description
stringlengths 2.98k
3.35M
| abstract
stringlengths 94
10.6k
| cpc
int64 0
8
|
|---|---|---|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a coating method.
Particularly, it relates to a coating method for applying coating compositions, such as photographic emulsion, magnetic material, or the like, onto a continuously moving web. Such a process is used in the manufacture of photographic light-sensitive materials, such as photographic film, photographic paper or the like, of magnetic recording materials, such as magnetic recording tape or the like or of other recording materials.
Even more particularly, it relates to a coating method for applying coating compositions, as a freely falling thin film, onto a moving web.
2. Background of the Invention
A typical example of the coating method for applying thin-layer coating compositions onto a moving web in the form of a freely falling coating composition film is a curtain coating method.
In the curtain coating method, a freely falling coating composition film prepared from one or more coating compositions is applied to an object to be coated. Heretofore, the curtain coating method has been used for coating of furnishing goods, iron plates and the like. As an improvement in coating quality has been demanded in the recent years, high precision coating has been required. Particularly, as disclosed in Japanese Patent Publication Nos. 24133/1974 and 35447/1974, attempts have been made to apply the curtain coating method to the fields in which high precision is required, for example, to the process of manufacturing photographic light-sensitive materials.
Referring to FIG. 1, there is shown an apparatus according to a conventional curtain coating method. In FIG. 1, fixed quantities of coating compositions S 1 and S 2 are fed to pockets 4 within a slide hopper 1 from liquid tanks (not shown) through respective quantitative pumps P 1 and P 2 . The coating compositions S 1 and S 2 flow out of the pockets 4 through slots 3 extending vertically from the pockets 4 and then flow down in the form of streamer layers 8 to a lip 7 along an inclined surface 6 of the slide hopper 1. At the lip 7, falling curtains of the coating compositions S 1 and S 2 , that is, a freely falling coating composition film 9, is formed. On the other hand, a web 11 fed from a web supply roll 5 is driven through pass rollers 2 and 12. The freely falling coating composition film 9 is applied to the moving web 11 to form a multilayer coating film 10. Two separated edge guides 20 vertically extend from the two ends of the lip 7 onto the coating path. The edge guides 20 facilitate the formation of the freely falling coating composition film 9 and determine the width of the film applied to the surface of the web 11. The hopper 1 has an air shield 13 for shielding the freely falling coating composition film 9 from the flow of the air entrained with the moving web before application to thereby prevent bubbles from entering between the freely falling coating composition film 9 and the surface of the web 11.
Heretofore, as a method for applying aqueous solution type coating composition, there has been known a coating method comprising the following steps. Silver halide emulsions having gelatin as a binder are applied to thereby simultaneously form a multilayer coating film. The multilayer coating film is converted to a gel by use of the sol-gel conversion characteristics of gelatin by cooling or with cool air so that the viscosity of the multilayer coating film increases so high as to be within a range of tens of thousands to hundreds of thousands cps to prevent mixing of the coating compositions into each other between layers. The multilayer coating film is finished by hot-air drying and the like.
Recently, the inventor of this application has proposed prior to this application an improvement in high-speed thin film coating, as disclosed in Japanese Patent Unexamined Publication No. 189967/1984.
In the recent years, however, it is required that the coating is made thinner and made quickly. With such a requirement, it becomes difficult to produce a coating film having multiple layers separated from each other because the probability increases that mixing of the coating compositions occurs before the multilayer coating film is formed on the web as the coating composition quantity per unit area in each layer decreases. This coating composition quantity will hereinafter be abbreviated to "coating quantity".
On the other hand, in the case where organic solvent type coating compositions are applied, mixing of the coating compositions at a portion for applying the freely falling coating composition film onto the web occurs relatively easily compared to that in the case where aqueous solution type coating compositions are applied. This difference arises because the surface tension of organic solvent type coating compositions is lower than that of aqueous solution type coating compositions. Accordingly, it is more difficult to attain a coating film having multiple layers separated from each other.
According to the Japanese Patent Publication Nos. 24133/1974 and 35447/1974, one or more kinds of coating compositions are supplied between the two edge guides 20, as shown in FIG. 1, by a slide type or extrusion type injector to form freely falling coating composition films 9 to be applied to the continuously moving web 11. The two edge guides 20 have the double function of limiting the coating width and stabilizing the freely falling coating films 9. Further, according to the Japanese Patent Publication No. 24133/1974, the air shield 13 is used for shielding the freely falling coating composition film 9 from the flow of the air entrained with the moving web.
In spite of the provision of the aforementioned mechanism for stabilizing the freely falling coating composition film, uniform coating becomes more difficult as the coating quantity decreases (that is, as the coating compositions are applied more thinly) or as the moving speed of the web increases (that is, as the coating compositions are applied more quickly). In short, in the curtain coating method, as the coating compositions are applied thinly and speedily, deformations or fluctuations occur when the multilayer coating film 10 on the moving web 11 is formed from the freely falling coating composition films 9. The occurrence of deformation or fluctuation causes mixing of the coating compositions within the multilayer coating film 10 formed on the web 11. On the other hand, according to the Japanese Patent Unexamined Publication No. 189967/1984, a lowermost layer part of the coating compositions is applied as a pretreatment for curtain coating. However, in the case where a solvent is applied as a lowermost layer part of the coating compositions, it is difficult to pile up two-layer coating compositions at the next step of applying the freely falling coating composition film so that mixing of the coating compositions between the two layers occurs easily. Further, because a lowermost layer part of the freely falling coating composition film is applied as a pretreatment, two coating compositions cannot be simultaneously applied. Accordingly, the proposed coating method is inferior in manufacturing efficiency, hence further improvement in manufacturing efficiency has been desired.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a coating method for applying at least two coating compositions to form a multilayer coating film without mixing the coating compositions into each other at the interface between layers.
Another object of the invention is to provide a coating method for applying coating composition both thinly and speedily.
A further object of the invention is to provide a curtain coating method with improved stability of the freely falling curtain.
To attain the foregoing objects, the coating method for applying at least two coating compositions onto a moving web, according to the present invention, comprises the steps of applying one of the two coating compositions onto the web to form a coating layer and then applying the other of two coating compositions onto the coating layer in the form of a freely falling coating composition film before the first coating layer has been completely dried.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a typical side view of a curtain coating apparatus according to a conventional coating method.
FIG. 2 is a typical side view showing a coating method according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 2, there is shown a coating method according to the present invention.
As shown in FIG. 2, a coating composition S 1 is applied onto a moving web 11 through a roll coater 16 to form a lowermost coating layer. Then, another coating composition S 2 is applied onto the lowermost coating layer in the form of a freely falling coating composition film before the lowermost coating layer has been completely dried. Thus, a multilayer film 10 is formed on the web 11 without mixing the coating compositions into each other between layers. Further, when the freely falling coating composition film is applied, a good wetness condition can be instantaneously attained. Accordingly, the multilayer film 10 can be applied thinly and speedily without deformation or fluctuation of the coating composition film.
In the present invention, it is preferable that the solvent content of the coating composition S 1 applied onto the web is 0.3 to 7.5 cc/m 2 just before the application of the freely falling coating composition. If it is less than 0.3 cc/m 2 , mixing of the coating compositions into each other between layers will often occur. If it is more than 7.5 cc/m 2 , the liquid film formation from the upper coating composition S 2 will be often hindered.
Although the embodiment has shown the case where a roll coating method is used for application of the lowermost layer coating compositions S 1 , it is to be understood that the present invention is not limited to the specific embodiment but any method, for example a doctor coating method or a gravure coating method, can be used for application of the lowermost layer coating composition S 1 .
The meaning of the words "before the lowermost coating layer has been completely dried" is that, when the next, freely falling coating composition film is applied, the lowermost coating layer is in a state where it is sufficiently wet to the next coating film but where the coating compositions are not mixed into each other between layers. Accordingly, the meaning is that the solvent in the lowermost layer is more or less evaporated, that is, is partially dried.
In the present invention, the freely falling coating composition film may be formed by use of a slide type hopper or may be formed by use of an extrusion type hopper.
Examples of the web used in the present invention include a paper web, a resin film web, a metal web, a resin-coated paper web, a synthetic paper web and the like. Typical examples of resin materials used in the resin film web are polyolefins, such as polyethylene, polypropylene and the like; vinyl polymers, such as polyvinyl acetate, polyvinyl chloride, polystyrene and the like; polyamides, such as 6, 6-Nylon, 6-Nylon and the like; polyesters, such as polyethylene terephthalate, polyethylene-2, 6-naphthalate, and the like; polycarbonates; cellulose acetates, such as cellulose triacetate, cellulose diacetate and the like. Typical examples of resin materials used in the resin-coated paper web are polyolefins, such as polyethylene and the like, but the resin materials are not limited thereto. A typical example of the metal web is an aluminum web.
With respect to the coating compositions used in the present invention, various kinds of liquid compositions can be used in accordance with the purpose. Examples of the coating compositions include: coating compositions for forming light-sensitive emulsion layers, sub layers, protective layers, back layers and the like as in photographic light-sensitive materials; coating compositions for forming magnetic layers, sub layers, lubricating layers, protective layers, back layers and the like as in magnetic recording media; and other coating compositions for forming adhesive layers, coloring layers, rust preventive layers and the like. These coating compositions are prepared by mixing the active material in soluble binders or organic binders.
The following example is given to illustrate the effect of the invention more clearly.
EXAMPLE
Coating composition A--a fluid of viscosity of 50 cp, composed of the following components.
Phenol resin: 29.8 parts by weight
Dye: 0.1 parts by weight
Cellosolve acetate: 54 parts by weight
Methylethyl ketone: 16 parts by weight
Fluorine-containing surface active agent: 0.1 parts by weight
Coating composition B--a fluid of viscosity of 3 cp, composed of the following components.
Polyvinyl formal resin: 2 parts by weight
Methylcellosolve: 58 parts by weight
Methanol: 40 parts by weight
Using the coating apparatus as shown in FIG. 2, a 180 μm thick web 11 made of polyethylene terephthalate was driven at a speed of 80 m per minute. The coating composition B was applied onto the moving web 11 through a roll coater 16 to thereby form a lower coating layer with a width of 120 cm and a coating quantity of 4 cc/m 2 . Before the coating layer was completely dried, the coating composition A was applied as a freely falling coating composition film onto the lower coating layer to thereby form a coating film with a width of 110 cm and a coating quantity of 20 cc/m 2 .
The lower layer coating portion and the freely falling coating composition film coating composition film coating portion of the apparatus were separated by a distance of 100 cm along the web moving path. The freely falling coating composition film 9 was dropped from a height of 3 cm. The freely falling coating composition film was so stable that deformation or fluctuation could not occur. Accordingly, the surface properties of the coating film was so excellent that mixing of the coating compositions into each other between the layers could not occur.
COMPARATIVE EXAMPLE
Using the coating apparatus as shown in FIG. 1, the 180 μm thick web 11 made of polyethylene terephthalate was driven at a speed of 40 m per minute. The two coating compositions were simultaneously applied as freely falling coating composition films onto the moving web to thereby form a two-layer coating film with a width of 110 cm and a quantity of 20 cc/m 2 . As a result, the freely falling coating composition films were so unstable that fluctuations occurred. Accordingly, stripe-like irregularities occurred on the coating surface and mixing of the coating compositions into each other between the layers occurred.
As described above, the present invention is directed to a coating method for applying at least two coating compositions onto a moving web. The method comprises the steps of applying one of the at least two coating compositions onto the web to form a coating layer and applying another of the at least two coating composition onto the coating layer in the form of a freely falling coating composition film before the first coating layer has been completely dried. Accordingly, mixing of the coating compositions into each other between the coating layers can be prevented. Further, the freely falling coating composition film becomes so stable that multilayer coating can be made speedily and thinly. In addition, the following effects can be attained.
(1) The coating and drying steps which must be repeated in the prior art due to the impossibility of simultaneous multilayer coating, can be greatly simplified by the coating method of the invention.
(2) Because the freely falling coating composition film becomes stable, there is no necessity of air shielding means.
(3) When the coating composition flows out of the slot to form a liquid film, a stripe-like irregularity is often caused by impurities or bubbles in the coating composition. However, such a stripe-like irregularity can be reduced accordingly to preparatory coating or in other words according to a so-called leveling effect.
|
A multi-layer coating method in which a first layer is first applied to a moving web and is allowed to partially dry before a second layer is applied as a freely falling coating composition film.
| 8
|
RELATED APPLICATION DATA
[0001] This application claims priority to previously filed U.S. Provisional Application No. 60/614,212 filed on Sep. 29, 2004, entitled “Size Controlled Fibers, Tubes and Channels Synthesized by Heterogeneous Deposition Using Sol-Gel Processing”, and is hereby incorporated by reference in its entirety.
FIELD OF THE INVENTION
[0002] The present invention generally relates to diameter-controlled nanostructured fibrous materials made through a process including deposition of a sol-gel film on an organic fiber followed by removing or degrading the organic fiber. The structures obtained thereby can be compact nanofibers or other similar or related structures. In general, the fibers obtained by the process of the present invention have substantially continuous surfaces rather than open, porous or vented surfaces.
BACKGROUND OF THE INVENTION
[0003] Forming nanofibrous ceramic materials can be challenging for a variety of reasons, including that ceramics are not generally amenable to ordinary fiber spinning techniques. The present invention overcomes this obstacle by forming ceramic nanofibers in a two stage process. In the first stage, an ordinary organic nanofiber is spun by any of a variety of conventional means. In the second stage, the ceramic fiber is formed by depositing a sol-gel film on the organic fiber and then degrading or otherwise removing the organic fibrous portion.
SUMMARY OF THE INVENTION
[0004] The present invention generally relates to a method for making a variety of diameter-controlled nanofibrous structures including solid fibers and other similar or related structures. The present invention also generally relates to the compositions made according to the methods of the present invention.
[0005] More particularly, the present invention is directed to a method for manufacturing a fiber comprising the steps of providing an organic fiber having a diameter that is selected as a template for forming a ceramic nanofiber of a similar size; coating an external surface of the polymeric fiber with a sol-gel coating, wherein the coating comprises a metal halide, metal alkoxide, or metal oxide; heating the coated polymeric fiber to a temperature sufficient to remove the polymeric fiber and form a fiber comprising substantially metal oxide, wherein removal comprises melting or pyrolyzing, and such removal results in forming a substantially solid fiber having a substantially continuous surface; and annealing the substantially metal oxide fiber at a temperature from about 600° C. to about 800° C. Additionally, the present invention is generally related to a fibrous composition made according to foregoing method.
BRIEF DESCRIPTION F THE FIGURES
[0006] FIG. 1 is a SEM of hollow nanofibrous structures after removing the inner polymer core;
[0007] FIG. 2 (A) is a SEM image of titania coated nylon-6 nanofibers; (B) is a SEM of titania coated nylon-6 nanofibers heated at 275° C. for 2 hours; (C) is a SEM image of titania nanofibers heated at 700° C. for 2 hours;
[0008] FIG. 3 is a Fourier transform infrared spectrum showing evidence of pyrolysis;
[0009] FIG. 4 is an X-ray photoelectron spectrum showing evidence of pyrolysis; and
[0010] FIG. 5 is an X-ray diffraction spectrum showing rutile reflection planes.
DETAILED DESCRIPTION OF THE INVENTION
[0011] The present invention generally relates to a process for fabricating diameter-controlled compact nanofibers fibers and related structures by sol-gel processing. More particularly, the present invention generally relates to a process for forming such nanostructures, wherein the process includes depositing sol-gel reagents on nanofibers and then melting or pyrolyzing the organic nanofiber, which results in compacting the fibrous structure. In general the fibers obtained by the process of the present invention have nano-scale diameters.
[0012] As used herein the term nano-scale diameter includes diameters from about 1 nm to about 1000 nm. The term also includes diameters from about 100 nm to about 400 nm, and from about 200 nm to about 400 nm.
[0013] As used herein, the term substantially continuous surface includes fiber surfaces substantially free from openings, vents, and the like, that can result from removing the organic polymer portion. The term is not meant to exclude materials having openings, pores or vents formed by other processes, or due to other physical properties. For instance, the term is not intended to exclude the pores that are inherent in zeolite crystal structures.
[0014] The present invention relates to using sol-gel processing to deposit any of a variety of metal oxides, silicates and/or aluminosilicates. Furthermore, such deposition typically involves heterogeneous growth of such sol-gel nanostructures on the surface of continuous electrospun nanofibers comprising one or more organic polymers. Thus, the process of the present invention includes forming at least a two-layered structure wherein an inner core comprises an organic nanofiber, and an outer layer comprises a sol-gel film. The fiber is formed from the two-layered structure by melting, pyrolyzing, or otherwise removing the polymer core, leaving behind highly temperature-resistant metal oxide, silicate and/or aluminosilicate fibers. The process of removing the organic polymer fiber generally causes the sol-gel portion to form a compacted solid structure. Furthermore, the diameter of the solid sol-gel fiber thus formed can be adjusted by controlling certain process parameters, such as organic fiber diameter, deposition time, metal alkoxide concentration, and pH. Significantly, the present invention is not limited to nano-scale structures. Rather, the process of the present invention can be adapted to form structures having a wide variety of dimensions including 1, 10, and 100 micron scale structures.
[0015] Depositing the sol-gel layer on organic fibers can be conducted in a variety of ways including, without limitation, depositing sol-gel precursors such as metal alkoxides; metal halides; or colloidal particles comprising metal oxides, silicates or aluminosilicates. Furthermore metal alkoxides within the scope of the present invention include, without limitation, titanium methoxides, titanium ethoxides, titanium propoxides, and the like and any combination thereof; silicon methoxides, silicon ethoxides, silicon centrifuging at about 10,000 rpm, and then dried at about 110° C. The fibers are then heated at 275° C. to remove the inner polymer fiber. As shown in FIG. 1 , the SEM of the product demonstrates that the nanofibers are intact after the heating process, and that the fibers have shrunk in size. There is no evidence of any hollow core structure in these images, indicating that these are compact solid fibers.
EXAMPLE 2
[0016] In another example of the present invention nanostructures are produced according to the following process. Sol gel precursor is prepared using titanium isopropoxide, isopropanol, nitric acid and triply distilled filtered water. The chemicals are used as received without further purification. The concentration of the nitric acid is adjusted to about 5 M by addition of triply distilled filtered water. Distilled water (144 ml) is mixed with 20 ml of nitric acid with vigorous stirring. Isopropanol (10 mL) is added to the resultant solution drop by drop under stirring. Cloudiness forms instantaneously after adding about 2 ml of titanium isopropoxide, and a transparent solution is produced after aqua-sonicating for 30 minutes. Electrospun polymer mats are soaked in the sol gel solution resulting in hydrolysis and condensation reactions. The whole mixture is kept at 60° C. for 3 hours in order to obtain rutile-coated polymer nanofibers. The same procedure, but at 90° C. for 1.5 hours, is used to create anatase-coated polymer nanofibers. Milky white precipitates are observed indicating the formation of titania nanoparticles.
[0017] The anatase to rutile transition takes place around 400° C. The crystalline structure of the titania can be altered by controlling the synthesis temperature and the concentration of the nitric acid. Uniformly coated polymer nanofibers are heated above the melting temperature of the polymer (275° C.) in order to degrade or remove polymer template. The sol gel coated nanofibers retain the fibrous morphology even after melting of the polymer nanofibers. Calcination at 300° C. and 700° C. produces anatase and rutile titania nanofibers, respectively.
[0018] Scanning electron microscope (SEM) images of rutile titania-coated nanofibers having diameters about 200 nm can be seen in FIG. 2A . FIG. 2B is an image of titania nanofibers after sol-gel processing and slow heating to 275° C. in an oven for 2 hours. Heating the resultant nanofibers to 700° C. pyrolyzes the nylon-6 completely, propoxides, and the like and any combination thereof; and zirconium methoxides, zirconium ethoxides, zirconium propoxides, and the like and any combination thereof. Furthermore, metal alkoxides within the scope of the present invention include alkoxides of tin, indium, aluminum, germanium, gallium, zinc and the like and any combination thereof.
[0019] Additionally, metal halides within the scope of the present invention include, without limitation, chlorides and bromides of titanium, silicon, zirconium, indium, aluminum, germanium, gallium, zinc and the like and any combination thereof. Finally, metal oxides within the scope of the present invention include, without limitation, oxides of titanium, silicon, zirconium, indium, aluminum, germanium, gallium, zinc and the like and any combination thereof.
[0020] Organic nanofibers of the present invention can be formed in any of a variety of known ways from any of a variety of spinnable polymers. For instance, appropriate methods for forming nanofibers include, without limitation, electrospinning, nanofibers by gas jet (NGJ), wet spinning, dry spinning, melt spinning, and gel spinning. Furthermore, polymer materials within the scope of the present invention include without limitation nylon, polyimide, poly lactic acid and the like and any combination thereof.
[0021] Exemplary patents that disclose NGJ methods include U.S. Pat. Nos. 6,695,992; 6,520,425; and 6,382,526, all of which are incorporated by reference in their entireties. A suitable electrospinning process is disclosed in, for example, U.S. Pat. No. 6,753,454, which is hereby incorporated by reference in its entirety.
EXAMPLE 1
[0022] An example of the present invention comprises the synthesis of compact solid silica fibers as described below. A sol-gel solution is made by adding tetraethyl orthosilicate (TEOS) (44.7 mL, 0.2 M), ammonium hydroxide (18 mL, 0.2 M), and water (45 mL, 3.2 M) to a reaction vessel, which is topped off to 1 liter using ethanol (about 890 mL). Nylon 6 (20 wt % solution in formic acid) nanofibers are electrospun at 15 cm distance and 20 kV directly into the sol-gel solution. The sol-gel solution with the Nylon-6 fibers suspended therein is left at room temperature for about 20 hours without agitation. The particle size resulting from this process is about 100 nm. The nylon 6 web does not dissolve. The web is washed twice by suspending in ethanol and leaving titania nanofibers with 150 nm diameters as seen in FIG. 2C . Shrinkage in the diameter of the nanofibers is observed when the nanofibers are heated, due to the thermal degradation of the polymer.
EXAMPLE 3
[0023] In another example of the present invention hollow nanofibrous structures are formed according to the following process. In order to sol-gel coat 0.2 grams of nylon-6 nanofibers, 110 ml of filtered distilled water is added to 15.2 ml of 5 M nitric acid at room temperature. After mixing, 7.6 ml of 2-propanol is then slowly added. Next, 1.6 ml of titanium isopropoxide is gradually added with a pipette and the solution is ultrasonically agitated for 30 minutes. After half an hour the solution becomes transparent indicating the formation of a sol having nano-scale particles. The electrospun polymer nanofibers are then placed in the sol and the mixture is heated to 65° C. for two hours. This induces the growth of titania nanoparticles on the surface of the nanofibers. The solution becomes cloudy after about two hours, indicating precipitation. The precipitate is separated from the solution by washing several times with methanol, which also removed residual alkoxides.
[0024] The electrospinning and sol-gel synthesis steps result in a coated nanofiber mat. After sol-gel processing the nanofibers are heated to 275° C., which converts the sol-gel and leads to fibers with diameters of about 200 nm. Heating the resultant nanofibers to 700° C. pyrolyzes the nylon-6, leaving titania nanofibers having 150-200 nm diameters.
[0025] Evidence for pyrolysis of the nylon-6 is provided by the Fourier transform infrared spectra of FIG. 3 . Curve A in FIG. 3 indicates that the coated fibers have significant IR absorption features due to the N—H, C—H, and C—O vibrations of nylon after two hours of heating at 275° C. Moisture incorporation may also lead to O—H stretching vibrations, which overlap with the N—H stretching region above 3000 cm −1 . Furthermore, since Ti—O vibrations are present, it appears that heating results in titania formation. As shown in Curve B of FIG. 3 , after annealing the fibers at 700° C. only Ti—O vibrations remain, indicating that pyrolysis of the nylon-6 material has occurred.
[0026] The IR data of FIG. 3 are consistent with the X-ray photoelectron spectra (XPS) of FIG. 4 . In FIG. 4A , the coated fibers heated to 275° C. contain significant amounts of carbon and nitrogen due to the nylon-6. Annealing for two hours at 700° C. diminishes both the C and N XPS features significantly, leaving a spectrum in FIG. 4B that is expected for titania. Some adventitious carbon remains on or within the titania nanofibers as shown in FIG. 4B .
[0027] Titania usually undergoes an anatase to rutile phase transition above 450° C. The X-ray diffraction (XRD) pattern of FIG. 5 verifies that the nanofibers are in the rutile phase after annealing at 700° C. for two hours.
EXAMPLE 4
[0028] In another example of the present invention, fibers made according to the methods disclosed herein can be used to form a filter medium. For instance, the fibers of the present invention can be worked up into a slurry with binder components, and then passed through a wire mesh under vacuum thereby forming a filter cake, which can be dried, calcined, annealed and/or sintered to form a filter medium.
[0029] The foregoing examples are considered only illustrative of the principles of the invention rather than an exclusive list of embodiments. Further, since numerous modifications and changes will readily occur to those of ordinary skill in the art, the invention is not intended to be limited to the exact construction and operation shown and described, and accordingly, all suitable modifications and equivalents are within the scope of the present invention.
|
The present invention is generally directed to a method for making sol-gel ceramic nanofibers, and the compositions resulting from practicing such method. Fibers so formed can be used for fabricating filter media and a wide variety of other ceramic fiber structures and devices.
| 2
|
FIELD OF THE INVENTION
The present invention relates to the field of engagement devices. More particularly, the invention relates to a spring actuated engagement device.
BACKGROUND OF THE INVENTION
The coupling of two elements together at inaccessible, hard to reach areas is often a laborious and time consuming task, requiring the user to access the engagement location from a distance in order to ensure that the elements will be successfully mated together.
It is an object of the present invention to provide an engagement device by which two elements may be mechanically coupled together or separated while a user is disposed at a distance from the engagement location.
It is an additional object of the present invention to provide an engagement device by which two elements are reliably coupled together.
Other objects and advantages of the invention will become apparent as the description proceeds.
SUMMARY OF THE INVENTION
The present invention provides a spring actuated engagement device for remotely coupling a movable member to a stationary member, comprising a fixture mountable onto a stationary member, a spring biased bar that is axially displaceable within a central recess formed within said fixture, an abutting element extending outwardly from one end of said bar for actuating said spring, at least one seating element outwardly spaced from an outer face of said fixture and longitudinally spaced from said abutting element, wherein said abutting element is configured to be axially displaced in a first direction when contacted by a first terminal edge of a movable member, allowing a second terminal edge of said movable member longitudinally spaced from said first edge to be receivable in an interspace between said at least one seating element and said outer face, and to be axially displaced in a second direction opposite to said first direction after a force that initiated said contact with said first edge is released, whereby to engage said movable member.
In one aspect, the fixture is rectilinear and has first and second terminal faces substantially perpendicular to the outer face, a border element being formed between said first terminal face and the central recess to limit displacement of the abutting element in the first direction.
In one aspect, the at least one seating element longitudinally extends from the second terminal face, allowing the movable member to be longitudinally engageable by the abutting element and a portion of said additional face adjoining the at least one seating element and to be transversally engageable by the fixture outer face and the at least one seating element.
In one aspect, the fixture has two side faces and further comprises a corresponding guide element outwardly and laterally protruding from each of said side faces to laterally engage the movable member. The guide element may be formed with a guiding surface for urging the movable member to a correct lateral alignment when the abutting element is being axially displaced in the first direction if said guiding surface is inadvertently contacted by a portion of the movable member.
As referred to herein, the abutment element is axially displaceable in a “longitudinal” direction, the side faces of the fixture are spaced in the “lateral” direction, and the outer face is spaced from the stationary member in the “transversal” direction.
In one aspect, a spring housing, which may longitudinally extend to the abutting element, protrudes outwardly from the bar and the spring retained within said housing is attached at one end to a base of the bar and at another end to a securing element extending outwardly from an inner face of the fixture which borders the central recess. A positioning element fitted in the base of the bar is adapted to contact an edge of an aperture formed in the inner face, to limit displacement of the bar in the second direction.
In one aspect, a position indicating element extends in the second direction from the abutting element to define an interspace between said position indicating element and the spring housing for positioning the movable member first edge when the abutting element is being axially displaced in the first direction. The position indicating element may be formed with an outer guiding surface for urging the movable member first edge into a correct alignment within the interspace between the position indicating element and the spring housing if the movable element is incorrectly transversally aligned.
In one aspect, the engagement device further comprises a locking device for preventing longitudinal displacement of the abutting element once the movable member is engaged.
In one aspect, the locking device is pivotally displaceable and releasably engages the border element when displaced to a locking position.
In one aspect, the first terminal face transversally extends inwardly from the outer face and is sufficiently thicker than the side faces to receive a pin in an aperture formed therein, the locking device being pivotable about said pin.
The present invention is also directed to a locking device for preventing displacement of an actuator, comprising first and second spaced and substantially mutually parallel elements, an end wall extending between said first and second elements, a handle spaced from said end wall, and a pin extending from a terminal portion of said first element into an aperture formed in a fixture and about which said locking device is pivotally displaceable, wherein, when said locking device is set to a locked condition, said first and second elements are sized to engage a border element of said fixture therebetween and said second element is positioned in abutment with said actuator to prevent actuator displacement in a direction between said first and second elements.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a perspective view of an engagement device according to one embodiment of the present invention, shown in an unlocked condition;
FIG. 2 is a rear view of the engagement device of FIG. 1 , shown in a locked condition;
FIG. 3 is a bottom view of the engagement device of FIG. 1 , shown in a locked condition;
FIG. 4 is a rear view of the engagement device of FIG. 1 , shown in an unlocked condition;
FIG. 5 is a perspective view of the engagement device of FIG. 1 , shown in a locked condition;
FIG. 6 is a side view of the engagement device of FIG. 1 , shown in a locked condition;
FIG. 7 is a perspective view of the engagement device of FIG. 1 , shown when an exemplary movable member is engaged therewith; and
FIG. 8 is a perspective view of the movable member of FIG. 7 , shown in an opened condition.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The engagement device of the present invention allows two members, a stationary member and a movable member, to be mechanically coupled together while a user is disposed at a distance from the engagement location. The engagement device has a spring biased bar that slides in the direction of displacement of the movable member, and a seat for receiving and immobilizing an element of the movable member.
FIGS. 7 and 8 illustrate a vertically disposed engagement device 10 , according to one embodiment of the present invention, with which is engaged a rectilinear bracket 5 of an angled arm 62 mounted onto an exemplary movable member embodied by a pivotal service hatch 67 for selectively occluding a passageway 69 through which a building related component, including but not limited to an electrical component, an air conditioner, a roller blind box, can be accessed. An exemplary stationary member is a plaster plate 71 mounted onto a ceiling by a plurality of aluminum beams 73 . When two engagement devices 10 are mounted on the same plaster plate sidewall 74 bordering passageway 69 , hatch 69 is able to pivot more 90 degrees, and up to 150 degrees by virtue of the configuration of angled arms 62 .
It will be appreciated that the present invention is also applicable to an engagement device that is configured to interface with any other configured stationary and movable members.
FIG. 1 illustrates a front view of an unlocked engagement device 10 , when a thin, inverted U-shaped bracket 5 of a movable member is in engagement therewith.
Engagement device 10 has a rectilinear fixture 35 configured with an outer face 7 , i.e. facing away from the stationary member onto which it is mounted, opposed side faces 1 and 11 , an upper face 20 substantially perpendicular to outer face 7 , and a central recess 9 which is recessed with respect to outer face 7 , to accommodate the sliding vertical movement of rectangular, spring biased bar 12 . Abutting element 13 substantially perpendicular to bar 12 extends outwardly from the top thereof. A rectilinear guide element 8 with an oblique guiding surface 25 may protrude laterally, i.e. in a direction away from the central recess, from a corresponding side face, and also outwardly from outer face 7 .
This description refers to an engagement device when the abutting element is disposed at the top of the spring biased bar. It will be appreciated, however, that the invention is also applicable when the engagement device assumes any other suitable orientation.
Seating elements 16 a - b protrude upwardly from the stepped engagement device bottom face 4 (see FIG. 3 ), and are spaced outwardly from the bottom of side faces 1 and 11 , respectively, extending laterally therefrom for a limited distance towards recess 9 . The length of each seating element is slightly longer than the lateral dimension of foot 3 , at the bottom of each leg 6 of bracket 5 .
Engagement device 10 may be mounted onto the stationary member by a bolt or any other suitable fastening element insertable within apertures 27 and 28 , shown in FIG. 2 at the rear of engagement device 10 . Apertures 27 and 28 may be formed in a corresponding recess 17 formed in outer face 7 .
As shown in FIGS. 1, 2 and 6 , abutting element 13 is a thin, relatively large-surface element that is contactable by bracket 5 of the movable member and serves as an actuator for the spring. Abutting element 13 , which may be bifurcated by narrow extending elements 29 when viewed from above or from below, protrudes outwardly beyond the guide elements 8 and extends inwardly to the inner face 15 of central recess 9 , although is separated therefrom.
A lip 33 may slightly extend downwardly from the outer edge of abutting element 13 . A position indicating element 36 , e.g. of triangular cross section, extends downwardly from the underside of abutting element 13 between bifurcated extending elements 29 and lip 33 , to define a guiding surface 39 .
Protruding outwardly from bar 12 is a spring housing 14 , in which is housed spring 18 shown in FIG. 2 . The bottom end of spring 18 is attached to base 19 of bar 12 by horizontal pin 23 , and the top end of the spring is attached to a securing element extending outwardly from rear face 21 of the engagement device. The securing element may be positioned within a cavity 2 formed at an inner region of abutting element 13 . A positioning element 23 , e.g. a pin, fitted horizontally in base 19 is adapted to contact the bottom of oval aperture 26 formed in rear face 21 , to limit the downward displacement of bar 12 .
Referring also to FIG. 4 , abutting element 13 divides central recess 9 into a lower chamber 32 within which bar 12 is slidingly displaceable and an upper chamber 34 within which abutting element 13 is displaceable. Spring 18 is biased to cause bar 12 and abutting element 13 attached thereto to be displaced downwardly when a force is released from abutting element 13 . When abutting element 13 is downwardly biased, upper chamber 34 is unobstructed, making upper border element 38 of outer face 7 which borders upper chamber 34 to become accessible.
Although bar 12 is longitudinally slidable within central recess 9 , detachment of bar 12 from engagement device 10 is prevented by means of a plurality of teeth 24 , e.g. having a rectangular profile, which protrude inwardly into recess 9 from a corresponding sidewall 22 of the latter, to contact bar 12 , as shown in FIGS. 1 and 3 , for example when abutting element 13 is pulled outwardly. Abutting element 13 may be notched at lateral ends thereof, to prevent interference with teeth 24 .
In operation, a user wishing to couple bracket 5 of the movable member to engagement device 10 directs upper edge 42 of bracket 5 to contact the portion of abutting element 13 between spring housing 14 and triangular position indicating element 36 , and applies an upward force to bracket 5 . Abutting element 13 is therefore displaced upwardly to the vicinity of upper border element 38 , providing a clearance between each bracket foot 3 and a corresponding seat 16 . Due to the presence of seating elements 16 a and 16 , bracket 5 is held obliquely with respect to outer face 7 during upward displacement of abutting element 13 , and then each bracket foot 3 is inwardly displaced to contact outer face 7 after the clearance is produced. When the applied force is released, each bracket foot 3 is received in the interspace between a seat and a corresponding side face. Bracket 5 is consequently engaged from the top by abutting element 13 , from the bottom by bottom face 4 , inwardly by outer face 7 , outwardly by seating elements 16 a and 16 and by position indicating element 36 , and to either lateral side by a corresponding guide element 8 .
If the user does not properly position the bracket upper edge 42 , guiding surfaces 25 and 39 urge bracket 5 into a correct alignment. That is, guiding surface 39 will urge bracket upper edge 42 downwardly to a correct position inwardly of position indicating element 36 if bracket upper edge 42 incorrectly contacts guiding surface 39 . Also, an inclined guiding surface 25 will urge the bracket to a correct lateral alignment if it is contacted by a bracket portion.
When it is desired to detach or replace the movable member, a force is simply transmitted from the bracket to the abutting element to cause the latter to be upwardly displaced, after which the bracket is removed from the engagement device.
To prevent inadvertent displacement of the abutting element, locking device 44 shown particularly in FIGS. 1, 2, 4 and 5 may be used.
Plastically deformable locking device 44 comprises an upper element 47 and a lower element 48 which are substantially parallel to engagement device upper face 20 , a vertical wall 51 extending between upper element 47 and lower element 48 , and a handle 56 spaced outwardly from vertical wall 51 when locking device 44 is positioned to a locked condition, as shown in FIG. 5 . Lower element 48 is significantly narrower and shorter than upper element 47 . Protruding upwardly from lower element 48 are a plurality of frictionally engageable elements 53 . The spacing between the bottom face of upper element 47 and frictionally engageable elements 53 is slightly less than the thickness of upper border element 38 .
Locking device 44 is pivotally displaceable about a vertical pin 43 insertable in an aperture formed in upper face 20 of thickened service element 41 , which is provided at the top of engagement device 10 and extends inwardly from outer face 7 . When locking device 44 is pivoted to a locked condition by contacting vertical wall 51 , upper element 47 covers a portion of border element 38 , lower element 48 is received in upper chamber 34 of central recess 9 , and frictionally engageable elements 53 grip the underside of border element 38 to retain engagement device 10 in the locked condition.
When engagement device 10 is in the locked condition, significant upward displacement of abutting element 13 is prevented as the latter will contact the bottom edge of lower element 48 and will not be able to be additionally displaced upwardly. The spring actuated by abutting element 13 is configured to be extended by a specific distance when bracket 5 is engaged by engagement device 10 , as shown in FIG. 5 , so that abutting element 13 will abut the bottom edge of lower element 48 . Thus bracket 5 is positively engaged and cannot be removed from device 10 even if a force is applied to bracket 5 or to abutting element 13 .
Pulling on handle 56 will cause locking device 44 to pivot to the unlocked position, enabling abutting element 13 to be upwardly displaced and bracket 5 to be removed from engagement device 10 .
While some embodiments of the invention have been described by way of illustration, it will be apparent that the invention can be carried out with many modifications, variations and adaptations, and with the use of numerous equivalents or alternative solutions that are within the scope of persons skilled in the art, without exceeding the scope of the claims.
|
A spring actuated engagement device for remotely coupling a movable member to a stationary member comprises a fixture mountable onto a stationary member, a spring biased bar that is axially displaceable within a central recess formed within the fixture, an abutting element extending outwardly from the bar for actuating the spring, and a seating element outwardly spaced from the fixture and longitudinally spaced from the abutting element. The abutting element is axially displaceable in a first direction when contacted by a first edge of a movable member, allowing a second edge of the movable member to be received in an interspace between the seating element and the outer face, and to be axially displaced in a second direction after a force that initiated the contact with the first edge is released. A pivotally displaceable locking device, when set to a locked condition, prevents displacement of the actuator.
| 4
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an image processing apparatus, an image processing method, and a storage medium with computer-executable instructions for processing a document containing authentication information.
2. Description of the Related Art
Japanese Patent Application Laid-Open No. 10-312447 discusses the QR CODE (registered trademark) that is a kind of two-dimensional code that can record a large amount of data in a tiny space.
Japanese Patent Application Laid-Open No. 2003-280469 discusses the GLYPH (registered trademark) code that can control a copying operation.
Using the technologies discussed in Japanese Patent Application Laid-Open No. 10-312447 or Japanese Patent Application Laid-Open No. 2003-280469, paper media such as a card or a document can contain information used for performing electronic control. Accordingly, an access control on the paper media can be realized.
When the technology discussed in the QR CODE® or the GLYPH® is applied to a multifunction peripheral (MFP), the MFP detects a two-dimensional code on a document by scanning, and decodes the two-dimensional code to obtain authentication information of the document. Based on the authentication result, the MFP can perform control for continuing the processing onto the document or stopping the processing.
When the MFP determines that it is possible to continue the processing, by using a send function provided in the MFP, the MFP can convert the document into electronic data and send the data to a file server or a personal computer (PC).
In such a case, authentication information contained in the document is stored as an image of two-dimensional code in the electronic data generated by the MFP.
In consequence, it is not possible to perform an authentication control of the electronic data in the file server or the PC that is the destination of the transmission by the MFP. As a result, even if the document has the authentication information, there is a risk that the document can be freely viewed or copied.
Further, if the authentication control is also performed on the electronic data according to the above-described flow, it may be necessary to analyze the image again.
SUMMARY OF THE INVENTION
According to an aspect of the present invention, an image processing apparatus is provided that includes a generation unit configured to scan a document and generate an original image, a decoding unit configured to decode a two-dimensional code on the original image generated by the generation unit to obtain original information, and a determination unit configured to determine whether the original information obtained in the decoding unit contains a password. The image processing apparatus also includes a conversion unit configured to convert the original image generated in the generation unit into an electronic file attaching the password if the determination unit determines that the original information contains the password, and convert the original image generated by the generation unit into an electronic file without attaching the password if the determination unit determines that the original information does not contain the password, and a sending unit configured to send the electronic file obtained by the conversion in the conversion unit.
According to another aspect of the invention, an image processing apparatus is provided that includes a generation unit configured to scan a document and generate an original image, a decoding unit configured to decode a two-dimensional code on the original image generated by the generation unit to obtain original information, and a determination unit configured to determine whether the original information obtained in the decoding unit requires a password as a condition to permit printing of to print the original image. The image processing apparatus also has a display unit configured to display a request to enter the password if the determination unit determines that the password is required, a conversion unit configured to convert the original image generated by the generation unit into an electronic file without the password if entry of the password is executed in response to the request to enter the password, and convert the original image generated by the generation unit into an electronic file with the password if entry of the password is not executed in response to the request to enter the password, and a sending unit configured to send the electronic file obtained by the conversion in the conversion unit.
Further embodiments, aspects and features of the present invention will become apparent from the following detailed description of exemplary embodiments with reference to the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate numerous exemplary embodiments, features and aspects of the invention and, together with the description, serve to explain principles of the invention.
FIG. 1 illustrates a configuration of a system according to a first exemplary embodiment of the present invention.
FIG. 2 illustrates a flowchart of an example of processing according to the first exemplary embodiment of the present invention.
FIG. 3 illustrates a flowchart of an example of processing according to the first exemplary embodiment of the present invention.
FIG. 4 illustrates a flowchart of an example of processing according to the first exemplary embodiment of the present invention.
FIG. 5 illustrates a flowchart of an example of processing according to a second exemplary embodiment of the present invention.
FIG. 6 illustrates an example of decoding and coding.
FIG. 7 illustrates a flowchart of an example of processing for password entry detection.
DETAILED DESCRIPTION OF THE EMBODIMENTS
Various exemplary embodiments, features and aspects of the present invention will now be herein described in detail below with reference to the drawings.
FIG. 1 illustrates a configuration of a system according to a first exemplary embodiment of the present invention. The system according to the first exemplary embodiment includes, at least one MFP 131 and a client computer 111 .
The MFP 131 may have functions to scan, print, copy, and send. The other functions of the MFP 131 will be described in detail in the following descriptions of exemplary embodiments of the present invention.
In the embodiment as shown, the client computer 111 can receive data sent by the MFP 131 via a network 101 and store the received data. Further, the client computer 111 can display the stored data. The other functions of the client computer 111 will be described in detail in the following descriptions of the exemplary embodiments of the present invention.
In the exemplary embodiments described below, as illustrated in FIG. 1 , a plurality of client computers 111 and 112 , a plurality of MFPs 131 and 132 , and a file server 121 can be connected to the network 101 .
Next, an example of a processing flow ( FIG. 2 ) according to the first exemplary embodiment is described.
The MFPs 111 and 112 in FIG. 1 first receive a user's selection of functions such as “send mode” or “print mode” displayed on operation screens, and receive a user's selection of a start button displayed on the operation screens of the MFPs 111 and 112 .
FIG. 2 illustrates a flowchart of the processing example that starts in response to the reception of the user's selection of the start button displayed on the operation screen of the MFP. The overall processing in the individual steps in the flowchart illustrated in FIG. 2 is controlled by a central processing unit (CPU) in the MFP.
In step S 2001 , the MFP scans a document on a document positioning plate and generates an original image as an electric signal.
In step S 2002 , the MFP detects an area where a two-dimensional code exists in the original image.
Then, in step S 2003 , the MFP decodes the two-dimensional code detected in step S 2002 , and the processing proceeds to step S 2004 .
In a case where the two-dimensional code is not detected or decoded in step S 2002 or step S 2003 , the MFP displays an appropriate error indication on the operation screen.
Definitions of the terms “decoding” and “coding” in the exemplary embodiment are described with reference to FIG. 6 . FIG. 6 illustrates information (e.g., original information) contained in a two-dimensional code. By coding the original information as an image, the two-dimensional code is generated.
For example, the two-dimensional code is generated by coding the original information “SCAN: PERMIT WITH CONDITIONS (PERMIT IF PASSWORD IS CORRECT), PASSWORD: abcdefg” as an image.
In the exemplary embodiment of the present invention, “coding” is defined as “coding an original information as an image and generating a two-dimensional code”. While, in the exemplary embodiment, “decoding” is defined as “obtaining the original information from the two-dimensional code”. These are meanings of the terms “decoding” and “coding” defined according to the exemplary embodiment.
In step S 2004 , the MFP stores the bit-mapped original image generated in step S 2001 , the original information obtained in step S 2003 , and the existing area of the two-dimensional code detected in step S 2002 . In the processing, the MFP stores the original image generated in step S 2001 according to a bit map method into the memory.
In step S 2005 , the MFP determines whether a selection of the “send mode” has been received or the “print mode” has been received before a selection of a start button is received.
In step S 2005 , if it is determined that the selection of the “print mode” has been received (PRINT MODE in step S 2005 ), the processing proceeds to step S 2007 . An example of processing performed by the MFP in step S 2007 is illustrated in FIG. 3 .
In step S 3001 in FIG. 3 , the MFP searches for authentication information for operation restriction in the information stored in the memory in step S 2004 , and the processing proceeds to step S 3002 .
In the description, the authentication information for operation restriction is described with three examples of “permit”, “inhibit”, and “permit with condition by a password entry”. However, in the authentication information for operation restriction, information other than the three examples of “permit”, “inhibit”, and “permit with condition by a password entry” may also be contained.
In step S 3002 , if the MFP determines the authentication information as “permit” (PERMIT in step S 3002 ), the processing proceeds to step S 3003 .
In step S 3003 , the MFP performs a normal copying processing. Processing then proceeds to step S 3013 .
In step S 3002 , if the MFP determines the authentication information as “inhibit” (INHIBIT in step S 3002 ), the processing proceeds to step S 3004 .
In step S 3004 , the MFP cancels the job, and processing is ended.
In step S 3002 , if the MFP determines the authentication information as “permit with condition by a password entry” (PERMIT WITH CONDITIONS in step S 3002 ), the processing proceeds to step S 3005 .
In step S 3005 , the MFP determines whether it is a top page of the job. In step S 3005 , if the MFP determined that it is a top page (YES in step S 3005 ), the processing proceeds to step S 3006 .
In step S 3006 , the MFP displays a password entry request screen on the operation screen to prompt the user to enter a password.
In step S 3006 , an example of a processing as illustrated in FIG. 7 may be implemented. More specifically, in step S 7001 , the MFP determines whether an entry of a password is detected.
In step S 7001 , if the entry of the password is not detected (NO in step S 7001 ), in step S 7002 , the MFP cancels the job.
On the other hand, if the entry of the password is detected (YES in step S 7001 ), the processing proceeds to step S 3007 .
In step S 3007 , the MFP performs an authentication by comparing the password information stored in the memory in step S 2004 with the password entered in step S 3006 , and the processing proceeds to step S 3008 .
In step S 3008 , if the MFP determines that the authentication is successful (YES in step S 3008 ), the processing proceeds to step S 3009 and the MFP performs normal copying processing.
In step S 3008 , if the MFP determines that the authentication is not successful (NO in step S 3008 ), the processing proceeds to step S 3010 where the MFP cancels the job and processing is ended.
In step S 3005 , if the MFP determines that it is not a top page (NO in step S 3005 ), the processing proceeds to step S 3011 .
In step S 3011 , the MFP determines whether the password stored in the memory in step S 2004 is the same as a password of a previous page of the job. In step S 3011 , if the MFP determines that the passwords are the same (YES in step S 3011 ), the processing proceeds to step S 3009 and the MFP performs normal copying processing. Processing then proceeds to step S 3013 .
In step S 3011 , if the MFP determines that the password is not the same as the password of the previous page of the job (NO in step S 3011 ), the processing proceeds to step S 3012 where the MFP cancels the job, and processing is ended.
Then, the MFP repeats the processing from step S 3001 to S 3012 until all pages in the job are processed. More specifically, in step S 3013 , the MFP determines whether it is processing a final page. Then, in step S 3013 , if the MFP determines that it is not the processing of the final page (NO in step S 3013 ), the processing returns to step S 3001 . On the other hand, if the MFP determines that it is the processing of the final page (YES in step S 3013 ), the processing ends.
In step S 2005 , if the MFP determines that the selection of “send mode” has been received (SEND MODE in step S 2005 ), the processing proceeds to step S 2006 . An example of processing performed by the MFP in step S 2006 is illustrated in FIG. 4 .
In step S 4001 , the MFP searches the information stored in the memory in step S 2004 for authentication information for operation restriction, and the processing proceeds to step S 4002 .
In the description, the authentication information for operation restriction is described with three examples of “permit”, “inhibit”, and “permit with condition by a password entry”. In the authentication information for operation restriction, information other than the three examples of “permit”, “inhibit”, and “permit with condition by a password entry” may also be contained.
In step S 4002 , if the MFP determines the authentication information as “permit” (PERMIT in step S 4002 ), the processing proceeds to step S 4003 .
In step S 4003 , the MFP performs normal send processing. Processing then proceeds to step S 4013 .
In step S 4002 , if the MFP determines the authentication information as “inhibit” (INHIBIT in step S 4002 ), the processing proceeds to step S 4004 .
In step S 4004 , the MFP cancels the job, and processing is ended.
In step S 4002 , if the MFP determines the authentication information as “permit with condition by password entry” (PERMIT WITH CONDITIONS in step S 4002 ), the processing proceeds to step S 4005 .
In step S 4005 , the MFP determines whether it is a top page of the job. In step S 4005 , if the MFP determines that it is the top page (YES in step S 4005 ), the processing proceeds to step S 4006 .
In step S 4006 , the MFP displays a password entry request screen on the operation screen to prompt the user to enter a password.
In step S 4007 , an example of processing as illustrated in FIG. 7 may be implemented. More specifically, in step S 7001 , the MFP determines whether an entry of a password is detected.
In step S 7001 , if the entry of the password is not detected (NO in step S 7001 ), in step S 7002 , the MFP cancels the job.
On the other hand, if the entry of the password is detected (YES in step S 7001 ), the processing proceeds to step S 4007 .
In step S 4007 , the MFP performs an authentication by comparing the password information stored in the memory in step S 2004 with the password entered in step S 4006 , and the processing proceeds to step S 4008 .
In step S 4008 , if the MFP determines that the authentication is successful (YES in step S 4008 ), the processing proceeds to step S 4009 .
In step S 4009 , the MFP generates an encrypted Portable Document Format (PDF) of the bit-mapped original image that was stored in the memory in step S 2004 , using the password also stored in the memory.
Here, the meaning of “generating an encrypted PDF using the bit-mapped original image and the password” is described in detail. In the exemplary embodiment, the encrypted PDF is one type of PDF file. The “generating an encrypted PDF using the bit-mapped original image and the password” means as follows: the bit-mapped original image is converted into the image of the PDF format and a PDF file is generated; then, in order to limit access to the original image of the PDF format, the password is added to the PDF file. By adding the password, the encrypted PDF is generated. In a case where a request to access the encrypted PDF is issued by the user on a transmission destination device (for example, a PC), and if the added password matches a password input by the user on the destination device, the original image of the PDF format is displayed. On the other hand, if the passwords do not match with each other, the original image of the PDF format is not displayed. The MFP sends the generated encrypted PDF to the destination device set in the “send mode”.
In the exemplary embodiment, as an example of the electronic file that records the electronic data generated from the original image read into the MFP, the PDF file is described. However, it is not limited to the PDF file. For example, if it is possible to encrypt, any electronic file can be employed in the exemplary embodiments of the present invention.
In step S 4008 , if the MFP determines that the authentication is not successful (NO in step S 4008 ), the processing proceeds to step S 4010 .
In step S 4010 , the MFP cancels the job, and processing is ended.
In step S 4005 , if the MFP determines that it is not a top page (NO in step S 4005 ), the processing proceeds to step S 4011 .
