheet 29. The projections 32 provide structural means against collapse of surfaces 33 upon surfaces 30 and vice versa. The projections 32 on one side 30 of sheet 28 are diametrically opposite corresponding projections 32 on the opposite side 30 of sheet 28 as clearly illustrated in FIG. 6a. This is done, to provide a greater strength against distortion of surfaces 33 upon surfaces 30. The projections 32 usually are designed as pebbles as depicted by arrows 32a in FIG. 6a, and as also shown in FIGS. 7cc and 7dd, etc.
These projections 32 may also be designed with a rod-shape as depicted in FIGS. 7a, 7aa and 7b, 7bb; by arrows 32b. The projections 32 may also be a combination of pebble and rod-shaped protuberances as depicted in FIGS. 7c, 7cc and 7d, 7dd.
The design of these projections allow for an expeditious flow of electrolyte through the compartments 8 and 9, respectively. The flow of electrolyte is accomplished without entrapping gas bubbles about projections 32 within the compartmental cavities 8 and 9.
The mid-portion of the separator-spacer sheet 28 can be comprised of a microporous membrane material known as Daramic®, Series HW-0835, which is made by W. R. Grace Co., Polyfibron Division, Cambridge, Mass. The raised side borders 31 of non-porous material may be any moldable plastic. The plastic of borders 31 is typycally overmolded around the separator-spacer insert by injection molding, as can be seen from FIG. 6a.
Sheets 28 and 29 are assembled by means of hollow male/female connectors 40 shown in detail in FIGS. 6 and 6a. When the sheets 28 and 29 are assembled in a stack 25, these hollow connectors 40 form electrolyte manifolds which supply compartments 8 and 9 with electrolyte via individual conduits or channels 60.
The male/female connectors 40 of sheets 28 fit through the holes 41 (FIGS 4 and 4a) in adjacent sheets 29, and snap into mating connectors 40 in subsequently adjacent sheets 28.
The electrode sheet 29 of FIGS. 4 and 4a is comprised of a coextruded sheet of plastic which has an electrically conductive mid-portion 33 and two side portions 37 of electrically non-conductive (insulating) plastic. The top and bottom side portions 37 are coextruded "side-by-side" along with the mid-portion 33 to form a one piece continuous electrode sheet, which continuous sheet is then cut to specific lengths to form a plurality of smaller sheets 29. The edges 38 of sheet 29 may be undercut to improve electrical isolation in stack 25.
This "side-by-side" profile co-extrusion of insulating and conductive plastic sheets 37 and 33, respectively, presents a new and an alternative fast method of production for all monopolar and bipolar electrodes including electrodes for zinc bromine batteries. Compared with compression molding, the co-extrusion method gives more uniformity in thickness, a stronger bonding between the insulating and conductive plastics, much desired flatness, and "electrode by yards" similar to dress fabrice. The fabrication cost is much lower because the process is continuous.
A special formulation of carbon plastic is needed for mid-portion 33 of sheet 29 to provide good electrical conductivity, which still exhibit good extrudibility, good strength, and excellent anti-corrosive properties against bromine and zinc bromide in the electrolyte.
The preferred composition of the conductive carbon plastic is covered by aforementioned U.S. Pat. No. 4,169,816; issued Oct. 2, 1979, to H. C. Tsien. This formulation gives good conductivity (1 to 2 ohm-cm in resistivity), good flex strength, low permeability inertness to bromine, good extrudibility, better weldability and less mold shrinkage.
The conductive plastic is a mixture of 100 parts by weight of polyolefin copolymer, 25 parts by weight of special conductive carbon, 5 parts by weight each of carbon fiber and glass fiber, and 1 part by weight of fumed silica powder.
Some of the other advantages of coextruding the section 33 and 37 are:
1. Good bonding between the insulating and conductive plastics.
2. Maintaining width, flatness and thickness dimensions with the tolerances specified.
3. Clear and sharp boundary lines between sections 33 and 37.
FIGS. 5a, 5b and 5c are respective top, front and side views of an extrusion die used to fabricate the electrode sheet. The center extrusion die 47 receives conductive plastic from a horizontal extruder through conduit 46, while the side extrusion dies 48, each receive non-conducting plastic from an overhead, vertical extruder via conduits 45a and 45b, respectively.
The horizontal extruder for the black conductive plastic is a 21/2" screw with L/D of 30:1, while the vertical extruder for the opaque insulating plastic is a 11/2" dia. screw with L/D of 24:1.
The melted insulating plastic enters into the die at 90 degrees from the vertical stream 45, divides into two steams 45a and 45b and flows into one left and one right separate "coat hangers" along side the main coat hanger 45. The die design is conventional, except that the side-by-side profile division is believed to be novel. The die is of split construction in order to facilitate any changes in the design and the ease of fabrication.
The main die assembly consists of a lower die body 55, upper die body 56, flexible upper lip 57 and fixed lower lip 58.
The die lip gap is ground to allow for the swell of plastics emerging out of the die. Lip gaps can be individually adjusted by screws 59 in conjunction with the nut bars 61. The two side plastics 62 and 63 close the two outsides of flow channels of the insulating plastics and give a box-like reinforcement.
Adapter 64 provides connection to the main extruder. There are (16) cartridge heaters 65 and (4) band heaters 66 for heating the two streams of plastics. Temperatures are controlled through thermocouples and individual zone temperature controllers.
The individual adjustment of the left and right streams 45a and 45b is made possible by ball headed adjusting screws 67 and locknut 68. Bushings 74 make good connection from valve blocks 75 to die block 56. All main parts of the die are made of A2 air hardening tool steel. The Bethelehem A2 air hardening steel has the following physical properties:
______________________________________ As-annealed Heat Treated______________________________________Hardness (R/C) 15-20 56-58Yield Strength psi 55,000 208,750U.T.S. psi 114,950 255,250Elongation % 18% .8%______________________________________
With the head pressures from the extruders well over 1000 psi, the die cannot operate free from internal leakage between the insulating and conducting streams if the die is in the soft annealed condition. The hardened and reground die eliminates internal leakage. Four different types of insulating plastics were tired, they are:
______________________________________ Melt Flow Index______________________________________Fiberfil J60/20E 230° C., 2160 gm load, 4.5 gm in 10 min.UGI LR711 HDPE 190° C., 2160 gm load, 10.5 gm in 10 min.Exxon P.P. 5052 P.P. 230° C., 2160 gm load, .9 to 1.5 gm in 10 min.Exxon P.P. 5011 P.P. 230° C., 2160 gm load, .45 to .85 gm in 10 min.______________________________________
Both Exxon homopolymer PP5011 and 5052 can match well with the conductive plastic. They came out of the die with no wrinkles, the sheets were flat and uniform.
Theoretically, aside from previous considerations, any polyethylene or polypropylene for side portions 37 can be a good match with the conductive plastic mid-portion 33, because the basic material used in the conductive plastic is the copolymer of the two. The melting points are in the range of 325° to 375° F. Therefore, approximately 400° F. is a proper temperature in range for the two streams to meet. Head pressures are 1500 to 1800 psi. These conditions made a good bond at the bonding line.
Close match of melt indices is necessary in order to eliminate scallops formed at the joint of the two edges. The viscosities and velocities of the streams from the two extruders has to be very closely equal. Pressures can be manipulated from two heads while varying the temperatures in various die zones to get the matching conditions. However, the differences between melt flow index of conductive and that of insulating plastics has to be minimized.
The extrusion speed can be around 20 ft./minute to 90 ft./minute.
There are many downstream attachments that can be added so that the co-extruded sheet can be worked on while still hot and soft. Thus, the repeated heating and cooling cycles with the accompanied plastic degradations can be eliminated. Powder of activated carbon can be sprayed on one face of the carbon plastic as the sheet is emerging from the die and before the sheet is pinched by the cold nip rolls. The powder spray is limited in the conductive area.
Various types of surface finishes can be obtained by changing the nip rolls from polished chrome-plated surface to Teflon coated and rubber rolls. It is also possible to replace nip rolls with dimpling rolls, so that cavities or special flow patterns can be formed on one or both faces of the co-extruded sheet. The hot forming rolls can make repeated patterns of design indentations in the electrode, if so desired.
The combination possibilities are only limited by imagination. For dimpling, the design is also repeated every revolution of the dimpling rolls. It is very much like printing repeated patterns on the fabric. These downstream modifications such as catalyst spraying, dimpling, or hot forming can be added so that all operations can be done without significant added production cost.
FIG. 5 is a schematic perspective view of the continuous electrode sheet emerging from the split die illustrated in FIGS. 5a, 5b and 5c.
Now referring to FIG. 2, a further safety feature for the electromechanical system is illustrated. In order to prevent or reduce the risk of spilling corrosive bromine and bromine compounds in the event of casing or compartmental rupture, the various compartments can be nested with the bromine-containing compartment 50 being the most internal compartment. The bromine compartment 50 is surrounded by the catholyte-containing compartment 51, which in turn is surrounded by the anolyte-containing compartment 52. Compartments 50, 51, and 52 are all enclosed by outer casing 53.
Shunt currents can be eliminated along formed manifolds (connectors 40) by means of applying a protective current along these electrolyte carrying conduits, in accordance with the teachings expressed in aforementioned U.S. Pat. No. 4,197,169 issued Apr. 8, 1980 to M. Zahn, P. G. Grimes and R. J. Bellows.
The two-leaved electrochemical cell construction of this invention reduces parts and is easier to fabricate and assemble than prior systems of this kind. Further modifications to the invention may occur to those skilled practitioners of this art. Such modifications have not been described for the sake of brevity.
The scope and breadth of the invention is meant to be encompassed by the following appended claims. | An electrochemical cell construction features a novel co-extruded plastic electrode in an interleaved construction with a novel integral separator-spacer. Also featured is a leak and impact resistant construction for preventing the spill of corrosive materials in the event of rupture. | 7 |
CLAIM OF PRIORITY
[0001] This application is a continuation of U.S. patent application Ser. No. 13/175,510, filed Jul. 1, 2011, now U.S. Pat. No. 8,336,231, which is a continuation of U.S. patent application Ser. No. 12/361,242, filed Jan. 28, 2009, which is a continuation of U.S. patent application Ser. No. 10/971,455, filed Oct. 22, 2004, now U.S. Pat. No. 7,484,322, the entire disclosures which are incorporated by reference herein.
FIELD OF THE INVENTION
[0002] This invention relates generally to a reduction system for removing soil to expose underground utilities (such as electrical and cable services, water and sewage services, etc.), and more particularly to a system for removing materials from the ground and backfilling the area.
BACKGROUND OF THE INVENTION
[0003] With the increased use of underground utilities, it has become more critical to locate and verify the placement of buried utilities before installation of additional underground utilities or before other excavation or digging work is performed. Conventional digging and excavation methods such as shovels, post hole diggers, powered excavators, and backhoes may be limited in their use in locating buried utilities as they may tend to cut, break, or otherwise damage the lines during use.
[0004] Devices have been previously developed to create holes in the ground to non-destructively expose underground utilities to view. One design uses high pressure air delivered through a tool to loosen soil and a vacuum system to vacuum away the dirt after it is loosened to form a hole. Another system uses high pressure water delivered by a tool to soften the soil and create a soil/water slurry mixture. The tool is provided with a vacuum system for vacuuming the slurry away.
SUMMARY OF THE INVENTION
[0005] The present invention recognizes and addresses disadvantages of prior art constructions and methods, and it is an object of the present invention to provide an improved drilling and backfill system. This and other objects may be achieved by a mobile digging and backfill system for removing and collecting material above a buried utility. The system comprises a mobile chassis, a collection tank mounted to the chassis, a water pump mounted to the chassis for delivering a pressurized liquid flow against the material for loosening the material at a location, a vacuum pump connected to the collection tank so that an air stream created by the vacuum pump draws the material and the fluid from the location into the collection tank, and at least one backfill reservoir mounted to the chassis for carrying backfill for placement at the location.
[0006] In another embodiment, a mobile digging and backfill system for removing and collecting material comprises a mobile digging and backfill system for removing and collecting material. The system has a mobile chassis, a collection tank moveably mounted to the chassis, and a digging tool comprising at least one nozzle and a vacuum passage proximate the nozzle. A water pump mounted on the chassis has an output connected to the nozzle for delivering a pressurized liquid flow against the material for loosening the material at a location. A vacuum pump mounted on the chassis has an input connected to the collection tank so that an air stream created by the vacuum pump draws the material and the fluid from the location into the collection tank. A motor mounted to the chassis and is in driving engagement with the water pump and said vacuum pump. A first backfill reservoir is moveably mounted on the chassis for carrying backfill for placement at the location.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] A full and enabling disclosure of the present invention, including the best mode thereof directed to one of ordinary skill in the art, is set forth in the specification, which makes reference to the appended figures, in which:
[0008] FIG. 1 is a perspective view of a drilling and backfill system constructed in accordance with one embodiment of the present invention;
[0009] FIG. 2 is a perspective view of a key hole drill for use with the drilling and backfill system of FIG. 1 ;
[0010] FIG. 3 is a perspective view of a reduction tool for use with the drilling and backfill system of FIG. 1 ;
[0011] FIG. 4 is bottom view of the reduction tool shown in FIG. 3 ;
[0012] FIG. 5 is a partial perspective view of the reduction tool of FIG. 3 in use digging a hole;
[0013] FIG. 6 is a perspective view of a key hole drilling tool base for use with the key hole drill of FIG. 2 ;
[0014] FIG. 6A is a bottom perspective view of the tool base shown in FIG. 6 ;
[0015] FIG. 7 is a perspective view of the reduction tool of FIG. 3 in use digging the hole;
[0016] FIG. 8 is a perspective view of the drilling and backfill system of FIG. 1 , showing the hole being backfilled;
[0017] FIG. 9 is a perspective view of the drilling and backfill system of FIG. 1 , showing the hole being tamped; and
[0018] FIG. 10 is a schematic view of the hydraulic, electric, water, and vacuum systems of the drilling and backfill system of FIG. 1 .
Repeat use of reference characters in the present specification and drawings is intended to represent same or analogous features or elements of the invention.
DETAILED DESCRIPTION
[0019] Reference will now be made in detail to presently preferred embodiments of the invention, one or more examples of which are illustrated in the accompanying drawings. Each example is provided by way of explanation of the invention, not limitation of the invention. In fact, it will be apparent to those skilled in the art that modifications and variations can be made in the present invention without departing from the scope and spirit thereof. For instance, features illustrated or described as part of one embodiment may be used on another embodiment to yield a still further embodiment. Thus, it is intended that the present invention covers such modifications and variations as come within the scope of the appended claims and their equivalents.
[0020] Referring to FIG. 1 , a drilling and backfill system 10 generally includes a water reservoir tank 12 , a collection tank 14 , a motor 16 , a drilling apparatus 18 , and back fill reservoirs 20 and 22 , all mounted on a mobile chassis 24 , which is, in this embodiment, in the form of a trailer. Trailer 24 includes four wheels 38 (only three of which are shown in FIG. 1 ) and a draw bar and hitch 40 . Drilling and backfill system 10 generally mounts on a platform 42 , which is part of trailer 24 . It should be understood that while drill and backfill system 10 is illustrated mounted on a trailer having a platform, the system may also be mounted on the chassis of a vehicle such as a truck or car. Further, a chassis may comprise any frame, platform or bed to which the system components may be mounted and that can be moved by a motorized vehicle such as a car, truck, or skid steer. It should be understood that the components of the system may be either directly mounted to the chassis or indirectly mounted to the chassis through connections with other system components.
[0021] The connection of the various components of system 10 is best illustrated in FIG. 10 . Motor 16 is mounted on a forward end of trailer 24 and provides electricity to power two electric hydraulic pumps 30 and 172 , and it also drives both a water pump 26 and a vacuum pump 28 by belts (not shown). Motor 16 is preferably a gas or diesel engine, although it should be understood that an electric motor or other motive means could also be used. In one preferred embodiment, motor 16 is a thirty horsepower diesel engine, such as Model No. V1505 manufactured by Kubota Engine division of Japan, or a twenty-five horsepower gasoline engine such as Model Command PRO CH25S manufactured by Kohler Engines. The speed of motor 16 may be varied between high and low by a wireless keypad transmitter 108 that transmits motor speed control to a receiver 110 connected to the throttle of motor 16 .
[0022] The water system will now be described with reference to FIG. 10 . Water reservoir tank 12 connects to water pump 26 , which includes a low pressure inlet 44 and a high pressure outlet 46 . In the illustrated embodiment, water pump 26 can be any of a variety of suitable pumps that delivers between 3,000 and 4,000 lbs/in 2 at a flow rate of approximately five gallons per minute. In one preferred embodiment, water pump 26 is a Model No. TS2021 pump manufactured by General Pump. Water tank 12 includes an outlet 50 that connects to a strainer 52 through a valve 54 . The output of strainer 52 connects to the low pressure side of water pump 26 via a hose 48 . A check valve 56 is placed inline intermediate strainer 52 and low pressure inlet 44 . High pressure outlet 46 connects to a filter 58 and then to a pressure relief and bypass valve 60 . In one preferred embodiment, pressure relief and bypass valve 60 is a Model YUZ140 valve manufactured by General Pump.
[0023] A “T” 62 and a valve 64 , located intermediate valve 60 and filter 58 , connect the high pressure output 46 to a plurality of clean out nozzles 66 mounted in collection tank 14 to clean the tank's interior. A return line 68 connects a low pressure port 69 of valve 60 to water tank 12 . When a predetermined water pressure is exceeded in valve 60 , water is diverted through low port 69 and line 68 to tank 12 . A hose 70 , stored on a hose reel 73 ( FIG. 1 ), connects an output port 72 of valve 60 to a valve 74 on a digging tool 32 ( FIG. 3 ). A valve control 76 ( FIG. 3 ) at a handle 78 of digging tool 32 provides the operator with a means to selectively actuate valve 74 on digging tool 32 . The valve delivers a high pressure stream of water through a conduit 80 ( FIGS. 3 , 5 , 7 , and 10 ) attached to the exterior of an elongated pipe 82 that extends the length of digging tool 32 .
[0024] Referring to FIG. 3 , digging tool 32 includes handle 78 for an operator 34 ( FIG. 7 ) to grasp during use of the tool. A connector 84 , such as a “banjo” type connector, connects the vacuum system on drilling and back fill system 10 ( FIG. 1 ) to a central vacuum passage 86 ( FIG. 4 ) in digging tool 32 . Connector 84 is located proximate handle 78 . Vacuum passage 86 extends the length of elongated pipe 82 and opens to one end of a vacuum hose 88 . The other end of hose 88 connects to an inlet port 90 on collection tank 14 ( FIG. 7 ). It should be understood that other types of connectors may be used in place of “banjo” connector 84 , for example clamps, clips, or threaded ends on hose 88 and handle 78 .
[0025] Referring to FIGS. 4 and 5 , a fluid manifold 92 , located at a distal end 94 of digging tool 32 , connects to water conduit 80 and contains a plurality of nozzles that are angled with respect to one another. In one preferred embodiment having four nozzles, two nozzles 96 and 98 are directed radially inwardly at approximately 45 degrees from a vertical axis of the digging tool, and the two remaining nozzles 100 and 102 are directed parallel to the axis of the digging tool. During use of the drilling tool, nozzles 96 and 98 produce a spiral cutting action that breaks the soil up sufficiently to minimize clogging of large chunks of soil within vacuum passage 86 and/or vacuum hose 88 . Vertically downward pointing nozzles 100 and 102 enhance the cutting action of the drilling tool by allowing for soil to be removed not only above a buried utility, but in certain cases from around the entire periphery of the utility. In other words, the soil is removed above the utility, from around the sides of the utility, and from beneath the utility. This can be useful for further verifying the precise utility needing service and, if necessary, making repairs to or tying into the utility.
[0026] Digging tool 32 also contains a plurality of air inlets 104 formed in pipe distal end 94 that allow air to enter into vacuum passage 86 . The additional air, in combination with the angled placement of nozzles 96 and 98 , enhances the cutting and suction provided by tool 32 . Returning to FIG. 6 , digging tool 32 may also include a control 106 for controlling the tool's vacuum feature. Control 106 may be an electrical switch, a vacuum or pneumatic switch, a wireless switch, or any other suitable control to adjust the vacuum action by allowing the vacuum to be shut off or otherwise modulated. An antifreeze system, generally 190 ( FIGS. 1 and 2 ), may be provided to prevent freezing of the water pump and the water system. Thus, when the pump is to be left unused in cold weather, water pump 26 may draw antifreeze from the antifreeze reservoir through the components of the water system to prevent water in the hoses from freezing and damaging the system.
[0027] Turning now to FIGS. 7 and 10 , vacuum pump 28 is preferably a positive displacement type vacuum pump such as that used as a supercharger on diesel truck. In one preferred embodiment, vacuum pump 28 is a Model 4009-46R3 blower manufactured by Tuthill. A hose 112 connects an intake of the vacuum pump to a vacuum relief device 114 , which may be any suitable vacuum valve, such as a Model 215V-H01AQE spring loaded valve manufactured by Kunkle. Vacuum relief device 114 controls the maximum negative pressure of the vacuum pulled by pump 28 , which is in the range of between 10 and 15 inches of Hg in the illustrated embodiment. A filter 116 , located up stream of pressure relief valve 114 , filters the vacuum air stream before it passes through vacuum pump 28 . In one preferred embodiment, the filter media may be a paper filter such as those manufactured by Fleet Guard. Filter 116 connects to an exhaust outlet 118 of collection tank 14 by a hose 120 , as shown in FIGS. 1 , 7 , 8 , and 9 . An exhaust side 122 of vacuum pump 28 connects to a silencer 124 , such as a Model TS30TR silencer manufactured by Cowl. The output of silencer 124 exits into the atmosphere.
[0028] The vacuum air stream pulled through vacuum pump 28 produces a vacuum in collection tank 14 that draws a vacuum air stream through collection tank inlet 90 . When inlet 90 is not closed off by a plug 127 ( FIG. 1 ), the inlet may be connected to hose 88 leading to digging tool 32 . Thus, the vacuum air stream at inlet 90 is ultimately pulled through vacuum passage 86 at distal end 94 of tool 32 . Because it is undesirable to draw dirt or other particulate matter through the vacuum pump, a baffle system, for example as described in U.S. Pat. No. 6,470,605 (the entire disclosure which is incorporated herein), is provided within collection tank 14 to separate the slurry mixture from the vacuum air stream. Consequently, dirt, rocks, and other debris in the air flow hit a baffle (not shown) and fall to the bottom portion of the collection tank. The vacuum air stream, after contacting the baffle, continues upwardly and exits through outlet 118 through filter 116 and on to vacuum pump 28 .
[0029] Referring once again to FIG. 1 , collection tank 14 includes a discharge door 126 connected to the main tank body by a hinge 128 that allows the door to swing open, thereby providing access to the tank's interior for cleaning. A pair of hydraulic cylinders 130 (only one of which is shown in FIG. 8 ) are provided for tilting a forward end 132 of tank 14 upwards in order to cause the contents to run towards discharge door 126 . A gate valve 140 , coupled to a drain 142 in discharge door 126 , drains the liquid portion of the slurry in tank 14 without requiring the door to be opened. Gate valve 140 may also be used to introduce air into collection tank 14 to reduce the vacuum in the tank so that the door may be opened.
[0030] Running the length of the interior of collection tank 14 is a nozzle tube 132 ( FIG. 10 ) that includes nozzles 66 for directing high pressure water about the tank, and particularly towards the base of the tank. Nozzles 66 are actuated by opening valve 64 ( FIG. 10 ), which delivers high pressure water from pump 26 to nozzles 66 for producing a vigorous cleaning action in the tank. When nozzles 66 are not being used for cleaning, a small amount of water is allowed to continuously drip through the nozzles to pressurize them so as to prevent dirt and slurry from entering and clogging the nozzles.
[0031] Nozzle tube 132 , apart from being a conduit for delivering water, is also a structural member that includes a threaded male portion (not shown) on an end thereof adjacent discharge door 126 . When discharge door 126 is shut, a screw-down type handle 134 mounted in the door is turned causing a threaded female portion (not shown) on tube 132 to mate with the male portion. This configuration causes the door to be pulled tightly against an open rim (not shown) of the collection tank. Actuation of vacuum pump 28 further assists the sealing of the door against the tank opening. Discharge door 126 includes a sight glass 136 to allow the user to visually inspect the tank's interior.
[0032] Backfill reservoirs 20 and 22 are mounted on opposite sides of collection tank 14 . The back fill reservoirs are mirror images of each other; therefore, for purposes of the following discussion, reference will only be made to backfill reservoir 22 . It should be understood that backfill reservoir 20 operates identically to that of reservoir 22 . Consequently, similar components on backfill reservoir 20 are labeled with the same reference numerals as those on reservoir 22 .
[0033] Referring to FIG. 1 , back fill reservoir 22 is generally cylindrical in shape and has a bottom portion 144 , a top portion 146 , a back wall 148 , and a front wall 150 . Top portion 146 connects to bottom portion 144 by a hinge 152 . Hinge 152 allows backfill reservoir 22 to be opened and loaded with dirt by a front loader 154 , as shown in phantom in FIG. 1 . Top portion 146 secures to bottom portion 144 by a plurality of locking mechanisms 156 located on the front and back walls. Locking mechanisms 156 may be clasps, latches or other suitable devices that secure the top portion to the bottom portion. The seam between the top and bottom portion does not necessarily need to be a vacuum tight seal, but the seal should prevent backfill and large amounts of air from leaking from or into the reservoir. Front wall 150 has a hinged door 158 that is secured close by a latch 160 . As illustrated in FIG. 8 , hydraulic cylinders 130 enable the back fill reservoirs to tilt so that dirt can be off loaded through doors 158 .
[0034] As previously described above, backfill reservoirs 20 and 22 may be filled by opening top portions 146 of the reservoirs and depositing dirt into bottom portion 144 with a front loader. Vacuum pump 28 , however, may also load dirt into back fill reservoirs 20 and 22 . In particular, back fill reservoir 22 has an inlet port 162 and an outlet port 164 . During normal operation, plugs 166 and 168 fit on respective ports 162 and 164 to prevent backfill from leaking from the reservoir. However, these plugs may be removed, and outlet port 164 may be connected to inlet port 90 on collection tank 14 by a hose (not shown), while hose 88 may be attached to inlet port 162 . In this configuration, vacuum pump 28 pulls a vacuum air stream through collection tank 14 , as described above, through the hose connecting inlet port 90 to outlet port 164 , and through hose 88 connected to inlet port 162 . Thus, backfill dirt and rocks can be vacuumed into reservoirs 20 and 22 without the aide of loader 154 . It should be understood that this configuration is beneficial when backfill system 10 is being used in an area where no loader is available to fill the reservoirs. Once the reservoirs are filled, the hoses are removed from the ports, and plugs 166 and 168 are reinstalled on respective ports 162 and 164 .
[0035] Referring once more to FIG. 10 , hydraulic cylinders 130 , used to tilt collection tank 14 and backfill reservoirs 20 and 22 , are powered by electric hydraulic pump 30 . Hydraulic pump 30 connects to a hydraulic reservoir 170 and is driven by the electrical system of motor 16 . A high pressure output line 171 and a return line 173 connect pump 30 to hydraulic cylinders 130 . Hydraulic pump 172 , mounted on trailer 24 , is separately driven by motor 16 and includes its own hydraulic reservoir 174 . An output high pressure line 175 and a return line 186 connect pump 172 to a pair of quick disconnect couplings 182 and 184 , respectively. That is, high pressure line 175 connects to quick disconnect coupling 182 ( FIGS. 1 and 2 ) through a control valve 178 , and return line 186 connects quick disconnect coupling 184 to reservoir 188 . A pressure relief valve 176 connects high pressure line 175 to reservoir 188 and allows fluid to bleed off of the high pressure line if the pressure exceeds a predetermined level. A pressure gauge 180 may also be located between pump 172 and control valve 178 .
[0036] Quick disconnect coupling 182 provides a high pressure source of hydraulic fluid for powering auxiliary tools, such as drilling apparatus 18 , tamper device 185 , or other devices that may be used in connection with drilling and backfill system 10 . The high pressure line preferably delivers between 5.8 and 6 gallons per minute of hydraulic fluid at a pressure of 2000 lbs/in 2 . Hydraulic return line 186 connects to a quick disconnect coupling 184 ( FIGS. 1 and 2 ) on trailer 24 . Intermediate quick disconnect coupling 184 and hydraulic fluid reservoir 174 is a filter 188 that filters the hydraulic fluid before returning it to hydraulic reservoir 174 . While quick disconnect couplings 182 and 184 are shown on the side of trailer 24 , it should be understood that the couplings may also be mounted on the rear of trailer 24 .
[0037] Referring to FIGS. 1 and 2 , drilling apparatus 18 is carried on trailer 24 and is positioned using winch and crane 36 . Drilling apparatus 18 includes a base 192 , a vertical body 194 , and a hydraulic drill motor 196 slidably coupled to vertical body 194 by a bracket 198 . A high pressure hose 200 and a return hose 202 power motor 196 . A saw blade 204 attaches to an output shaft of hydraulic motor 196 and is used to drill a coupon 206 ( FIG. 7 ) in pavement, concrete or other hard surfaces to expose the ground above the buried utility. The term coupon as used herein refers to a shaped material cut from a continuous surface to expose the ground beneath the material. For example, as illustrated in FIG. 7 , coupon 206 is a circular piece of concrete that is cut out of a sidewalk to expose the ground thereunder.
[0038] Body 194 has a handle 220 for the user to grab and hold onto during the drilling process. Hydraulic fluid hoses 200 and 202 connect to two connectors 222 and 224 ( FIG. 10 ) mounted on body 194 and provide hydraulic fluid to hydraulic drill motor 196 . A crank 226 is used to move the drill motor vertically along body 194 . Drilling apparatus 18 is a Model CD616 Hydra Core Drill manufactured by Reimann & Georger of Buffalo, N.Y. and is referred to herein as a “core drill.”
[0039] In prior art systems, base 192 was secured to pavement or concrete using lag bolts, screws, spikes, etc. These attachment methods caused unnecessary damage to the surrounding area and required additional repair after the utility was fixed and the hole was backfilled. Additionally, having to drill additional holes for the bolts or screws or pounding of the spikes with a sledge hammer presented unnecessary additional work. Thus, the drilling apparatus of the present invention uses the vacuum system of drilling and backfill system 10 to secure base 192 to the pavement.
[0040] Referring to FIGS. 6 and 6A , base 192 includes a flat plate 195 having a connector 206 attached to a top surface thereof. Connector 206 attaches to an outlet port 208 formed in a top surface of plate 195 that is in fluid communication with a recessed chamber 210 ( FIG. 6A ) formed in a bottom surface 212 of plate 195 . That is, outlet port 208 has a passageway therethrough that extends between the top and bottom surfaces. A groove 230 formed in bottom surface 212 receives a pliable gasket 232 that forms a relatively air tight seal between the bottom surface 212 and the pavement or concrete being drilled. It should be understood that while a gasket is shown, it may not be necessary depending on the strength of the vacuum air stream being pulled through connector 206 since bottom surface 212 can form a sufficient seal with the pavement or concrete. A bracket 214 coupled to a top surface of plate 195 fixedly secures body 194 ( FIG. 2 ) to base 192 . A bolt or screw 216 is received through body 194 and into a threaded bore 218 to secure the body to the base. Wheels attached to the base allow the drilling apparatus to be moved around the work area after it has been off loaded the trailer by winch and crane 36 . The term “base” as used herein refers to a drill support structure that maintains a secure connection of the drill to a surface proximate the area to be drilled. The drill base should have a generally planar bottom surface, and the remaining structure of the base may be of any suitable shape to secure the drill motor to the base.
[0041] Referring to FIG. 2 , hose 88 connects to connector 206 by a suitable clamp (not shown). Once core drill 18 is positioned, vacuum pump 26 is turned on and a vacuum is pulled through hose 88 into chamber 210 , providing a vacuum of between 12-15 inches of Hg, which is sufficient to fixedly secure base 192 to the pavement or concrete during the drilling process. Prior to moving core drill 18 , vacuum pump 28 is shut down to eliminate the vacuum produced in chamber 210 .
[0042] The operation of the drilling and backfill system will now be described with reference to FIGS. 2 , 7 to 9 and 10 . Prior to using drilling and backfill system 10 , water is added to water tank 12 , and valve 54 is opened to allow water to flow to water pump 26 . Motor 16 is powered up, and water pressure is allowed to build in the system.
[0043] Referring to FIG. 2 , if a utility is located under concrete, core drill 18 is positioned over the utility, and vacuum hose 88 is connected from inlet port 90 on collection tank 14 to connector 206 on base plate 195 . Hydraulic hoses 200 and 202 are connected to hydraulic motor 196 at connectors 222 and 224 , and vacuum pump 28 and hydraulic pump 172 are powered up. Saw 204 is used to cut coupon 206 ( FIG. 7 ) from the concrete to expose the ground over the utility. Hose 70 connects to saw 204 and provides a steady stream of water that flushes the drill bit during the drilling process. Coupon 206 is removed from the hole and placed aside so that it can be reused in repairing the hole after it is backfilled.
[0044] Next, and referring to FIG. 7 , the user disconnects vacuum hose 88 from connector 206 and connects the hose to digging tool handle 78 using banjo connector 84 . High pressure water hose 70 is also connected to valve 74 to provide water to the digging tool. As tool 32 is used, it is pressed downwardly into the ground to dig a hole. For larger diameter holes, digging tool 32 is moved in a generally circular manner as it is pressed downward. Slurry formed in the hole is vacuumed by tool 32 through vacuum passage 86 ( FIGS. 4 and 5 ) and accumulates in collection tank 26 . Once the hole is completed and the utility exposed, the vacuum system can be shut down, and the operators may examine or repair the utility as needed.
[0045] After work on the utility is completed, and referring to FIG. 8 , the operator may cover the utility with clean backfill from backfill reservoirs 20 and 22 . In particular, trailer 24 is positioned so that one of backfill reservoirs 20 or 22 is proximate the hole. Hydraulic cylinders 130 are activated, causing the tanks to tip rearward so that backfill can be delivered through door 158 into the hole. Once the hole is sufficiently filled, hydraulic cylinders 130 return reservoirs 20 and 22 to their horizontal position, and door 158 is secured in the closed position.
[0046] With reference to FIG. 9 , operator 34 may use a tamping device 185 to tamp the backfill in the hole. Tamping device 185 connects to hydraulic pump 172 through quick disconnect couplings 182 and 184 via hydraulic lines 200 and 202 . Tamping device 185 is used to pack the backfill in the hole and to remove any air pockets. Once the hole has been filed and properly packed, coupon 206 is moved into the remaining portion of the hole. The reuse of coupon 206 eliminates the need to cover the hole with new concrete. Instead, coupon 206 is placed in the hole, and grout is used to seal any cracks between the key and the surrounding concrete. Thus, the overall cost and time of repairing the concrete is significantly reduced, and the need for new concrete is effectively eliminated.
[0047] Drilling and backfill system 10 can be used to dig multiple holes before having to empty collection tank 14 . However, once collection tank 14 is full, it can be emptied at an appropriate dump site. In emptying collection tank 14 , motor 16 is idled to maintain a vacuum in tank 14 . This allows the door handle to be turned so that the female threaded member (not shown) is no longer in threading engagement with the male member (not shown) on nozzle rod 132 , while the vacuum pressure continuing to hold the door closed. Once motor 16 is shut down, the vacuum pressure is released so that air enters the tank, thereby pressurizing the tank and allowing the door to be opened. Once opened, hydraulic cylinders 130 can be activated to raise forward end 132 upward dumping the slurry from the tank.
[0048] Collection tank 14 may also include a vacuum switch and relay (not shown) that prevents the tank from being raised for dumping until the vacuum in the tank has dropped below a predetermined level for door 126 to be opened. Once the vacuum in the tank has diminished to below the predetermined level, tank 14 may be elevated for dumping. This prevents slurry from being pushed up into filter 116 if door 126 can not open.
[0049] It should be appreciated by those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope and spirit of the invention. It is intended that the present invention cover such modifications and variations as come within the scope and spirit of the appended claims and their equivalents. | A mobile digging and backfill system for removing and collecting material above a buried utility. The system comprises a mobile chassis, a collection tank mounted to the chassis, a water pump mounted to the chassis for delivering a pressurized liquid flow against the material for loosening the material at a location, a vacuum pump connected to the collection tank so that an air stream created by the vacuum pump draws the material and the fluid from the location into the collection tank, and at least one backfill reservoir mounted to the chassis for carrying backfill for placement at the location. | 4 |
FIELD OF THE INVENTION
The present invention relates to a water storage assembly and in particular to the storage of rainwater or grey water in a flexible bladder.
BACKGROUND OF THE INVENTION
Conservation of water has become a significant issue worldwide due to the reduction in rainfall, increase in population and salinity problems with existing water sources. These problems have increased the need to recycle and optimise use of existing water. For a household, the simplest way to reduce the quantity of mains water used is to collect rainwater in a tank. Water tanks capture rainwater at the point of use, for example, a dwelling, factory, school, building or the like. Unfortunately, due to an increased population and subsequent over development, adequate space in built-up areas to house water tanks is a significant problem. Further, with the growing focus on aesthetic looks of a dwelling or building, many people object to water tanks being visible.
The deficiencies of existing water tanks has led to the development of flexible water storage systems, such as that shown in WO 2004/053242. Flexible water storage systems are advantageous as they are more easily transportable when flat-packed than rigid tanks; relatively simple to construct on site; can be located in areas that are out of sight; in difficult access situations or where height restrictions exist (such as, under floors, decks or in walls) and complicated piping is generally not required.
However, the system of WO2004/053242 has been found to have practical installation and operation limitations. For example, the system uses a top fill method with a pivoting swing arm having o-rings as the method for sealing between the two arms. The o-rings have been found to leak after a period of time when the system is full. The swing arm also requires a significant space about it to operate correctly, thereby limiting the location in which the system can be installed and the potential capacity of the system as the fill potential fill height is limited by the presence of the filling mechanism. The o-rings have also been found to jam the swing arm mechanism in place thus preventing the system from filling to its full capacity.
Further, if a second reservoir is used, it is filled through a different inlet pipe from the primary reservoir. It is filled from the outlet pipe of the primary reservoir which in the case of WO2004/053242 is only a 32 millimeter pipe which restricts the flow. This has the potential to cause water to back up in the storm water downpipes because the primary reservoir is filling via a 90 mm pipe but only emptying to subsequent reservoirs via a 32 mm pipe. Still further, the system can not be installed by a home handyman.
Accordingly, there is a need to provide an efficient flexible water storage assembly to store rainwater or grey water which is easier to construct, install and operate is than existing systems, does not leak at junctions, will enable fixed pipe work to remain fixed without the risk of breaking from the weight or movement of the system, requires less maintenance and will fill several bladders more quickly and simultaneously and that can be filled via a 100 mm pipe or a 90 mm pipe. Further, there is a need for a flexible water storage assembly that can be installed by a home handyman.
OBJECT OF THE INVENTION
It is an object of the present invention to overcome or ameliorate one or more of the disadvantages of the prior art, or at least to provide a useful alternative.
SUMMARY OF THE INVENTION
The present invention provides a water storage assembly including:
a flexible bladder having a water storage cavity, said bladder being adapted to expand and contract upon flow of water into and out of said cavity,
one or more water inlets in fluid communication with said cavity,
one or more water outlets in fluid communication with said cavity,
a rigid frame adapted to support said bladder; and
one or more support slings having first and second ends, said first end being connected to said frame, and said second end being connected to said bladder, said sling being adapted to limit the movement of the bladder relative to the frame.
The water inlet and the water outlet are preferably mounted on a plate fixed relative to said frame.
The water inlet preferably includes an overflow adapted to direct water away from the bladder once the bladder is full.
The inlet is preferably positioned at approximately half of the vertical height of the bladder when full.
The water storage assembly preferably including a valve or number of valves adapted to isolate the flow of water through the bladder.
The water storage assembly preferably includes a plurality of said bladders.
The bladders are preferably connected to each other in parallel via the inlet pipes and the outlet pipes.
BRIEF DESCRIPTION OF THE DRAWINGS
A preferred form of the present invention will now be described by way of example only with reference to the accompanying drawings wherein:
FIG. 1 is a side elevational view of an assembly of an embodiment of the present invention, shown empty;
FIG. 2 is a side elevational view of FIG. 1 , shown full;
FIG. 3 is front elevational view of an assembly of an embodiment of the present invention, shown empty;
FIG. 4 is a front elevational view of FIG. 3 , shown full; and
FIG. 5 is a perspective view of a multiple bladder system of an embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the accompanying drawings, there is schematically depicted a water storage assembly 1 including a flexible bladder 5 having an internal cavity 6 permitting the storage of water or other liquids. An inlet duct 10 is connected to the cavity 6 within the bladder 5 . The inlet duct 10 may be 90 mm or 100 mm in diameter or another suitable size.
The inlet duct 10 permits the flow of water under the force gravity into the bladder 5 . One or more outlet ducts 15 are connected to the cavity 6 and are operable to dispense water from the cavity 6 to a user. The inlet duct 10 includes an overflow outlet 20 at some point within the inlet pipe which is operable to direct water away from the m bladder 5 when the bladder 5 is full. The overflow outlet 20 is located above the level of the bladder 5 , corresponding to the intended maximum fill volume of the bladder 5 . The overflow 20 may be positioned close to the bladder 5 or in fact some distance away, provided that the invert of the overflow is set to the maximum fill height of the bladder 5 .
A valve 25 is located on either the inlet duct 10 or outlet duct 15 and is operable to isolate the flow of water through the bladder 5 .
A rigid support frame 30 supports the bladder 5 . The frame 30 is in the form of a rectangular prism having an internal volume adapted to contain approximately half of the bladder 5 when full. The frame 30 in a preferred form is made from steel bars and may include several members or sub frames that can easily be assembled in restricted areas such as beneath floors.
The inlet pipe 10 and the outlet pipe 15 are connected to a fixed plate 7 which is secured to the frame 30 . The plate 7 ensures that the location and angular orientation of the pipes 10 , 15 does not change regardless of the position of the bladder 5 wall, or the amount of water contained therein.
The assembly 1 further includes one or more fabric slings 35 . All of the sides of the rigid frame 30 support the slings 35 . A first end of each fabric sling 35 is threaded in a loop around a portion of the frame 30 , and a second end of the sling 35 is connected to the bladder 5 . The sling 35 protects the bladder 5 from directly contacting the ground upon which the assembly 1 is located and provides protection from possible sharp objects that might harm the bladder. The sling 35 controls the expansion footprint of the bladder 5 , and also limits the movement of the bladder 5 relative to the frame, and hence influences the shape and internal volume of the bladder 5 during filling. The fabric sling 35 can be made from a geo-textile fabric or the like. The frame 30 and sling 35 secure the bladder 5 firmly in position, and keep the bladder 5 isolated relative to parts of the surrounding building, such as pylons or beams that could otherwise puncture or damage the bladder 5 .
The inlet duct 10 is connected to a rainwater or grey water collection system (not shown) or the like and utilises gravity, such that the water collection point is at a higher potential head (e.g. a gutter) relative to the inlet duct 10 of the bladder 5 . However, if necessary a pump 100 may be added to the assembly 1 . The assembly 1 may also be combined with other recycling devices utilising mains or grey water.
In the preferred form (and as best shown in FIG. 5 ) the assembly 1 includes two or more bladders 5 connected in parallel. The bladders 5 connected in parallel would be connected to the same inlet duct 10 and outlet duct 15 . However, the bladders 5 may be connected in parallel, series or any other configuration. In this case, two or more valves 25 may be utilised. The assembly 1 may also include a breather fitting 40 or the like. All the inlets and outlets may have some form of vector protection to prevent the ingress of insects such as mosquitos.
The bladders 5 are designed to be able to sit on uneven surfaces and may be folded or rolled to allow access through restricted entry points such as house sub-floor or wall areas. The inlet duct 10 is preferably a large diameter rainwater delivery pipe made from PVC. The inlet duct 10 allows the bladders 5 to fill simultaneously and efficiently during heavy water flow rates. This is important to ensure the maximum amount of rainwater is captured quickly with minimal loss of rainwater in large downpours.
The outlet duct is preferably a 32 mm PVC pipe, and there are preferably two outlet pipes connected to each bladder 5 . This will enable both the connection of multiple bladders and a pump, or alternatively a float chamber to measure when the water level is low when a mains water controller is then used to switch from stored rainwater or grey water to mains water.
In use, assembly 1 is connected to a liquid collection system of a dwelling or other building such as a rainwater collection system. Water (or another liquid to be stored) is gravity fed into the inlet duct 10 , filling the cavity within the flexible bladder 5 . As the bladder 5 expands the pressure on the water flowing through the duct 10 increases and once the bladder 5 is full, water travelling within the inlet duct 10 is forced out of the overflow 20 . Advantageously, there are no moving parts in the overflow 20 , the water pressure generated by the increase in potential head simply activates the overflow 20 as required. When two or more bladders 5 are placed in parallel (such as in FIG. 5 ) the water flowing by gravity from the rainwater collection system or the like flows through the inlet ducts 10 in parallel directly to the cavity within the bladders 5 . In this way, the flow is not be disrupted.
In the preferred form, the inlet duct 10 is manufactured of PVC piping or the like and is directly connected to the flexible expandable bladders 5 which will fill until the overflow 20 is reached. Alternatively flexible pipe might also be used. The overflow 20 can have a level which is adjustable by a user to enable the assembly 1 to be adapted for varying height restrictions when the assembly 1 is placed in a sub-floor installation. The overflow 20 would most likely direct the excess water to a stormwater dispersion pit or the like. The outlet 15 is preferably a threaded plastic pipe which delivers water to a pump 102 , simple dispersion system or the like.
The bladder 5 may be manufactured from two or more sheets of plastics material welded together to form a sealed unit or the like. It should also be noted that existing systems weld bladders together using a microwave process producing a non-continuous weld. The resultant bladder can leak due to weakness between the finish of one weld and the start of the next weld. The bladder is preferably fabricated using a “wedge” weld producing a continuous weld formed by passing the fabric edge over a heated wedge. One edge passes over the top and the other edge passes underneath. The edges are then compressed under a durable roller system or the like, producing a stronger weld than existing systems.