In step S 4011 , the MFP determines whether the password stored in the memory in step S 2004 is the same as a password of a previous page of the job. In step S 4011 , if the MFP determines that the passwords are the same (YES in step S 4011 ), the processing proceeds to step S 4009 . In step S 4009 , the MFP generates an encrypted PDF of the bit-mapped original image that was stored in the memory in step S 2004 , using the password also stored in the memory and sends the encrypted PDF to a destination device set in the “send mode”. In the exemplary embodiment, the electronic file such as an encrypted PDF was generated using the password. However, as a different exemplary embodiment, it is assumed that the electronic file was generated using a different password. In the different exemplary embodiment, entry of the different password is also requested in s 4006 and the different password is entered. In addition, in s 4009 , the electronic file was generated using the different word. This different exemplary embodiment also protects the electronic file by a password although it is a bit burden for the user to enter two passwords.
In step S 4011 , if the MFP determines that the password is not the same as the password of the previous page of the job (NO in step S 4011 ), the processing proceeds to step S 4012 .
In step S 4012 , the MFP cancels the job, and processing is ended.
Then, the MFP repeats the processing from step S 4001 to S 4012 until all pages in the job are processed. More specifically, in step S 4013 , the MFP determines whether it is processing a final page. Then, in step S 4013 , if the MFP determines that it is not processing of the final page (NO in step S 4013 ), the processing returns to step S 4001 . On the other hand, if the MFP determines that it is the processing of the final page (YES in step S 4013 ), the processing ends.
By performing the above-described processing, even if a document having embedded authentication information therein is scanned, electronic data is generated, and the electronic data is sent to a file server or a PC, the authentication information can still be applied. Furthermore, the security policy applied to the information on the document can also be applied to the electronic data.
A second exemplary embodiment of the present invention is realized by a configuration similar to the system illustrated in FIG. 1 .
The second exemplary embodiment differs from the first exemplary embodiment in processing performed when a selection of the “send mode” by the user is received. Accordingly, descriptions will be made only about those points that replace those FIG. 4 , with reference to FIG. 5 .
In step S 2005 in FIG. 2 , if the MFP determines that the selection of the “send mode” has been received (SEND MODE in steps S 2005 ), the processing proceeds to step S 2006 . The processing performed by the MFP in step S 2006 in this embodiment is illustrated in FIG. 5 .
In step S 5001 , the MFP determines whether the information stored in the memory in step S 2004 contains authentication information for operation restriction. In the description, the authentication information for operation restriction is described with three examples of “permit”, “inhibit”, and “permit with condition by a password entry”. However, in the authentication information for operation restriction, information other than the three examples of “permit”, “inhibit”, and “permit with condition by a password entry” may also be contained.
In step S 5002 , if the MFP determines the authentication information as “permit” (PERMIT in step S 5002 ), the processing proceeds to step S 5003 .
In step S 5003 , the MFP performs normal send processing. Processing then advances to step S 5015 .
In step S 5002 , if the MFP determines the authentication information as “inhibit”, the processing proceeds to step S 5004 .
In step S 5004 , the MFP cancels the job, and processing is ended.
In step S 5002 , if the MFP determines the authentication information as “permit with condition by a password entry” (PERMIT WITH CONDITIONS in step S 5002 ), the processing proceeds to step S 5005 .
In step S 5005 , the MFP determines whether it is a top page of the job. In step S 5005 , if the MFP determines that it is a top page of the job (YES in step S 5005 ), the processing proceeds to step S 5006 .
In step S 5006 , the MFP displays a password entry request screen on the operation screen to prompt the user to enter a password.
Then, in step S 5006 , the processing illustrated in FIG. 7 is implemented. More specifically, in step S 7001 , the MFP determines whether an entry of a password is detected.
In step S 7001 , if the entry of the password is not detected (NO in step S 7001 ), in step S 7002 , the MFP cancels the job.
On the other hand, in step S 7001 , if the entry of the password is detected (YES in step S 7001 ), the processing proceeds to step S 5007 .
In step S 5007 , the MFP performs an authentication by comparing the password information stored in the memory in step S 2004 with the password entered in step S 5006 . The password may be used as a condition to permit printing of the original image.
In step S 5008 , if the MFP determines that the authentication is successful (YES in step S 5008 ), the processing proceeds to step S 5009 .
In step S 5009 , the MFP performs normal send processing. In step S 5009 , the processing described in the first exemplary embodiment is not performed. That is, the processing in which the MFP generates an encrypted PDF of the bit-mapped original image that was stored in the memory in step S 2004 , using the password also stored in the memory, is not performed.
In step S 5008 , if the MFP determines that the authentication is not successful (NO in step S 5008 ), the processing proceeds to step S 5010 .
In step S 5010 , the MFP cancels the job, and processing is ended.
In step S 5005 , if the MFP determines that it is not a top page (NO in step S 5005 ), the processing proceeds to step S 5012 .
In step S 5012 , the MFP determines whether the password stored in the memory in step S 2004 is the same as a password of a previous page of the job. In step S 5012 , if the MFP determines that the passwords are the same (YES in step S 5012 ), the processing proceeds to step S 5013 .
In step S 5013 , the MFP determines whether a password entry by the user is detected.
In step S 5013 , if the MFP determines that the password entry is detected (YES in step S 5013 ), the processing proceeds to step S 5009 and the MFP performs normal send processing. Processing then advances to step S 5015 .
In step S 5013 , if the MFP determines that the password entry is not detected (NO in step S 5013 ), the processing proceeds to step S 5011 . In step S 5011 , the MFP generates an encrypted PDF of the bit-mapped original image that was stored in the memory in step S 2004 , using the password also stored in the memory and sends the encrypted PDF to a destination device set in the “send mode”. Processing then advances to step S 5015 .
In step S 5012 , if the MFP determines that the password is not the same as the password of the previous page of the job (NO in step S 5012 ), the processing proceeds to step S 5014 .
In step S 5014 , the MFP cancels the job, and processing is ended.
Then, the MFP repeats the processing from steps S 5001 to S 5014 until all pages in the job are processed. More specifically, in step S 5015 , the MFP determines whether it is processing a final page. Then, in step S 5015 , if the MFP determines that it is not processing of the final page (NO in step S 5015 ), the processing returns to step S 5001 . On the other hand, if the MFP determines that it is the processing of the final page (YES in step S 5015 ), processing ends.
In the case where the MFP scans a document having embedded authentication information, generates electronic data, and sends the electronic data to a file server or a PC, by performing the above-described processing, control described below can be performed.
A user once authenticated by the MFP to access a document may not be required to enter the password again. Accordingly, the convenience of the user can be increased. This may be effective when the user operating the MFP sends a document to a user's PC as a destination using the send function of the MFP. Whether the user operating the MFP is the same as the user of the destination address in the “send mode” can be determined using an available login function, which can be separately provided.
Further, even if a user operating the MFP does not know the authentication information of the document, the user can use the send function of the MFP. This may be effective when the user operating the MFP sends the document to a PC other than the user's PC as a destination using the send function of the MFP. Although the authentication control of the document is not performed in the MFP, an authentication control can be performed in the destination PC. Accordingly, the operability of the user can be increased while the security of the information of the document can be maintained.
In the above-described exemplary embodiments, the two-dimensional code has been employed. However, the present invention is not limited to that code, but instead a one-dimensional code, a digital watermark, a steganography, or the like, can also be employed.
Further, in the above exemplary embodiments, the memory has been used as a medium for storing data. However, the medium is not limited to the memory, but instead any medium can be employed if data can be stored (for example, any one or more of a hard disk drive (HDD) or a random access memory (RAM)) in place of the memory.
Further, in the above-described exemplary embodiments, it has been assumed that the MFP performs the scanning operation. However, in the present descriptions, the scanning refers to optically reading an image on a document. Thus, for example, the exemplary embodiments of the present invention can also be realized by photographing with a digital camera.
Further, in the above-described exemplary embodiments, the MFP can perform all of reading an image, processing information, and printing an image on a sheet. However, devices that can perform one or more of reading an image, processing information, and printing an image on a sheet may also be individually provided.
In the present specification, the image processing apparatus can be an apparatus that can perform at least processing of information. Further, in the present specification, the image processing apparatus can also be an apparatus that can perform at least processing of information and printing of an image on a sheet.
Further, the aspects of the present invention can also be achieved by providing a storage medium that contains computer-executable instructions, such as by recording a program code, that implements one or more of the procedures described in the flowcharts according to the above-described exemplary embodiments, and by reading and executing the computer-executable instructions stored in the storage medium with a computer. In such a case, the storage medium itself, containing the computer-executable instructions that are read from the storage medium, implements the functions according to the exemplary embodiments mentioned above, and accordingly, the storage medium having the computer-executable instructions may comprise an embodiment in accordance with the present invention.
As the storage medium for supplying such computer-executable instructions, for example, at least one of a flexible disk, a hard disk, an optical disk, magneto-optical disk, a CD-ROM, a CD-R, a magnetic tape, a nonvolatile memory card, or a ROM can be used.
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the exemplary embodiments disclosed herein. Rather, the scope of the following claims is to be accorded the broadest interpretation so as to encompass all modifications, equivalent structures, and functions.
This application claims priority from Japanese Patent Application 2008-015502 filed on Jan. 25, 2008, which is hereby incorporated by reference herein in its entirety.
|
An image processing apparatus includes a generation unit configured to scan a document and generate an original image, a decoding unit configured to decode a two-dimensional code on the original image generated in the generation unit to obtain original information, and a determination unit configured to determine whether the original information obtained in the decoding unit contains a password. The image processing apparatus also includes a conversion unit configured to convert the original image generated by the generation unit into an electronic file attaching the password if the determination unit determines that the original information contains the password, and convert the original image generated by the generation unit into an electronic file without attaching the password if the determination unit determines that the original information does not contain the password, and a sending unit configured to send the electronic file obtained by the conversion in the conversion unit.
| 6
|
BACKGROUND OF THE INVENTION
A. Field of the Invention
The present invention relates to methods and apparatus for detecting and abating leaks of flowing liquids from pipes in buildings and similar structures. More particularly, the invention relates to a method and apparatus which uses differential flow rate sensors for detecting water leaks, particularly in closed loop water circulation systems, and solenoid valves to shut off water flow if a detected leak rate exceeds a predetermined value.
B. Description of Background Art
Contemporary buildings of various types, and particularly hospitals, institutional buildings, and larger commercial and industrial buildings employ a variety of water distribution piping or plumbing systems. Thus, in addition to plumbing used to supply potable water for consumption by the building' occupants, highly purified water for use in production processing, or lower quality water for other purposes, many larger contemporary buildings also have at least one of the following two additional types of water distribution systems through which water is circulated, but infrequently discharged. One such water circulation or distribution system, which may be referred to as a “closed-loop” or closed-cycle system is used to supply water to ceiling-mounted fire extinguisher sprinkler heads. Obviously, water conveyed through plumbing of a building water supply system to fire sprinkler heads is discharged from the system rarely, that is, only in the event of a fire, or during periodic testing of the fire sprinkler system and sprinkler heads.
A second type of closed-loop water circulation system used in many larger contemporary buildings comprises part of the Heating, Ventilating and Air Conditioning (HVAC) system of the building. In particular, some larger buildings including hospitals use hot water as a primary working fluid to heat various regions or zones of the building to different individually controllable temperatures. The hot water is generated by a boiler which is generally located in a basement of the building, or in another structure which houses the “mechanical plant” of the building adjacent to the building. The hot water is typically circulated in a continuously, closed loop cycle, which originates at the hot, discharge side of a boiler heat exchanger.
Heated water issued from the discharge side of a boiler heat-exchanger is pumped upwardly through a vertical hot water source (HWS) riser pipe to the highest building floor requiring heating. At each location or zone of a building which requires heating, the hot water is input to a box-like heat exchanger terminal, such as a Variable Air Volume (VAV) terminal. Within the VAV terminal, air from an external source which is moved by an external or internal blower or fan is directed to flow in contact with the exterior surfaces of a coiled length of tubing called a heater coil which has an inlet port fitting which is connected to and receives hot water from the hot water source riser pipe.
The heater coil functions as a flowing air to hot water heat exchanger, and heats the air which flows through the heater coil. The flowing air is heated to a temperature which is adjusted by a thermostatically controlled fan and/or a damper valve for varying the volume of temperature controlled air which is discharged from the VAV terminal and conducted through ducts to ceiling diffusers or other outlet ports in various rooms of a building. Cooled water from the discharge side of the heat exchanger coil is conducted back down through a hot water return (HWR) riser line to the cold inlet side of the boiler heat exchanger. Thus, in such a system, a fixed volume of water is continuously circulated through the system, and is not discharged.
As can be well imagined, heating systems of the type described above, when used in large buildings with many zones and associated heat exchanger terminals, typically include a substantially large number of individual pipes, tubes and fittings. Thus there is the possibility of a leak developing at many different locations in the closed-loop system, the probability of which is increased in the event of seismic disturbance of the building. Therefore, it is understandable that prudent building maintenance procedures would necessitate monitoring such closed-loop water circulation systems for leaks, and providing an alarm signal to building maintenance personnel in the event of a leak. Also, it would be desirable to provide a method and apparatus for automatically shutting off flow of water if a leak is detected.
Regarding first the problem of detecting a water leak, there are of course a large variety of water leak detectors which employ sensors that utilize a supply voltage and a pair of electrodes to detect electrically conductive water which has leaked onto and bridged the sensor electrodes. However, such electrolytic water leak sensors are effective only in detecting water leakage at discrete locations where the sensors are placed. Such point sensors would be for detecting leaks in most closed-loop water circulation systems, such as an HVAC hot water circulation system of the type described above. This is because a water leak detection system using point sensors for systems such as closed-loop water circulating systems which extend over a large area would require an unreasonably large number of individual sensors which were placed near every possible leakage point.
That the detection and abatement of water leaks in contemporary buildings is an important problem is evidenced by two recent cases in California, where leakage from broken building hot water circulation systems caused more than one million dollars worth of damage in each of the buildings. Part of the expenses associated with water leaks in buildings results from modern building codes and potential legal liability which require the complete removal and replacement of all drywall that has been subjected to water leaks for more than 72 hours, to prevent the growth of molds which can cause health problems.
More important than potential financial losses which can result from water leakage that is not timely detected and abated is the possibility of serious injury or even death which can result if a leak in a hot water circulation system of a hospital building should occur. For example, a hot water leak may allow sufficient water to accumulate, leak through ceilings and scald patients in their beds on lower floors.
The foregoing considerations of potential financial losses, bodily injuries and even deaths which may result from water leaks in modern buildings, and the unavailability of an adequate solution to the problem of promptly detecting leaks and shutting off water flow in closed-loop water circulation systems prompted the present invention.
OBJECTS OF THE INVENTION
An object of the present invention is to provide a method and apparatus for detecting leaks in systems which convey flowing liquids such as water.
Another object of the invention is to provide a method and apparatus for detecting leaks from conduits which carry a flowing liquid such as water which uses a pair of differential flow-rate sensors to detect differences between upstream and downstream flow rates resulting from leakage of liquids at a location between upstream and downstream locations of a conduit where the flow rate sensors are located.
Another object of the invention is to provide a method and apparatus for detecting leakage of liquid flowing through a piping system including an upstream source line and a downstream return line, the apparatus using a pair of flow-rate sensors for detecting differences between upstream and downstream flow rates which signify leakage of flowing liquid at a location between the upstream and downstream flow-rate sensors.
Another object of the invention is to provide a method and apparatus for detecting leakage of liquid from a closed-loop liquid circulation piping system for conducting water to and from a terminal, the apparatus including an upstream flow rate sensor and a downstream flow rate sensor to detect differences in upstream and downstream flow rates, control logic circuitry which outputs an alarm status signal if the difference in upstream and downstream flow rates exceeds a predetermined threshold value, an upstream valve in the upstream line operatively interconnected and responsive to the alarm status signal in shutting off upstream flow of liquid to the terminal, and an optional downstream shut-off valve responsive to the alarm status signal in shutting off downstream flow of liquid from the terminal.
Various other objects and advantages of the present invention, and its most novel features, will become apparent to those skilled in the art by perusing the accompanying specification, drawings and claims.
It is to be understood that although the invention disclosed herein is fully capable of achieving the objects and providing the advantages described, the characteristics of the invention described herein are merely illustrative of the preferred embodiments. Accordingly, we do not intend that the scope of our exclusive rights and privileges in the invention be limited to details of the embodiments described. We do intend that equivalents, adaptations and modifications of the invention reasonably inferable from the description contained herein be included within the scope of the invention as defined by the appended claims.
SUMMARY OF THE INVENTION
Briefly stated, the present invention comprehends a method and apparatus for detecting leaks from a conduit such as a pipe carrying a flowing liquid, and for shutting off flow of the liquid if a detected leak rate exceeds a predetermined, preset value. More particularly, the method and apparatus of the present invention provide a means for detecting leakage of water flowing through a pipe, tube or other conduit, providing an alarm status signal if the detected leak rate exceeds a predetermined, preset value, and actuating an upstream shut-off valve and an optional downstream shut-off valve in response to the alarm status signal.
The novel leak detection and shut-off method and apparatus according to the present invention have a wide variety of useful applications. However, a primary intended application for the method and apparatus of the present invention is to minimize potential property damage and injuries to humans which could result from leakage of water from a hot water circulation system which comprises part of a Heating, Ventilating and Air Conditioning (HVAC) system of a building.
A water leak detection and shut-off apparatus according to the present invention includes a first, upstream flow rate sensor. The upstream flow rate sensor is used to measure the flow rate of a liquid such as hot water at a location between a source of flowing liquid, such as a hot water source (HWS) riser pipe, to an inlet port of a destination terminal for the flowing liquid, such as a Variable Air Volume (VAV) air-to-water heat exchanger box.
The leak detection and shut-off apparatus according to the present invention includes a second, downstream flow rate sensor. The downstream flow rate sensor is used to measure the flow rate of a liquid such as hot water at a location between an outlet port of a destination such as a VAV terminal and a return conduit for liquid from the terminal, such as a hot water return (HWR) riser pipe.
According to the present invention, the leak detection and shut-off apparatus also includes at least a first, upstream shut-off valve. The upstream shut-off valve is located between a source of flowing liquid, such as a HWS riser pipe, and a terminal such as a VAV box. In a preferred embodiment, the upstream shut-off valve is a solenoid actuated valve which has an inlet port connected to the HWS riser pipe and an outlet port connected to a section of pipe in which is located the first, upstream flow rate sensor.
The leak detection and shut-off apparatus according to the present invention includes a control module which contains electronic logic control circuitry that has a first set of input signal or interrupt lines which are electrically connected to signal output terminals of the upstream flow rate sensor. The control logic circuitry processes signals received from the upstream flow rate sensor, and uses scaling circuitry to produce a signal, preferably a digital signal which has a numeric value that has a magnitude which is proportional to the measured, flow rate of liquid through the upstream flow sensor. For example, if the range of normal flow rates through the upstream flow sensor were expected to be between 60 and 80 gallons per Minute (GPM), the upstream flow rate sensor and control circuitry, could be selected to have a full-scale output voltage of 5 volts D.C. for a flow rate of 100 GPM, 4 volts for 80 GPM, 3 volts for 60 GPM, etc.
The control module of the leak detection and shut-off apparatus according to the present invention includes a second set of input or interrupt lines which are electrically connected to the signal output terminals of the downstream flow rate sensor. Scaling circuitry within the control module outputs a voltage scaled to the flow rate measured by the downstream flow rate sensor, which has a similar and preferably the same sensitivity or scale factor as that of the upstream flow rate sensor, i.e., 5 volts for a measured downstream flow rate of 100 GPM, 4 volts for a 80 GPM flow rate, 3 volts for a 60 GPM flow rate, etc.
According to the invention, the control module also includes a subtractor which is preferably implemented as a software application that resides in a; microprocessor, micro-controller, or other such digital computational circuitry.
The subtractor of the control module outputs a signal which is proportional to the difference between upstream and downstream flow rates measured by the upstream and downstream flow rate sensors, respectively. The control module also has a memory location which contains a predetermined differential flow rate limit value, e.g., 0.1 GPM, which is input to the control module as a pre-programmed number, or input by an external data input.
If the predetermined differential flow rate limit value is exceeded, comparator circuitry within the control module which has an input connected to the subtractor outputs an alarm status signal, which typically would be a logic TRUE signal. For example, the control module could be programmed to provide an alarm status signal upon detecting a flow rate difference equal to or exceeding 0.1 GPM between upstream and downstream flow rate sensors. Since, in the absence of leakage at any place between upstream and downstream flow rate sensors, the flow rates measured by the two sensors would be substantially identical, save for small frictional losses, it can be inferred that any difference greater than a certain small threshold value between measured upstream and downstream flow rates signifies existence of a leak somewhere in the piping system between the two sensors.
When the difference between measured upstream and downstream flow rates exceeds a predetermined threshold limit value and thus causes the alarm status output line of the control module to go to a logic TRUE state, the alarm status signal actuates and energizes a solid state or electro-mechanical valve shut-off relay. In turn, the valve shut-off relay interrupts a 24-volt A.C. power supplied to the upstream solenoid shut-off valve.
The solenoid shut-off valve is a normally closed valve which opens to allow flow only when supplied with continuous electrical power. Therefore, if a leak rate which exceeds a predetermined limit value occurs, or if electrical power is interrupted to the building mains which supply power to the control apparatus, according to the present invention, the upstream shut-off valve immediately and automatically closes and interrupts the flow of hot water from the hot water source riser line to a destination which is downstream from the apparatus, such as a VAV terminal. Thus, in the event of a detected water leak or interruption of building power, the apparatus according to the present invention is effective in immediately terminating flow of hot water beyond the upstream shut-off valve. Optionally and desirably, the alarm status signal would also be sent to building maintenance stations to inform maintenance personnel of a detected leak.
A preferred embodiment of a leak detection method and apparatus according to the present invention also includes a normally closed, solenoid actuated downstream shut-off valve, which may be identical to the upstream shut-off valve. The downstream shut-off valve is located between the downstream flow rate sensor and the Hot Water Return (HWR) riser pipe. The downstream shut-off valve is operated in unison with the upstream shut-off valve, i.e., it is closed when a leak of a predetermined minimum value occurs, or if electrical power to the building is interrupted. The downstream shut-off valve is provided in addition to the upstream shut-off valve to prevent any water to the riser HWS or HWR lines from flowing back to the area where the leak has been detected.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of an apparatus for water leak detection and shut-off method according to the present invention, showing the apparatus installed in a closed-loop water circulation plumbing system.
FIG. 2 is a more detailed schematic diagram of a control module comprising part of the apparatus of FIG. 1 .
FIG. 3 is a partly diagrammatic view of a Variable Air Volume (VAV) terminal, one of a variety of different types of terminal equipment interconnectable to the leak detection and shut-off apparatus of FIG. 1 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 illustrates a basic embodiment of water leak detection and shut-off apparatus 10 using differential flow rate sensors according to the present invention. FIG. 2 is a more detailed schematic view of a control panel 11 A and control module 11 comprising part of the apparatus 10 of FIG. 1 . FIG. 3 is a partly diagrammatic view of a Variable Air Volume (VAV) terminal 12 which; typifies a terminal component of a closed-loop water circulation system of a type which apparatus 10 is intended for use with.
Referring now to FIG. 1 , it may be seen that water leak detection and shut-off apparatus 10 according to the present invention includes an upstream inlet port 13 for receiving a flowing liquid such as hot water which is pressurized above ambient atmosphere pressure by a pump and/or a gravity pressure head, i.e., from a pump at any elevation or a tank at a higher elevation than inlet port 13 . Upstream inlet port 13 is connected by a fluid pressure-tight tube or pipe to the inlet port 15 of a first, upstream solenoid valve 14 .
As shown in FIG. 1 , upstream inlet port 13 of apparatus 10 includes an inlet pipe 16 which is continuous with or connected through a fitting (not shown) to a source of pressurized liquid, such as an upper part of a Hot Water Source (HWS) riser pipe 17 which is connected at the lower end to a source of hot water, such as a boiler heat exchanger. As is also shown in FIG. 1 , inlet port 13 of apparatus 10 may optionally include an upstream inlet manual shut-off valve 18 which has an inlet port connected to inlet pipe 16 , and an outlet pipe 19 which is connected between an outlet port of manual shut-Off valve 18 and inlet port 15 of solenoid valve 14 .
Solenoid valve 14 is preferably a normally closed (NC) valve in which an internal spring maintains a gate element, such as a ball or plate, of the valve in a fully closed position unless an electrical power such as 24-volt A.C. power is input to terminals 20 , 21 of the valve, thus actuating a solenoid within the valve to open the gate against the closing force of the valve's internal spring. In an example embodiment of apparatus 10 which was designed, built and tested by the present inventors, upstream solenoid valve 14 was a B220+NC/FC+LF24US model manufactured by Belimo Amiricas, 43 Old School Rd., Danbury, Conn. 06810. That valve had the following characteristics spring return normally closed full port ball valve. As shown in FIG. 1 , valve 14 has an outlet port 22 .
Referring still to FIG. 1 , it may be seen that water leak detection and shut-off apparatus 10 according to the present invention includes a first, upstream flow rate sensor 23 . Flow rate sensor 23 has a tubular body 24 which has disposed longitudinally therethrough a bore 25 . Bore 25 of flow rate sensor 23 preferably has a cross-sectional area which is large enough to provide a negligibly small impedance or restriction to flow of liquid through apparatus 10 .
As shown in FIG. 1 , bore 25 of sensor 23 has an inlet port 26 which is connected in fluid pressure-tight connection through a pipe 27 to outlet port 22 of upstream solenoid valve 14 . Bore 25 of sensor 23 also has an outlet port 28 which is connected in a fluid pressure-tight connection to an upstream outlet pipe 29 of apparatus 10 . Optionally, apparatus 10 may include a manually operable upstream outlet shut-off valve 30 which has an inlet port connected in a fluid pressure-tight connection to pipe 29 and an outlet port connected to upstream outlet port 31 . In an example embodiment of apparatus 10 which was designed, built and tested by the present inventors, upstream flow rate sensor 23 was a 600 model manufactured by Imperial Flange and Fitting Company, P.O. Box 352262, Los Angeles, Calif. 90035.
The flow rate sensor 23 is a Pitot tube-type flow meter which has an upstream “high side” Pitot tube probe 32 that protrudes radially inwards through the cylindrical wall 33 of the sensor body 24 into bore 25 of the sensor. The upstream Pitot tube probe 32 has a transversely disposed, upstream pointing face in which is located at least one orifice which has a longitudinally disposed bore for measuring the stagnation pressure of liquid impacting the upstream face of the probe.
Pitot tube flow rate sensor 23 also has a second, downstream Pitot tube probe 24 which protrudes radially inwards through wall 33 of sensor body 24 into bore 25 of the sensor 23 . The downstream Pitot tube 34 has a transversely disposed, downstream pointing face in which is located at least one orifice for measuring the hydrostatic pressure of liquid in bore 25 of sensor body 24 . Since the stagnation pressure at the entrance orifice(s) of upstream Pitot tube 34 is proportional to the kinetic energy of fluid impacting the upstream orifice plate face, and hydrostatic pressure at the entrance orifice(s) of downstream Pitot tube is proportional to static pressure of fluid in the sensor bore, the difference between the two pressure measurements is a measure of the velocity and hence mass flow rate of liquid through bore 25 of sensor 23 .
Sensor 23 includes a transducer module for converting differences in measured pressures between upstream and downstream Pitot tube probes 32 and 34 into an electrical signal which is proportional to the velocity and hence mass flow rate of liquid through sensor 23 . For example, a sensor 23 having a maximum useable flow rate of 100 gallons per minute (GPM) may have an output signal at output terminal 36 of transducer module 35 of five volts, full scale output level for a flow rate of 100 GPM, 4-volts for a flow rate of 80 GPM, 3-volts for a flow rate of 60 GPM, etc. Signal output terminal 36 of transducer module 35 is connected to interrupt input terminal 97 of control module 11 .
As shown in FIG. 1 , transducer module 35 has input power terminals 37 , 38 for receiving DC power provided by control panel 11 A, for powering electronics within the transducer module.
In a preferred embodiment of apparatus 10 , at least the upstream Pitot tube probe 32 has a plurality of spaced apart orifices positioned on the rear, upstream face of the probe. This arrangement provides a measure of stagnation pressure which is averaged over the velocity profile of liquid flowing through bore 25 of sensor 23 , and thus provides a more accurate measurement of the mass flow rate of liquid through the sensor.
Referring still to FIG. 1 , it may be seen that the components 13 through 38 of apparatus 10 comprise what may be identified as an “upstream leg” 40 of the apparatus Upstream leg 40 of apparatus 10 has an inlet port consisting of an inlet pipe 16 which is connected to a source of pressurized water, which in the present example of an application for apparatus 10 , is a Hot Water Source (HWS) riser pipe. As is also shown in FIG. 1 , upstream leg 40 of apparatus 10 has an outlet port consisting of an outlet pipe 31 . Outlet pipe 31 is connected to the inlet port of equipment which is supplied with a flowing liquid from apparatus 10 , such as inlet port 41 of VAV terminal 12 , as shown in FIG. 3 .
Referring again to FIG. 1 , it may be seen that leak detection and shut-off apparatus 10 includes a “downstream leg” 50 which is substantially similar to and may in fact be identical in construction and function to upstream leg 40 . Thus, as will now be described, downstream leg 50 of apparatus 10 has components which are exact counterparts of those in upstream leg 40 , which were previously described in detail above. The foregoing detailed description should be referred to in conjunction with the following abbreviated description of components of the downstream leg 50 .
Referring to FIG. 1 , it may be seen that downstream leg 50 of water leak detection and shut-off apparatus 10 includes a return inlet port 53 for receiving flowing water which has been returned from equipment supplied with hot water from outlet pipe 31 of upstream leg 40 of the apparatus. Downstream return inlet port 53 of apparatus 10 includes a return inlet pipe 56 which is connected to hot water return line of a destination for hot water from outlet pipe 31 of the apparatus, such as outlet pipe 52 of VAV terminal 12 (see FIG. 3 ).
As shown in FIG. 1 , inlet port 53 of apparatus 10 may optionally include a manual inlet shut-off valve 58 which has an inlet port connected to a return inlet pipe 56 , and an outlet pipe 59 which is connected between an outlet port of manual inlet shut-off valve 58 and an inlet port 66 of a second, downstream flow-rate sensor 63 .
In a preferred embodiment of apparatus 10 , downstream flow-rate sensor 63 is identical in construction and function to upstream flow-rate sensor 23 , which was described in detail above. Thus, downstream flow-rate sensor 63 has a tubular body 64 which has disposed longitudinally through its length a cylindrically shaped, circular cross-section bore 65 . Inlet port 65 of downstream flow-rate sensor 63 is connected through pipe 59 to the outlet port of manual shut-off valve 58 .
Referring still to FIG. 1 , it may be seen that downstream flow-rate sensor 63 includes an upstream Pitot tube probe 72 and a downstream Pitot tube probe 74 , both of which protrude radially inwardly through the cylindrical wall 73 of sensor body 64 into bore 65 of the sensor. Pitot tube probes 72 , 74 are coupled to a pressure transducer transmitter module 75 , which has a signal output terminal 76 that outputs a signal voltage proportional to the pressure difference between the probes, and hence the mass flow-rate of liquid through bore 65 of sensor 63 . Pressure sensor transducer transmitter module 75 is provided with a 24-volt power from control module 11 , which is input to line and ground terminals 77 , 78 of the module. Signal output terminal 76 is connected to interrupt terminal 99 of control module 11 .
Referring still to FIG. 1 , it may be seen that downstream flow-rate sensor 63 has an outlet port 68 which is connected by an outlet pipe 69 to the inlet port 55 of a normally closed downstream solenoid valve 54 . Downstream solenoid valve 54 may be identical in construction and function to upstream solenoid valve 14 . Thus, as shown in FIG. 1 , downstream solenoid valve 54 has electrical power input terminals 60 , 61 , which must be continuously provided with 24-volt AC power from control module 11 for valve 54 to remain open. Solenoid valve also has an outlet port 62 which is connected to a Hot Water Return (HWR) riser pipe 81 . As shown in FIG. 1 , apparatus 10 optionally includes a manually operable downstream outlet shut-off valve 70 connected between outlet port 62 of solenoid valve 54 , and HWR riser pipe 81 .
Referring now to FIG. 2 , it may be seen that apparatus 10 includes a control panel 11 A on which is mounted control module 11 , along with other components which together comprise a Direct Digital Controller (DDC), of a type which is commonly used in HVAC systems to control parameters such as air temperature and air flow-rate in response to sensed parameters such as ambient temperature and humidity.
As shown in FIG. 2 , the DDC controller module 11 is of conventional design and includes a microprocessor (not shown) and power supply. As shown in FIG. 2 , DDC controller module 11 has a pair of bidirectional data signal terminals 91 , 92 connected to network port terminals 93 , 94 of a first, up-net network port 93 A of DDC control panel 11 A, and network port terminals 95 , 96 , of a second down-net port 95 A of DDC control panel 11 A. The network port terminals 93 , 94 and 95 , 96 of DDC control panel are used to enable interconnection of DDC control module 11 with previous and next DDC controller modules (not shown) which are part of a distributed network such as a Local Area Network (LAN).
Referring still to FIG. 2 , it may be seen that DDC control module 11 has a first interrupt port consisting of a high-side interrupt terminal 97 , and a low side or ground interrupt terminal 98 . High-side input terminal 97 is connected to an input terminal 128 of DDC Control Panel 11 A, which, as shown in FIG. 1 , is connected to signal output terminal 36 of pressure transducer transmitter module 35 of upstream flow-rate sensor 23 . Microprocessor circuitry within control module 11 converts an analog signal voltage present at the output signal terminal 36 of pressure transducer transmitter module 35 , and hence at interrupt input terminal 97 of the DDC Control Module 11 to a digital value, and stores that digital value in a first memory location of the microprocessor for subsequent processing.
As shown in FIGS. 1 and 2 , Control Module 11 also has a second interrupt input port consisting of a high-side interrupt terminal 99 , and a low-side or ground interrupt terminal 100 . High-side interrupt input terminal 99 is connected to an input terminal 127 of Control Panel 11 A, which is in turn connected to signal output terminal 76 of pressure transducer transmitter module 75 of downstream flow-rate sensor 63 . Microprocessor circuitry within control module 11 converts an analog signal voltage present at the output signal terminal 76 of pressure transducer transmitter 75 , and hence at interrupt input terminal 99 of DDC control module 11 to a digital value, and stores that digital value in a second memory location of the microprocessor for subsequent processing.
Microprocessor circuitry within control module 11 also has stored within a third memory location of the microprocessor a digital number representing a maximum allowable difference between upstream and downstream flow-rates measured by upstream and downstream flow-rate sensors 23 , 63 , respectively. A typical threshold flow-rate difference value might, for example, be in the range of 0.1 to 1.0 gallons per minute (GPM). A selected threshold flow-rate difference value is entered into control module 11 by conventional means, such as via network ports 93 A or 95 A.
Microprocessor circuitry within control module 11 cyclically and continuously samples the values of upstream flow-rate and downstream flow-rates stored in the upstream and downstream flow-rate memory locations, and inputs those values into minuend and subtrahend ports of a digital subtractor application. The difference output value of the digital subtractor is input to the second variable input of digital comparator; application of the microprocessor. That application has a first, set point value input into which is input the threshold flow-rate. If the flow-rate difference input to the variable input port of the comparator equals or exceeds the threshold flow-rate, the comparator outputs a digital TRUE alarm status signal.
DDC Control Module 11 also contains an electromechanical or solid state relay (not shown) which receives a continuous energization signal from the microprocessor in the control module as long as the alarm status signal is not TRUE. The relay conducts 24-volt AC power input to terminal control module 11 on terminal 103 to output terminal 104 of the control module. Output terminal 104 of control module 11 is connected to switched 24-AC high-side terminals 124 , 126 of control panel 11 A which are in turn connected to high-side terminals 61 , 21 of solenoid valves 54 , 14 respectively. Low-side 24-AC terminals 123 , 125 of control panel 11 A are connected to low-side terminals 60 , 20 of solenoid valves 54 , 14 . The switched 24-volt AC power supplied to solenoid valves 54 , 14 maintains the valves in a fully open position. However, if the microprocessor in the control module 11 outputs a logic TRUE alarm status signal in response to measured flow-rate difference between upstream flow-rate sensor 23 and downstream flow-rate sensor 63 which exceeds the preprogrammed threshold value, 24-volt AC power supplied to the solenoid valves is immediately interrupted, thus causing the values to close and thus shut off flow of water from apparatus 10 .
Referring to FIG. 2 , it may be seen that control panel 11 A includes a step-down transformer 130 which receives 115-volt AC power input to terminals 119 , 120 , of the control panel, and a circuit breaker 131 in series with input terminal 119 and the transformer. Transformer 130 supplies 24-volt AC power to terminals 101 , 102 of DDC control module 11 , as explained above, and to input terminals 134 , 135 of a 24-volt DC power supply 132 . Power supply 132 has plus and minus 24-volt DC output terminals 136 , 137 which are connected to output terminals 121 , 122 , respectively, of DDC control panel 11 A. As shown in FIG. 1 , 24-volt DC power output on terminals 121 , 122 of control panel 11 A is input to transducer transmitter modules 35 , 75 of flow-rate sensors 23 , 63 , respectively, on input terminal pairs 37 , 38 and 77 , 78 , respectively.
FIG. 3 illustrates a typical terminal 12 apparatus of the type which water leak detection and shutoff apparatus 10 is intended to be used with. As shown in FIG. 3 , a Variable Air Volume (VAV) terminal 12 includes an elongated box-like heat exchanger duct 141 which has an inlet opening 142 that receives cold air from a cold air inlet duct 143 . Heat exchanger duct 141 also has an air outlet opening 144 which is connected to a number of ceiling-mounted air flow diffusers 145 .
As shown in FIG. 3 , VAV terminal 12 includes an inlet air property sensor module 146 which contains a sensor for measuring properties of cold air inlet through duct 143 , such as temperature, humidity and flow-rate, and inputs the values of the properties to a VAV controller 147 , which may be part of DDC control panel 11 A, or a separate controller.
As shown in FIG. 3 , VAV terminal 12 includes a local or zone thermostat 148 by which a set point for a desired temperature range of a zone or zones services by terminal 12 may be manually or remotely input.
VAV terminal 12 also includes a damper valve 149 which has a damper plate 150 which is rotatable by a motor 151 to control the flow-rate of air input into entrance 142 of duct 141 from cold air inlet duct 143 .
As shown in FIG. 3 , VAV terminal 12 includes a heater coil 152 . Heater coil 152 is a flowing air to water heat exchanger which includes an elongated coil of tubing which has high thermal conductivity, such as copper tubing, an inlet filling 153 for receiving in fluid pressure-tight connection a source of hot, flowing water, such as a pipe 154 connected to inlet port 41 of VAV terminal 12 , and an outlet port 155 connected to a discharge or outlet pipe 156 .
The heater coil 152 which typically has the shape of a spiral or helix which has a longitudinal axis coincident with the longitudinal axis of heat exchanger duct 152 , provides an efficient means of transferring heat from the heated water input to inlet port 153 of the coil, to cold air flowing longitudinally through the heat exchanger duct and exiting through outlet opening 144 of the duct to ceiling diffusers 145 .
As shown in FIG. 13 , the temperature of air exiting heat exchanger duct 141 and conducted to ceiling diffusers 145 is controlled not only by controlling the air flow-rate via damper valve 149 , but also by controlling the rate of hot water flow through heater coil 152 . Thus, as shown in FIG. 3 , VAV terminal 12 includes a Normally Closed (NC) proportional control valve 157 which has an inlet port connected to heat exchange coil outlet. discharge pipe 156 , and an outlet port connected to VAV outlet pipe 52 . Valve 157 has an actuator control terminal 158 which is connected to controller 147 and enables the flow-rate of hot water through valve 157 and water coil 152 to be varied over a continuous range from zero to maximum flow-rate.
|
A method and apparatus for detecting leakage of flowing liquids from pipes includes an upstream flow-rate sensor positioned between a source of a flowing liquid which is conducted from a source to a destination terminal such as a VAV heat exchanger, and a downstream flow-rate sensor positioned between an outlet port of the destination terminal and a return line for the flowing liquid. The apparatus includes electronic control circuitry which is responsive to a differential flow-rate between upstream and downstream measured flow rates which exceeds a predetermined limit value in removing a valve-opening signal to the upstream shut-off valve, thus closing the valve to interrupt flow of liquid through the valve if the differential flow-rate signifies a leak. Optionally, the apparatus also includes a downstream shut-off valve positioned between the destination terminal and a return line, which is also closed in response to a differential flow-rate exceeding the limit value.
| 8
|
FIELD OF THE INVENTION
The field of the invention is installing and cementing well liners and providing a circulation system for formation treatment, conditioning, or gravel packing.
BACKGROUND OF THE INVENTION
Oil and gas operators often drill wells in formations that require treatment of the producing formation or gravel packing to ensure optimum production. In past installations, such treatment or gravel packing was not attempted until after a well liner was positioned and cemented in place. The liner and its cement seal served to isolate the producing formation, or pay zone, from other zones above the pay zone so that there was no cross-contamination or fluid and material loss during treatment or gravel packing.
Presently, the liner cementing and formation treatment or gravel packing are accomplished as separate steps, requiring multiple equipment runs into the well bore. First, the well bore is drilled to the point where the liner will be seated. The liner is lowered into position and cemented into place. After the cement has set, a second, smaller diameter drill string is used to drill beyond the cemented liner into the pay zone. The drill string is removed and a circulation system is lowered into the pay zone for treatment or gravel packing of the pay zone. This system is expensive and time-consuming because it requires multiple trips in and out of the hole and multiple drilling runs.
In some cases, a single hole can be drilled into the pay zone, and the liner and production strings lowered in a single trip. However, these situations only occur when there is no need to treat the formation or gravel pack the production string, and the production string can utilize large-opening slotted or perforated production casing. The liner can be cemented into position and the well brought on line without multiple trips in and out of the hole because there is little or no danger of formation contamination or debris plugging the production casing. When formation treatment or gravel packing is required, large-opening production casing cannot be used and this simpler, one-pass approach is unavailable due to the danger of formation damage or plugging the small openings in the production screens.
It is an object of this invention to allow a single drilling operation to complete the well bore into the pay zone when formation treatment or gravel packing is required.
It is a further object of this invention to allow simultaneous insertion of cementing apparatus and formation treatment or gravel packing apparatus into the well bore.
It is a further object of this invention to allow cementing operations without danger of contaminating or clogging either the formation or production equipment installed below the cementing apparatus.
SUMMARY OF THE INVENTION
An apparatus and method is provided that allows an operator to drill a well into a formation requiring treatment or gravel packing in a single pass, then to lower, position, and set the drill-in liner and production strings simultaneously. The invention allows cementing of the drill-in liner prior to any treatment or gravel packing, and provides an integral circulation system to allow formation treatment or gravel packing of the production string. Once treatment or gravel packing is completed, the invention provides mechanical fluid loss control as the circulation system is pulled out of the hole.
The invention comprises a liner assembly, a cementing assembly, and a circulation and production assembly. After the well bore has been drilled into the pay zone, the three assemblies are assembled at the surface and lowered into the well bore. The circulation and production assembly includes the shoe and production screens, with a wash pipe inserted into the interior of this string to provide circulation control during formation treatment or gravel packing.
The cementing assembly includes a cementing valve and means of isolating the annulus of the cementing assembly from the annulus of the circulation and production assembly. During cementing operations, the isolation means is used to prevent cement flow down into the pay zone. The bottom of the liner assembly connects to the top of the cementing assembly, so that cement pumped through the cementing assembly is forced upward to encase and seal the liner in position. "Cement" as used herein includes using cement or other means of achieving a seal between liner and the well bore.
Once the cementing operation is completed, the cementing wash pipe is withdrawn and a new wash pipe is lowered into position to connect to the circulation and production assembly wash pipe. Formation treatment or gravel packing is carried out to prepare the well to be brought on line. When the treatment or gravel packing is completed, the entire wash string is withdrawn. Mechanical means, such as a knock out isolation valve, provides mechanical fluid loss control to prevent fluid backwash in the production assembly.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A-E is a partially cut away drawing of the outer equipment string for one embodiment of the one trip cement and gravel pack system.
FIGS. 2A-F is a partially cut away drawing of the inner equipment string for one embodiment of the one trip cement and gravel pack system.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1A-E, one embodiment of the outer equipment string 10 of the one pass cement and gravel pack system is shown. The outer equipment string 10 comprises an outer liner assembly 12, an outer cementing assembly 14, and an outer circulation assembly 16.
The outer liner assembly 12 comprises a liner packer 18, such as Baker Product No. 296-14, a liner hanger 20, such as Baker Product No. 292-50, and a liner 22. The liner packer 18, the liner hanger 20, and the liner 22 are normally used in lining and cementing operations, and those skilled in the art will recognize that the particular specifications for these will vary depending on the conditions of the installation.
The outer cementing assembly 14 is in fluid communication with the outer liner assembly 12 and comprises a first seal bore extension 28, such as Baker Product No. 449-40, a cementing valve 30, such as Baker Product No. 810-80, a second seal bore extension 32, such as Baker Product No. 449-40, an external casing packer 34, such as Baker Product No. 301-13, and a third seal bore extension 36, such as Baker Product No. 449-40. Slip-on fluted centralizers 38 may be used to position the outer cementing assembly 14 and to protect the external casing packer 34 from premature setting during insertion into the well bore 40.
The outer circulating and production assembly 16 is in fluid communication with the outer cementing assembly 14 and comprises casing joints 42, a seal bore 44, a perforated extension 46, a lower seal bore 48, a knock-out isolation valve 50, pre-pack screens 52, flapper valves 54, a first O-ring seal subassembly 56, a slotted liner 58, a second O-ring seal subassembly 60, and a set shoe 62, such as a double "V" set shoe.
Referring to FIGS. 2A-F, one embodiment of the inner equipment string 110 of the one pass cement and gravel pack system is shown. The inner equipment string comprises an inner liner assembly 112, an inner cementing assembly 114, and an inner circulation assembly 116.
The inner liner assembly 112 comprises a lift nipple 118, such as Baker Product No. 265-20, a packer setting dog subassembly 120, such as Baker Product No. 270-09, a liner setting tool 122 such as Baker Product No. 265-88, a first wash pipe 124, and a ported landing subassembly 126, such as Baker Product No. 276-04. Seals 128 and 130 isolate a port 132 on the ported landing subassembly 126.
The inner cementing assembly 114 is in fluid communication with the inner liner assembly 112 and comprises a second wash pipe 136, a first seal assembly 138, a slurry placement indicator 140, such as a Baker Model "E," Baker Product No. 445-56, a circulating valve 142, such as a Baker Model "S2P," Baker Product No. 445-66, a closing tool 144, such as a Baker Model "HB," a second seal assembly 146, an indicating collet assembly 148, such as Baker Model "A," Baker Product No. 445-34, and an opening tool 150, such as Baker Model "HB."
The inner circulation assembly 116 is installed coaxially with the outer circulation and production assembly 16. The inner circulation assembly 116 comprises a crossover tool 152, such as Baker Product No. 445-72, a low bottom hole pressure flapper valve 154, an anchor seal assembly 156, and a third wash pipe 160.
Referring to FIGS. 1A-E and 2A-F, the well bore 40 is initially drilled to the depth at which the liner 22 is to be begun. The outer casing 64 is lowered into the well bore 40 and cemented into position. The well bore is then completed, drilling to the final position desired in the pay zone. The one trip cementing and gravel pack system is initially assembled at the surface with the inner equipment string 110 coaxial with and inside the outer equipment string 10 and lowered into position so that the set shoe 62 is in the pay zone at the bottom of the well bore 40. A ball 164 is dropped into the well bore 40 so that it will be caught by the ported landing subassembly 126. Once caught, the ball 164 blocks the fluid flow, allowing internal pressure to be built up from the surface. Seals 128 and 130 prevent the fluid from flowing in the annulus between the inner equipment string 110 and the outer equipment string 10. The increased fluid pressure is forced against the liner hanger 20 to set it. After the liner hanger 20 is set, the port 132 in the ported landing subassembly 126 is closed and the ball 164 is released. If the ported landing subassembly 126 is a type such as Baker Product No. 276-04, these actions are accomplished by further increasing the pressure in the inner equipment string 110, forcing the port 132 to close and breaking a shear pin to release the ball 164. The ball 164 is pumped to the circulating valve 142.
The circulating valve 142 must trap the ball and seal off fluid flow from the region below the circulating valve 142. If the circulating valve 142 is a valve such as a Baker "S2P," the ball 164 is caught on a teflon seat. The teflon seat flexes to form a tight seal between the teflon seat and the ball 164, preventing fluid flow into the region below the teflon seat. Several smaller balls are embedded in the teflon seat and act to hold the ball 164 in position. Once the ball 164 is in position against the teflon seat, fluid flow from above the ball is diverted through a circulating valve port 143.
The first seal assembly 138 is initially positioned inside of the third seal bore extension 36. When the ball 164 lands on the teflon seat, the fluid overpressure is prevented from releasing upwards in the inner equipment string 110 by the first seal assembly 138, and is instead forced downward into the inner circulation assembly 116. This positioning protects the external casing packer 34 from damage due to the fluid overpressure.
After the ball 164 is captured, the inner equipment string 110 is raised to position the first seal assembly 138 inside of the second seal bore extension 32, and the second seal assembly 146 inside the third seal bore extension 36. As the inner equipment string 110 is raised, the indicating collet assembly 148 locates onto the third seal bore extension 36, providing a weight indication on the inner equipment string 110 to indicate position. In this position, the circulating valve port 143 is aligned with the external casing packer 34. The external casing packer 34 is pressure set in accordance with the procedure for the specific model used.
When the external casing packer 34 is set, the internal equipment string 110 is again raised, positioning the first seal assembly 138 in the first seal bore extension 28, and the second seal assembly 146 in the second seal bore extension 32. As the inner equipment string 110 is raised, the indicating collet assembly 148 locates onto the second seal bore extension 32, providing a weight indication on the inner equipment string 110 to indicate position. In this position, the circulating valve port 143 is aligned with the cementing valve 30. Cement is pumped through the cementing valve 30 to fill the annulus between the liner 22 and the well bore 40. If the inner equipment string 110 is raised too far, the cementing valve 30 may be accidentally closed. If the cementing valve 30 is accidentally closed, the inner equipment string 110 may be raised further to use the opening tool 150 to reopen the cementing valve 30.
The slurry placement indicator 140, such as Baker Model "E," comprises a seat and a bypass. When the last of the cement is pumped into the well bore 40 at the surface, a wiper plug 166, such as Baker Product No. 445-56 is pumped on top of the cement and followed with completion fluid to force the cement through the circulating valve port 143. When it reaches the slurry placement indicator 140, the wiper plug 166 seats in the seat of the slurry placement indicator 140, causing a temporary rise in pressure at the surface to notify the surface crew of the location of the wiper plug 166. The increase in pressure forces the bypass in the slurry placement indicator 140 to open, relieving the pressure increase and allowing completion of the cementing operation.
When the cementing operation is completed, the inner equipment string 110 is again raised to use the closing tool 144 to close the cementing valve 30. After pressure testing to insure proper closure of the cementing valve 30, the inner equipment string 110 is lowered until the packer setting dog subassembly 120 engages the liner packer 18. Weight is applied to the inner equipment string 110 to set the liner packer 18.
After the completion of the cementing operation and setting the liner packer 18, the inner liner assembly 112 and the inner cementing assembly 114 of the inner equipment string 110 are raised sufficiently to allow reverse circulation to clean out any excess cement. The inner liner assembly 112 and the inner cementing assembly 114 are then pulled out of the well bore 40. The removed inner liner assembly 112 and the inner cementing assembly 114 may be replaced with a wash pipe which can be connected to the inner circulation assembly 116 for formation treatment or gravel packing operations.
To treat the formation or gravel pack in preparation for production, a wash pipe is run back into the well and engaged onto the inner circulation assembly 116 using conventional fishing equipment. A second ball 168 is dropped into the well bore 40 and is caught by the crossover tool 152. Once caught, the second ball 168 blocks fluid flow in the interior of the inner circulation assembly 116, causing an increase in liquid pressure. The increased pressure exposes the gravel pack port 170.
If the crossover tool 152 is a valve such as Baker "S2P," the second ball 168 is caught on a teflon seat. The teflon seat flexes to form a tight seal between the teflon seat and the second ball 168, preventing fluid flow into the region below the teflon seat. Several smaller balls are embedded in the teflon seat and act to hold the second ball 168 in position. Once the second ball 168 is in position against the teflon seat, fluid flow from above the ball is diverted through the gravel pack port 170.
The crossover tool 152 is initially positioned between the seal bore 44 and the lower seal bore 48, so that fluid flowing out of the crossover tool 152 flows out of the perforated extension 46 and downward into the pay zone, across the knockout isolation valve 50, pre-pack screens 52, flapper valves 54, first O-ring seal subassembly 56 and into the slotted liner 58. The fluid returns up the third wash pipe 160, through the by-pass in the crossover tool 152, and returns to the surface. This circulating position allows fluids to be pumped across the pay zone to treat or gravel pack as required.
Once sufficient circulation is achieved, the inner circulation assembly 116 is raised, pulling the anchor seal assembly 156 into the seal bore 44 and the lower seal bore 48, thereby isolating the perforated extension 46. In this position, the gravel pack port 170 is above the seal bore 44, allowing excess fluids to be reversed or circulated out of the well bore 40.
After the completion of treatment or gravel packing, inner circulation assembly 116 is separated from the anchor seal assembly 156. The inner circulation assembly 116, without the anchor seal assembly 156, is withdrawn from the well bore 40, leaving the anchor seal assembly 156 in position so that it permanently isolates the perforated extension 46.
As the inner circulation assembly 116 is removed, the knock-out isolation valve drops 50 into position to prevent the fluid in the inner circulation assembly 116 from flooding into the outer circulation and production assembly 16.
|
An apparatus and method is provided that allows an operator to drill a well into a formation requiring treatment or gravel packing in a single pass, then to lower and position the liner and production strings simultaneously. The invention allows cementing of the liner prior to any treatment or gravel packing, and provides an integral circulation system to allow formation treatment or gravel packing of the production string. Once treatment or gravel packing is completed, the invention provides mechanical fluid loss control as the circulation system is pulled out of the hole.
| 4
|
BACKGROUND OF THE INVENTION
[0001] This invention relates to shaft journal bearings and, more particularly, to an improved bearing assembly seal arrangement for use in a railway freight car.
[0002] Roller bearing assemblies incorporating two rows of tapered roller bearings preassembled into a self-contained, pre-lubricated package for assembly onto journals at the ends of axles or shafts are known. Such bearing assemblies are used as rail car bearings assembled onto journals at the ends of the axles. Bearings of this type typically employ two rows of tapered roller bearings fitted one into each end of a common bearing cup with their respective bearing cones having an inner diameter dimensioned to provide an interference fit with the shaft journal and with a cylindrical sleeve or spacer positioned between the cones providing accurate spacing and proper lateral clearance on the journal. Seals mounted within each end of the bearing cup provide sealing contact with wear rings bearing against the outer ends or back face of the respective bearing cones at each end of the assembly. Such seals are shown in U.S. Pat. Nos. 5,975,533, 7,607,836, and 7,534,047.
[0003] In a typical rail car installation, the axle journal is machined with a fillet at the inboard end. A backing ring having a surface complementary to the contour of the fillet and an abutment surface for engaging the inboard end of an inner wear ring accurately position the bearing assembly on the journal. An end cap mounted on the end of the axle by bolts threaded into bores in the end of the axle engages the outboard wear ring and clamps the entire assembly on the end of the axle. The wear rings typically have an inner diameter dimensioned to provide interference fit with the journal over at least a portion of their length so that the entire assembly is pressed as a unit onto the end of the journal shaft portion of the axle.
SUMMARY OF THE INVENTION
[0004] The bearing assembly of the present invention is a roller bearing that includes an inner race or cone fitted around the journal portion of the axle or shaft. The inner race includes an outwardly directed raceway. An outer race or cup has an inwardly directed raceway. Roller elements are located between and contacting the inner and outer raceways.
[0005] A backing ring has a contoured surface complementary to and engaging the contoured surface of a fillet formed on the shaft. The fillet leads from the journal to the shoulder of the shaft. The contoured surfaces cooperate to fix the backing ring against axial movement along the shaft.
[0006] The bearing assembly includes a seal assembly that provides a barrier for lubricant to be retained within the seal assembly and for contaminants to be kept out. A slinger is provided to interact with a wear ring and a seal element to provide an improved seal. The inter-related relationship between the seal element, wear ring, and slinger act to retain the lubricant within the seal assembly and to keep contaminants out.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] In the drawings,
[0008] FIG. 1 is a sectional view of a shaft journal having mounted thereon a tapered roller bearing assembly in accordance with a first embodiment of the present invention;
[0009] FIG. 2 is a detailed partial view in cross section of a tapered roller bearing seal assembly in accordance with the first embodiment of the present invention;
[0010] FIG. 3 is a detailed view in partial cross section of a tapered roller bearing assembly in accordance with a second embodiment of a present invention, and
[0011] FIG. 4 is a detailed view in partial cross section of a tapered roller bearing assembly in accordance with a third embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0012] Referring now to FIG. 1 of the drawings, a bearing assembly indicated generally by the reference numeral 10 on FIG. 1 is shown mounted on a journal 12 on the free, cantilevered end of a shaft or axle 14 , typically a rail car axle. Journal 12 is machined to very close tolerances and terminates at its inner end in a contoured fillet 22 leading to a cylindrical shoulder 18 of axle 14 . At the free end of the axle, journal portion 12 terminates in a slightly conical or tapered guide portion 24 dimensioned to facilitate installation of the bearing assembly onto the journal. A plurality of threaded bores 26 are formed in the end of axle 14 for receiving threaded cap screws, or bolts 28 for mounting a bearing retaining cap 30 on the end of the shaft to clamp the bearing in position as described more fully herein below.
[0013] Bearing assembly 10 is preassembled before being mounted and clamped on journal 12 by retaining cap 30 and bolts 28 . The bearing assembly includes a unitary bearing cup or outer raceway 32 having a pair of inner facing raceways 34 , 36 formed one adjacent each end thereof which cooperate with a pair of bearing cones 38 , 40 , having outer facing raceways respectively, to support the two rows of tapered rollers 42 , 44 , respectively there between. A center spacer 46 is positioned between cones 38 , 40 to maintain the cones in accurately spaced position relative to one another allowing for proper bearing lateral clearance.
[0014] Bearing cup 32 is provided with cylindrical counterbores 17 , 19 at its axially outer ends and a pair first end sections 48 , 50 of seal sections 52 , 54 are pressed one into each of the cylindrical counterbores 17 , 19 in cup 32 . Each second end section 55 , 63 of seal section 52 , 54 may include resilient sealing elements 56 , 58 which rub upon and form a seal with radial outer surfaces 37 , 61 of a pair of seal wear rings 60 , 62 having an inwardly directed end in engagement with the outwardly directed ends of bearing cones 38 , 40 respectively. Seal section 54 is similar to seal section 52 and will not be described in detail. The other end of wear ring 60 is received in a cylindrical counterbore 64 in the axially outwardly directed end of an annular backing ring 66 which, in turn, has a counterbore 68 at its other end which is dimensioned to be received in interference and non-interference relation on the cylindrical shoulder 18 of shaft 14 . The counterbore 64 and the outer diameter of wear ring 60 are also dimensioned to provide an interference fit so that wear ring 60 is pressed into the backing ring 66 which is accurately machined to provide a contoured inner surface 70 complementary to and engaging the contour of fillet 22 when the bearing is mounted on the shaft. The outwardly directed end of wear ring 62 bears against a counterbore 31 in a retaining cap 30 .
[0015] Referring now to FIG. 2 , a detailed view of seal assembly portion of bearing assembly 10 is provided. Seal section 52 is seen to comprise a generally cylindrical piece, having a larger diameter first end section 48 pressed or fit into a complementary counterbore 17 in a cup 32 . Seal section 52 includes an intermediate section 27 normal to first end section 48 and a main intermediate cylindrical section 53 that extends parallel to end section 48 , wherein main intermediate cylindrical section 53 has a smaller diameter than first end section 48 .
[0016] Second end section 55 of seal section 52 extends from main intermediate section 53 at a normal angle thereto. Resilient sealing element 56 is fitted onto second end section 55 . Resilient sealing element 56 is comprised of a rubber or elastomer compound, such as nitrile rubber compound. Resilient sealing element 56 includes a main section that includes an opening to receive second end section 55 of seal section 52 .
[0017] Slinger section 72 comprises a generally cylindrical structure having a base section 74 attached to outer surface 37 of seal wear ring 60 and end section 76 extending from base section 74 . Slinger section 72 is usually a unitary structure comprised of a structural plastic or steel.
[0018] Referring now to FIG. 3 , a second embodiment of the roller bearing seal assembly of the present invention is shown generally at 110 . Elements such as bearing cup 32 , backing ring 66 , seal section 52 and seal wear ring 60 are similar to FIGS. 1 and 2 and are similarly numbered.
[0019] Slinger section 172 comprises a generally cylindrical structure having a base section 174 attached to outer surface 37 of seal wear ring 60 , an intermediate section 178 extending from base section 174 , and end section 176 extending from and at an angle of approximately 90 degrees to intermediate section 178 . Intermediate section 178 is seen to have a protrusion 178 A that contacts the axially inward facing surface 55 A of second end section 55 of seal section 52 . Slinger section 172 is usually a unitary structure comprised of a structural plastic or steel. Slinger end section 176 extends toward and is adjacent the radial outer surface of main intermediate cylindrical section 53 of seal section 52 .
[0020] Referring now to FIG. 4 , a third embodiment of the roller bearing seal assembly of the present invention is shown generally at 210 . Elements such as seal section 52 and seal wear ring 60 with radial outer surface 37 are similar to FIGS. 1 and 2 and are similarly numbered. However, backing ring 266 is seen to have an annular protrusion 268 extending axially from its outer radial surface.
[0021] Slinger section 272 comprises a generally cylindrical structure having a base section 274 attached to outer surface 37 of seal wear ring 60 , an intermediate section 278 extending from base section 274 , and end section 276 extending from and normal to intermediate section 278 . Slinger section 272 is usually a unitary structure comprised of a structural plastic or steel. Intermediate section 278 is seen to have a protrusion 278 A that contacts the axially inward facing surface 55 A of second end section 55 of seal section 52 . Slinger end section 276 extends at a radius and an angle of approximately 90 degrees from intermediate section 278 and extends toward and is adjacent the radial outer surface of main intermediate cylindrical section 53 seal section 52 .
|
A bearing assembly is provided having a roller bearing with an inner raceway fitted around the journal portion of an axle. An outer raceway combines with the inner raceway to receive roller elements. An improved lubricant seal arrangement is provided between the wear ring and the supporting outer raceway comprising a slinger element.
| 5
|
FIELD OF THE INVENTION
The present invention relates generally to toilets and more specifically to a dual flow toilet bowl water flow adjustment system for controlling the volume of water in the holding tank used to flush a water-flush toilet.
BACKGROUND OF THE INVENTION
Water shortage is becoming a concern in many parts of the world including United States which uses the greatest amount of residential water in the world. In growing times of water shortages, the problem of having sufficient water supplies will most likely continue to get worse. A toilet uses the largest amount of water in the United States, representing more than ⅓ of the total household water used. According to Environmental Protection Agency (EPA), billions of gallons of water can be saved annually if toilet water usage in the United States can be reduced by ⅓. In fact, more than 640 billion gallons of water can be saved annually if the older model toilets in the United States can be replaced with the newer water efficient toilets.
Low flow toilets use 1.6 gallons per flush (gpf), which is compared to a conventional toilet which uses 3.5 to 7 gpf. Low flow toilets are simply designed to help reduce toilet water usage. Unfortunately, research shows that many of these low flow toilets actually waste more water than they are designed for. The key issue is that they do not release adequate amount of water to clear the waste. Consumers often have to flush two or three times more to clear the wastes.
To increase performance some of the newer low flow toilets use air pressure to help clear wastes. These “High Efficiency Toilets” (HET) clear wastes effectively, but the air pressure has a tendency to splash waste water causing droplets to become airborne. Another issue related to the HET toilets is a significant increase in noise during flushing. In addition, these toilets treat liquid waste the same as the solid waste. These problems tend to make these more expensive devices not practical for the average household.
Dual flush toilets have gained in popularity in recent years. These toilets treat liquid and solid wastes differently as they should. They provide two types of flushes, short flush (less water) for liquid waste and standard flushes for solid waste. While dual flush toilets are more effective than the low flow toilet in saving water, they tend to be more expensive requiring several years of payback period for consumers. Dual flush toilets are also designed with different mechanisms from the conventional toilets, therefore they are also more expensive for manufacturers to make due to replacement of the existing manufacturing equipment, purchase, and installation of new equipment. Prematurely replacing existing conventional toilets with dual flush toilets also creates environmental issues due to early disposal of the existing toilets to the landfill.
Dual flush toilet retrofit kits which convert existing conventional toilets into dual flush toilets can be a good alternative because they tend to be significantly cheaper than buying a new dual flush toilet and they do not require replacing the existing toilet. However, almost all retrofit kits currently on the market require replacing certain parts of the existing toilet and often need a professional plumber to complete the installation, which adds significant cost to consumers.
In these respects, one or more embodiments of the present invention substantially depart from the conventional concepts and designs of the prior art, and in so doing provide an apparatus/system primarily developed for the purpose of controlling the water volume utilized to flush an existing toilet or new toilet. The apparatus/system accomplishes the task efficiently and cost effectively, and accomplishes the task without replacing any existing parts, and is a portable device.
SUMMARY OF THE INVENTION
One or more of the embodiments in the present invention is directed to a toilet water flow adjustment system for usage within a toilet. The toilet can be a typical set-up having a handle arm connected to a flush connector, which when the handle arm is depressed a main flapper valve opens to flush the toilet. The system as described in one or more of the embodiments would include a divider positionable within a holding tank in a substantially vertical orientation. The divider has a height lower than a full water level in the holding tank and the divider separates the holding tank into a main portion and a reserve portion. The main portion would preferably contain the main flapper valve. The divider is defined as including a gate panel positioned against at least one side panel. The side panel includes an aperture. The gate panel is vertically movable with respect to the at least one side panel for providing selective fluid connection between the main portion and the reserve portion when the gate panel is moved and maintained towards an upward position. A first linkage is provided to connect the gate panel to the flush connector such that when the handle arm is depressed, the gate panel moves towards an upward position.
The system also includes a lever preferably having a weighted object freely moveably secured thereto. The lever has one end connected to the gate panel and has another end connected to a float. The lever is further pivotally connected to a region intermediate to the two ends to the side panel, such that when the gate panel moves towards an upward position the float moves towards a downward position. The float is also positioned within the reserve portion or above the divider, or within the main portion, and maintains a floating position on the full water level above the height of the divider.
Therefore, when the handle arm is initially depressed the gate panel being initially urged towards an upward position returns to a downward position sealing the aperture in the divider because the float maintains the floating position on top of the full water level and because the weighted object substantially remains at the end connected to the gate panel. The initial pressing of the handle arm will use the water in the main portion to flush the toilet reserving water in the reserve portion. Additionally, when the handle arm is depressed a second time in the same manner as the initial depression the gate panel is moved towards an upward position dropping the float to a position about the height of the divider which causes the weighted object to move towards the end of the lever connected to the float, thereby maintaining the gate panel in an upward position and opening the aperture in the side panel such that the water in the reserve portion and the main portion is utilized to flush the toilet.
In various objects of the embodiment the vertical orientated divider may include at least two side panels separately positioned on either side of the gate panel (the gate panel can be the divider which does not need side panels but requires “guard rails” on the toilet walls, when the gate panel is lifted upwards, the main and reserve portions are connected). Each side panel would have an aperture defined to provide fluid connection between the main portion and the reserve portion when the gate panel is maintained in an upward position. Additionally, the two side panels may each include flanged edges extending towards each other, such that when the flanged edges of the two side panels are secured together, the two side panels create a cavity and wherein the cavity is sized to receive the gate panel. It is further provided that each panel has a pair of ends positioned to engage a side wall of the holding tank such that when engaged the side panel fluidly separates the holding tank into the main portion and the reserve portion, and the pair of ends may further include a gasket secured there along to facilitate the fluid separation.
In addition, each side panel may further include an anchor system to secure the divider in the holding tank.
Various other aspects of the embodiments may provide for the gate panel having a first member protruding upwardly from a top edge of the gate panel and the first member being secured to the first linkage; and the first member including a plurality of openings to adjustably secure the first linkage thereto. Yet other aspects include connecting the end of the lever distal to the end connected to the float to a second linkage which connects to the gate panel.
Numerous advantages and features of the invention will become readily apparent from the following detailed description of the invention and the embodiments thereof, and from the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
A fuller understanding of the foregoing may be had by reference to the accompanying drawings, wherein:
FIG. 1A is a perspective view of a first system embodiment made in accordance with one or more principals of the present invention;
FIG. 1B is an enlarged perspective view of a top portion of a divider module in accordance with the FIG. 1A embodiment;
FIG. 1C is an enlarged perspective view of FIG. 1B illustrating a gate panel moved towards an upward position;
FIG. 1D is a top view of the FIG. 1A embodiment;
FIG. 2A is a perspective view of a side panel in accordance with the FIG. 1A embodiment;
FIG. 2B is a perspective view of the relationship of connecting the gate panel with two side panels;
FIG. 3A is a perspective view of a holding tank with the first system embodiment showing a full water level;
FIG. 3B is a perspective view of a holding tank with the first system embodiment showing an initial flush using the water from the main portion and maintaining the water level in the reserve portion;
FIG. 3C is a perspective view of a holding tank with the first system embodiment showing a double flush using the water from both portions since the gate panel in maintained in an upward position;
FIG. 4A is a side view of the system illustrated in FIG. 3A ;
FIG. 4B is a side view of the system illustrated in FIG. 3B ;
FIG. 4C is a side view of the system illustrated in FIG. 3C ;
FIG. 5A is a perspective view a second system embodiment made in accordance with one or more principals of the present invention;
FIG. 5B is a top view of the second system embodiment;
FIG. 6A is a side view of the second system embodiment showing a full water level;
FIG. 6B is a side view of the second system embodiment showing an initial flush and the use of water from the main portion;
FIG. 6C is a side view of the second system embodiment showing a double flush and the use of water from both the main and reserve portions; and
FIG. 7 is an enlarged perspective view of a third system embodiment showing the top portion of a gate panel movable secured in a holding tank by a pair of unshaped side edges.
DETAILED DESCRIPTION OF THE EMBODIMENTS
While the invention is susceptible to embodiments in many different forms, there are shown in the drawings and will described herein, in detail, the preferred embodiments of the present invention. It should be understood, however, that the present disclosure is to be considered an exemplification of the principles of the invention and is not intended to limit the spirit or scope of the invention, claims and/or embodiments illustrated.
Turning now descriptively to the drawings, in which similar reference characters denote similar elements throughout the several views, FIGS. 1A through 4C illustrate a toilet bowl water flow adjustment system 100 , which comprises a divider module 105 which separates a holding tank 10 of a toilet into a main portion 20 and a reserve portion 110 . The main portion 20 contains the main flapper valve 30 is connected to the handle arm 40 by a conventional flush connector 50 . The main flapper valve 30 engages the exit valve 60 of the holding tank 10 .
As mentioned, the flow adjustment system 100 includes a divider module 105 that keeps the two tank portions (main portion 20 and the reserve portion 110 ) in fluid separation from each other. Preferably, the divider module 105 includes a first panel 120 and a second panel 125 , with a movable gate panel 130 positioned there between. Both the first and second panels include an aperture 135 positioned near the bottom edge 137 of each panel. However, the location of the aperture 135 may be moved, but it is preferably positioned along the bottom edge 137 . The first and second panels include flanged edges 140 extending towards each other, such that the two panels when connected (such as by secured the flanged edges 140 together), the two-piece panel construction creates a cavity traversing from a top edge 143 to the bottom edge 137 . The cavity being sized to receive the movable gate panel 130 .
In addition to the above, each of the first and second panels 120 and 125 respectively may include a gasket end piece 142 that is able to engage the side walls of the holding tank to help keep the main portion 20 and the reserve portion 110 in fluid separate from each other. The gasket end pieces may be a suitably strip of rubber, vinyl, or similar resilient material, adhesively or otherwise secured in along the side walls of the holding tank. The gasket end pieces 142 may be an important aspect of a retrofit kit in existing toilets. Since toilets have variant holding tank shapes, the gasket end piece could help permit the divider module 105 to fit in virtually any sized holding tank 10 .
Similarly, in addition thereto, one or more of the first or second panels 120 or 125 may include an anchor system 145 used to secure the divider 105 in the holding tank 10 . The anchor system 145 consists of a pair of suction cups 150 which can laterally move outwardly from the outside edges 147 of the panels 120 125 . The suction cups 150 are controlled by turning the knob 152 . The knob 152 may simply connect to a rod which extends to a gear that is meshed to a rack and pinion gear. Depending on the direction, turning the knob would either push the suction cups away from the outside edges allowing them to engage the side walls of the tank or pull the suctions cups back towards the outside edges 147 .
When the divider 105 is assembled and secured/placed in the holding tank, the movable gate panel 130 is attached to the handle arm 40 by a conventional flush connector 50 . Connection to the conventional flush connector 50 is provided by linking the end of the conventional flush connector 50 to a movable gate panel 130 includes a first member 160 protruding from the top edge 162 of the moveable gate panel 130 . The first member 160 may include a plurality of openings 164 to adjustably receive the other end of the linkage 166 . Further connected to the protruding first member 160 is a second linkage 170 that has another end connected to one end 177 of a lever 175 . The second end 179 of the lever 175 is connected to a float 185 . In addition, the lever 175 further includes a weighted object 180 that has the freedom to move from one end to the other of the lever 175 . The lever 175 is pivotally secured about a portion 186 , which may be about the middle region thereof, to a second member 188 which extends and connects to the side panel 120 by a linkage member 190 . The second member 188 also provides a plurality of openings such that the lever 175 can be adjusted. The adjustments made by the first member 160 and the second member 188 permit the lever 175 to be adjusted such that the float 185 idly rests on the top of the water level in the holding tank when the holding tank is full of water and the system is at rest.
Operating the present system is efficient and easy and is designed such that any operator (especially children) can use the dual flush aspects of main embodiment. When the handle arm 40 is initially pushed down and released (once) the toilet begins its flushing cycle. The conventional flush connector 50 will pull the main valve flapper 30 and will also pull on the first member 160 causing the movable gate panel 130 to begin moving. When the handle arm 40 is released from the initial flush the water level in the holding tank is still above the divider module 105 . The float 185 is therefore kept in its top position which in turn keeps the moveable gate panel 130 in the downward position which keeps the aperture 135 closed separating the main portion 20 from the reserve portion 110 . As water flushes from the main portion 20 , the water level in both portions drops until the level in the reserve portion 110 is about the same height as the divider module 105 . While this could drop the float 185 , the weighted object 180 in the lever 175 keeps the lever 175 in a position that holds the float 185 above the water level and thus maintains the moveable gate panel 130 in a closed position.
To operate the present system in a dual flush capacity, the handle arm 40 is initially flushed as mentioned above. Immediately after the initial flush, the operator flushes the handle arm 40 a second time. Because a toilet ejects water quickly, the time between the initial flush and the second flush is sufficient to drop the water level to a position that the second flush will lower the float 185 and angle the lever 175 to a position that the weighted object 180 moves towards the end with the float 185 . The second flush will also raise the moveable gate panel 130 , which opens the aperture 135 between the main portion 20 and the reserve portion 110 . Since the float 185 is in a downward position and the weighted object 180 will keep the float 185 in the downward position, the moveable gate panel 130 will remain open. Therefore the second flush will empty both the main portion 20 and the reserve portion 110 .
While the shifting weighted object 180 may be critical for insuring proper close or open of the moveable gate panel 130 consistently, similar results may be achieved by carefully balancing the moveable gate panel, the float, and the forces on the gate provided by the water pressure differential between the main portion 20 and the reserve portion 110 .
The system can be made with no or minimum changes to any parts of the conventional toilet. From manufacturers' perspective, no expensive alterations of existing manufacturing assets are required since all existing toilet parts and the expensive equipment with which the toilets are made remain unchanged. In addition, no expensive new equipment is needed since there are no new specialized parts to be made with this mechanism. As a result, a dual flush toilet made with one or more of the aforementioned embodiments is significantly less costly to make than other dual flush toilets currently on the market.
The water quantity saved can be varied by the size of the main portion of the tank and the height of the divider module. In general, the smaller the size of the main portion of the tank is, the more water saving will be (there is a minimum size to be functional), and the taller the divider is, the more water saving will be. However, the maximum height of the divider should be slightly lower than the water level in the toilet tank when the tank is full.
One or more of the embodiments in the present invention includes a control mechanism with which a dual flush retrofit converter and a new model of dual flush toilet can be made. Such dual flush retrofit converter requires no replacement of any parts of the existing toilet (therefore is no risk to consumer should the consumer decide to go back to the original toilet), can be easily installed without professional support, and is user friendly. A dual flush toilet made with the mechanism costs significantly less than other dual flush toilets on the market and they are user friendly.
In another embodiment of the present invention, a retrofit system in accordance to similar principals to one or more of the above embodiments is described and illustrated in FIGS. 5A to 6C . The system 200 fits around the main flapper valve 30 completely enclosing the main flapper valve 30 by three walls 205 and a divider module 105 , creating a main portion 205 within the system 200 and a reserve portion 210 outside of the system. The ends 215 of the divider module 105 are connected to edges of two of the walls 205 . The operation of the system 200 would work similar to the aforementioned system 100 such that further explanation is not necessary.
In another embodiment of the present invention, a retrofit system in accordance to similar principals to one or more of the above embodiments is described and illustrated in FIG. FIG. 7 . The system 300 separates the holding tank into two portions, a main portion 20 and a reserve portion 110 . The system includes edge portions 305 that are secured to the side walls of the holding tank. Each edge portions 305 includes a channel 310 running along the length thereof. The channels 310 are sized to accommodate the gate panel 130 . The gate panel 130 is movably positioned in the edge portions 305 such that operation of the system 300 is similar to the above embodiments. A single or initial flush uses the water in the main portion, while a double flush, cause the gate panel 130 to be maintained off of the bottom wall of the holding tank, allowing the system to use the water from both the main portion and the reserve portion 110 . In other variant systems, the system 300 may also include a bottom portion having a channel sized to receive the bottom of the gate panel 130 . This helps ensures that the main portion and the reserve portion are in fluid separation of each other.
From the foregoing and as mentioned above, it will be observed that numerous variations and modifications may be effected without departing from the spirit and scope of the novel concept of the invention. It is to be understood that no limitation with respect to the specific methods and apparatus illustrated herein is intended or should be inferred. It is, of course, intended to cover all such modifications.
|
In one embodiment of the present system invention, there is provided a dividing module positioned in the holding tank of a toilet to separate the holding tank into a main portion and a reserve portion. The dividing module has a height lower than the full water level in the holding tank. The dividing module includes the ability to selectively connect the main portion and the reserve portion in fluid communication of each other. The embodiment allows an operator to press the handle arm an initial time to maintain the main portion and the reserve portion in substantially fluid separation of each other, such that water in the main portion is utilized to flush the toilet and wherein when the operator presses the handle a second time in the same manner as the initial time, the dividing module connects the main portion and the reserve portion in substantially fluid communication with each other, such that water in the reserve portion and the main portion is utilized to flush the toilet.
| 4
|
BACKGROUND OF THE INVENTION
This invention relates in general to structural panels and, more specifically, to a metal-surfaced polyimide foam structural panel in which the metal layer is diffused into interstices or discontinuities in the foam surface.
Metal surface layers have been applied to a very large variety of substrates. Typically, metals have been applied by electroless plating, electroforming, flame spraying, sputtering, plasma deposition and by simply bonding a metal film or foil to a substrate with an adhesive. While these techniques have generally produced acceptable results for many applications, when a composite panel produced by these methods is used in structural applications, problems of peeling of the metal layer from the substrate often occurs. Also, the metal is present only as a planar, parallel-surfaced, film and adds little to the structural strength of the panel. Further, these techniques have been less successful where the substrate is a foam material. Bonding to foam surfaces hav been found to be especially difficult, with low peel strength often resulting. Also, many of these application methods use temperatures or other conditions which tend to damage many insulating foam materials.
Attempts have been made to apply a metal surface layer to solid plastics or other substrates by chemical vapor deposition, such as is described by Popley in U.S. Pat. No. 3,519,473. Unfortunately, the coatings produced by these teachings do not have the desired adhesive strength since it is dependent upon simple adhesion. Ideally, where the composite structure is subject to stress causing catastrophic failure, the structure should fail by destruction of the substrate rather than failure along the metal-to-substrate bond line.
Complex techniques, such as the multi-layer, multi-metal, method described by Corwin in U.S. Pat. No. 3,537,881, have been used in an attempt to improve bonding. While some improvement results, peel strength is still not as great as is desirable. Attempts have been made to inter-lock sequential layers together, such as by using a layer of glass fibers extending both into a substrate and into a plastic surface coating, as detailed by El Bouhnini et al. in U.S. Pat. No. 4,242,406. This requires a complex and cumbersome mold and method in which the substrate and coating are produced at substantially the same time. This is not applicable to forming a metal coating or layer on a pre-existing substrate which may be highly contoured from previous shaping or re-shaping operations.
Thus, there is a continuing need for improved structural insulating panels having high insulating properties with a well-bonded metal surface layer and for methods of making such panels.
SUMMARY OF THE INVENTION
The above-noted problems, and others, are overcome by a method of making structural insulating panels which basically comprises providing a sheet of polyimide foam material and applying thereto a metal layer by chemical vapor deposition. Such foam structures, even when closed-cell, have natural microporosity in the surface. The resulting panel is found to have the metal diffused into the foam surface, forming a three-dimensional structure of metal and foam near the foam surface. Typically, the surface layer is 100% metal, generally having a thickness in accordance with desired structural properties. Metal penetrates to a depth corresponding to the density and porosity of the foam structure.
BRIEF DESCRIPTION OF THE DRAWING
Details of the invention, and of preferred embodiments thereof, will be further understood upon reference to the drawing, wherein;
FIG. 1 is a section through a structural insulating panel according to this invention, the section taken perpendicular to the panel face;
FIG. 2 is a section through a second embodiment of my structural insulating panel, taken perpendicular to the panel surface; and
FIG. 3 is a block flow diagram illustrating the method of my invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIG. 1, there is seen a polyimide foam sheet 10, here a sheet of bonded polyimide microballoons, having on one surface a smooth, continuous layer of metal 12. While diffusion of metal into the foam structure is difficult to illustrate, the metal layer 10 can be seen to have diffused into interstices between adjacent but slightly out of contact microballoons, such as at 14. These interstices are very small, often in the sub-micron range and should constitute at least about 1% of the foam surface.
Any suitable polyimide foam may be used to form sheet 10 which has the necessary surface openings to permit diffusion of the metal into the foam during deposition of layer 12. Typically, the foam sheet 10 may be an open-cell foam or may be a closed cell foam having the necessary interstices or surface discontinuities, such as are present in foam produce by bonding polyimide microballoons together. Typical polyimide foams may be produced by the methods described in U.S. Pat. Nos. 4,407,980; 4,394,464; 4,426,463; 4,425,441; 4,433,068 and 4,476,254.
Layer 12 may be formed from any suitable metal which plates out at a temperature below the decomposition temperature of the foam substrate. Typical metals include nickel, copper, and mixtures or alloys thereof. Metal layer 12 may be deposited to any suitable thickness. Typically, thicknesses in the 0.001 to 0.5 inch range are useful, with thickness of from about 0.015 to 0.125 inch giving good results. Best results are obtained with a nickel layer having a thickness of about 0.06 inch. The degree of diffusion of the metal into the foam surface depends in part on the deposition method used and on the number and size of foam sheet surface interstices. Typically, the metal may penetrate to produce a region of 50 volume percent metal and 50 volume percent foam at a depth below the foam surface of from about 0.03 to 0.50 inch. Excellent results are achieved with the 50% layer being at a depth below the foam surface of about 0.125 to 0.250 inch. For best structural bonding, a penetration depth (to the 50/50 volume ratio) should be about 25% to 30% of the overall panel thickness.
An alternate embodiment of the structural insulating panel is shown in FIG. 2. There, a layer of woven or matt fiberous material 18 (such as glass, polyimide, carbon, plastic or other suitable material) is laid over the surface of foam sheet 20 which is generally similar to foam sheet 10 of FIG. 1. When metal 22 is deposited on the panel, the metal atoms fill the spaces between the fibers of sheet 18 and the surface of foam sheet 20 (these spaces being somewhat exaggerated for clarity of illustration) and penetrate into interstices in the surface of foam sheet 20. The result is a composite having the fiber material imbedded in the metal layer which is structurally bonded to foam 20.
The method of preparing my structural insulating panels is schematically illustrated in FIG. 3. Initially, a sheet of suitable polyimide foam is prepared or otherwise provided, as indicated at 30. As described above, any suitable foam sheet having the necessary surface discontinuities or interstices may be used. Then, the metal layer is applied by chemical vapor deposition, as indicated at 32. If desired, a layer of fiberous fabric or matt may be placed over the surface of the foam sheet before the metal is deposited, as indicated at 34. If desired, a metal layer may be applied to both opposite surface (or all surfaces) of the foam sheet, any or all of which may bear a fiber sheet. Once the chemical vapor deposition of the metal is complete, the structural insulating panel is finished, as indicated at 36.
In a preferred method, the foam sheet is placed in the vacuum chamber which is then heated to a temperature below the degradation temperature of the foam while a slight vacuum, typically 1 to 10 torr, is applied slowly over about 10 to 60 minutes to allow any residual gases in the foam to escape. Typically the temperature may be relatively high, in the 200 to 280° C. range, since polyimides are very resistant to high temperature degradation. The chamber is then purged by flowing an inert gas, such as argon, therethrough. A gas or vapor which will, upon heating, decompose to produce an elemental metal (such as nickel carbonyl to produce nickel or any other conventional vapor deposition gas to produce any other selected elemental metal, or a mixture of gases to produce an alloy), is admitted to the chamber. The chamber is then heated to the decomposition temperature of the gas whereupon the elemental metal is plated on and into the foam surface. The gas or vapor may be held in the chamber prior to heating for a short (e.g., 1 to 10 minutes) period under slight pressure, such as about 20 to 40 mm of mercury, to allow the gas to "soak" into the surface interstices, which appears to aid in plating deeply into the interstices. After a sufficient period to produce a metal layer of the desired thickness (typically 60 to 300 minutes) the residual gas is removed and the plated foam sheet is removed from the chamber.
This panel may be used in building construction as a combined structural and insulating panel which also has outstanding high temperature and fire resistance, emitting no toxic gases when exposed to open flame. The metal layer serves as a heat reflector and vapor barrier and, because of the firm three-dimensional bond to the foam, greatly improves the structural strength of the panel.
The metal may be deposited by any suitable chemical vapor deposition method. Typical methods for the chemical vapor deposition of metals are described in U.S. Pat. Nos. 3,519,473 and 3,537,881 and in Chemical Engineering, Vol. 546, No. 10 (1949).
The following examples further detail certain preferred embodiments of methods of making my novel structural insulating panels. All parts and percentages are by weight unless otherwise indicated.
EXAMPLE 1
A 12 by 12 inch sheet of polyimide foam having a thickness of about0.5 inch is prepared by the process described in U.S. Pat. No. 4,407,980. The foam is a low density foam in which "macroballoons" or very small substantially spherical foam particles produced by expanding polyimide precursor particles are bonded together in a manner permitting surface discontinuities or interstices amounting to about 10% of the surface area. This sheet is placed inside a vacuum chamber which is tightly closed. The chamber is then evacuated by a vacuum pump to a slight vacuum, about 5 torr, very slowly to permit gasses in the foam to diffuse away. The chamber is maintained at about 260° C. for about 30 minutes. Argon gas is then admitted to the chamber to a pressure slightly above atmospheric. The temperature is lowered to about 90° C. and the argon is allowed to flow through the chamber to purge the chamber of other gases for about 10 minutes. Nickel carbonyl vapor is admitted into the chamber to a pressure of about 30 mm of mercury while the argon gas is allowed to pass from the chamber. At this point the nickel carbonyl begins to soak into the foam structure interstices. The chamber temperature is increased to about 195° C. The nickel carbonyl decomposes, producing atomic nickel and carbon monoxide. The nickel begins to coat the foam sheet surface. Areas of the apparatus not to be coated are protected by a thin layer of vacuum grease. After about 240 minutes the system is pumped down to remove residual gases, air is admitted and the chamber is opened. A dull nickel coating is found on the foam surface. Attempts to peel the nickel coating from the foam result in tearing of the foam below the surface. Close examination shows the nickel to have penetrated well into the foam interstices and to be very tightly adhered and mechanically bonded to the foam.
EXAMPLE II
The experiment of Example I is repeated, except that the foam sheet is suspended on several pins in the chamber. All exposed surfaces of the foam are found to have received a firmly adherent nickel coating.
EXAMPLE III
The experiment of Example I is repeated, except that a thin sheet of open weave glass fiber cloth is placed on the foam surface and position is continued for about 3 hours. A dull nickel coating is found to cover the fabric and foam surfaces, bonding them together and to the foam surface.
While the above examples, which describe preferred embodiments of the method and panel of this invention, describe in detail certain process variables and parameters, these may be varied, where suitable, with similar results. For example, the foam can contain any suitable additives, such as fillers, reinforcements and surfactants and other metals and surface reinforcing fabrics may be used.
Other variations, applications and ramifications of this invention will occur to those skilled in the art upon reading this disclosure. Those are intended to be included within the scope of this invention, as defined by the appended claims.
|
A structural panel having superior insulating properties which comprises a sheet of polyimide foam material having a metal layer on at least one surface, the metal layer being diffused into the foam structure, providing a superior metal-to-foam bond. The polyimide foam has excellent insulating and structural properties and is highly resistant to high temperatures and open flames. The metal layer adds considerable structural strength, since the diffusion of metal into the foam produces a three-dimensional metal structure rather than the usual planar surface film. The metal layer is applied to the foam sheet by chemical vapor deposition under conditions which improve the diffusion of the metal into the foam.
| 8
|
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims priority from U.S. Provisional Application No. 60/414,943 filed Sep. 30, 2002, which is incorporated by reference as if fully set forth herein.
FIELD OF THE INVENTION
[0002] This invention relates in general to reference transport channels (RTrCHs) in wireless communications, and in particular to a method and apparatus for RTrCH reselection implementation.
BACKGROUND OF THE INVENTION
[0003] As used herein, a wireless transmit/receive unit (WTRU) includes, but is not limited to, a user equipment, mobile station fixed or mobile subscriber unit, pager, or any other type of device capable of operating in a wireless environment. When referred to hereafter, a base station includes, but is not limited to, a base station, Node B, site controller, access point, or other interfacing device in a wireless environment.
[0004] In wireless communications, one of the most important features in maintaining the communication link quality under fading and interference situations is power control. In third generation partnership program (3GPP) wideband code division multiple access (W-CDMA) systems utilizing time division duplex (TDD) mode, the UTRAN (SRNC-RRC) sets the initial target signal to interference ratio (SIR) to the WTRU at the call/session establishment and then subsequently continuously adjusts the target SIR of the WTRU during the life term of the call as dictated by the observation of the uplink (UL) block error rate (BLER) measurement.
[0005] A variety of services, such as video, voice, and data, each having different Quality of Service (QoS) requirements, can be transmitted using a single wireless connection. This is accomplished by multiplexing several transport channels (TrCHs), each service on its own TrCH, onto a coded composite transport channel (CCTrCH). The transmitted information is sent in units of transport blocks (TBs). Each service's QoS requirement can be monitored on a BLER basis. The rate at which each service is transmitted is on a transmission time interval (TTI). The smallest interval is one frame of data, typically defined as 10 ms for a 3G communication system. Each frame is tracked by a system connection frame number (CFN), which is encoded into the frame header. TTIs are typically in intervals of 10 ms frame durations (i.e., 10, 20, 30, 40 ms, etc.). In particular for 3GPP systems, TTIs can only be 10, 20, 40, or 80 ms. The TTI for each service depends on the type of service and its QoS requirements. Because of these differences, a variety of TTIs associated with their respective TrCHs may exist on a single CCTrCH.
[0006] In order to monitor the BLER value at a CCTrCH level, as opposed to a TrCH level, one approach is to simultaneously monitor the BLER value of each TrCH multiplexed on the CCTrCH. A drawback to this approach is the potentially excessive use of system resources to monitor more channels than may be necessary.
[0007] Alternatively, in order to monitor the BLER level on a CCTrCH basis, a reference transport channel (RTrCH) may be selected among the transport channels multiplexed on the considered CCTrCH. The difficulty of this approach, especially for variable bit rate services, is the reselection of the RTrCH, since the initially selected RTrCH may become temporarily unavailable (OFF) during periods where it does not carry any data.
SUMMARY OF THE INVENTION
[0008] A method and implementing equipment are provided for a wireless communication system wherein wireless communications between communication stations includes the transmission of a composite channel on which a plurality of channels are multiplexed. The invention is intended for such systems wherein an error rate measurement is performed on received signals on a reference channel selected from the plurality of multiplexed channels. The error rate measurement is conventionally used in selectively controlling transmission of the composite channel, such as in power control for example.
[0009] A preferred method includes selecting a channel from the plurality of multiplexed channels as the reference channel initially used for error rate measurement. The reference channel is monitored based on quantitative data content criteria to determine an ON state when the quantitative data content criteria is met, and an OFF state when the quantitative data content criteria is not met. When monitoring of the reference channel reflects an OFF state, a different channel is selected from the plurality of multiplexed channels as the reference channel.
[0010] Preferably, the channels are transport channels (TrCHs), the reference channel is a reference transport channel (RTrCH), and each TrCH has a transport time interval (TTI) of a given size, of which a largest TTI size is an integer multiple, such as in a 3GPP system. In such systems, the TrCHs are multiplexed on a coded composite transport channel (CCTrCH) and a block error rate (BLER) measurement is performed on the RTrCH. Preferably, monitoring of the RTrCH is performed no less than once during each time interval corresponding to the TTI size of the RTrCH. Alternatively, the monitoring occurs upon a data reception on any TrCH.
[0011] Each TrCH has a BLER requirement. Preferably, a TrCH having a least restrictive BLER requirement is selected as the RTrCH initially used for BLER measurement. While there are N number of TrCHs multiplexed onto the CCTrCH, the TrCHs are preferably assigned a preference level for selection, first through N th , based first on their BLER requirement and then on TTI size, such that the first TrCH has a least restrictive BLER requirement and a smallest TTI size among TrCHs having the same BLER requirement and the N th TrCH has a most restrictive BLER requirement and a largest TTI size among TrCHs having the same BLER requirement. In such case, the first TrCH is selected as the RTrCH initially used for error rate measurement. When the first TrCH is selected as the RTrCH and monitoring of the first TrCH channel reflects an OFF state, the second TrCH is then selected as the RTrCH. Generally, when an i th TrCH is selected as the RTrCH, where i is less than N, and monitoring of the i th TrCH channel reflects an OFF state, a different TrCH is then preferably selected as the reselected RTrCH from among the group of channels consisting of the first TrCH through the (i+1) th TrCH.
[0012] In the general case, wherein an i th TrCH is selected as the RTrCH, where i is less than N, monitoring can be expanded such that the first through the i th TrCHs are monitored to determine ON and OFF states of each.
[0013] In general, monitoring of a TrCH is preferably performed no less than once during each time interval corresponding to the TTI size of the TrCH. Also, the determining when a TrCH is in an OFF state preferably includes determining that data was not received on the TrCH for a predetermined number of consecutive TTIs of the TrCH. Determining when the monitored TrCH is in an ON state preferably includes determining that data was received on the TrCH in at least one of a predetermined number of TTIs of the TrCH. A TrCH having the largest TTI size defines TTI boundaries based on that largest size for all TrCHs, and the selection of a different TrCH from the plurality of multiplexed TrCH as the reselected RTrCH preferably becomes effective at one of such defined TTI boundaries.
[0014] The invention includes a receiver for a communication station, either a base station or a WTRU, for use in such a wireless communication system. The receiver has composite channel signal processing circuitry that includes error measurement circuitry, monitoring circuitry, and reference channel selection circuitry. The error measurement circuitry is preferably configured to perform an error rate measurement on received signals on a selected reference channel of the composite channel. The monitoring circuitry is preferably configured to monitor the selected reference channel based on quantitative data content criteria to determine an ON state when the quantitative data content criteria is met, and an OFF state when the quantitative data content criteria is not met. The reference channel selection circuitry is preferably configured with a default channel selection and is responsive to the monitoring circuitry such that when monitoring of the reference channel reflects an OFF state, the reference channel selection circuitry selects a different channel from the plurality of multiplexed channels as the reference channel for the error measurement circuitry and the monitoring circuitry.
[0015] The receiver is preferably configured for a 3GPP like system, wherein the channels are TrCHs, the reference channel is a RTrCH, each TrCH has a TTI of a given size of which a largest TTI size is an integer multiple, and the TrCHs are multiplexed on a CCTrCH. In such case, the error measurement circuitry is configured to perform a BLER measurement on the RTrCH, and the monitoring circuitry is configured to monitor the RTrCH no less than once during each time interval corresponding to the TTI size of the RTrCH.
[0016] Where the TrCHs each have a block error rate (BLER) requirement, the reference channel selection circuitry is preferably configured with a TrCH having a least restrictive BLER requirement as the default TrCH selection initially used as the RTrCH. Generally, where there are N number of TrCHs multiplexed onto the CCTrCH, the reference channel selection circuitry is preferably configured to assign preference level for selection of the TrCHs, first through N th , based first on their BLER requirement and then on TTI size, such that the first TrCH has a least restrictive BLER requirement and a smallest TTI size among TrCHs having the same BLER requirement and the N th TrCH has a most restrictive BLER requirement and a largest TTI size among TrCHs having the same BLER requirement, and the first TrCH is selected as the RTrCH initially used for error rate measurement. In such case, the reference channel selection circuitry is preferably configured such that when the first TrCH is selected as the RTrCH and monitoring of the first TrCH channel reflects an OFF state, the second TrCH is then selected as the RTrCH. A TrCH having the largest TTI size defines TTI boundaries based on that largest size for all TrCHs. The reference channel selection circuitry is preferably configured such that the selecting a different TrCH from the plurality of multiplexed TrCH as the RTrCH becomes effective at one of such defined TTI boundaries.
[0017] In general, the reference channel selection circuitry is preferably configured such that when an i th TrCH is selected as the RTrCH, where i is less than N, and monitoring of the i th TrCH channel reflects an OFF state, a different TrCH is then selected as the RTrCH from among the group of channels consisting of the first TrCH through the (i+1) th TrCH. In such case, the monitoring circuitry is preferably configured such that when an i th TrCH is selected as the RTrCH, where i is less than N, the first through the i th TrCHs are monitored based on a quantitative data content criteria to determine an ON and OFF states. Preferably, the reference channel selection circuitry is then configured such that when monitoring of the i th TrCH channel reflects an OFF state, if any TrCH is determined to be in an ON state, the highest order TrCH that is determined to be in an ON state is then selected as the RTrCH.
[0018] In general, the monitoring circuitry is preferably configured such that monitoring of a TrCH is performed no less than once during each time interval corresponding to the TTI size of the TrCH. Also, the monitoring circuitry is preferably configured such that the determining when a TrCH is in an OFF state includes determining that data was not received on the TrCH for a predetermined number of consecutive TTIs of the TrCH. One alternative is that the monitoring circuitry is configured such that the determining when TrCH is in an ON state includes determining that data was received on the TrCH in at least one of a predetermined number of TTIs of the TrCH.
[0019] Other advantages will be apparent from the following description of preferred embodiments, and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] A more detailed understanding of the invention may be had from the following description of preferred embodiments, given by way of example and to be understood in conjunction with the accompanying drawing wherein:
[0021] [0021]FIG. 1A shows a block diagram of communication system;
[0022] [0022]FIG. 1B shows a block diagram of a WTRU related to the present invention;
[0023] [0023]FIG. 1C shows a BLER measurement unit related to the present invention;
[0024] [0024]FIG. 2 shows a flow diagram of an overview of a first embodiment for RTrCH monitoring and reselection;
[0025] FIGS. 3 A- 3 C show an example set of transport channels for prioritization by parameters;
[0026] [0026]FIG. 4 shows a flow diagram of the monitoring of the current RTrCH in “ON” state;
[0027] [0027]FIG. 5 shows a representation of a transport channel monitoring point with tolerance along the time axis;
[0028] [0028]FIG. 6 shows a flow diagram of the monitoring of the current RTrCH in “OFF” state;
[0029] [0029]FIG. 7 shows a flow diagram for switching of RTrCHs during reselection;
[0030] [0030]FIG. 8 shows an overview of a second embodiment for RTrCH monitoring and reselection shown in FIGS. 9 and 10;
[0031] [0031]FIG. 9 shows a flow diagram of the monitoring of transport channels in a hot-candidate list that are in “OFF” state;
[0032] [0032]FIG. 10 shows a flow diagram of the switching of RTrCHs during reselection using a hot-candidate list;
[0033] [0033]FIG. 11 shows a flow diagram of the monitoring of the current RTrCH in “ON” state at every data reception;
[0034] [0034]FIG. 12 shows a flow diagram of the monitoring of the current RTrCH in “OFF” state at every data reception; and
[0035] [0035]FIG. 13 shows a flow diagram of the monitoring at every data reception of transport channels in a hot-candidate list in “OFF” state.
ACRONYMS
[0036] The following acronyms are used in this application:
3G Third Generation BLER block error rate CCTrCH coded composite transport channel CFN connection frame number MAC medium access control OAM operation, administration, and maintenance QoS quality of service RNC radio network controller RRC radio resource control RTrCH reference transport channel SIR signal to interference ratio SRNC serving RNC TrCH transport channel TTI transmission time interval UL uplink UMTS universal mobile telecommunications system UTRAN UMTS terrestrial radio access network VBR variable bit rate WTRU wireless receive/transmit unit
DESCRIPTION OF PREFERRED EMBODIMENTS
[0037] Although the embodiments are described in conjunction with a third generation partnership program (3GPP) wideband code division multiple access (W-CDMA) system utilizing the time division duplex mode, the embodiments are applicable to any hybrid code division multiple access (CDMA)/time division multiple access (TDMA) communication system. Additionally, the embodiments are applicable to CDMA systems, in general, such as the proposed frequency division duplex (FDD) mode of 3GPP W-CDMA.
[0038] The preferred approach for BLER measurement according to the present invention is to limit the number of TrCHs to be monitored for BLER. The first embodiment exclusively limits the BLER monitoring to a single TrCH, that being the RTrCH. FIG. 2 shows a basic flow diagram for the selection of the initial RTrCH and the subsequent reselection of the RTrCHs for when it becomes necessary to replace the current RTrCH with a better candidate. To summarize, an initial RTrCH is selected based on prioritization criteria. The RTrCH is monitored for ensuring whether it is maintaining an ON status. If it is detected that its activity falls below an acceptable level, the next best candidate TrCH is chosen as the reselected RTrCH to replace the initial RTrCH, since an RTrCH in an OFF state is not preferred for BLER measurement. The timing of the reselection is also carefully tracked to prevent the transition from occurring at an inopportune time.
[0039] Each step of process 100 will now be described in further detail in reference to FIG. 2. After the step 101 start, the first step is to select the initial RTrCH in step 102 . This is achieved by assignment of a preference level PL to each TrCH multiplexed onto the CCTrCH. The TrCH with the highest preference level PL 1 is selected as the initial RTrCH. The remaining TrCHs are sorted in descending order of preference level PL.
[0040] As an example, FIGS. 3 A- 3 C show a set of five transport channels TrCH 1 -TrCH 5 for mapping onto the CCTrCH. FIG. 3A shows TrCH 1 -TrCH 5 sorted by channel number, each with a respective BLER requirement and TTI size. In FIG. 3B, each preference level PL is assigned based on the BLER requirement, with highest preference given to lowest BLER requirement (i.e., the least restrictive BLER requirement), which corresponds to the highest BLER requirement value. The next parameter for assigning preference level PL is TTI size. Accordingly, transport channel TrCH 2 is assigned preference level PL 1 because it has the lowest BLER requirement, 10 2 . Transport channels TrCH 4 and TrCH 1 each have a higher BLER requirement of 10 −3 , but transport channel TrCH 4 is assigned the higher preference level PL as it has the smaller TTI size of 20 ms compared to the 40 ms TTI size of TrCH 1 . Accordingly, transport channel TrCH 4 is assigned preference level PL 2 and transport channel TrCH 1 is assigned preference level PL 3 . Lastly, transport channels TrCH 3 and TrCH 5 are each assigned preference level PL 4 , as they both have the highest BLER requirement of 10 −4 and the same TTI size of 10 ms. When further tie breakers are necessary, such as with transport channels TrCH 3 and TrCH 5 , the selection of RTrCH from these two transport channels will be on a random basis.