Though the assembly 1 has been discussed above in respect of a dwelling it should be understood that the assembly 1 can easily be used in any domestic, commercial or industrial application for water or any other liquid. The assembly 1 may also be used outside a dwelling and the fabric may be manufactured from a UV protected material or the like. Where the assembly 1 is installed outside a dwelling, and the critical function of the frame 30 may no longer be required to protect building structures from the expanding assembly 1 , a flexible reinforced fabric might be used without the inclusion of the frame 30 provided that the mounting plate 7 supporting the inlet 10 and the outlets 15 is still utilised to connect the pipe work to the flexible bladder 5 . The mounting plate 7 would also need to be suitably supported. As the assembly 1 can be significantly compact prior to use it can also be placed in hard to reach locations and expanded in situ. The assembly 1 advantageously fills more efficiently than existing systems, will not leak at junction points as all the pipe joins would be glued. The additional bladders 5 may fill more efficiently than existing systems.
The assembly 1 is very easy to install even by a home handyman and requires very little maintenance and repair due to the fact that it has no moving parts nor does the inlet pipe 10 need to set at a specific angle as it enters the bladder 5 . The assembly 1 on account of its simplicity is less likely to fail than existing systems, has far fewer parts and is easier to transport and much faster to install. Further, the inlet duct 10 and outlet duct 15 could be any type of pipe including flexible pipes. A flexible pipe requires less installation time and fewer plumbing parts as a flexible pipe can go around corners without the need for pipe elbows and other fittings.
Although the invention has been described with reference to specific examples, it will be appreciated by those skilled in the art that the invention may be embodied in many other forms. | A water storage assembly is disclosed including a flexible bladder having a water storage cavity, a water inlet in fluid communication with said cavity, a water outlet in fluid communication with said cavity, and a rigid frame adapted to support said bladder wherein said bladder wherein said bladder is secured to said rigid frame and said bladder is adapted to expand and contract upon flow of said water into and out of said cavity. | 8 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] The entire subject matter of both U.S. patent application Ser. No. 11/290,781 filed 1 Dec. 2005 and the US Continuation-in-part patent application Ser. No. 11/600,747 filed 17 Nov. 2006 is incorporated herein by reference.
FIELD OF INVENTION
[0002] The present invention relates to methods for producing a high lubricity fraction and for producing bioactive fractions from fats, oils and greases derived from a wide variety of animal and vegetable sources. In this specification, the terms “oils, fats and greases” are used synonymously to describe starting materials derived from vegetable and animal sources. Oils tend to be liquid at room temperature and are derived from many biological sources such as whales, fish and oil seed. Fats are generally solid at room temperature and are derived from the same sources as oils. Greases usually have high melting points and they may be synthetic products. Some synthetic greases are plant derived, others are from animals. The novel methods either separate lower lubricity components of the fat, oil, or grease from higher lubricity fractions or enrich the concentration of high lubricity components or combine extraction and enrichment. In a preferred embodiment the lower lubricity components are made volatile by chemical reactions that split the triglyceride component of fat, oil, or grease. These reactions may produce industrially useful products such as fatty acid methyl esters, fatty acids, fatty alcohols, fatty aldehydes or fatty amides of the original fat, oil, or grease which may be separated from the higher lubricity components by distillation. The lower lubricity components from fat splitting have inherent value that is not diminished by the separation of the high lubricity fraction. In fact, the low lubricity fraction may have increased value as a result of the separation. The high lubricity fraction is a collection of higher molecular weight substances present in the fat, oil or grease or a modified component thereof. In another preferred embodiment the high lubricity component of the fat, oil or grease is separated from the triglyceride by absorption onto a solid phase medium. Depending on the nature of the solid phase extraction medium either the lower lubricity components or the higher lubricity components are preferentially bound to the solid phase extraction medium. The concentrate is then recovered from the solid phase by extraction or from the liquid phase by evaporation. In a further preferred embodiment the separation of higher lubricity and lower lubricity components is achieved by crystallisation from a solvent.
[0003] In another embodiment of the present invention the novel methods separate triglyceride components of the fat, oil, or grease from biologically active fractions. The methods also enrich the concentration of biologically active components in a selective extraction process. In a preferred embodiment the glyceride components are made volatile by chemical reactions that split the oil triglyceride. These reactions may produce industrially useful products such as fatty acids, fatty acid esters, fatty alcohols, fatty aldehydes or fatty amides of the original vegetable oil which may be separated from the biologically active components by distillation. The distilled components from fat splitting have inherent value that is not diminished by the separation of the biologically active fraction. In fact, the distilled components may have increased value as a result of the separation. The biologically active fraction is a collection of higher molecular weight substances present in the starting material.
[0004] Extraction procedures may also be manipulated to improve the content of compounds that impart lubricity to the fat, oil or grease. In a preferred embodiment canola seed is mechanically pressed to remove oil that has lower levels of the desired high lubricity compounds. Mechanical extraction of the seed is followed by solvent extraction that produces oil with a surprising level of lubricity. The lubricity is imparted through the high ratio of lubricity enhancing products to triglyceride extracted with the oil.
[0005] Extraction procedures may also be manipulated to improve the content of biologically active compounds. In a preferred embodiment canola seed is mechanically pressed to remove oil that has lower levels of the desired biologically active compounds. Mechanical extraction of the seed is followed by solvent extraction of the solids in a process that produces oil with a surprising level of biologically active components.
[0006] Surprisingly it has also been discovered that specific fractions of oil-bearing material may be selected that possess higher levels of biologically active components. In a preferred embodiment small seed is selected prior to extraction to enable recovery of greater levels of the biologically active component. The invention includes the selection of these materials by physical and other methods.
BACKGROUND OF THE INVENTION
[0007] Since 1993, environmental legislation in the U.S. has required that the sulfur content of diesel fuel be less than 0.05%. In 2007 the sulfur content of diesel has been legislated to contain less than 15 ppm sulfur. The reduction in the sulfur content of diesel fuel has resulted in lubricity problems. It has become generally accepted that the reduction in sulfur is also accompanied by a reduction in polar oxygenated compounds and polycyclic aromatics including nitrogen-containing compounds responsible for the reduced boundary lubricating ability of severely refined (low sulfur) fuels. While low sulfur content is not in itself a lubricity problem, it has become the measure of the degree of refinement of the fuel and thus reflects the level of the removal of polar oxygenated compounds and polycyclic aromatics including nitrogen-containing compounds.
[0008] Low sulfur diesel fuels have been found to increase the sliding adhesive wear and fretting wear of pump components such as rollers, cam plate, coupling, lever joints and shaft drive journal bearings.
[0009] Concern for the environment has resulted in moves to significantly reduce the noxious components in emissions when fuel oils are burnt, particularly in engines such as diesel engines. Attempts are being made, for example, to minimize sulfur dioxide emissions by minimizing the sulfur content of fuel oils. Although typical diesel fuel oils have in the past contained 1% by weight or more of sulfur (expressed as elemental sulfur) it is now mandatory to reduce the sulfur content to less than 15 ppm (0.0015%).
[0010] Additional refining of fuel oils, necessary to achieve these low sulfur levels, often results in a reduction in the levels of polar components. In addition, refinery processes can reduce the level of polynuclear aromatic compounds present in such fuel oils.
[0011] Reducing the level of one or more of the sulfur, polynuclear aromatic or polar components of diesel fuel oil can reduce the ability of the oil to lubricate the injection system of the engine. As a result of poor fuel lubrication properties the fuel injection pump of the engine may fail relatively early in the life of an engine. Failure may occur in fuel injection systems such as high-pressure rotary distributors, in-line pumps and injectors. The problem of poor lubricity in diesel fuel oils is likely to be exacerbated by future engine developments, aimed at further reducing emissions, which will result in engines having more exacting lubricity requirements than present engines. For example, the advent of high-pressure unit injectors is anticipated to increase the fuel oil lubricity requirement.
[0012] Similarly, poor lubricity can lead to wear problems in other mechanical devices dependent for lubrication on the natural lubricity of fuel oil.
[0013] Lubricity additives for fuel oils have been described in the literature. WO 94/17160 describes an additive, which comprises an ester of a carboxylic acid and an alcohol, wherein the acid has from 2 to 50 carbon atoms and the alcohol has one or more carbon atoms. Glycerol monooleate is an example. Although general mixtures were contemplated, no specific mixtures of esters were disclosed.
[0014] U.S. Pat. No. 3,273,981 discloses a lubricity additive being a mixture of A+B wherein A is a polybasic acid, or a polybasic acid ester made by reacting the acid with C 1 -C 5 monohydric alcohols; while B is a partial ester of a polyhydric alcohol and a fatty acid, for example glyceryl monooleate, sorbitan monooleate or pentaerythitol monooleate. The mixture finds application in jet fuels.
[0015] U.S. Pat. No. 6,080,212 teaches of the use of two esters with different viscosity in diesel fuel to reduce smoke emissions and increase fuel lubricity. In one preferred embodiment of that invention methyl octadecenoate, a major component of biodiesel, was included in the formula. Similarly, U.S. Pat. No. 5,882,364 also describes a fuel composition comprising middle distillate fuel oil and two additional lubricating components. Those components being (a) an ester of an unsaturated monocarboxylic acid and a polyhydric alcohol and (b) an ester of a polyunsaturated monocarboxylic acid and a polyhydric alcohol having at least three hydroxy groups.
[0016] The approach of using a two component lubricity additive was pioneered in U.S. Pat. No. 4,920,691. The inventors describe an additive and a liquid hydrocarbon fuel composition consisting essentially of a fuel and a mixture of two straight chain carboxylic acid esters, one having a low molecular weight and the other having a higher molecular weight.
[0017] In U.S. Pat. No. 5,713,965 the synthesis of alkyl esters from animal fats, vegetable oils, rendered fats and restaurant grease is described. The resultant alkyl esters are reported to be useful as additives to automotive fuels and lubricants.
[0018] Alkyl esters of fatty acids derived from vegetable oleaginous seeds were recommended at rates between 100 to 10,000 ppm to enhance the lubricity of motor fuels in U.S. Pat. No. 5,599,358. Similarly a fuel composition was disclosed in U.S. Pat. No. 5,730,029 comprising low sulfur diesel fuel and esters from the transesterification of at least one animal fat or vegetable oil triglyceride.
[0019] Most commercially available plant oils are highly enriched in triacylglycerol and diacyl glycerols. However, as well as including these more abundant substances, plant oils are known to contain a large number of biologically active components. While the biologically active components may occur at concentrations sufficient to impart useful biological responses their concentrations are often insufficient for many applications.
[0020] Phytosterols are known by those skilled in the art as dietary materials that can lower blood serum cholesterol. In fact knowledge that dietary phytosterols decrease cholesterol extend back to 1951 (Peterson, Proc soc Exp Biol Med 1951; 78:1143). Jones et al. (Can J Physiol Pharmacol 1997; 75:217) reports that phytosterols are consumed at a level of 200-400 mg/day. However clinical effects described in many publications are significant when phytosterols or their esters are utilised at concentrations well above the natural concentrations found in vegetable oils. For example Shin et al. (Nutritional Research 2003; 23:489) provided human test subjects with a beverage containing 800 mg/serving and with 2-4 servings/day. The eight-week protocol significantly lowered cholesterol in the test population.
[0021] Sterols occur at significant concentrations in many vegetable oils mainly as free sterols and as their fatty esters. Nevertheless, the concentrations found in most sources are less than sufficient to produce a therapeutic effect.
[0022] Meguro et al. (Nutrition 2003; 19:670-675) report that diacylglycerols interact with sterol provided in the diet to reduce cholesterol levels in New Zealand White (NZW) rabbits below that achieved by the same content of sterol in triacyl glycerol. They hypothesise that the diacyl glycerol interacts with the sterol partially through the higher solubility of the sterol in the diacyl glyceride phase.
[0023] Dolichol is a naturally occurring high molecular weight alpha-saturated polyprenol that is widely distributed in living organisms. Mammals synthesise dolichol in normal metabolism but may take it up from the diet as well (Jacobsson et al. 1989; FEBS 255:32). U.S. Pat. No. 4,599,328 teaches that dolichol is an effective treatment for hyperuricuria, hyperlipemia, diabetes and hepatic disease. It has also been demonstrated in animal model systems that dolichol and dolichol phosphate can act as antihypertensive treatments (U.S. Pat. No. 4,175,139).
[0024] Polyisoprenol compounds are similar to dolichol in structure but serve a different function in metabolism. Polyisoprenol compounds are widely distributed and known to be components of many vegetable oils.
[0025] Tocols are an important class of nutrients and includes the essential nutrient vitamin E or alpha tocopherol. While vitamin E has a wide range of metabolic functions that are realised at low rates of incorporation in the diet supplementation with vitamin E is believed to have potential benefits in the prevention of ageing and disease. While vegetable oils are significant sources of vitamin E in the diet levels may be inadequate to meet recommended daily allowances and recommended levels for therapeutic effects.
[0026] Plant oils also contain chromanols including ubiquinone, ubiquinol, plastoquinone and plastoquinol. These compounds are potent antioxidants and are thought to slow ageing processes.
[0027] Carotenoids and notably lutein and zeazanthin are important constituents of certain vegetable oils. Consumption of these carotenoids has been associated with the prevention of specific eye diseases. For example, an inverse association has been noted with the incidence of advanced, neovascular, age-related macular degeneration (AMD) and the dietary intake of lutein and zeaxanthin. Individuals whose diets are modified to include an increased intake of lutein and zeaxanthin generally respond with an increase in concentrations in these pigments in their serum and maculae (Hammond et al. 1997; Invest. Opthamol. Vis. Sci. 38:1795).
[0028] Typically phytosterol and vitamin E are obtained from industrial streams encountered in the processing of plant based oils. A phytosterol and tocopherol rich fraction is recovered during the refining of vegetable oil where in a late stage of refining vegetable oil is steam distilled under vacuum to deodorise the oil. The deodoriser concentrate is rich in free fatty acid, free sterol and tocopherol and substantially devoid of sterol ester, dolichol, diacylglycerol and carotenoids. This fraction is a major source of sterol and tocopherol used in nutritional applications.
[0029] Phytosterol is also derived from the pulp and paper industry where solution from alkali washed wood pulp is acidified to produce a complex mixture of plant lipids known as tall oil. This latter fraction can be divided to produce fatty acids, rosin acids and sterols.
[0030] Carotenoids used for dietary purposes may be derived from a number of sources. For example, marigold may be harvested and processed as a source of dietary lutein. Other dietary carotenoids, including astaxanthin and canthaxanthin are synthesised by classical organic synthetic methods.
[0031] While vegetable oils may be rich sources of sterol esters, tocols, and carotenoids methods of recovery of these components are inefficient and products must be fractionated and reformulated for use.
SUMMARY OF THE INVENTION
[0032] It is known by those skilled in the art that fuel additives that enhance lubricity may be produced that contain lower alkyl esters of fats, oils and greases yet surprisingly it is revealed, in the present invention, that these mixtures contain ingredients with substantially higher lubricity. Furthermore methods are disclosed to efficiently recover these high lubricity components. In preferred methods the triglyceride components of the fat, grease or oil are converted to lower molecular weight compounds such as fatty acids, fatty amides or fatty acid alkyl esters. In forming the lower molecular weight compound it becomes possible to readily separate the bulk material from the high lubricity components by distillation. In a preferred embodiment the fat, oil or grease is transesterified to produce a lower alkyl ester using methods known to those skilled in the art. The ester is then distilled and recovered for other purposes and the column bottoms of distillation are recovered and refined to remove free acids formed in distillation. The refined column bottoms recovered from the distillation have substantial efficacy as lubricity additives. In a preferred embodiment the fat, oil or grease is converted to fatty acids. The fatty acids are then distilled and recovered for other purposes and the column bottoms of distillation are recovered and refined to remove residual free acids formed in distillation. The refined column bottoms also have substantial efficacy as lubricity additives. The lubricity concentrate comprises a complex mixture of phospholipid, sterol, tocol, quinone, polyisoprene and polyisoprenol and other lipid soluble components. In a preferred embodiment of the present invention where the concentrate is an enriched concentrate of lipid substances with molecular weights greater than 400.
[0033] While the present invention may be accomplished through fat splitting or other chemical modification followed by crystallisation or distillation as preferred methods of concentrating the lubricity fraction, other methods of concentrating specific classes of oil soluble compounds from triglyceride are also acceptable. For example, those skilled in the art will recognise that it is possible to recover enriched fractions from fats, oils and greases by solid phase extraction and chromatographic methods. Solid phase extraction may be combined with chemical modification steps or the chemical modification may be forgone in the process of preparing the high lubricity concentrates.
[0034] Furthermore we have made the surprising discovery that the method of processing the oil may also act to concentrate the oil soluble components that impart lubricity. Processing conditions may be modified to enhance the extraction of high lubricity minor components of oilseed and animal fat. The present invention includes pre-extraction treatments that enhance either or both the concentration of high lubricity components in oils.
[0035] In another preferred embodiment of the present invention where the concentrate is enriched in dolichol, other polyisoprenols and their derivatives, and the present invention describes methods of optimally preparing concentrates of biologically active oil soluble compounds. In the preferred art the triglyceride components of vegetable oils are subject to chemical rearrangements to form new products that have a lower molecular weight and boiling point. Reaction conditions are selected so as to prevent the degeneration of the biologically active components. It has been found that the process of distillation under mild conditions can remove much of the modified glyceride product leaving behind a concentrate of biologically active substances. As most plant oils are sources of carotenoid, phytosterol, tocol, chromanol, and dolichol and these components have relatively high molecular masses it is common to find these compounds present in the concentrate.
[0036] In a preferred embodiment ethyl esters were synthesised using an alkaline catalyst reaction of ethanol with low erucic acid rapeseed oil, a plant oil that is highly rich in triglyceride. In this embodiment the reaction conditions are maintained under the mildest possible conditions to prevent the destruction of the biologically active components. After the reaction the glycerol released in the reaction and excess ethanol were removed, the esters were distilled in a thin film still to recover over 90 percent of the ethyl ester as a concentrate. The resulting concentrate was highly enriched in phytosterol, tocol, dolichol and carotenoid.
[0037] The instant invention also includes methods of pre-extraction that produce enriched concentrates of biologically active compounds. In a preferred embodiment low erucic acid rapeseed was crushed mechanically using a commercial expeller press under mild conditions to recover an oil fraction that had reduced levels of biologically active components. The mild conditions of mechanical extraction are known to those skilled in the art as cold pressing. After mechanical extraction the solid fraction was subject to solvent extraction to recover the remaining oil. The second oil possessed elevated concentrations of many biologically active components including phytosterol, tocol, dolichol and carotenoid. Although the triglyceride remained a major component of the solvent extracted oil the concentration step allowed for the use of more efficient process steps in the production of a concentrate of biologically active components. It is a particular benefit of this latter preferred embodiment that the manufacturing process generates a significant fraction of oil that has not been extracted by utilising a solvent.
DETAILED DESCRIPTION OF THE INVENTION
[0038] Vegetable oils, such as tall, soybean, canola, palm, sunflower, hemp, rapeseed, flaxseed, corn or coconut, are a complex mixture of molecular components of which triglycerides are usually the most abundant component. Numerous other seed oils are known and are also included in this invention. Palm and olive oil are derived by processing the fruits of the palm and olive trees. Tall oil is a vegetable oil recovered from the pulp and paper industry and is essentially the oil present in wood. Similarly, animal fats and greases, such as those derived from swine, poultry and beef, are predominantly triglyceride in composition. Triglycerides are triesters of glycerol and carboxylic acids that have great industrial importance. In industry triglycerides are reacted with water to form fatty acids, hydrogen to form fatty alcohols, reducing agents to form aldehydes, amines to form fatty amides and alcohols to form alkyl esters. Triglycerides have relatively high molecular weights, usually greater than 800 amu and thus are difficult to distill. However, fatty acids, fatty amides, fatty alcohols and fatty alkyl esters of lower alcohols have lower molecular weights and are readily distilled under vacuum. The residue left after vacuum distillation is a concentrate of substances with molecular weights above those of the fatty acid, amide, alcohol, aldehyde or ester.
Preconcentration
[0039] The oilseeds are typically processed both by mechanical and solvent extraction to recover the seed oil. Mechanical extraction methods include hydraulically operated oil presses, continuous screw presses, and extruders adapted for oil extraction. Mechanical extraction methods mobilise a portion of the oil by both shear and pressure which ruptures oil containing structures in the seed. Once the oil is mobilised it may flow away from the solids which are held in the press by physical structures such as metal bars. Depending on the severity of the pressure, temperature and shear conditions the amount of oil recovered from oilseed varies. In order to maximise the yield of oil it is possible to utilise more severe extraction conditions. It is common to those skilled in the art to utilise expeller presses in sequence to first remove a portion of the oil under milder extraction conditions then to follow this by a second expeller press treatment under more severe conditions. It is an example of the current art where the total pressed oil is utilised for recovery of biologically active components. It is a preferred embodiment of the present invention that the oil recovered from the second oilseed press is utilised as a superior source for the biologically active materials. In advanced expeller press designs it is common to increase the severity of pressing of the oilseed material as it passes along the press. Oil recovered from the early portion of the press is extracted under milder conditions than material recovered from the latter stages of the press. Surprisingly it has been found that the level of biologically active oil soluble ingredients is enriched in the oil recovered in the latter stages of pressing. It is a preferred embodiment of the present invention that the oil recovered from the latter stages of a press is recovered and utilised for extraction of the biologically active fraction. It is also common practise in industry to utilise an expeller press to remove a portion of the oil followed by placing the partially deoiled seed meal in a continuous or batch solvent extraction vessel. The seed meal may then be fully deoiled by extracting with a suitable non-polar solvent. Useful solvents include but are not limited to hexane, supercritical carbon dioxide, propane, ethanol, isopropanol and acetone. It is an embodiment of the present invention that oil recovered by solvent extraction, following mechanical removal of the oil is utilised as a superior source of the biologically active materials.
Molecular Weight Reduction: Transesterification
[0040] Once the oil has been separated, it is an object of the current invention to produce a useful concentrate of the biologically active fraction. In order to concentrate the biologically active molecules it is necessary to separate them from the higher molecular weight and often less biologically active triglyceride materials as they may constitute over 95 percent of the seed oil. Typical seed oil glycerides have molecular masses of greater than 800 g/mole. As such these compounds are difficult to distill. In the current art to achieve this separation it is necessary to convert the triglyceride oils to lower molecular weight forms so that they are readily distilled to leave a residue of the biologically active concentrate.
[0041] Glycerides are esters of glycerol and they are readily reacted to produce fatty compounds that have lower molecular weight than the parent glyceride. In a preferred embodiment of the current invention the glyceride component of the seed oil is converted to fatty acid esters. There are many documented approaches to the chemical conversion of triglycerides to alkyl esters known by those skilled in the art and such approaches other than those described herein are included in the instant invention. In a preferred embodiment vegetable oil that contains biologically active compounds is treated with a solution of an alkali base, such as potassium hydroxide dissolved in ethanol under anhydrous conditions. The ensuing reaction converts the triglyceride to the corresponding ethyl ester. After conversion, the molecular weight of the fatty ester compounds is substantially reduced while the biologically active components with higher molecular weights are not similarly reduced in molecular mass. Distillation will selectively remove the fatty ester compounds and leave a unique residue of biologically active materials with higher molecular weights. While the use of distillation is preferred for separation of the alkyl ester component of the reaction it is obvious to one skilled in the art that other methods of separating molecules that differ in size that could be used to separate the alkyl esters from the biologically active fraction. These methods are included in the present invention. As the products of the current invention may be produced using ethanol, the use of other lower alkanols with between 1 and 5 carbon atoms is included as a portion of the current art.
Molecular Weight Reduction: Hydrolysis
[0042] In a preferred embodiment of the current invention the glyceride component of the seed oil is converted to fatty acids. There are many documented approaches to the chemical conversion of triglycerides to fatty acids known to those skilled in the art and such approaches other than those described herein are included in the instant invention. In a preferred embodiment vegetable oil that contains biologically active compounds is treated with water and a suitable catalyst. The ensuing reaction converts the triglyceride to the corresponding fatty acids. After the conversion the molecular weight of the fatty acid compounds is substantially reduced while the biologically active components with higher molecular weights are not similarly reduced in molecular mass. Distillation will selectively remove the fatty acid compounds and leave a unique residue of biologically active materials with higher molecular weights. While the use of distillation is preferred for separation of the fatty acid component of the reaction it is obvious to one skilled in the art that other methods of separating molecules that differ in size that could be used to separate the fatty acids from the biologically active fraction. These methods are included in the present invention. The products of the current invention may be produced using enzymatic, organic and mineral catalysts and as these catalysts are known to those skilled in the art of lipid chemistry they are included as a portion of the current art.
Molecular Weight Reduction: Saponification
[0043] In a preferred embodiment of the present invention the glyceride component of the seed oil is converted to soaps which may be acidulated to release fatty acids. There are many documented approaches to the chemical conversion of triglycerides to soaps known by those skilled in the art and such approaches other than those described herein are included in the present invention. In a preferred embodiment vegetable oil that contains biologically active compounds is treated with water and a suitable base. The ensuing reaction converts the triglyceride to the corresponding soap. After the conversion the soaps may be converted by the addition of a suitable acid to yield a solution of fatty acids and the biologically active fraction. The molecular weight of the fatty acid compounds is substantially reduced while the biologically active components with higher molecular weights are not similarly reduced in molecular mass. Distillation will selectively remove the fatty acid compounds and leave a unique residue of biologically active materials with higher molecular weights. While the use of distillation is preferred for separation of the fatty acid component of the reaction it is obvious to one skilled in the art that other methods of separating molecules that differ in size could be used to separate the fatty acids from the biologically active fraction. These methods are included in the instant invention. The products of the current invention may be produced using a wide range of alkali materials known to those skilled in the art of lipid chemistry; the use of these materials is included as a portion of the current art.
Molecular Weight Reduction: Reduction
[0044] In a preferred embodiment of the current invention the glyceride component of the seed oil is converted to fatty alcohols. There are many documented approaches to the chemical conversion of triglycerides to fatty alcohols known by those skilled in the art and such approaches other than those described herein are included in the instant invention. In a preferred embodiment vegetable oil that contains biologically active compounds is treated with metallic potassium in butanol. The ensuing reaction converts the triglyceride to the corresponding alkanol. The molecular weight of the fatty alcohol compounds is substantially reduced while the biologically active components with higher molecular weights are not similarly reduced in molecular mass. Distillation will selectively remove the fatty alcohol compounds and leave a unique residue of biologically active materials with higher molecular weights. While the use of distillation is preferred for separation of the fatty alcohol component of the reaction it is obvious to one skilled in the art that other methods of separating molecules that differ in size could be used to separate the fatty alcohols from the biologically active fraction. These methods are included in the present invention. The products of the current invention may be produced using other alkali metals and by other reactions known to those skilled in the art of lipid chemistry; the use of these reactants and catalysts is included in the present invention.
Distillation
[0045] Wide ranges of distillation processes are known to those skilled in the art of lipid chemistry. It is known that lipid molecules are sensitive to damage by exposure to high temperatures encountered in distillation and as such distillation processes that minimise temperature exposure are preferred. Vacuum speeds distillation and minimises exposure to heat. Stills that operate under vacuum are thus preferred. Examples of preferred processes also include continuous distillation methods including but not limited to molecular distillation, thin film distillation and other short path and continuous distillation processes.
Size Exclusion Chromatography
[0046] It is also possible to separate compounds utilising size exclusion chromatography. In a preferred method higher molecular weight biologically active compounds are separated from lower molecular weight fatty compounds by passage over suitable size exclusion media. Examples of suitable media include but are not restricted to Sephadex LH-20 and Styragel GPC.
Measurement of Carotenoid
[0047] Carotenoids can be measured in whole vegetable oil and in concentrates by the presence of specific peaks in the visible range of the spectrum using a suitable spectrophotometer. The carotenoid content can be estimated utilising a standard curve prepared from a pure standard. Carotenoids were estimated on the basis of either beta carotene or lutein standards.
Measurement of Sterol
[0048] Sterol content was determined by non-destructive NMR analysis. In this procedure the oil or biologically active concentrate was dissolved in deuterated chloroform and the proton spectrum was recorded using a 400 MHz Bruker Spectrospin spectrometry. Based on standard curves established on solutions of phytosterol free esters and cholesterol it was determined that spectrometry could reliably determine the concentration of sterols in vegetable oil samples.
[0049] GC-FID and GC-MS was used to determine sterol concentration in fatty acids and esters.
Measurement of Tocopherol
[0050] GC-FID and GC-MS was used to determine tocopherol concentration in fatty acids and esters.
Measurement of Squalene
[0051] GC-FID and GC-MS was used to determine squalene concentration in fatty acids and esters.
Measurement of Dolichol
[0052] LC-MS was used to determine the presence of dolichol in fatty acid, ester and
Lubricity Measurements:
Laboratory Method:
[0053] Lubricity is measured using a Munson Roller On Cylinder Lubricity Evaluator (M-ROCLE; Munson, J. W., Hertz, P. B., Dalai, A. K. and Reaney, M. J. T. Lubricity survey of low-level biodiesel fuel additives using the “Munson ROCLE” bench test, SAE paper 1999-01-3590). The M-ROCLE test apparatus conditions are given in Table 1. During the test, the reaction torque was proportional to the friction force produced by the rubbing surfaces and was recorded by a computer data acquisition system. The recorded reaction torque was used to calculate the coefficient of friction with the test fuel. The image of each wear scar produced on the test roller was captured by a video camera mounted on a microscope and was transferred to image processing software, from which the wear scar area was measured. After determining the unlubricated Hertzian contact stress, a dimensionless lubricity number (LN), indicating the lubricating property of the test fuel, was determined using the following equation:
[0000] LN=φ ss /φ H φ ss ; φ ss =P/A
[0054] Where:
[0000] φ ss =steady state ROCLE contact stress (mPa);
φ H =Hertzian theoretical elastic contact stress (mPa);
[0055] Kerosene Reference Fuel was Escort Brand 1-K Triple Filtered, Low Sulfur, Canadian Tire Stock No. 76-2141-2, Lot 135, BO2943. Each fuel ester sample was lubricity tested six times on the machine followed by a calibration of the reaction torque.
[0000]
TABLE 1
M-ROCLE TEST CONDITIONS
Fuel temperature, ° C.
25 ± 1.5
Fuel capacity, mL
63
Ambient temperature, ° C.
24 ± 1.0
Ambient humidity, %
35-45
Applied load, N
24.6
Load application velocity, mm/s
0.25
Test duration, min
3
Race rotational velocity, rpm
600
Race Surface velocity, m/s
1.10
Test specimens
Falex test cylinder, F-S25 test rings, SAE 4620 steel
Outer diameter, mm
35.0
Width, mm
8.5
Falex tapered test rollers, F-15500, SAE 4719 steel
Outer diameter, mm
10.18, 10.74
Width, mm
14.80
Field Test Method:
[0056] Motor oil analysis was utilized to infer engine wear. This involved high-resolution Inductively Coupled Plasma (ICP) Spectrometry analysis of the used oil wear particles and oil additive elements. Ferrography, and magnetic particle analysis was determined for larger (>5 μm) wear particles. Physical and chemical analyses of oil viscosity, acid neutralizing-ability (Total Base Number (TBN) and Total Acid Number (TAN)), and any dilution by fuel, water, or glycol was also monitored. An independent laboratory, Fluid Life Corporation in Edmonton Alberta, conducted these analytical tests.
[0057] All motor oil analysis data was adjusted to calculate true wear rates considering oil volumes present in the crankcase, oil consumed, sample volumes, and oil additions. All wear metals were monitored, with engine wear iron examined most critically. As well, by sectioning the filters after each oil change, filter wear and contaminant particles were microscopically and spectrographically compared. Field test logs indicating daily ambient minimum and maximum temperatures, numbers of cold and hot starts, ratios of city to highway driving, and liters of fuel consumed were tabulated. Consistent driving styles were enforced. Fuel economy and any operational difficulties were noted throughout the test program. Esso brand regular unleaded gasoline and Pennzoil Multigrade SJ motor oils were used throughout the study. The canola additives were prepared or obtained as described in specific examples.
Calculation of True Wear Rate
[0058] Consider for example, a vehicle engine that operates “normally” or “ideally”, generating and depositing in the crankcase oil a constant 10 parts per million (10 ppm) of iron (Fe) in every 1,000 km of operation. Its “true wear rate” would be calculated by dividing the particle count by the distance traveled, yielding 10 ppm/1,000 km. Here, round numbers have been used to assist the reader in understanding the procedure. If the vehicle were operated for 10,000 km under uniform conditions the wear iron level would rise 10 fold to 100 ppm Fe. This rise in ppm could start from zero ppm for an initially “flushed clean” engine, or more often from some initial “reference” level, taken shortly after an oil change. A typical oil and filter change typically leaves 10% to 15% of the used oil behind, so referencing is an important initial first step in a comparative engine wear analysis.
[0059] If the crankcase capacity of the example engine is 10 L, the amount of elemental iron deposited in the oil after 10,000 km can be calculated as follows:
[0060] The 100 ppm Fe is present in the 10 L crankcase volume.
[0061] Therefore the iron wear volume is obtained by multiplying the iron concentration by the oil volume:
[0000] 100 parts Fe(10 6 )×10 L=1,000 μL Fe.
[0062] This 1,000 μL Fe is the engine wear volume under ideal 10,000 km conditions.
[0063] If the engine oil was referenced at, say 70 km, and found to contain 10 ppm Fe, this would cause the final test reading after the 10,000 km to be 10 ppm higher:
[0000] 100 ppm+10 ppm=110 ppm.
[0064] So to correct for initial residual iron one must subtract the reference ppm from the final test ppm, to obtain the “net” wear iron, which in this case is still:
[0000] 110 ppm−10 ppm 100 ppm.
[0065] Oil sampling itself requires a small amount of oil (˜200 mL) to be withdrawn from the crankcase each time the wear metals are monitored.
[0066] Assume 5 oil samples of 0.2 L=1.0 L of oil was removed during the 10,000 km run.
[0067] The average net ppm Fe concentrations in these 5 samples would be close to the average net crankcase concentration of 50 ppm, which started at 0 ppm and ended at 100 ppm. This oil sampling has caused two things to happen:
[0000] (a) There is now 1.0 L less oil in the 10.0 L crankcase due to the sampling, i.e. 9.0 L.
(b) 1.0 L of oil containing, on net average, ˜50 ppm Fe has been removed.
[0068] The indicated final net test value would no longer equal 100 ppm Fe but can be calculated by doing a wear iron balance on the removal of iron activity as follows:
[0000] (100 ppm×10 L)−(50 ppm×1 L)=Test Fe ppm×9 L,
[0069] Solving for the Test Iron level in ppm, we obtain:
[0000] Test ppm=(1000 μL Fe−50 μL Fe)/9 L,
[0000] Test ppm=950 μL/9 L=105.5 ppm Fe.
[0070] Due to sampling the “wear rate” based on the final test value of 105.5 ppm Fe, instead of the true net previous 100.0 ppm value, would be calculated in error as too high at:
[0000] 105.5 ppm Fe/10,000 km, or, 10.55 ppm Fe/1000 km.
[0071] To compensate for sampling, “adding back” the oil sample volumes with new oil, each time a sample was taken, could be tried. New oil may contain small levels of wear metals (0.0-2.0 ppm Fe) and high levels of additive metals (800-1200 ppm Zn).
[0072] Focusing, for now, on the iron, we can do another iron balance taking into account the 1.0 L sampling volumes and the 1.0 L add-back volumes (at 1 ppm Fe for new oil) as follows, starting with the previous true wear iron level:
[0000] (100 ppm×10 L)−(50 ppm×1 L)+(1 ppm×1 L)=Test ppm×10 L (Eq. 1)
[0000] Test ppm=(1000 μL Fe−50 μL Fe+1 μL)/10 L
[0000] Test ppm=951/10=95.1 ppm Fe
[0073] After taking samples, and adding oil back, the indicated wear rate result based on the final sample is now too low, at 95.1 ppm Fe/10,000 km or 9.51 ppm Fe/1000 km.
[0074] If an engine “uses” oil, this volume will be similar to us taking out oil samples.
[0075] If the oil is “topped-up” to the full mark, this is like adding back new oil after sampling.
[0076] If the crankcase ends up below or above “full”, this can also be taken into account with reference to the previous two examples.
[0077] It is desired to calculate the “true ppm” based on a “test ppm” wear indication.
[0078] In more general terms the previous iron balance (Eq. 1) can be rewritten as follows:
[0000]
(
True
ppm
×
Start
L
)
-
(
True
ppm
×
Used
L
/
2
)
+
(
New
ppm
×
Add
L
)
=
Test
ppm
×
Test
L
True
ppm
=
(
Test
ppm
×
Test
L
)
+
(
True
ppm
×
Used
L
/
2
)
-
(
New
ppm
×
Add
L
)
Start
L
(
Eq
.
2
)
[0079] For True ppm, we can approximate the True ppm in the second term of (Eq. 2) equal the Test ppm, to get (Eq. 3):
[0000]
True
ppm
=
(
Test
ppm
×
Test
L
)
+
(
Test
ppm
×
Used
L
/
2
)
-
(
New
ppm
×
Add
L
)
Start
L
(
Eq
.
3
)
[0080] Using the Test 95.1 ppm value from the example above, and substituting into (Eq. 3), yields a reasonably good True Fe value, close to the known 100.0 ppm, as:
[0000]
True
Fe
ppm
=
(
95.1
ppm
×
10
L
)
+
(
95.1
ppm
×
1
L
/
2
)
-
(
1
ppm
×
1
L
)
10
L
=
99.75
ppm
[0081] If a higher accuracy is required this 99.75 ppm value can be substituted for the Test ppm yielding:
[0000]
True
Fe
ppm
=
(
95.1
ppm
×
10
L
)
+
(
99.75
ppm
×
1
L
/
2
)
-
(
1
ppm
×
1
L
)
10
L
=
99.99
ppm
[0082] Therefore the following, repeated, Equation 3 can be used to calculate “True Wear” or “Normalize” indicated lubricant test results based on oil volumes used or sampled, crankcase capacity, new oil added, or any combination of the above:
[0000]
True
ppm
=
(
Test
ppm
×
Test
L
)
+
(
Test
ppm
×
Used
L
/
2
)
-
(
New
ppm
×
Add
L
)
Start
L
(
Eq
.
3
)
EXAMPLES
Example 1
Two Stage Transesterification of Canola Oil with Methanol and Potassium Hydroxide
[0083] Methyl esters of canola oil, also known to those skilled in the art as low erucic acid rapeseed oil, were prepared using a two-stage base catalysed transesterification. The two-stage reaction was required to remove glyceride from the final product. Prior to the reaction the catalyst was prepared by dissolving potassium hydroxide (10 g) in methanol (100 g). The catalyst solution was divided into two 55 g fractions and one fraction was added to 500 g of canola oil (purchased from a local grocery store) in a 1 L beaker. The oil, catalyst and methanol were covered and stirred vigorously for 1 hour on a stirring hot plate by the addition of a teflon stirring bar. After stirring, the contents of the beaker were allowed to settle for 2 hours. At this time a cloudy upper layer and a viscous lower layer had separated. The layers were separated using a seperatory funnel and the upper layer was mixed with the remaining potassium hydroxide in methanol solution. This second mixture was stirred vigorously in a covered beaker for 1 hour and allowed to settle overnight. The mixture settled to form two layers. The upper layer was collected using a seperatory funnel and used for further refining steps.
Example 2
Two Stage Transesterification of Tallow with Methanol and Potassium Hydroxide
[0084] Tallow was collected from a renderer. Five hundred grams of tallow were heated to 40° C. prior to esterification to liquify the solid mass. Thereafter, all processes and conditions were identical to those described in example 1.
Example 3
Refining and Distillation of Canola Oil Methyl Ester
[0085] Canola methyl ester prepared in example 1 was refined to remove methanol, glycerol, soaps and other compounds that might interfere with distillation. Methanol was removed under vacuum (28.5″) by a rotary vacuum evaporator equipped with a condenser. The methyl esters were maintained at 50° C. for 30 minutes to thoroughly remove alcohol. After evaporation the esters were treated with silica (0.25% w/w Trisyl 600; W.R. Grace Co.) and stirred at room temperature for 1 hour. After silica treatment methyl esters were filtered over a bed of Celite to remove both silica and other materials.
[0086] After refining the methyl esters, fractional high vacuum distillation was performed using a simple distillation apparatus. A vacuum of less than 1 mm was maintained throughout the procedure. During fractionation temperatures at the top of the column, before the condenser, were between 120° C. and 140° C. The distillation apparatus included a liquid nitrogen cooled vapour trap, which allowed the attainment of high vacuum conditions. Approximately 500 mL of distillate (about half the sample) was obtained and then the heating mantle was removed while maintaining the apparatus under vacuum. Vacuum was then broken and fractions of both distillate and bottoms were obtained for further studies. Distillation was then resumed until a further 200 mL of distillate were obtained (about half the sample). The apparatus was again chilled, vacuum was broken and samples of 100 mL of both bottoms and distillate were recovered. All samples of bottoms and distillate were analysed to determine the content of soaps and free fatty acids using AOCS methods Cc 17-95 and Ca 5a-40 respectively.
[0087] Some samples of column bottoms were noted to have elevated levels of free fatty acids. These samples were treated by briefly contacting with a mixture of 1 molar potassium hydroxide dissolved in glycerol to convert the fatty acids to soaps. The glycerol phase was easily separated from the oil phase by decanting. Following alkaline glycerol treatment silica (0.25% w/w Trisyl 600) and was added to the oil phase and the phase was filtered over a bed of celite.
Example 4
Refining and Distillation of Tallow Methyl Ester
[0088] Tallow esters were refined and distilled as described for rapeseed esters in Example 3.
Example 5
Lubricity Testing of Methyl Canola and Tallow Esters
[0089] Lubricity was measured using a Munson Roller On Cylinder Lubricity Evaluator (M-ROCLE; Munson, J. W., Hertz, P. B., Dalai, A. K. and Reaney, M. J. T. Lubricity survey of low-level biodiesel fuel additives using the “Munson ROCLE” bench test, SAE paper 1999-01-3590). The M-ROCLE test apparatus conditions are given in Table 1. M-ROCLE operation and equations used to describe lubricity number are described above. Table 2 describes the samples subjected to analysis.
[0090] Lubricity testing was performed on the first distillate and column bottoms, which constituted about a four-fold concentrate of high boiling substances. A total of 6 replications were performed to allow for statistical analysis. All tests were performed on a 1% solution of concentrate or distillate in kerosene. Table 3 contains the results of analyses.
[0091] In testing it was found that kerosene produced the lowest lubricity number and that all treatments increased lubricity number with respect to controls. Among the treated samples the concentrates consistently demonstrated the highest lubricity numbers. The lubricity numbers for concentrates of canola and the two tallow samples were not significantly different from each other and in all cases the concentrates had greater lubricity than the distillates. The lubricity numbers noted for the distillates were lower than the concentrates, though higher than controls, indicating that only half of the improvement in lubricity number was contributed by the distilled methyl ester. In the two tallow samples it was found that prior to distillation the lubricity number was similar to the lubricity number for the concentrate.
[0092] Uniformly it was found that all treatments also decreased wear scar area. Surprisingly it was found that although distilled methyl esters significantly decreased wear scar area concentrates produced the lowest wear scar areas. For example, tallow 1 methyl ester (sample number 4) produced a wear scar area of 0.2410 mm 2 while the distillate and concentrate of this sample produced wear scars of 0.2763 mm 2 and 0.2446 mm 2 respectively (Table 3).
[0093] It was discovered that the treatments had little impact on the coefficient of friction in the current test.
[0000]
TABLE 2
Description of refining and distillation conditions
used to prepare lubricity enhanced concentrates
All additive samples were Trisyl treated and Celite
Bottle
Filtered Methyl Esters
Sample
Base Material
Fatty
Bottle
#
for Methyl Ester
Acid %
Wt. gr.
#1
Canola Oil
0.04%
104
#2
Canola Oil
0.07%
105
Distillate
#3
Canola Oil
0.07%
84
Concentrate
#4
Tallow 1
0.07%
93
#5
Tallow 1
0.07%
96
Distillate
#6
Tallow 1
0.10%
90
Concentrate
#7
Tallow 2
0.03%
88
#8
Tallow 2
0.06%
84
Distillate
#9
Tallow 2
0.07%
98
Concentrate
[0000]
TABLE 3
Wear Scar
Lubricity
Area
Standard
Coefficient
Sample
Number
Standard
(mm{circumflex over ( )}2)
Deviation
of Friction
Standard
number*
(n = 6)
Deviation
(n = 6)
[mm{circumflex over ( )}2]
(n = 6)
Deviation
Kerosene
0.7547
0.0778
0.3195
0.0238
0.1142
0.0050
#1
0.8620
0.0579
0.2907
0.0029
0.1210
0.0034
#2
0.8341
0.0484
0.2783
0.0183
0.1095
0.0017
#3
0.9464
0.0706
0.2557
0.0121
0.1180
0.0022
#4
0.9561
0.0552
0.2410
0.0222
0.1136
0.0022
#5
0.8373
0.0352
0.2763
0.0120
0.1189
0.0020
#6
0.9625
0.0456
0.2446
0.0102
0.1183
0.0019
#7
0.9348
0.0438
0.2623
0.0113
0.1163
0.0023
#8
0.8513
0.0492
0.2723
0.0092
0.1116
0.0013
#9
0.9555
0.0712
0.2547
0.0162
0.1182
0.0009
*number corresponds to sample number in table 2
Example 6
Impact of Oil Extraction and Refining Procedures on the Lubricity of Canola Oil
[0094] Approximately twenty kg (20.8) of canola seed was crushed in a Komet expeller press through a 6 mm die face producing 7.9 kg of oil with fines and 12.8 kg of meal. The oil was clarified by passing over glass wool followed by centrifugation at 2000×g for 15 min in a swing out rotor. The mass of the clarified oil was 7.2 kg. This oil was identified as pressed and unrefined or P-0. The meal arising from pressing was extracted with hexane in 1.4 kg batches in a soxhlet extractor. The hexane was collected and evaporated in a rotary evaporator producing 1.5 kg of solvent extracted oil. This oil is identified as solvent extracted and unrefined or S-0. The combined oil yield from the two processes was 42% of the original seed mass. The two samples of oil were used for further processing and analysis. Blending the crushed and solvent extracted oils at a ratio of 5:1 produced the third sample. This oil is identified as pressed, solvent extracted and unrefined or PS-0.
[0095] All oil samples were analyzed to determine the level of sterols (NMR), free fatty acids (AOCS Ca 5a-40), minerals (ICP) and lubricity (Munson ROCLE).