[0041] Returning to step 102 of FIG. 2, a plurality of counters associated with the ON/OFF monitoring of TrCHs and the RTrCH are initialized. (See TABLE 1 for a summary of counters along with a brief description of their related function.) The list of candidate transport channels CAND_LIST includes all transport channels multiplexed on the CCTrCH, with the exception of the RTrCH, both at initialization and throughout the reselection process. Counter COUNT(RTrCH), which monitors the number of occurrences of presence or absence of data on the RTrCH during a monitoring cycle, is reset to zero. Observation period counter OP(RTrCH), which counts how long the RTrCH is being monitored, is also reset to zero. Counter OP(RTrCH) is expressed in terms of number of RTrCH TTIs and is used while monitoring a channel in OFF state. Since process 100 only monitors one channel at any given time (i.e., RTrCH), only one of each of the above initialized parameter counters is necessary to perform monitoring and reselection of RTrCH.
[0042] In step 103 , RTrCH is monitored every TTI, and the ON/OFF state of the RTrCH is recorded as RTrCH_ST. Determination of the ON/OFF state involves detection of data or the absence of data on the monitored channel RTrCH. Further, a designated observation period is used for establishing the density of the data detection for declaring an ON/OFF status with a degree of reasonable certainty. The ON/OFF status is therefore a matter of choice, established by comparing data detection to predetermined selection criteria parameters.
[0043] Next, the timing of the current frame is checked for correspondence to the largest TTI boundary in order to establish whether it is the proper time for RTrCH reselection (step 104 ). The current frame is tracked by counter COUNT(F). The largest TTI boundary is the largest common TTI among the all TrCHs, including the RTrCH. This is preferably obtained by using a modulo operation to determine the TTI boundary of each TrCH. An example for largest TTI boundary determination is shown in FIG. 3C with reference to TrCH 1 - 5 of FIGS. 3A and 3B. As shown in FIG. 3C, the largest TTI boundary occurs at intervals of 40 ms due to the largest TTI size of 40ms for this set of TrCHs.
[0044] In step 104 , if the current frame is not at the largest TTI boundary, then switching to a different RTrCH cannot occur at this point. The process is restarted at step 103 at the next frame. If, however, at step 104 , the current frame corresponds to the largest TTI boundary, then process 100 proceeds to step 105 , where a potential reselection of the RTrCH may occur.
[0045] Step 105 is an ON/OFF status check of RTrCH state counter RTrCH_ST that was recorded in step 103 . If RTrCH_ST=ON, there is no need to reselect RTrCH, so the process returns to step 103 for continuation of monitoring the RTrCH. If RTrCH_ST=OFF at step 105 , the process proceeds to step 106 for a decision on whether there are any other candidates for RTrCH. If the list of candidates CAND_LIST is null, i.e., there are no TrCHs in the candidate list CAND_LIST, the process returns to step 103 , keeping the same RTrCH despite its OFF state. The expectation is that shortly within the next occurring frames, either the current RTrCH will come back on, or another candidate RTrCH will become available. Thus, BLER measurement using an OFF RTrCH will be kept to a minimum. Reestablishing BLER measurement is based on selecting the best possible transport channel as the RTrCH. Returning to step 106 , if there is an available candidate, an RTrCH reselection is made at step 107 to the TrCH with the highest preference level PL.
TABLE 1 Counter Function COUNT(F) Provides the count of the current frame OP(RTrCH) Observation period counter of the RTrCH used during monitoring of channel in OFF state CAND_LIST Candidate list of TrCHs to be selected from at RTrCH reselection RTrCH_ST ON/OFF state of the RTrCH COUNT(RTrCH) Number of occurrences of presence or absence of data on RTrCH during one monitoring cycle
[0046] Each of the above steps of FIG. 2 will now be explained in further detail with reference to FIGS. 4 - 6 .
[0047] In FIG. 4, a flow diagram of RTrCH monitoring process 200 is shown for when RTrCH is active (i.e., RTrCH_ST=ON) at the start (step 201 ), for determining whether the level of activity has subsided enough to declare an OFF state for RTrCH (i.e., RTrCH_ST=OFF). Process 200 occurs during step 103 of process 100 . Process 200 verifies the current RTrCH state at every TTI for that RTrCH. For example, if TrCH 2 is the RTrCH, its TTI is 20 ms, and therefore, process 200 repeats every 20 ms (i.e., TTI(RTrCH)=20).
[0048] [0048]FIG. 5 illustrates adjustment of the timing of transport channel monitoring received at the MAC. In order to take into account the uplink transfer delay, the RTrCH state monitoring is not performed at the boundary (end-point) of the TTI, but rather after the end-point of the TTI. This accounts for the radio interface delay, data channel delay, and data processing delay. For simplicity, the offset with respect to the TTI end-point can be specified through OAM provisioning. For instance, a total delay is shown in FIG. 5 which is less than 0.5 TTI. In order to counteract the delay, an offset TTI_Tolerance can be specified as 0.5 TTI, where the monitoring point B is 0.5 TTI beyond the TTI boundary point A.
[0049] Returning to FIG. 4, a decision occurs at step 203 to check for whether data is received on the RTrCH. If so, the counter COUNT(RTrCH) is reset to zero at step 204 and the process cycle ends at step 208 . This reset at step 204 occurs since process 200 only tracks consecutive inactive readings of the RTrCH, as the objective is to determine when the RTrCH can be declared OFF. If at step 203 no data is received on the RTrCH, the RTrCH counter COUNT(RTrCH) is incremented by one in step 205 . Following step 205 is the decision (step 206 ) whether the incremented counter COUNT(RTrCH) value has reached the predefined parameter TTI_Inactive. For example, if it is desired to have no more than five (5) sequential inactive TTIs for a RTrCH, parameter TTI_Inactive is predefined to equal five (5). Once counter COUNT(RTrCH) is incremented to a value of five (5) at step 206 , the RTrCH is declared OFF (i.e., RTrCH_ST=OFF), as shown in step 207 . When the RTrCH is set to OFF, counter COUNT(RTrCH) is reset to zero and the monitoring cycle 200 is complete at 208 .
[0050] [0050]FIG. 6 shows a process 300 for monitoring the RTrCH while RTrCH_ST=OFF, to decide when it can be considered reactivated, and thus declared ON (i.e., RTrCH_ST=ON). Process 300 is part of step 103 in process 100 shown in FIG. 2. Because reselection of the RTrCH is to occur when the RTrCH is OFF, it is important to establish whether the RTrCH is indeed OFF prior to reselection. If it is determined in process 300 that the RTrCH is active enough such that RTrCH_ST can be switched from OFF to ON, the need for reselection is eliminated, and the RTrCH monitoring and reselection process 100 repeats at step 103 . Repetition of process 100 occurs at every TTI(RTrCH) plus TTI_Tolerance.
[0051] Returning to FIG. 6, process 300 begins at step 301 . At step 303 , the RTrCH observation period OP(RTrCH) is incremented by one. In step 304 , the RTrCH is monitored for whether data is received. If so, RTrCH counter COUNT(RTrCH) is incremented by one in step 305 . Following step 305 , the RTrCH counter COUNT(RTrCH) is compared to the predetermined reference TTI_Active for number of active TTIs, to determine whether enough activity on the RTrCH has occurred such that the status can be switched from OFF to ON. If counter COUNT(RTrCH) does not equal the required minimum TTI_Active reference, the process ends at step 311 . However, if in step 307 the count has reached the requisite number for activity TTI_Active, the RTrCH state is set to ON (step 309 ), and counters COUNT(RTrCH) and OP(RTrCH) are reset to zero, ending the process at step 311 .
[0052] Returning to step 304 , if data is not received on the RTrCH, step 306 examines whether the observation period OP(RTrCH) has reached parameter T_Activity, indicating that the predetermined number of observation periods has elapsed. Reference parameter T_Activity is useful for setting the desired period of monitored cycles of process 300 to ensure an acceptable density of activity. If the RTrCH has activity that is very spurious, then it is not ready to be considered ON. For example, if single bursts of activity are interspersed with several consecutive TTIs with no data, eventually COUNT(RTrCH) would reach TTI_Active, but with a low percentage of activity over the observation period, (e.g., 5%), the RTrCH would be of little use as a reference channel. Accordingly, with OP(RTrCH) reaching the T_Activity reference in step 306 , the counters for the RTrCH activity T_Activity and the observation period counter OP(RTrCH) are both reset to zero, bringing the monitoring process to an end at step 311 . If the observation period at step 306 is not equal to the value for T_Activity, the counters COUNT(RTrCH) and OP(RTrCH) are not reset so that their counts are maintained for subsequent cycles of process 300 , and the cycle ends at step 311 .
[0053] TABLE 2, below, summarizes the parameters defined by the RNC for analysis against the various counters used for monitoring the ON/OFF state of the RTrCH:
TABLE 2 Parameter Description TTI_Inactive Maximum number of consecutive TTIs with inactive RTrCH that can acceptably be endured (to declare ON RTrCH OFF)‘ TTI_Active Minimum required number of TTIs with active RTrCH over a period T_Activity (used to declare an OFF RTrCH ON) T_Activity period of TTIs to be monitored for RTrCH activity prior to declaring an OFF RTrCH ON TTI(RTrCH) TTI size for the RTrCH which is the duration for one monitoring cycle
[0054] Steps 105 - 107 of FIG. 2 are shown in more detail by the flow diagram of FIG. 7. Process 400 shown in FIG. 7 determines whether to reselect the RTrCH (i.e., whether or not to switch over to a better candidate TrCH to act as the RTrCH). Process 400 occurs at every largest TTI boundary, which is at every 40 ms for the set of five transport channels TrCH 1 - 5 shown in FIG. 3C. This boundary is chosen to avoid switching transport channels that may be in midstream. For instance, if the RTrCH reselection were to occur at 20 ms in FIG. 2, TrCH 1 has not yet completed its transmission of data, and it would be undesirable to switch over to TrCH 1 as the next RTrCH at that moment.
[0055] Returning to FIG. 7, process 400 begins at step 401 and proceeds to a decision at step 402 as to whether the RTrCH is ON or OFF. If the RTrCH is ON (i.e., RTrCH_ST=ON), BLER measurement on the RTrCH continues/resumes at step 406 , and switching process 400 is completed at step 407 . If the RTrCH is OFF (i.e., RTrCH_ST=OFF) at step 402 , the process proceeds to step 403 where candidate list CAND_LIST is checked for the absence of candidates. If CAND_LIST is null, the process ends at step 407 . It should be noted, however, that this would occur only if there were one TrCH multiplexed on the CCTrCH, which would indefinitely serve as the RTrCH. In such a case, monitoring process 400 continues to monitor the RTrCH to detect when its state changes to ON. If there are candidates in CAND_LIST at step 403 , process 400 proceeds to step 404 and a new RTrCH is chosen from CAND_LIST in order of highest preference level PL (step 404 ). BLER measurement on the new RTrCH commences at step 405 and the process is complete at step 407 .
[0056] In a second embodiment of the present invention, more than one TrCH is monitored by BLER measurement unit 20 to track ON/OFF states. Unlike the first embodiment where only the RTrCH is monitored, all TrCHs that were once the RTrCH are kept in a hot-candidate list HOTCAND_LIST sorted by preference level PL. During the reselection process, which occurs at every largest TTI boundary, the preferred TrCH for reselection as the RTrCH is the TrCH from among the hot-candidates in HOTCAND_LIST which has the highest preference level PL and is in the ON state. In addition to the hot-candidate transport channels, transport channels in CAND_LIST are available as candidates for reselection.
[0057] [0057]FIG. 8 shows a flow diagram of process 500 , which is the overview of the second embodiment for monitoring and reselection of the RTrCH. Following the start at step 501 , the RTrCH is selected from transport channels TrCHs in step 502 based on assigned preference levels PL, just as described for process 100 shown in FIG. 2, and the process counters are initialized. At step 503 , in addition to monitoring the RTrCH, each hot-candidate transport channel TrCH_i on the hot-candidate list HOTCAND_LIST is also monitored at intervals of TTI plus a nominal tolerance TTI_Tolerance for uplink transfer delay. The ON/OFF state for the RTrCH and the hot-candidates TrCH_i are recorded in TrCH_i_ST. Next, the current frame is compared for correspondence to the largest TTI boundary in step 504 . If the current frame is not at the largest TTI boundary, the process is delayed for one frame (step 506 ), and then resumed at step 503 . Once the current frame corresponds to the largest TTI boundary TTI_Boundary at step 504 , the process continues at step 505 where the next RTrCH is selected from either 1) TrCHs in the hot-candidate list HOTCAND_LIST in an ON state and with the highest preference level PL; or 2) from the candidate list CAND_LIST with the highest preference level PL. Once the RTrCH reselection is completed in step 505 the cycle is repeated beginning with step 503 .
[0058] Each of the above steps of process 500 will now be explained in further detail. During initialization in step 502 , candidate list CAND_LIST is loaded with the identity of each transport channel TrCH multiplexed on the CCTrCH other than the RTrCH. Counters HOTCAND_LIST, OP(RTrCH), COUNT(TrCH_i), OP(TrCH_i) are all initialized to zero. Each hot-candidate transport channel TrCH_i is monitored by its own counter represented by COUNT(TrCH_i). Observation periods of the RTrCH and TrCH_i (i.e., OP(RTrCH) and OP(TrCH_i), respectively), are counters used to monitor how long, in terms of TTI, a given channel is being monitored.
[0059] Step 503 is shown in further detail by the flow diagram of FIG. 9, which illustrates process 900 for RTrCH monitoring using TrCH hot-candidate list HOTCAND_LIST. Process 900 monitors each hot-candidate transport channel TrCH_i in HOTCAND_LIST (currently in OFF state) to determine whether it is possible to declare it to be in the ON state. Process 900 is run for each transport channel TrCH_i in the hot-candidate list at every TTI for the particular hot-candidate TrCH_i. Thus, if there are three hot-candidates TrCH_i, there will be three parallel processes 900 operating to monitor each hot-candidate TrCH_i respectively. Preferably, the monitoring point occurs at the TTI boundary of hot-candidate TrCH_i plus a nominal TTI_Tolerance.
[0060] Process 900 starts at step 901 and proceeds to step 903 where it is determined whether there are any hot-candidates TrCH_i in the hot-candidate list HOTCAND_LIST. If the hot-candidate list HOTCAND_LIST is empty, process 900 ends at step 912 . If, however, there are hot-candidates TrCH_i present in HOTCAND_LIST, observation period OP(TrCH_i) is incremented (step 904 ).
[0061] The next decision (step 905 ) is whether data has been received on the monitored hot-candidate TrCH_i. If data has been received, counter COUNT(TrCH_i) is incremented to reflect the data reception at step 906 . Next, COUNT(TrCH_i) is checked to determine whether the count has reached the predetermined reference value TTI_Active (i.e., to determine whether enough activity on the RTrCH has occurred such that the status TrCH_i_ST can be switched from OFF to ON). If counter COUNT(TrCH_i) does not equal the required minimum TTI_Active reference value, process 900 ends at step 912 . However, if in step 907 counter COUNT(TrCH_i) has reached the requisite number for activity, the hot-candidate state TrCH_i_ST is turned ON (step 908 ), and the hot-candidate counters COUNT(TrCH_i) and OP(TrCH_i) are reset to zero (step 911 ), before ending the process at step 912 .
[0062] Returning to decision step 905 , if data is not received on the hot-candidate TrCH_i, a decision at step 910 commences where the observation period for the hot-candidate OP(TrCH_i) is checked against parameter T_Activity, yielding whether the predetermined acceptable number of observation periods has elapsed. If so, the counter COUNT(TrCH_i) for hot-candidate TrCH_i and the observation period counter OP(TrCH_i) are both reset to zero (step 911 ), and process 900 ends at step 912 . If the observation period OP(TrCH_i) is not equal to the value for T_Activity, the counters maintain their counts for subsequent cycles of process 900 , and process 900 ends at step 912 .
[0063] [0063]FIG. 10 shows a flow diagram of process 1000 , which shows steps 504 and 506 in further detail. Process 1000 involves the decision making process for whether to reselect the RTrCH from the hot-candidate list HOTCAND_LIST, based on the appropriateness of the current frame timing, and if a suitable replacement transport channel has become sufficiently active. Process 1000 occurs at every largest TTI boundary, which is at every 40 ms for the set of five (5) transport channels TrCH 1 - 5 shown in FIG. 3C. As aforementioned, this boundary is chosen to avoid switching TrCHs that may be in midstream. Process 1000 begins at step 1001 and proceeds to a decision step 1002 as to whether there is at least one hot-candidate TrCH_i in the ON state in list HOTCAND_LIST. If so, BLER measurement on the current RTrCH is ceased as it now becomes the former RTrCH, and now the former RTrCH is added to HOTCAND_LIST. Next in step 1004 , the TrCH with the highest preference level PL from HOTCAND_LIST is reselected as the new RTrCH. Next in step 1005 , any TrCH_i in the HOTCAND_LIST with PL less than equal to either the new or the prior RTrCH preference level is removed. The removed TrCHs are added to CAND_LIST. Thus, HOTCAND_LIST is maintained with candidates having greater preference level PL than the current RTrCH. Reselection of RTrCH from hot-candidates TrCH_i will occur as soon as a hot-candidate TrCH_i goes ON, regardless if the RTrCH is ON or OFF. Meanwhile, monitoring is limited to hot-candidates TrCH_i, and resources are conserved by eliminating TrCHs from monitoring that are moved to the candidate list CAND_LIST. These CAND_LIST candidates will be eligible for monitoring and reselection if transferred back to HOTCAND_LIST, as described below. BLER measurement resumes in step 1006 using the new RTrCH, and process 1000 is complete at step 1007 .
[0064] Returning to the decision step 1002 , if there are no hot-candidates TrCH_i in the ON state in HOTCAND_LIST, step 1008 checks the ON/OFF state RTrCH_ST for the current RTrCH. If the state of the current RTrCH is ON, BLER measurement is continued using the current RTrCH (step 1009 ), and process 1000 ends at step 1007 . If the state of the current RTrCH is OFF at step 1008 , step 1010 commences to check whether CAND_LIST is empty, and if so, process 1000 ends at step 1007 . If CAND_LIST is not null, the new RTrCH is reselected from CAND_LIST taking the TrCH with the highest preference level PL, and the current RTrCH becomes the former RTrCH and is added to HOTCAND_LIST (step 1011 ). Any TrCH in CAND_LIST with PL equal to the new RTrCH PL is added to HOTCAND_LIST (step 1012 ). Hot-candidate counter COUNT(TrCH_i) is reset to zero for each TrCH added to HOTCAND_LIST. Thus, the list of hot-candidates HOTCAND_LIST is updated to include the best candidates for subsequent reselection. Next, BLER measurement is resumed at step 1006 using the new RTrCH, and process 1000 ends at step 1007 .
[0065] In an alternative of the first embodiment of the invention, reselection of the RTrCH is the same as the first embodiment process 100 using candidates from CAND_LIST, but the monitoring of the RTrCH is not in a periodic fashion on a TTI basis as in step 103 of FIG. 2. Instead, monitoring of the RTrCH occurs aperiodically at detection of data on any of the transport channels. Once data is detected, it can be established that at that moment, the current frame is at a TTI boundary. The current frame is tracked by using the encoded CFN contained in the received frame header.
[0066] [0066]FIG. 11 shows a flow diagram of a process 1100 , which performs RTrCH monitoring on a data reception basis. Process 1100 is a modification of process 200 shown in FIG. 4, where monitoring of an active RTrCH is performed to determine when the RTrCH activity subsides enough that it can be declared to be in an OFF state. Process 1100 starts at step 1101 , and is repeated at every data reception on any transport channel to accommodate current frame tracking performed in step 1103 . At step 1103 , the number of elapsed TTIs between data detections, represented by TTI_Difference, is calculated, using the following relationship:
TTI_Difference = FLOOR [ ( CFN_Current + 256 - CFN_Previous ( RTrCH ) ) mod 256 TTI ( RTrCH ) ] Equation 1
[0067] CFN_Current represents the current connection frame number CFN as identified in the received data frame received on any of the transport channels multiplexed on the CCTrCH. Value CFN_Previous(RTrCH) represents the CFN of the frame in which the last data detection occurred on the RTrCH. The FLOOR function yields the integer value rounded down from the ratio in Equation 1. The preferred frame structure is defined by a repeating set of 256 frames, as evident by the mod256 operation in Equation 1, but other frame parameter types may be readily used within the scope of the present invention, whereby Equation 1 can be modified accordingly.
[0068] Following calculation step 1103 is the decision whether the number of inactive TTIs from value TTI_Difference has reached or exceeded the predetermined threshold TTI_Inactive (step 1104 ). For example, if it is desired to have no more than five (5) sequential inactive TTIs for a RTrCH, parameter TTI_Inactive is predefined to equal five (5). If value TTI_Difference meets or exceeds five (5), the RTrCH is declared OFF (RTrCH_ST=OFF), as shown in step 1105 .
[0069] At decision step 1106 , it is determined whether the transport channel on which data was received is the RTrCH. If so, the counter CFN_Previous (RTrCH) is reset to zero at step 1107 and process 1100 ends at step 1108 . This reset occurs since process 1100 only tracks inactive readings of the RTrCH, as the objective is to determine when the RTrCH can be declared OFF. If, however, no data was received on the RTrCH at step 1106 , the RTrCH counter CFN_Previous(RTrCH) is not incremented in step 1107 , and process 1100 ends at step 1108 . With no data received on the RTrCH at the current frame, at least another frame has transpired without data reception, which will be accounted for at the next calculation of TTI_Difference when process 1100 is repeated at any data reception.
[0070] Turning to FIG. 12, a flow diagram for a process 1200 that operates under an alternative to the first embodiment of the invention, where monitoring of the RTrCH is performed while it is OFF, to decide when it can be considered reactivated, and thus declared ON (i.e., RTrCH_ST=ON). Process 1200 is an alteration of channel monitoring process 300 of FIG. 6, where the alteration is that monitoring is triggered by RTrCH data reception. Process 1200 begins at step 1201 and the process is repeated at every data reception on the RTrCH. At step 1203 , RTrCH counter COUNT(RTrCH) is incremented by one (step 1203 ) because data was detected on the RTrCH at commencement of process 1200 . Next, TTI_Difference is calculated in step 1204 using Equation 1 for establishing the number of TTIs elapsed between data detections on the RTrCH. Observation period OP(RTrCH) is then incremented by value TTI_Difference (step 1205 ) which captures possibly several TTIs. In contrast to process 300 , in which OP(RTrCH) is incremented every TTI regardless of data detection, process 1200 has the advantage of reduced processing as monitoring is suspended during the TTIs with no data reception.
[0071] Decision step 1206 examines whether the observation period OP(RTrCH) has reached parameter T_Activity indicating that the predetermined acceptable number of observation periods has elapsed. If so, RTrCH counters COUNT(RTrCH) and OP(RTrCH) are reset to zero and counter CFN_Previous(RTrCH) is reset to CFN_Current. These reset counters reflect that too much time has elapsed since the last data detection, preventing a valid channel state change from OFF to ON, and a new observation period commences.
[0072] Returning to step 1206 , a negative result means that there is still an opportunity for the channel state to change, and process 1200 proceeds to step 1209 . The RTrCH counter COUNT(RTrCH) is compared to the predetermined reference TTI_Active, to determine whether enough activity on the RTrCH has occurred such that the status can be switched from OFF to ON. If counter COUNT(RTrCH) is less than the required minimum TTI_Active reference, counter CFN_Previous(RTrCH) is reset to CFN_Current (step 1208 ) and process 1200 ends at step 1212 . However, if in step 1209 the counter COUNT(RTrCH) has reached the requisite number for activity TTI_Active, the RTrCH state is set to ON (step 1210 ), and counters COUNT(RTrCH) and OP(RTrCH) are reset to zero (step 1207 ) before resetting CFN_Previous(RTrCH) at step 1208 .
[0073] An alternative to the second embodiment of the present invention involves monitoring of hot-candidates, but the monitoring occurs at every data reception on any hot-candidate TrCH_i rather than at every TTI. FIG. 13 shows a flow diagram of process 1300 , which is similar to process 900 of FIG. 9. Once process 1300 commences at step 1300 , hot-candidate counter COUNT(TrCH_i) is incremented at step 1303 to reflect the reception of data. Next, value TTI_Difference is calculated according to Equation 2 (step 1304 ):
TTI_Difference = FLOOR [ ( CFN_Current + 256 - CFN_Previous ( TrCH_i ) ) mod 256 TTI ( TrCH_i ) ] Equation 2
[0074] CFN_Current represents the current connection frame number CFN as identified in the received data frame received on any of the transport channels multiplexed on the CCTrCH. Value CFN_Previous(TrCH_i) represents the CFN of the frame in which the last data detection occurred on the monitored hot-candidate TrCH_i. Hot-candidate observation period OP(TrCH_i) is incremented by the value TTI_Difference (step 1305 ). The first decision step 1306 checks whether observation period OP(TrCH_i) has reached the predetermined parameter T_Activity, yielding whether the predetermined acceptable number of observation periods has elapsed. If true, the counter COUNT(TrCH_i) for hot-candidate TrCH_i and the observation period counter OP(TrCH_i) are both reset to zero, (step 1307 ) and frame counter CFN_Previous(TrCH_i) is reset to value CFN_Current (step 1308 ), bringing process 1300 to an end at step 1312 . If at step 1306 the observation period OP(TrCH_i) is not equal to the value for T_Activity, hot-candidate counter COUNT(TrCH_i) is checked for whether the count has reached the predetermined reference value TTI_Active. This decision at step 1309 determines whether enough activity on the hot-candidate transport channel has occurred such that the status can be switched from OFF to ON. If counter COUNT(TrCH_i) does not equal the required minimum TTI_Active reference value, the frame counter is reset at step 1308 and process 1300 ends at step 1312 . However, if in step 1309 the count has reached the requisite number for activity, the hot-candidate state TrCH_i_ST is turned ON (step 1310 ), and hot-candidate counters COUNT(TrCH_i) and OP(TrCH_i) are reset to zero (step 1307 ), before resetting CFN_Previous(TrCH_i) at step 1308 .
[0075] Implementation of the preferred methods will now follow in reference to FIGS. 1 A- 1 C. FIG. 1A shows a block diagram for a 3GPP UTRAN system 10 , comprising a radio network controller (RNC) 11 communicating with WTRU 16 through base station 14 . Since the general functionality of an RNC, base station, and WTRU are known by those skilled in the art, these components will only be described hereinafter to the extent that such functionality is relevant to the present invention. RNC 11 comprises many components that interact on several communication layers, but those of interest for the purpose of the present invention are shown in FIG. 1A. They are a radio resource control (RRC) layer 12 , medium access control (MAC) layer 13 , and frame protocol (FP) entity 25 . RRC 12 is responsible for performing outer loop power control of communication system 10 , which produces target SIR adjustments. MAC 13 performs the BLER measurement, which is a necessary input for outer loop power control. Alternatively, frame protocol (FP) entity 25 performs the BLER measurement.
[0076] RRC 12 is linked to MAC 13 via communication path 22 , which is linked in turn to FP 25 via communication path 24 . MAC control path 23 is used to transmit the BLER measurement from MAC 13 to RRC 12 , from which the target SIR adjustment is generated. Data channel paths 20 and 21 transmit the received communication data from WTRU 16 to MAC 13 and FP entity 25 , respectively, via base station 14 .
[0077] WTRU 16 comprises RRC layer 19 , MAC layer 17 , and Li layer 18 . RRC 19 and MAC 17 perform functions similar to RRC 12 and MAC 13 associated with RNC 11 . L 1 layer 18 is a physical (PHY) layer to which transport channels are mapped on the CCTrCH for UL transmission 26 . MAC control path 27 is used to transmit the BLER measurement from MAC 17 to RRC 19 when BLER measurement is performed by MAC 17 . Alternatively, Li layer 18 performs BLER measurement of WTRU 16 and the BLER measurement is transmitted across L 1 layer control path 28 to RRC 19 .
[0078] Base station 14 communicates through data channels 20 , 21 with RNC MAC layer 13 and FP entity 25 . The SIR target adjustment is achieved through signaling over the air interface on the DL signal 15 between WTRU 16 and base station 14 . In an alternative embodiment, base station 14 includes a MAC layer, which may perform the BLER measurement in lieu of MAC layer 13 of RNC 11 .
[0079] [0079]FIG. 1B shows a block diagram of WTRU 16 , comprising antenna 51 , isolator 52 , modulator 53 , amplifier 54 , data generator 55 , transmit power control unit 56 , BLER measurement unit 60 , channel estimation unit 57 , and demodulator 58 . BLER measurement unit 60 includes composite channel signal processing circuitry that comprises error measurement circuitry, monitoring circuitry and reference channel selection circuitry. A description of the BLER measurement unit 60 in the context of the remainder of WTRU 16 components now follows.
[0080] On the receiver side of WTRU 16 , antenna 51 receives various RF signals. Alternatively, antenna 51 may comprise an antenna array. The received signals are passed through isolator 52 to demodulator 58 to produce a baseband signal. The baseband signal is processed by channel estimation device 57 , which commonly uses a training sequence component in the baseband signal to provide channel information, such as channel impulse responses. Channel estimation device 57 is capable of separating the RTrCH from all other channels in the baseband. BLER measurement unit 60 determines the BLER with respect to the current RTrCH. The BLER measurement is received by the transmit power control unit 56 , which converts the BLER information into a control signal for power adjustment in amplifier 54 . Amplifier 54 receives the data signal for transmission from data generator 55 . On the transmission side, the data signal is amplified according to the adjusted power control signal from transmit power control unit 56 . The amplified signal is modulated at modulator 53 , passed through isolator 52 , and transmitted over antenna 51 .
[0081] [0081]FIG. 1C shows BLER measurement unit 60 in further detail. Preferably, BLER measurement unit 60 performs BLER measurements within the MAC layer 13 for RNC 11 and MAC layer 17 of WTRU 16 . BLER measurement unit 60 comprises memory unit 62 , register 64 , preference level unit 30 , TTI_Boundary unit 40 , and timer 45 . BLER measurement unit 60 is responsible for ascertaining whether a TrCH or the RTrCH is ON or OFF based on a cumulative count of presence or absence of data in the form of transport blocks (TBs) over time period in terms of TTIs, according to the preferred method embodiments.
[0082] Preference level unit 30 assigns a preference level PL to each TrCH for selection as the RTrCH. Register 64 maintains the plurality of counters used in the ON/OFF state monitoring of TrCHs and the RTrCH according to the present invention, comprising frame counter COUNT(F), RTrCH observation period OP(RTrCH), candidate list CAND_LIST, hot-candidate list HOTCAND_LIST, the RTrCH ON/OFF state RTrCH_ST, RTrCH counter COUNT(RTrCH), hot-candidate observation period OP(TrCH_i), hot-candidate counter COUNT(TrCH_i), and hot-candidate ON/OF state TrCH_i_ST. Memory unit 62 stores predetermined reference settings utilized by BLER measurement unit 60 for the decision process of whether to declare a TrCH or the RTrCH in the ON or OFF state, as presented above in TABLE 2.
[0083] With respect to the RTrCH monitoring point, timer 45 increments frame counter COUNT(F) every 10 ms. TTI_Boundary unit 40 works in conjunction with timer 45 to confirm whether the current frame is at a TTI boundary, and also determines the largest common TTI boundary among the candidate TrCHs to allow optimum synchronization for the switching of the RTrCHs. TTI_Boundary unit 40 performs a ratio calculation to determine TTI_Difference based on the value from counter COUNT(F) and the TTI size of the monitored transport channel. If the ratio yields an integer value, it is established that the current frame is at a TTI boundary. For example, if the TTI size is 20 ms, and the COUNT(F) value is 5, the yielded result is 50/20=2.5, which is not at a TTI boundary. Alternatively, spontaneous detection of data could commence tracking of the RTrCH state, rather than the periodic monitoring points shown in regular intervals in FIG. 5. The system CFN identified in each frame header can be used to track the number of TTIs that elapsed between occurrences of data detection on the RTrCH. This alternative embodiment would require less processing resources and eliminate the need for using timer 45 . Reference channel selection circuitry within BLER measurement unit 60 is configured to reselect RTrCH responsive to monitoring of the ON and OFF states of RTrCH and hot-candidates TrCH_i. Once reselection is made, BLER measurement commences on the new reference channel RTrCH.
|
In a wireless communication system using a reference channel used for error rate measurement and associated with a plurality of transport channels multiplexed on a coded composite transport channel (CCTrCH), a method is employed for reselection of the reference channel from favorable candidate transport channels. A channel is initially selected from the plurality of multiplexed channels as the reference channel. Channels are monitored based on quantitative data content criteria to determine whether an ON or OFF state exists. A different channel is selected from the plurality of multiplexed channels as the reselected RTrCH when a better candidate transport channel in the ON state becomes available, or when the monitored RTrCH reflects an OFF state.
| 7
|
This is a continuation of co-pending application Ser. No. 511,515 filed on July 6, 1983, and now abandoned.
BACKGROUND OF THE INVENTION
The present invention relates to vacuum cleaner apparatus, and more particularly, to vacuum cleaner apparatus substantially reducing the level of sound produced by the apparatus.
Conventional vacuum cleaners which include blowers and blower motors, in operation, produce sound levels of between 70 and 80 dB A. However, such a high sound level is found to be bothersome.
It is, therefore, the aim of the invention to propose a vacuum cleaner with a considerably reduced sound level, for example, approximately 60 dB A.
SUMMARY OF THE INVENTION
To achieve this aim, the invention is characterized in that the blower with its blower motor is mounted in such a manner that vibrations are absorbed, in that the outgoing air of the blower is passed to an outlet through an outlet passage with multiple turns or baffles and the cross-section of which changes a number of times, in that the cooling air for the blower motor flows separately from the outgoing air through a cooling air duct which also has multiple turns or baffles and the cross-section of which also changes several times, and in that the air outlet passage and the cooling air passage are provided in the form of ducts and chambers with a sound-absorbent lining.
Due to the fact that the blower and blower motor are mounted in such a manner that vibrations are absorbed, a transmitting of the vibrations produced there by way of structure-borne noise to the housing of the vacuum cleaner is effectively reduced. The above-mentioned passing of the outgoing air of the blower and of the cooling air of the motor through long ducts and chambers provided with baffles ensures a good damping in the long blow-off passages, which in addition are damped by the sound-absorption linings or mats provided therein. The cross-sections change several times resulting in an absorption of airborne sound over a wide band. It is not absolutely essential to provide the aforementioned sound-absorbing measures on the suction side of the blower. The filter mat which is provided there to a certain degree also serves for the sound absorption and as a sound-absorption filter. It is also important that the cooling air system for the motor is separate from the system for the suction air and outgoing air of the blower. This reliably excludes a contamination of the motor or also a short-circuit which may be produced by possible moisture (dirty water) sucked up together with the suction air, and it is ensured that, independent of the degree of dirt on the filter mat and in the suction passages, the motor always receives sufficient cooling air.
These measures can even be used for cooling by means of the motor cooling air, the sensitive heat-producing electrical components of the vacuum cleaner, in which case these are arranged in the air flow of the motor cooling air.
To obtain as long as possible outlet passages, it is preferred that the housing of the vacuum cleaner should have a rectangular cross-section at least in the region of the outlet passage and of the cooling air passage. Compared to the usual round cross-section of the housing, which is also possible with this invention, the rectangular cross-section provides a larger volume and larger area available for the aforementioned sound-absorbing measures.
In front of the suction opening of the blower it is preferred to provide a grating which evens out the air flow, which also contributes to lowering the sound level.
A sound damper provided in the suction region of the blower serves the same purpose.
It is furthermore preferred that a contact spring be installed in a form-locking manner in the part which carries the blower, in which case the static charge of the metal dirt collecting tank, the antistatic suction hose as well as possibly of the accessories, is grounded by a protective conductor connected with the contact spring.
To prevent the sound absorption being adversely affected by wetting of the sound-absorption mats with which the air outlet passages are lined, it is furthermore preferred that a filter support basket and a one-way check valve with captive float ball be connected in an undetachable manner to the housing portion carrying the blower, thus to prevent any liquid or moist matter that is sucked up from getting into the repeated turns of the air outlet and cooling passages that are lined with sound-absorption mats.
Furthermore, in order to achieve the aim according to the invention, it is necessary that a large outlet opening is provided. To achieve this it is preferred that the rectangular housing be mounted on the round dirt collecting tank.
The materials and the passages of the flow media have been selected in such a manner that the housing portion carrying the blower and the portion bracing the blower are designed in such a way that dirt up to a temperature of 80° C. can be sucked up.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal sectional view of the upper portion of a vacuum cleaner according to the invention;
FIG. 2 is a sectional view taken at arrow II in FIG. 1;
FIG. 3 is a longitudinal sectional view of a sound damper utilized with the invention;
FIG. 4 is a longitudinal sectional view of an absorption damper utilized with the invention;
FIG. 5 is a longitudinal sectional view of a reflection damper utilized with the invention; and
FIG. 6 is a longitudinal sectional view of an interior member of the reflection damper of FIG. 5.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, a carrier plate 1 has mounted thereon a motor housing 3, rubber sealing elements or strips 2, typically fabricated of foam rubber being disposed between the motor housing and the carrier plate. The motor housing 3 consists of a broad turbine part 3a and a narrower motor part 3b, at the top of which a radial fan 4 is arranged. This radial fan sucks up the cooling air in the direction of arrow 5, which cooling air is blown off through a blow-off opening 5a and rises up in the direction of arrow 6 along the wall of an intermediate plate which will be described further on.
The fan 4 furthermore comprises a multipressure stage turbine wheel 7, with which the suction air is sucked up by way of the suction connection of a suction housing of which no further details are shown, via a suction hose and a filter, the suction air entering in the direction of arrow 8 by way of a suction opening 9 at the underside of the fan 4. According to the invention this suction air undergoes a substantial sound-damping.
In the suction opening 9 an air grating 10 is provided which has a mesh size of 3-8 mm and consists of square plastic rods, this grating having the important advantage that it evens out the flow air sucked up in the direction of arrow 8. It prevents above all a detrimental turbulence at the edges of suction opening 9, which causes whistling noises. The square ribs of this plastic grating are suitably rounded at the suction side.
The turbine wheel 7 has radial outlet or blow-off openings 11, through which the outgoing air flows in the direction of arrow 12 through a duct 13. The duct 13 is formed by an upwardly projecting flange 14 of the carrier plate 1, the wall of this duct being lined with a sound-absorption mat 15. It is important that the cross-section 13a of the duct becomes narrower, so that the air flowing through same is speeded up substantially. The other side of the duct is formed by the wall 16 of a clamping plate 18, the air being deflected at position 17 on the fact clamping plate 18 which is lined with damping strips 15. The flow of air is guided in the direction of arrow 19 into an annular duct 20 (see FIG. 2).
The annular duct 20 extends arcuately half-way about the housing. It is formed by two partial annular ducts which are approximately symmetrical to one another, as indicated on the right hand side in FIG. 1.
The annular ducts 20 are not exactly symmetrical to one another; they differ with regard to their radii. The annular duct on the left in FIG. 1 is hereafter described with reference to FIG. 2. It is seen that the air flows in the direction of arrow 21 into a housing opening 22, which can also be seen in FIG. 1. This housing opening 22 is partitioned off by a web 24 of the clamping plate 18, so that the air flows in the direction of arrows 25 and 28 through a duct 26, 27 shaped like a baffle, is then deflected again in the direction of arrow 29 on a web 30 of the clamping plate, and flows in the direction of arrow 31 through an outlet opening in the carrier plate, and at that point flows out of the housing.
However, in place of flowing into the opening 23 in the direction of arrow 21, the air may also continue to flow through the annular duct 20 in the direction of arrow 32, and may, in the direction of arrow 36, enter a chamber 37 by way of an inflow opening 33. The inflow opening 33 is formed by a rib or member 34 of the clamping plate and an adjacent rib 35. The chamber 37 leads into a further sound-damped duct 38, all surfaces which lie in the drawing plane of FIG. 2 being lined with foam mats. The air then flows on in direction of arrow 39 and then passes via a very long route in the region of duct 38 to an outlet opening 40 which is arranged in a hood 41.
On the right-hand side of FIG. 2 a baffle was chosen which is deflected three times so as to obtain relatively the same sound-damped path as that on the left-hand side with chamber 38 which has a baffle with only one deflection, but on the other hand a long, straight, sound-damped path.
An essential feature of the present invention is not, therefore, the splitting up into two sound-damped paths, since this could also be achieved in another manner, but generally the fact that long sound-damped paths are obtained in a clamping plate and an associated sound-proofing hood.
It is also important for the success of the soundabsorption measures that the air which enters the annular duct 20 with a large volume, is first of all speeded up very substantially on the deflection baffles, to subsequently be slowed down again in connected expansion chambers. This makes it possible to achieve a wide band sound-damping because all the surfaces which lie in the drawing plane of FIG. 2 are lined with sound-absorption mats.
The sound-damping of the motor cooling air is hereinafter explained with reference to FIG. 1.
In FIG. 1 the air is sucked up by way of the suction opening 42 of FIG. 2, which in FIG. 1 lies approximately in the region underneath this plate. The air flows by way of a relatively broad duct 44 lined with suitable sound-absorption mats into a chamber 45, where it is deflected in direction of arrow 43, and is fed by way of a radially extending duct 46 to the radial fan 4 of the drive motor. Important in this connection is that also the chamber 47 is damped very strongly with sound-absorption mats, so that all surfaces in contact with the cooling air are lined with suitable sound-absorption mats. The fan 4 now sucks up the cooling air, feeds this cooling air by way of the motor windings in the direction of arrow 48, and then this cooling air flows by way of a not further illustrated outlet opening 49 on the motor housing into a chamber 50 and from there in the direction of arrow 6 through an annular duct 51, to then be deflected on wall 52 which is provided with an opening which cannot be noted from FIG. 1. From there the air flows into an annular chamber 53 (direction of arrow 54) which extends practically over 270 degrees of the housing, in which connection it is advantageous when further electronic components of the apparatus are arranged in this annular chamber 53, so that they can be acted upon and cooled by this cooling air. The electronic components consist, for example, of a triac for an automatic switching on and off with an associated suppressor choke and similar parts which produce a considerable amount of waste heat, and which in this manner can be cooled. The air then flows by way of a housing operation 55 shown in FIG. 2 out of the clamping plate. This housing opening 55 lies underneath the horizontal part 56 of the carrier plate 1 and cannot be seen in FIG. 1.
Also here it is important that all the surfaces in contact with the motor cooling air are sound-damped, and the air is deflected a number of times by way of baffles, so that also here there occurs a considerable sound-damping of the motor cooling air.
The sound-absorption mats consist preferably of a foam material or of a closed-pore sponge rubber, a layer of bitumen mats 57 preferably being placed underneath same so as to ensure a wide-band sound-damping.
The housing hood 41 and the clamping plate 18, as well as the bearing plate 56 consist of injection-moulded plastic parts. Also important with the present invention is that on the horizontal part 56 of the carrier plate 1 a channel, open towards the bottom, is arranged extending circumferentially around same, in which duct 58 a U-shaped packing 59 is provided, the edge portion of the vacuum cleaner tank which is open to the top being inserted into and interfitting with the bottom of the U-profile. This ensures a further sound-damping and at the same time a sealing-off and, accordingly, a simultaneous centering of the carrier plate 1 in respect of the vacuum cleaner tank, i.e. there is no contact between solid parts, so that a transmitting of vibrations is avoided.
The sound-absorption measures according to the invention can be produced in an extremely economical manner seeing that all the parts consist of injection-molded parts, which only on the inside have to be provided with suitable sound-absorption measures, i.e. lined with sound-absorption mats and bitumen mats.
It is possible to use additional Helmholtz resonators. Likewise it is possible, as shown in FIG. 3 and FIG. 4, as well as in FIG. 5 and FIG. 6, to arrange either a sound-damper lined with mineral wool, or an absorption or reflection damper (as per FIGS. 5 and 6), in the suction region of the motor, i.e. in the region of the air grating 10 and the suction opening 9. In this case a plug-in collar is arranged flush with the outer edge of the suction opening 9, into which collar the sound-dampers shown in FIGS. 3-6 are plugged-in with their associated collars 60, 61.
FIG. 6 shows the inside member of the sounddamper of FIG. 5. The inside member 62 is inserted axially into the part 63 shown in FIG. 5. The air is sucked up in the direction of arrow 65, deflected through the shackles 66 in the direction of arrow 67, moved downwards in the direction of arrow 68, and is led in the direction of arrow 69 through the inside member 70 of the sound-damper to the suction opening 9 of the carrier plate.
Similar conditions also exist in the case of FIG. 3 where a dampened silencer is used. It is also possible to provide a dampened Helmholtz resonator on the side of the motor cooling air, which preferably is arranged in the region of the annular duct 45. The air does not flow through this duct 45 itself, but as a hollow element the duct is provided in its outer walls with bores of an accurately defined diameter and spacing, leading into the inside, so that the inflowing cooling air is moved along the surface and flows over the edges of these bores, as a result of which a damping effect is obtained.
In the region of the U-shaped sealing lip 59 a narrow strip of copper 71 is arranged, the shape of which is adapted to that of the U-profile and which rests electrically conductive on the metal edge of the vacuum cleaner tank. As shown in FIG. 1, this strip of copper is connected by way of a conductor lug 72 and a connection 73 to the grounded conductor of the mains voltage, so that the electrostatic charges occurring on the vacuum cleaner tank can be led off to the supply main by way of this copper conductor 71.
The soft rubber rings which ensure the low-vibration mounting of the blower and the blower motor, must have a suitable Shore hardness and size and must at the same time be constructed in such a manner that the turbine is prevented from turning round. The dimensions of the air passages and air chambers must also be correctly chosen, essentially as shown in the drawings. Important are the parameters of duct width, duct height and duct length. Also the correct choice of sound-absorption mats and the installation of the mats at the correct places are important. The inlet and outlet cooling air must also be guided, as explained in the foregoing, so that also here the sound level is kept as low as possible.
The invention has been described with reference to its illustrated preferred embodiment. Persons skilled in the art may, upon exposure to the teachings herein, conceive variations in the mechanical development of the components therein. Such variations are deemed to be encompassed by the disclosure, the invention being delimited only by the appended claims.
|
A vacuum cleaner apparatus having separate passages for outgoing air from the blower and for cooling air for the blower motor, and having a number of turns in each of said passages, each of said passages having a plurality of variations in cross-sectional area, the passages being provided with sound-absorbent linings.
| 0
|
CROSS-REFERENCE TO RELATED APPLICATION
This application claims the benefit of Taiwan Patent Application No. 101104498 filed on Feb. 10, 2012, in the Taiwan Intellectual Property Office, the disclosure of which is incorporated herein in its entirety by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a surface modification method, and more particularly to the method of modifying the surface properties of biomolecules and recovering the original status without any harsh treatment, such as strong basic agents, or thermal treatment (more than 37° C.). The invention can be used for functionalization, refunctionalization and rejuvenation of a substrate on a biosensor.
2. Description of Related Art
A biosensor is defined as “a device using a fixed bio-molecule probe and combining a transducer and an electronic device, such that a physical signal can be generated to detect chemical matters inside or outside a living organism, after a specific interaction of the bio-molecule probe and an object to be tested takes place”. For example, a bio-molecule such as an enzyme or an antigen converts a concentration of a chemical matter (such as glucose, potassium ions or cholesterol) into an electronic signal or an optical signal to measure a trace composition. Since the biosensor is usually used in clinic examinations, it has a relatively strict requirement on precision.
A specific bio-molecule probe (with deoxyribonucleic acid, protein, and etc) is fixed onto a substrate surface of the biosensor, not only functionalizing the substrate surface of the biosensor, but also providing the sensitivity and specificity for the test of the biosensor. However, once the bio-molecule probe is fixed onto the substrate surface of the biosensor and coupled to the object to be tested, it is very difficult to regenerate the bio-molecule probe to the original status before the examination takes place. Therefore, most biochips or biosensors are one-time-use disposable devices, which cannot be used repeatedly, such that the price of bio-chips or biosensors is high.
Traditionally, strong acid, strong alkali agents or a high temperature processing biomolecule probes are required to separate the object to be tested on the bio-molecule probe and resume the original un-examined status. However, these measures cause irreversible damage to the bio-molecule probe or electronic device of any biosensor while affecting the precision of the biosensor, so that the biosensor cannot be used repeatedly. In addition, the conventional method of separating an object to be tested on the bio-molecule probe is to use the strong acid, strong alkali or high temperature processing that may damage the substrate surface of the biosensor, so that another bio-molecule cannot functionalize the substrate surface again, and the biosensor cannot be used repeatedly.
In summation, the conventional method of modifying the surface of biomolecules still has the drawbacks of damaging biosensors or electronic devices, reducing the precision of the biosensor, failing to regenerate the biosensor for a repeated use, and incurring a high price, and thus requires further improvements and feasible solutions.
SUMMARY OF THE INVENTION
In view of aforementioned problems of the prior art, it is a primary objective of the invention to provide a method of modifying the surface of biomolecules to overcome the drawbacks of the conventional method of separating an object to be tested on the biomolecule probe that damages the biosensor or electronic device, fails to regenerate the biosensor, and causes low precision and high cost of the biosensor.
To achieve the foregoing objective, the present invention provides a method of modifying the surface of biomolecules, comprising the steps of: providing a bio-molecule combined with at least one single-stranded deoxyribonucleic acid (ssDNA) which is combined with a first protein by an affinity binding tag; adding a second protein having a concentration greater than that of the first protein; and replacing the first protein on at least one of the ssDNA by a second protein through a chemical competitive principle.
Preferably, the biomolecule includes a DNA probe having 18 to 3000 bases.
Preferably, at least one of the ssDNA has 15 to 35 bases.
Preferably, the first protein and the second protein are combined with the affinity binding tag on at least one of the ssDNA through an affinity tag, and a combination between the affinity tag and the affinity binding tag is a reversible combination.
Preferably, the affinity tag includes streptavidin, and the affinity binding tag includes biotin.
Preferably, the first protein and the second protein include alkaline phosphatase or horseradish peroxidase.
Preferably, the biomolecule is applied to a biochip or a biosensor.
To achieve the foregoing objective, the present invention further provides a method of modifying the surface of bio-molecules, with proper design of the biotinylated DNA probes. The functionalized ssDNA nanotemplates can be recovered to its unbound state in mild biological condition, rejuvenation of the bioactive DNA nanotemplate could be achieved by removing the biotinylated DNA probes on the ssDNA nanotemplate by using a recovery DNA.
steps of: providing a bio-molecule combined with at least one first ssDNA, wherein a first free energy (ΔG1) exists between at least one of the first ssDNA and the bio-molecule; adding a recovery ssDNA, wherein a second free energy (ΔG2) exists between the recovery ssDNA and at least one of the first ssDNA, and the second free energy is smaller than the first free energy; and separating at least one of the first ssDNA from the biomolecule and combining at least one of the first ssDNA with the recovery ssDNA through a thermodynamic principle.
Preferably, the bio-molecule includes a DNA probe having 18 to 3000 bases.
Preferably, at least one of the first ssDNA and the second ssDNA have 15 to 35 bases.
Preferably, the first free energy and the second free energy have a negative value.
Preferably, at least one of the first ssDNA is partially complemented with the bio-molecule, and the second ssDNA is wholly complemented with at least one of the first ssDNA.
Preferably, the bio-molecule is applied in a bio-chip or a biosensor.
The method of modifying the surface of bio-molecules of the present invention can replace the original bonded object to be tested and recover the original status of the object to be tested (before it is connected) by adopting the chemical competitive principle or thermodynamic principle at room temperature without using acidic or alkaline chemicals, or can change the chemical properties of the substrate surface of the biosensor. The present invention adds a competitive matter with a higher concentration to replace the original affinity binding to achieve the effect of replacing a matter with a specific function (such as an enzyme) by a matter with the same function or another function to change the original functionality of the substrate surface, so that the original substrate surface is regenerated. On the other hand, the present invention is also applicable for the principle of complementing paired DNAs by using a thermal stable recovery DNA, so that the originally combined object to be tested and the paired double-stranded DNA to resume the original ssDNA probe to regenerate the DNA probe.
In summation, the method of modifying the surface of bio-molecules of the present invention has one or more of the following advantages:
(1) The method of modifying the surface of biomolecules of the present invention is applicable for substrate surfaces of various different biosensors and bio-chips, and users can use the same set of biosensor for testing and maintaining the precision of signals and the specificity of the object to be tested.
(2) The method of modifying the surface of biomolecules of the present invention does not require any strong acid, strong alkali or high temperature for the reaction, but the reaction can take place at room temperature, so that the substrate surface of the biosensor and the electronic device will not be damaged, and the original chemical properties of the substrate surface can be maintained.
(3) The method of modifying the surface of bio-molecules of the present invention can replace the ssDNA for more than 90%, the enzyme for more than 83%, so that the substrate surface of the biosensor can be regenerated, and the regenerated surface can be modified.
(4) The method of modifying the surface of biomolecules of the present invention can regenerate the biosensor and the biochip and modify the regenerated surface, so that the biosensor and biochip can be used repeatedly to lower the examination and fabrication cost of biosensors and biochip.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a flow chart of a method of modifying the surface of a bio-molecule probe in accordance with a first preferred embodiment of the present invention;
FIG. 2 is a schematic view of a method of modifying the surface of bio-molecules in accordance with the first preferred embodiment of the present invention;
FIG. 3 is a flow chart of a method of modifying the surface of a bio-molecule probe in accordance with a second preferred embodiment of the present invention;
FIG. 4 is a schematic view of a method of modifying the surface of bio-molecules in accordance with the second preferred embodiment of the present invention;
FIG. 5A is an enzyme activity graph of a first example of a method of modifying the surface of bio-molecules in accordance with a first preferred embodiment of the present invention;
FIG. 5B is an enzyme activity graph of a second example of a method of modifying the surface of bio-molecules in accordance with the first preferred embodiment of the present invention; and
FIG. 6 is an enzyme activity graph of a method of modifying the surface of bio-molecules in accordance with a second preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The technical contents and characteristics of the present invention will be apparent with the detailed description of a preferred embodiment accompanied with related drawings as follows. For simplicity, same numerals are used in the following preferred embodiment to represent respective same elements.
Embodiment 1
Regeneration of the DNA Probe
With reference to FIGS. 1 and 2 for a flow chart and a schematic view of a method of modifying the surface of bio-molecules in accordance with the first preferred embodiment of the present invention respectively, the method of modifying the surface of bio-molecules comprises the following steps:
S 11 : Provide a bio-molecule combined with at least one ssDNA which is combined with a first protein through an affinity binding tag.
S 12 : Add a second protein with a concentration greater than that of the first protein.
S 13 : Replace the first protein on at least one ssDNA by a second protein through a chemical competitive principle.
In an example of this preferred embodiment, the bio-molecule 11 can be one selected from the collection of deoxyribonucleic acid (DNA), enzyme, antigen, receptors) and any bio-molecule applied in a biosensor or a bio-chip, and the present invention uses ssDNA as a DNA probe, and the DNA probe of the present invention has a length of 18 to 3000 bases, and preferably 500 to 2500 bases, but the invention is not limited to these numbers of bases only.
In an example of this preferred embodiment, the first protein 13 and the second protein 14 can be combined onto an affinity binding tag 16 of at least one ssDNA through an affinity tag 15 , and the affinity tag 15 and the affinity binding tag 16 are paired for their use. For example, biotin-streptavidin, (His tag-Ni2+), glutathione-S-transferase tag-glutathione can be paired, and other suitable pairs of the affinity tag 15 and the affinity binding tag 16 can be used according to the experiment requirements and conditions. In this embodiment of the invention, the affinity tag 15 is streptavidin, and the affinity binding tag 16 is biotin, but the invention is not limited to such arrangement only.
Wherein, the combination of the affinity tag 15 and the affinity binding tag 16 is a reversible combination. For example Protein A and Protein B are labeled as the affinity tag 15 and the affinity binding tag 16 respectively. If the Protein A and Protein B are combined through the affinity tag 15 and the affinity binding tag 16 , a high-concentration Protein C with a labeled affinity tag 15 can be used to replace the combination of Protein A and Protein B with the affinity tag 15 . Now, the combination of the affinity tag 15 and the affinity binding tag 16 is a reversible combination.
In an example of this preferred embodiment, the ssDNA 12 can be designed in any sequence according to the DNA probe, and the present invention adopts the ssDNA 12 with the sequence identification number: 1 as an example, and biotin is modified at an end 5′.
In an example of this preferred embodiment, the first protein 13 and the second protein 14 can be enzymes, antigens, or protein of the same or different types. In this embodiment of the present invention, the first protein 13 and the second protein 14 are different enzymes, wherein the first protein 13 is alkaline phosphatase, and the second protein 14 is horseradish peroxidase. In another example of this preferred embodiment, the first protein 13 is horseradish peroxidase, and the second protein 14 is alkaline phosphatase, but the invention is not limited to these arrangements only.
In addition, the bio-molecule used in the method of modifying the surface of bio-molecules of the present invention can be applied to various bio-chips or biosensors including but not limited to blood glucose meters, lipid meters, and micro array bio-chips.
Embodiment 2
Method of Regenerating the DNA Probe
With reference to FIGS. 3 and 4 for a flow chart and a schematic view of a method of modifying the surface of bio-molecules in accordance with the second preferred embodiment of the present invention respectively, the method of modifying the surface of bio-molecules comprises the following steps:
S 21 : Provide a bio-molecule combined with at least one first ssDNA, wherein first free energy (ΔG1) exists between the first ssDNA and the bio-molecule.
S 22 : Add a second ssDNA, as a recovery DNA, wherein a second free energy (ΔG2) exists between the second ssDNA and the first ssDNA, and the second free energy is smaller than the first free energy,
S 23 : Separate the first ssDNA from the bio-molecule and combine the first ssDNA with the second ssDNA through the thermodynamic principle.
In an example of this preferred embodiment, the bio-molecule 21 is one selected from the collection of deoxyribonucleic acid, enzyme, antigen and any bio-molecule applied in a biosensor or a bio-chip, and this embodiment of the present invention uses the ssDNA as the DNA probe, wherein the DNA probe has a length of 18 to 3000 bases and preferably 500 to 2500 bases, but the invention is not limited to such length only.
In an example of this preferred embodiment, this embodiment uses 21 bases as an example and prevents the ssDNA from producing a first ssDNA 22 and a second ssDNA 23 having a length of 12 to 40 bases, and preferably 15 to 35 bases, wherein the first ssDNA 22 of the sequence identification number: 2 is partially complemented with the DNA probe by 15 bases close to the end 5′, and 6 bases are extended from the end 3′, and the first ssDNA 22 has biotin modified at the end 3′. In addition, the second ssDNA 23 of the sequence identification number: 3 is wholly complemented with the first ssDNA 22 of the sequence identification number: 2.
In an example of this preferred embodiment, the first free energy (ΔG1) and the second free energy (ΔG2) have a negative value. Preferably, the first free energy (ΔG1) and the second free energy (ΔG2) are equal to −15.94 kcal/mL and −22.72 kcal/mL respectively in this preferred embodiment.
In addition, the bio-molecules used in the method of modifying the surface of bio-molecules of the present invention can be applied to various different bio-chips or biosensors such as blood glucose meters, lipid meters, and micro-array bio-chips, but the invention is not limited to such arrangement only.
Embodiment 3
Preferred Embodiment of the Present Invention
To allow persons ordinarily skilled in the art to implement the present invention, the following preferred embodiments are used to elaborate the present invention. It is noteworthy to point out that all parameters and chemical agents used in the embodiments are provided for the purpose of illustrating the present invention, but not intended for limiting the scope of the present invention.
Regeneration of DNA Probe
Add and react the ssDNA of the sequence identification number: 1 (with the quantity of 1.3 μM and having biotin modified at the end 5′) with the DNA probe, so that the ssDNA is combined with the DNA probe. Wash the compound by a phosphoric acid washing buffer. Add 150 μL of bovine serum albumin (BSA) to block the unbound area on the surface. Use 300 μL of washing buffer to rinse the compound for three times to wash away extra bovine serum albumin (BSA). Add 70 μL of streptavidin-alkaline phosphatase solution or streptavidin-horseradish peroxidase solution (5 nM), and allow the reaction to take place at 25° C. for 45 minutes, so that the alkaline phosphatase or horseradish peroxidase is connected to the DNA probe to functionalize the DNA probe. Use 300 μL of washing buffer to wash the compound for three times to wash away extra testing agent, enzyme and DNA.
Add streptavidin-horseradish peroxidase (0, 3.5, 17.5, 350 nM) or streptavidin-alkaline phosphatase (0, 7, 35, 700 nM) with different concentrations into the DNA probes connected with streptavidin-alkaline phosphatase or streptavidin-horseradish peroxidase respectively to compete for the biotin binding site, so as to replace the streptavidin-alkaline phosphatase or streptavidin-horseradish peroxidase originally combined with the DNA probe.
To confirm that the tested enzyme activity comes from the functionalized DNA probe, a tangent point of an enzyme HindIII is designed at an end where the DNA probe and the substrate surface are connected. After the enzyme HindIII is added for the reaction, the DNA probe can be removed, and then 20 units of restriction enzyme HindIII are used for the reaction taken place at 37° C. for 50 minutes to remove the DNA probe and the enzyme combined with the DNA probe.
Regeneration of the DNA Probe
Add and react the first ssDNA of the sequence identification number: 2 (with the quantity of 1.3 μM and having biotin modified at the end 3′) with the DNA probe, so that the ssDNA is combined with the DNA probe.
Wash the compound by a phosphoric acid washing buffer. Add 150 μL of bovine serum albumin (BSA) to perform a blocking. Use 300 μL of washing buffer to rinse the compound for three times to wash away extra bovine serum albumin (BSA). Add 70 μL of streptavidin-horseradish peroxidase, so that the streptavidin-horseradish peroxidase is combined with the DNA probe through the biotin of the first ssDNA to functionalize the DNA probe, and use it as an indication of a separation from the first ssDNA probe.
In order to remove the first ssDNA probe from the DNA probe and regenerate the DNA probe, a second ssDNA (sequence identification number: 3) wholly complemented with the first ssDNA is designed, and 100 μL of the second ssDNA (0, 1, 2, 3 μM) with different concentrations are added to allow a reaction to take place at 37° C. for 60 minutes to complete with the DNA probe and combined with the first ssDNA.
Testing the Enzyme Activity
After the functionalized DNA probe is washed by 300 μL of the washing buffer, the enzyme activity is tested. When the activity of the horseradish peroxidase is tested, 150 μL of tetramethylbenzidine solution are added. After an incubation takes place at 25° C. for 10 minutes, the 100 μL of reacted tetramethylbenzidine solution is removed and added into a 96-well microtiter plate, and a Victor multilabel counter (by Perkin-Elmer Life Science, Inc.; USA) is used to measure the light absorbance value of the wavelength 650 nm. When the activity of the alkaline phosphatase is measured, 150 μL of P-nitrophenyl phosphate (Sigma) are added. After incubation has taken place at 25° C. for 30 minutes, the Victor multilabel counter is used to measure the light absorbance value of the wavelength 405 nm.
Experiment Results
1. Generation of the DNA Probe
With reference to FIGS. 5A and 5B for enzyme activity graphs of the first and second examples of a method of modifying the surface of bio-molecules in accordance with the first preferred embodiment of the present invention respectively, FIG. 5A shows that the functionalized DNA probe with the horseradish peroxidase combined with the streptavidin-horseradish peroxidase on the DNA probe is gradually replaced by the streptavidin-alkaline phosphatase. More specifically, under the competition of 700 nM of streptavidin-alkaline phosphatase, approximately 83% of the streptavidin-horseradish peroxidase combined with the DNA probe are gradually replaced by the streptavidin-alkaline phosphatase. In other words, the original 0.81 mU (1.63 fmole) of horseradish peroxidase is combined with the DNA probe. After alkaline phosphatase is added, approximately 0.05 mU (0.17 fmole) of alkaline phosphatase replaces the horseradish peroxidase and combines with the DNA probe. Further, alkaline phosphatase with different concentrations is added for the competition, the measured horseradish peroxidase enzyme activity is reduced gradually by the concentration dependent method, and the alkaline phosphatase enzyme activity is gradually increased by the concentration dependent method. In other words, the streptavidin-alkaline phosphatase and the streptavidin-horseradish peroxidase compete with each other to combine with the labeled biotin of the ssDNA.
Similarly, the original functionalized DNA probe with the alkaline phosphatase combined with the streptavidin-alkaline phosphatase on the DNA probe is gradually replaced by streptavidin-horseradish peroxidase as shown in FIG. 5B . More specifically, after 350 nM of streptavidin-alkaline phosphatase are added for the competition, approximately 88% of streptavidin-alkaline phosphatase combined onto the DNA probe is replaced by the streptavidin-horseradish peroxidase. In other words, the original 0.04 mU (0.15 fmole) of alkaline phosphatase is combined onto the DNA probe. After the horseradish peroxidase is added, approximately 1.71 mU (3.43 fmole) of horseradish peroxidase replaces the alkaline phosphatase and combines onto the DNA probe. After the horseradish peroxidase of different concentrations is added for the competition, the measured alkaline phosphatase enzyme activity is gradually reduced by the concentration dependent method, and the horseradish peroxidase enzyme activity is gradually increased by the concentration dependent method. In other words, streptavidin-alkaline phosphatase and streptavidin-horseradish peroxidase compete with each other and combine with the biotin labeled on the ssDNA.
In FIG. 5B , the restriction enzyme HindIII is added to cut off the DNA probe in order to confirm that the measured enzyme activity comes from the enzyme combined to the DNA probe. After the HindIII is added to cut off the DNA probe, the originally measured horseradish peroxidase enzyme activity is almost eliminated, indicating that the measured horseradish peroxidase activity comes from the horseradish peroxidase combined with the DNA probe.
2. Regeneration of the DNA Probe
With reference to FIG. 6 for an enzyme activity graph of a method of modifying the surface of bio-molecules in accordance with a second preferred embodiment of the present invention, the measured horseradish peroxidase enzyme activity of the DNA probe becomes increasingly smaller as the concentration of the added second ssDNA increases. In the other words, the first ssDNA having the horseradish peroxidase enzyme activity and originally combined with the DNA probe is separated from the DNA probe, after the second ssDNA is added. More specifically, the first ssDNA and the DNA probe have a first free energy (ΔG1) −15.94 kcal/mL, and the first ssDNA and the second ssDNA have a second free energy (ΔG2) −22.72 kcal/mL. According to the thermodynamic principle, the first ssDNA tends to combine with the second ssDNA and separate from the DNA probe, so that the measured horseradish peroxidase enzyme activity of the DNA probe becomes gradually less and less.
In summation of the description above, the present invention breaks through the prior art to achieve the expected objectives and complies with the patent application requirements, and thus is duly filed for patent application.
|
A method that modifies surface properties of a substrate by manipulating the immobilized biomolecules in mild biological condition. The manipulation comprised steps of: providing a biomolecule combined with at least one ssDNA combined with a first protein through an affinity binding tag; adding a second ssDNA conjugated with a second protein with a concentration greater than that of the first protein; and replacing the first protein on the ssDNA with the second protein through chemical competitive principle. The invention may comprise the steps with proper design of biotinylated DNA probes, the functionalized ssDNA nanotemplates can be recovered to its unbound state through a thermodynamic principle.
| 2
|
BACKGROUND OF THE INVENTION
[0001] An end cap device, in particular for a wiper blade, having an end cap base member which can be securely connected to at least one main component of a wiper blade, has already been proposed.
SUMMARY OF INVENTION
[0002] The invention is based on an end cap device, in particular for a wiper blade, having an end cap base member which can be securely connected to at least one main component of a wiper blade.
[0003] It is proposed that the end cap device comprise at least one end cap spoiler element which is provided to release an assembly opening for a wiper arm in an assembly configuration. A wiper lip of the wiper blade can thereby advantageously be replaced in a simple manner. In a further advantageous manner, aerodynamic disturbances of the end cap device, in particular during travel operation, can be prevented. The term “main component” is intended in this context in particular to be understood to be at least one resilient rail, a wind deflection element and/or a retention element. The term “resilient rail” is intended in particular to be understood to be a macroscopic element which has at least one extent which can be resiliently changed in a normal operating state by at least 10%, in particular by at least 20%, preferably by at least 30% and, in a particularly advantageous manner, by at least 50%, and which in particular produces a counter-force which is dependent on a change of the extent and which is preferably proportional to the change and which counteracts the change. Preferably, the resilient rail is at least partially formed from a spring steel. In an unloaded state, the resilient rail is preferably substantially in the form of a bent rod and, in a particularly advantageous manner, a flattened bent rod. In a particularly advantageous manner, a curvature of the resilient rail along a longitudinal extent in an unloaded state is greater than a curvature of a vehicle surface of a motor vehicle, in particular a motor vehicle window, by means of which the resilient rail is guided in at least one operating state. The term “extent” of an element is intended in particular to be understood to be a maximum spacing between two points of a perpendicular projection of the element on a plane. The term “macroscopic element” is intended in particular to be understood to be an element with an extent of at least 1 mm, in particular at least 5 mm, and preferably at least 10 mm.
[0004] The term “wiper blade” is intended in particular to be understood to be a unit of a resilient material having a wiper lip which is provided, in order to clean a surface which is intended to be cleaned, in particular a window surface, preferably of a vehicle window, to be moved in contact over the surface to be cleaned. Preferably, the wiper blade is produced from a natural or synthetic elastomer material, in particular rubber. The term “wind deflection element” is intended in this context in particular to be understood to be an element which is provided to deflect a travel wind which acts on the wiper blade and/or to use it for pressing the wiper blade onto a vehicle window. Preferably, the wind deflection element has at least one concave wind deflection face. In particular, the wind deflection element is constructed to be different from a wiper blade adapter and/or an end cap. The term “retention element” is intended in this context to refer in particular to an element which is provided to retain a resilient rail. Preferably, the retention element is formed by an extruded member, in particular of plastics material.
[0005] The term “end cap spoiler element” is intended in this context in particular to be understood to refer to an element of an end cap which in at least one operating state is provided for an aerodynamic production of a pressing force of the end cap device, in particular in the direction of a vehicle window. Preferably, the at least one end cap spoiler element has at least one substantially concave-curved main flow face. The main flow face is in particular provided to deflect an incoming air flow. Preferably, the at least one end cap spoiler element has at least a first face which in at least one operating state extends at least substantially parallel with a vehicle window. In a further advantageous manner, the at least one end cap spoiler element has at least a second face which in at least one operating state extends at least substantially perpendicularly to the vehicle window. The second face is preferably smooth in this instance, in particular free from corrugation. The term “at least substantially” is in this context intended in particular to be understood to be an angular deviation of less than 15°, preferably less than 10°, in a particularly preferred manner less than 5°, in a quite particularly preferred manner less than 2°. The term “can be securely connected” is intended in this context in particular to be understood to be able to be connected in a non-detachable and/or non-releasable manner. The term “connected in a non-releasable manner” is intended in this context in particular to be understood to mean that destruction-free separation is prevented.
[0006] The term “assembly configuration” is intended in this context to be understood in particular to be a configuration of the end cap device in which a wiper arm can be assembled and/or disassembled. In particular, the wiper blade in the assembly configuration can be pulled out of and/or pushed into a wiper blade. The term “assembly opening” is intended in this context to refer in particular to an opening, in particular a gap, through which the wiper arm can be guided during assembly and/or disassembly. Preferably, the assembly opening opens the end cap device in a longitudinal direction. The term “longitudinal direction” in this context is intended to be understood in particular to be a direction which extends at least substantially parallel with a main longitudinal extent of the end cap device and/or at least substantially parallel with a main longitudinal extent of the wiper arm. The term “provided” is intended in particular to be understood to be specifically configured and/or equipped. The fact that an object is provided for a specific function is intended in particular to be understood to mean that the object performs and/or carries out this specific function in at least one application and/or operating state.
[0007] In another embodiment of the invention, it is proposed that the at least one end cap spoiler element be movably supported on the end cap base member, whereby a particularly simple production of the assembly configuration can be achieved.
[0008] It is further proposed that the at least one end cap spoiler element be displaceably supported on the end cap base member, whereby a movement which may be obtained in a particularly simple and intuitive manner in respect of the at least one end cap spoiler element can be achieved. Preferably, the at least one end cap spoiler element is displaceably supported on the end cap base member in a wiping direction. In an additional and/or alternative embodiment, it is proposed that the at least one end cap spoiler element be pivotably supported on the end cap base member.
[0009] It is further proposed that the at least one end cap spoiler element have an opening direction which is directed from the end cap base member at least partially toward a leeward side. Preferably, the at least one end cap spoiler element can be opened at least partially in the opening direction. The term “opening direction” in this context is intended to be understood in particular to be a direction in which the at least one end cap spoiler element is constructed so as to be able to be at least partially displaced relative to the end cap base member in order to produce an opening. Preferably, this is intended in particular to be understood to be a direction in which the end cap spoiler element can be displaced from a position mounted on the end cap base member relative to the end cap base member, in particular is displaced at least substantially in the direction toward an opening. In a particularly preferred manner, this is intended in particular to be understood to be a direction which extends at least substantially parallel with a translation axis of the displacement movement of the end cap spoiler element relative to the end cap base member. The fact that the opening direction “is directed in the direction toward a leeward side” is intended in particular to be understood to mean that the opening direction is directed from the end cap base member in the direction of a leeward side of the end cap device. Preferably, this is intended in particular to be understood to mean that the opening direction corresponds to a wiping direction of the wiper blade during a movement with the wind, that is to say, in particular during an upward movement. In this instance, the term “leeward side” is in this context intended in particular to be understood to be a side facing away from the wind, in particular a side facing away from the travel wind. This is preferably intended in particular to be understood to be a side facing away from the wind, in particular a side facing away from the travel wind, of the end cap device and/or in particular the wiper blade. Furthermore, the term “wiper direction” is intended in particular to be understood in this instance to be a tangential direction in which the wiper blade is guided in an operating state over a vehicle window which is intended to be wiped. It is thereby possible in particular to achieve an advantageously comfortable opening of the end cap spoiler element. Furthermore, it is thereby possible to provide a movement which may be obtained in a simple and intuitive manner in respect of the at least one end cap spoiler element.
[0010] It is further proposed that the at least one end cap spoiler element have an opening direction, which is directed from the end cap base member at least partially toward a windward side. The fact that the opening direction “is directed toward a windward side” is intended in particular to be understood to mean that the opening direction is directed from the end cap base member in the direction of a windward side of the end cap device. This is preferably intended in particular to be understood to mean that the opening direction corresponds to a wiper direction of the wiper blade during a movement against the wind, that is to say, in particular during a downward movement. In this instance, a “windward side” in this context is intended in particular to be understood to be a side facing the wind, in particular a side facing the travel wind. This is preferably intended in particular to be understood to be a side facing the wind, in particular a side facing the travel wind, of the end cap device and/or in particular the wiper blade. It is thereby possible to achieve in particular an advantageously comfortable opening of the end cap spoiler element. Preferably, it is thereby possible to prevent undesirable release of the end cap spoiler element from the end cap base member, which release is caused by the travel wind. In particular, it is thus possible to achieve, as a result of a pressing force caused by the travel wind, additional retention of the end cap spoiler element on the end cap base member.
[0011] A particularly reliable and rapid securing of the at least one end cap spoiler element can be achieved when the end cap device comprises a catch unit, which is provided to engage the at least one end cap spoiler element on the end cap base member in an operating configuration. The term “catch unit” in this context is intended in particular to be understood to be a unit which has at least one catch hook, which is provided during a locking operation to be redirected from a starting position in a resilient manner and, when a locking position is reached, moves in a resilient manner at least partially back into the starting position.
[0012] If the catch unit comprises at least one catch hook which is constructed integrally with the at least one end cap spoiler element, a locking of the at least one end cap spoiler element can be achieved, which locking is particularly cost-effective to produce and stable.
[0013] It is further proposed that the end cap device have an operating unit which is provided to move the catch unit into a release configuration. It is thereby possible for an operator to release the catch unit in a particularly simple manner without the use of tools. The term “release configuration” is intended in this context in particular to be understood to be a configuration in which the at least one end cap spoiler element can be moved, in particular displaced, in order to release the assembly opening.
[0014] It is further proposed that the operating unit comprise at least one operating element which is constructed integrally with the at least one end cap spoiler element. The operating element can thereby be produced in a particularly cost-effective manner. Preferably, the operating unit has at least one corrugated operating region. In a particularly preferred manner, the corrugated operating region extends on a face which extends at least substantially parallel with a vehicle window to be wiped.
[0015] If the end cap device has a limitation unit which is provided to limit a movement freedom of the at least one end cap spoiler element in an assembly configuration in an opening direction, the at least one end cap spoiler element can advantageously be prevented from falling off the end cap base member and/or becoming lost.
[0016] The end cap device can be constructed in an aerodynamically advantageous manner when the at least one end cap spoiler element has at least partially a flush surface extent with respect to the end cap base member. The term “flush” is intended in this context in particular to be understood to be offset-free, smooth and/or without edges.
[0017] A system having a wiper blade and an end cap device according to the invention is further proposed.
[0018] Furthermore, a method for releasing an assembly opening of an end cap base member is proposed, wherein at least one end cap spoiler element is moved relative to the end cap base member.
[0019] The end cap device according to the invention is in this instance not intended to be limited to the above-described application and embodiment. In particular, the end cap device according to the invention may have, in order to carry out an operating method described herein, a number which differs from a number mentioned herein of individual elements, components and units.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Other advantages will be appreciated from the following description of the drawings. In the drawings, two embodiments of the invention are illustrated. The drawings, the description and the claims contain a number of features in combination. The person skilled in the art will advantageously also consider the features individually and combine them to form other advantageous combinations.
[0021] In the drawings:
[0022] FIG. 1 is a perspective view of a wiper blade with an end cap device according to the invention,
[0023] FIG. 2 is a perspective view of an end cap base member of the end cap device according to the invention according to FIG. 1 ,
[0024] FIG. 3 is another perspective view of an end cap base member of the end cap device according to the invention according to FIG. 1 ,
[0025] FIG. 4 is a perspective view of an end cap spoiler element of the end cap device according to the invention according to FIG. 1 ,
[0026] FIG. 5 is another perspective view of an end cap spoiler element of the end cap device according to the invention according to FIG. 1 ,
[0027] FIG. 6 is a sectioned illustration through VI-VI of a system having a wiper blade and the end cap device,
[0028] FIG. 7 is a perspective illustration of the system according to FIG. 6 in an assembly configuration,
[0029] FIG. 8 is another perspective view of the system according to FIG. 6 in an assembly configuration,
[0030] FIG. 9 is a perspective view of a wiper blade with an alternative end cap device according to the invention,
[0031] FIG. 10 is a perspective view of a system having a wiper blade and the alternative end cap device according to the invention in an assembly configuration,
[0032] FIG. 11 is a perspective view of an end cap base member of the alternative end cap device according to the invention,
[0033] FIG. 12 is a perspective view of an end cap spoiler element of the alternative end cap device according to the invention,
[0034] FIG. 13 is a schematic partially sectioned illustration of the system with the wiper blade and the alternative end cap device according to the invention in an operating configuration, and
[0035] FIG. 14 is a schematic illustration of the system with the wiper blade and the alternative end cap device according to the invention in another assembly configuration.
DETAILED DESCRIPTION
[0036] FIG. 1 shows a wiper blade 12 a and an end cap device for the wiper blade 12 a. The wiper blade 12 a is provided for wiping a vehicle window, in particular a vehicle window of a motor vehicle. The end cap device is provided to close the wiper blade 12 a in a longitudinal direction 38 a. Furthermore, the end cap device is provided to retain a wiper arm 20 a of the wiper blade 12 a in a secure position in an operating state. The wiper arm 20 a is produced from a resilient material, in particular from rubber. Furthermore, the wiper arm 20 a has a wiper lip 58 a . The wiper lip 58 a is provided for cleaning a vehicle window.
[0037] The end cap device has an end cap base member 14 a. The end cap base member 14 a is securely connected to a main component 10 a of the wiper blade 12 a. The main component 10 a is formed by means of two resilient rails 36 a which extend parallel with each other. The resilient rails 36 a are constructed from a spring steel. In the embodiment shown, the end cap base member 14 a is securely connected to at least one resilient rail 36 a. More specifically, the end cap base member 14 a is connected to the resilient rail 36 a in a non-releasable manner. However, in this context it is also conceivable for the end cap base member 14 a to be securely connected to a wind deflection element 40 a of the wiper blade 12 a. The end cap base member 14 a is at least substantially formed from plastics material. The end cap base member 14 a has a spoiler attachment 42 a. The spoiler attachment 42 a is provided to deflect travel wind and to produce a pressing pressure in the direction of a vehicle window. The spoiler attachment 42 a is arranged at a side of the end cap base member 14 a facing away from the vehicle window.
[0038] Furthermore, the end cap device comprises an end cap spoiler element 16 a. The spoiler attachment 42 a merges with a wind flow face 44 a in a flush manner into the end cap spoiler element 16 a. The end cap spoiler element 16 a has in this instance a flush surface extent with respect to the end cap base member 14 a. The end cap spoiler element 16 a comprises a single component. However, it is also conceivable in principle for the end cap spoiler element 16 a to comprise a plurality of components, in particular to be constructed in two parts. The end cap spoiler element 16 a is connected to the end cap base member 14 a in a non-releasable manner.
[0039] The end cap base member 14 a is illustrated in greater detail in FIGS. 2 and 3 . The end cap base member 14 a has at least one guiding rail 46 a, 48 a which is provided for movable support of the end cap spoiler element 16 a. More specifically, the end cap base member 14 a has two guiding rails 46 a, 48 a which are provided for movable support of the end cap spoiler element 16 a. The end cap spoiler element 16 a is consequently movably supported on the end cap base member 14 a. The guiding rails 46 a, 48 a extend at least substantially parallel with a wiping direction 22 a. The wiping direction 22 a extends in this instance perpendicularly to the longitudinal direction 38 a. Consequently, the end cap spoiler element 16 a is displaceably supported on the end cap base member 14 a. More specifically, the end cap spoiler element 16 a is displaceably supported on the end cap base member 14 a in the wiping direction 22 a. The end cap spoiler element 16 a has an opening direction 34 b. The end cap spoiler element 16 a can be opened partially in the opening direction 34 a. The opening direction 34 a extends parallel with the wiping direction 22 a. The opening direction 34 a is the direction in which the end cap spoiler element 16 a can be displaced from an operating configuration in a state supported on the end cap base member 14 a into an assembly configuration. The opening direction 34 a is directed from the end cap base member 14 a toward a leeward side. The opening direction 34 a is directed from the end cap base member 14 a toward a side facing away from the wind, in particular a side facing away from travel wind. The end cap spoiler element 16 a is closed counter to the opening direction, that is to say, pushed into an operating configuration on the end cap base member 14 a . The end cap base member 14 a further has a barb 52 a. The barb 52 a is constructed integrally with the end cap base member 14 a, in particular with the spoiler attachment 42 a.
[0040] The end cap spoiler element 16 a is shown in greater detail in FIGS. 4 and 5 . The end cap spoiler element 16 a aerodynamically produces in an operating state a pressing pressure of the end cap device in the direction of the vehicle window. Preferably, the end cap spoiler element 16 a has a main flow face 54 a which is curved in a concave manner. The end cap spoiler element 16 a has a closure wall 56 a. The closure wall 56 a extends at least substantially perpendicularly relative to the longitudinal direction 38 a. The closure wall 56 a forms a closure of the end cap device in the longitudinal direction 38 a. Furthermore, the closure wall 56 a closes an assembly opening 18 a in an operating state. In an assembly configuration, the wiper arm 20 a can be guided through the assembly opening 18 a.
[0041] The end cap device comprises a catch unit 24 a which is provided to engage the end cap spoiler element 16 a in an operating configuration on the end cap base member 14 a. The catch unit 24 a has to this end a catch hook 26 a which is constructed integrally with the end cap spoiler element 16 a. The catch hook 26 a is provided to be redirected in a resilient manner from a starting position during a locking operation. More specifically, the catch hook 26 a is resiliently redirected by the barb 52 a during the locking operation. When a locking position is reached, the catch hook 26 a moves resiliently back into the starting position. In this instance, the catch hook 26 a engages with the barb 52 a and prevents movement of the end cap spoiler element 16 a relative to the end cap base member 14 a.
[0042] The end cap device further has an operating unit 28 a which is provided to move the catch unit 24 a into a release configuration. The operating unit 28 a comprises an operating element 30 a. The operating element 30 a is constructed integrally with the end cap spoiler element 16 a. The operating element 30 a is constructed integrally with the catch hook 26 a. The operating element 30 a can be resiliently redirected by hand. When the operating element 30 a is redirected, the catch hook 26 a is released by the barb 52 a. The end cap spoiler element 16 a can subsequently be displaced along the guiding rails 46 a, 48 a between an operating configuration and the assembly configuration. The end cap spoiler element 16 a can subsequently be displaced in an opening direction 34 a along the guiding rails 46 a, 48 a between an operating configuration and the assembly configuration. The end cap spoiler element 16 a is consequently provided to release the assembly opening 18 a for the wiper arm 20 a in an assembly configuration.
[0043] As shown in FIG. 6 , the end cap device additionally has a limitation unit 32 a. The limitation unit 32 a is provided to limit a movement freedom of the end cap spoiler element 16 a in the assembly configuration in the opening direction 34 a. The limitation unit 32 a comprises a stop element 50 a. The stop element 50 a is constructed integrally with the end cap base member 14 a. The stop element 50 a is constructed in a plate-like manner. The stop element 50 a has in this instance a stop face 60 a which extends at least substantially perpendicularly relative to the wiping direction 22 a. In the assembly configuration, the catch hook 26 a abuts the stop element 50 a, in particular the stop face 60 a.
[0044] FIG. 7 shows the wiper blade 12 a and the end cap device in the assembly configuration. In the assembly configuration, the wiper arm 20 a can be assembled or disassembled ( FIG. 8 ). The wiper arm 20 a can in this instance be pulled out of or pushed into a wiper blade 12 a. The assembly opening 18 a is produced by means of a gap between the end cap base member 14 a and the closure wall 56 a of the end cap spoiler element 16 a in the assembly configuration.
[0045] In order to exchange the wiper blade 20 a, in a first disassembly step, the operating element 30 a is redirected manually. The end cap device is thereby moved from an operating configuration into a release configuration. In the release configuration, the catch unit 24 a releases a movement freedom of the end cap spoiler element 16 a relative to the end cap base member 14 a. In a second disassembly step, the end cap spoiler element 16 a is moved in the opening direction 34 a until it strikes the stop element 50 a. Consequently, the end cap spoiler element 16 a is moved relative to the end cap base member 14 a. In the second disassembly step, the assembly opening 18 a is released. In a third disassembly step, the wiper arm 20 a is pulled out of the wiper blade 12 a through the assembly opening 18 a in a displacement direction 62 a. The displacement direction 62 a extends at least substantially parallel with the longitudinal direction 38 a. Subsequently, a new wiper arm is pushed in a first assembly step through the assembly opening 18 a into the wiper blade 12 a. In a second assembly step, the end cap spoiler element 16 a is moved counter to the opening direction 34 a until the catch unit 24 a engages the end cap base member 14 a and the end cap spoiler element 16 a with each other. Consequently, the end cap device is moved back into the operating configuration.
[0046] In FIGS. 9 to 14 , another embodiment of the invention is shown. The following descriptions are substantially limited to the differences between the embodiments, wherein, with respect to components, features and functions which remain the same, reference may be made to the description of the embodiment of FIGS. 1 to 8 . In order to differentiate the embodiments, the letter a in the reference numerals of the embodiment in FIGS. 1 to 8 is replaced by the letter b in the reference numerals of the embodiment of FIGS. 9 to 14 . With regard to components which remain the same, in particular with regard to components with the same reference numerals, it is in principle also possible to refer to the drawings and/or the description of the embodiment of FIGS. 1 to 8 .
[0047] FIG. 9 shows a wiper blade 12 b and an end cap device for the wiper blade 12 b. The wiper blade 12 b is provided for wiping a vehicle window, in particular a vehicle window of a motor vehicle. The end cap device is provided to close the wiper blade 12 b in a longitudinal direction 38 b. Furthermore, the end cap device is provided to retain a wiper arm 20 b of the wiper blade 12 b in a fixed position in an operating state.
[0048] The end cap device has an end cap base member 14 b. The end cap base member 14 b is securely connected to a main component 10 b of the wiper blade 12 b. The main component 10 b is formed by means of two resilient rails 36 b which extend parallel with each other. Furthermore, the end cap device comprises an end cap spoiler element 16 b. The spoiler attachment 42 b merges with a wind flow face 44 b in a flush manner in the end cap spoiler element 16 b. The end cap spoiler element 16 b in this instance has a flush surface extent with respect to the end cap base member 14 b. The end cap spoiler element 16 b is connected to the end cap base member 14 b in a non-releasable manner.
[0049] The end cap base member 14 b is illustrated in greater detail in FIG. 11 . The end cap base member 14 b has at least one guiding rail 46 b, 48 b which is provided to movably support the end cap spoiler element 16 b. More specifically, the end cap base member 14 b has two guiding rails 46 b, 48 b which are provided to movably support the end cap spoiler element 16 b. The end cap spoiler element 16 b is consequently movably supported on the end cap base member 14 b . The guiding rails 46 b, 48 b extend at least substantially parallel with a wiping direction 22 b. The wiping direction 22 b extends perpendicularly relative to the longitudinal direction 38 b in this case. Consequently, the end cap spoiler element 16 b is displaceably supported on the end cap base member 14 b. More specifically, the end cap spoiler element 16 b is displaceably supported in the wiping direction 22 b on the end cap base member 14 b. The end cap spoiler element 16 b has an opening direction 34 b. The end cap spoiler element 16 b can be partially opened in the opening direction 34 b. The opening direction 34 b extends parallel with the wiping direction 22 b . The opening direction 34 b is the direction in which the end cap spoiler element 16 b can be displaced from an operating configuration in a state supported on the end cap base member 14 b into an assembly configuration. The opening direction 34 b is directed from the end cap base member 14 b toward a windward side. The opening direction 34 b is directed from the end cap base member 14 b toward a side facing the wind, in particular a side facing a travel wind. The end cap spoiler element 16 b is closed counter to the opening direction, that is to say, pushed onto the end cap base member 14 b in an operating configuration. The end cap base member 14 b further has a barb 52 b. The barb 52 b is integrally constructed with the end cap base member 14 b, in particular with the spoiler attachment 42 b.
[0050] The end cap spoiler element 16 b is shown in greater detail in FIG. 12 . The end cap spoiler element 16 b aerodynamically produces in an operating state a pressing pressure of the end cap device in the direction of the vehicle window. Preferably, the end cap spoiler element 16 b has a concave-curved main flow face 54 b. The end cap spoiler element 16 b forms a large portion of a flow face 44 b, 54 b of the end cap device. The end cap spoiler element 16 b has a closure wall 56 b. The closure wall 56 b extends at least substantially perpendicularly to the longitudinal direction 38 b. The closure wall 56 b forms a closure of the end cap device in the longitudinal direction 38 b. Furthermore, the closure wall 56 b closes an assembly opening 18 b in an operating state. The wiper arm 20 b can be guided through the assembly opening 18 b in an assembly configuration.
[0051] The end cap device comprises a catch unit 24 b which is provided to engage the end cap spoiler element 16 b in an operating configuration on the end cap base member 14 b. The catch unit 24 b has to this end a catch hook 26 b which is constructed integrally with the end cap spoiler element 16 b.
[0052] The end cap device further has an operating unit 28 b which is provided to move the catch unit 24 b into a release configuration. The operating unit 28 b comprises an operating element 30 b. The operating element 30 a is constructed integrally with the end cap spoiler element 16 b. The operating element 30 b is constructed integrally with the catch hook 26 b. The operating element 30 b can be resiliently redirected manually. When the operating element 30 b is redirected, the catch hook 26 b is released from the barb 52 a. The end cap spoiler element 16 b can subsequently be displaced along the guiding rails 46 b, 48 b between an operating configuration and the assembly configuration. The end cap spoiler element 16 b can subsequently be displaced in an opening direction 34 b along the guiding rails 46 b, 48 b between an operating configuration and the assembly configuration. The end cap spoiler element 16 b is consequently provided to release the assembly opening 18 b for the wiper arm 20 b in an assembly configuration.
[0053] Furthermore, the end cap device additionally has a limitation unit 32 b. The limitation unit 32 b is provided to limit a movement freedom of the end cap spoiler element 16 b in an opening direction 34 b in the assembly configuration.
[0054] FIGS. 10 and 14 show the wiper blade 12 b and the end cap device in the assembly configuration. In the assembly configuration, the wiper arm 20 b can be assembled or disassembled. In this instance, the wiper arm 20 b can be pulled out of a wiper blade 12 b or pushed into a wiper blade. The assembly opening 18 b is produced by means of a gap between the end cap base member 14 b and the closure wall 56 b of the end cap spoiler element 16 b in the assembly configuration.
[0055] In order to replace the wiper arm 20 b, in a first disassembly step, the operating element 30 b is redirected manually. The end cap device is thereby moved from an operating configuration into a release configuration. In the release configuration, the catch unit 24 b releases a movement freedom of the end cap spoiler element 16 b relative to the end cap base member 14 b. In a second disassembly step, the end cap spoiler element 16 b is moved in the opening direction 34 b until it strikes the stop element 50 b. Consequently, the end cap spoiler element 16 b is moved relative to the end cap base member 14 b. In the second disassembly step, the assembly opening 18 b is released. In a third disassembly step, the wiper arm 20 b is pulled out of the wiper blade 12 b through the assembly opening 18 b in a displacement direction 62 b . The displacement direction 62 b extends at least substantially parallel with the longitudinal direction 38 b. Subsequently, a new wiper arm is inserted in a first assembly step through the assembly opening 18 b into the wiper blade 12 b. In a second assembly step, the end cap spoiler element 16 b is moved counter to the opening direction 34 b, until the catch unit 24 b engages the end cap base member 14 b and the end cap spoiler element 16 b with each other. Consequently, the end cap device is moved back into the operating configuration.
|
The invention relates to an end cap arrangement, more particularly for a wiper blade ( 12 a; 12 b ), comprising an end cap main part ( 14 a; 14 b ) that can be fixedly connected to a main component ( 10 a; 10 b ) of a wiper blade ( 12 a; 12 b ). It is proposed that the end cap arrangement comprise at least an end cap spoiler element ( 16 a; 16 b ) which is designed so that in an installed condition an installation opening ( 18 a; 18 b ) is left free for a wiper rubber ( 20 a; 20 b ).
| 1
|
[0001] The instant application claims the benefit of U.S. Provisional Patent Application No. 60/839,086, filed Aug. 21, 2006. The disclosure of this Application is hereby incorporated by reference.
CROSS REFERENCE TO RELATED PATENTS AND PATENT APPLICATIONS
[0002] The subject matter of the instant application is related to U.S. patent application Ser. No. 11,583,439, filed Oct. 19, 2006, and Ser. No. 11/524,471, filed Sep. 21, 2006. The disclosure of the previously identified patent applications is hereby incorporated by reference.
FIELD OF THE INVENTION
[0003] The instant invention relates to zinc oxide (ZnO) nanoparticle dispersions and to such dispersions having a defined color, and films obtained from such dispersions. The inventive zinc oxide dispersions can be used as a UV-absorber, for catalytic applications, electronic applications, production of antifungal or antibacterial materials, sensors, actuators, photovoltaic devices, conductive coatings, among other applications
BACKGROUND OF THE INVENTION
[0004] Exposure to UV radiation can lead to the degradation of certain materials. There is a need to protect exposed materials against UV and in some cases to avoid transmission of UV radiation through transparent covers or coatings. In order to be used for transparent coatings, UV protecting agents are preferably transparent and, in some cases, colorless in the final application. For some applications or end-uses these agents are permanent, non migratory and stable against degradation. Organic UV protecting agents or absorbers can be migratory and have unacceptable long term stability (e.g., less than 10 years). In some cases organic UV absorbers are not stable against oxidation or at relatively high temperatures. Inorganic UV absorbers (e.g. ZnO, TiO 2 , Fe 2 O 3 , CeO 2 , among other inorganic compounds), can have enhanced stability in comparison to organic absorbers. However, inorganic absorbers may not be transparent and/or colorless, or they may be photocatalytically active and in some cases adversely affect a surrounding polymeric matrix when exposed to UV. There is a need in this art for dispersions which can be used as an inorganic transparent UV blocking additive for preparing transparent materials or coatings with low haze levels.
BRIEF SUMMARY OF THE INVENTION
[0005] It is known in the art that a white dispersion will be produced when mixing a white powder, e.g. ZnO with a colorless liquid (e.g. water, ethanol, toluene, among others). Surprisingly, it was found, that, under certain conditions, which are described below certain ZnO nanoparticle dispersions in colorless solvents have a yellow color tone. Such yellow zinc oxide nanoparticle dispersions can show improved properties in comparison to white ZnO dispersions. Commercial, white nanoparticle ZnO dispersions and the inventive yellow dispersions were used as a UV absorbing additive in an acrylic coating. The haze values of the acrylic coatings were measured and the haze values were significantly lower for the coatings made from the inventive yellow dispersions.
BRIEF DESCRIPTION OF SEVERAL VIEWS OF THE DRAWINGS
[0006] FIG. 1 is a plot of color as represented by the CIE L*a*b* parameters.
DETAILED DESCRIPTION OF THE INVENTION
[0007] This invention solves problems associated with conventional UV absorbers by providing zinc oxide dispersions which can be used as an inorganic transparent UV blocking additive to transparent coatings or materials. The zinc oxide particles will normally range in size from about 5 to about 200 nanometers with a mean particle size of about 50 nm. The dispersion will normally comprise or consist essentially of about 10 −3 to about 95 wt. % of zinc oxide nanoparticles and about 0.1 to about 50 wt. % of at least one dispersing agent. Examples of suitable dispersing agents comprise at least one member selected from the group consisting of diammoniumcitrate, catechols (e.g. 4,5-dihydroxy-m-benzenedisulfonic acid disodium salt), certain block copolymers with pigment affinic groups (e.g., Byk 190, methoxy-ethoxy-ethoxy-acetic acid, oligo- or polyacrylic acids and their compounds, mixtures thereof, among others.
[0008] The dispersion can also comprise at least one carrier or diluent. The carrier can be aqueous (e.g., deionized water), or based upon one or more suitable organic compounds. Examples of suitable organic compounds can comprise at least one member selected from the group consisting of isoproproxyethanol, ethanol, toluene, alcohol, butanol, isoacyl alcohol, cetone, acetone, MEK, dicetone, diole, carbitole, glycole, diglycole, triglycole, glycol ether, ethoxy-, propoxy-, isopropoxy-, butoxyethanol-acetate, ester, glycolester, ethyl acetate, butyl acetate, butoxyethyl acetate, alcane, toluene, xylene, acrylic acid, methacrylic acid, acrylate or methacrylate monomers as well as their derivatives, among other suitable substrates. The amount of carrier can range from about<10 wt. % to about 99 wt. % of the dispersion.
[0009] The dispersions can be prepared by any suitable methods such as stirring, shaking, all kind of milling, e.g. media milling, three roll milling, high speed dispersing, rotor stator techniques, sonication, jet milling, to name a few applicable techniques
[0010] In one aspect of the invention, the inventive dispersions can be employed for preparing transparent materials or coatings with low haze levels and other desirable properties. The inventive dispersions can be used for making a coating or film having a haze of about lower or equal to 0.5 to about 3.0 when measured in accordance with ASTM D1003. The coating is also normally transparent as determined by ASTM D1003. The thickness of the coating will typically be about 100 nm to about 50 microns.
[0011] The inventive dispersion can be added to a wide range of polymeric formulations and systems. Examples of such systems including acrylic, polyurethane, epoxy, polyesters, polyethers, polyolefines, siloxanes, organic inorganic (nano)composites, among others. The amount of dispersion that is added to the polymeric formulation will normally range from about 10 −3 wt. % to about 80 wt. % of the formulation.
[0012] The inventive dispersions can be added to the foregoing formulations and systems by any suitable method. Examples of suitable methods comprise shaking, stirring, the previously described milling/dispersing processes, dynamic, static mixers or other blending techniques.
[0013] In another aspect of the invention, the inventive dispersion can be applied onto any suitable substrate. Examples of suitable substrates comprise at least one member selected from the group consisting of glass, polymeric substrates, e.g. PC, PMMA, PET, PVC, PE, PP, PVB, PA, polyesters, polyamides, epoxy, polyurethanes, siloxanes, cotton, linen, wool, textiles, nonwovens, among other suitable substrates.
[0014] In a further aspect of the invention, the inventive dispersion after incorporated into a suitable coating composition and the coating applied onto a suitable substrates. Examples of suitable substrates comprise at least one member selected from the group consisting of e.g. PC, PMMA, PET, PVC, PE, PP, PVB, PA, polyesters, polyamides, epoxy, polyurethanes, siloxanes, cotton, linen, wool, textiles, nonwovens,
[0015] If desired, either the dispersion or a coating composition comprising the dispersion can be applied onto a suitable substrate and heated treated (e.g., to a temperature greater than 100 C). The heat treatment can be sufficient to remove substantially all components other than ZnO nanoparticles. The remaining ZnO coated substrate can be employed in a wide range of applications including, without limitation, such as UV-absorber, catalyst, electronic device, antifungal or antibacterial material, sensor, actuator, photovoltaic device, conductive material, bearing, among other applications.
[0016] If desired the dispersion can include at least one additive such as wetting agents, surfactants, defoamers, and other additives used to formulate inks, coatings and adhesives.
[0017] The following examples are set forth to assist in understanding the invention and do not limit the invention described and claimed herein. Such variations of the invention, including the substitution of all equivalents now known or later developed, which would be within the purview of those skilled in the art, and changes in formulations or minor changes in experimental design, fall within the scope of the present invention.
EXAMPLES
Example 1
[0018] 3 g of Diammoniumcitrate were dissolved in 237 g deionized water. While stirring, 60 g of nanoparticle ZnO, primary particle size 30 nm, were slowly added. The mixture was pumped through a flow cell (a “flow cell” is a continuously working reactor wherein the dispersion was ultrasonically agitated), and ultrasonically agitated for 2.5 h. After that, the dispersion was milled with a Netzsch MiniCer at 2500-3000 rpm. for 160 min.
Example 2
[0019] 15 g of 4,5-dihydroxy-m-benzenedisulfonic acid disodium salt were dissolved in 685 g deionized water. While stirring, 300 g of nanoparticle ZnO (as described in Example 1) were slowly added. The mixture was further stirred for two hours, then 37.5 g Disperbyk 190 were added. Afterwards, the dispersion was pumped through a flow cell and ultrasonically agitated for 4.5 h. After that, the dispersion was divided into two portions and every portion was milled with a Netzsch MiniCer at 2500-3000 rpm for 160 min.
Example 3
[0020] 70 g of nanoparticle ZnO (as described in Example 1), 4.2 g Methoxy-ethoxy-ethoxy-acetic acid and 23 g Isopropoxyethanol were mixed in a beaker. The mixture was further homogenized using a three roller mill (i.e., Exakt 80E). The resulting paste was diluted with ethanol while stirring until a solid content of about 30 wt. % ZnO was achieved. Afterwards, the dispersion was pumped through a flow cell and ultrasonically agitated for 2.5 h. After that, the dispersion was milled with a Netzsch MiniCer at 2500-3000 rpm for 160 min.
Example 4
[0021] 70 g of nanoparticle ZnO (as described in Example 1) and 70 g Byk 9077 were mixed in a beaker. The mixture was further homogenized using the three roller mill described in Example 3. The resulting paste was diluted with of toluene while stirring until a solid content of about 30 wt. % ZnO was achieved. Afterwards, the dispersion was pumped through a flow cell and ultrasonically agitated for 2.5 h. After that, the dispersion was milled with a Netzsch MiniCer at 2,500-3,000 rpm for 160 min.
Example 5
[0022] A commercial aqueous dispersion of nanoparticle ZnO (solid content 45 wt. %) was mixed with an aqueous acrylic emulsion (solid content 50 wt. %, particle size about 400 nm). The acrylic solid to ZnO solid ratio was adjusted to 0.7:0.3. The resulting mixture was coated on glass with a wet coating thickness of 24 g/m 2 . The coating was dried for 5 min at 120° C. The resulting haze value (measured with Haze Gard Plus, Byk Gardner and in accordance with ASTM D 1003), was 34.
Example 6
[0023] Example 5 was repeated except that instead of the commercial dispersion of Example 5, the dispersion of Example 2 was used. The resulting haze value of the coating was 2.9.
Example 7
[0024] 40 g Pentaerythritol tetraacrylate, 10 g Hexanedioldiacrylate and 2 g Irgacure 184 were dissolved in 50 g ethanol. To this solution, 1.5 g of ZnO dispersion of Example 3 were added. The solution was coated onto a glass sheet with a wet coating thickness of 50 μm. The coating was cured by UV radiation (1760 mJ/cm 2 ). The transparency in the visible of the resulting coating was 90.2% and the haze value was 0.5.
[0025] Referring now to FIG. 1 , FIG. 1 illustrates the relationship among color parameters wherein L* corresponds to the brightness, a* the red/green parameter, b* the yellow/blue parameter, C* the Saturation and h* the color angle or hue of the testing Sample. A positive a* parameter indicates a red color whereas a negative a* corresponds to green. A positive b* parameter indicates a yellow color whereas a negative b* corresponds to blue.
[0026] The color parameters (CIE L*a*b*) of all dispersions were measured with a spectral photometer Byk Gardner Color Sphere (Table 1) in accordance with ASTM D 2244, E 308, E 1164
[0027] Table 1 illustrates that the inventive ZnO dispersions all have a b* value greater than 10.