[0096] Oils (P-0, S-0 and PS-0) were degummed by adding 0.2% by weight of fifty percent citric acid to the oil while heating to 40-45° C. for 30 minutes with agitation. After reaction with the acid an additional of 2% of water (w/w) was added. The water treated oils were then heated to 60-70° C. for a further 20 minutes then centrifuged (2,000×g for 15 minutes). The upper layer of clear oil was recovered and analyzed to determine FFA, minerals and lubricity. Degumming produced three oil products: pressed degummed oil, P-1; solvent extracted degummed oil, S-1; and pressed and solvent extracted degummed oil PS-1
[0097] Approximately 300 g of each oil (P-1, S-1 and PS-1) was neutralized or alkali refined, for further analyses and processing. Alkali refining was achieved by adding a solution of 10% (w/w) sodium hydroxide to the degummed oil. The free fatty acid level was used to determine the stoichiometric amount of sodium hydroxide solution required for neutralization with a small excess. Neutralization was accomplished at 60-70° C. with a reaction time of 5 minutes with agitation. After neutralization the oil and soap water solution were separated by centrifugation (2,000×g for 15 minutes). The oil had a cloudy appearance. Evaporation of the cloudy oil produced clear oil that was analyzed for FFA, minerals and lubricity. Neutralization produced three oil products: Pressed neutralized oil, P-2; solvent extracted neutralized oil, S-2; and pressed and solvent extracted neutralized oil PS-2.
[0098] The alkali refined, neutralized oils (P-2, S-2 and PS-2) were bleached by the addition of 1% (w/w) bleaching clay to oil that had been preheated to 110° C. under vacuum. The oil was agitated in the presence of the bleaching clay for 30 min after which the temperature was allowed to fall to 60° C. prior to release of the vacuum. The oil and clay were then filtered through a bed of celite and Whatman No. 1 filter paper in a Buchner funnel. The filtered oil was analyzed to determine FFA, minerals and lubricity. Bleaching produced three oil products: Pressed bleached oil, P-3; solvent extracted bleached oil, S-3; and pressed and solvent extracted bleached oil PS-3.
[0099] In the final stage of processing the oils (P-3, S-3 and PS-3) were deodorized by passage through a 2.0 inch diameter Pope wiped film still. The still was adjusted to deliver oil at 2 mL/min, evaporation temperature was 170° C. and vacuum was 10 −2 mbar. Deodorizing produced three oil products: Pressed deodorized oil, P-4; solvent extracted deodorized oil, S-3; and pressed and solvent extracted deodorized oil PS-3.
[0100] Sterol is observed as a peak at 0.66 ppm in the proton spectrum. The peak is small but may be quantified with a sufficiently powerful spectrometer. The level of sterol in the solvent extracted portion of the oil is approximately the level found in the pressed oil (Table 4). With the exception of deodorizing treatments none of the refining steps affected the measured level of sterol.
[0101] Nine different mineral elements are observed in the ICP data including silicon, sodium, potassium, iron, boron, phosphorous, zinc, calcium, and magnesium. The amounts of most minerals are higher in solvent extracted oils than the pressed oil. Refining tends to remove minerals but its effect is different among the three samples. Degumming reduced the phosphorous content of pressed oil from 8 to 4 ppm (P-0 vs P-1) and from 168 to 57 ppm in the mixed oil (PS-0 vs. PS-1) but had no effect on the level of phosphorous (1030 ppm) in the solvent extracted oil (S-0 vs. S-1). Upon completion of all refining steps the pressed oil was virtually devoid of all mineral contamination showing only traces of tin (1 ppm, probably spurious) and silicon (7 ppm). Refining similarly improved the quality of the mixed oil (PS-4) where only traces of silicon, phosphorous, calcium and magnesium (3, 2, 2 and 2 ppm respectively) were observed. Full refining was not useful in removing materials from the solvent extracted oil where silicon, sodium, phosphorous, calcium and magnesium were observed at appreciable levels (10, 41, 197, 225 and 69 ppm respectively). Trace levels of potassium and lead were reported but the latter measurement was likely spurious instrument noise.
[0102] The effect of the three oils at all stages of refining on kerosene lubricity was evaluated by preparing a 1% (w/w) solution in kerosene and testing in a Munson Roller On Cylinder Lubricity Evaluator to determine the coefficient of friction and wear scar area. Lubricity number (LN) was calculated from the two numbers. Wear scar area was greatly reduced by all treatments. Several differences were observed among treatments but generally the size of differences among treatments was much smaller than the difference between untreated kerosene and the individual treatments. Wear scar area was for all three unrefined oils from all treatments. Degumming resulted in oils that produced a larger wear scar. Other refining treatments did not affect wear scar significantly.
[0103] All treatments lowered the coefficient of friction but substantial differences among treatments were observed. Alkali refined oils that had a greater coefficient of friction in all cases while bleaching reduced friction coefficients only for solvent extracted oil (S and PS, Table 4). Deodorizing also increased the coefficient of friction for the two solvent extracted oils. On average the coefficient of friction was lowest in oils containing the solvent extracted components.
[0104] Lubricity number reflects the effect of the oil on both wear scar and coefficient of friction. All oils regardless of the treatment increase the lubricity number. The solvent extracted oil provided the greatest increase in lubricity number over the blended and pressed oil types. Refining does not appear to affect the LN of pressed oil while it does result in interesting changes in the LN of the solvent extracted fractions. In the solvent extracted oils it is seen that degumming the oil lowers LN. Alkali refining has little additional affect on LN but bleaching appears to restore the LN though not to the levels observed in unrefined oil. Deodorizing lowers LN in the solvent extracted and the blend oils.
[0000]
TABLE 4
Effect of oil refining on select metal component concentrations and lubricity factors
wear
FFA
Si
Na
K
B
P
Zn
Ca
Mg
Sterol
scar
(%)
(PPM)
(PPM)
(PPM)
(PPM)
(PPM)
(PPM)
(PPM)
(PPM)
(NMR)
(μM 2 )
C of F*
LN
P**-0***
1.244
0
0
1
1
8
1
12
3
0.024
0.2634
0.1270
0.8193
P-1
1.231
1
1
0
3
4
0
1
1
0.021
0.2732
0.1179
0.8507
P-2
0.084
1
7
0
2
1
0
0
0
0.022
0.2830
0.1239
0.7800
P-3
0.070
1
0
0
1
0
0
0
0
0.021
0.2689
0.1222
0.8359
P-4
0.056
7
0
0
0
0
0
0
0
0.018
0.2754
0.1218
0.8167
PS-0
1.866
2
1
32
1
168
1
70
33
0.240
0.2519
0.1143
0.9543
PS-1
1.840
2
1
8
2
57
0
20
9
0.011
0.2944
0.1092
0.8527
PS-2
0.141
1
2
0
1
5
0
4
0
0.027
0.2877
0.1233
0.7722
PS-3
0.126
1
0
0
0
3
0
2
1
0.023
0.2716
0.1143
0.8844
PS-4
0.084
3
0
0
0
2
0
2
2
0.007
0.2870
0.1171
0.8146
S-0
4.573
10
8
209
1
1030
3
368
190
0.040
0.2365
0.1127
1.0318
S-1
5.434
12
10
207
3
1040
3
378
190
0.042
0.2658
0.1143
0.9006
S-2
0.310
10
45
4
1
207
0
273
74
0.034
0.2504
0.1228
0.8960
S-3
0.364
10
42
3
1
199
0
255
71
0.035
0.2601
0.1082
0.9738
S-4
0.364
10
41
3
0
197
0
255
69
0.033
0.2578
0.1241
0.8559
*Coefficient of friction
**P = pressed oil, PS = pressed and solvent extracted oil S = solvent extracted oil
***0 = unrefined, 1 = Degummed, 2 = Degummed and neutralized, 3 = Degummed, neutralized and bleached, 4 = Degummed, neutralized, bleached and deodorized.
Example 7
Influence of Canola Oil Additization on Wear and Fuel Economy
[0105] This example describes the canola lubricity field performance of a fully wear documented gasoline engine, a 3.0 L V6 Toyota Camry. Tests began with an additization rate of 250 ppm Canola Oil in unleaded commercial gasoline under summer driving conditions. To reference these tests a control summer test of 10,000 km was conducted without the canola oil present. The same motor oil Pennzoil SJ SAE 10W-30 was used through out the reference and treatment test periods. Eight oil samples were taken. Data was analyzed in two parts, 0 to 5,800 km and 5,800 km to 10,510 km. The driving was 65% highway and 35% city. Starts totaled 458 Cold and 327 Hot. Ambient temperatures ranged from a mean minimum of 8.5° C. to a maximum of 20.8° C. Table 5 shows the comparison of net wear iron ppm levels generated up to the 6,000 summer distances with regular gasoline and with 250 ppm canola oil additization.
[0106] Canola oil supplemented gasoline produced a significant ICP wear reduction compared with the control. The overall averaged wear rate with regular gasoline was 0.99 ppm Fe/1,000 km while the instantaneous method yielded a rate of 0.87 ppm Fe/1,000 km for the reference fuel. The reference results exceeded the 0.63-0.66 ppm Fe/1,000 km obtained with canola oil present and revealed that canola oil additized fuel had resulted in a 33% wear reduction overall and a 26% reduction instantaneously. The average mileage obtained with canola oil present was 28.1 MPG while reference gas mileage was 4% better at 29.3 MPG. In this test canola oil additization lowered fuel economy.
[0107] In Table 6 the ferrography for reference gasoline revealed a wear particle density of 15 with other contaminants counting 8. The canola oil additized fuel run analysis indicated 14 for wear particles and 8 for other debris, indicating no effect of the treated fuel on larger ferrographic particles.
[0108] The filter analysis with 250 ppm canola oil additized fuel reveals rust, dirt, and varnish particles. The largest translucent particles of varnish measure about 200 μm. The spectrographic analysis of the filter residues indicated silicon, iron, copper traces and sodium. The presence and level of the contaminants is normal.
[0109] Both neutralization numbers were not affected significantly by canola oil treatment. Motor oil taken from the vehicle after operation on 250 ppm canola oil additized fuel lowered the total base number to 6.06 while the total acid number remained at 3.66 (Table 6).
[0110] After summer operation on gasoline containing 250 ppm canola oil (6,261 km) viscosity was lowered to 57.6 cSt at 40° C. and 8.95 cSt at 100° C. This represented a 17% drop in viscosity at 40° C. and an 18% change at 100° C. Also the presence of 1% fuel dilution of the oil was indicated after driving 10,243 km, when the oil was changed.
Example 8
Influence of Canola Methyl Ester Additization on Wear and Fuel Economy
[0111] This example describes the Canola lubricity field performance of a fully wear documented gasoline engine, a 3.0 L V6 Toyota Camry. Tests began with an additization rate of 125 ppm canola oil methyl ester (CME) in unleaded commercial gasoline under summer driving conditions. To reference these tests a control summer test of 10,000 km was conducted without the canola methyl ester present. The same motor oil Pennzoil SJ SAE 10W-30 was used through out the reference and treatment test periods. For canola methyl ester additization tests a distance of 10,017 km was covered with 74% highway driving. Cold starts added up to 278 while hot starts equaled 311. Temperature means ranged from 12.3° C. to 25.4° C.
[0112] The ICP iron wear rates were remarkably low with the 125 ppm CME treatment (Table 5). The overall rate method yielded only 0.50 ppm Fe/1,000 km while the instant point-to-point mean was similar at 0.48 ppm Fe/1,000 km. This lower CME treatment resulted in 49% to 45% wear reduction compared to the unadditized reference. It is clearly illustrated that CME wear performance is superior to both the reference and the 250 ppm canola oil additized fuel performance. Both canola additives are considerably better than the reference regular gasoline. The calculated mean fuel economy with 125 ppm CME was some 5% better than for the reference gasoline, yielding 30.8 MPG compared to the former 29.3 miles per Imperial gallon on regular gasoline.
[0113] The consistency of the reference wear readings were established by comparing average ICP data wear rates (Table 5) for regular gasoline. These averages were 0.87, 0.85, 0.99 and 0.87 ppm Fe/1,000 km. On the basis of this long-term reference, the listed per-cent summer wear rate reductions were 33% and 28% for instantaneous and cumulative wear when operating on 125 ppm CME.
[0114] Ferrography analysis of motor oil obtained after operation on 125 ppm CME totaled 6 wear particles and 2 other particles. This represents a reduction of 60% and 87% reduction from reference analysis. Most of these wear metals were described in the ferrography reports as “low alloy steel showing rubbing/sliding wear” although it is difficult to distinguish between very small steel and cast-iron particles, originating from the cylinder block.
[0115] The last filter obtained after operation on 125 ppm CME had far less debris in it compared to the other two filters. The white filter paper support shows through the particles, which are at a much lower concentration. Dirt/dust, rust and varnish are the major contaminants. The presence of silicon, iron, and traces of lead, copper and tin appeared spectrographically.
[0116] Operation on the CME additized fuel lowered the TBN to 6.19 while the TAN climbed to 4.20. This revealed that both neutralization numbers were not affected significantly by the Canola methyl ester.
[0117] Viscosity of the motor oil was also determined after operation on 125 ppm CME. After the 10,016 km ended, the oil tested 59.4 at 40° C., a 13% drop. For 100° C. the values 9.43 cSt were reported, with a 14% drop. Viscosity performance was within specifications
[0118] With 125 ppm Canola Methyl Ester added to the gasoline engine wear rate was reduced by almost one-half, to only 0.5 ppm Fe/1,000 km, potentially doubling engine life. Field fuel economy rose by 5%. The engine oil remained within neutralization and viscosity specifications after some 10,000 km of field-testing. The ferrographic and oil filter debris levels were markedly reduced and appeared normal. Furthermore no driveability or other engine performance problems were detected as the result of the specific CME treatment rate used in unleaded regular gasoline.
Example 9
Winter Canola Oil Gasoline Field Testing, Wear and Fuel Economy
[0119] This example describes the Canola lubricity field performance of a fully wear documented gasoline engine, a 3.0 L V6 Toyota Camry. Tests began with an additization rate of 250 ppm canola oil in unleaded commercial gasoline under winter driving conditions. To reference these tests a series of winter reference runs were performed without the additive. The same motor oil Pennzoil SJ SAE 10W-30 was used through out the reference and treatment test periods.
[0120] The reference wear rate data is recorded in Table 5 reflecting the accumulation of iron (ppm Fe/1,000 km value) averaged 2.24 (overall) and 1.91 (measuring point to point). Reference gasoline economy records averaged 24.5 MPG. The numbers of cold and hot starts during the winter reference period were recorded. Mean ambient winter temperatures were in the −15° C. to −7° C. range. The proportion of highway driving was calculated as 71% and 43% for the reference tests.
[0121] The canola oil additive was pre-mixed with 50% gasoline to facilitate tank blending upon cold refueling. The canola oil test data involved 224 cold and 101 hot starts with 72% highway driving. The fuel economy rose to 27.5 MPG, a 12% improvement in referenced shorter-term mileage. Table 5 compares regular gasoline and the 250 ppm canola oil additive. Calculations in Table 5 indicated that wear rates decreased slightly with 250 ppm canola oil additized fuel, to 2.02 and 1.73 ppm Fe/1,000 km. These reductions in wear were 6% and 20% based on the long-term reference and 10% and 9% based on the shorter-term comparative regular gas references.
[0122] For the canola oil additized fuel treatment, the level of ferrographic wear particles reached “12” while contaminants remained at “7”. This represented 11% lower wear particle count than previously referenced. The magnetic iron trend remained very low and unchanged at 0.2 μg/mL.
[0123] The oil filter taken after operation on 250 ppm canola oil additized fuel revealed contaminants as dirt, rust and varnish. The spectrographic analysis revealed iron, silicon, and traces of sodium, copper, and potassium in the filter debris. Filter analysis results were normal.
[0124] The winter 250 ppm canola oil fuel additive resulted in a 5.8 TBN and a 2.5 TAN indication. This 5.8 reading revealed a similar drop in reserve alkalinity for TBN, noting the 5.7 TBN for the reference fuel. The TAN of 2.5 for canola oil additized fuel treatment had not varied significantly from the 2.5 value for new oil or the 2.7 value for oil after operation on the reference fuel.
[0125] Motor oil obtained after operation on 250 ppm canola oil additized fuel under winter operation conditions had viscosity of 48.5 cSt at 40° C. and 8.73 cSt at 100° C. The viscosity had decreased 21% at 40° C. and 17% drop at 100° C. from new oil. Compared to regular fuel, the relative additional loss of viscosity was 5% at 40° C. and 4% at 100° C. for the canola oil additized gasoline.
[0126] The winter tests with 250 ppm canola methyl ester added to the gasoline were encouraging. Engine wear rate was reduced by almost one-half, to only 0.5 ppm Fe/1,000 km, potentially doubling engine life. Field fuel economy rose by 5%. The engine oil remained within neutralization and viscosity specifications after some 10,000 km of field-testing. The ferrographic and oil filter debris levels were markedly reduced and appeared normal. Furthermore no driveability or other engine performance problems were detected as the result of the specific CME treatment rate used in unleaded regular gasoline.
Example 10
Winter Canola Methyl Ester Gasoline Field Testing, Wear and Fuel Economy
[0127] This example describes the Canola lubricity field performance of a fully wear documented gasoline engine, a 3.0 L V6 Toyota Camry. Tests began with an additization rate of 250 ppm canola methyl ester in unleaded commercial gasoline under winter driving conditions. To reference these tests a series of winter reference runs were performed without the additive. The same motor oil Pennzoil SJ SAE 10W-30 was used through out the reference and treatment test periods.
[0128] The reference wear rate data is recorded in Table 5 reflecting the accumulation of iron (ppm Fe/1,000 km value) averaged 2.24 (overall) and 1.91 (measuring point to point). Reference gasoline economy records averaged 24.5 MPG. The numbers of cold and hot starts during the winter reference period were recorded. Mean ambient winter temperatures were −7.9° C. and −3.7° C. the daily averaged minimum and maximums. The proportion of highway driving was calculated as 71% and 43% for the reference tests.
[0129] The canola methyl ester tests spanned 4,202 km with 106 cold and 113 hot starts logged with 72% highway driving. The average fuel economy during this test was 27.0 MPG, some 10% better compared to the regular gas references. Table 5 compares the net wear iron in the two winter test runs. The gasoline alone graph climbs higher than with 250 ppm the canola methyl ester supplement. The engine-wear iron spectrometry calculations revealed rates of 1.55 and 1.27 ppm Fe/1,000 km with canola methyl ester. These were 28% and 41% lower than the long-term references and 31% and 41% below the shorter-term gasoline references as shown in Table 5. No driveability problems were experienced, with good power, starting, and stable idling rpm demonstrated while using 250 ppm canola methyl ester as a gasoline additive.
[0130] With the canola methyl ester additive, ferrography indicated wear particles were at the “13” level while a ranking of “8” appeared for contaminants. Most metal particles are low alloy steel showing rubbing/sliding. Traces of copper/copper alloy (up to 40 microns) present were comments. The magnetic iron trend stayed minimally the same at 0.2 μg/mL.
[0131] Analysis of the oil filter after operation on 250 ppm canola methyl ester in winter conditions indicated that contaminants were dirt, dust, rust and varnish. The debris texture looked fine with some metallic reflections. Spectrographic analysis revealed silicon, iron, and traces of sodium, potassium, copper and tin in the residue. These filter results were also judged normal.
[0132] Oil viscosity from oil taken after operation on canola methyl ester for 4,104 km was 51.9 cSt at 40° C. and 9.46 at 100° C. No fuel dilution of the motor oil was observed during the trial. These test values represented similar viscosity to that obtained after similar operation on reference gasoline. The 250 ppm canola methyl ester treatment under winter conditions appeared better in terms of viscosity dilution than the 250 ppm canola oil additive.
Example 11
[0133] Twenty liters of methyl esters were prepared according to example 1 using canola oil obtained at a local grocery. The esters were then placed in 2 L lots in a high vacuum vessel used to feed a 2″ wiped film evaporator (Pope Scientific, Saukville Wis.). Vacuum (0.01 torr) was applied to the high vacuum flask to remove residual volatile materials. After vigorous bubbling had ceased the material was passed through the wiped film still at an initial high rate (20 mL/min) to remove low-boiling materials. The walls of the still were heated to 80° C. for this process. During evaporation vapors were condensed by traps chilled with liquid nitrogen. After removing removing volatiles from the methyl ester solution the still was heated to 170° C. and the methyl esters were re introduced and the vacuum was maintained. The flow of liquid was adjusted so that the flow of distillate was approximately 20 times the flow of residue. During this time 1.5 L of residue was collected. The undistilled residue was introduced to the still and after distillation under the same conditions a concentrate of 300 mL was obtained.
[0134] Analysis of the methyl esters and the canola oil with high field proton NMR Spectroscopy (500 MHz Bruker, Milton, ON Canada) revealed a small but observable peak in the spectrum contributed by plant sterols at 0.67 ppm. The distillate did not have observable sterol peaks. Addition of pure sterol (cholesterol or cholestanol) to the distillate restored the peak. The residue of the distillation was also observed using high-field proton NMR. The proton spectrum was comparable to a mixture of plant free and bound sterols with small amount of residual of methyl esters. With further preparation steps known to those skilled in the art, the free and bound sterol fraction may be separated and used as components of nutritional concentrates.
Example 12
Production of Safflower Oil Ethyl Esters
[0135] Potassium hydroxide pellets (100 g) were dissolved in a 4 L beaker containing 3500 g of absolute ethanol. The caustic ethanol solution was added to ten kg of safflower oil in a 20 L plastic pail held at room temperature and the mixture was stirred for 2 hours at room temperature. After 2 hours the solution was allowed to settle for 24 hours and the clear upper layer of ethyl esters was decanted into a clean plastic 20 L pail. The lower layer was transferred to a 4 L separatory funnel and the lower layer of glycerin was separated from the remaining upper layer of ethyl esters. The recovered ethyl esters were combined with the decanted esters. The ethyl esters were then washed by the addition of 200 g of water and vigorous agitation of the solution. The water was allowed to settle and the methyl ester layer was again decanted into a clean plastic pail. The lower water layer was transferred to a 2 L separatory funnel and allowed to settle for 4 hours. The lower water layer was drained and the upper layer of washed methyl esters was combined with the decanted washed esters. The washed esters were placed in a 20 L rotary evaporator and all water and ethanol was removed by evaporation for 2 hours at 80° C. The dried ester layer had a slightly cloudy appearance.
[0136] Celite (250 g) was mixed with a one liter portion of the cloudy ester layer. The slurry was then used to form a filtration bed in a 20 cm clean and oven dry ceramic Buchner funnel. The first sample of ester was returned to the top of the filter bed. Thereafter the remaining volume of ethyl esters was passed over the filter bed to remove particulate matter. Proton NMR and analysis of the fatty acid esters using gas chromatography indicated that the clear solution was greater than 95% fatty acid ethyl esters.
Example 13
Wiped Film Distillation of Safflower Oil Ethyl Esters
[0137] Ten liters of fatty acid ethyl esters were prepared according to example 12 using safflower oil obtained at a local grocery. The esters were then placed in 2 L lots in a high vacuum vessel used to feed a 2″ wiped film evaporator (Pope Scientific, Saukville Wis.). Vacuum (0.01 torr) was applied to the high vacuum flask to remove residual volatile materials. After vigorous bubbling had ceased the material was passed through the wiped film still at an initial high rate (20 mL/min) to remove low-boiling materials. The walls of the still were heated to 80° C. for this process. During evaporation vapors were condensed by traps chilled with liquid nitrogen. After removing removing volatiles from the methyl ester solution the still was heated to 140° C. and the ethyl esters were re introduced and the vacuum was maintained. The flow of liquid was adjusted so that the flow of distillate was approximately 10 times the flow of residue. During this time 1 L of residue was collected. The residue of distillation was introduced to the still and after distillation under the same conditions a concentrate of 50 mL was obtained.
[0138] Analysis of the ethyl esters and the safflower oil with high field proton NMR Spectroscopy (500 MHz Bruker, Milton, ON Canada) revealed two small but observable peaks in the spectrum contributed by plant sterols and other triterpene alcohols. The distillate did not have observable sterol peaks. The residue of the distillation was also observed using high-field proton NMR. The proton spectrum was comparable to a mixture of ethyl esters with plant free and bound sterols and triterpene alcohols. With further preparation steps known to those skilled in the art the free and bound sterol fraction may be separated and used as components of nutritional concentrates. The preparation may also be used as a direct source of sterols.
Example 14
Two Stage Transesterification of Canola Oil with Methanol and Potassium Hydroxide
[0139] Methyl esters of canola oil, also known to those skilled in the art as low erucic acid rapeseed oil, were prepared using a two-stage base catalysed transesterification. The two-stage reaction was required to remove glyceride from the final product. Prior to the reaction the catalyst was prepared by dissolving potassium hydroxide (190 g) in methanol (3800 g). The catalyst solution was divided into two 1995 g fractions and one fraction was added to 20 L of canola oil (purchased from a local grocery store) in a 30 L stainless steel pot. The oil, catalyst and methanol were covered and stirred vigorously for 1 hour with an overhead stirrer. After stirring, the products of the reaction were allowed to settle for 2 hours. At this time a cloudy upper layer and a viscous lower layer had separated. The majority of the upper layer was decanted and the remaining layers were separated using a seperatory funnel. The upper layers were pooled, returned to the stainless pot with overhead stirrer and the remaining potassium hydroxide in methanol solution was added. This second mixture was stirred vigorously in a covered beaker for 1 hour and allowed to settle overnight. The mixture settled to form two layers. The upper layer was collected by decanting and using a separatory funnel.
[0140] After separation of phases the upper layer was mixed with 400 mL of water. The water was removed from the upper phase by decanting. The washed esters were placed in a 20 L rotary evaporator and all water and ethanol was removed by evaporation for 2 hours at 80° C. The resulting esters had a slightly cloudy appearance.
[0141] Celite (250 g) was mixed with a one liter portion of the cloudy ester layer. The slurry was then used to form a filtration bed in a 20 cm clean and oven dry ceramic Buchner funnel. The first sample of ester was returned to the top of the filter bed. Thereafter the remaining volume of methyl esters was passed over the filter bed to remove particulate matter. Proton NMR and analysis of the fatty acid esters using gas chromatography indicated that the clear solution was greater than 95% fatty acid methyl esters.
Example 15
Preparation of a Nutritional Concentrate from Transesterified Canola Oil and Analysis of a Potential Biologically Active Concentrate
[0142] Twenty liters of methyl esters were prepared according to example 14 using canola oil obtained at a local grocery. The esters were then placed in 2 L lots in a high vacuum vessel used to feed a 2″ wiped film evaporator (Pope Scientific, Saukville Wis.). Vacuum (0.01 torr) was applied to the high vacuum flask to remove residual volatile materials. After vigorous bubbling had ceased the material was passed through the wiped film still at an initial high rate (20 mL/min) to remove low-boiling materials. The walls of the still were heated to 80° C. for this process. During evaporation vapors were condensed by traps chilled with liquid nitrogen.
[0143] The still was then heated to 170° C. and the methyl esters were re introduced and the vacuum was maintained. The flow of liquid was adjusted so that the flow of distillate was approximately 20 times the flow of residue. During this time 1.5 L of residue was collected. The undistilled residue was introduced to the still and after distillation under the same conditions a concentrate of 300 mL was obtained.
[0144] Analysis of the methyl esters and the canola oil with high field proton NMR Spectroscopy (500 MHz Bruker, Milton, ON Canada) revealed a small but observable peak in the spectrum contributed by plant sterols at 0.67 ppm. The distillate did not have observable sterol peaks. Addition of pure sterol (cholesterol or cholestanol) to the distillate restored the peak. The residue of the distillation was also observed using high-field proton NMR. The proton spectrum was comparable to a mixture of plant free and bound sterols with small amount of residual of methyl esters. With further preparation steps known to those skilled in the art the free and bound sterol fraction may be separated and used as components of nutritional concentrates.
Example 16
Transesterification of Safflower Oil with Ethanol
[0145] Potassium hydroxide pellets (100 g) were dissolved in a 4 L beaker containing 3500 g of absolute ethanol. The caustic ethanol solution was added to ten kg of safflower oil in a 20 L plastic pail held at room temperature and the mixture was stirred for 2 hours at room temperature. After 2 hours the solution was allowed to settle for 24 hours and the clear upper layer of ethyl esters was decanted into a clean plastic 20 L pail. The lower layer was transferred to a 4 L separatory funnel and the lower layer of glycerin was separated from the remaining upper layer of ethyl esters. The recovered ethyl esters were combined with the decanted esters. The ethyl esters were then washed by the addition of 200 g of water and vigorous agitation of the solution. The water was allowed to settle and the methyl ester layer was again decanted into a clean plastic pail. The lower water layer was transferred to a 2 L separatory funnel and allowed to settle for 4 hours. The lower water layer was drained and the upper layer of washed methyl esters was combined with the decanted washed esters. The washed esters were placed in a 20 L rotary evaporator and all water and ethanol was removed by evaporation for 2 hours at 80° C. The dried ester layer had a slightly cloudy appearance.
[0146] Celite (250 g) was mixed with a one liter portion of the cloudy ester layer. The slurry was then used to form a filtration bed in a 20 cm clean and oven dry ceramic Buchner funnel. The first sample of ester was returned to the top of the filter bed. Thereafter the remaining volume of ethyl esters was passed over the filter bed to remove particulate matter. Proton NMR and analysis of the fatty acid esters using gas chromatography indicated that the clear solution was greater than 95% fatty acid ethyl esters.
Example 17
Preparation of a Nutritional Concentrate from Transesterified Safflower Oil and Analysis of a Potential Nutritional Concentrate
[0147] Ten liters of fatty acid ethyl esters were prepared according to example 16 using safflower oil obtained at a local grocery. The esters were then placed in 2 L lots in a high vacuum vessel used to feed a 2″ wiped film evaporator (Pope Scientific, Saukville Wis.). Vacuum (0.01 torr) was applied to the high vacuum flask to remove residual volatile materials. After vigorous bubbling had ceased the material was passed through the wiped film still at an initial high rate (20 mL/min) to remove low-boiling materials. The walls of the still were heated to 80° C. for this process. During evaporation vapors were condensed by traps chilled with liquid nitrogen. After removing volatiles from the methyl ester solution the still was heated to 140° C. and the ethyl esters were re introduced and the vacuum was maintained. The flow of liquid was adjusted so that the flow of distillate was approximately 10 times the flow of residue. During this time 1 L of residue was collected. The residue of distillation was introduced to the still and after distillation under the same conditions a concentrate of 50 mL was obtained.
[0148] Analysis of the ethyl esters and the safflower oil with high field proton NMR Spectroscopy (500 MHz Bruker, Milton, ON Canada) revealed two small but observable peaks in the spectrum contributed by plant sterols and other triterpene alcohols. The distillate did not have observable sterol peaks. The residue of the distillation was also observed using high-field proton NMR. The proton spectrum was comparable to a mixture of ethyl esters with plant free and bound sterols and triterpene alcohols. With further preparation steps known to those skilled in the art the free and bound sterol fraction may be separated and used as components of nutritional concentrates. The preparation may also be used as a direct source of sterols.
Example 18
Recovery of Non Esterified Sterols from Canola Methyl Ester Distillate Residue
[0149] The residue of distillation obtained from Example 15 (0.50 g) was mixed with KOH (0.3 g) dissolved in ethanol (2.5 mL) and water (2.5 mL) The mixture was heated at 65° C. for 3 hours after which the ethanol was removed under vacuum. The resulting residue was diluted with water (15 mL) and the unsaponifiable matter was extracted with petroleum ether (3×15 mL). The combined organic phases were dried over anhydrous sodium sulphate. Evaporation of the petroleum ether under reduced pressure gave a white solid (158 mg). A portion of the solid was dissolved in deuterated chloroform and placed in an NMR tube. Analysis of the solid with high field proton NMR Spectroscopy (500 MHz Bruker, Milton, ON Canada) revealed that the solid was primarily a mixture of the free alcohol forms of phytosterol compounds.
Example 19
Separation of Fractions from the Canola Methyl Ester Distillate Residue by Silica Chromatography
[0150] Fifteen grams of silica gel 60 was packed in a 10 cm −1 glass column and the column was washed with 50 mL of n-hexane. The wash was discarded. Canola methyl ester distillate residue (0.4 g) was dissolved in hexane and added to the column. The column was then washed sequentially with 50 mL of n-hexane, 50 mL of 3% diethyl ether in n-hexane, 50 mL of 10 percent ethyl acetate in n-hexane and, finally, 50 mL of 25% ethyl acetate in n-hexane. The repeated extractions produced four fractions with masses of 250 mg, 50 mg, 10 mg and 65 mg respectively after the complete removal of the extraction solvent. The first three fractions were oil like in nature while the last fraction was a white solid. Desolventized samples were dissolved in deuterated chloroform and placed in NMR tubes for analysis. Analysis of the fractions with high field proton NMR Spectroscopy (500 MHz Bruker, Milton, ON Canada) revealed that the fractions were 1) a mixture of sterol esters of fatty acids with some fatty acid methyl ester; 2) a mixture of fatty acid methyl esters with some sterol ester; 3) a complex mixture containing Fatty acid esters as well as some unknown compounds; 4) A highly enriched fraction of phytosterols in a free alcohol form. | Methods for recovery of concentrates of lubricating compounds and biologically active compounds from vegetable and animal oils, fats and greases that allow separation of triglycerides, from components with higher lubricity or biological activity or enrichment protocols that increase the concentration of high lubricity or biologically active compounds in the triglyceride. The triglycerides are transesterified with a lower alcohol to produce alkyl esters. Following the conversion process the esters are separated from high molecular weight high lubricity compounds and biologically active compounds by distillation. The esters have some lubricity and may be sold as pollution reducing fuel components. The high boiling point compounds that are the residues of distillation, however, can either contribute significant lubricity and may be used widely in lubricant applications or added to petroleum fuels to decrease friction or the biologically active components may be used in nutritional, cosmetic and therapeutic applications. Therapeutic applications include use in human diets to lower cholesterol. | 2 |
BACKGROUND OF THE INVENTION
The present invention relates to a detection system for receiving incoming signals coming from many different directions and presenting indications of the direction and/or range of a source of incoming signals. More particularly, it relates to a detection system which comprises (i) means for receiving incoming signals in a manner that the Doppler effect is produced to vary the carrier frequency of the incoming signals (ii) a matched filter coupled to the receiving means to pulse-compress output signals therefrom, and (iii) an indicator for displaying output signals from the matched filter, and which forms a plurality of reception beams successively in angular directions. This type of detection system is enclosed in U.S. Pat. No. 4,425,634.
Hereinafter, the invention will be described as embodied in a scanning sonar for receiving incoming signals from many different directions in a wide range of angles to indicate the direction and range of objects on the face of an indicator.
Referring to FIG. 12 in which a relevant portion of a prior art detection system is shown, one hundred and twenty ultrasonic transducers 1CH through 120CH are disposed on an imaginary circle as equidistantly spaced, which forms one row of transducers Preamplifiers P1 through P120 amplify reception signals caught by the ultrasonic transducers 1CH through 120CH respectively. A selector SW successively connects, at a predetermined speed, the output terminal of each of the preamplifiers P1 through P120 to the input terminal of a beamformer BM to supply the beamformer with the output signals of each of the preamplifiers P1 through P120. As a result the Doppler effect is produced to vary the carrier frequency of the incoming signals received The beamformer comprising a matched filter pulse-compresses the received signals to produce signals having come in a desired direction and detected The reception signals produced by each of the transducers 1CH through 120CH are selected and derived at the output terminals of the preamplifiers P1 through P120 to be supplied to the input terminal of the beamformer.
With the prior art detection system, six rows of ultrasonic transducers are disposed in parallel with each other on the surface of a cylinder along the circumference thereof, with each row comprising one hundred and twenty ultrasonic transducers. Thus, seven hundred and twenty ultrasonic transducers are disposed on the surface of a cylinder, and the same number of preamplifiers are required to be incorporated in the receiving unit of the detection system, since all the ultrasonic transducers are separately and respectively connected to the corresponding preamplifiers. The switch SW is incorporated between the output terminals of the preamplifiers P1 through P120 and the input terminal of the beamformer, and the reception signals produced by each of the transducers 1CH through 120CH are selected by the switch SW to be applied at the input terminal of the beamformer BM. Accordingly, the dimensions of the receiving unit and the electric power consumed by the receiving unit are determined by the number of the preamplifiers. Manufacturing cost of the receiving unit is substantially determined by the cost of the preamplifiers.
SUMMARY OF THE INVENTION
Accordingly, an object of the present invention is to provide a detection system which is greatly reduced in size without degrading the performance of the system, so that it is easy to handle and to be maintained.
Another object of the invention is to provide a detection system which is capable of successively deriving output signals of each of the ultrasonic transducers with lesser number of the preamplifiers, thereby reducing the dimensions of the receiving unit, manufacturing cost thereof and the electric power consumption thereof.
Another object of the invention is to provide a detection system which derives the reception signals produced by the ultrasonic transducers by means of a switch incorporated between the transducers and the input terminals of the preamplifiers and another switch incorporated between the output terminals of the preamplifiers and the input terminal of a beamformer
According to one aspect of the present invention, a detection system for receiving incoming signals from a plurality of directions in a manner that the Doppler effect is produced to vary the carrier frequency of the incoming signals, and presenting a display resulting from the received incoming signals on an indicator is provided which comprises (i) a plurality of ultrasonic transducers for receiving incoming signals (ii) a plurality of preamplifiers for amplifying the reception signals produced by the ultrasonic transducers, (iii) first coupling means: for connecting each of the ultrasonic transducers to corresponding one of the preamplifiers, (iv) a matched filter for pulse-compressing reception signals produced by the ultrasonic transducers, (v) second coupling means for successively coupling the output terminals of the preamplifiers to the input terminal of the matched filter, and (vi) an indicator for displaying output signals from said matched filter
Referring to FIG. 1 and FIG. 2 the principle of the present invention will be explained hereinafter. One hundred and twenty reception transducers 1CH through 120CH are disposed on a circle as equidistantly spaced. These transducers are divided into two groups, with one group including the transducers 1CH through 60CH, and with the other group having the transducers 61CH through 120CH. The input terminal of each of preamplifiers p1 through P60 is alternately connected by means of a switch SWa to corresponding one transducer of the two transducer groups, i.e., the transducers 1CH through 60CH and the transducers 61CH through 120CH. The switch SWa comprises sixty switch elements SW1 through SW60. A switch SWb successively connects the output terminals of the preamplifiers p1 through P60 to the input terminal of a beamformer BM The switch SWb is comprised of digitally controlled analog switches, for example, of analog multiplexers the MC14051Bs manufactured by Motorola Inc. Thus, the reception signals amplified by the preampifiers p1 through P60 are successively derived and supplied to the beamformer BM.
Referring to FIG. 2, the portions designated as (a) through (e) illustrate how the switch SWa comprising sixty switch elements SW1 through SW60 is operated. Symbols 1CH through 120CH in brackets are the ones assigned to the ultrasonic transducers. Thus, it is illustrated how the ultrasonic transducers are connected to the input terminals of corresponding preampifiers. The portions designated as (f) through (j) illustrate how the switch SWb is operated, i.e., how the output terminal of a preamplifier corresponding to transducer is connected to the input terminal of the beamformer. Symbols 1CH through 120CH are also assigned to the transducers it will be apparent from the time sequence diagrams that the ultrasonic transducers 1CH through 120CH are successively coupled to the input terminal of the beamformer BM by means of the switches SWa and SWb which are controlled by a controller
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 shows a schematic block diagram of a relevant principal portion of an embodiment according to the present invention,
FIG. 2 shows a time sequence diagram illustrating how the switches in FIG. 1 are operated, and how the ultrasonic transducers and the input terminal of the beamformer are coupled,
FIG. 3 shows a circuit configuration of a portion of a switch SWa of an embodiment according to the invention shown in FIG. 6,
FIG. 4 shows a circuit configuration of a signal generator producing control signals for controlling field effect transistors as shown in FIG. 3,
FIG. 5 shows a time sequence diagram illustrating how switches SWa, SWb1 and SWb2 shown in FIG. 6 are operated, i.e., how the input terminal of the beamformer is coupled to transducers,
FIG. 6 shows a bock diagram of an embodiment according to the invention,
FIG. 7 shows amplitude variations of input signals applied at the two input terminals of the multipliers 11 and 12 shown in FIG. 6,
FIGS. 8, 9 and 10 show response characteristics of a filter included in each of the preamplifiers shown in FIGS. 1, 3 and 6,
FIG. 11 shows a block diagram of each of the preamplifiers used in an embodiment of the invention,
FIG. 12 shows a schematic block diagram of a relevant part of a prior art detection system, and
FIG. 13 shows another circuit configuration of the signal generator producing control signals for controlling field-effect transistors as shown in FIG. 3.
Throughout the drawings, the same reference numerals and symbols are given to like components
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 6, one hundred and twenty ultrasonic electrostrictive transducers 1CH through 120 CH are disposed on a circle equidistantly spaced apart. These transducers are divided into two qroups, with the one group including the transducers 1CH through 60CH and the other group consisting of the transducers 61CH through 12OCH. The input terminal of each of the preamplifiers P1 through P60 is: connected by means of a switch SWa to a corresponding one of the transducers of each of the two groups 1CH through 60CH and 61CH through 120CH. The switch SWa comprises sixty switching elements SW1 through SW60. The switching element SW1 alternately connects the input terminal of the preamplifier P1 to one o the transducers 1CH and 61CH. The switching element SW2 connects the input terminal of the preamplifier p2 to one of the transducers 2CH and 62CH. In the same way, each of the switching elements SW3 through SW60 alternately connects the input terminal of one of the preamplifiers P3 through P60 to one transducer of each corresponding pair of the transducers 1CH and 63CH through 60CH and 120CH. A switch SWb1 comprises thirty switching elements which successively connect the output terminals of the odd-numbered preamplifiers P1, P3, ..., P59 to the input terminal of a multiplier 11. A switch SWb2 comprises thirty switching elements which successively connect the output terminals of the even-numbered preamplifiers p2, P4, . . . , P60 to the input terminal of a multiplier 12. A switch select control circuit 10 controls the switches SWa SWb and SWb2 to select switching elements to perform connecting and disconnecting operations as desired The switch SWa firstly and successively connects the input terminal o& each of the preamplifiers P1 through p60 to a corresponding one of the ultrasonic transducers 1CH through 60CH and then successively connects the input terminal of each of the preamplifiers P1 through p60 in the order of p1, P2 . . , P60 to corresponding one of the transducers 61CH through 120CH. The switches SWb1 and SWb2 successively and respectively connect the output terminals of the odd-preamplifiers numbered and even-numbered preamplifiers P1 through P60 to the input terminals of the multipliers 11 and 12 so that the output terminals of the preamplifiers P1 through p60 are successively coupled to the input terminal o the beamformer. A signal generator 13 produces triangular waveform signals which are shifted in phase from each other, and supplies the multipliers 11 and 12 with these shaped signals designated as "c" and "d" (shown in FIG. 7) at the other inputs thereof respectively. The multiplier 11 multiples the reception signals designated as "a" (shown in FIG. 7) supplied from the preamplifiers at the one input thereof with triangular wave signals designated as "c" (shown in FIG. 7) supplied at the other input terminal thereof and supplies an adder 14 with the resultant signals at one input terminal thereof The mutiplier 12 multiplies the reception signals designated as "b" (shown in FIG. 7) supplied from the preamplifiers at the one input terminal thereof with triangular wave signals designated as "d" (shown in FIG. 7) supplied at the other input thereof and supplies the adder 14 with the resultant signals at the other input thereof The adder 14 adds the signals supplied to the two input terminals to one another and supplies the resultant added signals to a signal input terminal of an analog-delay circuit 15.
The relationship between the signals designated as "a", "b", "c" and "d" is as shown in FIG. 7. In FIG. 7a and FIG. 7b, the numerals given to each block correspond to the numbers assigned to the ultrasonic transducers 1CH through 120CH. As will be apparent, the reception signals produced by two adjacent transducers are increasingly or decreasingly weighted with time to average the reception signals, thereby obtaining the same signals as received by one ultrasonic transducer mechanically rotated at a constant speed.
The analog-delay circuit 15 has a plurality of i.e., n, output terminals equidistantly spaced apart, and stores the reception signals produced by ultrasonic transducers of a group used for forming a reception beam. Resistors r1, r2, r3, and are inserted between the corresponding output terminals of the analog-delay circuit 15 and one input terminal of operational amplifiers 16 and 17. To the one input of the operational amplifier 16, signals obtained by sampling the positive portions of the input signals applied at the input of the analog-delay circuit 15 are supplied To the one input of the operational amplifier 17, signals obtained by sampling the negative portions of the signals inputted to the delay circuit 15 are supplied. The output terminal of the operational amplifiers 16 and 17 are connected to the two input terminals of an operational amplifier 18 respectively. The input signals applied at the signal input of the delay circuit 15 are advanced therein each time a clock pulse is applied at the clock input of the circuit 15, and the signals stored therein appear at the corresponding output terminals. These output signals of the analog-delay circuit 15 are weighted by the resistors r1, r2, r3, , rn and resistors R1 and R2 inserted between the one input terminal of the operational amplifiers 16 and 17 and the output terminals thereof respectively to produce resultant signals which are added to one another by the operational amplifier 18. The values of the resistors r1, r2, r3, . . . , and resistors R1 and R2 are respectively determined in such a way that the amplitude of the signals from a sound source in a desired direction becomes maximum with respect to that of other incoming signals from the other directions when a first signal supplied at the signal input of the analog-delay circuit reaches the right end thereof and al the output signals appear at the respective output terminals thereof Thus, a matched filter is formed by the analog-delay circuit 15, resistors r1, r2, r3, . . . , rn, operational amplifiers 16, 17 and 18, and resistors R1, R2, R3 and R4.
An amplifier 21 amplifies the output signals &rom the operational amplifier 18 containing only the incoming signals having come from a desired direction and supplies the resultant amplified signals to the input terminal of an indicator 22 comprising, for example, a cathode-ray tube. A deflect ion circuit 23 produces deflection signals for deflecting the electron beams of the cathode-ray tube concentrically. A controller 20 produces timing control signals and supplies the switch select control circuit 10, signal generator 13, analog-delay circuit 15 and deflection circuit 23 with the respective control signals
Referring to FIG. 3, one output terminal o the ultrasonic transducer 1CH is connected to the source terminal of a depletion-mode p-channel junction field-effect transistor (hereinafter called as "FET") Q1 such as 2SJ103 manufactured by Toshiba. The drain terminal of the FET Q1 is connected to the input terminal of the preamplifier P1. One output terminal of the ultrasonic transducer 61CH is connected to the source terminal of a FET Q61. The drain terminal of the FET Q61 is also connected to the input terminal of the preamplifier P1. The qate terminals of the FETs Q1 and Q61 are respectively supplied with control signals having a TTL amplitude level from the switch select control circuit 10 to switch the FETs on and to pass therethrough reception signals caught by the transducers 1CH and 61CH. Two pairs of diodes shown in FIG. 3 for limiting circuits to limit the amplitude levels of the input signals supplied to the FETs Q1 and Q61.