[0000]
TABLE 1
Sample
L*
a*
b*
C*
h*
Commercial
D65/10°
84.89
0.23
5.39
5.40
87.60
dispersion
A/10°
85.29
1.59
5.57
5.79
74.09
CWF/10°
85.18
0.15
6.09
6.09
88.55
Example 1
D65/10°
76.22
−0.26
13.48
13.48
91.11
A/10°
77.06
2.85
13.57
13.87
78.14
CWF/10°
76.88
−0.19
15.48
15.48
90.71
Example 2
D65/10°
75.71
2.59
13.81
14.05
79.37
A/10°
76.90
5.73
14.78
15.85
68.82
CWF/10°
76.48
1.69
15.78
15.87
83.88
Example 3
D65/10°
62.50
−0.21
13.40
13.40
90.89
A/10°
63.33
2.60
13.50
13.74
79.09
CWF/10°
63.22
−0.13
15.49
15.50
90.50
Example 4
D65/10°
58.12
−0.05
11.79
11.79
90.26
A/10°
58.86
2.33
11.98
12.20
78.99
CWF/10°
58.78
−0.01
13.61
13.61
90.05
[0028] The present invention is not to be limited in scope by the specific embodiments disclosed in the examples which are intended as illustrations of a few aspects of the invention and any embodiments that are functionally equivalent are within the scope of this invention. Indeed, various modifications of the invention in addition to those shown and described herein will become apparent to those skilled in the art and are intended to fall within the scope of the appended claims.
|
The disclosure relates to zinc oxide (ZnO) nanoparticle dispersions and to such dispersions having a defined color, and films obtained from such dispersions. The zinc oxide dispersions can be used as a UV-absorber, for catalytic applications, electronic applications, production of antifungal or antibacterial materials, sensors, actuators, photovoltaic devices, conductive coatings, among other applications.
| 2
|
[0001] The present invention relates to the field of synthesizing and biologically evaluating of a novel class of carbohydrate-based vaccines. The new vaccines consist of a multi-modular structure which allows applying the vaccine to a whole variety of pathogenes. This method allows preparing vaccines against all pathogens expressing immunogenic carbohydrate antigens. As conjugation of antigenic carbohydrates to proteins is not required the conjugate vaccine is particularly heat stable. No refrigeration is required, a major drawback of protein-based vaccines.
BACKGROUND OF THE INVENTION
[0002] High prevalence of many infectious diseases, such as invasive pneumococcal disease (IPD) and increasing antibiotic resistance of the related pathogens requires urgent development of protective vaccines. Especially as existing vaccines exhibit major drawbacks such as variable immunogenicity and the lack of development of immunological memory.
[0003] Vaccines have traditionally consisted of live attenuated pathogens, whole inactivated organisms or inactivated toxins. In many cases, these approaches have been successful at inducing immune protection based on antibody mediated responses. However, certain pathogens, e.g., HIV, HCV, TB, and malaria, require the induction of cell-mediated immunity (CMI). Non-live vaccines have generally proven ineffective in producing CMI. In addition, although live vaccines may induce CMI, some live attenuated vaccines may cause disease in immunosuppressed subjects.
[0004] In contrast to older vaccines which were typically based on live attenuated or non-replicating inactivated pathogens, modern vaccines are composed of synthetic, recombinant, or highly purified subunit antigens. Subunit-vaccines are designed to include only the antigens required for protective immunization and are believed to be safer than whole inactivated or live-attenuated vaccines. However, the purity of the subunit antigens and the absence of the self-adjuvanting immunomodulatory components associated with attenuated or killed vaccines often result in weaker immunogenicity.
[0005] The immunogenicity of a relatively weak antigen can be enhanced by the simultaneous or more generally conjoined administration of the antigen with an “adjuvant”, usually a substance that is not immunogenic when administered alone, but will evoke, increase and/or prolong an immune response to an antigen. In the absence of adjuvant, reduced or no immune response may occur, or worse the host may become tolerized to the antigen.
[0006] Adjuvants can be found in a group of structurally heterogeneous compounds (Gupta et al., 1993, Vaccine, 11: 293-306). Classically recognized examples of adjuvants include oil emulsions (e.g., Freund's adjuvant), saponins, aluminium or calcium salts (e.g., alum), non-ionic block polymer surfactants, lipopolysaccharides (LPS), mycobacteria, tetanus toxoid, and many others. Theoretically, each molecule or substance that is able to favor or amplify a particular situation in the cascade of immunological events, ultimately leading to a more pronounced immunological response can be defined as an adjuvant.
[0007] A galactosylceramide (α-GalCer) is a glycolipid, more specifically a glycosylceramide, originally isolated from Okinawan marine sponges (Natori et al., Tetrahedron, 50: 2771-2784, 1994), or its synthetic analog KRN7000 [(2S,3S,4R)-1-O-(α-D-galactopyranosyl)-2-(N-hexacosanoylamino)-1,3,4-octadecanetriol], which can be obtained from Pharmaceutical Research Laboratories, Kirin Brewery (Gumna, Japan) or synthesized as described previously (see, e.g., Kobayashi et al., 1995, Oncol. Res., 7:529-534; Kawano et al., 1997, Science, 278: 1626-9; Burdin et al., 1998, J. Immunol., 161:3271; Kitamura et al., 1999, J. Exp. Med., 189:1121; U.S. Pat. No. 5,936,076).
[0008] It was shown that α-GalCer can stimulate natural killer (NK) activity and cytokine production by natural killer T (NKT) cells and exhibits potent antitumor activity in vivo (Kawano et al., 1998, Proc. Natl Acad. Sci. USA, 95:5690). After intake by antigen presenting cell (APC), which is represented by dendritic cell (DC) and the like, α-galactosylceramide is presented on the cellular membrane by a CD1d protein similar to major histocompatible complex (MHC) class I molecule. NKT cells are activated by recognition using TCR (T cell receptor) of the thus-presented complex of CD1d protein and α-galactosylceramide, which triggers various immune reactions. Invariant Natural Killer T cells have been also shown to induce B cell activation, enhancing B cell proliferation and antibody production (Galli et al, Vaccine, 2003, 21: 2148-S2154; Galli et al, J Exp. Med, 2003, 197: 1051-1057).
[0009] These studies open the possibility that α-GalCer may play an equally important role in bridging not only innate immunity mediated by NKT cells, but also adaptive immunity mediated by B cells, T helper (Th) cells and T cytotoxic (Tc) cells. Recently, α-GalCer has been shown to act as an adjuvant for a variety of co-administered protein antigens and saccharide antigens (W003/009812).
[0010] The development so far exhibits the simultaneous use of the vaccine and an adjuvant that produces the desired immunogenicity. A major drawback of protein-based vaccines, where a conjugation of antigenic carbohydrates to proteins is required, is that the vaccine is particularly heat unstable and a refrigeration of the vaccine is required. Moreover the use of at least two components to achieve a sufficient vaccination is also a significant drawback, since the procedure of administration is rather complex, e.g. the point in time where the adjuvant is administered is essential to achieve the desired immunogenicity (WO003009812).
DESCRIPTION OF THE INVENTION
[0011] To fulfill these requirements and to overcome the disadvantages of current vaccines the invention exhibits a new type of conjugate vaccine, wherein the carbohydrate antigen is covalently bound to the glycolipid adjuvant.
[0012] Protection against an infectious disease is provided by neutralization of virulence factors or opsonizing antibodies. The antibodies (Abs.) have to be directed against the carbohydrate antigen of the pathogen, e.g from capsules composed of polysaccharides or viral glycoproteins. Therefore, an ideal efficient vaccine has to induce high affinity and complement-fixing anti-carbohydrate antibodies. This is actually fulfilled by the conjugates of the present invention.
[0013] The novel carbohydrate-glycolipid conjugate derivatives according to the present invention are represented by the following general formula (I). It was surprisingly found that extraordinary potent and stable vaccine can be derived when a polysaccharide antigen is bound via a linker and a carbohydrate moiety to a ceramide moiety. Thus the present invention relates to compounds of the general formula (I)
[0000] A[L-CH—CA] p (I)
[0000] wherein
A represents a carbohydrate antigen of 1 to 10.000 carbohydrate monomers, wherein the carbohydrate monomers of the carbohydrate antigen are optionally modified to carry amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylenyl, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and/or urea moieties, p is the number of residues -L-CH—CA which are bound to the carbohydrate antigen A, and
p is an integer defined as follows:
p is 1 or 2 if u is 1
p is 1, 2, 3 or 4 if u is 2
p is 1, 2, 3, 4, 5 or 6 if u is 3
p is 1, 2, 3, 4, 5, 6, 7 or 8 if u is 4
1≦p≦10 if 5≦u≦10
2≦p≦50 if 11.≦u≦100
20≦p≦200 if 101≦u≦1000
50≦p≦400 if 1001≦u≦10000
u is the number of carbohydrate monomers of the carbohydrate antigen A
L represents -L 1 -L 2 -, -L 2 -, -L 2 -L 3 - or -L 1 -L 2 -L 3 -;
L 1 represents one of the following residues:
[0000]
[0000] wherein x is in integer from 1 to 60;
Y represents a bond, —NH—, —O—, —S—;
L 2 represents —CH 2 —, —C 2 H 4 —, —C 3 H 6 —, —C 4 H 8 —, —C 5 H 10 —, —C 6 H 12 —, —C 7 H 14 —, —C 8 H 16 —, —C 9 H 18 —, —C 10 H 20 —, —CH(CH 3 )—, —C[(CH 3 ) 2 ]—, —CH 2 —CH(CH 3 )—, —CH(CH 3 )—CH 2 —, —CH(CH 3 )—C 2 H 4 —, —CH 2 —CH(CH 3 )—CH 2 —, —C 2 H 4 —CH(CH 3 )—, —CH 2 —C[(CH 3 ) 2 ]—, —C[(CH 3 ) 2 ]—CH 2 —, —CH(CH 3 )—CH(CH 3 )—, —C[(C 2 H 5 )(CH 3 )]—, —CH(C 3 H 7 )—, —(CH 2 —CH 2 —O) n —CH 2 —CH 2 —, —CO—CH 2 —, —CO—C 2 H 4 —, —CO—C 3 H 6 —, —CO—C 4 H 8 —, —CO—C 5 H 10 —, —CO—C 6 H 12 —, —CO—C 7 H 14 —, —CO—C 8 H 16 —, —CO—C 9 H 18 —, —CO—C 10 H 20 —, —CO—CH(CH 3 )—, —CO—C[(CH 3 ) 2 ]—, —CO—CH 2 —CH(CH 3 )—, —CO—CH(CH 3 )—CH 2 —, —CO—CH(CH 3 )—C 2 H 4 —, —CO—CH 2 —CH(CH 3 )—CH 2 —, —CO—C 2 H 4 —CH(CH 3 )—, —CO—CH 2 —C[(CH 3 ) 2 ]—, —CO—C[(CH 3 ) 2 ]—CH 2 —, —CO—CH(CH 3 )—CH(CH 3 )—, —CO—C[(C 2 H 5 )(CH 3 )]—, —CO—CH(C 3 H 7 )—, —CO—(CH 2 —CH 2 —O) n —CH 2 —CH 2 —;
n represents an integer from 1 to 60;
L 3 represents —CO—, —O—CO—, —NH—CO—, —NH(C═NH)—, —SO 2 —, —O—SO 2 —;
CH represents a monosaccharide, a disaccharide or a trisaccharide;
CA represents or
[0000]
[0000] R* and R# represent independently of each other a linear or branched or cyclic, substituted or unsubstituted, saturated or unsaturated carbon residue consisting of 1 to 30 carbon atoms;
and enantiomers, stereoisomeric forms, mixtures of enantiomers, diastereomers, mixtures of diastereomers, prodrugs, hydrates, solvates, tautomers, and racemates of the above mentioned compounds and pharmaceutically acceptable salts thereof.
Antigen
[0014] A represents a carbohydrate antigen consisting of 1 to 10.000 carbohydrate monomers.
[0015] The term “antigen” as used herein refers to a substance which cause after introduction into the organism of humans and animals, a specific immune response. This manifests itself either in the formation of antibodies (humoral response) and the development of cell-mediated immunity (cellular immune response) or a specific immune tolerance. Depending on whether the formation of the immune response involving T-lymphocytes (T cells) is required, it is called thymus-dependent or -independent antigen. A prerequisite for an immune response (for the immunogenicity of the antigen) is that the antigen is recognized as foreign by the organism, that it has a molecular weight of at least 1000 and that it belongs to the class of proteins or polysaccharides, rare deoxyribonucleic acids or lipids. More complex structures such as bacteria, viruses, or erythrocytes (particulate antigens) are generally more effective antigens. At the molecular level, an antigen is characterized by its ability to be “bound” at the antigen-binding site of an antibody.
[0016] Foreign substances that do not stimulate an immune response by themselves, but by the chemical binding to immunogenic macromolecules, are called haptens. For the efficacy of immunogenic antigens the route of administration (single or multiple dose, dose intradermally or intravenously, with or without adjuvant) is determining. Repeated attacks by the same antigens accelerate the immune response and may result in the worst case of a specific hypersensitivity (allergy, where the antigens are often called allergens). In the presence of large amounts of antigen or chronic persistent amounts of antigen the formation of soluble immune complexes may occur, which can cause anaphylaxis.
[0017] An immunogen is a specific type of antigen. An immunogen is a substance that is able to provoke an adaptive immune response if injected on its own. An immunogen is able to induce an immune response, whereas an antigen is able to combine with the products of an immune response once they are made. Immunogenicity is the ability to induce a humoral and/or cell-mediated immune response
[0018] The term “antigen” may shortly be described as a substance, belonging to the class of proteins or polysaccharides, generally comprising parts (coats, capsules, cell walls, flagella, fimbrae, and toxins) of bacteria, viruses, and other microorganisms, and also rare deoxyribonucleic acids or lipids, smaller molecules or ions (haptens), which are recognized as foreign by the organism of humans and animals and which may cause after introduction into the organism of humans and animals, a specific immune response, which comprises a humoral and/or or a cellular immune response, which leads to the formation of antibodies (humoral response) and/or the development of cell-mediated immunity (cellular response), wherein the mentioned antibodies may lead to a specific binding of the antigen.
[0019] Specifically, the term “antigen” can be described as a substance, which is recognized as foreign by the organism of humans and animals and which may cause after introduction into the organism of humans and animals, a specific immune response, which comprises a humoral and/or or a cellular immune response.
[0020] Preferably A represents an isolated, a semi-synthetic or a synthetic carbohydrate antigen. The isolated carbohydrate antigen consists of 1 to 10,000 carbohydrate monomers, preferably of 10 to 5,000 carbohydrate monomers, and more preferably of 20 to 3,000. The semi-synthetic carbohydrate antigen preferably consists of 1 to 1.000 carbohydrate monomers, more preferably of 5 to 900 and still more preferably of 10 to 800 carbohydrate monomers and the synthetic carbohydrate antigen preferably consists of 1 to 1.000 carbohydrate monomers, more preferably of 5 to 900 and still more preferably of 10 to 800 carbohydrate monomers.
[0021] The antigens and especially the isolated antigens are normally mixtures of antigens having a certain range of carbohydrate monomers so that the term “antigen consisting of 500 carbohydrate monomers” refers to a mixture of antigens having in average the number of 500 carbohydrate monomers. Such a mixture might contain 10% of the antigens with 450 to 470 carbohydrate monomers, 10% of the antigens with 530 to 550 carbohydrate monomers, 20% of the antigens with 471 to 490 carbohydrate monomers, 20% of the antigens with 510 to 529 carbohydrate monomers and 40% of the antigens with a number of 491 to 509 carbohydrate monomers.
[0022] Preferably the carbohydrate monomers belong to heptoses, hexoses, pentoses, tetroses or sialic acids, wherein the carbohydrate monomers are connected to each other via α/β glycosidic bonds which belong to the group consisting of 1,2; 1,3; 1,4; 1,5; 1,6; 2,2; 2,3; 2,4; 2,5; or 2,6 glycosidic bonds. Also, the carbohydrate monomers can be more specifically derivatives of peptidoglycanes such as N-acetylmuramic acid, N-acetyl-D-glocosamine or N-acetyl talosaminuronic acid.
[0023] Some of the hydroxyl groups (—OH) of the carbohydrate monomers of the antigen A can independently of each other optionally be substituted with the following substituents —CH 3 , —C 2 H 5 , —SO 3 H, —SO 3 − , —CH 2 —COOH, —CH 2 —COO − , —C 2 H 4 —COOH, —C 2 H 4 —COO − or some of the hydroxyl groups (—OH) of the carbohydrate monomers can be replaced by the following moieties:
[0000]
[0000] wherein
q is an integer from 1 to 4, and
R′, R″ and R′″ independently of each other represent one of following residues: —H, —CH 3 , —C 2 H 5 , —C 3 H 7 , -cyclo-C 3 H 5 , —CH(CH 3 ) 2 , —C(CH 3 ) 3 , —C 4 H 9 , -Ph, —CH 2 -Ph, —CH 2 —OCH 3 , —C 2 H 4 —OCH 3 , —C 3 H 6 —OCH 3 , —CH 2 —OC 2 H 5 , —C 2 H 4 —OC 2 H 5 , —C 3 H 6 —OC 2 H 5 , —CH 2 —OC 3 H 7 , —C 2 H 4 —OC 3 H 7 , —C 3 H 6 —OC 3 H 7 , —CH 2 —O-cyclo-C 3 H 5 , —C 2 H 4 —O-cyclo-C 3 H 5 , —C 3 H 6 —O-cyclo-C 3 H 5 , —CH 2 —OCH(CH 3 ) 2 , —C 2 H 4 —OCH(CH 3 ) 2 , —C 3 H 6 —OCH(CH 3 ) 2 , —CH 2 —OC(CH 3 ) 3 , —C 2 H 4 —OC(CH 3 ) 3 , —C 3 H 6 —OC(CH 3 ) 3 , —CH 2 —OC 4 H 9 , —C 2 H 4 —OC 4 H 9 , —C 3 H 6 —OC 4 H 9 , —CH 2 —OPh, —C 2 H 4 —OPh, —C 3 H 6 —OPh, —CH 2 —OCH 2 -Ph, —C 2 H 4 —OCH 2 -Ph, —C 3 H 6 —OCH 2 -Ph.
[0024] These groups are naturally occurring substituents which can be present in the carbohydrate antigens.
[0025] The carbohydrate monomers of the carbohydrate antigen can therefore be optionally modified or can be modified to carry amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylenyl, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and/or urea moieties.
[0026] The term “hydroxylalkyl” refers preferably to linear or branched C 1 -C 4 hydroxyalkyl residues which consist in total of 1 to 4 carbon atoms including the carbon atoms of the branches wherein one of the hydrogen atoms is substituted by a hydroxyl group such as —CH 2 OH, —C 2 H 4 OH, —CHOHCH 3 , —CH 2 CH 2 CH 2 OH, —CH 2 CHOHCH 3 , —CHOHCH 2 CH 3 , -cyclo-C 3 H 4 OH, —COH(CH 3 ) 2 , —CH(CH 3 )CH 2 OH, —CH 2 CH 2 CH 2 CH 2 OH, —CH 2 CH 2 CHOHCH 3 , —CH 2 CHOHCH 2 CH 3 , —CHOHCH 2 CH 2 CH 3 , —C(CH 3 ) 2 CH 2 OH, —CHOH—CH(CH 3 ) 2 , —CH(CH 3 )—CHOHCH 3 , —CCH 3 OH—C 2 H 5 , —CH 2 —C(CH 3 ) 2 OH.
[0027] As used herein, the term alkenyl refers preferably to “linear or branched C 2 -C 8 -alkenyl” such as —CH═CH 2 , —CH 2 —CH═CH 2 , —C(CH 3 )═CH 2 , —CH═CH—CH 3 , —C 2 H 4 —CH═CH 2 , —CH═CH—C 2 H 5 , —CH 2 —C(CH 3 )═CH 2 , —CH(CH 3 )—CH═CH, —CH═C(CH 3 ) 2 , —C(CH 3 )═CH—CH 3 , —CH═CH—CH═CH 2 , —C 3 H 6 —CH═CH 2 , —C 2 H 4 —CH═CH—CH 3 , —CH 2 —CH═CH—C 2 H 5 , —CH═CH—C 3 H 7 , —CH 2 —CH═CH—CH═CH 2 , —CH═CH—CH═CH—CH 3 , —CH═CH—CH 2 —CH═CH 2 , —C(CH 3 )═CH—CH═CH 2 , —CH═C(CH 3 )—CH═CH 2 , —CH═CH—C(CH 3 )═CH 2 , —C 2 H 4 —C(CH 3 )═CH 2 , —CH 2 —CH(CH 3 )—CH═CH 2 , —CH(CH 3 )—CH 2 —CH═CH 2 , —CH 2 —CH═C(CH 3 ) 2 , —CH 2 —C(CH 3 )═CH—CH 3 , —CH(CH 3 )—CH═CH—CH 3 , —CH═CH—CH(CH 3 ) 2 , —CH═C(CH 3 )—C 2 H 5 , —C(CH 3 )═CH—C 2 H 5 , —C(CH 3 )═C(CH 3 ) 2 , —C(CH 3 ) 2 —CH═CH 2 , —CH(CH 3 )—C(CH 3 )═CH 2 , —C(CH 3 )═CH—CH═CH 2 , —CH═C(CH 3 )—CH═CH 2 , —CH═CH—C(CH 3 )═CH 2 , —C 4 H 8 —CH═CH 2 , —C 3 H 6 —CH═CH—CH 3 , —C 2 H 4 —CH═CH—C 2 H 5 , —CH 2 —CH═CH—C 3 H 7 , —CH═CH—C 4 H 9 , —C 3 H 6 —C(CH 3 )═CH 2 , —C 2 H 4 —CH(CH 3 )—CH═CH 2 , —CH 2 —CH(CH 3 )—CH 2 —CH═CH 2 , —CH 2 —CH═CH—CH 3 , —CH(CH 3 )—C 2 H 4 —CH═CH 2 , —C 2 H 4 —CH═C(CH 3 ) 2 , —C 2 H 4 —C(CH 3 )═CH—CH 3 , —CH 2 —CH(CH 3 )—CH═CH—CH 3 , —CH(CH 3 )—CH 2 —CH═CH—CH 3 , —C(C 4 H 9 )═CH 2 , —CH 2 —CH═CH—CH(CH 3 ) 2 , —CH 2 —CH═C(CH 3 )—C 2 H 5 , —CH 2 —C(CH 3 )═CH—C 2 H 5 , —CH(CH 3 )—CH═CH—C 2 H 5 , —CH═CH—CH 2 —CH(CH 3 ) 2 , —CH═CH—CH(CH 3 )—C 2 H 5 , —CH═C(CH 3 )—C 3 H 7 , —C(CH 3 )═CH—C 3 H 7 , —CH 2 —CH(CH 3 )—C(CH 3 )═CH 2 , —CH(CH 3 )—CH 2 —C(CH 3 )═CH 2 , —CH(CH 3 )—CH(CH 3 )—CH═CH 2 , —CH 2 —C(CH 3 ) 2 —CH═CH 2 , —C(CH 3 ) 2 —CH 2 —CH═CH 2 , —CH 2 —C(CH 3 )═C(CH 3 ) 2 , —CH(CH 3 )—CH═C(CH 3 ) 2 , —C(CH 3 ) 2 —CH═CH—CH 3 , —CH(CH 3 )—C(CH 3 )═CH—CH 3 , —CH═C(CH 3 )—CH(CH 3 ) 2 , —C(CH 3 )═CH—CH(CH 3 ) 2 , —C(CH 3 )═C(CH 3 )—C 2 H 5 , —CH═CH—C(CH 3 ) 3 , —C(CH 3 ) 2 —C(CH 3 )═CH 2 , —CH(C 2 H 5 )—C(CH 3 )═CH 2 , —C(CH 3 (C 2 H 5 )—CH═CH 2 , —CH(CH 3 )—C(C 2 H 5 )═CH 2 , —CH 2 —C(C 3 H 7 )═CH 2 , —CH 2 —C(C 2 H 5 )═CH—CH 3 , —CH(C 2 H 5 )—CH═CH—CH 3 , —C(C 3 H 7 )═CH—CH 3 , —C(C 2 H 5 )═CH—C 2 H 5 , —C(C 2 H 5 )═C(CH 3 ) 2 , —C[C(CH 3 ) 3 ]═CH 2 , —C[CH(CH 3 )(C 2 H 5 )]═CH 2 , —C[CH 2 —CH(CH 3 ) 2 ]═CH 2 , —C 2 H 4 —CH═CH—CH═CH 2 , —CH 2 —CH═CH—CH 2 —CH═CH 2 , —CH═CH—C 2 H 4 —CH═CH 2 , —CH 2 —CH═CH—CH═CH—CH 3 , —CH═CH—CH 2 —CH═CH—CH 3 , —CH═CH—CH═CH—C 2 H 5 , —CH 2 —CH═CH—C(CH 3 )═CH 2 , —CH 2 —CH═C(CH 3 )—CH═CH 2 , —CH 2 —C(CH 3 )═CH—CH═CH 2 , —CH(CH 3 )—CH═CH—CH═CH 2 , —CH═CH—CH 2 —C(CH 3 )═CH 2 , —CH═CH—CH(CH 3 )—CH═CH 2 , —CH═C(CH 3 )—CH 2 —CH═CH 2 , —C(CH 3 )═CH—CH 2 —CH═CH 2 , —CH═CH—CH═C(CH 3 ) 2 , —CH═CH—C(CH 3 )═CH—CH 3 , —CH═C(CH 3 )—CH═CH—CH 3 , —C(CH 3 )═CH—CH═CH—CH 3 , —CH═C(CH 3 )—C(CH 3 )═CH 2 , —C(CH 3 )═CH—C(CH 3 )═CH 2 , —C(CH 3 )═C(CH 3 )—CH═CH 2 , —CH═CH—CH═CH—CH═CH 2 , —C 5 H 10 —CH═CH 2 , —C 4 H 8 —CH═CH—CH 3 , —C 3 H 6 —CH═CH—C 2 H 5 , —C 2 H 4 —CH═CH—C 3 H 7 , —CH 2 —CH═CH—C 4 H 9 , —C 4 H 8 —C(CH 3 )═CH 2 , —C 3 H 6 —CH(CH 3 )—CH═CH 2 , —C 2 H 4 —CH(CH 3 )—CH 2 —CH═CH 2 , —CH 2 —CH(CH 3 )—C 2 H 4 —CH═CH 2 , —C 3 H 6 —CH═C(CH 3 ) 2 , —C 3 H 6 —C(CH 3 )═CH—CH 3 , —C 2 H 4 —CH(CH 3 )—CH═CH—CH 3 , —CH 2 —CH(CH 3 )—CH 2 —CH═CH—CH 3 , —C 2 H 4 —CH═CH—CH(CH 3 ) 2 , —C 2 H 4 —CH═C(CH 3 )—C 2 H 5 , —C 2 H 4 —C(CH 3 )═CH—C 2 H 5 , —CH 2 —CH(CH 3 )—CH═CH—C 2 H 5 , —CH 2 —CH═CH—CH 2 —CH(CH 3 ) 2 , —CH 2 —CH═CH—CH(CH 3 )—C 2 H 5 , —CH 2 —CH═C(CH 3 )—C 3 H 7 , —CH 2 —C(CH 3 )═CH—C 3 H 7 , —C 2 H 4 —CH(CH 3 )—C(CH 3 )═CH 2 , —CH 2 —CH(CH 3 )—CH 2 —C(CH 3 )═CH 2 , —CH 2 —CH(CH 3 )—CH(CH 3 )—CH═CH 2 , —C 2 H 4 —C(CH 3 ) 2 —CH═CH 2 , —CH 2 —C(CH 3 ) 2 —CH 2 —CH═CH 2 , —C 2 H 4 —C(CH 3 )═C(CH 3 ) 2 , —CH 2 —CH(CH 3 )—CH═C(CH 3 ) 2 , —CH 2 —C(CH 3 ) 2 —CH═CH—CH 3 , —CH 2 —CH(CH 3 )—C(CH 3 )═CH—CH 3 , —CH 2 —CH═C(CH 3 )—CH(CH 3 ) 2 , —CH 2 —C(CH 3 )═CH—CH(CH 3 ) 2 , —CH 2 —C(CH 3 )═C(CH 3 )—C 2 H 5 , —CH 2 —CH═CH—C(CH 3 ) 3 , —CH 2 —C(CH 3 ) 2 —C(CH 3 )═CH 2 , —CH 2 —CH(C 2 H 5 )—C(CH 3 )═CH 2 , —CH 2 —C(CH 3 )(C 2 H 5 )—CH═CH 2 , —CH 2 —CH(CH 3 )—C(C 2 H 5 )═CH 2 , —C 2 H 4 —C(C 3 H 7 )═CH 2 , —C 2 H 4 —C(C 2 H 5 )═CH—CH 3 , —CH 2 —CH(C 2 H 5 )—CH═CH—CH 3 , —CH 2 —C(C 4 H 9 )═CH 2 , —CH 2 —C(C 3 H 7 )═CH—CH 3 , —CH 2 —C(C 2 H 5 )═CH—C 2 H 5 , —CH 2 —C(C 2 H 5 )═C(CH 3 ) 2 , —CH 2 —C[C(CH 3 ) 3 ]═CH 2 , —CH 2 —C[CH(CH 3 )(C 2 H 5 )]═CH 2 , —CH 2 —C[CH 2 —CH(CH 3 ) 2 ]═CH 2 , —C 3 H 6 —CH═CH—CH═CH 2 , —C 2 H 4 —CH═CH—CH 2 —CH═CH 2 , —CH 2 —CH═CH—C 2 H 4 —CH═CH 2 , —C 2 H 4 —CH═CH—CH═CH—CH 3 , —CH 2 —CH═CH—CH 2 —CH═CH—CH 3 , —CH 2 —CH═CH—CH═CH—C 2 H 5 , —C 2 H 4 —CH═CH—C(CH 3 )═CH 2 , —C 2 H 4 —CH═C(CH 3 )—CH═CH 2 , —C 2 H 4 —C(CH 3 )═CH—CH═CH 2 , —CH 2 —CH(CH 3 )—CH═CH—CH═CH 2 , —CH 2 —CH═CH—CH 2 —C(CH 3 )═CH 2 , —CH 2 —CH═CH—CH(CH 3 )—CH═CH 2 , —CH 2 —CH═C(CH 3 )—CH 2 —CH═CH 2 , —CH 2 —C(CH 3 )═CH—CH 2 —CH═CH 2 , —CH 2 —CH═CH—CH═C(CH 3 ) 2 , —CH 2 —CH═CH—C(CH 3 )═CH—CH 3 , —CH 2 —CH═C(CH 3 )—CH═CH—CH 3 , —CH 2 —C(CH 3 )═CH—CH═CH—CH 3 , —CH 2 —CH═C(CH 3 )—C(CH 3 )═CH 2 , —CH 2 —C(CH 3 )═CH—C(CH 3 )═CH 2 , —CH 2 —C(CH 3 )═C(CH 3 )—CH═CH 2 , —CH 2 —CH═CH—CH═CH—CH═CH 2 , —C 6 H 12 —CH═CH 2 , —C 5 H 10 —CH═CH—CH 3 , —C 4 H 8 —CH═CH—C 2 H 5 , —C 3 H 6 —CH═CH—C 3 H 7 , —C 2 H 4 —CH═CH—C 4 H 9 , —C 5 H 10 —C(CH 3 )═CH 2 , —C 4 H 8 —CH(CH 3 )—CH═CH 2 , —C 3 H 6 —CH(CH 3 )—CH 2 —CH═CH 2 , —C 2 H 4 —CH(CH 3 )—C 2 H 4 —CH═CH 2 , —C 4 H 8 —CH═C(CH 3 ) 2 , —C 4 H 8 —C(CH 3 )═CH—CH 3 , —C 3 H 6 —CH(CH 3 )—CH═CH—CH 3 , —C 2 H 4 —CH(CH 3 )—CH 2 —CH═CH—CH 3 , —C 3 H 6 —CH═CH—CH(CH 3 ) 2 , —C 3 H 6 —CH═C(CH 3 )—C 2 H 5 , —C 3 H 6 —C(CH 3 )═CH—C 2 H 5 , —C 2 H 4 —CH(CH 3 )—CH═CH—C 2 H 5 , —C 2 H 4 —CH═CH—CH 2 —CH(CH 3 ) 2 , —C 2 H 4 —CH═CH—CH(CH 3 )—C 2 H 5 , —C 2 H 4 —CH═C(CH 3 )—C 3 H 7 , —C 2 H 4 —C(CH 3 )═CH—C 3 H 7 , —C 3 H 6 —CH(CH 3 )—C(CH 3 )═CH 2 , —C 2 H 4 —CH(CH 3 )—CH 2 —C(CH 3 )═CH 2 , —C 2 H 4 —CH(CH 3 )—CH(CH 3 )—CH═CH 2 , —C 3 H 6 —C(CH 3 ) 2 —CH═CH 2 , —C 2 H 4 —C(CH 3 ) 2 —CH 2 —CH═CH 2 , —C 3 H 6 —C(CH 3 )═C(CH 3 ) 2 , —C 2 H 4 —CH(CH 3 )—CH═C(CH 3 ) 2 , —C 2 H 4 —C(CH 3 ) 2 —CH═CH—CH 3 , —C 2 H 4 —CH(CH 3 )—C(CH 3 )═CH—CH 3 , —C 2 H 4 —CH═C(CH 3 )—CH(CH 3 ) 2 , —C 2 H 4 —C(CH 3 )═CH—CH(CH 3 ) 2 , C 2 H 4 —C(CH 3 )═C(CH 3 )—C 2 H 5 , —C 2 H 4 —CH═CH—C(CH 3 ) 3 , —C 2 H 4 —C(CH 3 ) 2 —C(CH 3 )═CH 2 , —C 2 H 4 —CH(C 2 H 5 )—C(CH 3 )═CH 2 , —C 2 H 4 —C(CH 3 )(C 2 H 5 )—CH═CH 2 , —C 2 H 4 —CH(CH 3 )—C(C 2 H 5 )═CH 2 , —C 3 H 6 —C(C 3 H 7 )═CH 2 , —C 3 H 6 —C(C 2 H 5 )═CH—CH 3 , —C 2 H 4 —CH(C 2 H 5 )—CH═CH—CH 3 , —C 2 H 4 —C(C 4 H 9 )═CH 2 , —C 2 H 4 —C(C 3 H 7 )═CH—CH 3 , —C 2 H 4 —C(C 2 H 5 )═CH—C 2 H 5 , —C 2 H 4 —C(C 2 H 5 )═C(CH 3 ) 2 , —C 2 H 4 —C[C(CH 3 ) 3 ]═CH 2 , —C 2 H 4 —C[CH(CH 3 )(C 2 H 5 )]═CH 2 , —C 2 H 4 —C[CH 2 —CH(CH 3 ) 2 ]═CH 2 , —C 4 H 8 —CH═CH—CH═CH 2 , —C 3 H 6 —CH═CH—CH 2 —CH═CH 2 , —C 2 H 4 —CH═CH—C 2 H 4 —CH═CH 2 , —C 3 H 6 —CH═CH—CH═CH—CH 3 , —C 2 H 4 —CH═CH—CH 2 —CH═CH—CH 3 , —C 2 H 4 —CH═CH—CH═CH—C 2 H 5 , —C 3 H 6 —CH═CH—C(CH 3 )═CH 2 , —C 3 H 6 —CH═C(CH 3 )—CH═CH 2 , —C 3 H 6 —C(CH 3 )═CH—CH═CH 2 , —C 2 H 4 —CH(CH 3 )—CH═CH—CH═CH 2 , —C 2 H 4 —CH═CH—CH 2 —C(CH 3 )═CH 2 , —C 2 H 4 —CH═CH—CH(CH 3 )—CH═CH 2 , —C 2 H 4 —CH═C(CH 3 )—CH 2 —CH═CH 2 , —C 2 H 4 —C(CH 3 )═CH—CH 2 —CH═CH 2 , —C 2 H 4 —CH═CH—CH═C(CH 3 ) 2 , —C 2 H 4 —CH═CH—C(CH 3 )═CH—CH 3 , —C 2 H 4 —CH═C(CH 3 )—CH═CH—CH 3 , —C 2 H 4 —C(CH 3 )═CH—CH═CH—CH 3 , —C 2 H 4 —CH═C(CH 3 )—C(CH 3 )═CH 2 , —C 2 H 4 —C(CH 3 )═CH—C(CH 3 )═CH 2 , —C 2 H 4 —C(CH 3 )═C(CH 3 )—CH═CH 2 and —C 2 H 4 —CH═CH—CH═CH—CH═CH 2 ,
[0028] As used herein, the term alkylenyl refers to preferably “linear or branched C 1 -C 4 -alkylenyl” such as
[0000]
[0029] Preferred examples of modified hydroxylgroups of carbohydrate monomers of the carbohydrate antigen A are
[0000]
[0030] Modified hydroxylgroups of carbohydrate monomers of the carbohydrate antigen A may be formed by the activation of the carbohydrate antigen in order to couple the residues -L-CH—CA to the carbohydrate antigen. Since not all activated groups of the carbohydrate antigen are thereafter coupled to one of the residues -L-CH—CA, activated groups of the carbohydrate antigen remain which are not converted to an antigen linker (A-L) linkage. Such activated but not converted groups of the carbohydrate antigen are normally hydrolyzed during work-up of the A[L-CH—CA] p complex and remain on the carbohydrate antigen A as amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylenyl, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and/or urea moieties.
[0031] That means, in case the carbohydrate antigen A is activated to form the covalent bond to the residues -L-CH—CA, the originally isolated or synthesized antigen is modified to bear such amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylenyl, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and/or urea moieties.
[0032] Only in case the residue -L-CH—CA is activated at the L-terminus to form the covalent bond to the carbohydrate antigen A, the functional groups of the carbohydrate antigen A which are not linked to the residues -L-CH—CA remain unaltered.
[0033] Generally the carbohydrate antigen consists of a plurality of carbohydrate monomers, wherein each carbohydrate monomer has further more than one functionality which could be used for a covalent linkage of the residue -L-CH—CA, thus more than one residue -L-CH—CA and generally a larger number of residues -L-CH—CA is bound to the carbohydrate antigen A. It is clear to a skilled person that the more residues -L-CH—CA can be bound to one carbohydrate antigen the more carbohydrate monomers are contained in said carbohydrate antigen. For instance, a carbohydrate antigen consisting of 2 (u=2) carbohydrate monomers can bear 1, 2, 3 or 4 residues -L-CH—CA, while a carbohydrate antigen consisting of 50 (u=50) carbohydrate monomers might bear between 2 and 50 residues -L-CH—CA, and a carbohydrate antigen consisting of 3,000 (u=3000) carbohydrate monomers might have between 50 and 400 residues -L-CH—CA.
[0034] The bonding mode is represented by the integer p. p is the number of residues -L-CH—CA which are bound to the carbohydrate antigen A.
[0035] p represents an integer from 1 to (φ*u), wherein φ represents the following integers: φ=2 (if u is 1 to 4); φ=1 (if u is 5 to 10); φ=0.5 (if u is 11 to 100); φ=0.2 (if u is 101 to 1000); φ=0.04 (if u is 1001 to 10000); wherein u is the number of carbohydrate monomers of the carbohydrate antigen A.
[0036] In another preferred embodiment of the invention p is an integer and is defined as follows:
p is 1 or 2 if u is 1 p is 1, 2, 3 or 4 if u is 2 p is 1, 2, 3, 4, 5 or 6 if u is 3 p is 1, 2, 3, 4, 5, 6, 7 or 8 if u is 4 1≦p≦10 if 5≦u≦10 2≦p≦50 if 11.≦u 100 20≦p≦200 if 101≦u≦1000 50≦p 5400 if 1001≦u≦10000 wherein u is the number of carbohydrate monomers of the carbohydrate antigen A.
[0046] In a preferred embodiment of this invention p is an integer falling within the range from 0.02 u≦p≦(0.7 u+3) with the proviso that p≧1, wherein u is an integer from 1 to 10000, representing the total number of carbohydrate monomers within the carbohydrate antigen A.
[0047] In order to connect the linker L or respectively the moiety -L-CH—CA to the carbohydrate antigen, two ways are possible. On the one hand the antigen could be activated and than reacted with the linker L or the moiety -L-CH—CA or on the other hand the linker L could be activated and than reacted with the antigen.
[0048] In case the linker L is activated in order to form a covalent bond with the carbohydrate antigen the number p of -L-CH—CA moieties present in the carbohydrate antigen depends on the molar equivalents of the moieties -L-CH—CA in regard to the number u of carbohydrate monomers present in the carbohydrate antigen. Thus, if u=100, i.e. the carbohydrate antigen A consists of 100 carbohydrate monomers, one molar equivalent of the moiety -L-CH—CA means that each carbohydrate antigen A bears only one moiety -L-CH—CA, while 50 molar equivalents of the moiety -L-CH—CA means, that in average every second carbohydrate monomer of the carbohydrate antigen A has one moiety -L-CH—CA, while 200 molar equivalents means that in average each carbohydrate monomer of the carbohydrate antigen A has two moieties -L-CH—CA.
[0049] In case the carbohydrate antigen A is activated and not the linker L, the carbohydrate antigen normally comprises a larger number of activated groups which are theoretically all possible to form a covalent bond with the linker L or respectively with the moiety -L-CH—CA. Generally not all activated groups of the carbohydrate antigen A are reacted with the linker L or respectively with the moiety -L-CH—CA, thus several activated groups remain in the carbohydrate antigen after reaction with the linker L or respectively with the moiety -L-CH—CA. These remaining activated groups normally react during workup of the reaction product of the activated carbohydrate antigen with the linker L or respectively with the moiety -L-CH—CA. Thus during workup these remaining activated groups of the carbohydrate antigen A are, for instance, hydrolyzed, oxidized, isomerized, cyclized and/or crosslinked. During work up and especially during aqueous workup these remaining activated groups are, for instance, converted to amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylenyl, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and/or urea moieties.
[0050] The activated groups which can be converted to the amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylene, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and urea moieties are, for instance, cyano, chloro, bromo, iodo, azido, imino groups, vinyl, styryl and allyl groups, anhydrides, oxiranes, cyanates, isocyanates, thiocyanates, isothiocyanates, triazines and especially 1,3,5-triazines, imidazoles, methoxy ethers as well as sulfonyl groups such as para-toluenesulfonyl (Ts-), trifluoromethanesulfonyl (Tf-, CF 3 SO 2 —), benzenesulfonyl (C 6 H 5 SO 2 —) or methanesulfonyl (Ms-).
[0051] In the following more specific examples for such activated groups are given. The activation method comprising the modification of the functional groups of the carbohydrate monomers of the carbohydrate antigen may lead to the formation of activated moieties which are covalently bound to heteroatoms (N, O, S) of the functionalities of the carbohydrate antigen, wherein the activated moieties preferably belong to the following group comprising or consisting of:
[0000]
[0000] wherein x is in integer from 1 to 60.
[0052] Thus, the modification of the carbohydrate monomers of the carbohydrate antigen also implies that the carbohydrate monomers comprise or contain amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylenyl, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and/or urea moieties. That means, that the modification of the carbohydrate monomers of the carbohydrate antigen A implies that the functional groups of the carbohydrate monomers are modified to amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylenyl, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and/or urea moieties.
[0053] Therefore, the optional modification of the carbohydrate monomers of the carbohydrate antigen may be the result of an activation method which comprises the reaction of the carbohydrate functionalities with one activation agent or several activation agents and wherein the activation agent or the activation agents may form especially after hydrolysis, oxidation, isomerization, cyclization and/or crosslinking amide, carbonate, carbamate, carbonyl, thiocarbonyl, carboxy, thiocarboxy, ester, thioester, ether, epoxy, hydroxyalkyl, alkylenyl, phenylene, alkenyl, imino, imide, isourea, thiocarbamate, thiourea and/or urea moieties.
[0054] The mentioned activation agent or agents can be used for the coupling of the carbohydrate antigen to the linker L or respectively to the residues -L-CH—CA and preferably belong to the group comprising:
[0000] allylbromide, allylchloride, bis-NHS-esters like bis[sulfosuccinimidyl] suberate, cyanogen bromide, 1,4-cyclohexanedimethanol divinyl ether, 1,1′-carbonyldiimidazole (CDI), N,N′-(1,2-dihydroxyethylene)bisacrylamide, divinylbenzene, epichlorhydrin (ECH), ethylene-glycol-di(meth)acrylates, ethylene-glycol-diacrylates, N-hydroxysuccinimide (NHS), N-(1-hydroxy-2,2-dimethoxyethyl)-acrylamide, methylenebisacrylamides, 4,4′-methylenebis(cyclohexylisocyanate), 1,4-phenylenediacryloylchloride, phosgene, diphosgene, triphosgene, polyethylene-glycol-di(meth)acrylates, polyethylene-glycol-diacrylates, tetraethylene glycol dimethyl ether, 1,1′-thiocarbonyldiimidazol (TCDI), thiophosgene, 2,4,6-trichlorotriazine (TCT).
[0055] In case the carbohydrate antigen A is activated, the activation method leads to a conversion of the functionalities of the carbohydrate monomers of the carbohydrate antigen into activated species which react with the residues -L-CH—CA in a further step.
[0056] Not all of the activated groups of the carbohydrate antigen A react with the residues -L-CH—CA and may therefore hydrolize, oxidize, isomerize, cyclize or crosslink with other sugar moieties of the carbohydrate antigen during workup to form hydrolized, oxidized, isomerized, cyclized or crosslinked residues. These hydrolized, oxidized, isomerized, cyclized or crosslinked residues derive from the activation agent itself and their chemistry due to hydrolysis, oxidation, isomerization, cyclization or crosslinking reactions. The hydrolized, oxidized, isomerized, cyclized or crosslinked residues are covalently bound to any hetero atom (N, O, S) of the functionalities of the carbohydrate monomers of the carbohydrate antigen, and belong preferably to the group comprising or consisting of:
[0000]
[0000] wherein x is in integer from 1 to 60.
[0057] The modification of the functionalities of the carbohydrate monomers of the carbohydrate antigen comprises the reaction of the functionalities of the carbohydrate monomers of the carbohydrate antigen with one activation agent or activation agents and/or with the activated linker L or respectively the activated linker L in -L-CH—CA or when the carbonhydrate monomers of the carbohydrate antigen with the non-activated linker to form a covalent bond between the hetero atom (N, O, S) of the functionality of the carbohydrate monomer or the modified carbohydrate monomer and the activation agent and/or with the activated or non-activated linker L. The formation of this covalent bond is accompanied by the cleavage of a N—H, O—H or S—H bond and the loss of a H-atom. Possible reactions for the formation of this covalent bond are belonging to the group comprising nucleophilic substitution, esterification, etherification, amidation, acylation.
[0058] The carbohydrate monomers of the carbohydrate antigen A preferably belong to hexoses, pentoses, tetroses or sialic acids.
[0059] In a preferred embodiment of the invention, the sialic acids belong to the group of N- or O-substituted derivatives of neuraminic acid of the following formula:
[0000]
[0000] wherein Z represents —NH 2 , —NHAc, or —OH.
[0060] In case such a sialic acid carbohydrate monomer is present in the carbohydrate antigen A, linkage to the subsequent carbohydrate monomer is achieved through a glycosidic bond (and replacement of the corresponding hydrogen atom at the glycosidic hydroxyl group) and/or through linkage of another carbohydrate monomer to one of the hydroxyl groups of the sialic acid by replacement of the corresponding hydrogen atom at this hydroxyl group.
[0061] In a preferred embodiment the sialic acid carbohydrate monomer represents within the building block A as follows:
[0000]
[0000] wherein Z represents —NH 2 , —NHAc, or —OH.
[0062] In a preferred embodiment of the invention, the used carbohydrate monomers of the A-moiety belong to the following group of α- and β-D/L-carbohydrates comprising or consisting of:
[0000] α-D-ribopyranose, α-D-arabinopyranose, α-D-xylopyranose, α-D-lyxopyranose, α-D-allopyranose, α-D-altropyranose, α-D-glucopyranose, α-D-mannpyranose, α-D-glucopyranose, α-D-idopyranose, α-D-galactopyranose, α-D-talopyranose, α-D-psicopyranose, α-D-fructopyranose, α-D-sorbopyranose, α-D-tagatopyranose, α-D-ribofuranose, α-D-arabinofuranose, α-D-xylofuranose, α-D-lyxofuranose, α-D-Allofuranose, α-D-Altrofuranose, α-D-Glucofuranose, α-D-Mannofuranose, α-D-gulofuranose, α-D-idofuranose, α-D-galactofuranose, α-D-talofuranose, α-D-psicofuranose, α-D-fructofuranose, α-D-sorbofuranose, α-D-tagatofuranose, α-D-xylulofuranose, α-D-ribulofuranose, α-D-threofuranose, α-D-rhamnopyranose, α-D-erythrofuranose, α-D-glucosamine, α-D-glucopyranuronic acid, β-D-ribopyranose, β-D-arabinopyranose, β-D-xylopyranose, β-D-lyxopyranose, β-D-allopyranose, β-D-altropyranose, β-D-glucopyranose, β-D-mannpyranose, β-D-glucopyranose, β-D-idopyranose, β-D-galactopyranose, β-D-talopyranose, β-D-psicopyranose, β-D-fructopyranose, β-D-sorbopyranose, β-D-tagatopyranose, β-D-ribofuranose, β-D-arabinofuranose, β-D-xylofuranose, β-D-lyxofuranose, β-D-rhamnopyranose, β-D-allofuranose, β-D-altrofuranose, β-D-glucofuranose, β-D-mannofuranose, β-D-gulofuranose, β-D-idofuranose, β-D-galactofuranose, β-D-talofuranose, β-D-psicofuranose, β-D-fructofuranose, β-D-sorbofuranose, β-D-tagatofuranose, β-D-xylulofuranose, β-D-ribulofuranose, β-D-threofuranose, β-D-erythrofuranose, β-D-glucosamine, β-D-glucopyranuronic acid, α-L-ribopyranose, α-L-arabinopyranose, α-L-xylopyranose, α-L-lyxopyranose, α-L-allopyranose, α-L-altropyranose, α-L-glucopyranose, α-L-mannpyranose, α-L-glucopyranose, α-L-idopyranose, α-L-galactopyranose, α-L-talopyranose, α-L-psicopyranose, α-L-fructopyranose, α-L-sorbopyranose, α-L-tagatopyranose, α-L-rhamnopyranose, α-L-ribofuranose, α-L-arabinofuranose, α-L-xylofuranose, α-L-lyxofuranose, α-L-Allofuranose, α-L-Altrofuranose, α-L-Glucofuranose, α-L-Mannofuranose, α-L-gulofuranose, α-L-idofuranose, α-L-galactofuranose, α-L-talofuranose, α-L-psicofuranose, α-L-fructofuranose, α-L-sorbofuranose, α-L-tagatofuranose, α-L-xylulofuranose, α-L-ribulofuranose, α-L-threofuranose, α-L-erythrofuranose, α-L-glucosamine, α-L-glucopyranuronic acid, β-L-ribopyranose, β-L-arabinopyranose, β-L-xylopyranose, β-L-lyxopyranose, β-L-allopyranose, β-L-altropyranose, β-L-glucopyranose, β-L-mannpyranose, β-L-glucopyranose, β-L-idopyranose, β-L-galactopyranose, β-L-talopyranose, β-L-psicopyranose, β-L-fructopyranose, β-L-sorbopyranose, β-L-tagatopyranose, β-L-ribofuranose, β-L-arabinofuranose, β-L-xylofuranose, β-L-lyxofuranose, β-L-allofuranose, β-L-altrofuranose, β-L-glucofuranose, β-L-mannofuranose, β-L-gulofuranose, β-L-idofuranose, β-L-galactofuranose, β-L-talofuranose, β-L-psicofuranose, β-L-fructofuranose, β-L-sorbofuranose, β-L-tagatofuranose, β-L-xylulofuranose, β-L-ribulofuranose, β-L-threofuranose, β-L-erythrofuranose, β-L-glucosamine, β-L-glucopyranuronic acid, and β-L-rhamnopyranose.
[0063] In another preferred embodiment of the invention, the carbohydrate monomers of the A-moiety and the CH moiety are selected independently of each other from the group comprising or consisting of the following α- and β-D-carbohydrates:
[0000]
[0064] According to the present invention these carbohydrate monomers as defined herein are abundant in an antigen and occur as linking building block by deprotonation of two hydrogen atoms of different hydroxyl groups and formation of a bond to the rest of the molecule of the antigen A and to the moiety L, respectively.
[0065] L represents a linker moiety which is covalently bound to any atom, especially any hetero atom and most preferably any oxygen atom of a former hydroxyl group of the carbohydrate monomers of the carbohydrate antigen. Moreover the linker L is covalently bound to any hetero atom of CH and especially any oxygen atom of a hydroxyl group of CH. Thus, the linker molecule interconnects between the antigen A and the carbonhydrate moiety CH. Further, according to the present invention the interconnection between the antigen A and the carbonhydrate moiety CH occurs as described herein preferably by activation of the carbohydrate monomers of the carbohydrate antigen a and/or by activation of the linker molecule. Thereby, in a preferred embodiment of the present invention it is not merely connected the antigen A with the carbonhydrate moiety CH via the linker L, but it is the interconnection between the antigen A and the carbonhydrate moiety CH already bond to the ceramid CA forming the inventive compounds of the general formula (I)
[0000] A[L-CH—CA] p (I).
[0066] The linker L can be subdivided into subunits -L 1 -, -L 2 - and -L 3 - and can be formed of the subunits alone or of combinations thereof. Therefore, L may represent -L 1 -L 2 -, -L 2 -, -L 2 -L 3 - or -L 1 -L 2 -L 3 -. The preferred order of connectivity in the above cases with A and CH is as follows: A-L 1 -L 2 -CH—, A-L 2 -CH—, A-L 2 -L 3 -CH— or A-L 1 -L 2 -L 3 -CH—. However, it is also possible that the different fragments such as -L 1 -L 2 -, -L 2 -, -L 2 -L 3 -, -L 3 -L 2 -L 3 -, -L 2 -L 3 -L 2 - or -L 1 -L 2 -L 3 - are aligned in all possible orders as long as the connection between the different parts is chemically reasonable and possible.
[0067] The linker L may be bound to the carbohydrate moiety in such a manner that this bond can be cleaved in cell, e.g. a B help cell, a T help cell, in order to release the fragment A-L on the one hand and the fragment —CH—CA on the other hand.
[0068] L may include the functionality or a fragment of the functionality derived from the activation of the carbohydrate monomers of the carbohydrate antigen. L is preferably covalently bound to any hetero atom (N, O, S) of the carbohydrate monomers of the carbohydrate antigen A. L 1 if present is covalently bound to the linker subunit L 2 preferably through the moiety Y, which could also be a chemical bond. L 1 is preferably selected from the following residues:
[0000]
[0000] x is an integer from 1 to 60;
Y represents a bond, —NH—, —O—, —S—, —S—S—;
L 2 represents —CH 2 —, —C 2 H 4 —, —C 3 H 6 —, —C 4 H 8 —, —C 5 H 10 —, —C 6 H 12 —, —C 7 H 14 —, —C 8 H 16 —, —C 9 H 18 —, —C 10 H 20 —, —CH(CH 3 )—, —C[(CH 3 ) 2 ]—, —CH 2 —CH(CH 3 )—, —CH(CH 3 )—CH 2 —, —CH(CH 3 )—C 2 H 4 —, —CH 2 —CH(CH 3 )—CH 2 —, —C 2 H 4 —CH(CH 3 )—, —CH 2 —C[(CH 3 ) 2 ]—, —C[(CH 3 ) 2 ]—CH 2 —, —CH(CH 3 )—CH(CH 3 )—, —C[(C 2 H 5 )(CH 3 )]—, —CH(C 3 H 7 )—, —(CH 2 —CH 2 —O) n —CH 2 —CH 2 —, —CO—CH 2 —, —CO—C 2 H 4 —, —CO—C 3 H 6 —, —CO—C 4 H 8 —, —CO—C 5 H 10 —, —CO—C 6 H 12 —, —CO—C 7 H 14 —, —CO—C 8 H 16 —, —CO—C 9 H 18 —, —CO—C 10 H 20 —, —CO—CH(CH 3 )—, —CO—C[(CH 3 ) 2 ]—, —CO—CH 2 —CH(CH 3 )—, —CO—CH(CH 3 )—CH 2 —, —CO—CH(CH 3 )—C 2 H 4 —, —CO—CH 2 —CH(CH 3 )—CH 2 —, —CO—C 2 H 4 —CH(CH 3 )—, —CO—CH 2 —C[(CH 3 ) 2 ]—, —CO—C[(CH 3 ) 2 ]—CH 2 —, —CO—CH(CH 3 )—CH(CH 3 )—, —CO—C[(C 2 H 5 )(CH 3 )]—, —CO—CH(C 3 H 7 )—, —CO—(CH 2 —CH 2 —O) n —CH 2 —CH 2 —. L 2 is in case L 3 is not present preferably linked to an oxygen atom of a former hydroxyl group of the carbohydrate residue CH.
[0069] n represents an integer from 1 to 60;
[0070] L 3 represents —CO—, —O—CO—, —NH—CO—, —NH(C═NH)—, —SO 2 —, —O—SO 2 —, —NH—, —NH—CO—CH 2 —. L 3 if present is preferably linked to an oxygen atom of a former hydroxyl group of the carbohydrate residue CH.
[0071] Preferred examples for linker moieties L of the moiety A-L-CH—CA as at least one representative of all moieties in the compounds of the general formula (I) as defined herein are
[0000]
[0000] wherein n is as defined herein, and A, CH and CA represent an antigen, a carbohydrate moiety and a ceramid as defined herein.
[0072] The linker molecule L may optionally be further substituted with 1 to 3 of the substituents Z 6 , Z 7 , Z 8 . However, it is clear to a skilled person that the term “can be substituted” refers to the replacement of a hydrogen atom by one of the substituents Z 6 , Z 7 , Z 8 .
[0073] The substituents Z 6 , Z 7 and Z 8 represent independently of each other —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O-cyclo-C 3 H 5 , —OCH(CH 3 ) 2 , —OC(CH 3 ) 3 , —OC 4 H 9 , —OPh, —OCH 2 -Ph, —OCPh 3 , —CH 2 —OCH 3 , —C 2 H 4 —OCH 3 , —C 3 H 6 —OCH 3 , —CH 2 —OC 2 H 5 , —C 2 H 4 —OC 2 H 5 , —C 3 H 6 —OC 2 H 5 , —CH 2 —OC 3 H 7 , —C 2 H 4 —OC 3 H 7 , —C 3 H 6 —OC 3 H 7 , —CH 2 —O-cyclo-C 3 H 5 , —C 2 H 4 —O-cyclo-C 3 H 5 , —C 3 H 6 —O-cyclo-C 3 H 5 , —CH 2 —OCH(CH 3 ) 2 , —C 2 H 4 —OCH(CH 3 ) 2 , —C 3 H 6 —OCH(CH 3 ) 2 , —CH 2 —OC(CH 3 ) 3 , —C 2 H 4 —OC(CH 3 ) 3 , —C 3 H 6 —OC(CH 3 ) 3 , —CH 2 —OC 4 H 9 , —C 2 H 4 —OC 4 H 9 , —C 3 H 6 —OC 4 H 9 , —CH 2 —OPh, —C 2 H 4 —OPh, —C 3 H 6 —OPh, —CH 2 —OCH 2 -Ph, —C 2 H 4 —OCH 2 -Ph, —C 3 H 6 —OCH 2 -Ph, —NO 2 , —F, —Cl, —Br, —COCH 3 , —COC 2 H 5 , —COC 3 H 7 , —CO-cyclo-C 3 H 5 , —COCH(CH 3 ) 2 , —COC(CH 3 ) 3 , —COOH, —COOCH 3 , —COOC 2 H 5 , —COOC 3 H 7 , —COO-cyclo-C 3 H 5 , —COOCH(CH 3 ) 2 , —COOC(CH 3 ) 3 , —OOC—CH 3 , —OOC—C 2 H 5 , —OOC—C 3 H 7 , —OOC-cyclo-C 3 H 5 , —OOC—CH(CH 3 ) 2 , —OOC—C(CH 3 ) 3 , —CONH 2 , —CONHCH 3 , —CONHC 2 H 5 , —CONHC 3 H 7 , —CONH-cyclo-C 3 H 5 , —CONH[CH(CH 3 ) 2 ], —CONH[C(CH 3 ) 3 ], —CON(CH 3 ) 2 , —CON(C 2 H 5 ) 2 , —CON(C 3 H 7 ) 2 , —CON(cyclo-C 3 H 5 ) 2 , —CON[CH(CH 3 ) 2 ] 2 , —CON[C(CH 3 ) 3 ] 2 , —NHCOCH 3 , —NHCOC 2 H 5 , —NHCOC 3 H 7 , —NHCO-cyclo-C 3 H 5 , —NHCO—CH(CH 3 ) 2 , —NHCO—C(CH 3 ) 3 , —NH 2 , —NHCH 3 , —NHC 2 H 5 , —NHC 3 H 7 , —NH-cyclo-C 3 H 5 , —NHCH(CH 3 ) 2 , —NHC(CH 3 ) 3 , —N(CH 3 ) 2 , —N(C 2 H 5 ) 2 , —N(C 3 H 7 ) 2 , —N(cyclo-C 3 H 5 ) 2 , —N[CH(CH 3 ) 2 ] 2 , —N[C(CH 3 ) 3 ] 2 , —OCF 3 , —CH 2 —OCF 3 , —C 2 H 4 —OCF 3 , —C 3 H 6 —OCF 3 , —OC 2 F 5 , —CH 2 —OC 2 F 5 , —C 2 H 4 —OC 2 F 5 , —C 3 H 6 —OC 2 F 5 , —CH 2 F, —CHF 2 , —CF 3 , —CH 2 Cl, —CH 2 Br, —CH 2 —CH 2 F, —CH 2 —CHF 2 , —CH 2 —CF 3 , —CH 2 —CH 2 Cl, —CH 2 —CH 2 Br.
The Carbohydrate Moiety CH
[0074] CH represents a monosaccharide, a disaccharide or a trisaccharide, wherein the carbohydrate monomers thereof preferably belong to hexoses, pentoses, tetroses. In case CH represents a monosaccharide, the carbohydrate monomer is identical to the monosaccharide. The disaccharide contains two carbohydrate monomers and the trisaccharide contains three carbohydrate monomers. In the disaccharide and trisaccharide the carbohydrate monomers are connected to each other via a/13 glycosidic bonds which preferably belong to the group consisting of 1,2; 1,3; 1,4; 1,5; 1,6; 2,2; 2,3; 2,4; 2,5; or 2,6 glycosidic bonds.
[0075] The monosaccharide, the disaccharide and the trisaccharide CH are covalently bound to L and also to CA via a heteroatom (N, O, S) of the CH moiety and most preferably through an oxygen atom of a former hydroxyl group of CH.
[0076] As used herein the term “former hydroxyl group” means that the oxygen atom of a carbohydrate monomer which is now linked to L or CA was the oxygen atom of a hydroxyl group and linked to a hydrogen atom which is now replaced by the residue L or CA.
[0077] In a preferred embodiment of this invention, the monosaccharide, the disaccharide or the trisaccharide CH is covalently bound by one oxygen atom to L and through another oxygen atom to CA.
[0078] In another preferred embodiment of this invention, the monosaccharide, the disaccharide or the trisaccharide CH is covalently bound by one hydroxyl oxygen atom to L and through another hydroxyl oxygen atom to CA.
[0079] In another preferred embodiment of this invention, L or CA is bound to CH, i.e. to the monosaccharide, the disaccharide or the trisaccharide, by a glycosidic bond at C1 of the saccharide.
[0080] In a more preferred embodiment of this invention, L is bound by a glycosidic bond to C1 of the monosaccharide, the disaccharide or the trisaccharide and CA is bound by the oxygen at C6 of a hexose or by the oxygen at C5 of a pentose or by the oxygen at C4 of a tetrose.
[0081] In another more preferred embodiment of this invention, CA is bound by a glycosidic bond to C1 of the monosaccharide, the disaccharide or the trisaccharide and L is bound by the oxygen at C6 of a hexose or by the oxygen at C5 of a pentose or by the oxygen at C4 of a tetrose.
[0082] In a preferred embodiment of the invention, the monosaccharide, the disaccharide or the trisaccharide CH consists of one, two or respectively 3 carbohydrates selected from the following group comprising or consisting of the following α- and β-D/L-carbohydrates:
[0000] α-D-ribopyranose, α-D-arabinopyranose, α-D-xylopyranose, α-D-lyxopyranose, α-D-allopyranose, α-D-altropyranose, α-D-glucopyranose, α-D-mannpyranose, α-D-glucopyranose, α-D-idopyranose, α-D-galactopyranose, α-D-talopyranose, α-D-psicopyranose, α-D-fructopyranose, α-D-sorbopyranose, α-D-tagatopyranose, α-D-ribofuranose, α-D-arabinofuranose, α-D-xylofuranose, α-D-lyxofuranose, α-D-Allofuranose, α-D-Altrofuranose, α-D-Glucofuranose, α-D-Mannofuranose, α-D-gulofuranose, α-D-idofuranose, α-D-galactofuranose, α-D-talofuranose, α-D-psicofuranose, α-D-fructofuranose, α-D-sorbofuranose, α-D-tagatofuranose, α-D-xylulofuranose, α-D-ribulofuranose, α-D-threofuranose, α-D-erythrofuranose, α-D-glucosamine, α-D-glucopyranuronic acid, α-D-rhamnopyranose, β-D-ribopyranose, β-D-arabinopyranose, β-D-xylopyranose, β-D-lyxopyranose, β-D-allopyranose, β-D-altropyranose, β-D-glucopyranose, β-D-mannpyranose, β-D-glucopyranose, β-D-idopyranose, β-D-galactopyranose, β-D-talopyranose, β-D-psicopyranose, β-D-fructopyranose, β-D-sorbopyranose, β-D-tagatopyranose, β-D-ribofuranose, β-D-arabinofuranose, β-D-xylofuranose, β-D-lyxofuranose, β-D-allofuranose, β-D-altrofuranose, β-D-glucofuranose, β-D-mannofuranose, β-D-gulofuranose, β-D-idofuranose, β-D-galactofuranose, β-D-talofuranose, β-D-psicofuranose, β-D-fructofuranose, β-D-sorbofuranose, β-D-tagatofuranose, β-D-xylulofuranose, β-D-ribulofuranose, β-D-threofuranose, β-D-erythrofuranose, β-D-rhamnopyranose, β-D-glucosamine, β-D-glucopyranuronic acid, α-L-ribopyranose, α-L-arabinopyranose, α-L-xylopyranose, α-L-lyxopyranose, α-L-allopyranose, α-L-altropyranose, α-L-glucopyranose, α-L-mannpyranose, α-L-glucopyranose, α-L-idopyranose, α-L-galactopyranose, α-L-talopyranose, α-L-psicopyranose, α-L-fructopyranose, α-L-sorbopyranose, α-L-tagatopyranose, α-L-ribofuranose, α-L-arabinofuranose, α-L-xylofuranose, α-L-lyxofuranose, α-L-Allofuranose, α-L-Altrofuranose, α-L-Glucofuranose, α-L-Mannofuranose, α-L-gulofuranose, α-L-idofuranose, α-L-galactofuranose, α-L-talofuranose, α-L-psicofuranose, α-L-fructofuranose, α-L-sorbofuranose, α-L-tagatofuranose, α-L-xylulofuranose, α-L-ribulofuranose, α-L-rhamnopyranose α-L-threofuranose, α-L-erythrofuranose, α-L-glucosamine, α-L-glucopyranuronic acid, β-L-ribopyranose, β-L-arabinopyranose, β-L-xylopyranose, β-L-lyxopyranose, β-L-allopyranose, β-L-altropyranose, β-L-glucopyranose, β-L-mannpyranose, β-L-glucopyranose, β-L-idopyranose, β-L-galactopyranose, β-L-talopyranose, β-L-psicopyranose, β-L-fructopyranose, β-L-sorbopyranose, β-L-tagatopyranose, β-L-ribofuranose, β-L-arabinofuranose, β-L-xylofuranose, β-L-lyxofuranose, β-L-allofuranose, β-L-altrofuranose, β-L-glucofuranose, β-L-mannofuranose, β-L-gulofuranose, β-L-idofuranose, β-L-galactofuranose, β-L-talofuranose, β-L-psicofuranose, β-L-fructofuranose, β-L-sorbofuranose, β-L-tagatofuranose, β-L-xylulofuranose, β-L-ribulofuranose, β-L-threofuranose, β-L-erythrofuranose, β-L-glucosamine, β-L-glucopyranuronic acid, and β-L-rhamnopyranose.
[0083] In another preferred embodiment of the invention, the monosaccharide, the disaccharide or the trisaccharide CH consists of one, two or respectively 3 carbohydrates selected from the α- and β-D/L-carbohydrates as mentioned on pages 25-29 and as defined for the A-moiety.
[0084] The monosaccharide, the disaccharide or the trisaccharide CH according to the present invention may further be substituted at specific positions, preferably at hydroxyl groups not involved in the bonding to the moieties A and L, or at an amino group if present in the saccharide moiety. In a preferred embodiment of the present invention the monosaccharide, the disaccharide or the trisaccharide CH bear one of the following substituents, preferably instead of a hydrogen atom at a hydroxyl groups one of the following substituents:
[0000] —CH 3 , —C 2 H 5 , —C 3 H 7 , -cyclo-C 3 H 5 , —CH(CH 3 ) 2 , —C(CH 3 ) 3 , —C 4 H 9 , -Ph, —CH 2 -Ph, —CH 2 —OCH 3 , —C 2 H 4 —OCH 3 , —C 3 H 6 —OCH 3 , —CH 2 —OC 2 H 5 , —C 2 H 4 —OC 2 H 5 , —C 3 H 6 —OC 2 H 5 , —CH 2 —OC 3 H 7 , —C 2 H 4 —OC 3 H 7 , —C 3 H 6 —OC 3 H 7 , —CH 2 —O-cyclo-C 3 H 5 , —C 2 H 4 —O-cyclo-C 3 H 5 , —C 3 H 6 —O-cyclo-C 3 H 5 , —CH 2 —OCH(CH 3 ) 2 , —C 2 H 4 —OCH(CH 3 ) 2 , —C 3 H 6 —OCH(CH 3 ) 2 , —CH 2 —OC(CH 3 ) 3 , —C 2 H 4 —OC(CH 3 ) 3 , —C 3 H 6 —OC(CH 3 ) 3 , —CH 2 —OC 4 H 9 , —C 2 H 4 —OC 4 H 9 , —C 3 H 6 —OC 4 H 9 , —CH 2 —OPh, —C 2 H 4 —OPh, —C 3 H 6 —OPh, —CH 2 —OCH 2 -Ph, —C 2 H 4 —OCH 2 -Ph, —C 3 H 6 —OCH 2 -Ph.
[0085] Preferred α- and β-D/L-carbohydrates for the moiety CH with indicated connectivity by the dotted lines are the following residues:
[0000]
[0086] The substituents Q 1 , Q 2 , Q 3 and Q 6 have the meanings as defined herein.
[0087] In other preferred embodiments of the invention the CH moiety of the inventive carbohydrate-glycolipid conjugates has the following connectivity:
[0000]
[0000] wherein the A, L, p and CA are defined as disclosed herein.
[0088] R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 represent independently of each other:
[0000] —H, —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O—SO 2 —CH 3 , —O—SO 2 —C 2 H 5 , —O—SO 2 —C 3 H 7 , —O—COOCH 3 , —NHCOCH 3 , or —NH 2 .
[0089] In more preferred embodiments of the invention the CH moiety of the inventive carbohydrate-glycolipid conjugates has the following connectivity as shown in the following preferred formula
[0000]
[0000] wherein the A, L, p and CA are defined as disclosed herein.
[0090] The glycosidic bonds within CH belong preferably to the group of glycosidic bonds wherein the hydroxyl function of the anomeric carbon is condensed with another hydroxyl function of another carbohydrate or of the CA moiety respectively. The glycosidic bond between two carbohydrates comprises the glycosidic bond between the anomeric carbon of one carbohydrate and the non-anomeric carbon of the other carbohydrate. Due to the stereochemistry of the anomeric carbon there is the possibility to form a or -glycosidic bonds such as:
[0000]
[0091] The Greek letters α and β are applicable only when the anomeric carbon atom has a lower locant than the anomeric reference atom. If this is not the case then the anomeric configuration is described by normal R/S-symbols.
The Ceramide Moiety CA
[0092] CA represents
[0000]
[0000] and more preferably
[0000]
[0000] or
CA represents
[0000]
[0000] and more preferably
[0000]
[0000] or
CA represents
[0000]
[0000] and more preferably
[0000]
[0000] R* and R# represent independently of each other a linear or branched or cyclic, substituted or unsubstituted, saturated or unsaturated carbon residue consisting of 1 to 30 carbon atoms and up to 5 hetero atoms selected from N, O, S, F, Br and Cl.
[0093] Thus, R* and R# represent independently of each other a carbon residue of 1-30 carbon atoms, wherein the carbon residue may be a linear carbon chain or a branched carbon chain. The carbon residue may also contain carbocyclic structures or heterocyclic structures. The carbon residue may furthermore contain heteroatoms such as N, O, S and/or may have functional groups such as halogen like F, Cl and Br or functional groups containing the hetero atoms N, O, and/or S or functional groups such as double bonds and triple bonds.
[0094] The carbon residue or the carbon chain may contain one or more C═C double bonds and/or one or more C≡C triple bonds. The carbocyclic structures which might be present in the carbon residue or the carbon chain are, for instance, saturated 3-membered or 4-membered carbocyclic rings, saturated or unsaturated 5-membered carbocyclic rings or saturated, unsaturated or aromatic 6-membered carbocyclic rings which can be present as substituents on the carbon residue or carbon chain or can be incorporated into the carbon residue or carbon chain.
[0095] The heterocyclic structures which might be present in the carbon residue or the carbon chain are, for instance, saturated 3-membered or 4-membered heterocyclic rings containing one N or O atom, saturated or unsaturated 5-membered heterocyclic rings containing 1, 2, 3 or 4 N atoms or 1 or 2 S or O atoms or 1 O or S atom together with 1 or 2 N atoms or saturated, unsaturated or aromatic 6-membered heterocyclic rings containing 1, 2, 3 or 4 N atoms or 1 or 2 S or O atoms or 1 O or S atom together with 1 or 2 N atoms which can be present as substituents on the carbon residue or carbon chain or can be incorporated into the carbon residue or carbon chain.
[0096] The term “carbon residue of 1 to 30 carbon atoms” refers to one carbon atom or a chain of 2 to 30 carbon atoms which can be straight aligned (linear) by a suitable chemical bond or arranged in such an order that from 1 carbon atom two or three individual carbon atoms are bound (branched), and optionally proceed in different directions from the branching carbon atom. Further, the arrangement of the carbon atoms may also form a ring shape (cyclic). Also, any of the above mentioned arrangements of carbon atoms forming a carbon residue may include one or more double or triple bonds (unsaturated). In case the chain of carbon atoms does not include any double or triple bond the carbon residue is considered saturated. Optionally the “carbon residue of 1 to 30 carbon atoms” can be further substituted with 1 to 5 of the substituents Z 1 , Z 2 , Z 3 , Z 4 , Z 5 . However it is clear to a skilled person that the term “can be substituted” refers to the replacement of a hydrogen atom by one of the substituents Z 1 , Z 2 , Z 3 , Z 4 , Z 5 each. In case the carbon residue of 1 to 30 carbon atoms does not contain any of the additional substituents Z 1 , Z 2 , Z 3 , Z 4 , Z 5 the residue is considered as unsubstituted.
[0097] More preferably R* and R# represent independently of each other linear or branched C 1 -C 30 -alkyl residue, a linear or branched C 2 -C 30 -alkenyl residue, a linear or branched C 2 -C 30 -alkynyl residue, a C 3 -C 10 -carbocycloalkyl residue, a C 4 -C 30 -alkylcycloalkyl, a C 4 -C 30 -alkylheterocycloalkyl residue, or a substituted C 1 -C 30 -carbon residue containing 1 to 5 of the substituents Z 1 , Z 2 , Z 3 , Z 4 , Z 5 .
[0098] The substituents Z 1 , Z 2 , Z 3 , Z 4 , and Z 5 represent independently of each other —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O-cyclo-C 3 H 5 , —OCH(CH 3 ) 2 , —OC(CH 3 ) 3 , —OC 4 H 9 , —OPh, —OCH 2 -Ph, —OCPh 3 , —CH 2 —OCH 3 , —C 2 H 4 —OCH 3 , —C 3 H 6 —OCH 3 , —CH 2 —OC 2 H 5 , —C 2 H 4 —OC 2 H 5 , —C 3 H 6 —OC 2 H 5 , —CH 2 —OC 3 H 7 , —C 2 H 4 —OC 3 H 7 , —C 3 H 6 —OC 3 H 7 , —CH 2 —O-cyclo-C 3 H 5 , —C 2 H 4 —O-cyclo-C 3 H 5 , —C 3 H 6 —O-cyclo-C 3 H 5 , —CH 2 —OCH(CH 3 ) 2 , —C 2 H 4 —OCH(CH 3 ) 2 , —C 3 H 6 —OCH(CH 3 ) 2 , —CH 2 —OC(CH 3 ) 3 , —C 2 H 4 —OC(CH 3 ) 3 , —C 3 H 6 —OC(CH 3 ) 3 , —CH 2 —OC 4 H 9 , —C 2 H 4 —OC 4 H 9 , —C 3 H 6 —OC 4 H 9 , —CH 2 —OPh, —C 2 H 4 —OPh, —C 3 H 6 —OPh, —CH 2 —OCH 2 -Ph, —C 2 H 4 —OCH 2 -Ph, —C 3 H 6 —OCH 2 -Ph, —NO 2 , —F, —CI, —Br, —COCH 3 , —COC 2 H 5 , —COC 3 H 7 , —CO-cyclo-C 3 H 5 , —COCH(CH 3 ) 2 , —COC(CH 3 ) 3 , —COOH, —COOCH 3 , —COOC 2 H 5 , —COOC 3 H 7 , —COO-cyclo-C 3 H 5 , —COOCH(CH 3 ) 2 , —COOC(CH 3 ) 3 , —OOC—CH 3 , —OOC—C 2 H 5 , —OOC—C 3 H 7 , —OOC-cyclo-C 3 H 5 , —OOC—CH(CH 3 ) 2 , —OOC—C(CH 3 ) 3 , —CONH 2 , —CONHCH 3 , —CONHC 2 H 5 , —CONHC 3 H 7 , —CONH-cyclo-C 3 H 5 , —CONH[CH(CH 3 ) 2 ], —CONH[C(CH 3 ) 3 ], —CON(CH 3 ) 2 , —CON(C 2 H 5 ) 2 , —CON(C 3 H 7 ) 2 , —CON(cyclo-C 3 H 5 ) 2 , —CON[CH(CH 3 ) 2 ] 2 , —CON[C(CH 3 ) 3 ] 2 , —NHCOCH 3 , —NHCOC 2 H 5 , —NHCOC 3 H 7 , —NHCO-cyclo-C 3 H 5 , —NHCO—CH(CH 3 ) 2 , —NHCO—C(CH 3 ) 3 , —NH 2 , —NHCH 3 , —NHC 2 H 5 , —NHC 3 H 7 , —NH-cyclo-C 3 H 5 , —NHCH(CH 3 ) 2 , —NHC(CH 3 ) 3 , —N(CH 3 ) 2 , —N(C 2 H 5 ) 2 , —N(C 3 H 7 ) 2 , —N(cyclo-C 3 H 5 ) 2 , —N[CH(CH 3 ) 2 ] 2 , —N[C(CH 3 ) 3 ] 2 , —OCF 3 , —CH 2 —OCF 3 , —C 2 H 4 —OCF 3 , —C 3 H 6 —OCF 3 , —OC 2 F 5 , —CH 2 —OC 2 F 5 , —C 2 H 4 —OC 2 F 5 , —C 3 H 6 —OC 2 F 5 , —CH 2 F, —CHF 2 , —CF 3 , —CH 2 Cl, —CH 2 Br, —CH 2 —CH 2 F, —CH 2 —CHF 2 , —CH 2 —CF 3 , —CH 2 —CH 2 Cl, —CH 2 —CH 2 Br.
[0099] The term “linear or branched C 1 -C 30 -alkyl residue” refers to a residue which is linked through a carbon atom and which consists in total of 1 to 30 carbon atoms including the carbon atoms of the branches. The same definition applies accordingly to the terms “linear C 20 -C 30 -alkyl residue”, “linear C 1 -C 10 -alkyl residue” and “linear C 10 -C 19 -alkyl residue”,
[0100] The term “linear or branched C 2 -C 30 -alkenyl residue” refers to a residue which is linked through a carbon atom and which consists in total of 2 to 30 carbon atoms including the carbon atoms of the branches and which has at least one but not more than 15 double bonds. If branched, the longest carbon chain is the main chain while the side chains are the branches. The 1 to 15 C═C double bonds may be present in the main chain and/or the side chain(s).
[0101] The term “linear or branched C 2 -C 30 -alkynyl residue” refers to a residue which is linked through a carbon atom and which consists in total of 2 to 30 carbon atoms including the carbon atoms of the branches and which has at least one but not more than 15 triple bonds and preferably 1, 2 or 3 triple bonds. If branched, the longest carbon chain is the main chain while the side chains are the branches. The 1 to 15 C≡C triple bonds may be present in the main chain and/or the side chain(s).
[0102] The term “C 3 -C 10 -carbocycloalkyl residue” refers to a residue which is linked through a ring carbon atom and contains at least one carbocyclic ring and which consists in total of 3 to 10 carbon atoms including the carbon atoms of any alkyl, alkenyl or alkinyl substituent. The carbocyclic ring in the C 3 -C 10 -carbocycloalkyl residue can be saturated, partly unsaturated or fully unsaturated and might be aromatic. If the carbocyclic ring is part of a bicyclic ring or is connected to another ring, both carbocyclic rings may be saturated or unsaturated and might be aromatic or one ring is saturated and the second ring is partly or fully unsatured.
[0103] Examples for preferred C 3 -C 10 -carbocycloalkyl residues to which it is also referred to as substituents M 1 are as follows:
[0000]
[0104] The term “C 4 -C 30 -alkylcycloalkyl” refers to a residue which is linked through a carbon atom not part of the carbocyclic ring and contains at least one carbocyclic ring and which consists in total of 4 to 30 carbon atoms including the carbon atoms of any alkyl, alkenyl or alkinyl substituent. The carbocyclic ring in the C 4 -C 30 -carbocycloalkyl residue can be saturated, partly unsaturated or fully unsaturated and might be aromatic. If the carbocyclic ring is part of a bicyclic ring or is connected to another ring, both carbocyclic rings may be saturated or unsaturated and might be aromatic or one ring is saturated and the second ring is partly or fully unsatured.
[0105] The term “C 4 -C 30 -alkylheterocycloalkyl residue” refers to a residue which is linked through a carbon atom not part of the heterocyclic ring and contains at least one heterocyclic ring and which consists in total of 4 to 30 carbon atoms including the carbon atoms of any alkyl, alkenyl or alkinyl substituent. The heterocyclic ring in the C 4 -C 30 -alkylheterocycloalkyl residue can be saturated, partly unsaturated or fully unsaturated and might be aromatic. 1 or 2 oxygen atoms can be attached to the heterocyclic ring thus forming one or two carbonyl groups. If the heterocyclic ring is part of a bicyclic ring or is connected to another ring which can be a carbocyclic or heterocyclic ring, both rings may be saturated or unsaturated and might be aromatic or one ring is saturated and the second ring is partly or fully unsatured and might be aromatic. The heterocyclic ring contains 1 or 2 O atoms, 1 or 2 S atoms, 1, 2, 3, or 4 N atoms, 1 O and 1 or 2 N atoms or 1 S and 1 or 2 N atoms. Examples for such 0C 4 -C 30 -alkylheterocycloalkyl residues are:
[0000]
[0106] The term “substituted C 1 -C 30 -carbon residue containing 1 to 5 of the substituents Z 1 , Z 2 , Z 3 , Z 4 , Z 5 ” refers to a residue which is linked through a carbon atom and which consists in total of 1 to 30 carbon atoms including the carbon atoms of any substituent such as alkyl, alkenyl, alkinyl, Z 1 , Z 2 , Z 3 , Z 4 , and/or Z 5 substituent. The residue bears 1 to 5 of the substituents Z 1 , Z 2 , Z 3 , Z 4 , Z 5 and can be linear or branched and saturated or unsaturated. Thus in addition to the at least one substituent Z 1 , the residue may contain one or more C═C double bonds and/or one or more C≡C triple bonds. Moreover the substituted C 1 -C 30 -carbon residue may contain 1 to 10 hetero atoms N, O, S in the carbon chain or attached to the carbon chain. One or more oxygen atoms might be attached to the carbon chain thus forming one or more carbonyl groups. If branched, the longest chain is the main chain while the side chains are the branches. The carbonyl functionalities, the double bonds, the triple bonds as well as the substituents Z 1 , Z 2 , Z 3 , Z 4 , Z 5 can be present in or on the main chain and also in or on the side chain(s). Examples for such substituted C 1 -C 30 -carbon residue are:
[0000]
[0107] In a preferred embodiment of the invention the residues R* and R# represent independently of each other:
[0000] —CH 3 , —(CH 2 ) r —CH 3 , —CH(OH)—(CH 2 )—CH 3 , —CH═CH—CH 3 , —CH═CH—(CH 2 ) t —CH 3 , —CH(OH)—(CH 2 ) v —CH(CH 3 ) 2 , —CH(OH)—(CH 2 ) w —CH(CH 3 )—CH 2 —CH 3 , —(CH 2 ) a —CH═CH—(CH 2 ) b —CH 3 , —(CH 2 ) c —CH═CH—(CH 2 ) d —CH═CH—(CH 2 ) e —CH 3 , —(CH 2 ) f —CH═CH—(CH 2 ) g —CH═CH—(CH 2 ) h —CH═CH—(CH 2 ) i —CH 3 , —(CH 2 ) j —CH═CH—(CH 2 ) k —CH═CH—(CH 2 ) l —CH═CH—(CH 2 ) o —CH═CH(CH 2 ) q CH 3 ,
wherein a, b, c, d, e, f, g, h, i, j, k, l, o, q are integers from 1 to 26 with the proviso that: (a+b)≦27; (c+d+e)≦25; (f+g+h+i)≦23; (j+k+l+o+q)≦21; and wherein r is an integer from 1 to 29, s is an integer from 1 to 28, t is an integer from 1 to 27, v is an integer from 1 to 26, and w is an integer from 1 to 25 and furthermore —(CH═CH—CH 2 ) q —CH 3 , —(CH 2 —CH═CH) q —CH 3 , —(CH═CH) A —CH 3 ,
wherein q is an integer from 1 to 9, A is an integer from 1 to 14 and furthermore —(CH═CH—CH 2 ) B —(CH 2 ) C —CH 3 , —(CH 2 —CH═CH) B —(CH 2 ) C —CH 3 , —(CH═CH) D —(CH 2 ) E —CH 3 , —(CH 2 ) E —(CH═CH) D —CH 3 , —(CH 2 ) F —(CH═CH) G —(CH 2 ) H —CH 3 , —(CH 2 ) J —(CH═CH—CH 2 ) K —(CH 2 ) N —CH 3 , —(CH 2 ) P —(CH═CH) Q —(CH 2 ) R —(CH═CH) S —(CH 2 ) T —CH 3 , —(CH 2 ) U —(CH═CH—CH 2 ) V —(CH 2 ) W —(CH═CH—CH 2 ) X —(CH 2 ) Y —CH Z ,
wherein B, C, D, E, F, G, H; I, J, K, L, M, N, P, Q, R, S, T, U, V, W, X, Y and Z represent independently from each other an integer between 1 and 26 with the proviso that the total number of carbon atoms of the afore-mentioned residues does not exceed 30.
[0108] In another preferred embodiment of the invention the residues R* and R# represent independently of each other:
[0000] ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, dodecyl, tetradecyl, cis-9-tetradecenyl, cis-9-hexadecenyl, cis-6-octadecenyl, cis-9-octadecenyl, cis-11-octadecenyl, cis-9-eicosenyl, cis-11-eicosenyl, cis-13-docosenyl, cis-15-tetracosenyl, trans-9-octadecenyl, trans-11-octadecenyl, trans-3-hexadecenyl, 9,12-octadecadienyl, 6,9,12-octadecatrienyl, 8,11,14-eicosatrienyl, 5,8,11,14-eicosatetraenyl, 7,10,13,16-docosatetraenyl, 4,7,10,13,16-docosapentaenyl, 9,12,15-octadecatrienyl, 6,9,12,15-octadecatetraenyl, 8,11,14,17-eicosatetraenyl, 5,8,11,14,17-eicosapentaenyl, 7,10,13,16,19-docosapentaenyl, 4,7,10,13,16,19-docosahexaenyl, 5,8,11-eicosatrienyl, 9c 11t 13t eleostearyl, 8t 10t 12c calendyl, 9c 11t 13c catalpyl, cis-9 tetradecenyl, cis-9-hexadecenyl, cis-6-octadecenyl, cis-9-octadecenyl, cis-11-octadecenyl, cis-9-eicosenyl, cis-11-eicosenyl, cis-13-docosenyl, cis-15-tetracosenyl, 9,12-octadecadienyl, 6,9,12-octadecatrienyl, 8,11,14-eicosatrienyl, 5,8,11,14-eicosatetraenyl, 7,10,13,16-docosatetraenyl, 4,7,10,13,16 docosapentaenyl, 9,12,15-octadecatrienyl, 6,9,12,15-octadecatetraenyl, 8,11,14,17-eicosatetraenyl, 5,8,11,14,17-eicosapentaenyl, 7,10,13,16,19-docosapentacnyl, 4,7,10,13,16,19-docosahexaenyl, 5,8,11-eicosatrienyl, 1,2-dithiolane-3-pentanyl, 6,8-dithiane octanyl, docosaheptadecanyl, eleostearyl, calendyl, catalpyl, taxoleyl, pinolenyl, sciadonyl, retinyl, 14-methyl pentadecanyl, pristanyl, phytanyl, 11,12-methyleneoctadecanyl, 9,10-methylenehexadecanyl, 9,10-epoxystearyl, 9,10-epoxyoctadec-12-enyl, 6-octadecynyl, t11-octadecen-9-ynyl, 9-octadecynyl, 6-octadecen-9-ynyl, t10-heptadecen-8-ynyl, 9-octadecen-12-ynyl, t7,t11-octadecadiene-9-ynyl, t8,t10-octadecadiene-12-ynyl, 5,8,11,14-eicosatetraynyl, 2-hydroxytetracosanyl, 2-hydroxy-15-tetracosenyl, 12-hydroxy-9-octadecenyl or 14-hydroxy-11-eicosenyl, 4,7,9,11,13,16,19-docosaheptadecanyl, 6-octadecynyl, t11-octadecen-9-ynyl, isopalmityl, 9,10-methylenhexadecyl, coronaryl, (R,S)-lipoyl, 6,8-bis(methylsulfanyl)-octanyl, 4,6-bis(methylsulfanyl)-hexanyl, 2,4-bis(methylsulfanyl)-butanyl, 1,2-dithiolanyl, cerebronyl, hydroxynervonyl, ricinyl, lesqueryl, brassylyl, thapsyl, dodecyl, hexadecyl, octadecyl, eicosanyl, docosanyl, tetracosanyl, cis-9-tetradecenyl, cis-9-hexadecenyl, cis-6-octadecenyl, cis-9-octadecenyl, cis-11-octadecenyl, cis-9-eicosenyl, cis-11-eicosenyl, cis-13-docosenyl, cis-15-tetracosenyl, 9,12-octadecadienyl, 6,9,12-octadecatrienyl, 8,11,14-eicosatrienyl, 5,8,11,14-eicosatetraenyl, 7,10,13,16-docosatetraenyl, 4,7,10,13,16-docosapentaenyl, 9,12,15-octadecatrienyl, 6,9,12,15-octadecatetraenyl, 8,11,14,17-eicosatetraenyl, 5,8,11,14,17-eicosapentaenyl, 7,10,13,16,19-docosapentaenyl, 4,7,10,13,16,19-docosahexaenyl, 5,8,11-eicosatrienyl, 1,2-dithiolane-3-pentanyl, 6,8-dithiane octanyl, docosaheptadecanyl, eleostearyl, calendyl, catalpyl, taxoleyl, pinolenyl, sciadonyl, retinyl, 14-methyl pentadecanyl, pristanyl, phytanyl, 11,12-methyleneoctadecanyl, 9,10-methylenehexadecanyl, 9,10-epoxystearyl, 9,10-epoxyoctadec-12-enyl, 6-octadecynyl, t11-octadecen-9-ynyl, 9-octadecynyl, 6-octadecen-9-ynyl, t10-heptadecen-8-ynyl, 9-octadecen-12-ynyl, t7,t11-octadecadiene-9-ynyl, t8,t10-octadecadiene-12-ynyl, 5,8,11,14-eicosatetraynyl, 2-hydroxytetracosanyl, 2-hydroxy-15-tetracosenyl, 12-hydroxy-9-octadecenyl, and 14-hydroxy-11-eicosenyl.
[0109] In another preferred embodiment of the invention the residues R* and R# are independently of each other substituted with a phenyl ring, preferably an unsubstituted phenyl ring. Further, it is preferred that said phenyl ring is positioned at the residues R* and R# at the opposite end where the residues R* and R# are bond to the rest of the moiety CA.
[0110] Also, in a preferred embodiment of the present invention the residues R* and R# are the same, preferably a linear alkyl residue, and more preferably a linear C 10 -C 30 -alkyl residue, and most preferably a linear —C 14 H 29 .
[0111] In another preferred embodiment of the present invention the residues R* and R# are different from each other and represent different linear alkyl residues, preferably the residue R* represents a linear C 20 -C 30 -alkyl residue and the residue R# represents a linear C 10 -C 19 -alkyl residue, and more preferably R* represents a linear —C 25 H 51 residue and the residue R# represents a linear —C 14 H 29 residue.
[0112] In another preferred embodiment of the present invention the residues R* and R# are different from each other and represent different linear alkyl residues, preferably the residue R* represents a linear C 1 -C 10 -alkyl residue and the residue R# represents a linear C 10 -C 19 -alkyl residue, and more preferably R* represents a linear —C 4 H 9 residue and the residue R# represents a linear —C 14 H 29 residue.
[0113] Yet, in another preferred embodiment of the present invention the residues R* and R# are different from each other and represent different linear alkyl residues, wherein the residues R* is further substituted with a phenyl ring, preferably the residue R* represents a phenyl-substituted linear C 1 -C 10 -alkyl residue and the residue R# represents a linear C 10 -C 19 -alkyl residue, and more preferably R* represents a linear —C 6 H 12 -Ph residue and the residue R# represents a linear —C 14 H 29 residue. In another preferred embodiment of the present invention the residues R* and R# are different from each other and represent different linear alkyl residues, preferably the residue R* represents a linear C 20 -C 30 -alkyl residue and the residue R# represents a linear C 1 -C 10 -alkyl residue, and more preferably R* represents a linear —C 25 H 51 residue and the residue R# represents a linear —C 5 H 11 residue.
[0114] The following formulas (II, III, IV and V) of the general formula (I) are preferred:
[0000]
[0000] wherein
A, L, R*, R# and p have the meanings as defined herein.
R 1 , R 2 , R 3 represent independently of each other: —H, —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O—SO 2 —CH 3 , —O—SO 2 —C 2 H 5 , —O—SO 2 —C 3 H 7 , —O—COOCH 3 , —NHCOCH 3 , —NH 2 ,
[0115] Furthermore, the following formulas (VI, VII, VIII, IX) of the general formula (I) are preferred:
[0000]
[0000] wherein
A, L, R*, R# and p have the meanings as defined herein.
R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 represent independently of each other: —H, —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O—SO 2 —CH 3 , —O—SO 2 —C 2 H 5 , —O—SO 2 —C 3 H 7 , —O—COOCH 3 , —NHCOCH 3 , —NH 2 ,
[0116] In a specifically preferred embodiment of the present invention the following subformulas (IIb, IIIb, IVb and Vb) of the general formula (I) are preferred:
[0000]
[0000] wherein
A, L, R*, R# and p have the meanings as defined herein.
R 1 , R 2 , R 3 represent independently of each other: —H, —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O—SO 2 —CH 3 , —O—SO 2 —C 2 H 5 , —O—SO 2 —C 3 H 7 , —O—COOCH 3 , —NHCOCH 3 , —NH 2 ,
G represents —NH—, —O—, —S—,
[0117] Furthermore, the following subformulas (VIb, VIIb, VIIIb, IXb) of the general formula (I) are preferred:
[0000]
[0000] wherein
A, L, R*, R# and p have the meanings as defined herein.
R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 represent independently of each other: —H, —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O—SO 2 —CH 3 , —O—SO 2 —C 2 H 5 , —O—SO 2 —C 3 H 7 , —O—COOCH 3 , —NHCOCH 3 , —NH 2 ,
G represents —NH—, —O—, —S—,
[0118] Furthermore the following substructures (X, XI, XII, XIII) of the general structure (I) are preferred:
[0000]
[0000] wherein
A, L, R*, R# and p have the meanings as defined herein.
[0119] Furthermore the following substructures (XIV, XV, XVI, XVII) of the general structure (I) are preferred:
[0000]
[0000] wherein
A, L, R*, R# and p have the meanings as defined herein.
[0120] Furthermore the following substructures (XVIII, XIX, XX) of the general structure (I) are preferred:
[0000]
[0000] wherein
A, L and p have the meanings as defined herein.
R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 represent independently of each other: —H, —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O—SO 2 —CH 3 , —O—SO 2 —C 2 H 5 , —O—SO 2 —C 3 H 7 , —O—COOCH 3 , —NHCOCH 3 , —NH 2 ,
[0121] In a specifically preferred embodiment of the present invention the following substructures (XVIIb, XIXb, XXb) of the general structure (I) are preferred:
[0000]
[0000] wherein
A, L and p have the meanings as defined herein.
R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 represent independently of each other: —H, —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O—SO 2 —CH 3 , —O—SO 2 —C 2 H 5 , —O—SO 2 —C 3 H 7 , —O—COOCH 3 , —NHCOCH 3 , —NH 2 , G represents —NH—, —O—, —S—,
[0122] Furthermore the following substructures (XXI, XXII, XXIII, XXIV) of the general structure (I) are preferred:
[0000]
[0000] wherein
A, L and p have the meanings as defined herein.
[0123] Especially preferred are compounds of the subformulas (XXV), (XXVI) and (XXVII) of the general formula (I):
[0000]
[0000] wherein
A, L 1 and p have the meanings as defined herein.
[0124] Yet in another preferred embodiment of the present invention the compounds of the present invention refer to the following subformulas
[0125] The following subformulas (IIc, IIIc, IVc and Vc) of the general formula (I) are preferred:
[0000]
[0000] wherein
A, L, R*, R# and p have the meanings as defined herein.
Q 1 , Q 2 , Q 3 represent independently of each other: —H, —CH 3 , —C 2 H 5 , —C 3 H 7 , —SO 2 —CH 3 , —SO 2 —C 2 H 5 , —SO 2 —C 3 H 7 , —COCH 3 ,
[0126] Furthermore, the following subformulas (VI, VII, VIII, IX) of the general formula (I) are preferred:
[0000]
[0000] wherein
A, L, R*, R# and p have the meanings as defined herein.
Q 1 , Q 2 , Q 3 , Q 4 , Q 5 , Q 6 , Q 7 , Q 8 , Q 9 represent independently of each other: —H, —CH 3 , —C 2 H 5 , —C 3 H 7 , —SO 2 —CH 3 , —SO 2 —C 2 H 5 , —SO 2 —C 3 H 7 , —COCH 3 ,
[0127] All embodiments of this invention comprise the enantiomers, stereoisomeric forms, mixtures of enantiomers, anomers, deoxy-forms, diastereomers, mixtures of diastereomers, prodrugs, tautomers, hydrates, solvates and racemates of the above mentioned compounds and pharmaceutically acceptable salts thereof.
[0128] The expression prodrug is defined as a pharmacological substance, a drug, which is administered in an inactive or significantly less active form. Once administered, the prodrug is metabolized in the body in vivo into the active compound.
[0129] The expression tautomer is defined as an organic compound that is interconvertible by a chemical reaction called tautomerization. Tautomerization can be catalyzed preferably by bases or acids or other suitable compounds.
[0130] The extraction and isolation of carbohydrate antigens from a pathogen may be accomplished by a variety of means (MICROBIOLOGICAL REVIEWS, Vo. 42, Nr. 1, 84-113, 1978; JOURNAL OF IMMUNOLOGICAL METHODS Vo. 44, Nr. 3, 249-270, 1981). One common method is described as follows:
[0131] The isolation and purification usually involve alkaline extraction of cell walls or cells that first had been delipidated with organic solvents, followed by precipitation with organic solvents. Further purification is achieved with ion-exchange chromatography.
[0132] Proteolytic enzymes are used to remove remaining peptide or protein components followed by affinity chromatography as a final purification step.
[0133] The synthesis of synthetic carbohydrate antigens may be accomplished by a variety of means (Nature Reviews Drug Discovery 4, 751-763, September 2005). The automated solid-phase method is described as follows:
[0134] Automated solid-phase oligosaccharide synthesis has been developed from insights gained from oligopeptide and oligonucleotide assembly. The first building block is added to a polystyrene resin equipped with an easily cleavable linker containing a free hydroxyl group. An activating agent induces couplings involving glycosyl phosphate and glycosyl trichloroacetimidate building blocks. Unlike oligonucleotide and peptide couplings, glycosidic bond formation occurs mostly at low temperatures and requires a reaction chamber that can be cooled. Excess building blocks (that is, a 5-10-fold molar excess, sometimes applied twice) are added to the chamber for each coupling.
[0135] Washing and filtration remove any side products or remaining reagents before selective removal of a temporary protective group readies the next hydroxyl group for subsequent coupling. Coupling efficiencies can be assessed by spectrometric read-out after protecting-group removal when temporary protecting groups that absorb ultraviolet radiation, such as 9-fluorenylmethyloxycarbonyl (Fmoc), are used. Originally, this coupling-deprotection cycle was automated using a converted peptide synthesizer.
[0136] After completion of the oligosaccharide sequence, the fully protected product is cleaved from solid support. After global deprotection, the oligosaccharide is purified and its structure verified. A series of increasingly complex oligosaccharides has been assembled, each within 1 day or less, using the automated oligosaccharide synthesizer. This compares favourably with the weeks to months taken using solution-phase methods.
[0137] Another aspect of the present invention comprises the synthesis of the compounds of the general formula (I)
[0000] A[L-CH—CA] p (I)
[0138] In one embodiment the synthesis of the compounds of the present invention are proceeds as follows:
[0000] L+CH→L-CH
[0000] L-CH+CA→L-CH—CA
[0000] L-CH—CA+A→A[L-CH—CA] p
[0139] Specifically, in a particular preferred embodiment of the present invention the CH moiety is reacted with a linker molecule L after being protected with appropriate protection groups (PGs). Therein, the PGs may either be the same PGs or may also be different PGs such as PG′ and PG″ depending on the hydroxyl group on the CH moiety.
[0140] In a preferred embodiment of the present invention the protections groups PG′ and PG″ are different from each. In another preferred embodiment the protection groups PG′ and PG″ are the same.
[0141] As used herein protecting groups are preferably useful for secondary alcohols. In one embodiment silyl protecting groups such as trimethylsilyl (TMS), tert-butyldiphenylsilyl (TBDPS), tert-butyldimethylsilyl (TBS or TBDMS), triisopropylsilyl (TIPS) and [2-(trimethylsilyl)ethoxy]methyl (SEM) are used. In another preferred embodiment carbon ether protection groups are used such as methyl, n-butyl, tert.-butyl, p-methoxybenzyl, methoxy-methyl, trityl, vinyl, allyl, benzyloxymethyl, acetyl, pivolyl, 2-trichlor-1-imidoacetyl, 2-trichlor-1-N-phenylimioacetyl and tetrahydropyranyl. Yet, in another preferred embodiment of the present invention at least one silyl group for PG′ and at least one carbon ether for PG″ are used in one of the molecules (XXIX), (XXX) and (XXXII). Still in another preferred embodiment of the present invention in the molecules (XXIX), (XXX) and (XXXII) two different carbon ether protection groups are used for the protection groups PG′ and PG″, preferably at least one benzyl for PG″ and at least one allyl group for PG′, more preferably three benzyl groups for PG″ in each 3, 4 and 5 four position in molecules (XXIX), (XXX) and (XXXII) and one allyl group for PG′ in 2 position in molecules (XXIX) and (XXX).
[0142] Therefore, in a particular preferred embodiment a reaction sequence is conducted as follows:
[0000]
[0000] wherein L, PG′ and PG″ are as defined herein.
[0143] Subsequently in this embodiment the L-CH molecule (XXX) is converted in at least one reaction step, preferably in two reaction steps to intermediate L-CH—CA with a suitable precursor (XXXI) for the molecule CA:
[0000]
[0000] wherein A, L, PG′, PG″, R* and R# are as defined herein.