FIG. 4 shows a circuit diagram for producing the control signals supplied to the gate terminals of the FETs such as Q1 and Q61 shown in FIG. 3. Referring to FIG. 4 shift-registers 30 and 31 are connected in series with each other to have thirty output terminals To one input terminal of the shift-register 30, there are supplied FS signals determining on-off periods of the FETs such as the FETs Q1 and Q61 shown in FIG. 3, while clock pulses are supplied to the clock input terminal thereof At respective output terminals to the shift-registers 30 and 31, there are produced FS signals which are successively shifted by a time equivalent to the recurrence period of the clock pulses. A waveform conversion circuit 32 is comprised of an operational amplifier, a condenser, a resistor and zener diodes and functions to convert an FS signal shaped in a rectangular form into a substantial trapezoid waveform A signal level lowering circuit 33 is comprised of an operational amplifier and resistors A signal level conversion circuit 36 functions to raise the voltage level of the output signals of the signal level lowering circuit 33 to the pinch-off voltage level of the FET. A polarity inversion circuit 34 is comprised of an operational amplifier and resistors and functions to inverse the polarity of the output signals of the signal level lowering circuit 33. A signal level conversion circuit 35 is constructed in the same way as the signal level conversion circuit 36. The output signal of the signal level conversion circuit 35 is supplied to the gate terminals of the FETs Q1 and Q2. The output signal of the signal level conversion circuit 36 is supplied to the gate terminals of the FETs Q61 and Q62. In the same way, the output terminals of the other signal level conversion circuits are respectively coupled to the gate terminals of a corresponding pair of the FETs. Thus, the switching elements i.e., the FETs, are driven by rectangular waveform signals, the leading and trailing edges of which are rounded off at the upper and lower points thereof. The use of such modified signals suppresses high frequency components included in the control signals, thereby drastically reducing noises produced when switching operations are performed by the FETs.
Referring to FIG. 5, the portions designated as (1) through (10) illustrate how the switch SWa is operated. Numerals in brackets correspond to the numbers assigned to the ultrasonic transducers 1CH through 120CH The portions designated as (11) through (20) illustrate how the switches SWb1 and SWb2 are switched on and off. Numerals in this part of the figure respectively correspond to the transducers supplying their output signals to the corresponding preamplifiers in this embodiment of the present invention, as shown in FIG. 5 (1) through (10), pairs of two adjacent transducers such as 1CH and 2CH, 3CH and 4CH are connected to or disconnected from corresponding preamplifiers p1 through P4 at the same time. This arrangement reduces the number of the drive circuits shown in FIG. 4 for the switching elements by one-half
Some aspects of the filter included in the preamplifier will be explained below. In the foregoing embodiment of the present invention, for example, to the input of the preamplifier p1, the reception signals caught by the transducers 1CH and 61CH are alternately supplied When the FETs Q1 and Q61 are respectively switched on and off for connecting the transducers 1CH and 61CH to the input terminal of the preamplifier P1 and disconnecting the transducers therefrom, noises are produced and are also applied at the input terminal of the preamplifier. The noises are prominent in terms of amplitude with respect to the reception signals applied at the input terminal of the preamplifier, since the reception signals transmitted from the transducers thereto are weak and small. Further, the reception signals in rectangular shapes applied at the input terminal of the preamplifiers are rounded off thereby at the leading and trailing edges of the signals since the frequency characteristics of the preamplifiers are of narrow bandwidth. The phenomena is illustrated in FIG. 8. Referring to FIG. 8, "Ta" shows an instant at which the reception signals produced by the transducer 1CH are sampled, while "Tb" shows an instant at which the reception signals produced by the transducer 61CH are sampled. If a noise tail resulting from the switching operation in relation to the transducer 61CH is still existing at the instant " Ta", the noise tail becomes a noise having directional information, thereby decreasing the S/N ratio. While, if a noise tail resulting from the switching operation in relation to the transducer 1CH is still existing at the instant "Tb", the noise will be crosstalk in the signals produced by the transducer 61CH. Accordingly, effects caused by the noise tail have to be reduced in designing the filter included in the preamplifier.
Referring to FIG. 11, a mixer 40 is supplied with the reception signals with their frequency "fi" rom the corresponding transducers at one input terminal thereof and with signals having their frequency "f" from a local oscillator at the other input terminal thereof. The mixer YO performs frequency conversion to produce output signals with their frequency "fo=fi-f" to the input terminal of an amplifier 41 for amplifying the input signals A bandpass filter 42 passes the signals having frequencies within a predetermined frequency range. The effects explained above are reduced by appropriately designing the frequency characteristics of the filter 42.
With regard to noises produced by a corresponding FET when switched on and off, impulse response is first analyzed which is possessed by the filter. FIG. 9 shows a waveform illustrating an impulse response for the filter. The time "ts" represents a period from a time instant at which a switching noise is produced to another time instant at which signals are sampled. The filter is designed to have an impulse response, the value of which becomes smaller than a predetermined value with respect to the amplitude of the reception signals at the time instant when the signals are sampled.
With regard to a signal tail resulting from the reception signals, the filter response to a burst signal is analyzed. FIG. 10 shows burst signals and resultant response waveforms. Here, "to" represents delay time, and is given by phase spectrum incination in the frequency range of the filter. "tr" is rise time and is inversely proportional to the frequency bandwidth of the filter. Further, the amplitude of ripples included in a tail portion is obtained by analyzing the variation of a sinusoidal +equal function. In this way, the filter characteristics are determined in such a way that the impulse response of the filter for burst signals is anayzed, and the difference between the amplitude of the reception signals produced by he transducer 1CH and that of the reception signals produced by the transducer 61CH i.e., the crosstalk ratio, becomes qreater than a predetermined level.
Reduction of the switching noises and improvement of decoupling the crosstalk are attained by widening the frequency bandwidth of the preamplifiers. But, improper widening of the bandwidth results in decreasing the S/N ratio. Thus, the frequency bandwidth of the filter is required to be made as narrow as possible. A desired frequency bandwidth o the preamplifiers is determined based on the frequency bandwidth in relation to the Doppler-shift with the carrier frequency and the frequency bandwidth in relation to the pulse-width of the search pulse signal radiated into the water. With regard to the Doppler-shift, the following approximate equation to obtain the frequency bandwidth is used:
±Δf1=0.7 m f [Hz]
Herein
m: Ship's relative speed with respect to objects detected [Knot ]
f: center frequency [KHz ]
With regard to the pulse-width of the search pulse signal, the following approximate equation to obtain the frequency bandwidth is used:
±Δf2=1.3/2ΔT
Herein
ΔT: pulse-width of the search pulse signal
It should be noted that although the signal generator producing control signals for controlling the FETs is used in the foregoing embodiment, another signal generator shown in FIG. 13 is also used. Referring to FIG. 13, the signal generator comprises a counter 130 a memory 131, a selector 132, thirty digital-to-analog converters (hereinafter referred to as "D-A converters") 133 and 140 The D A converter 133 comprises a match circuit 134 comprising D-type flip-fops, resistors, two operational amplifiers 135 and 136, two resistors and two condensors. The operational amplifier 135 produces control signals supplied to the gate terminals o the FETs Q1 and Q2, while the operational amplifier 136 produces control signals supplied to the gate terminals of the FETs Q61 and Q62. The control signals are formed with the upper and lower flat level portions and curved portions between the upper and lower levels, with the curved portions being shaped in sine waveforms Four output signals appearing at four output terminals of a group of the latch circuit 134 are respectively weighted with the four respective resistors, the values of which are respectively represented as R, R/2, R/4 and R/8. The resultant weighted signals are supplied to one input terminal of the operational amplifier 135. Four output signals appearing at four output terminals of the other group of the latch circuit 134 are respectively weighted with the four resistors. The resultant weighted signals are supplied to one input terminal of the operational amplifier 136. Clock pulses are supplied to one input terminal of the counter 130 and the selector 132. The counter 130 successively produces varying count values supplied to the fifteen input terminals: of the memory 131 which comprises a read-only-memory. The memory 131 stores thirty kinds of digital signals each representative of two portions of a sine waveform corresponding to the curved portions of the signals produced by the D-A converter. The memory 131 supplies digital signals of a group representative of portions of sire waveforms to the four input terminals o the latch circuit 134 and also supplies digital signals of the other group to the selector 132 comprising a decoder. The selector 132 successively selects the thirty D-A converters and supplies the match circuits of the D-A converters with pulses at the clock input terminals thereof. The latch circuit 134 produces output signals in response to the pulses applied at the clock input terminals thereof.
lt should be noted that although the signal generator 13 produces triangular waves for the multipliers 11 and 12 in the foregoing embodiment, it can also produce and transmit sine or cosine waves thereto to obtain the same result as in the above embodiment.
It should be noted that although any a row of one hundred and twenty ultrasonic transducers disposed on an imaginary circle is used in the foregoing embodiment according to the present invention, a plurality of the rows of transducers can be arranged vertically equidistantly spaced apart between two adjacent rows of transducers. This arrangement enables one to direct the reception beams in any desired tilt direction by controlling the phase of the reception signals caught by transducers disposed on an imaginary vertical line with respect to one another
lt should be noted that although the number of the preamplifiers is reduced by one-half in the foregoing embodiment according to the invention, the number of the preamplifiers can be reduced by two thirds by dividing the ultrasonic transducers into three groups.
While, the invention has been described in detail and with reference to specific embodiments thereto, 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 of invention. | A detection system forms a plurality of reception beams successively in angular directions by receiving incoming signals from various directions in a manner that the Doppler effect is produced to vary the carrier frequency of the incoming signals. The detection system displays underwater conditions on an indicator. To determine the underwater conditions, the detection system uses a plurality of ultrasonic transducers for receiving incoming signals, a plurality of preamplifiers for amplifying the reception signals produced by the ultrasonic transducers. A first coupling device which connects at least two of the ultrasonic transducers to a single preamplifier, and a matched filter for pulse-compressing reception signals produced by the ultrasonic transducers. A second coupling device successively couples the output terminals of the preamplifiers to an input terminal of the matched filter. The indicator displays output signals from the matched filter. The use of the first coupling device reduces the number of the preamplifiers. | 8 |
CROSS-REFERENCE
This application claims priority to German patent application no. 10 2015 220 962.8 filed on Oct. 27, 2015, the contents of which are fully incorporated herein by reference.
TECHNOLOGICAL FIELD
The present disclosure relates to a bearing assembly for a wheel bearing assembly of a vehicle with a seal assembly.
BACKGROUND
Bearing assemblies for wheel bearing assemblies are often embodied as tapered-roller-bearing assemblies. Here two cooperating tapered roller bearings are axially preloaded against each other and received on or in a hub. Furthermore, a seal assembly is provided that seals the bearing assembly against an entry of dirt and/or water, and/or against a discharge of lubricant. This seal assembly is usually embodied as a cassette seal and is applied as a complete component on the bearing assembly, in particular on the bearing rings.
Furthermore, the setting of the preload in tapered roller bearings is a relatively complex and also inexact process, wherein it is attempted to set the correct preload by displacing the two inner rings of a tapered roller bearing unit axially towards each other (in the case of a back-to-back bearing arrangement) or axially away from each other (in the case of a face-to-face bearing arrangement). The correct displacement path is determined by a complex measuring of the components and set by shims such that the desired preload arises. The preload is then maintained by tightening a shaft nut with which the entire bearing assembly is fixed to a shaft part.
Since the securing of the nut or the fixing of the inner rings is achieved via a corresponding clamping force, it must be taken into account here in turn that the bearing preload complexly set via shims is influenced by the usually very large clamping force. An exact desired preload can thus only be achieved with difficulty.
It has therefore been proposed, in particular in DE 10 2012 221 297, to dispose at least one of the flanges on the bearing ring such that it is adjustable in the axial direction relative to the bearing ring carrying it, wherein the adjustable flange includes a thread via which its axial position is adjustable.
However, the problem thereby arises that the cassette seal usually used can no longer be used, and must be adapted to the particular circumstance and preload. This is on the one hand expensive and on the other hand requires a very time-consuming installation.
SUMMARY
An aspect of the present disclosure is therefore to provide a bearing assembly wherein the preload on the bearing assembly can be simply and precisely set and that makes possible a simple installation of the seal assembly.
In the following a bearing assembly, in particular a wheel bearing assembly for a vehicle, with at least one rolling-element bearing, in particular with two tapered roller bearings, is presented, wherein the at least one rolling-element bearing includes a bearing outer ring and a bearing inner ring that define a bearing interior between them in which rolling elements are disposed. Furthermore, the bearing assembly includes a seal assembly for sealing the bearing assembly, wherein the seal assembly includes a carrier element that is connectable, for example, via an axially extending ring arm, to one of the bearing rings of the bearing assembly such that they rotate together, and includes a radially extending annular flange, wherein the radially extending flange carries a radially encircling seal with at least one seal lip. The seal lip in turn extends toward the other bearing ring and sealingly abuts on a sleeve-shaped element that is connectable to the other bearing ring of the bearing assembly such that they rotate together.
In order to provide both a simple installation but also, as further precisely explained below, a simple and precise preload in the bearing assembly, it is proposed to form the sleeve-shaped element as a preferably axially adjustable flange that forms an axial stop for the rolling elements. Thus the seal and the flange can be installed in a single work step. Moreover, in addition to the faster installation, a cost advantage can arise in that a metal-plate part for the seal and a metal-plate part for the flange need not be used, rather a single metal-plate part suffices.
According to an advantageous exemplary embodiment the sleeve-shaped element is adjustable in the axial direction relative to the associated bearing ring or disposed relative to the bearing ring. A defined preload force can thereby be applied onto the bearing assembly, and the bearing assembly simultaneously sealed against an entry of dirt and/or water.
According to a further advantageous exemplary embodiment, the sleeve-shaped element forming the flange is disposed with a press-fit on or relative to the bearing ring and displaceable on or relative to the bearing ring against a friction given by the press-fit. A simple installation of the axially displaceable flange can thereby be achieved since no thread need be provided on the sleeve-shaped element, rather it is simply disposed with press-fit on or relative to the bearing ring and is configured displaceable on or relative to the bearing ring against a friction given by the press-fit.
Moreover, if a preload is to be set via the sleeve-shaped element forming the flange, this is possible in a simple manner since the preload is achieved via the size of the friction force of the press-fit with the axial displacing of the sleeve-shaped element forming the displaceable flange. In addition, a separation of the two preload circuits, namely of the preload circuit of the roller preload and the preload circuit of the inner-ring clamping, can be achieved by the pushing-on under press-fit, which in turn causes the negative influence of an inner-ring clamping or a nut-locking to be able to be separated from the actual bearing preload. Furthermore, via the press-fit or the magnitude of the friction generated by the press-fit during displacing of the sleeve-shaped element forming the adjustable flange it can be precisely determined what force the rolling elements exert on the flange and thus what preload prevails in the bearing assembly. A defined preload on the bearing assembly can thereby be simply and quickly achieved. Here it is also possible to achieve different preloads via the use of different press-fits of the flange.
Furthermore, a great diversity of arrangement possibilities of the sleeve-shaped element forming the flange is advantageously achieved. Thus, for example, the sleeve-shaped element forming the adjustable flange can be disposed on the outer ring or inner ring or also on a bearing housing receiving the rolling-element bearing or on a shaft rotatably supported by the bearing.
In particular with the disposing on the bearing inner ring a seal can thus be provided that is designed more durable overall. The reason for this is that the sleeve element functioning as a flange has a smaller diameter than a bearing ring formed integrated with the flange, so that the rotational speed with which the seal lip runs along the sleeve-shaped element is reduced, and thus friction losses and wear are reduced.
According to a further advantageous exemplary embodiment, the inner ring or the outer ring includes a cylindrical seat onto which the sleeve-shaped element forming the flange is pushable-on, preferably under press-fit. Due to the cylindrical seat it can also be achieved that a constant friction force opposes the displaceability of the sleeve-shaped element forming the displaceable flange and thus a defined preload can be determined and generated.
Furthermore, it is advantageous if the sleeve-shaped element forming the flange is fixable on the bearing ring in an axially non-adjustable manner. The sleeve-shaped element can thereby be fixedly connected to the bearing ring. If the sleeve-shaped element is configured as an axially adjustable flange, then after the desired preload is generated the sleeve-shaped element can be axially secured in order to prevent slipping of the sleeve-shaped element forming the adjustable flange during operation of the bearing.
Here the sleeve-shaped element forming the flange can be connected to the bearing ring and/or the bearing housing in an interference-fit or materially-bonded manner, in particular by laser welding. Due to the interference-fit or materially-bonded connection the sleeve-shaped element can be very quickly and reliably connected to the bearing ring or the bearing housing. Here a preferably circumferentially disposed groove can also be provided on the bearing ring and/or the bearing housing, into which the sleeve-shaped element is rolled-up and/or connected with interference-fit to the sleeve-shaped element in another manner
Moreover, if the sleeve-shaped element is configured slightly deformable at least in a partial region, in particular the region that interacts with the groove, then the sleeve-shaped element can be deformed in the region of the groove, for example, via hammering, whereby an interference fit arises. As already explained above this makes possible a simple interference-fit connection between the sleeve-shaped element and the bearing ring and/or the bearing housing.
According to a further advantageous exemplary embodiment the sleeve-shaped element forming the flange is configured at least partially hardened, in particular inductively hardened, wherein preferably an axial end region facing the rolling elements and/or a region contacting at least one seal lip is configured hardened. Since the sleeve-shaped region should preferably include a hard contact region for the roller guiding and for the abutment of the seal lip, but also a plastically deformable region for the fixing of the sleeve-shaped element on the bearing ring, an inductively hardened contact zone is favored in particular. A regionally precise hardening and a plastic deforming for an interference fit with the groove can thereby be provided.
Alternatively or additionally the sleeve-shaped element forming the flange at least partially includes, in particular on an outer surface, a wear-resistant coating. Here the axial end region facing the rolling elements and/or a region contacting the at least one seal lip preferably includes the wear-resistant coating. The wear-resistant coating can be, for example, a DLC (diamond-like carbon) layer, carbonitriding- and/or nitriding layer, but a ceramic layer, a hard-chromium layer, or another wear-resistance-promoting layer known in the prior art is also conceivable. Due to the wear-resistant coating, even with long operating durations premature signs of wear in the contact region of rolling elements or seal lips can be avoided, whereby the service life of the bearing can be increased.
A further aspect of the present disclosure relates to a method for setting a preload in a sealed rolling-element bearing, in particular a tapered roller bearing, wherein the rolling-element bearing includes two bearing rings that are configured as inner ring and outer ring and between which at least one rolling element is disposed. Furthermore, a seal assembly and an axially adjustable flange is disposed on the inner ring and/or on the outer ring, wherein the axially adjustable flange is formed by a sleeve-shaped element that simultaneously serves as contact sleeve for a seal lip of the seal assembly. The sleeve-shaped element is preferably disposed with a press-fit on or relative to the bearing ring and is displaceable on or relative to the bearing ring against a friction given by the press-fit. Here the method comprises the following steps:
disposing the sleeve-shaped element forming the flange on or relative to the bearing ring;
disposing the at least one rolling element on the inner ring;
introducing the inner ring with the at least one rolling element disposed thereon in the outer ring;
displacing the inner ring and/or the outer ring with respect to each other up to a stop of the at least one rolling element on the sleeve-shaped element;
displacing of the sleeve-shaped element on or relative to the bearing ring against the friction given by the press-fit by further displacing the inner ring and/or of the outer ring so that a predetermined preload is achieved in the tapered roller bearing;
fixing the sleeve-shaped element in the position that the sleeve-shaped element has assumed with reaching of the predetermined preload; and
applying a seal carrier with an axially extending ring arm and a radially extending annular flange, which carries a radially encircling seal with at least one seal lip, on the bearing ring opposing the sleeve-shaped element such that the seal lip sealingly contacts the sleeve-shaped element.
It is preferred here in particular if this method for preloading and sealing is used with an above-described bearing assembly.
Further advantages and advantageous embodiments are defined in the description, the drawings, and the claims. Here in particular the combinations of features specified in the description and in the drawings are purely exemplary, so that the features can also be present individually or combined in other ways.
In the following the disclosure is described in more detail with reference to the exemplary embodiments depicted in the drawings. Here the exemplary embodiments and the combinations shown in the exemplary embodiments are purely exemplary and are not intended to define the scope of the invention. This scope is defined solely by the pending claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic sectional view through a first exemplary embodiment of the disclosed bearing assembly; and
FIG. 2 is a detail view of the bearing assembly depicted in FIG. 1 .
DETAILED DESCRIPTION
In the following, identical or functionally equivalent elements are designated by the same reference numbers.
In FIG. 1 a bearing assembly 1 is depicted that includes two tapered roller bearings 2 and 3 . The two tapered roller bearings 2 , 3 each have an inner ring 4 or 5 , but a common outer ring 6 , or as depicted in FIG. 2 each have their own outer ring 6 , 7 . Rolling elements 8 or 9 are disposed between the bearing rings. Such bearing assemblies can be found in particular in wheel bearing units, wherein the bearing assemblies are fitted in a wheel hub R.
The bearing assembly depicted is embodied in a back-to-back arrangement. Flanges 10 and 11 on the inner rings 4 , 5 limit the movability of the tapered rollers 8 , 9 in the axial direction.
Here the flanges 10 , 11 are configured as sleeve-shaped elements (flange sleeves), that are pushed-on onto the bearing rings 4 , 5 . While the sleeve-shaped element 11 of the inner ring 5 is fixed on the inner ring 5 as a fixed flange, this does not apply for the sleeve-shaped element 10 that forms the flange 10 on the inner ring 4 . This sleeve-shaped element is embodied as an axially adjustable flange 10 , i.e., it can also be adjusted in the axial direction on the inner ring 4 after the assembly of bearing rings and rolling elements.
Furthermore, it can be seen from FIG. 1 that the flange sleeves 10 , 11 are simultaneously configured as contact sleeves for seal assemblies 12 , 13 . The seal assemblies 12 , 13 are configured as cassette seals and include, as can also be seen in particular in the enlarged depiction from FIG. 2 , an axially extending ring arm 14 and a radially extending annular flange 15 . Furthermore, a seal lip 16 is attached on the radially extending flange 15 , which seal lip 16 extends away from the axially extending ring arm 14 towards bearing inner ring 4 , 5 and sealingly abuts on the flange sleeves 10 , 11 . Here the seal lip 16 can also be configured as a multi-part seal lip 16 , which abuts with a first section 16 -A on an axially extending section 10 -A, 11 -A of the flange sleeve 10 , 11 , and a second section 16 -B on the section 10 -B, 11 -B of the flange sleeve 10 , 11 , which section 10 -B, 11 -B forms the flange.
Furthermore, FIG. 2 shows in particular that the flange sleeves 10 , 11 are configured with press-fit to the inner ring 4 . Here it is advantageous in particular if, as FIGS. 1 and 2 show, the inner ring 4 includes a cylindrical shoulder 18 on which the flange sleeve 10 is pushed-on under press-fit. Here during the assembly the sleeve-shaped element 11 forming the fixed flange is first pushed-on on the inner ring 5 under press-fit and fixed. This fixing can be effected via welding, in particular laser welding; however it is also possible to provide a groove 20 in the bearing inner rings 4 , 5 , into which groove 20 the flange sleeves 10 , 11 are rolled up. It is also possible to deform the flange sleeves 10 , 11 by hammer blows such that a clamping in the groove 20 occurs. In contrast, during installation, the sleeve-shaped element forming the axially adjustable flange 10 is axially displaced against the resistance of a friction between flange sleeve 10 and bearing ring 4 so that a predetermined preload can be generated in the bearing assembly.
The displacing of the sleeve-shaped element 10 forming the adjustable flange occurs here advantageously during the tightening of a shaft nut 22 , via which the inner rings 4 and 5 are fixed against each other. During the tightening of the shaft nut 22 , the rolling elements 8 , 9 are pressed-on on the outer ring 6 via the inner rings 4 , 5 . Since the press-fit of the flange sleeve 10 is usually less than the force with which the shaft nut 22 displaces the inner rings 4 , 5 into their end position, i.e., abutting each other, the flange sleeve 10 is displaced axially outward along the cylindrical shoulder 18 . However, this displacing only occurs after overcoming of the counterforce generated by the friction, so that a preload is generated that is on the scale of the friction force. A predetermined preload can thereby be defined and determined.
At the same time the two preloads, namely the preload of the bearing assembly corresponding to the preload circuit V 1 and the preload or clamping of the inner rings 4 , 5 corresponding to the preload circuit V 2 are separated from each other via the advancing of the shaft nut 22 , so that even with a later inexact installation of the inner rings 4 , 5 with respect to each other the predefined preload in the tapered roller bearing 1 itself remains.
If after advancing the shaft nut 22 the flange sleeve 10 is positioned in its end position on the cylindrical shoulder 18 , the position of the flange sleeve 10 can be fixed, for example, using an interference fit or material bonding. It is thereby ensured that even in operation a further axial displacing or loosening of the flange sleeve 10 does not occur. For this purpose, as with the fixed flange sleeve 11 on the inner ring 4 a groove 20 can be incorporated that preferably extends circumferentially about the bearing ring 4 . After achieving of the predetermined preload the flange sleeve 10 can then be rolled up into the groove 20 or deformed, for example, by hammer blows, such that a clamping of the flange sleeve 10 in the groove 20 occurs. Alternatively it is of course also possible to attach the flange sleeve 10 on the inner ring 4 in a materially-bonded manner, for example, by welding, in particular laser welding. The forming of the groove 20 can then be omitted.
In order to keep the wear on the flange sleeve 10 , 11 as low as possible it is furthermore provided that the axial flange section 10 -B, 11 -B of the flange sleeve 10 - 11 , which flange section 10 -B, 11 -B faces the rolling elements 8 , is induction-hardened. In contrast, an axial end region 10 -C, 11 -C (see FIG. 2 ) that faces away from the rolling elements 8 is not hardened. The not-hardened region 10 -C, 11 -C of the flange sleeve 10 , 11 can thereby be plastically deformed so that a deforming of material into the groove 20 is possible. It is also possible to harden the region 10 -A, 11 -A on which the seal lips 16 -A, 16 -B run. The wear in this region can thereby be reduced.
Alternatively or additionally it is possible to provide the axial flange section 10 -B, 11 -B facing the rolling elements 8 and/or the region 10 -A, 11 -B of the flange sleeves 10 - 11 , which region 10 -A, 11 -B faces the seal lips, with a wear-resistant coating. Due to this coating particularly with long operating times premature signs of wear in a contact region between the flange sleeves 10 , 11 and the rolling elements 8 or the seal lips 16 -A, 16 -B can be avoided.
Instead of disposing the flange sleeves 10 , 11 on the inner ring 4 , as is depicted in FIGS. 1 and 2 , it is of course also possible to place the flange sleeves 10 , 11 on the outer ring 6 or on a bearing housing R comprising the outer ring.
As already mentioned above the disclosed bearing assemblies are of advantage in particular in wheel bearing units wherein the tapered roller bearings are installed under a predetermined preload. Simultaneously the inner rings 4 and 5 must usually generally be brought into a tightly abutting position in order to dispose a clip ring 24 (see FIG. 1 ) between them and axially secure the two inner rings 4 and 5 with respect to each other in operation. In particular in the solutions with location rings known from the prior art this has led to the problem that in the assembly precisely defined positions of the shaft nut are necessary in order to generate a defined preload. However, since this is very complicated in terms of assembly, to date a predetermined preload has usually been omitted.
If the tapered roller bearings are also to be sealed against an external environment, it has been shown that the use of standardized cassette seals with axially adjustable flanges was often not to be realized. In particular in solutions with axially adjustable flange sleeves the seals must be specially manufactured. Due to the above-described use of the flange sleeve as seal-lip contact and rolling-element support a standardized solution can thus be provided that can also be used with axially adjustable flange sleeves. However, sealed bearings with fixed flange sleeves can also be equipped with flange sleeves, which are simultaneously configured as contact sleeves for the seal lips of the seal assembly. If the seals are not introduced as a complete assembly set, it can be advantageous to design the seal carrier such that the axial ring section is disposed on the bearing inner side and the radial flange section is disposed on the bearing outer side. The seal carrier can thereby be simply pushed-on into the bearing assembly and in particular onto the flange sleeve.
In addition to a wear-reducing coating or hardening, the service life of the seal assembly and thus of the bearing assembly can also be increased by the rotational speed of the seal lips on the flange sleeve being lower than with an abutment of the seal lips on a bearing inner ring with a flange configured in an integrated manner. The reason for this is that the outer diameter in a bearing inner ring with integrated flange corresponds to the bearing-ring thickness+the flange height. A diameter reduction due to the cylindrical shoulder 18 is omitted. However, the rotational speed of the seal lips also thereby decreases, which leads to the increased service life.
It is further noted that rolling-element bearings other than the tapered roller bearing depicted can also include a flange sleeve that simultaneously serves as contact sleeve for the seal lips of a seal assembly.
Overall with the above-described bearing assembly a sealed bearing assembly can be provided that synergistically uses one element whereby on the one hand costs are saved and on the other hand installation steps can be simplified. At the same time with axially adjustable flanges using which a predetermined precise preload is achieved in the bearing a standardizable and easy-to-install solution for a seal is also provided.
Representative, non-limiting examples of the present invention were described above in detail with reference to the attached drawings. This detailed description is merely intended to teach a person of skill in the art further details for practicing preferred aspects of the present teachings and is not intended to limit the scope of the invention. Furthermore, each of the additional features and teachings disclosed above may be utilized separately or in conjunction with other features and teachings to provide improved bearing assemblies.
Moreover, combinations of features and steps disclosed in the above detailed description may not be necessary to practice the invention in the broadest sense, and are instead taught merely to particularly describe representative examples of the invention. Furthermore, various features of the above-described representative examples, as well as the various independent and dependent claims below, may be combined in ways that are not specifically and explicitly enumerated in order to provide additional useful embodiments of the present teachings.
All features disclosed in the description and/or the claims are intended to be disclosed separately and independently from each other for the purpose of original written disclosure, as well as for the purpose of restricting the claimed subject matter, independent of the compositions of the features in the embodiments and/or the claims. In addition, all value ranges or indications of groups of entities are intended to disclose every possible intermediate value or intermediate entity for the purpose of original written disclosure, as well as for the purpose of restricting the claimed subject matter.
REFERENCE NUMBER LIST
1 Bearing assembly
2 Rolling-element bearing
3 Rolling-element bearing
4 Inner ring
5 Inner ring
6 Outer ring
7 Outer ring
8 Rolling element
9 Rolling element
10 Adjustable flange sleeve
11 Fixed flange sleeve
12 , 13 Seal assembly
14 Axial ring section
15 Radial flange
16 Seal lip
18 Cylindrical seat
20 Groove
22 Shaft nut
24 Clip ring
V 1 Preload circuit
V 2 Preload circuit
R Hub | A wheel bearing assembly for a vehicle includes at least one rolling-element bearing having a first bearing ring and a second bearing ring defining therebetween a bearing interior, rolling elements disposed in the interior, and a seal assembly for sealing the bearing assembly. The seal assembly includes a sleeve-shaped element connected to the second bearing ring such that the sleeve-shaped element rotates with the second bearing, and the sleeve-shaped element includes a flange that forms an axial stop for the rolling elements. A carrier element is connected to the first bearing ring such the carrier element rotates with the first bearing ring, and the carrier element includes a radially extending annular flange. The radially extending annular flange supports a radially encircling seal having at least one seal lip, and the seal lip extends toward the second bearing ring and sealingly abuts on the sleeve shaped element. | 5 |
This invention is the result of a contract with the Department of Energy (Contract No. W-7405-ENG-36).
BACKGROUND OF THE INVENTION
This invention relates to the art of materials science and, more particularly, to nonmetallic materials and powder metallurgy.
Ceramic materials have certain outstanding properties, such as high temperature strength, corrosion resistance, low density, and low thermal expansion, which make them attractive materials for high temperature applications. Silicon nitride (Si 3 N 4 ) is a ceramic which has a desirable combination of properties for structural use at high temperatures. These are high strength, oxidation resistance, and resistance to thermal shock. However, the fracture toughness (resistance to fracture) of Si 3 N 4 at both room temperature and elevated temperature is only moderate. Also, it is susceptible to slow crack growth at temperatures above about 1200° C.; when cracks develop, strength is degraded. Slow crack growth also is the cause of Si 3 N 4 having a relatively short stress rupture lifetime. Monolithic Si 3 N 4 is currently being tested in a fleet of automobiles as a turbocharger rotor material. Operating temperature is limited to 1000° C., which is an undesirably low temperature for this application. If the deficiencies of Si 3 N 4 can be overcome, it has the potential to become an important high temperature structural material.
There is a class of materials which offers the advantages of a ceramic and certain of the beneficial mechanical characteristics of a metal. These materials are intermetallics, which at high temperatures have the excellent properties of a ceramic, but also behave mechanically like a metal in that they show yielding and stress-relieving characteristics. Molybdenum disilicide (MoSi 2 ) is an intermetallic compound which has potential for structural use in oxidizing environments at high temperatures. It has a melting point of 2030° C. and its oxidation resistance at high temperatures is excellent, since it forms a protective SiO 2 layer. Mechanically, MoSi 2 behaves as a metal at high temperatures since it undergoes a brittle-to-ductile transition at about 900-1000° C. Thus, MoSi 2 has a stress relieving characteristic at high temperatures. These characteristics of MoSi 2 point toward its use in combination with Si 3 N 4 . Reinforcement of Si 3 N 4 with MoSi 2 particles may significantly improve the elevated temperature mechanical properties as compared to pure Si 3 N 4 . It is expected that Si 3 N 4 --MoSi 2 composites will possess improved strength, fracture toughness and resistance to crack growth at high temperatures. It is believed that above 1000° C. MoSi 2 particles will restrain initiation and propagation of brittle cracks in the ceramic matrix by means of plastic deformation energy absorption mechanisms. Such mechanisms for aluminum metal particles in glass have been shown to improve fracture toughness of the glass composite by a factor of seven. Also, because the MoSi 2 particles are a second phase reinforcement, the possibility exists for improvements in low temperature fracture toughness through toughening mechanisms such as crack deflection even though MoSi 2 is brittle at room temperature. MoSi 2 is thermodynamically stable and chemically stable with Si 3 N 4 at elevated temperature. Examples of immediate applications for the inventive materials are vehicular engine components such as turbocharger rotors, valves, swirl chambers, rocker arm tips, piston pins, and tappet faces.
Because the room temperature electrical conductivity of MoSi 2 is relatively high, it may be possible to use electrodischarge machining of the inventive composites. This method of machining is significantly less expensive than the diamond machining process which is presently used for silicon nitride. Also, though Si 3 N 4 will not couple to 2.45 GHz microwave radiation at room temperature, it is expected that the inventive composites will do so, so that microwave processing can be used in their manufacture.
SUMMARY OF THE INVENTION
This invention is compositions of matter comprised of silicon nitride and molybdenum disilicide and methods of making the compositions, where the molybdenum disilicide is present in amounts ranging from about 5 to about 50 vol %. A densification aid may be added to the mixture. The strength of a 20 vol % MoSi 2 composite is about double that of monolithic Si 3 N 4 at 1500° C.
BRIEF SUMMARY OF THE DRAWING
The drawing presents strength versus temperature of 20 vol % MoSi 2 in an Si 3 N 4 matrix and monolithic Si 3 N 4 , where both materials contain 5 wt % of a densification aid.
DESCRIPTION OF THE INVENTION
Inventive compositions were made in the following manner. MoSi 2 powder of 99.9% purity obtained from Alfa Products of Danvers, Mass. was screened to obtain powder which passed through a 400 mesh screen (opening of approximately 37 microns). The resulting -400 mesh MoSi 2 powder, Si 3 N 4 powder, and a densification agent for the Si 3 N 4 consisting of magnesium oxide were mixed in a high speed mechanical blender in the amounts required to provide the desired composition. The Si 3 N 4 powder was Grade LC-12 from the German company H. C. Starck.
The mixture was placed, in a Grafoil® lined die and hot-pressed into disks measuring approximately 31.8 mm in diameter by 6.35 mm thick. Hot pressing was performed in argon and temperatures were measured optically. The pressure applied was about 30 MPa and the specimen in the die was heated to about 1750° C., at which point heating was stopped and a hold period started. Hold time at the peak temperature of about 1750° C. and the peak pressure was about 5 minutes and then slow cooling was started, though it may be desirable to use a longer hold time of up to about eight hours. When the decreasing temperature reached 1200° C., the load was slowly removed and the specimen in the die was allowed to cool to room temperature. A coherent shape was then removed from the die. It is expected that the peak temperatures used in this process will fall within a range of about 1100° to about 2000° C. The pressure applied may be as high as 210 MPa or as low as 1.0 MPa or 0 MPa if pressureless sintering is used.
Composites were prepared which contained 5 wt % of magnesium oxide and 95 wt % of a blend consisting of 20 vol % MoSi 2 and 80 vol % Si 3 N 4 . These had a density of 96% of theoretical. Examination of the microstructure showed that the MoSi 2 particles were well distributed in the densified Si 3 N 4 matrix. X-ray diffraction analyses of the composites showed that there was no reaction between the MoSi 2 particles and the Si 3 N 4 matrix, thus indicating that there was thermodynamic stability between these species under the hot pressing conditions. No extraneous reaction phases associated with the MgO densification aid were detected by x-ray diffraction.
Elevated temperature four-point bend tests were performed on the specimens and on specimens of Si 3 N 4 with 5 wt % MgO which were hot pressed in the same manner as the inventive specimens. Test temperatures were 1200° C., 1400° C., and 1500° C. All testing was performed in air using an Instron mechanical testing unit, a MoSi 2 element furnace, SiC loading rams, and a SiC pin-Si 3 N 4 base bend test fixture. Four-point bend tests are a method for determining the strength of a material in a relatively simple and inexpensive manner. This test utilizes compressive loading, which allows the test to be easily run at high temperatures. Note that strengths of ceramics may vary widely in accordance with the type of test used to determine strength. The test equipment, methods of conducting tests, and the equation used to solve for strength values are known to those skilled in the art.
Test members in the shape of rectangular bars having the dimensions 2.5×5.1×25.4 mm long were diamond machined from the hot pressed disks. The hot pressing direction was parallel to the tensile face of the bend specimen. Two load points on a 5.1 mm wide face of the test member were 9.5 mm apart and the other two load points on the opposite face were 19.0 mm apart. Each of the tests was duplicated several times and the results reported in the Drawing are averages of several tests. The test members were soaked at temperature for about 1/2 hour to allow equilibration. The test members were loaded using a constant strain rate of 0.0508 mm/min.
The Drawing presents strength versus temperature of the specimens which were prepared. Both materials exhibited brittle behavior at 1200° C. in that the specimens fractured before they deformed. At 1400° C. and 1500° C., both materials yielded before fracture occurred and the Drawing shows yield strength. The yield strength shown for 1400° and 1500° C. is that at 0.05 mm plastic offset deviation. At 1200° C., the strength of the composite is lower than that of monolithic Si 3 N 4 , but at the two higher temperatures, the composite is stronger. At 1500° C., the strength of the inventive composites is twice that of the unreinforced material.
Pressureless sintering of a dry blend of materials may also be used to make the inventive compositions; this involves applying only heat to cause the powder to bond together to form a coherent shape. A slip casting step may be added to the process for making the compositions; this step is performed after the dry powders are mixed together. Slip casting to form a green body and then treating it by means of a size reduction process is often done to provide a more homogenous material or a material which is better adapted for hot pressing than a dry mixture of the components. This step would be performed as follows. An aqueous slip suspension containing the blended powders and having a solids loading of about 50 weight percent will be prepared. The amount of solids is not critical, but it is expected that solids loading from about 40% to about 65 wt % will be preferred. Deionized water having a pH adjusted to 9.5 with ammonium hydroxide will be used to make the slip. The pH value and the adjusting agent used are not expected to be critical. The suspension will be mechanically stirred and ultrasonified to keep the constituents from settling before casting is accomplished. The slip will be cast into a plaster of paris mold and allowed to set. The green slip cast body will be dried and then comminuted to -10 mesh (less than 2 mm) shards to yield a material suitable for hot pressing, that is, a material of particle size which will fit into and fill the die. Of course each shard, or large particle, will be substantially homogenous as a result of mixing both the starting dry materials and the suspension.
Other compounds which are known to those skilled in the art may be used as densification aids. The amount of a densification aid which is used may vary from about 0.5 to about 10 wt % of the mixture. Also, it may be desirable to obtain a relatively light composite by omitting the densification aid from the inventive compositions.
A composition of the present invention comprised of equal amounts of Si 3 N 4 and MoSi 2 is known as a cermet. It may be advantageous to prepare compositions comprised of MoSi 2 reinforced with Si 3 N 4 in amounts of about 10 vol % Si 3 N 4 or more up to the 50/50 mixture claimed herein. It is expected that MoSi 2 reinforced with Si 3 N 4 particles will have useful high temperature properties. | Compositions of matter comprised of silicon nitride and molybdenum disilicide and methods of making the compositions, where the molybdenum disilicide is present in amounts ranging from about 5 to about 50 vol. %. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a National Stage of International Patent Application No. PCT/EP2014/050128, filed on Jan. 7, 2014, which claims priority to and all the benefits of German Patent Application No. 10 2013 200 274.2, filed on Jan. 10, 2013, both of which are hereby expressly incorporated herein by reference in their entirety.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The invention relates to a method for operating an attached compactor according to the preamble of claim 1 , as well as a storage medium and an attached compactor according to the preambles of the coordinate independent Claims.
[0004] 2. Description of the Related Art
[0005] Attached compactors are known, for example, from DE 10 2009 018 490 A1 and DE 10 2008 006 211 A1. They are used as an auxiliary device for excavators, in particular in trench and pipeline construction. In conjunction with quick coupling devices and turning heads, as an inexpensive attachment device they offer a significant potential in terms of cost-saving measures and for increasing work safety, because people are no longer needed for compacting work in trenches and ditches.
[0006] DE 203 07 434 U1 discloses an attached compactor having a metering device that is not defined in greater detail, for determining the compaction state of the ground in order to be able to check whether the processed soil already has the necessary degree of compaction, or must be re-worked. U.S. Pat. No. 5,695,298 does not describe an attached compactor, but rather a roller compactor. For such a roller compactor, it is proposed that the excitation of a vibrating body be controlled such that a harmonic vibration component, having a frequency that is half of the excitation frequency, is in a predefined relation to the overall vibration. Ultimately, with this roller compactor, the vibration is thus determined as a function of a variable characterizing a harmonic distortion.
SUMMARY OF THE INVENTION
[0007] The object of the present invention is to provide a method that enables an economical operation of an attached compactor having a vibrating lower part.
[0008] The present invention overcomes the disadvantages in the related art in a method for operating an attached compactor having a vibrating lower part wherein completion of the compaction is indicated by a corresponding signal. In addition, the present invention is directed toward a storage medium wherein a computer program is stored on said medium and is programmed to execute this method.
[0009] More specifically, it is proposed that in stationary, i.e. in fixed, operation of an attached compactor having a vibrating lower part, a completion of a possible compaction is indicated by a corresponding signal. The method according to the invention thus allows the user to identify that point in time at which a further operation of the attached compactor results in no, or no substantial, further compaction of the soil. The invention can thus be summarized with the keyword “compaction completion identification.” In that said point in time is identified, an unnecessary, and thus uneconomical, operation of the attached compactor can be avoided. The soil compaction is thus accelerated, because it is possible to move more quickly to the next position where the attached compactor is to be operated. Furthermore, the service life of the attached compactor is increased, because an unnecessary operation thereof is avoided, and because an operation thereof, resulting in excess wear, on soil that has already been compacted to a maximum extent is avoided.
[0010] One possible design for the invention makes use of the knowledge that a variable, which can characterize a compaction state, e.g. a harmonic distortion, or a variable that characterizes this, or corresponds thereto, is then substantially constant on a temporal basis when the state of the soil has achieved a maximum possible compaction, such that this variable, however, likewise varies when the compaction continues to vary. It is thus proposed, according to the invention, that the temporal variation of this variable, which characterizes, or corresponds to, a compaction state or a harmonic distortion, respectively, be monitored, in that the value thereof is compared with a limit value (which may be close to zero). When the temporal variation of the variable reaches the limit value, it may be assumed that a state of a maximum compaction has been reached at the current position where the attached compactor is in operation, such that a corresponding action can be initiated. This action can amount to the attached compactor being automatically switched off, but it can also consist of the machine operator being provided with a corresponding indication thereof.
[0011] In one embodiment, a method for the operation of an attached compactor having a vibrating lower part is proposed, comprising the following steps:
[0012] a. recording a first variable, which characterizes the vibrations of the vibrating lower part;
[0013] b. determining a second variable, which can characterize a compaction state from the variable recorded in step a.
[0014] c. determining a third variable, which characterizes a temporal variation of the second variable determined in step b.
[0015] d. comparing the third variable determined in step c with a limit value; and
[0016] e. initiating an action, depending on the results of the comparison.
[0017] The term “harmonic distortion” specified in the introduction is not to be understood as limiting thereby. Any variable that varies with an increasing degree of compaction, and no longer varies when the degree of compaction also no longer increases, can be used as a variable that characterizes the compaction state, or harmonic distortion, respectively. These variables include, aside from the classic “harmonic distortion,” a “total harmonic distortion” or suchlike as well, for example, wherein there is an entire series of definitions, differing in details in the professional field, for both the harmonic distortion as well as the total harmonic distortion. Furthermore, it is to be understood that one of the fundamental aspects of the method according to the invention is the fact that compaction with an attached compactor having a vibrating lower part, in the form of a compacting plate, for example, occurs in a spatially stationary manner, thus, a first surface, or the contents of the spatial region lying thereunder, is first compacted until a maximum compaction has been achieved, and then a subsequent surface, or the contents of the spatial region lying thereunder, is compacted, and so on.
[0018] It is furthermore worth noting that the method according to the invention can also be used when the load with which the supporting vehicle (e.g. an excavator arm of an excavator) pushes the attached compactor against the soil is not known. The reason for this that, although the absolute value, e.g. the harmonic distortion, is dependent on said load, this is not the case, however, for its temporal variation with the increasing extent of compaction.
[0019] In still another embodiment of the method, it is proposed that in step d of the method, in which the third variable, determined in step c, is compared with a limit value, this third variable is compared with a limit value and then in step e, when the limit value has been reached and/or the third variable falls below the limit value, a signal is generated that can be perceived by an operator. This development is useful, in particular, when a harmonic distortion or a total harmonic distortion is used as the second variable. The limit value can only be slightly above or below zero in practice, because a temporal variation from zero means that no further compaction will be obtained. The generation of a signal that can be perceived by the operator allows the operator to freely decide if, for some reason, the attached compactor should then be continued to be operated, for example, for it to be simply moved to the next compaction site without shutting it off. It is understood that then, when an inverted variable is used for the third variable, rather than testing to see if the variable falls below the limit value, an exceeding of the limit value must be tested for.
[0020] The signal can be perceived acoustically, visually and/or in a tactile manner thereby. In the simplest case, the signal is simply a light signal generated, for example, by a lamp, or a sound signal generated, for example, by a load speaker, or a vibratory signal on an operating handle with which the operator controls the attached compactor. The signal can be generated directly on the attached compactor thereby, or in a cab on the supporting vehicle to which the attached compactor is attached. In the latter case it is conceivable that a wireless data transfer from the attached compactor to the supporting vehicle occurs, by radio signals or infrared, for example.
[0021] It is furthermore proposed that then, when the limit value has not been reached, a current frequency of the vibrating lower part is determined from the first variable and indicated to the operator.
[0022] According to the invention, the method can include the additional supplementary steps: comparing the second variable determined in step b with a limit value; suspending the processing of steps c to e as long as the second variable is less than the limit value. This further development can be summarized with the keyword “idle detection.”
[0023] An idling state exists then when the attached compactor is in operation, that is, the eccentric drive is powered, but the vibrating lower part does not rest on the compacted soil. This is the case, for example, during the moving of the attached compactor from one compaction surface to the next. When the attached compactor is raised, it is clear that no compaction occurs, such that the variable determined in step c of the method according to the invention must be, at least substantially, equal to zero. In order to prevent coming to the conclusion as a result, that a supposed completion of the compaction has been reached, this state is detected with the additional method steps proposed here, and the indication of a supposed completion of compaction is suppressed.
[0024] This is based on the physical knowledge that in the idling state the vibrations of the vibrating lower part substantially correspond to the harmonic vibration of the eccentric drive, thus exhibiting hardly any harmonics. A harmonic distortion or a total harmonic distortion in this case is quite large. An idling can be reliably detected using this further development according to the invention, as is the case, for example, when the attached compactor is raised away from the soil for cleaning purposes. Here as well it is to be understood that then, when an inverse variable is used for the third variable, rather than testing to see if the variable has fallen below a limit value, an exceeding of the limit value is to be tested for.
[0025] The second variable can be determined in a particularly simple manner using a Fourier analysis.
[0026] In still another possible embodiment, the invention is distinguished in that the attached compactor has a power generator for supplying at least the sensor, which is powered, at least indirectly, by a drive motor for the eccentric drive. A power generator of this type can be a classic generator, for example, which is coupled to a shaft of the hydraulic drive motor. The use of a so-called “energy harvester” is also an option, however, which generates power from the vibrations of the vibrating lower part.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Other advantages of the invention will be readily appreciated as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings, wherein:
[0028] FIG. 1 is a side view of an attached compactor and an excavator;
[0029] FIG. 2 is a diagram, in which the amplitudes of a fundamental vibration and two harmonic vibrations of a vibrating lower part in the form of a compactor plate of the attached compactor from FIG. 1 are plotted over time; and
[0030] FIG. 3 is a flow chart for a method for operating the attached compactor from FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
[0031] In FIG. 1 , an attached compactor is generally indicated at 10 . It is connected to an arm 11 of an excavator 14 via a hydraulic quick coupling device 12 . The attached compactor 10 includes a turning device 16 , beneath the quick coupler 12 in FIG. 1 . The underside thereof is connected to an upper part 18 , which is connected to a lower part 22 via elastic coupling elements 20 .
[0032] The lower part 22 includes, in turn, a vibrating lower part in the form of a compactor plate 24 , on which an eccentric device 26 is disposed. This includes a hydraulic drive motor, not shown in detail, which is connected, via a shaft, running perpendicular to the drawing plane of the Figure, to a mass disposed eccentrically in relation to the shaft axis. Furthermore, the eccentric device 26 has a generator, which provides electrical power for the components of the attached compactor 10 .
[0033] The attached compactor is mechanically connected not only to the arm 11 of the excavator 14 via the quick coupler 12 , but also to the hydraulic supply lines of the excavator 14 . On one hand, the turning device 16 , and on the other hand, the eccentric device 26 , are controlled via these lines. When the attached compactor 10 is in operation, the upper part 18 and the lower part 22 can be rotated by the turning device 16 about an axis of rotation 28 that is orthogonal to the plane of the compactor plate 24 . A sinusoidal force component, orthogonal to the plane of the compactor plate 24 , is generated on the compactor plate 24 by operation of the eccentric device 26 . When the operator starts up the attached compactor 10 , and presses it against the soil 30 that is to be compacted at a specific location 32 via the excavator arm 11 , the spatial region 34 lying beneath the compactor plate 24 is compacted.
[0034] The attached compactor 10 depicted in FIG. 1 can be used, in particular, in canalization, in earth-moving, as well as with back filling. It is particularly important in these situations to ensure that a certain compaction of the spatial region 34 is achieved. It is frequently the case thereby that a maximum possible compaction is desired. Soils are frequently used in these situations that cannot be used, for example, for the construction of a road surface, such as soils that are not frost-proof and are less resistant to sliding, in particular fine grained and mixed grained soils, as well as rock fills.
[0035] In order to indicate to the operator of the excavator 14 functioning as the supporting vehicle that an at least substantially, maximum possible compaction state has been obtained in the spatial region 34 , the attached compactor 10 has a device that indicates to the operator when said maximum possible compaction has been obtained. This device, as a whole, has the reference numeral 36 in FIG. 1 .
[0036] It includes a sensor 38 , which is rigidly coupled to the compactor plate 24 , and with which the amplitudes and frequency of the vibrations of the compactor plate 24 can be detected in a direction orthogonal to the plane of the compactor plate 24 . The device 36 further includes an electronic processing device 40 , disposed in the region of the upper part 18 of the attached compactor 10 in the present embodiment, and which receives the signal from the sensor 38 , and processes said signal in accordance with a method described below in detail (in an embodiment that is not shown, the processing device 40 is disposed in the lower part ( 22 ). For this, the processing device 40 has a storage medium on which a computer program is stored, which is programmed for executing said method. Electrical power is supplied to the processing device 40 from the generator for the eccentric device 26 mentioned above. The device 36 also has a signal lamp 42 , attached to the upper surface of the upper part 18 , and connected to the processing device 40 .
[0037] In one embodiment that is not shown, only the sensor 38 for the device is disposed on the attached compactor 10 . The processing device 40 , on the other hand, is disposed directly in the cab 44 of the excavator 14 , as is also the case with the signal lamp 42 . The signal from the sensor 38 is transmitted to the processing device 40 in this case in a wireless manner.
[0038] The method, according to which the device 36 functions, and which is executed in the processing device 40 in accordance with the computer program stored therein, shall now be explained in detail with reference to the attached FIGS. 2 and 3 .
[0039] The sinusoidal course of the fundamental vibration of the compactor plate 24 is shown in FIG. 2 , with the reference numeral 46 , for a full period thereof. The ordinate indicates the amplitude A thereby, the abscissa indicates time. This fundamental vibration is present when the attached compactor 10 is operated without a load, that is, when it is not pressed against the soil 30 with the excavator arm 11 . An amplitude of the fundamental vibration 46 is indicated in FIG. 2 by A 46 .
[0040] When the attached compactor 10 is pressed against the soil 30 by the excavator arm 11 , in order to compact the spatial region 34 lying beneath the compactor plate 24 , the vibrational behavior of the compactor plate 24 varies. Instead of the harmonic fundamental vibration 46 , there is now a distorted fundamental vibration 46 ′, which is depicted, for one half of a period, in an exemplary manner in FIG. 2 , by a broken line. This distorted fundamental vibration 46 ′ can, for example, can be divided in turn, by use of a Fourier analysis, into the harmonic fundamental vibration 46 and numerous harmonic vibrations 48 i (i=a, b, c, . . . ). This is shown in an exemplary manner in FIG. 2 for the first two harmonic vibrations 48 a and 48 b. The harmonic vibration 48 a has an amplitude A 48a , the harmonic vibration 48 b has an amplitude A 48b .
[0041] The physical circumstances specified above are employed in the processing device 40 for executing a method, which shall now be explained in reference to FIG. 3 . The method starts in a start Block 50 . In Block 52 a harmonic distortion K is determined from the signal 54 from the sensor 38 . The harmonic distortion K is the quotient of the sums of the amplitudes A, of the harmonics of the vibration of the compactor plate 24 and the amplitude A of the fundamental vibration, according to the following equation:
[0000]
K
=
∑
A
i
2
A
2
[0000] For the example depicted in FIG. 2 , the following equation is obtained:
[0000]
K
=
A
48
a
2
+
A
48
b
2
A
46
2
[0042] Instead of the harmonic distortion K, any other variable could be determined in Block 52 that varies with the compaction state of the spatial region 34 . This also includes, by way of example, a total harmonic distortion.
[0043] The determined harmonic distortion K is compared in Block 56 with a limit value G 1 . If the harmonic distortion K is less than the limit value G 1 , the program jumps to Block 58 . If the harmonic distortion K is greater than or equal to the limit value G 1 , the program jumps to Block 60 . With the comparison in Block 56 , it is detected whether the attached compactor 10 is pressed by the excavator arm 11 against the soil 30 , or whether it is raised above the soil 30 , thus in a so-called “idling operation.” This occurs, for example, when the attached compactor 10 is moved from the position 32 after successful compaction to an adjacent position 32 , or when it is being cleaned.
[0044] If the attached compactor 10 does not rest against the soil 30 with the compactor plate 24 , then for all practical purposes, there are no relevant harmonics 48 i, or the amplitudes Ai thereof are only very small. This results in a very small harmonic distortion K, which is detected by the comparison in Block 56 . The limit value G 1 is selected such that there is a greater probability that the compactor is in an idling operation. It may, for example, lie in the range of 0.2. In this case, simply the current vibrational frequency of the compactor plate 24 is indicated in Block 58 by a corresponding display device.
[0045] If the compactor is not in idling operation, an actual checking of whether the maximum compaction of the spatial region 34 has been obtained occurs in Block 60 . For this, the temporal division dK/dt of the harmonic distortion K, that is, the temporal variation of the harmonic distortion, is first determined. This temporal variation dK/dt is then compared with a limit value G 2 . If the temporal variation dK/dt is greater than the limit value, the program jumps to Block 58 , referred to above. If the temporal variation dK/dt is less than or equal to the limit value G 2 , however, it may be assumed that the maximum possible compaction of the spatial region 34 has been achieved, and this is visually indicated to the operator in Block 62 by a corresponding activation of the signal lamp 42 . Additionally, or alternatively, an acoustic signal may be emitted, by a signal sound, for example, or a tactile signal may be emitted, by a vibrating of a control element in the cab 44 , for example. The method ends in Block 64 .
[0046] The comparison in Block 60 results in the following: the absolute value of the harmonic distortion K is directly dependent on the current compaction state of the spatial region 34 , when the pressure force form the attached compactor 10 by the excavator arm 11 against the soil 30 at the position 32 is constant. Because this compaction state varies during the compaction, the harmonic distortion K also varies. If a state of an at least substantially maximum compaction of the spatial region 34 has been obtained, the density of the soil within the spatial region 34 no longer varies, and thus the harmonic distortion K also no longer varies. In this case the temporal derivation dK/dt of the harmonic distortion K thus approaches zero. This is detected by the comparison with the limit value G 2 , which for practical purposes is selected such that it is close to zero.
[0047] The invention has been described in an illustrative manner. It is to be understood that the terminology which has been used is intended to be in the nature of words of description rather than of limitation. Many modifications and variations of the invention are possible in light of the above teachings. Therefore, within the scope of the appended claims, the invention may be practiced other than as specifically described. | In a method for spatially fixed operation of an attached compactor having a vibrating lower section it is proposed such that an end of a possible compaction be indicated by a corresponding signal. | 4 |
PRIORITY INFORMATION
[0001] This application claims priority from U.S. Provisional Patent Application No. 60/976,069 filed Sep. 28, 2007.
FIELD OF THE INVENTION
[0002] The present invention relates to the field of microsystems and devices. The present invention in particular relates to an apparatus comprising an array of devices for applying strain to a material and methods of using said apparatus. The present invention includes applications in the fields of biomedical engineering.
BACKGROUND OF THE INVENTION
[0003] High-throughput screening (HTS) is a method used in life science research and the biopharmaceutical industry for drug discovery, toxicology testing, and functional genomics. Typically, HTS is used to rapidly determine the physiological response of groups of cells to various combinations and quantities of biologically active chemical compounds and biomaterials surrounding the cell.
[0004] Cellular activity is also influenced by applied mechanical stimulation, which has been shown to have a strong impact on biological function in certain types of cells (McBeath, et al., Dev. Cell 2004; Wang & Thampatty, Biomech Model Mechanobiol 2006; Saha et al., J Cell Physiol, 2006). Existing experimental techniques are unable to adequately characterize cellular response to varying degrees of mechanical stimulation with a high accuracy in a high-throughput manner. These limitations have prevented systematic investigations into the effects of mechanical stimuli on cell behaviour and hindered discovery of new control strategies for cell-based therapies.
[0005] Furthermore, despite the demonstrated individual importance of mechanical forces; chemical cues; and the composition and structure of surrounding biomaterials in regulated cellular function, the lack of HTS techniques for mechanical factors precludes the ability to effectively study combinations of these various parameters. This patent application discloses a system designed to meet this need for rapidly probing either single cells or colonies of cells.
[0006] Existing low-throughput experimental techniques in this field make use of three main mechanical loading schemes to probe cellular response: compressive loading, deformation of the substrate to which cells adhere, and fluid flow-induced shear stresses. U.S. Pat. No. 6,048,723 discloses a flexible bottom culture plate for applying mechanical loads to cell culture; U.S. Pat. No. 6,218,178 discloses the loading assembly for the plates of U.S. Pat. No. 6,048,723; U.S. Pat. No. 6,645,759 discloses a device for growing cells in culture under shear stress and/or strain; and U.S. Pat. No. 6,037,141 discloses a system for culturing cells under compression conditions. However, the systems described the cited US patents are all low-throughput, applying a single strain across at most, six experimental locations. This drawback significantly impacts the time required to perform such studies. It also precludes the ability to perform combinatorial manipulation of chemical and mechanical parameters, as can be performed in our disclosed invention.
[0007] Moreover, there are two modes of cell culture: two-dimensional culture on a flat surface, and three-dimensional culture within a porous biomaterial. Each of these culture techniques and loading scenarios provide insight into the inner workings of the cell, but typically require radically different experimental setups.
[0008] Microsystems are engineered systems with critical structural or functional features of micrometers, where the microfabricated component of the system typically ranges in size from millimeters to centimeters. They have such advantages as low cost, small size, minimal reagent consumption and fast response time. Because of the reduced system footprint, a dense array of functional sub-units is possible, and as such they are ideal for developing array based HTS systems. Similarities between system feature sizes and the size of a cell make this technology suitable for developing HTS systems for single- or multi-cell biology. Advances in microfabrication have enabled the rapid development of complex, elastomeric, monolithic polymer structures with well-defined features with a resolution of micrometers. To provide an example, these techniques—termed Multilayer Soft Lithography (MSL)—have been used to develop a fully controllable microfluidic network, actuated by a number of 2-state valves (Unger et al., “Monolithic microfabricated valves and pumps by multilayer soft lithography,” Science, vol. 288, pp. 113-6, Apr. 7 2000; and U.S. Pat. No. 6,793,75).
[0009] In view of the foregoing, an improved apparatus, system and method for HTS applications is desirable.
[0010] The disclosed invention introduces new aspects in MSL device development, including the use of mechanical solid elements in an all-polymer device, and the application of a single pressure load to obtain a range of mechanical activity.
SUMMARY OF THE INVENTION
[0011] The present invention relates to an apparatus for applying mechanical forces of varying magnitudes to a material and methods of using said apparatus.
[0012] In one aspect, the present invention is an apparatus for applying mechanical forces of varying magnitudes to a material characterized in that the apparatus comprises at least one array defining a surface and a plurality of actuation devices disposed thereon, each of said actuation devices having a structural configuration, said structural configuration including an opening; and a flexible membrane fixed to the surface and covering said opening, said membrane having an upper surface that permits attachment of the material thereto, wherein the array is structured to enable pressure or vacuum to be delivered to the plurality of actuation devices, and wherein the array is further structured to enable variation of said structural configuration from actuation device to actuation device such that the delivery of pressure or vacuum to the plurality of actuation devices results in application of varying magnitudes of mechanical force to the material by means of actuation of the flexible membrane covering said openings_based on the structural configuration thereof.
[0013] In one aspect the strain fields produced by the mechanical, forces on the material comprise non-uniform strain fields of varying magnitudes on the material.
[0014] In another aspect, the present invention is an apparatus for applying mechanical forces of varying magnitudes to a material comprising at least one array defining a surface and a plurality of actuation devices disposed thereon, each of said actuation devices having a structural configuration, said structural configuration including: (i) a base including a first opening, (ii) a flexible actuation membrane fixed to the base and covering said first opening, said actuation membrane having an upper surface; and (iii) an upper structure resting on said upper surface of the actuation membrane and including a second opening that opens on the surface; a moving member extending from the upper surface of the actuation membrane into the upper structure towards the second opening; a substrate membrane fixed to the surface and covering said second opening, said substrate membrane having an upper surface that permits attachment of the material thereto, wherein the array is structured to enable pressure or vacuum to be delivered to the plurality of actuation devices, and wherein the array is further structured to enable variation of said structural configuration from actuation device to actuation device such that the delivery of pressure or vacuum to the plurality of actuation devices results in application of varying magnitudes of mechanical force to the material by means of actuation of the actuation membrane covering said first openings based on the structural configuration thereof thereby moving said moving member to direct the mechanical force to the material.
[0015] In one aspect of the disclosed invention, the strain fields comprise various uniform strain fields of varying magnitudes on the material.
[0016] In yet another aspect of the invention is an apparatus for applying mechanical forces of varying magnitudes to a material characterized in that the apparatus comprises: at least one array defining a surface and a plurality of actuation devices disposed thereon, each of said actuation devices having a structural configuration, said structural configuration including an opening; a flexible membrane fixed to the surface and covering said opening, said membrane having an upper surface; a moving member extending from the upper side of the membrane and having a top that permits attachment of the material thereto; and a weight means, wherein the array is structured to enable pressure or vacuum to be delivered to the plurality of actuation devices, and wherein the array is further structured to enable variation of said structural configuration from actuation device to actuation device such that the delivery of pressure or vacuum to the plurality of actuation devices results in application of varying magnitudes of mechanical force to the material by means of actuation of the flexible membrane covering said openings based on the structural configuration thereof thereby moving said moving member to compress the material against the weight means.
[0017] In a further aspect of the present invention is a method of high-throughput screening responses of a material to mechanical forces of varying magnitudes, characterised in that the method comprises: providing an apparatus of the invention; delivering pressure or vacuum to the apparatus; and measuring the effect of said mechanical forces on the material.
[0018] Non-limiting advantages of the apparatus of the present invention include an apparatus that allows high-throughput screening and large out-of-plane actuation distances, which are difficult to achieve in a traditional low-throughput apparatus. Another advantage of the apparatus of the present invention comprises the capability of translating a single input pressure into mechanical forces of varying magnitudes. Yet another advantage of the present invention includes a single apparatus capable of delivering mechanical stimulation and chemical stimulation simultaneously to a material of interest. Yet another advantage of the present invention includes a single apparatus capable of delivering a number of mechanical loading schemes simultaneously to a material of interest. Other advantages of the present invention will become apparent in the description of this invention.
BRIEF DESCRIPTION OF DRAWINGS
[0019] FIG. 1A : illustrates a radial distribution network of channels to supply pressure or lubricant to individual units in the microfabricated array.
[0020] FIG. 1B : illustrates a branching distribution network of channels to supply pressure or lubricant to individual units in the microfabricated array.
[0021] FIG. 2 : top-down schematic of the non-uniform substrate strain embodiment of the invention, illustrating the varying size of the actuation cavities across the array.
[0022] FIG. 3 : cross-sectional view of non-uniform substrate strain embodiment of the invention, illustrating the actuation cavity, and polymeric thin film.
[0023] FIG. 4 : demonstrates the working principles of this embodiment of the invention. Increases in actuation cavity size create different vertical displacements.
[0024] FIG. 5 : Finite element simulations displaying radial and circumferential strains obtained across the radius of bulged films of different sizes.
[0025] FIG. 6 : Picture of sample microfabricated device for the substrate strain embodiment of the invention.
[0026] FIG. 7 : Image of the non-uniform substrate strain microsystem in the cell culture incubator, with associated peripheral devices (including pump, valves and controllers).
[0027] FIG. 8 : Graph presenting results for percentage of cells expressing alpha-smooth muscle actin across the mechanically active culture regions of the array.
[0028] FIG. 9 : illustrates the working principles of the uniform substrate strain embodiment of the invention. As pressure is applied to the actuation cavity beneath the support layer, the loading post is driven upwards into the culture membrane.
[0029] FIG. 10 : demonstrates the working principles of this embodiment of the invention. Increases in actuation cavity size create increases in vertical displacements of the loading post, for a given applied pressure.
[0030] FIG. 11A-F : Sequence of images from the finite element analyses performed for this embodiment of the device.
[0031] FIG. 12 : Graphical representation of the radial and circumferential strains obtained across the surface of the device, for different sizes of actuation cavity, for a circular loading post profile.
[0032] FIG. 13 : Finite element simulation results for a square loading post profile.
[0033] FIG. 14A-E : demonstrates variations in various segments of the material area.
[0034] FIG. 15A : illustrates the 5×5 array produced as an example of this embodiment of the invention.
[0035] FIG. 15B : top down view of the example array fabricated as an embodiment of this invention.
[0036] FIG. 15C : images of the device at rest and while actuated.
[0037] FIG. 16 : example of a larger array for the uniform substrate-strain embodiment of this invention.
[0038] FIG. 17 : illustrates the displacement of fluorescent beads on the surface of the membrane, used to calibrate the strains produced by the device.
[0039] FIG. 18 : Graph representing radial and circumferential strains results obtained from analysis of the fluorescent bead displacements.
[0040] FIG. 19 : Graph presenting results for the fluorescent bead calibration across the array.
[0041] FIG. 20 : Fluorescently stained image where Blue=Hoechst nuclear stain, and Red=BrdU stain for proliferating cells.
[0042] FIG. 21 : Graph presenting results for the fraction of proliferating cells across mechanically active culture regions of the array.
[0043] FIG. 22 : Schematic illustrating the incorporation of microfluidic channels to deliver and control available chemical factors.
[0044] FIG. 23A , B: illustrates the procedure by which hydrogels can be micropatterned onto the device, creating an array of three dimensional constructs.
[0045] FIG. 24A , B: Schematic illustrating compressive loading of the constructs.
[0046] FIG. 25 : Image demonstrating micropatterning of polyethylene glycol into an array of hydrogel cylinders.
[0047] FIG. 26 : Cross-sectional view of the hydrogel cylinders fabricated.
[0048] FIG. 27 : Schematic of peripheral setups for each embodiment of the invention.
[0049] In the drawings, one or more embodiments of the present invention are illustrated by way of example. It is to be expressly understood that the description and drawings are only for the purpose of illustration and as an aid to understanding, and are not intended as a definition of the limits of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0050] The present invention is particularly useful for applying a range of mechanical forces to a material across length scales on the order of micrometers and millimeters. This novel actuation scheme is versatile, and can be used in several configurations and for various purposes. Examples related to uniform and non-uniform substrate-stretch and tissue construct deformation with multiple loading modes are outlined in this disclosed invention. The various embodiments of the invention can be used to apply: (a) non-uniform strain fields of varying magnitudes to a material sample of interest; (b) uniform strain fields of varying magnitudes to a material sample of interest; and (c) compressive stresses of varying magnitudes to a three-dimensional construct.
[0051] Commonalities between each of the embodiments will be described first, followed by details relevant to specific configurations.
[0052] “Material” as used herein should be understood to indicate any material of interest, including without limitation organic and inorganic materials, films, a combination of multiple substances into an aggregate mixture, cells, tissues, organs, cell cultures.
[0053] The major structural components of the apparatus may be made, for example, from polydimethylsiloxane (PDMS, Sylgard 184, Dow-Corning). The apparatus of the invention may be fabricated using principles of multilayer soft lithography (MSL) in several layers, each layer is formed by casting the liquid prepolymer onto a negative relief mold. The layers are then aligned and bonded to create complex multilevel structures. The integration of other membrane types is also permitted through the use of uncured PDMS as an adhesive layer. Through such bonding techniques, when the material to be tested include cell cultures, membranes of other polymers, including but not limited to polyurethane, polyacrylamide, or a custom-designed polymer membrane can be used as a substrate for the cell culture. The inventors have successfully demonstrated this technique to integrate alternative materials into the PDMS fabrication process with membranes of polydimethylsiloxane and polyurethane. Although not necessary for the utility of the present invention, limiting these membranes to optically transparent materials enables the use of inverted microscopy, a standard tool in biology labs used to visually examine cells and to observe fluorescent reporters and reagents. The transparent feature is advantageous because it enables spatially and temporally heterogeneous cell responses to be visually detected, which is not possible if an assay only measures the end-point response of the entire population, as is typical with HTS.
[0054] The apparatus of the present invention allows for large out-of-plane actuation distances, which are difficult to achieve in a traditional microdevice. Although the magnitude of strain fields can be varied by changing the pressure applied, this would require several external pump systems, to obtain a variety of strain magnitudes in one device. The present inventors have solved the problem of requiring several external pump systems by providing a mechanical design solution. In order to apply a range of mechanical forces across the microfabricated array in each of the embodiments, variations in geometry are employed. A single external pressure and vacuum source is connected to the apparatus of the invention, which by means of a network of microfabricated channels delivers pressure or vacuum to each of the individual units (also known as “actuation devices”) in the array. FIG. 1A and FIG. 1B illustrate examples of such pressure delivery channel network 22 . Variations in geometric dimensions of individual units 10 in the array are used to vary the amount of mechanical force generated by that actuation device 10 . The mechanisms for generating the types of mechanical forces are outlined in the following embodiments.
[0055] In one aspect the present invention is an apparatus for applying mechanical forces of varying magnitudes to a material characterized in that the apparatus comprises: at least one array defining a surface and a plurality of actuation devices disposed thereon, each of said actuation devices having a structural configuration, said structural configuration including an opening; and a flexible membrane fixed to the surface and covering said opening, said membrane having an upper surface that permits attachment of the material thereto, wherein the array is structured to enable pressure or vacuum to be delivered to the plurality of actuation devices, and wherein the array is further structured to enable variation of said structural configuration from actuation device to actuation device such that the delivery of pressure or vacuum to the plurality of actuation devices results in application of varying magnitudes of mechanical force to the material by means of actuation of the flexible membrane covering said openings_based on the structural configuration thereof.
[0056] A top-down schematic of the array 1 is shown in FIG. 2 . A cross-sectional view of a single actuation device 10 in the array 1 is provided in FIG. 3 , showing the single unit 10 in the array 1 at rest. The actuation device 10 comprises a structural configuration including an opening 9 . The actuation device 10 includes an actuation cavity 18 including a cavity wall 12 having a thickness 13 and a bottom wall 14 . A flexible membrane 20 is fixed to the array surface (not shown) and covering the opening 9 . The flexible membrane 20 has an upper surface 21 that permits attachment of a material of interest. In one aspect the flexible membrane 20 comprises a thin polymer film. Applying a positive or negative pressure within the actuation cavity 18 bows the thin film 20 upwards or downwards. FIG. 4 illustrates the use of variation in geometry to provide different non-uniform strain fields. The left side of the figure shows cross-sectional views of actuation devices with two dimensions of the actuation cavity 18 . A pair of dimensions are used merely for illustration purposes. The right side of the figure shows the effect of varying actuation cavity 18 geometry on the bending applied to the thin polymeric film 20 under the same positive pressure. By increasing the thickness 13 of the cavity wall 12 the unsupported membrane 20 over the actuation cavity 18 increases, the stiffness of that membrane 20 decreases, and the membrane 20 is bowed further. FIG. 5 shows finite element simulation results for various actuation geometries of a circular unit. The results show non-uniform strain fields in the radial and circumferential directions of the polymeric film 20 . The finite element analysis shown in FIG. 5 simulates a circular membrane being deformed by a pressure applied beneath it. These simulations were conducted using the same applied pressure for circular membranes of various dimensions, ranging from diameters of 500 μm to 1.6 mm in 100 μm increments. A three-quarter view of a representative simulation is provided to better illustrate the function of this embodiment. Radial and circumferential strains across the surface of the membrane are presented in graphical form. The results indicate non-uniform strain fields across the surface of the membrane, with unequal radial and circumferential components of the applied strains.
[0057] To demonstrate the applicability of the first embodiment of the present invention, FIG. 6 depicts an apparatus 5 of the present invention having circular actuation cavities 18 , however other obvious patterns may be used ( FIG. 6 ). In the apparatus of FIG. 6 , the circular actuation cavities 18 are used to provide strain fields similar to those shown in the finite element simulations of FIG. 5 . However, various strain fields can also be generated by changing the shape of the actuation cavity 18 . This requires no change to the actual manufacturing process of the apparatus, and can be achieved by modifying the template used to build the apparatus. The sample apparatus 5 of FIG. 6 shows six isolated, identical groups, each of which contains twenty mechanically active actuation sites 10 . By applying a single positive pressure to the entire apparatus 5 (not shown), the channel network 22 delivers the pressure from a source of pressure to each of the mechanically active actuation sites 10 in all the isolated groups, bowing the membranes, the out-of-plane displacement of which is commensurate with the actuation cavity geometry. In this example, polyurethane films are bonded to the surface of the PDMS device.
[0058] In one non-limiting example the experimental setup of FIG. 6 is being used to apply a range of non-uniform strain fields to adherent biological cells cultured on the surface of the array 1 . The setup shown in a cell culture incubator is shown in FIG. 7 . The well 7 shown in the apparatus 5 is used to hold cell culture media, which allows the array 1 in the apparatus 5 to respond to a specific set of chemical factors in the culture media. In this specific example extra-cellular matrix (ECM) proteins are deposited by adsorption on the surface of the polyhrethane films—these ECM proteins can include but are not limited to collagen (Types I-IV), fibronectin, laminin, vinculin and heparin. Each array 1 in each apparatus 5 can be patterned with a different ECM protein at different concentrations. A further extension to this example would be achieved by employing well-established techniques for protein patterning, such as those described in R. S. Kane et al., “Patterning proteins and cells using soft lithography,” Biomaterials , vol. 20, pp. 2363-2376, December 1999, which can be used to deposit on each actuation site 10 in the array 1 various types and concentrations of proteins. This will allow control over extra-cellular matrix composition for individual bioreactor units.
[0059] Specific to this particular experiment, subcultured porcine aortic valvular interstitial cells (PAVICs) isolated from pig heart valve leaflets were seeded on the surface of the array and allowed to attach and spread without mechanical stimulation. This was achieved using standard cell culture techniques. Initial experiments involved applying a cyclic mechanical deformation to the film upon which the cells were attached, over a period of two days. Analysis of the effects of mechanical stimulation involve staining the cells for the presence of a-smooth muscle actin (αSMA), a mechanosensitive cytoskeletal protein. Fluorescent imaging and analysis yielded results shown in FIG. 8 for the percentage of cells expressing αSMA from the total population on each experimental unit. This experiment demonstrates the practicality of collecting data on biological cell response through fluorescent imaging techniques. Various other combinations of ECM proteins, culture media composition and mechanical stimulation to tease out differences in biological activity in response to varying non-uniform strain fields may be studied with the use of the apparatus of the present invention.
[0060] The apparatus of the present invention is useful to probe all adherent cell types, including but not limited to heterogeneous cell populations, stem cells, progenitor cells, primary isolates, and cell lines, which has broad scope for use in experiments in biomedical research. Possible applications include determining the effects of various external stimuli in combination with non-uniform cyclic mechanical strain on cells, including but not limited to levels of drug uptake, efficacy of gene therapy, receptor formation, cytokine production, proliferation, apoptosis, structural reorganization, morphology, gene and protein expression, and differentiation on a large number of cell types from various model organisms.
[0061] The apparatus of the present invention could also be used to applying varying non-uniform strains to native tissue samples, cells encapsulated in a thin membrane, or as a material testing unit for thin polymer films. This last application is of particular relevance to the materials science community, looking for novel experimental methods to test mechanical properties of thin films, membranes and biological tissue samples, which have been shown to have different properties than when in their bulk forms. Previously patented techniques include mechanical characterization through laser excitation (U.S. Pat. No. 5,672,830); microindentation using piezoelectric positioners (U.S. Pat. No. 5,553,486). These techniques are serial in nature, and cannot collect data quickly. A more recent attempt to create a high-throughput system has been patented (U.S. Pat. No. 6,772,642), in which an array of samples is tested by a positionable force generator. However, data collection is still serial.
[0062] This potential setup has the advantage of higher throughput over current attempts—a series of data for responses to a range of mechanical forces is collected simultaneously. In one aspect a sample of the material of interest, such as a thin membrane of the material or biological tissue to be studied is bonded by an adhesive agent to the surface of an array and suspended over a series of actuation devices with increasing radii. By applying a controlled positive pressure and determining the vertical displacement of the membrane, the stiffness and Young's modulus of the film can be determined. Increasing the pressure to breakage determines ultimate stress properties of the material. Continuous cycling of the pressure source determines fatigue, elasticity and plasticity. Because of the device throughput, a great deal of data for various stresses can be obtained simultaneously.
[0063] FIGS. 9 through 13 depict the mechanical principles of the second embodiment of the present invention. With reference to FIG. 9 , each actuation device 110 comprises: a base 120 including a first opening 121 and comprising a first actuation cavity 126 including a cavity wall 122 having a thickness 123 and a bottom wall 124 . The said cavity wall 122 has an upper end 128 configured to fix a flexible actuation membrane 130 that covers the opening 121 , said actuation membrane 130 having an upper side 132 ; an upper structure 140 comprising a side wall 142 that ends on the array surface 144 , a second opening 146 and a second cavity 148 . A substrate membrane 220 is fixed to the surface 144 and covers the second opening 146 . The substrate membrane 220 is configured to support a material of interest 222 across the opening 146 ; a post 160 extending from the upper side 132 of the actuation membrane 130 into the second cavity 148 towards the second opening 146 .
[0064] As a non-limiting example, FIG. 9 demonstrates the principle for applying a substrate-induced deformation to adherent cells in a two-dimensional culture. The upper diagram illustrates the cross-sectional view of a single unit of the actuation device 110 at rest. The actuation membrane 130 then bows upwards, driving the post 160 up into the substrate membrane 220 , atop which adherent cells 222 are cultured. The culture membrane 220 then slips and stretches over the raised loading post 160 , creating a uniform strain field, the features of which depends on the geometry of the loading post 160 . Examples include but are not limited to: a circular post, which will create a cylindrical equibiaxial strain field; a square post which will create an equibiaxial strain field; and a rectangular post which will create an anisotropic biaxial strain field, approaching uniaxial strains. As in the previous embodiment, this embodiment of the system can be used to probe all adherent cell types, including but not limited to heterogeneous cell populations, stem cells, progenitor cells, primary isolates, and cell lines.
[0065] The use of varying geometry to change mechanical forces applied is demonstrated in FIG. 10 , which uses the substrate-stretch embodiment of this invention as a descriptive aid. The right half of the image depicts a cross-sectional view of the actuation device 110 with no external positive pressure applied (at rest). The device 110 of lower quadrant of FIG. 10 features a much larger size actuation cavity 126 than the upper quadrant of FIG. 10 . As the size of the unsupported actuation membrane 130 increases, the stiffness of the membrane 130 decreases, and the post 160 is vertically displaced further. In this way, by varying the lateral geometry of the system, the vertical actuation distance is varied for a fixed applied pressure, and hence the strains generated in the culture membrane 220 are also varied. The magnitudes of generated strain fields are limited by the material's ultimate elastic strain: preliminary finite element simulations indicate a range from 0-5% strain for our specific initial design—however, based on experimental results, the design can be realistically adjusted to provide mechanical stimulation ranging from 0 to approximately 20% strain.
[0066] To better illustrate the mechanical actuation of the system, a sequence of images taken from a finite element simulation have been included. The simulation depicts a circular loading post as an example, in a substrate-stretch configuration. The simulation assumes frictionless interaction between the post and the membrane. The images shown in FIG. 11A-F show how the post is driven up into the membrane, causing stretch to occur. Note that this sequence is not indicative of any specific elapsed time. The quantitative results for this simulation are shown in FIG. 12 . The radial and circumferential strains along the membrane surface are graphically displayed. This exercise confirms an equibiaxial stretch for this particular situation, and indicates a region of uniform strain within the radius of the loading post. Two-dimensional simulations were also performed for a square post geometry: results for a section of square post geometries indicate similarly uniform results, and are shown in FIG. 13 .
[0067] The fabrication process for this second embodiment of the device 110 may be based on known standard processes of multilayer soft lithography. No claims of novelty are made on these techniques. Essentially, a negative relief mold is created for each layer of the device, again by standard processes. Two examples are provided for illustration and not, limitation. The first is the use of Microchem's SU-8 negative photoresist to pattern molds of various thicknesses. Alternatively, silicon micromachining in a silicon-on-insulator wafer can be used with Deep Reactive Ion Etching to create molds with vertical side walls and flat bottoms. A liquid prepolymer (for example, PDMS) is poured over the mold and temperature-cured. The PDMS can then be peeled off the mold and it retains the microscale features. PDMS can also be spin coated on a second mold, resulting in a very thin patterned film. Alternatively, the technique developed by Jo et al., (B. H. Jo, L. M. Van Lerberghe, K. M. Motsegood, and D. J. Beebe, “Three-dimensional micro-channel fabrication in polydimethylsiloxane (PDMS) elastomer,” Journal of Microelectromechanical Systems , vol. 9, pp. 76-81, March 2000.) can be used in which the liquid polymer layer is squeezed in a mechanical clamp, creating a very thin film. These films are then aligned using a micromanipulator and bonded together by treating the surfaces with a corona discharge unit.
[0068] One aspect of novelty is introduced into the fabrication process. When bonding the culture membrane to the first three layers of the device, in order to prevent the partially cured culture membrane from bonding to the post, a vacuum is applied to the actuation membrane, sucking the posts away from the culture membrane. The membrane is then bonded, and cured while the actuation membrane is under vacuum. Low viscosity oil is heated to further reduce viscosity and then flushed between the post and the actuation membrane, providing a lubricating layer, and preventing excessive friction. When the vacuum is released the loading post returns to its original position, unattached to the culture membrane, and lubricated by the oil.
[0069] To illustrate the range of other design considerations encompassed by the present invention, a number of modifications have been made to the design of the device 110 , and shown in FIG. 14A-E . In FIG. 14A , a different material is used for one of the structural layers of the device 110 . FIG. 14B shows a modified structural configuration in which structural means or notches 150 extend from surface 144 of the array are used to limit vertical movement of the actuation membrane 130 . FIG. 14C incorporates the use of a ‘lip’ 162 on the loading post 160 to reduce the friction between the post and the culture membrane 220 , by reducing the total area of contact. FIG. 14D demonstrates one of the possibilities of actuation cavity geometry 170 achieved through a different fabrication process. FIG. 14E shows a post 164 profile that is different in the vertical as well as the planar directions.
[0070] To demonstrate the practicality and feasibility of such a system, a sample 5×5 array of individual units was constructed ( FIG. 15A ). Actuation of the structure is demonstrated in FIGS. 15B and C. Arrays with larger number of units can easily be fabricated ( FIG. 16 ), but for demonstration and initial experimentation purposes, a 5×5 array was used. This array has been successfully constructed with a polydimethylsiloxane culture layer, or with a polyurethane culture layer, using bonding techniques discussed previously. The density of the experimental units is equivalent to that of a 1536-well plate, which can provide a 256-fold increase over currently available substrate-stretching equipment.
[0071] In order to calibrate the strains exerted by the device, fluorescent beads, 1 micron in diameter were deposited on the surface, and imaged in a standard fluorescent microscope. The array was then actuated, and the locations of the fluorescent beads tracked, using standard image analysis techniques. The radial and circumferential strains across the surface of the membrane were then extracted from the raw displacement data, and the results plotted in FIGS. 18A and B. The graphs indicate uniform strains across the surface, and an equibiaxial condition (equal radial and circumferential strains). Deviations from uniformity can be attributed to errors in measurement of the fluorescent bead positions. The nominal strain values for the radial and circumferential axes were then tabulated for each of the differently-sized units in the array. The results for a polyurethane membrane are shown in FIG. 19 , and indicate an increasing strain level across the array, as demonstrated by simulation.
[0072] The specific application of the particular experimental setup constructed is to provide uniform substrate strains as mechanical stimuli to determine the effects on biological cells grown on the culture membrane surface. As in the first embodiment of this invention, a PDMS well is used to hold cell culture media, to control the chemical stimuli seen by the cells, and to deposit ECM proteins prior to seeding the adherent cells. Also as in the first embodiment, standard techniques can also be used to pattern ECM protein type and concentration on individual units of the array. For a demonstration experiment, a mesenchymal stem cell line (C3H10T1/2) was seeded onto a polyurethane membrane, and subjected to cyclic 1 Hz strains ranging from 0 to 8% in 2% increments. The BrdU stain for proliferating cells was then used to determine the fraction of total cells that were proliferating, for each of the mechanically active regions (sample image shown in FIG. 20 ). Obtaining fluorescent images can require purging the oil lubrication channels if the oil autofluoresces at a specific excitation wavelength. This can be done with a soap and water solution. The results, shown in FIG. 21 , demonstrate the practicality of using fluorescent analysis techniques to obtain data from cells cultured on the apparatus of the present invention.
[0073] Although the apparatus of the present invention has been used for particular applications, the description of such is not intended to limit the scope of this invention. Theoretically, any culture membrane material that can be processed into a thin film can be used on the device. Any adherent cell type can be used, and because of the 1536-well plate format, currently available robotic dispensing is capable of controlling the chemical environment for individual units within the array. Furthermore, a microfluidic network can be incorporated (as in FIG. 22 ) to deliver precise quantities and combinations of chemicals to individual cell locations. Provided the chemicals are in liquid form, they can be distributed to each individual bioreactor. Examples of such chemical stimulation can include but are not limited to growth factors, hormones, cytokines, dissolved gases, and bioactive molecules. With this configuration, the bioreactor array can combinatorially probe cellular response to various mechanical strains, chemical cues, and extra-cellular matrix compositions. Controlling the flow rate of chemicals in the microfluidic channel also allows control over shear stresses exerted on the cells. Variations in shape of the loading post can create different strain fields in the culture membrane.
[0074] With reference to FIGS. 22 through 26 in a third embodiment, the present invention discloses a modification to the structure of the device 310 , which allows compressive strains to be applied to a three-dimensional construct. This embodiment makes use of the lower portion of the above described embodiments—the culture membrane is removed entirely and the supporting structure for the culture membrane can optionally be removed. Three-dimensional constructs can then be fabricated with standard materials, including but not limited to natural or synthetic hydrogels, porous polymeric scaffolds, other tissue engineering scaffolds, biomaterials for cell encapsulation, native tissue or a custom-designed material. These constructs can be patterned and seeded with cells, using standard techniques (such as in Liu & Bhatia: “Three-dimensional Photopatterning of Hydrogels containing Living Cells”, Biomedical Microdevices, 4, p 257, 2004).
[0075] FIGS. 23A-B illustrate the process by which a patterned hydrogel is photopolymerized atop the loading posts: a cell suspension and prepolymer mixture is flushed between the loading posts and a chemically functionalized glass slide. A mask is then aligned and placed atop the glass slide. UV light is then used to photopolymerize the array over the loading posts. FIG. 24 demonstrates compressive loading of the structure. Compressive loading is achieved using the same mechanism as in the previous embodiment: a pressure-actuated loading post atop an actuation cavity of varying dimensions. The loading posts squeeze the constructs against a holding means, which in this case comprises the functionalized glass slide.
[0076] This embodiment of the system can be used to study both adherent and non-adherent cell types. Non-adherent cell types would necessitate the use of an encapsulating polymer as the construct. Obtaining this setup is achievable by a number of methods—an alternative method is provided here: A cell suspension in pre-polymer solution can be prepared and patterned onto a glass substrate. The patterned constructs are then aligned with the array and spaced by means of a gasket. The setup is then mounted in a light clamp with appropriately flexible spacers. A positive pressure applied to the actuation cavity will bow the post upwards, compressing the construct ( FIG. 24 ). Cycling the pressure will result in a dynamic, high-throughput compressive bioreactor array.
[0077] To demonstrate the practicality of this approach, an array of cells encapsulated within photopolymerizable polyethylene-glycol (PEG) constructs are photopatterned on a chemically functionalized glass slide using a standard masking technique: The unpolymerized solution is then washed away, and the results, shown in FIG. 25 demonstrate the formation of large arrays of micropatterned cylinders. FIG. 26 illustrates a side view of one of the constructs. These arrays are then aligned with the device and clamped into place using a suitable supporting structure, for dynamic mechanical compressive stimulation.
[0078] The following numbers are reasonable estimates. The strain ranges for compressive testing are estimated to range between 0 and 80%—the upper end is limited by the porosity and stiffness of the construct, and the lower limit would depend on the size of the desired construct. Tensile testing can be expected to generate strains between 0 and 200%, based on finite element results for the distention of the loading post, and the minimum size of a desirable construct.
[0079] An idealized peripheral setup and integrated system for each of the embodiments described above is outlined in FIG. 27 , which includes a computer controlled pump with a pressure sensor and valve to form a closed-loop control system for accurately applying dynamic pressures to the reactor array. The computer also controls chemical feed rates through a multichannel peristaltic or syringe pump, which provide nutrients to the cells, and can also be used to apply shear forces to each cell. The required control algorithms are simple and readily available in the public domain. The entire array is mounted in a ‘live cell’ imaging chamber, on an automated motion stage. The live-cell imaging system allows the cells to survive under a microscope for an extended period of time, and the motion stage will allow the microscope to take pictures of each unit at various time intervals. All this data can then be time-stamped and catalogued, and saved on the computer for subsequent automated or manual analysis. | The present invention details the design and operation of a miniaturized device array in which a range of simultaneous mechanical forces are produced by a single external pressure source. The invention is primarily embodied in a microfabricated device arrays designed to rapidly probe biological cell response to various combinations of mechanical, chemical and extra-cellular matrix parameters in a high-throughput fashion. | 2 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application No. 60/073,222, filed on Jan. 30, 1998 and also of U.S. Provisional Application No. 60/082,259, filed on Apr. 17, 1998.
STATEMENT OF GOVERNMENT SUPPORT
The work leading to this invention was supported by one or more grants from the U.S. Government. The U.S. Government therefore has certain rights in the invention.
FIELD OF THE INVENTION
The present invention is in the field of medical diagnostics and therapeutics. It is specifically directed to methods for detecting and treating cancer based upon the expression of the calcium-sensing receptor (CaR) in transformed tissue.
BACKGROUND OF THE INVENTION
An extracellular calcium-sensing receptor (CaR) has been cloned from both bovine and human parathyroids, as well as from human kidney tissue and rat brain (Pollak, et al., Cell 75:1297-1303 (1993); Aida, et al., Biochem. Biophys. Res. Commun . 214:524-529 (1995); Ruat, et al., Proc. Nat'l Acad. Sci. USA 92:3161-3165 (1995)). This receptor appears to play a key role in regulating extracellular calcium homeostasis (Pollak, et al., Nature Genet . 8:303-307 (1994); Pollak, et al., J. Clin. Invest . 93:1108-1112 (1994)).
Previous studies have suggested that calcium may be important in processes leading to tumor formation and spread. For example, it is known that cancerous breast and brain tissue tends to form microcalcifications (Galkin, et al. Radiology 124:245-249 (1977)) and calcium has been shown to stimulate cellular division and differentiation. Defining the relationship between calcium and tumor cell biology may lead to new clinical approaches to treating cancer patients. The present invention is based upon the discovery that CaR, a primary regulator of calcium, is expressed at abnormal levels in human tumors. This has led to the development of new diagnostic and therapeutic methods.
SUMMARY OF THE INVENTION
The present invention is directed to a method for treating cancer in a human patient by administering a ligand that binds with specificity to CaR. Specific conditions that may be treated in this manner include breast cancer, prostate cancer, multiple myeloma, brain tumors, Leydig cell tumors, colon cancer, renal cell carcinoma, cervical cancer, ovarian cancer, vulvar cancer, skin cancer, esophageal cancer, lung cancer and cancers of the head or neck. For the purposes of the present invention, a ligand “binds with specificity” if it has at least a hundred-fold greater affinity for CaR than for any other protein. It is expected that some cancers will respond to calcium agonists whereas others will respond to calcium antagonists. The preferred calcium agonists are those agents described in PCT/US93/01642 and U.S. Pat. No. 5,688,938 (particularly the compound designated as NPS S-568). Other examples of calcium agonists that may be used include protamine and neomycin. An example of a calcium antagonist that may be administered to patients is suramin. However, other small molecular weight antagonists may be developed that will offer advantages over suramin and be preferred.
The calcium ligand should be administered at a dosage and for a duration sufficient to produce an improvement in one or more of the symptoms associated with the cancer being treated. Examples of such symptomatic improvement include a stabilization or reduction in tumor size or growth, a reduction in metastases, a normalization of calcium metabolism as reflected in parameters such as blood or tissue calcium concentrations, rate of bone resorption, etc. It has been discovered that CaR-specific ligands may be used to inhibit the production of parathyroid hormone related peptide (PTH-RP). Thus, antagonists may be given to a patient with cancer at a dosage sufficient to reduce plasma levels of PTH-RP and thereby reduce symptoms associated with aberrant calcium metabolism, particularly excessive bone resorption, or hypercalcemia.
The present invention is also directed to a method for detecting neoplastically transformed cells in a human patient by quantitating the number of CaR receptors present in test tissue, e.g. tissue obtained at biopsy, and comparing the results to those obtained from tissue known to be normal. The presence of transformed cells is indicated by a statistically significant increase or decrease in receptor number. One way to determine receptor number is by carrying out a binding assay using a detectably labeled ligand that binds with specificity to CaR. In a preferred embodiment, the ligand used in this method is a CaR-specific antibody. Biopsy tissue for use in the method includes tissue from the breast, prostate, brain, lung, cervix, ovary, colon or tissue comprised of Leydig cells. In the case of tissue from the colon, the presence of transformed cells is indicated by a lower number of CaR receptors compared to the number of CaR receptors in normal colon tissue.
In another aspect, the present invention is directed to a method for determining whether an abnormal growth, typically a tumor-like mass, in a human patient is cancerous. This is accomplished by administering a compound that binds with specificity to the calcium-sensing receptor and that is labeled with an agent that allows the compound to be detected using in vivo imaging techniques such as X-rays, sonograms, CAT scans, or magnetic resonance imaging. The extent to which the detectably labeled compound of step a) becomes localized in the abnormal growth is then determined and compared with the amount in tissue known to be noncancerous. If the amount of labeled compound in the abnormal growth is present at a statistically higher or lower level than the amount found in the nontransformed tissue, this is an indication that the abnormal growth is cancerous. It is expected that this method will be especially useful in determining whether a lump in a woman's breast is a cyst or a cancerous growth. The method may also be used to examine abnormal growths from the colon, lung, or brain.
In other work, it has been discovered that, when the calcium-sensing receptor is activated, cells become more resistant to apoptosis. This suggests two ways in which agents that interact with CaR may be used to augment the action of chemotherapeutic agents. In cases where a patient is treated with a chemotherapeutic agent that acts by inducing apoptosis in cancer cells, the method may be improved by the coadministration of a CaR antagonist. The antagonist should be administered at a dosage sufficient to sensitize the cancer cells, i.e. to induce a statistically significant higher percentage of the cells to undergo apoptosis in response to a fixed concentration of chemotherapeutic agent. Any method may be used to determine whether a given dosage of antagonist has caused apoptotic activity in cells to change. For example, cells may be stained and examined microscopically to determine the percentage with an apoptotic morphology (nuclear and cytoplasmic condensation, nuclear fragmentation, membrane blebbing, and apoptotic body formation). By performing such an assay both before and after the administration of CaR antagonist, one can determine if a statistically significant change has occurred.
In cases where a patient is treated with a chemotherapeutic agent that acts by some means other than inducing apoptosis in cancer cells but which induces apoptosis in normal cells as a side effect, the method may be improved by the coadministration of a CaR agonist. The agonist should be administered at a dosage effective to make cells more resistant to apoptosis. In this manner, the therapeutic efficacy of a treatment may be maintained while its undesirable side effects are decreased. In addition the invention includes the compositions that are used in the methods. Thus, it includes both compositions comprising a cancer chemotherapeutic agent and a CaR antagonist and compositions comprising a cancer chemotherapeutic agent and a CaR agonist.
The present invention encompasses not only a method for augmenting cancer chemotherapy as discussed above, but also, more generally, a method of altering the sensitivity of the cells of a mammal to apoptosis by administering an effective dose of a ligand that binds with specificity to the CaR receptor. Thus, CaR agonists and antagonists may be used in the treatment of diseases characterized by abnormal apoptotic activity, including autoimmune diseases and AIDS. The agents should be given at a dosage effective to cause an improvement in at least one symptom associated with the disease treated following the basic guidelines discussed in connection with cancer chemotherapy.
DETAILED DESCRIPTION OF THE INVENTION
Cancer patients, particularly patients with multiple myeloma or tumors of the breast, prostate, brain, colon, kidney, ovary, cervix, esophagus, skin or lung, may be treated by administering a ligand specific for CaR. Depending upon the particular cancer being treated, either antagonists or agonists of calcium may be effective. Thus, a physician should begin by administering a low dose of either an agonist such as protamine or neomycin, or an antagonist, such as suramin. A determination should then be made as to whether there is an improvement in one or more of the symptoms associated with the cancer. An improvement would be evidenced by a reduction in tumor growth, a reduction in tumor size, a reduction in the number of metastases associated with the tumor, improved calcium balance within the patient's blood, reduced bone absorption of calcium, or in an improvement in any other clinical parameter typically associated with cancer patients. If no response is seen at the initial dosage, it may be then raised until a maximum is reached. For example, a physician may begin by initially administering suramin at a dosage of 1 nmol/kg/day and increase the dosage up to a maximum of 1 μmol/kg/day. During this time, the symptoms of the patient would be periodically evaluated. If no improvement was observed over a period of, for example, three months, the patient may be switched to a calcium agonist and the procedure repeated. These are, of course, simply guidelines. Actual dosages will be carefully selected and titrated by the attending physician based upon clinical factors unique to each patient. The optimal daily dose will be determined by methods known in the art and will be influenced by factors such as the age of the patient, disease state, side effects associated with the particular agent being administered and other clinically relevant factors.
The present invention is not limited to any particular dosage form or route of administration. Although oral administration will generally be most convenient, the invention is compatible with parenteral, transdermal, sublingual, buccal, or implantable routes of administration as well. Agents may be given in a substantially purified form or, preferably, as part of a pharmaceutical composition containing one or more excipients or flavoring agents. The preparations may be solid or liquid and take any of the pharmaceutical forms presently used in medicine, e.g., tablets, gel capsules, granules, suppositories, transdermal compositions or injectable preparations. The active ingredient or ingredients may be incorporated into dosage forms in conjunction with the vehicles which are commonly employed in pharmaceutical preparations, e.g., talc, gum arabic, lactose, starch, magnesium stearate, cocoa butter, aqueous or non-aqueous solvents, oils, paraffin derivatives, glycols, etc. Methods for preparing appropriate formulations are well known in the art (see e.g. Remington's Pharmaceutical Sciences, 16th ed., A. Oslo ed., Easton, Pa. (1980)).
Compositions may also include other active ingredients for the treatment of patients. In particular, compositions may contain cancer chemotherapeutic agents such as cisplatin, tamoxifen, paclitaxel, vincristine and vinblastin. As mentioned above, it has been found that CaR activation makes cells more resistant to apoptosis. Therefore, if a chemotherapeutic agent acts by inducing apoptosis in cancer cells, the presence of a CaR antagonist may increase its effectiveness. Alternatively, if a chemotherapeutic agent exerts its therapeutic effect in some other way but, as a side effect, induces apoptosis in normal cells, the presence of a CaR agonist may reduce this side effect without adversely affecting efficacy.
In order to determine the effect of a treatment on disease, patients should be evaluated on a regular basis over an extended period of time. It may take several weeks for the full therapeutic effect of a treatment to become apparent. The effect of treatment on apoptotic activity can be determined on biological samples obtained from the patient by staining tissue samples and examining them microscopically to look for morphological characteristics indicative of programmed cell death. Blood may be assayed for calcium levels using standard procedures and levels of PTH-RP may be determined using methods described in the art. By comparing the results obtained to those obtained in samples from normal individuals, conclusions concerning the effectiveness of a treatment may be made. The effect of treatment on tumor size, tumor growth and tumor metastasis may be determined using standard radiological procedures.
In another aspect, the present invention is directed to a method for detecting transformed cells by quantitating the number of CaR receptors present in tissues suspected of being cancerous and comparing the results with those obtained from normal tissue. The presence of a statistically significant change in the number of receptors is indicative of transformation. One method for determining the number of receptors present is to incubate biopsy tissue with a detectably labeled ligand that binds with specificity to CaR. Typically, a CaR-specific antibody will be labeled with a radioactive isotope (e.g., 125 I) or with an easily quantitatable enzyme, e.g. horseradish peroxidase. Methods for making appropriate antibodies are well known to those of skill in the art as evidenced by standard reference works such as: Harlow, et al., Antibodies, A Laboratory Manual , Cold Spring Harbor Laboratory, N.Y. (1988); Klein, Immunology: The Science of Self-Non Self Discrimination (1982); Kennett, et al., Monoclonal Antibodies and Hybridomas: A New Dimension in Biological Analyses (1980); and Campbell, “Monoclonal Antibody Technology,” in: Laboratory Techniques in Biochemistry and Molecular Biology.
The antibodies of the present invention may be used to detect the presence of CaR using any of a variety of immunoassays. For example, the antibodies may be used in radioimmunoassays or in immunometric assays, also known as “two-site” or “sandwich” assays (see Chard, “An Introduction to Radioimmune Assay and Related Techniques” in: Laboratory Techniques in Biochemistry and Molecular Biology , North Holland Publishing Co., N.Y. (1978)). Many variations of these types of assays may be employed for the detection of CaR.
The results obtained from the biopsy tissue should be compared with results obtained from tissue known to be normal. For example, the number of receptors present in prostate biopsy tissue would be compared to the number present in normal prostate tissue. Again, a statistically significant change in receptor number suggests that the biopsy tissue is cancerous.
Alternatively patients having an abnormal growth suspected of being cancerous may be directly administered a ligand that binds to CaR receptors with specificity. The ligand should be labeled with an agent that can be detected using an in vivo imaging technique and then administered to the patient. The amount of label that becomes localized within the abnormal growth may then be compared with surrounding tissue (or tissue otherwise known to be non-cancerous) to determine whether the growth is cancerous. For example, a radioactive isotope may be attached to a CaR-specific ligand and administered to a woman with a lump in her breast. The localization of radioactivity within the lump would suggest that it was cellularly dense and probably cancerous. In contrast, a lack of localization would suggest that the lump was more likely a cellularly sparse cyst. Other imaging techniques that may be used include computer assisted tomography, sonograms, nuclear imaging and magnetic resonance imaging.
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 performed 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 methods for treating cancer patients by administering ligands that bind with specificity to the calcium-sensing receptor. In addition, the invention is directed to methods for detecting transformed cells by determining the number of calcium-sensing receptors present. | 0 |
This application is a continuation of Ser. No. 09/568,022 filed May 10, 2000 now U.S. Pat. No. 6,237,776, which is a continuation of U.S. patent application Ser. No. 09/122,088 filed Jul. 24, 1988 now U.S. Pat. No. 6,092,661.
This invention relates generally to portable packs that include a cooling compartment. In particular it relates to a kind of portable pack that can be used in a number of outdoor activities, such as, for example, while golfing.
BACKGROUND OF THE INVENTION
People enjoying outdoor activities often desire refreshment. In the summer the usual desire is for something cool to drink. In the spring or fall a warm beverage or snack may be preferred. It may be that those persons wishing refreshment are a considerable distance from the nearest tea shop or refreshment stand. They may have hiked some distance, or, in the case of golf, have reached a point far out on the course. In such circumstances it is convenient to be able to take a supply of cooled or heated refreshments along, for use as desired.
Another related problem, particularly when golfing as a visitor, is that secure locker facilities may not be available. It is often uncomfortable to golf with a wallet or set of keys contained in one or another pants pocket. A golfer may wish to keep his or her valuables, such as a wallet and car keys, close at hand during a round of golf, in a container that is within the golfer's view. In recent times the growing popularity of cellular telephones has made it possible for golfers, hikers, cross country skiers, picnickers or others, to remain in touch with their business colleagues while enjoying their outdoor activities, often so smoothly that others may be scarcely aware that they are not at the office. A cellular telephone is another object that is uncomfortable to carry when golfing or skiing, for example. Cellular telephones are easily stolen and highly marketable. For both convenience of use and discouragement of theft they should be kept relatively close to the user. At the same time, the ability to carry, for example, extra golf balls, chocolate bars, or gum, and to carry a score card or map in a visible position, with enhanced accessibility are further common needs.
It may be uncomfortable, or cumbersome to having a multiplicity of objects to carry. A number of items may fit within a golf bag, along with various clubs, but the golf bag may not be sufficiently large to carry some items, and some items may risk damage if placed in the golf bag itself. Also, a golf bag is not generally a convenient place to have a cooling medium, such as ice cubes. Further, the prospect of spilling lemonade, carbonated drinks, or beer, however much by accident, inside either the golf bag amongst the woods and irons, or in a pocket of the golf bag, is not one that would be greeted with enthusiasm by many golfers. A segregated auxiliary carrying case that is separately washable, that is mountable to the golf bag, and that can be carried with it is preferable. It would be even more advantageous to have a pack that can be mounted with the golf bag when the bag is carried on a wheeled carriage or in a golf cart. In this way a golfer's hands are not further encumbered.
SUMMARY OF THE INVENTION
In a first aspect of the invention there is a pack. It has an insulated compartment, an auxiliary compartment mounted next to the insulated compartment and a mount for attaching the pack to another object. The auxiliary compartment has a receptacle of a size for receiving a telephone handset, another receptacle of a size for receiving a wallet, and a closure securable in a closed position to conceal the contents of the receptacles.
In an additional feature of that aspect of the invention, the pack has a breadth corresponding to the thickness of a golf bag. In another additional feature of that aspect of the invention, the pack has a second mount for inhibiting swaying of the pack relative to the other object. In a further additional feature of that aspect of the invention, the pack includes a see-through pocket mounted externally to the auxiliary compartment. The see-through pocket is of a size to receive a golf ball.
In another additional feature of that aspect of the invention, the pack has a leading panel for placement adjacent to the golf bag, a pair of side regions, a trailing region, a bottom and a top. A see-through pocket is mounted to one of the side regions. The see-through pocket has an access lip that has a leading portion and a trailing portion. The leading portion has a greater altitudinal dimension relative to the pocket than the trailing portion.
In a further additional feature of that aspect of the invention, the pack has a lid. The lid has a handle. The handle has a reinforced attachment to the lid, whereby, when closed, the pack can be carried by the handle.
In a still further additional feature of that aspect of the invention, the insulated compartment has a substantially impermeable liner; and the liner can be inverted to facilitate washing. In yet another additional feature, the insulating compartment has a thermal transfer medium holder, and that holder is vented.
In still another further additional feature of that aspect of the invention, the auxiliary compartment includes a key holder. In a still further feature of that additional feature, the key holder includes a lanyard secured within said auxiliary compartment.
In another aspect of the invention there is an insulated pack. It has an insulated compartment. It has a first mount, for carrying the weight of the pack. The first mount is located on an upper region of the pack and is for attaching the pack to another object. The pack also has a second mount located on a lower region of the pack for attaching to the other object at a different location than the first mount.
In an additional feature of this aspect of the invention, the pack is reinforced at the location at which the first mount is attached to it. In another additional feature of the invention, the pack is reinforced at the location at which the second mount is attached to it. In a further additional feature, the first mount is a quick release hanging mount and the second mount is a cinch strap.
In another additional feature of that aspect of the invention, the pack further comprises a soft shell wall having a leading portion, a trailing portion, a pair of side portions, and a bottom portion. The soft shell wall has an opening in the upper region. The opening has a rim. The pack has a lid for closing the opening, and an upper girth reinforcement for reinforcing the rim. It also has a lower girth reinforcement for reinforcing the lower region. In a further additional feature, the lid has a carrying handle, is moveable to a closed position, and has a securable closure whereby, when closed, the pack can be carried by the handle. In a yet further additional feature of that aspect of the invention, the soft shell wall is an insulating wall and forms the boundary of the insulated compartment. The auxiliary compartment is mounted externally of the soft shell wall.
In a yet further again additional feature of that aspect of the invention, the pack includes a see through pocket located externally on the soft shell wall and has an access opening that is tapered from a tall leading portion to a short trailing portion. In again another additional feature of that aspect of the invention, the soft shell wall is an insulating wall bounding the insulated compartment. The insulated compartment has a substantially impermeable liner mounted to the rim. The liner can be inverted to facilitate washing.
In another aspect of the invention there is a pack for mounting to a golf bag. It has an insulated compartment and an auxiliary compartment having a closure for concealing the contents thereof. It also has a first mount for carrying the vertical load of the pack located on an upper region of the pack for attaching the pack to the golf bag. There is a second mount located on a lower region of the pack for attaching to the golf bag at a different location than the first mount.
In another aspect of the invention there is an insulated pack. It has a flexible, soft shell wall structure having a flexible insulated layer, and having a bottom portion, a top portion, and a sidewall member. The sidewall member has a leading portion, a trailing portion and left and right hand side portions. The leading, trailing and left and right hand side portions extend between the top and bottom portions. The portions of the soft shell wall structure co-operate to define therewithin an insulated compartment.
The top portion includes a lid that is moveable from a closed position to an open position to give access to the insulated compartment. The sidewall member has a height and a breadth. The height is greater than the breadth, and the trailing portion is arcuate when viewed from above. A liner is mounted within the compartment to receive objects introduced when the lid is in the open position. The liner is moveable to an inverted position to facilitate washing thereof.
A lifting member is attached to the sidewall member. A secondary wall structure is mounted to the trailing portion of the sidewall member. The secondary wall structure stands outwardly of the trailing portion of the sidewall member and defines an auxiliary compartment therewithin. The secondary wall structure has an auxiliary compartment closure member operable to give access to the auxiliary compartment.
In an additional feature of that aspect of the invention, the pack further comprises an external peripheral reinforcing band extending about the sidewall member adjacent to the upper margin. In another additional feature of that aspect of the invention, the pack further comprises an external peripheral reinforcing band that extends about the sidewall member adjacent to the bottom portion of the flexible soft shell wall structure. In a further additional feature of that aspect of the invention, the lid has a hingedly mounted edge and the closure member is a tracked fastener mounted peripherally to the lid opposite to the hingedly mounted edge.
In a still further additional feature of that aspect of the invention, the lid is moveable to the closed position relative to the insulated compartment. The lid has an inside surface facing the insulated compartment when the top portion is in the closed position and has a peripheral bead formed thereabout. The bead extends downwardly relative to the inside surface of the top when the top portion is in the closed position. The sidewall member has an upwardly extending peripheral bead formed thereabout. The upwardly extending bead stands in opposition to the downwardly extending bead of the lid when the lid is in the closed position.
In still another additional feature of that aspect of the invention, the leading portion has an upper region proximate to the top portion and a lower region proximate to the bottom portion of the flexible soft shell wall structure. The upper region of the leading portion has a lateral reinforcing band mounted thereto. The lateral reinforcing band extends between the left and right hand side portions of the sidewall member.
In yet another additional feature of that aspect of the invention, the lifting member is attached to the upper region of the leading portion at an attachment location. The attachment location is reinforced by the lateral reinforcing band. In still another additional feature of that aspect of the invention, the leading portion has an upper region proximate to the top portion and a lower region proximate to the bottom portion of the flexible soft shell wall structure. The lower region of the leading portion has a lateral reinforcing band mounted thereto that extends between the left and right hand side portions of the side wall member.
In a still further additional feature of that aspect of the invention, the leading portion has an upper region proximate to the top portion and a lower region proximate to the bottom portion of the flexible soft shell wall structure. The upper region of the leading portion has an upper lateral reinforcing band extending between the left and right hand side portions of the sidewall members. The lower region of the leading portion has a lower lateral reinforcing band extending between the left and right hand side portions of the sidewall member. In yet another additional feature of that aspect of the invention, the side pocket has a leading edge, a trailing edge and an access lip extending therebetween. The trailing edge is shorter than the leading edge.
In still another additional feature of that aspect of the invention, the auxiliary compartment has a left side wall and a right side wall. The left and right side walls extend away from the trailing portion of the sidewall member. An auxiliary compartment trailing wall extends between the left and right hand side walls. The trailing wall portion has an upper region and a lower region. The upper region of the trailing wall has an upwardly extending flap. The flap has a detachable margin moveable to an open position to give access to the auxiliary compartment. The flap has an upper margin, a left hand side margin, and a right hand side margin forming an inverted U-shaped boundary along which the auxiliary compartment closure member is mounted.
In another aspect of the invention, there is a cooler. It has a top, a bottom, and an insulated sidewall extending between the top and the bottom to define an insulated compartment therewithin. The sidewall has a height and a breadth. The height is greater than the breadth. The sidewall has a first portion and a second portion. The second portion is arcuate. The first and second portions of the sidewall are connected in a manner such that the sidewall has a D-shaped cross-section. The top is attached to the first portion of the sidewall. The top is attached to the second portion of the sidewall by a releasable fastener. The releasable fastener is operable to permit the top to move to an open position relative to the insulated compartment.
In an additional feature of that aspect of the invention, there is a secondary wall structure mounted to the arcuate portion of the sidewall. The secondary wall structure defines an auxiliary compartment therewithin. The secondary wall structure has first and second side portions extending vertically along, and standing outwardly of, the arcuate portion of the sidewall. The secondary wall structure has an intermediate wall extending between the first and second side portions of the secondary wall structure. The intermediate wall has a lower portion and an upper portion. The upper portion has a flap. The flap is releasable along margins thereof to give access to the auxiliary compartment. In another additional feature of that aspect of the invention, the lower portion of the intermediate wall of the secondary wall structure has a first region attached to the arcuate portion of the sidewall and extending away therefrom. A second region extends upwardly from the first region toward the flap.
In still another additional feature of that aspect of the invention, the cooler further comprises a liner mounted inwardly of the sidewall. The liner has a peripheral margin defining an opening thereof. The peripheral margin of the liner is mounted to the sidewall. The liner is positionable within the sidewall to contain objects introduced through the opening. The liner is moveable to an inverted position, and, in the inverted position, the peripheral margin of the liner remains attached to the sidewall and the liner extends outside the insulated compartment to facilitate washing thereof.
In yet another additional feature of that aspect of the invention, The top is moveable to a closed position relative to the insulated compartment. The top has an internal surface facing the insulated compartment when the top is in the closed position and has a peripheral bead formed thereabout. The bead extends downwardly relative to the inside surface of the top when the top is in the closed position. The sidewall has an upper margin adjacent to the top. The upper margin has a peripheral bead formed thereabout. The bead stands in opposition to the downwardly extending bead of the top when the top is in the closed position.
In still another aspect of the invention, there is a cooler comprising a bottom, and a flexible insulated sidewall extending upwardly of the bottom to define an insulated compartment therewithin. The sidewall has an upper margin distant from the bottom. The bottom has, in plan view, a D-shaped periphery. The sidewall has a lower margin mated to the D-shaped periphery of the bottom. The upper margin has a first portion, and a second portion opposed to the first portion, the second portion being arcuate. The sidewall has a height and a breadth, the height being greater than the breadth. A top is attached to the first portion of the upper margin. The top is moveable to an open position to permit objects to be placed in the insulated compartment.
In an additional feature of that aspect of the invention, the cooler further comprises a liner mounted to the sidewall. The liner can be positioned within the insulated compartment. The liner is impermeable to liquids and is moveable to an inverted position. In said inverted position, a portion of said liner extends outside the compartment to facilitate washing of the liner.
In another additional feature of that aspect of the invention, the top of the cooler is moveable to a closed position relative to said insulated compartment. The top has an inside surface facing said insulated compartment when the top is in the closed position, and has a peripheral bead formed thereabout. The bead extends downwardly relative to the inside surface of the top when the top is in the closed position. The upper margin of the sidewall has an upwardly extending peripheral bead formed thereabout. The upwardly extending bead stands in opposition to the downwardly extending bead of the top when said top is in said closed position.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a perspective view of a preferred embodiment of a pack according to the present invention;
FIG. 2 is another perspective view of the pack illustrated in FIG. 1 with a lid of the pack in an open position;
FIG. 3 is a perspective view of the pack illustrated in FIG. 1 with the lid and an external compartment open;
FIG. 4 is a perspective view of another embodiment of a pack according to the present invention;
FIG. 5 illustrates, another perspective view of the pack illustrated in FIG. 4;
FIG. 6 illustrates a top view of the pack of FIG. 2, in an open state, with the pack of FIG. 4 partially nested therein; and
FIG. 7 illustrates a partial sectional view of the pack of FIG. 1 showing a detail of a coolant pouch and a detail of the wall construction of the pack.
DETAILED DESCRIPTION OF THE INVENTION
The description which follows, and the embodiments described therein, are provided by way of illustration of an example, or examples of particular embodiments of the principles of the present invention. These examples are provided for the purposes of explanation, and not of limitation, of those principles and of the invention. In the description which follows, like parts are marked throughout the specification and the drawings with the same respective reference numerals. The drawings are not necessarily to scale and in some instances proportions may have been exaggerated in order more clearly to depict certain features of the invention.
Referring to FIGS. 1-3, an insulated pack having a shape that is generally similar to a golf bag, but on a smaller scale, is shown generally as 20 . It has a leading portion 22 , a trailing portion 24 , a pair of left and right hand side portions 26 and 28 , a top portion 30 having a lid 32 , and a bottom portion 34 . The pack 20 has an insulated compartment 36 bounded by a modestly flexible soft shell insulating wall 38 , as shown in FIG. 7 . The breadth of pack 20 , that is, the overall width when viewed from the leading or trailing directions, is approximately 8.5 inches when empty. When undeformed, pack 20 has a gently bulging D-shaped cross section when seen from above, similar to a golf bag, although this may change somewhat when loaded. The breadth is roughly the same as the thickness of a middling to large size of golf bag. Referring briefly to the detail of FIG. 7, wall 38 has an outer covering 42 of webbed construction, and an internal closed cell foam layer 44 within the outer covering 42 .
Further, liner 46 is not, in the example illustrated, fixed to a bottom of the compartment 36 , but can be pulled out of the compartment 36 to an inverted position, while still remaining attached at a rim 48 , to facilitate washing, such as, for example, with soap, and to facilitate drying, to discourage the growth of fungus therein and the like. Liner 46 has a single circumferential seam to join a bottom face, and a single wall seam running from the circumferential bottom seam to rim 48 . In an optional alternative, liner 46 could be made from a polymer that has been impregnated with an antimicrobial compound prior to fabrication, a desirable feature for this kind of liner. The top of compartment 36 is formed by generally D shaped lid 32 . Lid 32 also has a through section structure of a flexible reflective inner layer 52 , a flexible skin in the nature of a canvas or webbing covering 54 , and a flexible closed cell insulation layer 55 , which is somewhat similar to layer 44 described above, captured inbetween. Lid 32 is joined to the main body of pack 20 , along the roughly straight side of the “D” shape, by a hinge in the nature of a flexible fabric hinge 56 , and a peripheral tracked closure in the nature of a zipper 58 having a pair of opposed zipper cars.
Rim 48 has a resiliently spongy beaded lip 60 wrapped within the upper edge of liner 46 , adjacent to the set of zipper teeth 59 of zipper 58 that is mounted to the main body of pack 22 . Lid 32 has a mating generally “D” shaped peripheral lip 62 immediately next to the set of zipper teeth 61 of zipper 58 mounted to lid 32 . When the zipper 58 is closed, lip 62 is drawn down to bear on the outside surface of beaded lip 60 , encouraging a sealing contact to be formed.
Within main compartment 36 a thermal transfer storage medium compartment is provided against a leading wall portion of insulating wall 38 by the use of a sack 64 for holding the thermal storage medium 66 . Thermal storage medium 66 may be used as a source of heat to be transferred into the contents of compartment 36 , that is, to maintain a warm temperature distribution in compartment 36 . Alternatively, the thermal storage medium 66 can be used as a heat sink to maintain a cool, chilled, or freezing temperature distribution in the contents of compartment 36 , as circumstances may require. Sack 64 has an array of perforations 68 to allow air to circulate through sack 64 more easily, thereby facilitating drying of the sack 64 after washing.
The pack 20 also has an auxiliary compartment in the nature of a valuables compartment 70 , that is mounted to the trailing portion 24 externally of the soft shelled insulating wall 38 . Compartment 70 has a pair of left and right hand side portions 72 and 74 that are connected to and extend vertically along, and rearwardly from the trailing portion of insulating wall 38 ; and a single piece trailing wall 76 extending between the distal extremities of side portions 72 and 74 . In the preferred embodiment wall 76 is, like the rest of cover 42 , made of a 600 denier polyester fabric, treated, as are all external surfaces of pack 20 , to be stain and water resistant. Other wall fabrics can be used, such as leather or leather-like vinyl.
Wall 76 has a lower or underside area 78 that meets, and is joined to, the trailing portion of insulating wall 38 . Underside area 78 forms the bottom of compartment 70 . Wall 76 also has a medial, outer area 80 that extends approximately two-fifths of the way up compartment 70 . An upper area 82 of wall 76 , in the nature of a flap, is contiguous with outer area 80 on one edge, and has closures on the remainder of its periphery. Two of those closures are left and right hand vertical zippers, 84 and 86 , that join with the uppermost pails of the distal edges of side portions 72 and 74 . The third is a hook and eye fabric closure 88 for releasably attaching an end lip 90 of wall 76 to insulated wall 38 just below rim 48 .
Referring to FIG. 3, in which closures 84 , 86 and 88 are undone, and upper area 82 lies open, a first receptacle, in the nature of a soft sided, durable fabric pocket 92 with a covering flap 94 has a horizontal hook and eye fastener part 96 mounted on its underside just inside its lip, for mating with a vertically aligned mating hook and eye fabric fastener part 98 , the combination of orientations providing an adjustable size, and flexibility inclosure position. Pocket 92 is of a size for carrying a cellular telephone handset, having a girth of approximately 5.5 inches comprised of approximately 1.25 inches deep sides and approximately 3.0 inches width and a depth of approximately 6.5 inches from bottom to lip. The interior of pocket 92 is lined with a cushioning material. Pocket 92 can be used for other objects than cellular telephones such as for sunglasses, a glasses case, and the like.
An adjacent receptacle in the nature of a soft-sided, open top pocket 94 , without cover, has a convenient size of approximately 4-5 inches in girth and approximately 5.5 inches in depth for holding a deodorant container, or other object of similar size. It can, for example, be used as a storage space for a carrying strap. Adjacent to pocket 94 is a key holder in the nature of a lanyard 96 having one end fastened within compartment 70 just below rim 48 . At its other, depending end lanyard 96 has a quick-release spring clip 98 for hooking about the ring of a key chain. Use of a strap, such as lanyard 96 , makes it easy to retrieve keys, rather than having to fish around the bottom of compartment 70 . The remaining enclosed space within medial outer area 80 and above underside area 78 has a height of approximately 4 inches, and a width of approximately 7 inches between the piping along the outer edges of side portions 72 and 74 , leaving space for a wallet, or other items.
Other arrangements of closures are possible for auxiliary compartment 70 . A single three sided zipper closure, with one or two zipper cars could be used, and the hook and eye fastener eliminated. Other kinds of fasteners, such as laces and grommets, interference fit seals, snaps, buttons, and the like are possible. The present arrangement is preferred.
Similarly, other arrangements of receptacles and key holders, or like items can be used, although the present configuration is convenient, and preferred.
A vented, see-through pocket 100 is mounted externally to medial outer area 80 , and is of a size for accommodating, for example, extra golf balls, gum, candy bars or other items. Open form mesh 102 permits objects in pocket 100 to dry more easily. Pocket 100 is closed by a sliding closure in the form of zipper 104 .
A main attachment, suitable, for example, for hanging pack 20 from a golf bag, or for clipping pack 20 to a golf bag or golf cart, is shown as a quick release brass hook fitting 110 is mounted to an upper region of pack 20 on leading portion 22 . Hook fitting 110 is free to revolve within its hinge fitting 112 , which itself is able to swing up and down within the confines of a broad loop of webbing 114 .
A second attachment, suitable for tightening to another fastening location of a golf bag or golf cart, in the nature of an adjustable cinch strap 116 is mounted to a lower region of pack 20 , also on leading portion 22 . Strap 116 has a releasable catch 118 , and can be used to tighten the lower region of pack 20 to a golf bag, golf cart, or other object, to restrain its swaying motion about the main attachment at hook fitting 110 .
It is anticipated that a significant use of main insulated compartment 36 will be for carrying cans of liquid, such as carbonated beverages, fruit drinks, or beer, whether or not accompanied by ice cubes or crushed ice. Inasmuch as the preferred is embodiment illustrated has a capacity of 12 cans of 385 milliliters and ice, a load of 10 to 12 pounds (50 to 55 N) would not be unexpected. The height of the preferred embodiment illustrated to the lip of rim 48 is approximately 12 inches. Liner 46 is not taut when lying against the inner walls of compartment 36 . That is, liner 46 has some slack, and is somewhat elastic in any event. Consequently load is taken up primarily, if not entirely, in soft shelled insulating wall 38 , and more specifically, principally in outer covering 42 of wall 38 .
The main attachment at hook fitting 110 is able to carry the entire weight of pack 20 , and the second attachment at cinch strap 116 inhibits swaying of pack 20 about the first attachment. Outer covering 42 has an upper reinforcing band 120 extending externally about the periphery of insulating wall 38 next to rim 48 . A lower reinforcing band 122 extends externally about the bottom edge of pack 20 where leading portion 22 , trailing portion 24 , and side portions 26 and 28 meet bottom portion 34 , that is to say, about the lower region of pack 20 .
A pair of left and right hand web doublers 124 and 126 commence at a relatively high location at the leading edges of respective side portions 26 and 28 , extend across the surface of those sides, and terminate at a lower location on the trailing edge of side portions 26 and 28 . That is, they extend from the leading edge of the upper region to the trailing edge of a lower region of pack 20 .
The attachment of hook fitting 110 to pack 20 is reinforced by an upper lateral reinforcing band 130 , in addition to upper reinforcing band 120 , the effect being to spread the stress concentration out. Lateral reinforcing band 130 ends at the leading edges of side portions 26 and 28 , close to the leading ends of doublers 124 and 126 , yielding a reinforced load path between the lower region of pack 20 and hook fitting 110 .
Similarly, each end of cinch strap 116 is sewn under a vertical left or right hand root reinforcement 132 or 134 , each of these in turn leading to either lower reinforcing band 122 or a lower lateral reinforcement band 136 , whose ends reach to the leading edges of side portions 26 and 28 .
For ease and comfort of carrying pack 20 by hand, lid 32 is provided with a carrying handle 140 having a padded bail 142 , and a pair of webbing feet 144 and 146 that extend filly to opposite points on the periphery of lid 32 , such that loads carried through handle 140 are transmitted not only through the outer covering layer of lid 32 but also through the reinforcement of feet 144 and 146 . At the edge of lid 32 the presence of upper reinforcing band 122 helps to spread the load more evenly to and from the vertical sidewalls formed by portions 22 , 24 , 26 , and 28 . Alternatively, pack 20 can be carried by a shoulder strap 148 fastened by spring clips to D-shaped rings 150 and 152 , mounted on either of sides 26 and 28 .
Left hand side portion 26 is provided with a trapezoidally shaped external pocket 154 having a breathing, see-through mesh 156 similar to mesh 102 . A scorecard, or map, placed in this pocket can be seen for retrieval. Lip 158 of pocket 154 is set on a rake angle, yielding a somewhat larger opening for sliding a scorecard in, without having as carefully to fit it into a narrow opening as might otherwise be the case for a square cut pocket.
Referring to FIGS. 4 and 5, a second insulated pack, is shown generally as 170 . In this embodiment, pack 170 is of a size for carrying 5 cans. It has a leading portion 172 , a trailing portion 174 , a pair of left and right hand side portions 176 and 178 , a top portion 180 having a lid 182 , and a bottom portion 184 . The pack 170 has an insulated compartment 186 bounded by a modestly flexible soft shell insulating wall 188 , whose wall construction is substantially the same as that shown in FIG. 7 and discussed above. The breadth of pack 170 , that is, the overall width when viewed from the leading or trailing directions, is approximately 6.5 inches when empty. When undeformed, pack 170 has a gently bulging D-shaped cross section when seen from above again, not dissimilar in general appearance to a golf bag. The breadth is approximately the same as the thickness of a small size of golf bag, and, is such that pack 170 can nest comfortably compartment 36 of pack 20 . This is shown in FIG. 6 .
The top of compartment 186 is formed by generally D-shaped lid 182 . Lid 182 has substantially the same layered construction as lid 32 . Lid 182 is joined to the main body of pack 170 , along the roughly straight side of the “D” shape, by a hinge in the nature of a flexible fabric hinge 206 , and a peripheral tracked closure in the nature of a zipper 208 having a pair of opposed zipper cars. The manner of closing lid 182 on compartment 186 of pack 170 is the same as for lid 36 of pack 20 . Further, the same kind of substantially impermeable liner and thermal storage medium are used. The thermal storage medium is held in a sack like sack 64 .
The insulated pack 170 also has an auxiliary compartment in the nature of a valuables compartment 220 , that is mounted to trailing portion 174 , externally of soft shelled insulating wall 188 . Compartment 220 has a generally downwardly opening, U-shaped member 221 that has pair of left and right hand side portions 222 and 224 that are connected to and extend vertically along, and rearwardly from the trailing portion of insulating wall 188 and a top cross portion 223 extending between them. Compartment 220 also has a single piece trailing wall 226 extending between the distal extremities of side portions 222 and 224 . Wall 226 is made of canvas. Wall 226 has a lower or underside area 228 , that meets and is joined to the trailing portion of insulating wall 188 . Underside area 228 forms the bottom and lower trailing face of compartment 220 . Wall 226 also has an upper area 232 , being a flap contiguous with underside area 228 on one edge. Upper area 232 has a three sided wrap-around closure, being a zipper 234 that joins the corresponding edge of U-shaped member 221 . As described above in the context of pack 20 , compartment 220 has internal receptacles lined with cushioning for receiving valuables, glasses, keys, and so on.
A main attachment, suitable, for example, for hanging pack 170 from a golf bag, or for clipping pack 170 to a golf bag or golf cart, is shown as a quick release brass hook fitting 240 , mounted to an upper region of pack 170 on leading portion 172 . Hook fitting 240 is free to revolve within its hinge fitting 242 , which itself is able to swing up and down within the confines of a broad loop of webbing 244 .
A second attachment, suitable for tightening to another fastening location of a golf bag or golf cart, in the nature of an adjustable cinch strap 246 is mounted to a lower region of pack 170 , also on leading portion 172 , but in this case being rooted at the outside edges of leading portion 172 where they meet the leading edges of side portions 176 and 178 . Strap 246 has a releasable catch 248 , and can be used to tighten the lower region of pack 170 to a golf bag, golf cart, or other object, to restrain its swaying motion about the main attachment at hook fitting 240 .
Outer covering 192 has an upper reinforcing band 250 extending externally about the periphery of insulating wall 188 next to rim 198 . A lower reinforcing band 252 extends externally about the bottom edge of pack 170 where leading portion 172 , trailing portion 174 , and side portions 176 and 178 meet bottom portion 184 , that is to say, about the lower region of pack 170 .
A pair of left and right hand doublers, 254 and 256 commence at a relatively high location at the leading edges of respective side portions 176 and 178 , extend across the surface of those sides, and terminate at a lower location on the trailing edge of side portions 176 and 178 .
The attachment of hook fitting 240 to pack 170 is reinforced by an upper lateral reinforcing band 260 , in addition to upper reinforcing band 250 , the effect being to spread the load out. Lateral reinforcing band 250 ends at the leading edges of side portions 176 and 178 , close to the leading ends of doublers 254 and 256 , yielding a reinforced load path between the lower region of pack 170 and hook fitting 240 .
Lid 182 is provided with a carrying handle 270 having a padded bail 272 , and a pair of webbing feet 274 and 276 that extend fully to opposite points on the periphery of lid 182 , such that loads carried through handle 270 are transmitted not only through the outer covering layer of lid 182 but also through the reinforcement of feet 274 and 276 . At the edge of lid 182 the presence of upper reinforcing band 252 helps to spread the load more evenly to and from the vertical sidewalls formed by portions 172 , 174 , 176 , and 178 .
Left hand side portion 176 is provided with a trapezoidally shaped external pocket 284 having a breathing, see-through mesh 286 similar to mesh 102 . Lip 288 of pocket 284 is set on a rake angle.
A preferred embodiment has been described in detail and a number of alternatives have been considered. As changes in or additions to the above described embodiments may be made without departing from the nature, spirit or scope of the invention, the invention is not to be limited by or to those details, but only by the appended claims or their equivalents. | An insulated pack has a main, insulated compartment suitable for holding refreshments at either a warmed or chilled temperature. It also has another compartment for valuables that has receptacles for such objects as cellular telephone handsets, wallets, and keys. It has a reinforced web framework structure, and a carrying handle mounted on the lid. Use of two of these packs, allows a user to keep different objects at different temperatures. The pack is particularly useful for attachment to a golf bag or golf cart to provide cool drinks during a round of golf. | 0 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims the benefit of the filing date of U.S. Provisional Patent Application No. 61/871,046 filed Aug. 28, 2013, the disclosure of which is hereby incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] With the advancement of surgical techniques and electronic components, there is a greater desire to implant such electronic components within the body of a human or other animal. However, when electronic components are to be implanted, it is important to ensure secure and safe connections among such components. For example, an implantable electronic component may be mounted within a housing and connected to a remote component by an elongated structure such as wire or cable extending through a wall of the housing. The arrangement of an elongated structure extending through the wall is commonly referred to as a “pass-through.” The pass-through is intended to provide a fluid-tight seal around the elongated structure and, in some cases, should also hold the fluid-tight structure in place relative to the wall of the housing. Moreover, a pass-through used in an implantable housing ordinarily should be biocompatible.
BRIEF SUMMARY OF THE INVENTION
[0003] One aspect of the invention provides pass-through assembly. An assembly according to this aspect of the invention desirably includes a first wall having oppositely-directed inner and outer sides. The first wall may define a first opening extending from the inner side to the outer side. The assembly desirably also includes an elongated structure extending into the opening from the outer side of the first wall, and a first material contacting the first wall and the elongated structure so as to at least partially seal the opening. The assembly also may include a second material different from the first material, the second material overlying the first material on the outer side of the wall, the second material adhering to the elongated structure and the first wall.
[0004] The second material may one or more have physical properties different from those of the first material. For example, the second material may have an elastic modulus, tensile strength, toughness or adhesion greater than the corresponding property of the first material. Merely by way of example, the first material may be a relatively soft sealant such as a silicon, for example, a biocompatible silicon or a room temperature vulcanizing (“RTV”) silicone, whereas the second material may be a material such as an epoxy which forms a secure attachment between the elongated structure and the wall. Moreover, the second material may have greater biocompatibility than the first material.
[0005] A further aspect of the invention provides methods of sealing an opening defined in a first wall of a housing. A method according to this aspect of the invention desirably includes; advancing an elongated structure through the opening; applying a first material to the first wall, the first material surrounding the elongated structure; and applying a second material atop the first material, the second material surrounding the elongated structure.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 is a perspective view of a housing assembly according to one embodiment of the invention with certain elements omitted for clarity of illustration;
[0007] FIGS. 2A-2C are plan views of the housing assembly of FIG. 1 ;
[0008] FIG. 3A is a fragmentary cross-sectional view of the housing of FIGS. 1-2C at a stage of a manufacturing process; and
[0009] FIG. 3B is a view similar to FIG. 3A depicting the housing assembly of FIGS. 1-3A in a completed state.
DETAILED DESCRIPTION
[0010] FIG. 1 is a perspective view of an implantable housing assembly 100 according to one aspect of the disclosure. The housing assembly 100 may be any shape, and in one example may have a generally rectangular shape from a plan view, with or without rounded edges, as shown in the plan view of FIGS. 2A-C . The housing assembly 100 may have a plurality of walls 110 a - d that may define a partially or completely enclosed area therebetween. Stated another way, a first wall 110 d, together with additional walls 110 a - 110 c cooperatively define a partially or completely enclosed interior space. Any of the walls 110 a - d may be integrally formed with one another, or may be detachably secured to one or more of the other walls 110 a - d.
[0011] As shown in FIGS. 2C and 3A , a wall 110 d of the housing assembly 100 may have an inner side 112 and an outer side 114 . Portions of the inner side 112 may be substantially flat. Wall 110 d may define at least one opening 116 extending entirely through the wall from the inner side 112 to the outer side 114 . The opening 116 may be generally cylindrical, or may be any other shape to accommodate an elongate structure 118 discussed further below.
[0012] The outer side 114 may define a recess 128 between ridges 129 of the housing assembly. Ridges 129 may be integral with wall 110 d or may be defined by other walls of the housing. A base portion 120 forms a floor of the recess facing outwardly. The outer side may have at least one inner ring 122 around the opening 116 , and at least one outer ring 124 around the inner ring 122 . These rings project in outwardly from the base (toward the top of the drawings in FIG. 3A ), such that an annular space 126 is formed between the inner ring and the outer ring. In the particular embodiment depicted, rings 124 and 122 are tapered in the outward direction, away from base 120 . Thus, the inner ring 122 defines a conical lead entrance to the opening 116 . The base portion 120 , rings 122 , 124 , and annular space 126 may be disposed within the recess 128 between the ridges 129 , such that the rings 122 and 124 extend outwardly from the base portion 120 but do not extend outside the recess 128 or past the ridges 129 .
[0013] The wall 110 d may be assembled to the other of the walls 110 to define a partially or completely enclosed area. In one example, electronic components, schematically depicted at 111 , may be stored therein. Such electronic components may be, for example, components for the operation of an implantable medical device, such as an implantable ventricular assist device, an implantable battery, or an implantable transcutaneous energy transfer system.
[0014] The elongated structure 118 extending though hole 116 may be a flexible wire or electrical cable that may be connected to electronic components 111 within the housing assembly 100 . Typically, the opposite end of elongated structure (not shown) is connected to other electronic components (not shown) either implanted within the body or positioned outside the body.
[0015] In an assembly process according to one aspect of the invention, one or more elongate structures 118 are inserted through the openings 116 . A first material 130 may be applied to outer side 114 . For example, as shown in FIG. 3C , the first material 130 may be applied to an exterior portion of the elongate structure 118 , atop the inner ring 122 , and at least partially within the annular space 126 . The first material 130 may also be applied at least partially within the opening 116 itself. In the embodiment shown in FIGS. 3A and 3B , the first material does not extend beyond the outer ring 124 .
[0016] The first material 130 may at least partially seal the opening 116 when the elongate structure 118 is disposed therein. The first material optionally may form a physical bond with the wall of the elongated structure 118 , with the portions of wall 110 d defining opening 116 , or both. The first material may be an RTV silicone and has a first elastic modulus.
[0017] Although only one hole is depicted in FIGS. 3A and 3B , elongated structures and first material desirably are provided for the other holes in the same manner.
[0018] A second material 140 may be applied atop the first material. The second material 140 may partially or completely cover the first material 130 within the recess 128 . In one example, the second material 140 may at least partially, but not completely, fill the recess 128 as depicted in FIG. 3B . For example, a single continuous mass or layer of second material may cover the first material at all of the openings 116 . In other examples, discrete portions of the second material are proved at each opening 116 . The second material 140 may contact each of the elongated structures and also may contact the wall 110 d as, for example, at the base portion 120 . The second material also may contact other walls of the housing. The second material 140 may form a bond with the outer surfaces of the elongated elements and with at least one wall of the housing.
[0019] Typically, both the first material and the second material are applied in a flowable condition, such as in a liquid, gel or paste-like state. One or both of the materials may be cured to a solid state after application. The curing process may involve a chemical reaction. The conditions required for curing will depend on the compositions of the materials. The curing processes may be performed sequentially, so that the first material is cured before the second material is applied, or simultaneously. Application of the first and second materials desirably takes place after insertion of elongated elements 118 through the openings 116 , and may occur before or after the elongated elements are connected to the electronic components 111 .
[0020] The second material may be different from the first material. For example, the second material may be an epoxy. The second material may have a second elastic modulus. In one example, the second elastic modulus may be different from the first elastic modulus. For example, the second elastic modulus may be greater than the first elastic modulus such that the second material is stiffer than the first material. Alternatively or additionally, the second material may have greater adhesion than the first material to the walls of the housing, to the elongated structures, or both. Also, the second material may have greater biocompatibility than the first material.
[0021] This configuration provides a secure interface at the opening 116 . In particular, the first material may be selected to provide an effective seal around the elongated components, whereas the second material may be selected to provide a secure physical attachment between the elongated elements and the wall. Moreover, the second material may have a greater degree of biocompatibility than the first material. This allows the use of a first material which provides an effective seal but may not have the desired degree of biocompatibility. The bass-through assembly limits the localized, concentrated stress and/or strain that may be placed on the elongate structure 118 while it is disposed within the opening 116 . Limiting of the stress and/or strain may prevent damage to the elongate structure 118 while it is implanted within the body of a mammal and may also prevent the elongate structure 118 from becoming disengaged with the opening 116 of the wall 110 d.
[0022] In a further variant, a third material may be applied wall 110 d, and desirably to the entire housing assembly 110 , after application of the second material. In one example, the third material is a biocompatible material in the form of a coating as schematically depicted at 137 . In this example, the third material covers the second material. The third material may be selected primarily for its biocompatibility, rather than for physical properties.
[0023] In the embodiments discussed above, the elongated structures 118 are wires or cables. However, other elongated structures such as tubes, rods or the like may be used. The pass-through assemblies can form secure attachments and seals even with flexible elongated elements which may pose difficulties with ordinary sealing and attachment techniques.
[0024] Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims. | A pass-through assembly including a first wall having oppositely-directed inner and outer sides, the first wall defining a first opening extending from the inner side to the outer side; an elongated structure extending into the opening from the outer side of the first wall; a first material contacting the first wall and the elongated structure so as to at least partially seal the opening, and a second material different from the first material, the second material overlying the first material on the outer side of the wall, the second material adhering to the elongated structure and the first wall, the second material having at least one physical property different than a corresponding physical property of the first material. | 0 |
BACKGROUND OF THE INVENTION
This invention relates generally to magnetic tape drive mechanisms, and, more particularly, to tape drive mechanisms wherein tape is driven from a supply reel to a take-up reel by an endless drive belt engaging the wound tape packs on both tape reels. Tape drive mechanisms of this general type are well known in the art and provide a relatively inexpensive and reliable tape drive device, particularly for use in the recording of digital data.
An underlying problem in such belt driven tape drive mechanisms is to provide some means for loading and unloading tapes. Since the drive belt engages the periphery of both tape packs, removal of the supply reel is no simple matter. U.S. Pat. No. 3,692,255 issued in the name of Von Behren, addresses this problem by enclosing a complete drive mechanism with supply and tack-up reels in one removable cartridge. This solution renders the cartridges extremely costly or encompasses substantial performance limitations if cost is a consideration. U.S. Pat. Nos. 4,054,923 and 4,072,279 issued in the name of Lewis, disclose a single-reel cartridge for use in a belt-driven tape transport. However, the Lewis cartridge loading mechanism is relatively complex, requiring that the supply reel be held by peripheral rollers after insertion in the mechanism. Moreover, the loading mechanism is in continuous engagement after a tape supply reel has been loaded, and it appears that this would compromise the overall performance of the tape transport.
It will be apparent from the foregoing that there is still a significant need for a belt-driven tape transport having simple and reliable means for loading a tape supply reel, and that preferably the loading means be completely disengaged during normal operation. The present invention satisfies this need.
SUMMARY OF THE INVENTION
The present invention resides in a belt-driven tape transport in which the drive belt is automatically disengaged from the tape supply reel for loading and unloading. Briefly, and in general terms, the tape transport of the invention comprises a fixed housing, a tape transport support frame mounted for sliding movement with respect to the housing, means for mounting a supply tape reel and a take-up tape reel on the frame, a drive motor and drive pulley, an endless drive belt engageable with the drive pulley and with both tape packs on the supply and take-up reels, and means for automatically disengaging the drive belt from the supply tape pack when the tape transport support frame is moved out from its housing.
More specifically, the tape transport support frame is mounted in the housing in the manner of a drawer. When the support frame is slid to a closed position with respect to the housing, the drive belt is fully engaged with both tape packs and operates in a normal manner. When the tape transport support frame is moved out from the housing, the drive belt is disengaged from the supply reel tape pack, and the supply reel may be easily removed, and a new supply reel loaded into the tape transport.
In a presently preferred embodiment of the invention, the drive belt passes around at least one roller that moves with respect to the supply reel as the tape transport support frame is moved with respect to the housing. When the support frame is moved out from the housing, the movable roller pivots about the supply reel axis and disengages the drive belt from the supply reel tape pack. At the same time, a drive belt pick-up post, attached to the housing, retains at least a portion of the drive belt in the housing and takes up slack in the drive belt as the support frame is moved outwardly with respect to the housing.
In the preferred embodiment, the movable roller is mounted on a pivot plate mounted for rotation about the axis of the supply reel, and an actuator bar is pivotally connected both to the plate and to a portion of the housing. As the support frame is moved outwardly from the housing, the actuator bar rotates the pivot plate and thereby moves the movable roller around the supply reel. The drive pulley is located between the supply reel and take-up reel, and the path of the drive belt extends around the drive pulley, around the take-up tape pack, then around two additional pulleys fixed to the support frame, around the movable roller, and finally around the supply tape pack and back to the drive pulley. The drive belt pick-up post is disposed between the two additional fixed rollers when the tape drive is in an operative position. When the support frame is moved out from the housing, the drive belt pick-up post engages the drive belt between the two fixed rollers, and retains a portion of the drive belt in the housing as the movable roller is rotated to disengage the drive belt from the supply reel.
To maintain a desired tension in the recording tape, a braking torque is applied to one or more of the rollers or to the tape reels. In the preferred embodiment of the invention, braking torque is applied to only one of the drive belt rollers, while the other rollers and the tape reels are mounted on practically frictionless bearings. The use of only one braking device allows for more convenient control and adjustment of the tape tension. Alternatively, the two tape reels can be tensioned by differential braking torques.
The tape transport of the invention may also include means for automatically threading the tape from the supply reel to the take-up reel. This threading means includes means for picking a tape leader from the supply reel, guide means for guiding the tape leader, and with it the tape, past a tape recording head and towards the take-up reel, and means for automatically engaging the leader with the take-up reel and initiating winding of the tape onto the take-up reel.
It will be appreciated from the foregoing that the present invention represents a significant advance in the field of belt-driven tape transports. In particular, the invention provides a novel technique for automatically disengaging the drive belt from the take-up reel to facilitate loading and unloading of tape. Other aspects and advantages of the invention will become apparent from the following more detailed description, taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a simplified plan view of a belt-driven tape transport embodying the present invention;
FIG. 2 is a simplified view of the tape transport of the invention illustrating an alternative braking arrangement for providing tape tension;
FIG. 3 is a bottom plan view of the tape transport of FIG. 1;
FIG. 4 is a plan view similar to FIG. 1, but drawn to a reduced scale and showing how the transport is moved for loading and unloading of tape;
FIG. 5 is a cross-sectional view of the tape transport taken substantially along the line 5--5 in FIG. 1;
FIG. 6 is an enlarged cross-sectional view taken substantially along the line 6--6 of FIG. 1;
FIG. 7 is an elevational view, partly in section, of the tape take-up reel of the invention;
FIG. 8 is simplified plan view of an end portion of the recording tape and the tape leader used in the tape transport of the present invention; and
FIG. 9 is an elevational view, partly in section, of a modified actuator bar which may be employed in the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
As shown in the drawings for purposes of illustration, the present invention is principally concerned with an improved belt-driven tape transport. A well known type of tape transport employs a resilient drive belt passing over a drive pulley and guide rollers, and engaging wound packs of tape on a supply reel and a take-up reel. When the drive pulley is rotated at a constant speed, a constant linear tape speed is obtained as the tape passes from the supply reel to the take-up reel. Tape drives of this type have the principal disadvantage that, since the drive belt is engaged with the periphery of the supply tape pack, loading and unloading of the supply reel is difficult.
In accordance with the present invention, the drive belt is automatically disengaged from the supply reel tape pack, to facilitate loading and unloading of the supply reel. As best shown in the cross-sectional view of FIG. 5, the tape transport of the invention is contained in a housing, indicated by reference numeral 10, and is mounted on a support frame 12. The support frame 12 is carried in the housing 10 by means of chassis slides 14 and 16. Thus, the support frame 12 moves slidably with respect to the housing 10 in the manner of a drawer. As will shortly become apparent, the support frame 12 is moved out from the housing 10 for loading and unloading of tape.
As shown in FIG. 1, there are two spindles 18 and 20 mounted on the support frame 12, to support a tape supply reel 22 and take-up reel 24, respectively. A span of magnetic tape 26 extending from the supply reel 22 to the take-up reel 24 passes through a tape guide channel, indicated generally by reference numeral 28. The tape guide channel 28 is defined in part by a number of irregularly shaped tape leader guide elements 32 arranged in such a manner that, when a tape leader is taken from the supply reel 22, it will be guided past the tape recording head 30 and on towards the take-up reel 24. Contained within the tape guide channel 28 are a number of tape guide pins or rollers 34, which define the path of the tape after threading through the guide block 28.
The tape is driven from the supply reel 22 to the take-up reel 24 by a drive belt 40 engaging the wound pack of tape 42 on the drive reel 22 and the wound pack of tape 44 on the take-up reel 24. Also mounted on the support frame 12 is a drive motor 46, having a drive pulley 48 which projects through the support frame 12 to engage the drive belt 40. The axis of the drive motor 46 is located approximately midway between the spindles 18 and 20, but is displaced to one side of a line between these spindles, such that the drive belt 40 passes around approximately 180 degrees of the periphery of the drive pulley 48 and engages at least 90 degrees of the periphery of each tape pack. After passing around a portion of the take-up tape pack 44, the drive belt 40 engages two rollers 50 and 52 rotatably mounted on the support framed 12, and then passes around a movable roller 54 before engaging the supply tape pack 42.
In accordance with an important aspect of the invention, the movable roller 54, in addition to being mounted for rotation on its own axis, is movable about a circular arc with respect to the spindle 18 on which the supply tape reel 22 is mounted. The movable roller 54 is rotatably mounted on a pivot plate 56 mounted beneath the support frame 12 for rotation about the same axis as the spineld 18. Thus, as the pivot plate 56 is rotated the axis of the movable roller 54 moves along an arcuate slot 58 in the support frame 12. As shown in the bottom plan view of FIG. 3, an actuating bar 60 connects the pivot plate 56 to a mounting bracket 62, which is rigidly connected to the housing 10. The actuating bar 60 is pivoted at each end and, when the support frame 12 is moved out of the housing 10, to the left as shown in the drawings, the actuating bar 60 rotates the pivot plate 56 counter-clockwise as viewed from beneath and clockwise as viewed from above in FIG. 1.
It will be seen from FIG. 1 that this movement of the movable roller 54 disengages the drive belt 40 from the supply tape pack 42. A broken line 63 in FIG. 4 indicates the new position of the drive belt 40 when the movable roller 54 has been translated all the way to the end of the arcuate slot 58. In this position, the supply reel 22 may easily be removed and replaced without interference with the drive belt 40.
To keep the drive belt 40 under tension during the loading and unloading operation, the belt drive path length is increased by means of a pair of drive belt pick-off pins 64 secured to the housing bracket 62. When the tape transport is in normal operation, the pins 66 are disposed between the two rollers 50 and 52 on the support frame and do not engage the drive belt 40. As the support frame 12 is moved out from the housing 10, the pins 64 engage a short span of the drive belt between the two rollers 50 and 52, thereby retaining the portion of the belt in the housing, as indicated by the broken lines 65 in FIG. 4. This compensates for the shortening of drive belt path length caused by movement of the movable roller 54 on withdrawal of the suppport frame 12 from the housing 10.
During the loading operation, as well as when no supply reel is loaded, the belt 40 is stretched to various degrees, but typically is stretched 20-30% less than in the normal operating position with the supply reel engaged with the belt. If the overall stretch of the belt between its operating position and its unstretched position is less than 20-30%, a modification of the actuator bar 60 will prove advantageous, to prevent the belt from falling off during the operations described above. FIG. 9 shows the modified bar, referred to as 60', which has two telescoping portions 66 and 67 biased into an extended position by a compression spring 68. Relative movement is limited by a transverse pin 69 passing through the portions 66 and 67. In the normal operating position of the drive, the spring 68 is compressed. During loading operations, if belt tension is low expansion of the spring 68 will keep the belt under increased tension.
It is important to maintain an appropriate tape tension in the tape during normal recording or playback operation. The following tape tension formula has been derived:
F.sub.tape =T.sub.50 /R.sub.50 +T.sub.52 /R.sub.52 +T.sub.54 /R.sub.54 +T.sub.22 /R.sub.42 -T.sub.24 /R.sub.44
where:
F tape =the tape tension,
T=braking torque,
R=the radius of engagement of the drive belt, and the subscripts refer to the reference numerals of the pulleys and tape reels.
In accordance with this expression, the tape tension is given by taking the sum of the quotients obtained by dividing the braking torque by the effective radius for each of the pulleys 50, 52 and 54, and for the supply reel 22, and subtracting the quotient obtained by dividing the braking torque on the take-up reel 24 by the take-up pack radius.
It is preferable to apply braking torque to only one roller or reel and to design the remaining bearings to be as frictionless as possible, as by the use of ball bearings. This allows for easier control and adjustment of the tape tension, since only a single adjustment needs to be made. As shown in FIGS. 1 and 6, for example, the pulley 52 is braked by means of a brake band 70 engaging approximately 180 degrees of a portion of the pulley 52, and a pair of adjustable springs 72 for applying a desired amount of braking torque. Alternatively, as shown in FIG. 2, the supply and take-up spindles 18 and 20, respectively, can be selectively braked by means of brake bands 74 and 76 and two pairs of springs 78 and 80.
Threading of a tape on the supply reel 22 is accomplished by conventional tape picking and threading techniques. A tape pick 80 is rotatably mounted on a shaft 82 at one end of a lever arm 84. The lever arm 84 is pivotally attached by its other end to an actuator rod 86, and pivoted at a point 88 between its ends. The actuator rod 88 is movable axially by a solenoid 90 and is biased by a tension spring 92. The pick 80 is torsionally spring-biased on its shaft 82 toward the tape pack, but is normally prevented from contacting the tape by a post 94 that it engages when the spring 92 is effective in moving the lever arm 84 counter-clockwise, as viewed in FIG. 3. When the solenoid 90 is actuated, the pick 80 is moved away from the post 94 and is biased against the tape pack. A relatively stiff leader 96 on the tape 26 is picked from the supply reel 22 and pushed through the tape guide channel 28. As the leader 96 emerges from the channel 28, it is directed toward the take-up reel 24, and is there engaged by a pinch roller 98 mounted at the end of another lever arm 100. Actuation of the solenoid 90 also rotates the lever arm 100 and moves the pinch roller 98 into engagement with the hub of the take-up reel 24. The leader 96 is retained by resilient grips 102 on the take-up reel 24, and the solenoid 90 is subsequently deactuated, to disengage the pinch roller 98 and the pick 80.
It will be appreciated from the foregoing that the present invention represents a significant advance in the field of belt-driven tape transports. In particular, the invention provides a tape transport with all the advantages of a belt-driven device, but with the added advantage of easy loading and unloading of tape. It will also be appreciated that, although a specific embodiment of the invention has been described in detail for purposes of illustration, various modifications may be made without departing from the spirit and scope of the invention. Accordingly, the invention is not to be limited except as by the appended claims. | A tape transport of the belt driven type, wherein an endless belt engages a drive pulley and peripheral portions of tape packs on a supply reel and a take-up reel. The transport is mounted on a support frame, which is in turn mounted for sliding movement in a housing. A drive belt roller is mechanically coupled to movement of the support frame, and withdrawal of the support frame from the housing results in movement of the drive belt roller and disengagement of the belt from the supply tape pack, to facilitate tape loading and unloading. Drive belt pick-off posts affixed to the housing retain a portion of the drive belt in the housing, to maintain belt tension during tape loading and unloading, and to ensure disengagement from the supply tape pack. | 6 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application claims priority from U.S. patent application Ser. No. 12/565,288, filed 23 Sep. 2009, which is a continuation from International Application under the PCT, Application No. PCT/US08/58112, filed 25 Mar. 2008, which claims priority from U.S. Provisional Patent Application 60/896,933, filed 25 Mar. 2007, which applications are hereby incorporated by reference.
BACKGROUND
Recovery of oil from oil shale involves heating the oil shale rock to sufficient temperature such that kerogen, the organic material contained in oil shale, converts to gases, liquids and residue. The residue, which may be a form of coke, is left deposited on the mineral matter of the oil shale. In the prior art the principal objectives of such processes are to (a) efficiently get the heat into the oil shale rock and (b) separate the desirable products from the spent oil shale.
The process of heating oil shale to conversion temperatures is generally called retorting, a word of European origin that describes a process for distillation or destructive distillation. The retorting process may be conducted in-situ by supplying heat to a bed of ore largely undisturbed. The retorting process may also be conducted by modified in-situ, by first preparing the bed of ore prior to heating. Retorting may also be conducted in surface vessels to which mined ore is introduced.
In the prior art, the methods for recovering oil values have exhibited various problems that adversely affect the efficiency or reliability, which in turn, adversely affect the economics. For example, vertical, solids down-flow, product up-flow processes have proven to be reliable, but yield a relatively low grade of product because the product is required to exit the reactor overhead, forcing the product to remain in the reactor longer than desirable. Vertically-inclined retorts that provide a means for removal of products from the bottom (product down-flow), and counter-currently pump the ore from the bottom by means of a ‘rock pump’ (solids up-flow) have proved to suffer from poor mechanical reliability.
Horizontally-inclined vessels, patterned after rotary kilns, suffer from slow heat transfer and result in much larger vessels than vertically-oriented vessels and are expensive to fabricate. True in-situ methods, while lower in capital costs, are not as controlled and result in uncertainty about legacy environmental issues such as ground water contamination. Modified in-situ methods experience better control than true in-situ, but might result in poorer control than surface processes. Modified in-situ processes are also likely to suffer from lower production efficiency compared to surface processes.
In historic retorting processes the production of CO 2 from decomposition of carbonate minerals was not considered an environmental issue. However, it was considered an energy consumption issue in that decarbonation is an endothermic reaction and consumes up to 8% of the energy value available from the ore. Various proposals have been made to limit the amount carbonate decomposition that gives rise to these endothermic reactions, the most common being maintaining a temperature below which decomposition occurs. However, a lower final temperature results in a lower rate of production, and possibly lower product yields.
Tar sands are also processed to recover and convert the organic materials (bitumen) to marketable products. In typical practice tar sands are mined, mixed with water, and the bitumen (tar) is separated from the sand by flotation. In yet other practice pipes are laid, or drill-holes are made into a bed of the resource and steam is injected to raise the temperature of the bed. Viscosity of the bitumen is reduced, which then drains to a second lower pipe where it is withdrawn. While practiced in rich, unconsolidated ores such as those found in Alberta, Canada, not all resources in the United States or Canada are rich or unconsolidated. Some are consolidated, with low permeability and sufficiently lean (lower grade) that only small amounts of bitumen are recovered by water extraction or will drain in a steam stimulation process. In principal, tar sands can also be retorted.
Thus, there remains a need for a process that is efficient, reliable, environmentally friendly and cost-effective for both oil shale and tar sand resources.
SUMMARY
Both the environmental problems with CO 2 production and the associated energy losses are solved by means of a three cycle system that is energy self-sufficient and thermodynamically efficient. The cycles are comprised of non-oxidative pyrolysis (NOP), oxidative combustion (OC), and environmental sequestration (ES).
An aspect is an OC cycle where metal carbonates (mostly of Ca, Mg, K, and Na) are allowed to decompose (decarbonation), but are restored to their metal carbonate form through recycle of CO 2 rich gas (recarbonation). When recycling CO 2 to the inlet of the OC cycle, the resulting recarbonation of metal oxides is exothermic, and this exothermic energy is captured by the gases and is used to raise steam. Thus, the process suffers a lower or no net energy penalty from the initial endothermic decarbonation reactions, while at the same time allowing for high temperature combustion which favors faster reaction kinetics and more efficient energy utilization.
Substantially all of the CO 2 produced from decarbonation reactions is reacted with the metal oxides to reverse the decarbonation reaction. Further, by passing the combustion gases through alkali metal oxide/carbonate beds in the OC cycle and in an ES cycle, other pollutants are sequestered. A stoichiometric excess of CO 2 , produced substantially from the combustion of organic carbon, is collected at the outlet of the ES cycle. The result is a clean, industrial grade CO 2 suitable for oil field injection, as a displacement gas for coal-bed methane, as a hydroponic gas, as an inerting gas, or any variety of industrial uses of CO 2 . Industrial grade CO 2 that displaces CO 2 produced naturally or by recovery from air serves the purpose of reducing, or at least not adding to the CO 2 that otherwise would be released. The pure CO 2 may also be sequestered in geologic formations.
Another aspect is configuring the NOP cycle such that oil is recovered from the bottom and gas is recovered from the top by using a flow of heated gas. A suitable gas is steam, because steam has a high vapor heat capacity and is readily separated from produced gases. Other gasses are contemplated, but may be less satisfactory, such as, for example, carbon dioxide, nitrogen, or light hydrocarbons of about 5 carbons or less. Oxidizing gasses cause deleterious effects on product yield and quality. Direct heating the bed using hot inert gasses also allows for precise temperature control where adequate retort rates are achieved while avoiding the premature decomposition of carbonates. Conditions are such that liquid products are not vaporized or atomized into a gas stream, but are allowed to drain through the bed where they can be withdrawn from the bottom. Withdrawing a large portion of the product as in a liquid phase provides several yield and product quality benefits over withdrawing most of the product in a gas phase.
Another aspect is to provide an ES cycle by using the spent oil shale bed as an environmental sequestration bed for oxides of N and S. Fully carbonating the ES bed also leaves a relatively pH neutral spent shale for land fill.
Another aspect is producing industrial grade CO 2 from the excess CO 2 produced. This is, in part, accomplished by producing the carbon dioxide in a separate OC cycle, where carbon dioxide is produced by combustion and metal carbonate decomposition, whereas the hydrocarbon product is produced in the NOP cycle, where product is produced under conditions where a minimum of carbon dioxide is formed. Accordingly, there is no need to separate hydrocarbon product and carbon dioxide from a single outlet steam. This allows for optimization of the hydrocarbon product without materially comprising the ability to produce a purified, industrial quality carbon dioxide product. In addition, the separate NOP and OC cycles allow for optimum removal of residual hydrocarbons from the bed without compromising the product through excess combustion of product and excess introduction of carbon dioxide into the product stream.
A purified carbon dioxide product is also largely achieved by use of the optional ES cycle, which is used to sequester undesired contaminants from the final carbon dioxide stream.
Another aspect is controlling the system for essentially energy self-sufficient operation. Once the process is started there are no external demands for power or fuel (If liquid fuels are needed additional systems can be provided, for example, an on site upgrader, and fuel preparation facility produces the needed fuels from the liquid product).
Among the advantages of the present process is its energy efficiency. Virtually all of the original energy values in the oil shale are converted to either products or heat energy. The products are high quality and the heat energy (high temperature) is high quality. Thus, utilization of the produced values is economically and thermodynamically enhanced, and losses are reduced to a minimum. Much of the original energy value of the hydrocarbonaceous materials of the ore is recovered as fluid products during the NOP cycle. Remaining energy values in the residual materials are recovered during the OC cycle where these materials are oxidized, producing a high-temperature effluent gas from which heat is recovered by steam production, or the like. Energy consumed by decarbonation of metal carbonates to metal oxides in the OC cycle is recovered by recycling carbon dioxide back into the bed under conditions to convert the metal oxides back to metal carbonates, producing heat that is passed into the effluent gas.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a flow sheet of illustrated an ore treating process.
FIG. 2 is in five parts, FIG. 2A to 2E . When 2 B, 2 C, 2 D, and 2 E are arranged as in 2 A, they show a mass balance diagram illustrating an exemplary embodiment.
FIGS. 3A , 3 B, and 3 C are schematics illustrating an exemplary bed of ore treated by an exemplary process.
DETAILED DESCRIPTION
Referring to FIG. 1 , a hydrocarbonaceous containing rubblized ore is treated successively in three cycles, a non-oxidative pyrolysis (NOP) cycle, an oxidative combustion (OC) cycle, and an environmental sequestration (ES) cycle.
Reference is now made to FIG. 2 , which is a mass balance chart exemplifying a process. In a reactor space an NOP cycle is conducted with a fixed or moving bed of oil shale. The bed is heated by direct contact with steam, introduced through suitable injectors, such as for example, slotted pipes, nozzles, grates or other convenient means. Steam is introduced until the bed is heated to temperatures high enough to achieve substantial conversion of kerogen to oil and gas with minimal decomposition of carbonate minerals found in the oil shale, e.g. at a maximum temperature greater than about 700 degrees F., for example, between about 700 and 1000 degrees F. The bed is so configured as to allow produced liquids to drain to the bottom of the bed by gravity, where they are withdrawn through a suitable outlet. Gases are withdrawn from the upper portion of the bed by gas lines, or any convenient means.
The reactor space conditions are then changed for an OC cycle. In the OC cycle an oxidizing gas, such as air, oxygen-enriched air, or oxygen, is introduced to the bed through the same or different injectors used for the introduction of steam. Residual hydrocarbonaceous material left on the mineral surface from the kerogen conversion is combusted to generate heat and which during the process of combustion forms CO 2 , H 2 O, oxides of sulfur and nitrogen, as well as small amounts of other constituents. During the OC cycle high temperatures are desired in order to accelerate the oxidation reaction rate and provide for efficient heat utilization. In the high temperature combustion zone, metal carbonates, principally alkali metal carbonates, are allowed to decompose to CO 2 and their corresponding metal oxides. The hot gas so produced during combustion, consisting predominantly of CO 2 and H 2 O, if oxygen is used and N 2 , CO 2 and H 2 O if air is used, as well as lesser amounts of oxides of nitrogen and sulfur, is withdrawn from the reactor through gas withdrawal lines. Heat is recovered from the hot OC combustion gas to produce steam using steam generators of any suitable construction. The steam can then be cycled for use in the NOP cycle. Excess steam may be used to produce power, by, for example, steam turbines, or can be used directly where shaft power is required to power the process, such as compression of air in the air separation process, blowing of the oxidizing gas, or flue gas to the ES cycle or for driving electrical generators. The electricity is also used on-site to power the process; and excess electricity is sold to the electric grid.
During the OC cycle CO 2 is produced both from the combustion of the residual organic matter and the decomposition of carbonates. After recovery of heat from the OC gas a portion of the cool CO 2 -laden gas is recirculated along with the air or oxygen to the bottom of the OC bed, where it cools the lower bed and restores the alkali metal oxides to their carbonate form. Oxides of nitrogen and sulfur contained in the stream are deposited on the combusted shale where they react to form alkali metal salts. Oxides of N and S, being more acidic than oxides of C or H, will preferentially displace carbonates or hydrates on the combusted shale. Excess CO 2 not required for conversion of alkali metal oxides to carbonates absorbs heat from the upper bed and along with newly formed combustion gases and is directed to the steam generators as the combustion gas stream. The flow rate of the CO 2 -laden gas recycled into the OC cycle can be selected to adjust the temperature of the exit gases to a desired temperature or to adjust the rate of heat generation to coincide with the desired rate of steam production for the retorting in the NOP cycle and electric power generation.
As the OC cycle progresses, starting at the bottom of the bed a zone becomes cooled and metal oxides are there converted to carbonates from the cooled carbon dioxide in the gas recycle. As this cooled recarbonation zone progresses up through the bed, the hot combustion zone where residues are oxidized and metal oxides formed travels up and above the cooler zone. When the combustion zone reaches the top, or when the OC cycle has consumed essentially all of the available fuel (residue material) in the bed the reactor zone is switched to an ES cycle. At the same time, a reactor bed operating under a NOP cycle is switched to OC cycle, and a freshly prepared bed is started on the NOP cycle, thus making a semi-continuous process from a series of batch processes.
Accumulations of CO 2 -laden gas (that also contains oxides of nitrogen and sulfur) greater than that necessary for the OC and NOP cycle are sent to a third, ES cycle, which follows the OC cycle. In the ES cycle, the CO 2 -laden gas is injected into the bed through the piping or inlet system previously installed. Additional cleaning of the CO 2 occurs and essentially all of the remaining oxides of nitrogen and sulfur are sequestered. The cleaned CO 2 gas is withdrawn by suitable means as product. If oxygen is utilized as the oxidizing gas in the OC cycle, relatively pure CO 2 is produced for sale or use. If air is used, a clean, enriched stream of CO 2 in N 2 is produced which is suitable for recovery of CO 2 by conventional gas separation technologies. Whether to separate the N 2 from CO 2 at the tail end of the process or to separate the N 2 from O 2 at the beginning of the process is a matter of economic optimization. In either case highly concentrated CO 2 can be produced for industrial use.
Reference is now again made to FIG. 2 , which is a mass-balance diagram. This diagram is based upon preliminary modeling and can be understood with reference to the above discussion. In Table I is a listing describing the stream names. The NOP cycle is shown by the box on the right, with heated steam stream S 2 , which has been heated by combustion vapors S 29 from the OC cycle (shown as the middle box). Some of the exhaust vapors S 28 are used to generate steam for plant power requirements. Cooled exhaust vapors S 19 from the OC cycle are dewatered to S 31 and split into two streams, one a recycle to the OC reactor S 32 , and the other, the excess CO 2 stream S 14 is directed to the ES cycle (box on the left). Obviously, control of heat duties is conducted to make operational use of heat available.
TABLE I
Stream Names
S1
Oil shale feed, or initial charge
S2
Hot steam or other inert gas
S3
liquid products and water
S4
vapor products and steam
S4a
condensed vapor products and water
S5
primary oil products
S6
retort water for recycle
S7
non-condensable hydrocarbon gases
S8
condensed light overhead product and water
S9
condensed light hydrocarbon product
S10
condensed water for recycle
S11
makeup water (could derive from S27a)
S12
condensed water from combustion gas
S13
secondary oil products
S14
excess combustion gas for ES cycle
S15
oxidizing gas for OC cycle
S16
vapors from OC cycle
S17
oxidizing gas for afterburner on OC cycle
S18
hot combustion gas
S19
combined cooled and condensed combustion gas
S20
combined water to steam generator
S21
pure CO 2 or pure CO 2 + N 2 (may contain filterable particulates)
S22
intermittent recycle for process control purposes
S23
CO 2 product
S24
combined oil products (optional)
S25
solids at completion of NOP cycle
S26
solids at completion of OC cycle
S27
cooling water
S27a
warm cooling water
S28
hot combustion gas split for steam turbine exchanger
S28a
cool combustion gas from turbine steam exchanger
S29
hot combustion gas split for retort steam exchanger
S29a
cool combustion gas from retort steam exchanger
S30
solids at completion of ES cycle
S31
dewatered combustion gasses
S32
combustion gas recycled to OC cycle
In another example based upon preliminary modeling, a 50,000 bbl/day plant charging 25 gpt oil shale results in the following overall mass balance (assume 85% efficiency on Fischer assay, but recover the remaining 15% as combustion heat, before losses). This balance assumes all CO 2 produced from carbonate decomposition is sequestered on the spent shale. This is a model of a modified in-situ process where there is lower energy lost to the environment. While it is not possible to run any system with absolutely no energy loss due to edge effects, (e.g., piping, loses to surrounding), an in-situ process would be expected to show lower energy loss than a surface process, which may show slightly greater energy loss. The mass and energy balances are shown in TABLE II
TABLE II
Mass balance
In
Organic matter in =
14,979
Oxygen consumed =
12,100
27,079
ton/day
Out
Noncondensible gases =
1,486
Naphtha =
3,775
Mid distillate shale oil =
4,134
Heavy shale oil =
1,396
CO2 (98% indust. grd) =
13,064
Water (to tailings) =
2,854
NO 2 (sequestered) =
291
SO 3 (sequestered) =
79
27,079
ton/day
Energy balance (no energy imported)
In
Energy available in oil shale =
5.61 × 10 11 Btu/day
Out
Energy in oil and gas products =
4.04 × 10 11 Btu/day
Electric energy produced =
11,000 MW-hr/day (537 MW
plant)
Heat lost to surroundings =
4.7 × 10 10 Btu/day
Estimated First Law efficiency =
(56.1 − 4.7)/56.1 = 92%
In the practice of the process in which fixed beds are utilized, it can be operated with three reactors that will operate simultaneously. In the figure, a first, second and third reactors are provided. In the first reactor at this point in operation, an NOP cycle is in progress, which receives steam produced from the heat, energy generated for the second OC reactor. In the third reactor an ES cycle is in progress and finishes the cleanup of the produced CO 2 gases. The cycles continue until all of combustible, residual material in the OC cycle in the second reactor has been combusted, at which time the second reactor changes from an OC cycle to an ES cycle. The NOP cycle in the first reactor is changed to an OC cycle. A new NOP cycle is brought on-line. In practice of a fixed bed configuration, four units can make a convenient full cycle, with one unit being discharged and recharged, and, freshly prepared in anticipation of its next use, during the time the other three are on their respective cycles.
In an optional operation of multiple reactors, the temperature and heat flows are controlled in such a fashion as to facilitate steady-state operation and to complete NOP cycles simultaneously with the completion of OC cycles. Upon completion of the NOP and OC cycles, the cycle in the respective reactors is switched and NOP and OC cycles initiated in different reactors. For example, previous NOP reactor becomes the next OC reactor. The previous OC reactor becomes the next ES reactor. The previous ES reactor may be taken off-line or used as an additional ES reactor for further sequestration of NOx and SOx produced in miscellaneous flue-gases throughout the process.
The fixed bed may be configured in surface vessels situated side by side and operated in a swing configuration, or three modified in-situ cells. The modified in-situ cells may be constructed by the staged blasting technique of Geokinetics, the partial mining and rubblization concept forwarded by Occidental oil shale, or an engineered cell, for example, engineered cells similar to Red Leaf capsule technology.
In principle, the process could be applied to reactor units engineered for true in-situ, especially if some form of gaseous or liquid communications is provided. Such communications could be provided through vertical or horizontal drill- or boreholes, conduits, hydraulic fracturing, or other convenient means. Variations may include an initial short-term combustion cycle to open up the fractures that would facilitate larger, successive steam flows. Upon completion of the NOP cycle the permeability of the bed is greatly enhanced, allowing for an efficient combustion cycle and efficient sequestration in the ES cycle.
In a modified in-situ system an inclined, engineered, permeable bed of oil-bearing ore is constructed and the permeable bed may be encapsulated between impervious layers. The engineered impervious layers may be omitted if geophysical and hydrological conditions allow. A bed under NOP cycle conditions is heated by introducing steam through a first porous pipe, situated in the lower portion of the bed. A second porous pipe, situated in the upper portion of the bed accepts vapors produced in the process. As many porous pipes as are needed for effective recovery may be laid in the bed. Heating of the bed continues until a desired temperature is reached and a desired reaction is complete.
Vapors, which may consist of condensable hydrocarbons, non-condensable gases, and water vapor, are cooled; non-condensable gases are collected for sale, further processing, or used on-site. Condensed liquids are sent to a separator where light hydrocarbons are decanted in an overflow, and water is withdrawn from the underflow for recycle to the steam generator. Liquids, consisting of both an oil and aqueous phase, produced within the bed drain to a sump at the lower end of the bed where they are pumped to the surface for separation into their respective phases. The oil phase is sold or further processed.
When the bed is switch to OC cycle conditions, the oxidation (combustion) reaction is initiated in the vicinity of the first porous pipe and air or oxygen is injected at a controlled rate. The air or oxygen is diluted with an amount of CO 2 for purposes of (a) controlling combustion temperature, (b) converting alkali metal oxides to their respective carbonates, and (c) controlling heat recovery from the hot, combusted shale. The oxygen inflow rate is controlled to be sufficient to support combustion, but insufficient to cause premature breakthrough of the oxygen in the exit gas. Hot gases from the combustion flow by pressure differential toward a second porous pipe where they are withdrawn and used to generate steam, preheat water, or other beneficial use of heat. The OC cycle is allowed to continue until all, or a practical amount, of the combustible fuel left from the NOP cycle is consumed. The now relatively cool cell resulting from the now complete OC cycle is switched to serve as the ES cell. Additional liquids that may be produced during the OC cycle are sold, processed separately from liquids produced in the NOP cycle, or combined with liquids produced in the NOP cycle for sale or further processing.
When the bed is operated under ES cycle conditions, cool flue gas (vapor products from the OC cycle or other surface combustion process) is introduced to the first porous pipe. The vapors are allowed to contact the partially cooled bed where the CO 2 , NOx, SOx, and H 2 O substantially react with the activated ore where they are sequestered respectively as carbonates, nitrates, sulfates, hydrates, and related compounds.
In ordinary practice it is contemplated that there be at least three modified in-situ beds, and the cycles are performed in semicontinuous, sequential fashion. That is, a first bed having advanced to the ES stage would receive cooled flue gas whose heat has been recovered for beneficial use that was, produced in a second OC bed, which in turn, had previously completed the NOP cycle in a third bed. While the process is operating a new NOP cycle is being prepared in anticipation of a changeover of cycles. Thus, the process achieves a near steady state by marching the sequence of cycles through beds constructed in the resource zone. If the resource geometry allows, multiple simultaneous sequences are operated, staged in such a fashion as to produce steady product flow and make efficient use of labor and equipment.
In another aspect, a moving bed system is provided where the three cycles may be performed in three surface vessels. One vessel serves as a continuous NOP reactor, the second as a continuous OC reactor and the third as a continuous ES reactor. Prepared ore is charged to the top of the NOP vessel. Steamed or heated ore is removed from the bottom of the NOP vessel and charged to the top of the OC vessel. Hydrocarbon-free, reduced-temperature solids are removed from the bottom of the OC vessel and charged to the top of the ES vessel. Finishing of CO 2 purification and cooling occurs in the ES vessel. Cool, environmentally benign solids are discharged from the bottom of the ES vessel and sent back to the mine area for storage and land reclamation.
In an aspect of the semicontinuous, sequential operation of several beds of ore, once an operation with three cycles (NOP, OC, and ES) is in operation a new bed is prepared for a new NOP-cycle. The new NOP cycle bed can be initially preheated to make use of low grade heat as available. This new bed is brought into the operation once the initial NOP bed is completely reacted, at which time the initial NOP bed is switched to an OC cycle and the previous OC cycle is switched to an ES cycle. In instances where the optional ES cycle is not used, the sequence is similar, but without the ES cycle. If surface-engineered reactors are used, the prior ES zone is then converted to the next NOP zone and thus, the process cycles more or less continuously. If the zones are subsurface (in-situ or modified in-situ) there is no need to complete the initial ES cycle before a new NOP cycle is initiated. In principle there could be at any given time several NOP cycles in various stages of heatup, several OC cycles in various stages of oxidation and several stages of ES cycles in various stages of cooldown and sequestration.
Reference is now made to FIGS. 3A , 3 B, and 3 C, which are schematics that illustrate an exemplary bed of ore as it is treated by an exemplary process. In FIG. 3A is a rubblized bed of ore 101 containing hydrocarbonaceous materials. In the NOP cycle, a heated gas is introduced through line 103 , which heats the ore producing a fluid product, the liquid portion being withdrawn though line 105 and the vapor portion being withdrawn through line 107 .
Referring now to FIG. 3B , in the OC cycle, heated oxygen containing gas is introduced through line 203 , to create a combustion zone 221 in the bed 201 . The heating and the combustion/oxidation of remaining hydrocarbons in the bed creates temperatures in the combustion zone where a portion of carbonates in the ore decompose to oxides, forming carbon dioxide gas. The gaseous combustion products and carbon dioxide are withdrawn as an effluent gas stream through line 207 . After heat is recovered from stream 207 through suitable means 213 , the effluent gas stream is split to form an ES steam 209 , and recycle stream 211 . The cooled recycle stream is introduced into the bed below the combustion zone and creates a recarbonation zone 223 in the bed. The carbonation zone occurs where the combustion zone has already depleted the ore of hydrocarbons and formed metal oxides, and is at temperature conditions lower than in the combustion zone due to introduction of the cooled recycle stream. Under these conditions carbon dioxide in the recycle stream combines with metal oxides that were formed when the combustion zone passed up through the same region ore. The combustion zone with the recarbonation zone behind it passes up through the reactor until the combustion zone reaches to the top and the combustion and decomposition reactions cease. Whatever the kinetics or equilibrium thermodynamics of the recarbonation of various alkali oxides, there is a temperature zone in the cooler recarbonation process which is favorable to the recarbonation reaction, which is also enhanced by an excess of CO 2 in the recycle gas.
Referring to FIG. 3C , an ES stream, which may originate from another bed of ore being treated, such as 209 in FIG. 3B , is introduced into the recarbonated ore bed 301 through line 303 and as gas from the ES stream passes up through the bed metal oxides in the bed sequester nitrogen and sulfur oxides in the gas. A cleaned gas stream is withdrawn through line 315 . Piping and conduits can optionally be used for dual purposes. For example, lines 107 and 207 may be the same or different conduits, and likewise for lines 103 , 203 , and 303 .
While this invention has been described with reference to certain specific embodiments and examples, it will be recognized by those skilled in the art that many variations are possible without departing from the scope and spirit of this invention, and that the invention, as described by the claims, is intended to cover all changes and modifications of the invention which do not depart from the spirit of the invention. | A process for the energy efficient, environmentally friendly recovery of liquid and gaseous products from solid or semi-solid hydrocarbon resources, in particular, oil shale or tar sands. The process involves non-oxidative pyrolysis to recover fluid energy values, oxidative combustion to recover energy values as recoverable heat, and environmental sequestration of gases produced. | 5 |
[0001] This application is a continuation of part of U.S. patent application Ser. No. 11/746,637, which claims the benefit of the earlier filing date of May 9, 2007. Claim 1 of this application is revised from the previous claim 1, claims 2 , 3 , 10 of this application correspond to the previous claims 2, 3 and 4 of the U.S. patent application Ser. No. 11/746,637, respectively, and claims 4 - 9 of this application are new.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a handling device, and more particularly to a handling device that utilizes a clamping arm to move horizontally and vertically to perform handling operation.
[0004] 2. Description of the Prior Art
[0005] In the automatic flow, handling is the most basic operation step and is used most widely. With the development of science and the micromation of technique, handling step is used more and more widely in many fields. For example, in the replication and production of optical discs, a disc handling device is a necessary mechanism for moving between different machines. However, a conventional disc handling device has to use complex connecting rod structure and control system to move discs in the horizontal direction or vertical direction. It is obvious that the more complicated structure of the conventional handling device is, the higher the failure rate brings, and maintenance fee consequently increases. Therefore a simple structure that can achieve the objective of handling goods is needed to improve the automatic technique.
[0006] Hence, many efforts have been made by the author of the application to further improve the existing technology, such as the “power source driven stand-up urinal” disclosed in U.S. Pat. No. 6,129,320, which is directed to aids for disabled persons and includes a guide rod on which are mounted two cylinders extending along the axial direction of the guide rod, and each of the cylinders has horizontal slots and a vertically extending gap. A nut provided with a swing arm is screwed on the guide rod, and the swing arm is able to extend out of the horizontal slots. When the vertical gaps of the two cylinders are aligned with each other, the guide rod can drive the swing arm to move within the vertical gaps. When the vertical gaps are misaligned, the guide rod drives the swing arm to move within the horizontal slots of the two cylinders. Such structure is able to drive the swing arm to move vertically or horizontally, so that disabled person can stand up by placing a hand on the swing arm for support. It is believed to play a certain role if this structure is applied to the handling technology.
[0007] After further analysis, however, we found that the displacement of the swing arm in radial direction is still restricted by the horizontal slots of the two cylinders, and the swing arm is consequently unable to rotate 360 degree. Furthermore, the positions of the vertical gaps of the two cylinders cannot be adjusted, hence, the axial displacement of the swing arm is restricted. Such a technology which is restricted both in radial and axial directions is inapplicable to handling device.
[0008] The present invention has arisen to mitigate and/or obviate the afore-described disadvantages.
SUMMARY OF THE INVENTION
[0009] The primary objective of the present invention is to provide a handling device that utilizes a clamping arm to be screwed on a guide rod, and a C-shaped housing and a locking mechanism control the clamping arm to move in the horizontal direction and vertical direction, therefore achieving the objective of handling goods.
[0010] In order to achieve the abovementioned objectives, the handling device in accordance with the present invention comprises a guide rod, a clamping arm, a C-shaped housing and a locking mechanism. The guide rod is provided on its surface with an outer thread. The axial direction and the rotation direction of the guide rod are vertical to and intersect each other. The axial direction of the guide rod is in the vertical direction, and the rotating direction of the guide rod is in the horizontal direction. The clamping arm is screwed on the guide rod. The C-shaped housing is formed with a longitudinal gap for a mounting the clamping arm, and movably restricts the clamping arm in the meantime. The locking mechanism comprises a power source and at least one positioning block which is driven to swing by the power source, each positioning block being used to press against the C-shaped housing to stop it from rotation.
[0011] The clamping arm and the C-shaped housing moves in a horizontal direction synchronously along with the rotation of the guide rod under the condition that the horizontal movement of the clamping arm is not restricted, and the clamping arm moves in a vertical direction synchronously along with the rotation of the guide rod under the condition that the positioning block locks and stops the C-shaped housing and the horizontal movement of the clamping arm is restricted, thus handling the goods clamped by the clamping arm.
[0012] Furthermore, the positioning block of the locking mechanism can be connected to a driven member, the power source employs a transmission member to drive the driven member which then drives the positioning block to swing. The power source can be a motor, the transmission member can be a worm, and the driven member can be a driven gear which is eccentrically connected with the positioning block.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a perspective view showing a goods handling device in accordance with a first embodiment of the present invention, wherein the goods handling device has three positioning blocks located in the C-shaped housing;
[0014] FIG. 2 is a cross sectional view in accordance with the first embodiment of the present invention showing that the three positioning blocks move away from the C-shaped housing and the clamping arm moves horizontally;
[0015] FIG. 3 is a cross sectional view in accordance with the first embodiment of the present invention showing that the three positioning blocks press against the C-shaped housing;
[0016] FIG. 4 is an illustrative view in accordance with the first embodiment of the present invention showing that the three positioning blocks press against the C-shaped housing and the clamping arm moves vertically;
[0017] FIG. 5 is a perspective view showing a goods handling device in accordance with a second embodiment of the present invention, wherein the goods handling device has two positioning blocks, one of which is located in the C-shaped housing, and the other is located outside the C-shaped housing;
[0018] FIG. 6 is a cross sectional view in accordance with the second embodiment of the present invention showing that the two positioning blocks move away from the C-shaped housing and the clamping arm moves horizontally;
[0019] FIG. 7 is a cross sectional view in accordance with the second embodiment of the present invention showing that the two positioning blocks press against the C-shaped housing;
[0020] FIG. 8 is an illustrative view in accordance with the second embodiment of the present invention showing that the two positioning blocks press against the C-shaped housing and the clamping arm moves vertically.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0021] The present invention will be clearer from the following description when viewed together with the accompanying drawings, which show, for purpose of illustrations only, the preferred embodiment in accordance with the present invention.
[0022] Referring to FIGS. 1-4 , a handling device in accordance with the present invention comprises a guide rod 10 , a clamping arm 20 , a C-shaped housing 30 , and a locking mechanism 40 .
[0023] The axial direction of the guide rod 10 is in the vertical direction, and the rotating direction of the guide rod 10 is in the horizontal direction.
[0024] The clamping arm 20 is provided with a nut 21 that has an outer side and an inner side. The outer side of the nut 21 is fixed to the clamping arm 20 , and the inner side of the nut 21 is provided with threads and is directly screwed on the guide rod 10 .
[0025] The C-shaped housing 30 is tubular-shaped and surrounds the guide rod 10 in the horizontal direction, and the axial length of the C-shaped housing 30 corresponds to the length of the guide rod 10 . The C-shaped housing 30 movably clamps the clamping arm 20 in the meantime.
[0026] The locking mechanism 40 comprises a power source 41 , a plurality of middle gears 42 , a main gear 43 and three driven members 44 . In this embodiment, the power source 41 is a motor, a shaft 411 of the power source 41 is provided with a transmission member 412 which is a worm wheel. Each of the middle gears 42 includes a big toothed wheel 421 and a small toothed wheel 422 which are concentrically assembled together. The middle gears 42 are connected in such a manner that the big toothed wheel 421 of one middle gear 42 is engaged with the small toothed wheel 422 of another middle gear 42 , and a big toothed wheel 421 of one of the middle gears 42 is engaged with the transmission member 412 of the power source 41 . The main gear 43 and the guide rod 10 are coaxially and movably disposed. A small toothed wheel 422 of one of the middle gears 42 is engaged with the main gear 43 . In this embodiment, the transmission member 412 is engaged with the big toothed wheel 421 of a first middle gear 42 , and then the small toothed wheel 422 of this first middle gear 42 is engaged with the big toothed wheel 421 of a second middle gear 42 , and the small toothed wheel 422 of this second middle gear 42 is engaged with the big toothed wheel 421 of a third middle gear 42 , the middle gears 42 are repeatedly engaged in this way, and finally the small toothed wheel 422 of the last middle gear 42 is engaged with the main gear 43 . The three driven members 44 are driven gears which are engaged with the main gear 43 , respectively, and meanwhile, each of the driven members 44 is eccentrically connected with a positioning block 441 which is located in the C-shaped housing 30 .
[0027] The handling device in accordance with the present invention can achieve an objective of handling goods through the abovementioned structures. As shown in FIG. 2 , the locking mechanism 40 employs the power source 41 to rotate the middle gears 42 , the main gear 43 and the driven members 44 , making the driven members 44 drive the positioning blocks 441 to move away from the C-shaped housing 30 . Rotating the guide rod 10 can cause the rotation of the C-shaped housing 30 and horizontal displacement of the clamping arm 20 .
[0028] Referring then to FIGS. 3 and 4 , the power source 41 drives the driven members 44 to rotate, and the driven members 44 drive the positioning blocks 441 to swing outward from the inner side of the C-shaped housing 30 . When the positioning blocks 441 press against the C-shaped housing 30 , the C-shaped housing 30 cannot rotate and will stop the horizontal movement of the clamping arm 20 , so that the clamping arm 20 cannot rotate. Since the movement in the horizontal direction is restricted, the clamping arm 20 will move up and down in the vertical direction along with the rotation of the guide rod.
[0029] When the clamping arm 20 carries goods, the goods can be moved to the destination through the horizontal and the vertical movement of the clamping arm 20 ; and then goods handling operation is finished by releasing the goods.
[0030] The above embodiment is to stop the rotation of the C-shaped housing 30 by pressing the inner surface of the C-shaped housing 30 with the locking mechanism 40 . Besides that, another embodiment of the locking mechanism 40 can also press against the inner and outer surfaces of the C-shaped housing 30 simultaneously to stop the rotation of the C-shaped housing 30 , as shown in FIGS. 5-8 , the locking mechanism 40 comprises a power source 41 , a plurality of middle gears 42 and two driven members 44 .
[0031] In this embodiment, the power source 41 is a motor, and a shaft 411 of the power source 41 is provided with a transmission member 412 which is a worm wheel. Each of the middle gears 42 includes a big toothed wheel 421 and a small toothed wheel 422 which are concentrically assembled together. The middle gears 42 are connected in such a manner that the big toothed wheel 421 of one middle gear 42 is engaged with the small toothed wheel 422 of another middle gear 42 , and a big toothed wheel 421 of one of the middle gears 42 is engaged with the transmission member 412 of the power source 41 . The two driven members 44 are driven gears driven by one of the middle gears 42 to rotate. In this embodiment, the transmission member 412 is engaged with the big toothed wheel 421 of a first middle gear 42 , and then the small toothed wheel 422 of this first middle gear 42 is engaged with the big toothed wheel 421 of a second middle gear 42 , and the small toothed wheel 422 of this second middle gear 42 is engaged with one of the driven members 44 . The two driven members 44 are engaged with each other. Each of the driven members 44 is eccentrically connected with a positioning block 441 , one of the positioning blocks 441 is located in the C-shaped housing 30 , and the other positioning block 441 is located outside the C-shaped housing 30 .
[0032] The locking mechanism 40 can employ the power source 41 to rotate the middle gears 42 and the driven members 44 , making the driven members 44 drive the positioning blocks 441 to swing away from the C-shaped housing 30 , so that the clamping arm 20 is allowed to move horizontally. Or, the power source 41 can drive the positioning blocks 441 to simultaneously clamp against the inner and outer side of the C-shaped housing 30 . When the positioning blocks 441 press against the C-shaped housing 30 , the C-shaped housing 30 cannot rotate and will stop the horizontal movement of the clamping arm 20 , so that the clamping arm 20 cannot rotate. Since the movement in the horizontal direction is restricted, the clamping arm 20 will move up and down in the vertical direction along with the rotation of the guide rod.
[0033] While we have shown and described various embodiments in accordance with the present invention, it is clear to those skilled in the art that further embodiments may be made without departing from the scope of the present invention. | A handling device and method utilizes a clamping arm that is screwed on a guide rod. The axial direction of the guide rod is in the vertical direction, and the rotating direction of the guide rod is in the horizontal direction. Makes the clamping arm rotate in the horizontal direction when the clamping arm is not restricted, and makes the clamping arm move in the vertical direction when the clamping arm is restricted. By such arrangements, the clamping arm can perform handling in the horizontal direction and in the vertical direction. | 1 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] None.
ABSTRACT
[0002] A modified dental implant fixture designed with a multiple of three or more thread or groove patterns such that the threads or grooves transition from smaller to larger moving in the apical direction along the long axis of the dental implant body. Such a modified implant maintains adequate wall thickness for a deep conical connection.
BACKGROUND OF THE INVENTION
[0003] The present disclosure relates generally to dental implants, and more specifically to a dental implant having a deep female conical connection which can result in limited wall thickness. By combining an innovative thread or combination of thread and groove patterns that transition from smaller coronal to larger and deeper apical threads, which are helpful in providing greater primary stability, a dental implant that maintains adequate wall thickness, when a deep conical connection is utilized, is achieved.
[0004] Dental implants are used in place of missing natural teeth to provide a base of support for single or multiple teeth prosthetics. These implants generally include two components, the implant itself and the prosthetic mounting component referred to as an abutment upon which the final prosthesis is installed. The implant has apical and coronal ends, whereby the coronal end accepts the base of the prosthetic abutment using connection mechanisms of different designs. One such mechanism is a deep female conical receptor with an internal alignment or anti-rotational component such as a hex, double hex, spline or other single/multi-sided arrangement used for prosthetic alignment and anti-rotation stability. Deep female conical connections have been shown to prevent micro movement between the implant body and the abutment when loaded but can have the disadvantage of limited wall thickness especially if the implant is of a tapered design.
[0005] In practice, the implant body is surgically inserted in the patients jaw and becomes integrated with the bone. More specifically, the implant body is screwed or pressed into holes drilled in the respective bone. The surface of the implant body is characterized by macroscopic and microscopic features that aid in the process of osseointegration. Once the implant is fully integrated with the jaw bone, the abutment is ready to be mounted. For two-stage implant designs, the abutment passes through the soft tissue that covers the coronal end of the implant after healing and acts as the mounting feature for the prosthetic device to be used to restore oral function. Implants of the single-stage design extend at least partially through the soft tissue at the time of surgical insertion. The coronal end of the implant body acts as part of a built-in abutment design with the margin of the coronal collar usually being employed as the margin of attachment for the prosthesis used to restore oral function.
[0006] Both single and two stage implants are characterized by a central bore hole at their coronal ends that is generally threaded to accept a central screw to hold the abutment securely to the implant body. The exception would be some implants where the abutment is friction fit into the central bore hole and no screw is required. In any event, the implant, abutment, and screw are typically fabricated from titanium or a titanium alloy. Some implants are zirconia based, alumina based or sapphire based ceramics, and, in regions of high esthetic demands, the abutments are zirconia based. In some instances, ceramics and metals are combined to make a single component, though this is usually limited to the abutment component of the implant system. There is also promising research on the use of titanium zirconia alloys as well.
[0007] One of the original implant designs was the so-called Branemark type implant characterized by an external hex. The hex was originally used to insert the implant and later utilized as an external anti-rotational and alignment element. This design usually displays a bone loss pattern described as a cupping of the bone at the coronal end of the implant once loaded with occlusal forces. This cupping pattern usually stabilizes after about one year of function with vertical bone loss of approximately 2 mm. By that time, loss of bone critical to the predictable support of overlying soft tissue is lost. As implant designs evolved internal connections utilizing an internal hex became much more common. For example, Astra Tech Inc. (“Astra”) was one of the first companies to introduce a deep conical design and use a double hex as their internal orientation element.
[0008] In addition to having a more stable implant connection (deep female conical connection), Astra has also addressed the coronal bone loss by introducing micro threads at the coronal aspect of the implant body. This further modification is designed to distribute and transfer forces to the surrounding bone. However, clinicians are increasingly demanding dental implants with macro designs that achieve higher insertion torque values that generally translate to high initial implant stability. Prior Astra implants with a coronal flair had a single lead micro thread of 0.185 mm combined with a single lead apical thread of about 0.6 mm. To increase primary stability the micro threads were increased to 0.22 mm and made triple lead so as to be timed, together with having the same pitch, as the apical threads. This dramatically increased the required insertion torque and primary stability. Accordingly, in order to have more aggressive/deeper apical threads with wider spacing in combination with coronal micro threads of a similar dimension and still allow for adequate wall thickness for the deep female conical connection, an additional transitional thread pattern(s) of intermediate thread size(s) between the coronal micro threads and the larger apical threads is disclosed herein. However, the same thread pattern with inherent advantages can be utilized with any implant and is not limited to one with a deep conical connection.
[0009] Another advantage to a larger apical thread, in addition to increasing primary stability, is to increase surface area particularly on larger diameter implants when wall thickness is less of an issue. While apical threads in the size range of 0.6 to 0.66 may be ideal for implants in the 3.0 to 4.5 mm diameter, larger diameter implants have adequate distance between the central bore hole and the outer wall to allow for deeper apical threads. The resulting increase in surface area is particularly beneficial for large diameter, shorter implants which, depending on the clinical circumstances, would allow surgeons to avoid the maxillary sinus in the upper posterior region of the mouth.
[0010] More recent Astra implants have moved away from using an untimed micro thread of approximately 0.185 mm paired to a single lead apical thread of 0.6 mm, and now use a triple lead micro threads of about 0.22 mm timed to a single apical thread of approximately 0.66 mm. Meanwhile, U.S. Pat. No. 7,677,891 to Niznick (incorporated herein by reference) proposes quadruple lead (i.e. 4×) coronal threads spaced 0.3 mm apart and timed to double lead (i.e. 2×) apical threads spaced 0.6 mm apart with the 4× coronal threads being spaced considerably greater than 0.22 mm. Referring to FIG. 1 , the implant 10 , includes a tapered body 12 with two externally-threaded regions 14 and 16 . Proximal, externally-threaded region 14 includes V-shaped ×4 lead threads all of which have the same pitch. Distal portion 16 includes V-shaped ×2 lead threads. This type of implant design has a couple of disadvantages. First, in soft bone, the apical threads are limited to approximately 0.6 mm because coronal micro threads cannot be any larger than 0.3 mm and maintain crestal bone. Perhaps more critical, is the fact that a 2× apical thread increases the insertion speed. Specifically, if a sloped topped (e.g. U.S. Pat. No. 6,655,961) or asymmetric (e.g. copending application U.S. Ser. No. 12/494,510) coronal configuration is utilized, controlling the speed of the implant advancement into the host bone is essential. Accordingly, and as disclosed herein, the most apical thread should be a single thread (i.e. ×1).
[0011] There is considerable prejudice among dentists and manufactures as to the benefits of tapered or straight walled implant designs. Some, like Astra, even combine a tapered coronal aspect with a parallel walled apical portion of the implant. Most now agree that some type of tapered apical cutting end, even on the parallel walled design, is desirable. This is demonstrated on Astra's recently introduced TX (tapered apex) design. Referring to FIG. 2 in particular, the implant 20 , includes a straight walled body 22 with two externally-threaded regions 24 (proximal) and 26 (distal). The tapered apex 28 has been added to make initial installation, into holes drilled in the respective bone, easier.
[0012] However, both straight, tapered or a combination of tapered and straight bodied dental implants have their place in the field of implant dentistry depending on bone type and clinical application. For example, in the upper arch the bone is softer and the apical ends of adjacent teeth are closer together than in the lower arch. Therefore, a tapered design (that with a smaller apical end) fits between the roots of adjacent teeth more suitably while the tapered design compresses the softer maxillary bone upon insertion thus increasing implant primary stability at the time of placement. In the lower arch the bone is denser and root proximity is less of an issue so implants with parallel walls are considered more suitable by many clinicians.
[0013] A tapered implant with a truly more concave profile has not been utilized in the dental implant field. While Astra does transition from a straight apical end to a 6 degree flared coronal design, the transition is abrupt. What is proposed herein is a 2 and then a 5 degree concave flare (or any like progressive) transition be utilized. Besides allowing adequate wall thickness, another advantage, when combined with the proposed herein combination of thread sizes, is to increase implant primary stability as measured by resonance frequency analysis while possibly lowering the amount of torque required to seat the implant.
[0014] Accordingly, it is a general object of this dosclosure to provide a series of thread or a combination of groove and thread patterns that transition in spacing, size, pitch and depth such that adequate wall thickness for a deep internal female conical connection is maintained while allowing for an apical macro tread design that will result in greater primary stability for the dental implant while still keeping the rate of insertion within the limits that allow for either a sloped or asymmetric coronal configuration.
[0015] It is a another object of this disclosure to enable implants with a tapered implant body to maintain adequate wall thickness when utilizing a deep female internal conical connection and still allow for a macro tread design that will result in greater primary stability while still keeping the rate of insertion within the limits that allow for either a sloped or asymmetric coronal configuration to be aligned with the surrounding bony topography.
[0016] It is a further object of this disclosure to enable implants with a concave tapered implant body profile to maintain adequate wall thickness when utilizing a deep female internal conical connection and still allow for a macro thread design that will result in greater primary stability while still keeping the rate of insertion within the limits that allow of either a sloped or asymmetric coronal configuration to be aligned with the surrounding bony topography.
[0017] It is a more specific object of this disclosure to enable a large diameter, shorter length implants with deeper apical threads with increased surface area while maintaining adequate wall thickness for a deep conical connection and coronal micro threads.
[0018] These and other objects, features and advantages of this disclosure will be clearly understood through a consideration of the following detailed description.
SUMMARY OF THE INVENTION
[0019] According to an embodiment of the present invention, there is provided a dental implant for implanting within a human jawbone having an implant body with an outer surface, a longitudinal axis, a coronal end and an apical end. The coronal end includes a deep female conical receptor that creates a wall thickness between the outer surface of the implant body and the receptor. At least three differently sized threaded regions are positioned on the outer surface of the implant body with each region transitioning from smaller to larger in the apical direction along the axis.
[0020] There is also provided a dental implant for implanting within the human jawbone having a longitudinal implant body with an outer surface, an apical end and a coronal end. A series of three or more thread patterns that start near the coronal end are in series with each one becoming progressively larger, deeper and/or wider in size when moving in the apical direction along the implant body.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] FIG. 1 is a side elevational view of a prior art implant.
[0022] FIG. 2 is a side elevated view of a prior art implant having a tapered apex.
[0023] FIG. 3 is a cross-sectional side elevated view of a prior art implant without thread timing or a tapered apex.
[0024] FIG. 4 is a cross-sectional side elevational view a prior art implant with thread timing and a tapered apex.
[0025] FIG. 5 is a cross-sectional side elevational view of an implant according to the principles of an embodiment of the present invention.
[0026] FIG. 6 is a cross-sectional side elevational view of an alternate embodiment of an implant.
[0027] FIG. 7 is a cross-sectional side elevational view of an alternate embodiment of an implant.
[0028] FIG. 8 is a cross-sectional side elevational view of an alternate embodiment of an implant.
[0029] FIG. 9 is a cross-sectional side elevational view of an alternate embodiment of an implant.
[0030] FIG. 10 is a cross-sectional side elevational view of an implant.
[0031] FIG. 11 is a side elevated view of an implant according to the principles of an embodiment of the present invention.
[0032] FIG. 12 is a side elevated view of an alternate embodiment of an implant.
[0033] FIG. 13 a is a side elevated view of an alternate embodiment of an implant.
[0034] FIG. 13 b is a cross-sectional side elevational view of the implant of FIG. 13 a.
[0035] FIG. 13 c is a top plan view of the implant of FIG. 13 a.
[0036] FIG. 13 d is a perspective view of the implant of FIG. 13 a.
[0037] FIG. 13 e is a detailed view of the variable thread form detail of FIG. 13 a.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0038] An embodiment of the subject invention will now be described with the aid of numerous drawings and included measurement designations. Unless otherwise indicated, such measurements are used for explanatory purposes only and they are not deemed to be limiting of the disclosed embodiments herein. The purpose of describing these measurements is to illustrate that the concept of using three or more thread or groove patterns while maintaining adequate wall thickness for a deep conical connection can be utilized for a wide variety of implant sizes and designs.
[0039] In any event, turning now to the Figures, and in particular FIG. 3 , a prior art dental implant 30 is illustrated. This implant 30 is 11 mm long and has a step-wise diameter taper from 4.5 mm at its coronal end to 3 mm at its apical end. Two 60° thread patterns, at 1× to 1× are used on this implant 30 . The coronal threads 32 are 0.185 mm apart with grooves 0.1 mm deep, while the apical threads 34 are 0.6 mm apart with grooves 0.325 mm deep. The deep female conical connection 36 is the space within the implant 30 denoted by the dotted lines. This design provides for an upper wall thickness 38 of 0.303 mm and a lower wall thickness 40 of 0.440 mm.
[0040] The prior art implant 50 of FIG. 4 is the next generation Astra design of FIG. 3 and is again 11 mm long, but instead of having a step-wise diameter taper from 4.5 mm to 3 mm ( FIG. 3 ), it utilizes a tapered apex (similar to FIG. 2 ) going down to 2 mm. While such a tapered apex makes installation of the implant easier, the thread pattern needed to be adjusted in an attempt to increase wall thickness for the deep conical connection. Specifically, two 80° thread patterns, at 1× to 3×, are used on this implant 50 . With 80°, the resulting reduced thread depth will increase the wall thickness. The coronal threads 52 are 0.22 mm apart with grooves 0.082 mm deep, while the apical threads 54 are 0.66 mm apart with grooves 0.246 mm deep. The deep conical connection 56 has an upper wall thickness 58 of 0.321 mm and a lower wall thickness of 0.519 mm. The change to 0.22 mm 3× coronal thread timing dramatically increases implant primary stability while the change to 80 degree threads increases all thickness for both the coronal threads 52 and the apical threads 54 .
[0041] It has become apparent that an implant having a deep female conical connection is preferred to prevent micro movement between the implant and the abutment. In order to have both deeper apical threads that increase primary stability and coronal micro threads or grooves that better distribute force to the surrounding bone, an embodiment of the present invention adds at least one intermediate or middle thread to the pattern. This additional thread provides the necessary wall thickness to prevent implant breakage during function.
[0042] There have been studies claiming that certain thread timing patterns are more ideal than others. Specifically, that a 2× to 4× combination allows for the micro threads to follow partially in the path of the major apical thread with only a new middle thread being cut. However, Astra's 1× to 3× thread does much the same thing where the transition to 3× from 1× merely adds one smaller thread above and one below the major thread which itself transitions to a micro thread following the prior path of the major thread. While the 2× to 4× pattern avoids cross cutting the major apical threads, the 1× to 3× Astra pattern does essentially the same thing. Accordingly, in one of the solutions disclosed herein, a 1× to 2× to 3× thread pattern, there would be cross cutting for the 2× apical threads but not for the most coronal 3× micro thread. However, as long as the same thread pitch is maintained in a tapered implant design or one with a slightly concave coronal profile cross cutting is inconsequential as the bone is being compressed and expanded outward.
[0043] Cross cutting may be avoided for either a straight walled or tapered body implant using a 1× to 2× to 4× combination. However, bone gap jumping of up to 0.5 mm is clinically proven upon the immediate implant placement and therefore the only possible benefit might be for the ease of implant insertion as bone healing will fill in any cross threaded area in the bone. Taken to the extreme, and taking a 1× to 3× to 5× combination as an example, only the 5× portion would start to cross cut the 3× threads and only for the most coronal 20-25% or less. Furthermore, with a 1× to 2× to 4×, or a 1× to 3× to 6× no cross cutting would take place. For those knowledgeable in multiple lead thread timing this is well understood.
[0044] The utilization of a middle thread to the pattern will now be described. An example thereof is first shown in FIG. 5 . In particular, this implant 70 is 11 mm long and has a step-wise diameter taper from 4.5 mm at its crown to 2 mm at its apex and is shown with 5° of coronal taper 72 and 2° of mid wall taper 74 . Three thread patterns, 80° at 1× to 80° at 2× to 80° at 4×, are used on this implant 70 . The coronal threads 76 are 0.22 mm apart with grooves 0.082 mm deep, the middle threads 78 are 0.44 mm apart with grooves 0.164 mm deep and the apical threads 80 are 0.88 mm apart with grooves 0.476 mm deep. The deep conical connection 82 has a mid wall thickness 84 of 0.372 mm and a lower wall thickness 86 of 0.607 mm, both of which exceed the parameters for prior art FIGS. 3 and 4 .
[0045] While the straight walled apical diameter 88 has increased to 3.868 mm due to the increased thread depth in that region, the implant will go into the same diameter bone site as the prior art implant of FIG. 4 . Further, since the apical wall thickness has been increased to 0.607 mm, the parallel walled region could become slightly tapered with a minimal apical wall thickness equal to or greater than 0.519 mm shown in FIG. 4 . It should be noted that the implant of FIG. 4 does not allow the parallel walled section to become tapered because the apical threads were changed from 60° to 80° from the prior art of FIG. 3 in order to increase wall thickness for additional strength.
[0046] It will be appreciated that merely adding an intermediate or middle or transitional thread to any implant will not create the acceptable wall thickness. For example, implant 90 of FIG. 6 differs from FIG. 5 by using 6° of coronal and 3° of mid wall taper and again all three thread patterns are at 80° and the apical thread 92 depth is 0.328 mm. This allows a mid wall thickness 94 of only 0.304 mm and a lower wall thickness 96 of 0.518 mm. The lower wall thickness is acceptable but the middle wall thickness is less than prior art FIG. 4 and the parallel wall section could not become slightly tapered as for the implant shown in FIG. 5 as it is already 0.001 mm below minimum dimension per FIG. 4 . Accordingly, the implant described in FIG. 5 is preferable to the implant of FIG. 6 .
[0047] Three or more thread patterns can also be used on larger implants. For example, 11 mm long with step-wise diameter taper from 5 mm to 2.5 mm implants are shown in FIGS. 7 and 8 . Referring first to FIG. 7 , the implant 100 has a thread pattern of 60° at 1× to 80° at 3× to 80° at 5×. The coronal threads 102 are 0.2 mm apart with grooves 0.074 mm deep, the middle threads 104 are 0.33 mm apart with grooves 0.123 mm deep and the apical threads 106 are 1 mm apart with grooves 0.541 mm deep. The deep conical connection 108 has a mid wall thickness 110 of 0.595 mm and a lower wall thickness 112 of 0.553 mm.
[0048] The implant 120 of FIG. 8 has all three thread patterns at 80° with a 1× to 3× to 6× pitch. The coronal threads 122 are 0.2 mm apart with grooves 0.074 mm deep, the middle threads 124 are 0.4 mm apart with grooves 0.149 mm deep and the apical threads 126 are 1.2 mm apart with grooves 0.447 mm deep. The deep conical connection 128 has a mid wall thickness 130 of 0.569 mm and a lower all thickness 132 of 0.647 mm.
[0049] Referring now to FIG. 9 , this implant 140 is 11 mm long and has a step-wise diameter taper from 4.5 mm at its crown to 2 mm at its apex. Three thread patterns, 80° at 1× to 80° at 2× to 80° at 3×, are used on this implant 140 . The coronal threads 142 are 0.22 mm apart with grooves 0.082 mm deep, the middle threads 144 are 0.44 mm apart with grooves 0.164 mm deep; and the apical threads 146 are 0.66 mm apart with grooves 0.246 mm deep. The deep conical connection 148 has a mid wall thickness 150 of 0.372 mm and a lower wall thickness 152 of 0.689 mm.
[0050] The slightly more tapered implant 160 of FIG. 10 has the same thread pattern and measurements of FIG. 9 . However, as discussed with regard to FIG. 6 , and due to the implant 160 dimensions, acceptable wall thickness is not created. While the deep conical connection 162 has a lower wall thickness 164 of 0.599 mm, the mid wall thickness 166 is merely 0.304 mm. Accordingly, the implant described in FIG. 9 is preferable to the implant of FIG. 10 .
[0051] FIG. 11 shows a dental implant 170 with multiple thread patterns in profile. In this case, the deep apical threads 172 are followed by middle threads 174 and then coronal threads 176 up to the unthreaded portion 178 and top surface 180 .
[0052] FIG. 12 shows a dental implant 190 with an addition set of threads. In particular, the deep apical threads 192 are followed by middle threads 194 and coronal threads 196 leading to parallel groove threads 198 before reaching the unthreaded portion 200 and the top surface 202 . It will be appreciated that two or more parallel groove patterns may be employed.
[0053] One of the more advantageous uses for the present invention is to allow for wider diameter dental implants; the same can be said of shorter and wider diameter implants. For example, FIG. 13 a shows an implant 210 that is 6.50 mm long and has a diameter taper from 5.50 mm at its crown to 4.75 mm at its apex. Three thread patterns, a 1× to 2× to 3× all at 60°, are used on this implant 210 . The coronal threads 212 are 0.25 mm apart with grooves 0.14 mm deep and the middle threads 214 are 0.375 mm apart with grooves 0.20 mm deep. As for the apical threads 216 , they are shown with the apical minor diameters progressively being lowered, which results in the most apical thread having a more aggressive cutting profile (see FIG. 13 e ). Conversely, allowing the minor diameter to migrate coronally will result in a most apical buttress thread. The deep conical connection 218 of this shorter implant 210 is shown in FIG. 13 b - d. The combination multiple thread pattern of this design maintains the necessary wall thickness 220 between the deep conical connection 218 and the grooves of the thread patterns.
[0054] Alternatively, 60° 1×, 2×, 4× threads could be used with the coronal threads 212 being 0.22 mm apart and 0.12 mm deep and the middle threads 214 being 0.44 mm and 0.24 mm while the apical threads would be spaced 0.88 mm apart and be variable or of consistent depth.
[0055] The present disclosure addresses the issue of limited wall thickness associated with a deep conical connection. However, there are other advantages inherent in the design that could equally be applied to the implant with a different abutment connection Accordingly, while particular embodiments of the invention have been shown and described, it will be apparent to those skilled in the art that changes and modifications may be made therein without departing from the invention if its broader aspects, and, therefore, the aim in the appended claims is to cover all such changes and modifications as fall within the true spirit and scope of the present invention. | A modified dental implant fixture designed with a multiple of three or more thread or groove patterns which provide adequate wall thickness for a deep female conical connection such that the threads or grooves transition from smaller to larger moving in the apical direction along the long axis of the dental implant. | 0 |
[0001] This application is a continuation of my U.S. patent application Ser. No. 11/924,704 filed Sep. 26, 2007, which is a continuation of my U.S. patent application Ser. No. 10/522,422, now U.S. Pat. No. 7,357,175.
FIELD OF THE INVENTION
[0002] The invention relates to heating bodies, and in particular, to towel dryers for drying and warming towels.
BACKGROUND OF THE INVENTION
[0003] Towel dryers are used to dry and warm towels in bathrooms and the like. A towel dryer has an outer surface that supports a towel to be dried. The surface is heated above ambient room temperature by connecting the surface to an energy source, typically heated fluid or an electrical energy source. Towel dryers for residential use are typically plugged into a home's electrical receptacle if electrically heated, and may be connected to a home's hot water system if heated by fluid. The hot water system may also supply water to radiators that heat the home.
[0004] It is believed that a towel dryer operates mainly by transferring heat to the towel by conduction and natural convection. Heat is transferred by conduction directly from the dryer surface to the portion of the towel in contact with the surface. Heat is also transferred indirectly from the towel dryer to the towel by natural convection, the towel dryer heating the surrounding air and the heated air transferring heat to the towel.
[0005] It is believed that at normal operating temperatures, radiant heat transfer is not an important mechanism in transferring heat from the towel dryer to the towel. However, heat can be lost from the towel dryer by such radiant heat transfer. Heat loss by radiant heat transfer wastes energy and lowers the efficiency of the towel dryer because radiant heat transfer cools the dryer surface without effectively contributing to warming and drying the towel. Reducing heat loss by radiant heat transfer would enable the towel dryer to be more energy efficient: the towel dryer could reach a higher operating temperature with the same energy input, or would reach the same operating temperature with reduced energy input.
[0006] Towel dryers are generally constructed of a base body of unalloyed steel with a surface coating, in order to attain certain desirable coloration appearances. In this practice, depending upon the location of the said towel dryer, different coating procedures are used. Thus it is possible, for example, that towel dryers in residential areas are provided with a powdery coating or they may be lacquered. Most likely a towel dryer in a bathroom can be electrically chromed.
[0007] The above described procedures and materials have the disadvantage, that the surface coating negatively affects the heating capacity of a steel towel dryer. The term “heating capacity” is related to the amount of energy that must be supplied to maintain the towel dryer at its operating temperature. A towel dryer with a higher heating capacity will maintain its operating temperature with less energy input than would a similar towel dryer with a lower heating capacity.
[0008] Thus, for example, an electrically chromed, steel towel dryer, as compared to a lacquered or powder covered steel towel dryer, will yield only 20 to 30% as much heat. This poor rendition of heat from chrome covered steel heating bodies results in the construction of very large heating bodies, which in turn, each disadvantageously require a large space allotment.
[0009] It is believed that a chromed steel body loses more heat by radiant heat transfer than a lacquered or powder covered steel body. This appears to be due to the higher emissivity of the chromed steel body as compared to the lacquered or powder covered steel body. The greater the emissivity a body has, the more efficient it is in losing heat by radiant heat transfer. The higher emissivity of the chromed steel body causes greater heat loss through radiant heat transfer, reducing the heating capacity of the body and reducing the energy efficiency of the towel dryer.
[0010] The purpose of the present invention is to create a towel dryer with a similar, highly reflective surface, which resembles a towel dryer having a chromed body, which sets aside the above named disadvantages and is further, simple and economical to produce. In other words, the purpose of the present invention is to provide a functionally more energy efficient towel dryer that retains a visually appealing, highly reflective body. The towel dryer would be capable of transferring a larger percentage of its heat by conduction or convection, and so could also be made smaller for the same rate of heat transfer to a towel.
SUMMARY OF THE INVENTION
[0011] The towel dryer in accord with the invention has a base body of metal, especially aluminum. The surface of the said invented base body is worked in such a manner, that a conventional electrically applied chrome coating or gilding, for the purpose of and bringing about a highly reflective surface, can be eliminated. Instead of aluminum, it is also possible to make use of any other metal, such as, for instance, a highly refined steel.
[0012] Highly polished aluminum may have an emissivity of about 0.04 or less, and highly polished stainless steel may have an emissivity of about 0.1, each significantly lower than the emissivity of chromed steel that may be about 0.17. A towel dryer made of highly polished aluminum or highly polished stainless steel would have less radiant energy loss and thus greater heating capacity and greater operating efficiency than would the same conventional towel dryer made of chromed steel.
[0013] In accord with the invention, the surface is then of high polish and possesses a degree of reflectivity of 80% to 100%. This provides a body having a sufficiently low emissivity to be more efficient than a conventional chromed steel towel dryer.
[0014] Because of the aluminum, that is to say a metallic, base body and the elimination of the electrical chrome application, the invented towel dryer has a substantially greater thermal efficiency than does a towel dryer having the conventional chromed, steel heating body. Thus, a conventional towel dryer, which possesses a chromed coating, when compared to an invented, highly polished towel dryer constructed of aluminum, exhibits a thermal efficiency which is about 30% to 40% less. In other words, the invented towel dryer, when operating at the same heating load, can clearly be made smaller and less expensively. This is a considerable advantage in bathrooms with predominately less available space.
[0015] For the achievement of the desired degree of burnish, the metal construction of the invented towel dryer base body is mechanically ground, mechanically polished and chemically and electrochemically polished.
[0016] One embodiment of the invented towel dryer advantageously possesses, for the purpose of increasing the resistance to corrosion and for the retention of the high degree of burnish, an electrochemically anodized surface or has an Eloxal coating. Plain anodized aluminum may have an emissivity of 0.04, which enables a towel dryer having polished aluminum surface to be anodized for corrosion resistance and yet retain a lower emissivity than a conventional chromed steel towel dryer.
[0017] Another embodiment provides, for the increase of resistance to corrosion, and for the retention of the high degree of burnish, a clear lacquer coating.
[0018] Intrinsically, known towel dryers with an aluminum base body are often chromed for the purpose of creating a highly reflective surface, which requires not only a complicated procedure and is expensive, but further, notably reduces the emission of heat, that is, notably reduces the heating capacity and energy efficiency of the towel dryer.
[0019] In the following, the invention is more closely described with the aid of an illustrated presentation of a preferred embodiment.
BRIEF DESCRIPTION OF THE DRAWING
[0020] FIG. 1 shows a perspective view of an invented towel dryer.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0021] The invented towel dryer 2 has a base body 4 and two connection fittings 6 , 8 that connect the base body 4 to an energy source 18 represented schematically in FIG. 1 . Illustrated energy source 18 is a supply of heated water, with connection fittings 6 , 8 connecting respectively to an inlet line for water supply and to an outlet line for the removal of the used water. The external inlet and outlet lines are not shown. The base body 4 has two parallel running tubes 12 , 14 , which are distanced from one another by the crossover tubes 16 . With this arrangement, the water can flow between the two tubes 12 , 14 , so that, for example, hand towels (not shown) can be hung on the crossover tubes 16 to be dried.
[0022] In accord with the invention, the base body requires no surface coating for the attainment of the desired degree of reflectivity, but rather the surface is worked in such a manner, that both the aesthetic total impression of the heating body 2 is increased and the base body is also protected against corrosion and damage.
[0023] In a preferred embodiment, the surface possesses a degree of reflectivity of 80% to 100%.
[0024] As an aid for the judgment of the luster of the finish, a reflectometer is applicable, which is in accord with DIN 67 530.
[0025] An essential advantage of the invented towel dryer 2 is, that in comparison to conventional chromed steel towel dryers, it possesses an improved degree of heat transfer. For example, of a chromed heating body, the statement is made, that a heat load of some 750 W is developed. Contrary to this, an equally sized aluminum towel dryer 2 develops a heating load of about 1100 W. That is to say, the invented towel dryer 2 possesses, size for size, about a 50% greater heat production, whereby its high heat transfer capability permits a quicker reaction for the input and output control, such as, for example, might be called for by thermostatic regulation. Such an advantage can markedly reduce the heating costs.
[0026] The metal base body 4 of the towel dryer 2 , in keeping with the invention, is mechanically ground for the achievement of the desired degree of reflectivity, then mechanically polished and chemically (electro-chemically) brought to a high reflectivity.
[0027] The mechanical abrasive treatment is mostly done by rough grinding for the removal of gross protrusions and depressions of the surface 10 . This is generally carried out by a grinding disk. In general dry grinding is employed, whereby the circumferential speed is held to within a range of 420 to 1200 RPM.
[0028] After the rough grinding, then a secondary grinding takes place. For this operation, advantageously, a grinding disk arrangement is again used wherein the laminated disks are impregnated with special clay. The 60 to 120 mesh clay is impregnated into a fabric which can be of cloth, sheepskin, or muslin. The disks may turn within a range of 1500 to 1800 RPM. However, even a rotation speed up to 3000 RPM may be used.
[0029] Subsequent to the secondary grinding, fine abrasive treatment takes place. This can also be known as pre-polishing. Normally, the disks for this purpose, as described above, can be of felt, sheepskin or bias cut muslin fabric with impregnated 100 to 200 mesh clay. The operation is cooled by air flow. The circumferential speed lies somewhere in the ranges as given above, although it may be slightly increased.
[0030] After the mechanical grinding, the surface 10 , for the removal of abrasion traces, and for the acquiring of a luster, is similarly mechanically treated, this time with a polishing disk. The polishing disk possesses more laminations, preferably of loose or battened cotton material and turns at some 2000 to 2600 RPM. This polishing is optionally carried out dry or wet. In order that the hardness of the polishing disk may be changed, it is possible, that among other changes of a fiber count of the cotton material, also cloth, wood or paper insertions may be interposed between the individual disks.
[0031] Care must be taken, in regard to the mechanical polishing of the invented towel dryer, that, in particular, no metal particulate are to be allowed to adhere to the polishing disks, since such inserts, without fail, lead to a lessening of the surface quality.
[0032] Fundamentally, attention must be given during the mechanical grinding and polishing, that no excessive temperatures are generated and no gouging of the surface takes place. A protection of such temperature can be brought about, for the safety of the surface, by an appropriate choice of the speed of rotation, pressure of the abrasive means, as well as by means of proper design of the said disks or by the use of abrasive or polishing means such as greases, oil or pastes.
[0033] By the employment of abrasive and/or polishing means, the impingement of these materials in the surface 10 is to be avoided, since such embedded materials can be released during the next process step and thus impair the quality of the surface 10 .
[0034] Further, in a case of large towel dryers 2 with greater surfaces 10 , it can be of advantage, to replace the grinding disks with abrasive belts.
[0035] For the achievement of a final luster, the surface 10 is treated, after the mechanical phase, chemically or electrochemically. Preference is given to the chemical treatment, since such a procedure, counter to the electrochemical method, such as, for instance, the Erft-works process has the advantage, that no electrical energy is required. In this way, instead of electrical current, oxidizing agents are used.
[0036] Advantageously, the surface 10 is finally electrochemically anodized, or treated with Eloxal, so that the resistance to corrosion of the said surface is increased by an Eloxal-coating. This is especially valuable, if the heating body 2 is to be used in rooms subject to high humidity, such as, for example, bathrooms or, as mentioned above, the heating body is to be used for the drying of towels.
[0037] By the above, the surface 10 is chemically changed, so that a porous aluminum oxide layer is formed, which is still to be sealed in a final step of the process.
[0038] It is also possible, that the surface 10 , instead of being coated with the Eloxal layer, receives a finish of a clear lacquer for the increase of the resistance to corrosion. In this case, the lacquer coating can be applied by spraying, or in the form of a powder, or by means of a fine brush, or the lacquer can be applied by dipping into an immersion bath.
[0039] Disclosed is a towel dryer with a base body of metal, preferably aluminum or high quality steel, the surface of which, is caused to be of high reflectivity and resistant to corrosion. While I have illustrated and described a preferred embodiment of my invention, it is understood that this is capable of modification, and I therefore do not wish to be limited to the precise details set forth, but desire to avail myself of such changes and alterations as fall within the purview of the following claims. | A towel dryer includes an aluminum body having an outer surface that supports a towel to be dried. The surface has a degree of reflectance of not less than 80% for more efficient transfer of heat from the body to the towel. The outer body surface is an oxidized surface to resist corrosion, and a clear coating may be provided over the surface. | 8 |
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