[0144] In the next reaction sequence of this particular embodiment intermediate (XXXII) is then deprotected from the protection groups PG″ to intermediate (XXXIII) and reacted with any suitable antigen A to yield the compound (X) as one representative of the inventive compounds of the general formula (I):
[0000]
[0000] wherein A, L, PG″, R* and R# are as defined herein.
[0145] In the synthesis of the compounds of the general formula (I) A[L-CH—CA] p , and in particular as shown above in the synthesis of compounds of the general formula (X) it is preferred that the linker molecule L is introduced via a precursor which originates from diol (glycol) compound. Preferred are asymmetric precursor molecules for the linker L which have on the one side a nucleophilic group such as a halide or an activated hydroxy group and on the other side a functional group which can be converted into an amino group such as an azide, a protected amino group or nitrile. In a more preferred embodiment of the present invention the precursor molecules for the linker L have on the one side an activated alcohol functional group with a leaving group such as tosylate, triflat, or mesylate, and on the other side preferably a protected amino group or an azide. In a particularly preferred embodiment of the present invention the precursor molecule for the linker L has the general formula (XXXV)
[0000]
[0000] which can be generally synthesized from diol (glycol) compounds of the general formula (XXXVI) HO-L-OH (XXXVI).
[0146] Also, preferred are linker being a linear or branched carbon chain with 2 to 30 carbon atoms and 0 to 6 hetero atoms selected from the group of —O—, —S— and —N(R N )— and/or with one or more aromatic and/or carbocyclic and/or heterocyclic ring systems, wherein the linker is bond through a carbon atom to an oxygen atom of the carbonhydrate moiety (CH), preferably to the oxygen atom at the C6 carbon atom of the carbonhydrate moiety, and is directly or indirectly bond through a carbon atom to the antigen. This carbon chain is preferably bond through a methylen group of the carbon chain to the oxygen and preferably the C6-oxygen of the carbonhydrate moiety. Moreover this carbon chain is preferably bond through a methylen group or a carbonyl group of the carbon chain to a heteroatom and preferably a nitrogen atom of the antigen (A) and more preferably to a nitrogen atom of an amino group of the antigen. As used herein “directly bond” means that the carbon chain is attached to a functional group of the antigen, preferably an amino group of the antigen while the term “indirectly bond” refers to an attachment of the carbon chain to a spacer attached to the antigen so that the carbon chain is attached to the spacer which is connected to the antigen. Thus, such a spacer is interposed between the linker or respectively carbon chain and the antigen and can for example arise from the cleavage of an anhydride or a succinimide. Preferably the carbon chain has 2 to 25, more preferably 2 to 20, still more preferably 2 to 15 or 2 to 12 carbon atoms. It is also preferred that the carbon chain has up to 4 oxygen atoms and more preferably 1, 2 or 3 oxygen atoms and/or up to 4 sulfur atoms, preferably 1 or 2 sulfur atoms. Furthermore one or two substituted or unsubstituted phenylen rings can be present within the carbon chain.
[0147] In all described embodiments above a residue —R N represents —H, —CH 3 , —C 2 H 5 , —C 3 H 7 , —C 4 H 9 , —C 5 H 11 , —C 6 H 13 , —C 7 H 15 , —C 8 H 17 , —OH, —OCH 3 , —OC 2 H 5 , —OC 3 H 7 , —O-cyclo-C 3 H 5 , —OCH(CH 3 ) 2 , —OC(CH 3 ) 3 , —OC 4 H 9 , —OPh, —OCH 2 -Ph, —OCPh 3 , —CH 2 —OCH 3 , —C 2 H 4 —OCH 3 , —C 3 H 6 —OCH 3 , —CH 2 —OC 2 H 5 , —C 2 H 4 —OC 2 H 5 , —C 3 H 6 —OC 2 H 5 , —CH 2 —OC 3 H 7 , —C 2 H 4 —OC 3 H 7 , —C 3 H 6 —OC 3 H 7 , —CH 2 —O-cyclo-C 3 H 5 , —C 2 H 4 —O-cyclo-C 3 H 5 , —C 3 H 6 —O-cyclo-C 3 H 5 , —CH 2 —OCH(CH 3 ) 2 , —C 2 H 4 —OCH(CH 3 ) 2 , —C 3 H 6 —OCH(CH 3 ) 2 , —CH 2 —OC(CH 3 ) 3 , —C 2 H 4 —OC(CH 3 ) 3 , —C 3 H 6 —OC(CH 3 ) 3 , —CH 2 —OC 4 H 9 , —C 2 H 4 —OC 4 H 9 , —C 3 H 6 —OC 4 H 9 , —CH 2 —OPh, —C 2 H 4 —OPh, —C 3 H 6 —OPh, —CH 2 —OCH 2 -Ph, —C 2 H 4 —OCH 2 -Ph, —C 3 H 6 —OCH 2 -Ph, —NO 2 , —F, —CI, —Br, —COCH 3 , —COC 2 H 5 , —COC 3 H 7 , —CO-cyclo-C 3 H 5 , —COCH(CH 3 ) 2 , —COC(CH 3 ) 3 , —COOH, —COOCH 3 , —COOC 2 H 5 , —COOC 3 H 7 , —COO-cyclo-C 3 H 5 , —COOCH(CH 3 ) 2 , —COOC(CH 3 ) 3 , —OOC—CH 3 , —OOC—C 2 H 5 , —OOC—C 3 H 7 , —OOC-cyclo-C 3 H 5 , —OOC—CH(CH 3 ) 2 , —OOC—C(CH 3 ) 3 , —CONH 2 , —CONHCH 3 , —CONHC 2 H 5 , —CONHC 3 H 7 , —CONH-cyclo-C 3 H 5 , —CONH[CH(CH 3 ) 2 ], —CONH[C(CH 3 ) 3 ], —CON(CH 3 ) 2 , —CON(C 2 H 5 ) 2 , —CON(C 3 H 7 ) 2 , —CON(cyclo-C 3 H 5 ) 2 , —CON[CH(CH 3 ) 2 ] 2 , —CON[C(CH 3 ) 3 ] 2 .
[0148] In another embodiment of the present invention the order of connecting the respective moieties of the compounds of the present invention may be varied.
[0149] In another particular embodiment of the present invention first the moieties CH and CA are connected via suitable chemical reaction or reactions to yield intermediate CH—CA, and subsequently a linker molecule L is added to yield intermediate L-CH—CA which is then further reacted to furnish the compounds of the present invention of the general formula (I).
[0150] In another embodiment of the present invention antigen A is modified with linker molecule L to yield intermediate [L-] q A. Intermediate [L-] q A can then further be reacted with intermediate CA-CH yielding the compounds of the present invention of the general formula (I).
[0000] L+A→[L-] q A
[0000] CH+CA→CH—CA
[0000] [L-] q A+CH—CA→A[L-CH—CA] p
[0151] All reaction approaches may be modified to use or yield the respective preferred compounds of the subformulas (II) to (XXVII).
[0152] In that, according to the reaction sequence
[0000] L+CH→L-CH
[0000] L-CH+CA→L-CH—CA
[0000] L-CH—CA+A→A[L-CH—CA] p
[0153] CH moieties with different connectivity as exemplified in subformulas (II) to (V) may be used. Similarly, CH moieties being monosaccarides, disaccarides or trisaccarides as exemplified in subformulas (VI) to (XIII), also with respect to stereochemical aspects as exemplified in subformulas (XIV) to (XVII) are suitable for the above reaction sequence. Further, the synthetic approach is also suitable to be applied to specific ceramid moieties as exemplified in subformulas (XVIII) to (XXIV), which also holds true for specific linker molecules as exemplified for the subsformulas (XXV) and (XXVII).
[0154] Therefore, the reaction sequence
[0000] L+CH→L-CH
[0000] L-CH+CA→L-CH—CA
[0000] L-CH—CA+A→A[L-CH—CA] p
[0000] is suitable also for the synthesis of intermediates (II) to (XXVII) by choosing the respective moieties L, CH, and CA.
[0155] In a further preferred embodiment of the present invention the carbohydrate moiety and the ceramide are first joined together prior to introduction of the linker molecule. Therefore, a reaction sequent could also be as follows:
[0000] CH+CA→CH—CA
[0000] CH—CA+L→L-CH—CA
[0000] L-CH—CA+A→A[L-CH—CA] p
[0156] The present invention also comprises pharmaceutically acceptable salts of the compounds according to the general formula (I), all stereoisomeric forms of the compounds according to the general formula (I) as well as solvates, especially hydrates or prodrugs thereof.
[0157] In case, the inventive compounds bear basic and/or acidic substituents, they may form salts with organic or inorganic acids or bases. Examples of suitable acids for such acid addition salt formation are hydrochloric acid, hydrobromic acid, sulfuric acid, phosphoric acid, acetic acid, citric acid, oxalic acid, malonic acid, salicylic acid, p-aminosalicylic acid, malic acid, fumaric acid, succinic acid, ascorbic acid, maleic acid, sulfonic acid, phosphonic acid, perchloric acid, nitric acid, formic acid, propionic acid, gluconic acid, lactic acid, tartaric acid, hydroxymaleic acid, pyruvic acid, phenylacetic acid, benzoic acid, p-aminobenzoic acid, p-hydroxybenzoic acid, methanesulfonic acid, ethanesulfonic acid, nitrous acid, hydroxyethanesulfonic acid, ethylenesulfonic acid, p-toluenesulfonic acid, naphthylsulfonic acid, sulfanilic acid, camphorsulfonic acid, china acid, mandelic acid, o-methylmandelic acid, hydrogen-benzenesulfonic acid, picric acid, adipic acid, d-o-tolyltartaric acid, tartronic acid, (o, m, p)-toluic acid, naphthylamine sulfonic acid, and other mineral or carboxylic acids well known to those skilled in the art. The salts are prepared by contacting the free base form with a sufficient amount of the desired acid to produce a salt in the conventional manner.
[0158] Examples for suitable inorganic or organic bases are, for example, NaOH, KOH, NH 4 OH, tetraalkylammonium hydroxide, lysine or arginine and the like. Salts may be prepared in a conventional manner using methods well known in the art, for example by treatment of a solution of the compound of the general formula (I) with a solution of an acid, selected out of the group mentioned above.
[0159] Some of the compounds of the present invention may be crystallised or recrystallised from solvents such as aqueous and organic solvents. In such cases solvates may be formed. This invention includes within its scope stoichiometric solvates including hydrates as well as compounds containing variable amounts of water that may be produced by processes such as lyophilisation.
[0160] Certain compounds of the general formula (I) may exist in the form of optical isomers if substituents with at least one asymmetric center are present, e.g. diastereoisomers and mixtures of isomers in all ratios, e.g. racemic mixtures. The invention includes all such forms, in particular the pure isomeric forms. The different isomeric forms may be separated or resolved one from the other by conventional methods, or any given isomer may be obtained by conventional synthetic methods or by stereospecific or asymmetric syntheses. Where a compound according to the general formula (I) contains an alkene moiety, the alkene can be presented as a cis or trans isomer or a mixture thereof. When an isomeric form of a compound of the invention is provided substantially free of other isomers, it will preferably contain less than 5% w/w, more preferably less than 2% w/w and especially less than 1% w/w of the other isomers.
[0161] Another aspect of the present invention relates to the use of the inventive carbohydrate-glycolipid conjugate derivatives as drugs, i.e. as pharmaceutically active agents applicable in medicine.
[0162] Surprisingly it was found that the novel carbohydrate-glycolipid conjugates of the present invention are also suitable to raise an immune response in an animal and are suitable for vaccination against infectious diseases which are caused by pathogens selected from the group of bacteria, viruses, sporozoa, parasites or fungi. Moreover if the saccharide antigen is specific to cancer cells, the novel carbohydrate-glycolipid conjugates are suitable for the treatment and prophylaxis of cancers.
[0163] Both isolated and synthetic carbohydrate antigens are suitable for the formation of the described conjugate. Moreover it was found, that the treatment of an animal with the novel carbohydrate-glycolipid conjugates of the current invention lead to the formation of immunoglobuline IgG-isotypes, which prove the development of memory B-cells in the living organism. The presence of memory B-cells demonstrates immunological memory. Thus it has been shown, that the carbohydrate-glycolipid conjugates of the current invention are capable to induce a long term protection in an animal against a pathogen. The described vaccination is moreover independent on further adjuvants, does not need any protein-carrier and refrigeration of the vaccine.
[0164] Therefore, compounds according to the general formula (I-XXVII) are suitable for the use as a pharmaceutically active agent applicable in medicine, especially for use in vaccination against infectious diseases.
[0165] The infectious diseases for which vaccines can be provided by the compounds according to the present invention are selected from the group of bacterial, sporozoal, parasitic, fungal or viral infectious diseases. The bacterial infectious disease for which vaccines can be provided by the compounds according to the invention is caused by a pathogen selected from the group comprising:
[0000] Allochromatium vinosum, Acinetobacter baumanii, Bacillus anthracis, Campylobacter jejuni, Clostridium spp., Citrobacter spp., Escherichia coli, Enterobacter spp., Enterococcus faecalis., Enterococcus faecium, Francisella tularensis, Haemophilus influenzae, Helicobacter pylori, Klebsiella spp., Listeria monocytogenes, Moraxella catharralis, Mycobacterium tuberculosis, Neisseria meningitidis, Neisseria gonorrhoeae, Proteus mirabilis, Proteus vulgaris, Pseudomonas aeruginosa, Salmonella spp., Serratia spp., Shigella spp., Stenotrophomonas maltophilia, Staphyloccocus aureus, Staphyloccocus epidermidis, Streptococcus pneunmoniae, Streptococcus pyogenes, Streptococcus agalactiae, Yersina pestis , und Yersina enterocolitica.
[0166] The parasitic infectious disease for which vaccines can be provided by the compounds according to the invention is caused by a pathogen selected from the group comprising:
[0000]
Babesia, Balantidium, Besnoitia, Blastocystis, Coccidia, Cryptosporidium, Cytauxzoon, Cyclospora, Dientamoeba, Eimeria, Entamoeba, Enterocytozoon, Enzephalitozoon, Eperythrozoon, Giardia, Hammondia, Isospora, Leishmania, Microsporidia, Naegleria, Plasmodium, Plasmodium falciparum, Plasmodium vivax, Plasmodium ovale, Plasmodium malariae, Plasmodium knowlesi, Pneumocystis, Schistosoma, Sarcocystis, Theileria, Trichinella, Toxoplasma, Trichomonas, Trypanosoma, Unicaria, Cestoda, Dipylidium, Dranunculus, Echinococcus, Fasciola, Fasciolopsis, Taenia, Ancylostoma, Ascaris, Brugia, Enterobius, Loa loa, Mansonella, Necator, Oncocerca, Strongyloides, Strongylus, Toxocara, Toxascaris, Trichuris oder Wucheria.
[0167] The fungal infectious disease for which vaccines can be provided by the compounds according to the invention is caused by a pathogen selected from the group comprising:
[0000] Trichophyton mentagrophytes, Trichophyton rubrum, Trichophyton interdigitale, T. schönleinii, T. verrucosum, T. violaceum, T. tonsurans, Trichophyton spp., M. canis, Candida albicans, C. guillermondii, C. krusei, C. parapsilosis, C. tropicalis, C. glabrata, Candida spp., Microsporum spp., Microsporum canis, Microsporum audonii, Microsporum gypseum, M. ferrugineum, Trichosporum beigelii, Trichosporum inkiin, Aspergillus niger, Alternaria, Acremonium, Fusarium , or Scopulariopsis.
[0168] The viral infectious disease for which vaccines can be provided by the compounds according to the invention is caused by a pathogen selected from the group comprising:
[0000] Adenoviruses, Ebolavirus, Epstein-Barr-virus, Flavivirus, FSME-virus, Influenza virus, Hanta-virus, human immunodeficiency virus (“HIV”), herpes simplex virus (“HSV”, type 1 or 2), human herpes virus 6 (HHV-6), human Papilloma virus (“HPV”, type 16 or 18), human Cytomegalovirus (“HCMV”), human hepatitis B or C virus (“HBV”, Type B; “HCV”, type C), Lassavirus, Lyssavirus (EBL 1 or EBL 2), Marburgvirus, Norovirus, Parvovirus B19, Pestvirus, Poliovirus, Rhinovirus, Rotaviruses, SARS-assciated Coronavirus, Varicella-Zoster virus.
[0169] Among the cancers the novel carbohydrate-glycolipid conjugates are suitable for, the attention has been given to Bladder Cancer, Breast Cancer, Colon and Rectal Cancer, Endometrial Cancer, Kidney (Renal Cell) Cancer, Leukemia, Lung Cancer Melanoma, Non-Hodgkin Lymphoma, Pancreatic Cancer, Prostate Cancer, Thyroid Cancer.
[0170] Among the infectious diseases, the attention has been given to Haemophilus influenzae and Streptococcus pneunmoniae.
[0171] Therefore, another aspect of the present invention is directed to pharmaceutical compositions comprising at least one compound of the present invention as active ingredient, together with at least one pharmaceutically acceptable carrier, excipient and/or diluents. The pharmaceutical compositions of the present invention can be prepared in a conventional solid or liquid carrier or diluent at suitable dosage level in a known way. The preferred preparations are adapted for oral application. These administration forms include, for example, pills, tablets, film tablets, coated tablets, capsules, powders and deposits.
[0172] Furthermore, the present invention also includes pharmaceutical preparations for parenteral application, including dermal, intradermal, intragastral, intracutan, intravasal, intravenous, intramuscular, intraperitoneal, intranasal, intravaginal, intrabuccal, percutan, rectal, subcutaneous, sublingual, topical, or transdermal application, which preparations in addition to typical vehicles and/or diluents contain at least one compound according to the present invention and/or a pharmaceutical acceptable salt thereof as active ingredient.
[0173] The pharmaceutical compositions according to the present invention containing at least one compound according to the present invention, and/or a pharmaceutical acceptable salt thereof as active ingredient will typically be administered together with suitable carrier materials selected with respect to the intended form of administration, i.e. for oral administration in the form of tablets, capsules (either solid filled, semi-solid filled or liquid filled), powders for constitution, extrudates, deposits, gels, elixirs, dispersable granules, syrups, suspensions, and the like, and consistent with conventional pharmaceutical practices. For example, for oral administration in the form of tablets or capsules, the active drug component may be combined with any oral non-toxic pharmaceutically acceptable carrier, preferably with an inert carrier like lactose, starch, sucrose, cellulose, magnesium stearate, dicalcium phosphate, calcium sulfate, talc, mannitol, ethyl alcohol (liquid filled capsules) and the like. Moreover, suitable binders, lubricants, disintegrating agents and coloring agents may also be incorporated into the tablet or capsule. Powders and tablets may contain about 5 to about 95 weight % of the benzothiophene-1,1-dioxide derived compound and/or the respective pharmaceutically active salt as active ingredient.
[0174] Suitable binders include starch, gelatin, natural carbohydrates, corn sweeteners, natural and synthetic gums such as acacia, sodium alginate, carboxymethylcellulose, polyethylene glycol and waxes. Among suitable lubricants there may be mentioned boric acid, sodium benzoate, sodium acetate, sodium chloride, and the like. Suitable disintegrants include starch, methylcellulose, guar gum, and the like. Sweetening and flavoring agents as well as preservatives may also be included, where appropriate. The disintegrants, diluents, lubricants, binders etc. are discussed in more detail below.
[0175] Moreover, the pharmaceutical compositions of the present invention may be formulated in sustained release form to provide the rate controlled release of any one or more of the components or active ingredients to optimise the therapeutic effect(s), e.g. antihistaminic activity and the like. Suitable dosage forms for sustained release include tablets having layers of varying disintegration rates or controlled release polymeric matrices impregnated with the active components and shaped in tablet form or capsules containing such impregnated or encapsulated porous polymeric matrices.
[0176] Liquid form preparations include solutions, suspensions, and emulsions. As an example, there may be mentioned water or water/propylene glycol solutions for parenteral injections or addition of sweeteners and opacifiers for oral solutions, suspensions, and emulsions. Liquid form preparations may also include solutions for intranasal administration. Aerosol preparations suitable for inhalation may include solutions and solids in powder form, which may be present in combination with a pharmaceutically acceptable carrier such as an inert, compressed gas, e.g. nitrogen. For preparing suppositories, a low melting fat or wax, such as a mixture of fatty acid glycerides like cocoa butter is melted first, and the active ingredient is then dispersed homogeneously therein e.g. by stirring. The molten, homogeneous mixture is then poured into conveniently sized moulds, allowed to cool, and thereby solidified.
[0177] Also included are solid form preparations which are intended to be converted, shortly before use, to liquid form preparations for either oral or parenteral administration. Such liquid forms include solutions, suspensions, and emulsions.
[0178] The compounds according to the present invention may also be delivered transdermally. The transdermal compositions may have the form of a cream, a lotion, an aerosol and/or an emulsion and may be included in a transdermal patch of the matrix or reservoir type as is known in the art for this purpose.
[0179] The term capsule as recited herein refers to a specific container or enclosure made e.g. of methyl cellulose, polyvinyl alcohols, or denatured gelatins or starch for holding or containing compositions comprising the active ingredient(s). Capsules with hard shells are typically made of blended of relatively high gel strength gelatins from bones or pork skin. The capsule itself may contain small amounts of dyes, opaquing agents, plasticisers and/or preservatives. Under tablet a compressed or moulded solid dosage form is understood which comprises the active ingredients with suitable diluents. The tablet may be prepared by compression of mixtures or granulations obtained by wet granulation, dry granulation, or by compaction well known to a person of ordinary skill in the art.
[0180] Oral gels refer to the active ingredients dispersed or solubilised in a hydrophilic semi-solid matrix. Powders for constitution refers to powder blends containing the active ingredients and suitable diluents which can be suspended e.g. in water or in juice.
[0181] Suitable diluents are substances that usually make up the major portion of the composition or dosage form. Suitable diluents include carbohydrates such as lactose, sucrose, mannitol, and sorbitol, starches derived from wheat, corn rice, and potato, and celluloses such as microcrystalline cellulose. The amount of diluent in the composition can range from about 5 to about 95% by weight of the total composition, preferably from about 25 to about 75 weight %, and more preferably from about 30 to about 60 weight %.
[0182] The term disintegrants refers to materials added to the composition to support break apart (disintegrate) and release the pharmaceutically active ingredients of a medicament. Suitable disintegrants include starches, “cold water soluble” modified starches such as sodium carboxymethyl starch, natural and synthetic gums such as locust bean, karaya, guar, tragacanth and agar, cellulose derivatives such as methylcellulose and sodium carboxymethylcellulose, microcrystalline celluloses, and cross-linked microcrystalline celluloses such as sodium croscaramellose, alginates such as alginic acid and sodium alginate, clays such as bentonites, and effervescent mixtures. The amount of disintegrant in the composition may range from about 2 to about 20 weight % of the composition, more preferably from about 5 to about 10 weight %.
[0183] Binders are substances which bind or “glue” together powder particles and make them cohesive by forming granules, thus serving as the “adhesive” in the formulation. Binders add cohesive strength already available in the diluent or bulking agent. Suitable binders include carbohydrates such as sucrose, starches derived from wheat corn rice and potato, natural gums such as acacia, gelatin and tragacanth, derivatives of seaweed such as alginic acid, sodium alginate and ammonium calcium alginate, cellulose materials such as methylcellulose, sodium carboxymethylcellulose and hydroxypropylmethylcellulose, polyvinylpyrrolidone, and inorganic compounds such as magnesium aluminum silicate. The amount of binder in the composition may range from about 2 to about 20 weight % of the composition, preferably from about 3 to about 10 weight %, and more preferably from about 3 to about 6 weight %.
[0184] Lubricants refer to a class of substances which are added to the dosage form to enable the tablet granules etc. after being compressed to release from the mould or die by reducing friction or wear. Suitable lubricants include metallic stearates such as magnesium stearate, calcium stearate, or potassium stearate, stearic acid, high melting point waxes, and other water soluble lubricants such as sodium chloride, sodium benzoate, sodium acetate, sodium oleate, polyethylene glycols and D,L-leucine. Lubricants are usually added at the very last step before compression, since they must be present at the surface of the granules. The amount of lubricant in the composition may range from about 0.2 to about 5 weight % of the composition, preferably from about 0.5 to about 2 weight %, and more preferably from about 0.3 to about 1.5 weight % of the composition.
[0185] Glidents are materials that prevent caking of the components of the pharmaceutical composition and improve the flow characteristics of granulate so that flow is smooth and uniform. Suitable glidents include silicon dioxide and talc. The amount of glident in the composition may range from about 0.1 to about 5 weight % of the final composition, preferably from about 0.5 to about 2 weight %.
[0186] Coloring agents are excipients that provide coloration to the composition or the dosage form. Such excipients can include food grade dyes adsorbed onto a suitable adsorbent such as clay or aluminum oxide. The amount of the coloring agent may vary from about 0.1 to about 5 weight % of the composition, preferably from about 0.1 to about 1 weight %.
[0187] Said pharmaceutical compositions may further comprise at least one active carbohydrate-glycolipid conjugate of the general formula (I).
[0188] The pharmaceutical compositions may further comprise at least one further active agent. It is preferred if this active agent is selected from the group consisting of anti-depressant and other psychotropic drugs. It is further preferred if the anti-depressant is selected from amitriptyline, amioxide clomipramine, doxepine, duloxetine, imipramine trimipramine, mirtazapine, reboxetine, citaloprame, fluoxetine, moclobemide and sertraline.
[0189] A further embodiment of the invention comprises the average ratio of the carbohydrate antigen A to the glycolipid (L-CH—CA) which may vary between 1:4 and 1:100 (n/n).
[0190] Another embodiment of the invention comprises the compounds of the invention, according to the general formula (I) which may be used for the preparation of a vaccine formulation for the use in vaccination of an animal. The mentioned vaccine formulation may comprise one or more of the compounds of the present invention or a mixture of different compounds of the invention and preferably of the general formula (I), wherein the mixture of different compounds of the general formula (I) preferably comprises a mixture of different serotypes of the used carbohydrate antigen A, and/or the mixture of different compounds of the general formula (I) may comprise a mixture of different carbohydrate antigens A, which are used in different compounds of the general formula (I). The mentioned mixture of different compounds of the general formula (I) within the vaccine formulation can therefore constitute a combinantion of vaccines which can be used for a combinated vaccination against more than at least one pathogen.
[0191] In a further embodiment of the invention, the vaccine formulation may comprise a mixture of different compounds of the general formula (I).
[0192] The mentioned vaccine formulations may further comprise a combination with at least one pharmaceutically acceptable carrier, excipient and/or diluents.
[0193] The compounds of the invention of the general formula (I) are present in said vaccine formulation in the range of 10 to 1000 μg/g.
[0194] In a preferred embodiment of the invention the compounds of the general formula (I) are present in said vaccine formulation in the range of 10 to 1000 ng/g.
[0195] In a more preferred embodiment of the invention the compounds of the general formula (I) are present in said vaccine formulation in the range of 100 to 1000 pg/g.
[0196] The mentioned vaccine formulation displays an extraordinary stability at room temperature due to the modulary constitution of the compounds of the present invention, wherein said vaccine formulation may be maintained at a temperature of at least 25° C. for a period of at least 3 months prior to reconstitution.
[0197] In a preferred embodiment of the invention the said period is comprises 6 months or at least 12 months.
[0198] The surprising advantages of the conjugates of the present invention were found by in vitro and in vivo application.
[0199] Specifically, when applied in an in vitro the glycoconjugate vaccine according to the present invention retains the capacity to stimulate iNKT cells when presented by CD1d-positive antigen-presenting cells (APC). Additionally it was found that the compounds of the present invention fail to stimulate the same iNKT cells when loaded onto plate-bound recombinant CD1d. Without being bound to theory it appears that the saccharidic moiety is properly coupled and hinders T cell recognition.
[0200] Further, when applied in vivo the conjugates of the present invention were found of being capable of effectively and continuously immunizing against a pathogen. This is rather advantageous since thereby the conjugates of the present invention cannot only stimulate the generation of antibodies of high titers and long lasting resistance in in vivo conditions, moreover the compounds of the present invention themselves exhibit a long-term stability at room temperature. Therefore, the conjugates of the present invention are particular heat stable and thus no refrigeration is required.
EXAMPLES
General Methods
Cells.
[0201] The APC lines MOLT-4 (ATCC CRL 1582), which expresses only negligible CD1d, and human CD1d-transfected C1R and HeLa cells (C1R-hCD1d and HeLa-hCD1d, respectively) [6] were maintained in RPMI-1640 medium containing 10% FCS, 2 mM L-glutamine, 1 mM sodium pyruvate, 100 μM non-essential aminoacids, and 100 μg/ml kanamycin. The same maintenance conditions were used for RAW (mouse leukemic monocyte macrophage cell line), J774A.1 (mouse, BALB/c, monocyte-macrophage, not defined tumor), HL60 and NB4 (both human promyelocytic leukemia) cells. Isolation of iNKT cell clones from PBMC of healthy donors has been described before [7]. iNKT cells were maintained in RPMI-1640 medium containing 5% HS, 2 mM L-glutamine, 1 mM sodium pyruvate, 100 μM non-essential aminoacids, 100 μg/ml kanamycin, and 100 U/ml recombinant IL-2.
Mice.
[0202] C57BL/6, BALB/c and B6; 129-CD1<tmlGru> (CD1KO) [8] mice were bred at our institute (Versuchsstation Departement Biomedizin, Basel, Switzerland) or C57BL/6 were also bought from Charles River Laboratories (Sulzfeld, Germany). This study was reviewed and approved by the “Kantonales Veterinäramt Basel-Stadt” 20 in Basel, Switzerland.
Bacteria.
[0203] Streptococcus pneumoniae serotype 4 reference strain (Statens Serum Institute, Denmark) was grown in Todd-Hewitt broth supplemented with 0.5% yeast extract at 37° C.
Infections.
[0204] Non-/ and vaccinated mice were challenged with S. pneumoniae serotype 4 and mortality, weight loss and clinical score were recorded over time.
Opsonizations.
[0205] 5 mM 5-chloromethylfluorescein diacetate (CMFDA, Invitrogen, Switzerland) labeled and non-fixed or fixed bacteria were coated with 10% rabbit complement (HD supplies, UK) and/or purified CPS-specific mAbs for up to 1 h. Mixed bacteria with dimethylformamide-(Sigma-Aldrich, Switzerland) or non-induced cells at a ratio of 10-100:1 for up to 2 h at 37° C. Samples were acquired on a CyAn ADP flow cytometer (Beckman Coulter, Switzerland). Data were gated to exclude non-viable cells on the basis of light scatter, pulse width, and incorporation of propidium iodide and further analyzed using Summit software (Beckman Coulter).
Activation Assays.
[0206] In vitro antigen presentation assays by living APC or plate-bound antigen-presenting molecules were performed as previously described [9]. Briefly, living APC were plated at 2.5×10 4 /well in 96-well plates and incubated during the whole assay at 37° C. with vehicle or titrating doses of αGalCer or conjugate vaccine. After 1 h human iNKT cells (0.5-1×10 5 /well) were added. Cell culture supernatants were harvested after 24-48 h and release of cytokines was measured by ELISA. For plate-bound activation, purified recombinant soluble human CD1d (rshCD1d) was obtained by IEF and added to Bir1.4 mAb-coated (10 μg/ml, specific for the BirA tag of rshCD1d) MaxiSorp Plates (Nunc) overnight. Bound rshCD1d was pulsed with 2 μg/ml αGalCer or different doses of conjugate vaccine. Human iNKT cell clones (1.5×10 5 /well) were added to the plate and after 24-48 h released cytokines were measured by ELISA.
ELISA.
[0207] For detection of human cytokines, the following purified capture and biotinylated detection monoclonal antibody (mAb) pairs (all BioLegend, San Diego, USA) were used: hTNFα (MAb1 1 μg/ml and MAb11 0.5 μg/ml), hIFNγ (MD-1 2 μg/ml and 4S.B3 0.5 μg/ml), hIL-4 (8D4-8 1 μg/ml and MP4-25D2 0.5 μg/ml), hGM-CSF (BVD2-23B6 3.33 μg/ml and BVD2-21C11 0.5 μg/ml), hIL-8 (JK8-1 1.25 μg/ml and JK8-2 1 μg/ml). For detection of mouse cytokines, the following mAb pairs (all Becton Dickinson (BD), Allschwil, Switzerland) were used: mIL-2 (JES6-1A12 2 μg/ml and JES6-5H4 1 μg/ml), mIL-4 (11B11 1 μg/ml and BVD6-24G2 1 μg/ml), mIFNγ (R4-6A2 2 μg/ml and XMG1.2 1 μg/ml). For detection of Abs, plates were coated with 1 μg/ml biotin goat anti-mouse (GAM) Ig (BD, 553999) and revealed with 1:10′000 HRP-labeled GAM-IgG (Sigma-Aldrich, Buchs, Switzerland, A0168) or with 1:1′000 (all SouthernBiotech, Birmingham, USA) HRP-labeled GAM-IgM (1020-05), GAM-IgG1 (1070-05), GAM-IgG2a (1080-05), GAM-IgG2b (1090-05), GAM-IgG3 (1100-05) or coated with 2.5 μg/ml CPS and revealed with (all Biolegend) biotinylated rat anti-mouse (RAM)-IgG1 (clone RMG1-1, 1 μg/ml), -IgG2a (clone RMG2α-62, 1 μg/ml), -IgG2b (clone RMG2b-1, 0.5 μg/ml), -IgG3 (clone RMG3-1, 0.5 μg/ml) or donkey anti-mouse IgM (Jackson ImmunoResearch, Suffolk, UK, 0.95 μg/ml) or GAM F(ab′)2 IgG (abcam, 0.1 μg/ml) GAM Ig (BD, 2 μg/ml).
Statistical Analysis.
[0208] Survival data were compared with the Mantel-Cox and Gehan-Breslow-Wilcoxon test. All analyses were performed using GraphPad Prism software (version 5.03). Differences were considered significant at P<0.05.
Chemicals and Structure Analysis.
[0209] All chemicals used were reagent grade and used as supplied except where noted. Dimethylformamide (DMF), tetrahydrofuran (THF), toluene, dichloromethane (CH 2 Cl 2 ) and diethyl ether (Et 2 O) were purchased from JT Baker or VWR International and purified by a Cycle-Tainer Solvent Delivery System. Pyridine, triethylamine (NEt 3 ) and acetonitrile (MeCN) were refluxed over calcium hydride and distilled. Solvents for chromatography and workup procedures were distilled. Reactions were performed under an argon or nitrogen atmosphere except where noted. Analytical thin-layer chromatography was performed on E. Merck silica gel 60 F 254 plates (0.25 mm). Compounds were visualized by UV-light at 254 nm and by dipping the plates in a cerium sulfate ammonium molybdate (CAM) solution or a sulfuric acid/methanol solution followed by heating. Liquid chromatography was performed using forced flow of the indicated solvent on Fluka silica gel 60 (230-400 mesh). 1 H NMR spectra were obtained on a Varian VXR-300 (300 MHz), Varian VXR-400 (400 MHz), Bruker DRX500 (500 MHz), and Bruker AV600 (600 MHz) and are reported in parts per million (6) relative to the resonance of the solvent or to TMS (0.00 ppm). Coupling constants (J) are reported in Hertz (Hz). 13 C NMR spectra were obtained on a Varian VXR-300 (75 MHz), Varian VXR-400 (101 MHz), Bruker DRX500 (125 MHz), and Bruker AV600 (150 MHz) and are reported in δ relative to the resonance of the solvent or to TMS (0.00 ppm). IR Spectra: Measured as 1-2% CHCl 3 solution on a Perkin-Elmer-782 spectrophotometer or neat on a Perkin-Elmer-100 FT-IR spectrometer. Recycling preparative size exclusion HPLC (LC-9101, Japan Analytical Industry Co.); flow rate: 3.5 mL/min; solvent: CHCl 3 . Optical rotations [α] rt D were measured on a Jasco DIP-370 polarimeter (10 cm, 1 mL cell); the solvents and concentrations (in g/100 mL) are indicated. High-resolution mass spectra were performed by the MS service FU Berlin and are given in m/z.
Example 1
In Vitro Activity of the Conjugate Vaccine
[0210] The glycoconjugate vaccine ( S. pneumoniae serotype 4 CPS coupled to αGalCer) retains the capacity to stimulate iNKT cells when presented by CD1d-positive antigen-presenting cells (APC) but fails to stimulate the same iNKT cells when loaded onto plate-bound recombinant CD1d ( FIGS. 3A and 3B , respectively). These findings indicate that the saccharidic moiety is properly coupled and hinders T cell recognition but can be cleaved off from the stimulatory αGalCer glycolipid by living APC.
Example 2
In Vivo Activity of the Conjugate Vaccine
[0211] The glyconjugate consisting of CPS type 4 coupled to αGalCer was used to immunize wild-type (WT) C57BL/6 mice. Three immunizations were performed with intervals of 14 days. These mice showed high titers of anti-polysaccharide Abs compared to naïve or CPS only immunized mice ( FIG. 4A ) up to 3 months after the last immunization. This argues in favor of a long-lasting Abs response by B cells only when helped by αGalCer-responsive iNKT cells.
[0212] The glyconjugate vaccine was used to immunize WT C57BL/6 and CD1d-deficient (CD1d−/−, CD1KO) mice. Two immunizations were performed with an interval of 7 days. WT mice showed high titers of anti-polysaccharide antibodies (Abs), which instead were not observed in CD1d-deficient mice ( FIG. 4B ), indicating that expression of CD1d is necessary for the adjuvant-like effect of αGalCer.
[0213] Conclusively, the glycoconjugate vaccine-induced antibody response is dependent on the presence of iNKT cells and of CD1d as CD1d KO mice fail to generate high titers of CPS-specific antibodies after immunization.
Example 3
Analysis of the In Vivo Antibody Response after Vaccination
[0214] When CPS-specific Abs were investigated by ELISA using isotype-specific secondary reagents, the presence of IgG1 CPS-specific Abs was detected only in WT mice whereas CD1KO mice were unable to induce IgG1 ( FIG. 5A ). The same finding was confirmed with other IgG subtypes. These experiments prove that immunization with CPS type 4 coupled to αGalCer glyconjugate facilitates the class switch of polysaccharide-specific antibodies to all IgG isotypes.
[0215] The generated Abs partially cross-reacted with CPS of type 2 S. pneumoniae ( FIG. 5B ). They might also recognize common epitopes on CPS of other serotypes as very high titers of total immunoglobulin were detected assessing reactivity to a CPS mix of several S. pneumoniae serotypes (data not shown).
[0216] Several hybridomas expressing CPS-specific Abs were established from mice immunized twice and sacrificed 1.5 months after the last boost. We could isolate hybridomas expressing IgM and all IgG subclasses, with the exception of IgG2b. The IgM-positive hybridomas were affinity matured ( FIG. 6 ).
[0217] These preliminary experiments demonstrate that immunization with CPS type 4 coupled to αGalCer glycoconjugate facilitates switching of polysaccharide-specific B cells to IgG isotypes and/or affinity maturation of the CPS-specific Abs.
[0218] All hybridomas derived from glycoconjugate immunized mice showed class switching and affinity maturation. Somatic mutation seems a frequent event as two of the IgG1 hybridomas used the same VDJ rearrangement. Moreover several IgM hybridomas were identical except for junctional diversity by P- and N-nucleotides.
[0219] These mAbs were assessed for their ability to fix complement and enhance opsonization by phagocytic cells. Using CMD-labelled bacteria, we found that CPS-specific Abs upregulated bacterial phagocytosis ( FIG. 7 ).
Example 4
Protection from Infection with S. pneumoniae in a Mouse Model
[0220] Immunization with the glycoconjugate vaccine protects C57BL/6 mice from infection with S. pneumoniae . αGalCer-CPS type 4 vaccinated mice show short- and long-term protection to challenge with S. pneumoniae ( FIG. 8B ). Furthermore, mice vaccinated with αGalCer-CPS type 4 suffered a less severe disease than CPS type 4 only immunized mice as shown by no weight loss upon infection ( FIG. 8A , 3 and 3 representative animals).
Example 5
Synthesis of the Carbohydrate-Glycolipid Conjugate Vaccine
[0221] Synthesis of the lipid portion of the conjugate vaccine started using Weinreb amide of N-Boc-L-serine 2 (Scheme 1) which was formed using EDCl as coupling reagent, N-methyl morpholine as base, and N,O-dimethyl hydroxylamine. Mixed N,O-acetal formation with 2,2-dimethoxypropane and catalytic amounts of BF 3 OEt 2 yielded amide 3. Reduction of the latter with lithium aluminium hydride at 0 C yielded Garner's aldehyde 4. Z-Selective Wittig olefination using pentadecyltriphenylphosphonium ylide furnished alkene 5. Removal of the acetal group on olefin 5 was followed by Sharpless' asymmetric dihydroxylation with AD-mix 1 and methylsulfonamide, furnishing N-Boc protected diol 6 in good yield and selectivity. Subsequent removal of the carbamate group furnished phytosphingosine 7. Amide bond formation was performed with hexacosanoic N-hydroxy succinimidyl ester 11 and triethylamine as base, to yield 8. Addition of TBSOTf and 2,6-lutidine yielded trisilyl ether 9. The silyl ether on the primary hydroxyl group was then selectively removed with aq. TFA to give ceramide acceptor 10. [2]
[0000]
[0000]
[0222] p-Toluensulfonic acid catalyzed Fischer glycosidation of galactose 12 with allyl alcohol yielded glycoside 13 (Scheme 2). [5] Subsequent tritylation of the primary C6 hydroxyl group yielded triol 14. Benzyl ether formation with sodium hydride and benzylbromide furnished the fully protected galactose 15. The trityl group was subsequently removed with trifluoroacetic acid and triethyl silane to free the C6 hydroxyl group for further functionalization. Williamson etherification of alcohol 16 and azide 23 using sodium hydroxide furnished galactose derivative 17. Catalytic isomerization of the anomeric allyl protecting group to the corresponding enol ether with palladium(II) chloride and subsequent hydrolysis yielded lactol 18 which was converted into glycosyl imidate 19 with cesium carbonate and N-phenyltrifluoroacetimidazoyl chloride 24.
[0223] Linker 23 was prepared starting from 1,6-hexanediol 20 which was reacted with tosyl chloride to yield a mixture of the corresponding mono- and di-tosylated product along with the starting material. After separation, the tosyl group of 21 was displaced by sodium azide to yield azide 22. Subsequent tosylation of the hydroxyl group on 22 gave the tosylate 23.
[0000]
[0224] Linker-equipped glycolipid 25 (Scheme 3) was obtained via TMSOTf-catalyzed glycosylation of galactose building block 19 and ceramide 10. The reaction proceeded in 72% yield and with complete α-selectivity. Removal of the silylether protecting groups with TBAF yielded diol 26 that was converted to 27 by hydrogenolysis with Perlman's catalyst.
[0000]
[0225] The glycolipid 36 was prepared in three steps from the known compound 33 by reacting the activated compound 34 with derivatives of compounds 10 by the above TMSOTf-catalyzed glycosylation of galactose building block. After deprotection of compound 35 the linker was introduced by condensation reaction with compound 38 in moderate yields. The linker-equipped glycolipid 27a was subsequently prepared via intermediates 25a and 26a by complete deprotection of linker-equipped compound 37.
[0226] Conjugation of the polysaccharide to the glycolipid 27 was accomplished via a covalent linkage. To this end PS4 was activated with cyanogen bromide to which 27 was added in order to give conjugate 1 (Scheme 4).
[0000]
[0227] A hydrazone linkage provides an alternative conjugation method to link the epitope moiety with the glycolipid. To this end a hydrazone linkage can be used (Scheme 5). Antigen 28 has to be modified to aromatic aldehyde 30 using NHS-ester 29 and GSL 27 will be converted to hydrazone 32 using NHS-ester 31. Coupling of aldehyde 30 and hydrazone 32 occurs at a pH of 4.7 to 7.2. The linker system is commercially available from Novabiochem (HydraLinK™).
[0000]
Experimental Procedures
(S)-3-(tert-Butoxycarbonyl)-N-methoxy-2,2,N-trimethyloxazolidine-4-carboxamide (3)
[0228] To a solution of L-Boc-serine 2 (12.33 g, 60.1 mmol) in CH 2 Cl 2 (240 mL) were added N,O-dimethylhydroxylamine hydrochloride (6.04 g, 61.9 mmol) and N-methylmorpholine (6.8 mL, 61.9 mmol) at 0° C. To this solution was added N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (11.86 g, 61.9 mmol) portionwise over a period of 20 min. and the solution was stirred for another 1 h. Then, aq. HCl solution (1.0 M, 30 mL) was added and the aqueous layer was extracted with CH 2 Cl 2 (2×100 mL). The combined organic layers were washed with sat. aq. NaHCO 3 solution (30 mL) and the aqueous layer was again extracted with CH 2 Cl 2 (100 mL). The combined organic layers were dried over MgSO 4 and the solvent was removed in vacuo to obtain the corresponding Weinreb amide (14.07 g, 94%) as white solid. R f =0.3 (EtOAc); 1 H NMR (250 MHz, CDCl 3 ) δ 5.60 (d, J=6.0 Hz, 1H), 4.77 (br s, 1H), 1.42 (s, 9H), 3.80 (d, J=3.3 Hz, 2H), 3.76 (s, 3H), 3.21 (s, 3H), 2.66 (br s, 1H). The crude product was dissolved in acetone (180 mL) to which 2,2-dimethoxypropane (57 mL) and BF 3 Et 2 O (0.5 mL) were added. The orange solution was stirred for 90 min. at r.t. and then quenched with Et 3 N (1.2 mL) and solvents removed in vacuo. The crude product was purified by flash column chromatography on silica gel (gradient EtOAc/cyclohexane=1:2→1:1) to yield isopropylidene-protected Weinreb amide 3 (15.32 g, 89% over two steps) as a white solid. The NMR spectra consist of two sets of signals due to the presence of rotamers. [α] D r.t. =−30.9 (c=1, CHCl 3 ); R f =0.45 (Hexanes/EtOAc=1:1); IR (film) ν max 2976, 2938, 1702, 1682, 1364, 1167, 1098, 998, 848, 768, 716; 1 H NMR (250 MHz, CDCl 3 ) δ 4.77 (dd, J=9.8, 2.8 Hz, 1H), 4.70 (dd, 7.5, 3.8, Hz, 1H), 4.18 (dd, J=7.5, 4.0 Hz, 1H), 4.15 (dd, J=7.8, 3.8 Hz, 1H), 3.95 (dd, J=9.3, 3.0 Hz, 1H), 3.91 (dd, J=9.0, 3.5 Hz), 3.72 (s, 3H), 3.68 (s, 3H), 3.19 (s, 6H), 1.68 (s, 3H), 1.66 (s, 3H), 1.54 (s, 3H), 1.50 (s, 3H), 1.47 (s, 9H), 1.39 (s, 9H); 13 C NMR (101 MHz, CDCl 3 ) δ 171.4, 170.7, 152.2, 151.4, 95.1, 94.5, 80.6, 80.0, 66.2, 66.0, 61.3, 61.3, 57.9, 57.8, 28.5, 28.4, 25.8, 25.5, 24.8, 24.6; HR ESI Calcd for C 13 H 24 N 2 O 5 [M+Na + ]: 311.1577. found: 311.1582.
tert-Butyl (S)-4-formyl-2,2-dimethyloxazolidine-3-carboxylate (4)
[0229] To a solution of Weinreb amide 3 (8.00 g, 27.7 mmol) in THF (100 mL) at 0° C. were added LiAlH 4 (1.0 M in THF, 13.9 mL, 13.9 mmol) dropwise and the solution was stirred for 1 h at 0° C. After 1 h, the solution was cooled to −10° C. and KHSO 4 (1M, 70 mL) was added carefully and the solution was diluted with Et 2 O (170 mL). The mixture was allowed to warm to r.t. and stirred for 30 min. The organic layer was separated, dried over MgSO 4 , filtered and the solvent was removed in vacuo to yield Garner's aldehyde 4 as a pale yellow oil (6.24 g, >95% purity by 1 H NMR). The NMR spectra consist of two sets of signals due to the presence of rotamers. 1 H NMR (250 MHz, CDCl 3 ) δ 9.58 (d, J=0.8 Hz, 1H), 9.52 (d, J=2.5 Hz, 1H), 4.32 (m, 1H), 4.16 (m, 1H), 4.06 (m, 4H), 1.53-1.63 (m, 12H), 1.49 (s, 9H), 1.40 (s, 9H). The crude product was used in the subsequent reaction without further purification.
(4R,1′Z)-3-(tert-Butoxycarbonyl)-2,2-dimethyl-4-(1′-hexadecenyl)oxazolidine (5)
[0230] n-BuLi (1.6 M in hexane, 25.2 mL, 40.3 mmol) was added dropwise to pentadecyltriphenylphosphonium bromide (24.03 g, 43.4 mmol) in anhydrous THF (220 mL) at −78° C. The resulting orange solution was allowed to warm to 0° C. and stirred for another 30 min. The solution was then cooled to −78° C. and Garner's aldehyde 4 (6.23 g, 27.2 mmol) in anhydrous THF (30 mL) was added slowly. After being stirred for 2 h at r.t., the reaction was diluted with sat. aq. NH 4 Cl solution (35 mL) and the layers were separated. The aqueous layer was extracted with CH 2 Cl 2 (3×35 mL) and the combined organic extracts were washed with sat. aq. NaCl solution (50 mL), dried over MgSO 4 and concentrated in vacuo. Purification by flash column chromatography on silica (EtOAc/Hexanes=1:2) gel gave (Z)-olefin 5 as a pale yellow oil (11.27 g, 78%). [α] D r.t. =+45.2 (c=1, CHCl 3 ); R f =0.40 (EtOAc/Hexanes=1:2); IR (film) ν max 2923, 2854, 1699, 1457, 1382, 1251, 1175, 1093, 1056, 850, 768 cm −1 ; 1 H NMR (250 MHz, CDCl 3 ) δ 5.27-5.40 (m, 2H), 4.58 (br s, 1H), 4.02 (dd, J=6.3, 8.8 Hz, 1H), 3.61 (dd, J=3.3, 8.5 Hz, 1H), 1.96 (br s, 2H), 1.23-1.56 (m, 39H), 0.85 (t, J=7 Hz, 3H); 13 C NMR (101 MHz, CDCl 3 ) δ 152.1, 130.9, 130.4, 94.1, 79.8, 69.2, 54.7, 32.1, 29.9, 29.8, 29.8, 29.8, 29.7, 29.6, 29.5, 29.4, 28.6, 28.6, 27.6, 22.8, 14.2; HR ESI Calcd for C 26 H 49 NO 3 [M+Na + ]: 446.3605. found: 446.3614. All spectral data were in good accordance with reported data. [4].
[0231] The desired (Z)-olefin can easily be distinguished from the undesired (E)-olefin by-product, when considering the olefinic protons in the 1 H NMR spectrum: Z-5 1 H NMR (250 MHz, CDCl 3 ) δ 4.05 (dd, J=6.3, 8.6 Hz, 1H), 3.64 (dd, J=3.3, 8.6 Hz, 1H) cf. E-5 1 H NMR (250 MHz, CDCl 3 ) δ4.01 (dd, J=6.1, 8.7 Hz, 1H), 3.71 (dd, J=2.1, 8.7 Hz, 1H).
Pentadecyltriphenylphosphonium Bromide
[0232] A solution of 1-bromopentadecane (30.0 g, 103 mmol) and triphenylphosphine (27.02 g, 103 mmol) in MeCN (200 mL) was refluxed at 80° C. for five days. After removal of the solvent in vacuo, Et 2 O (30 mL) was added and the resulting white precipitate was filtered off, washed with Et 2 O and dried on high vacuum for 24 h to give pentadecyltriphenylphosphonium bromide (49.66 g, 87%) as a white powder.
(2R,3Z)-2-(tert-Butoxycarbonyl)amino-3-octadecen-1-ol (5b)
[0233] Para-Toluensulfonic acid (371 mg, 1.95 mmol) was added to a stirred solution of (Z)-olefin 5 (5.00 g, 12.2 mmol) in MeOH/water (50 mL total, ratio=9:1 v/v) and the mixture was stirred for 68 h. The reaction mixture was concentrated in vacuo to yield a white solid, which was re-dissolved in CH 2 Cl 2 (100 mL). The solution was washed with brine (30 mL), dried over MgSO 4 and the solvent was removed in vacuo. Purification by flash column chromatography on silica gel (gradient cyclohexane/EtOAc=4:1→2:1) afforded alcohol 5b as a white solid (2.71 g, 59%). All spectral data were in good accordance with reported data.
(2S,3S,4R)-2-(tert-Butoxycarbonyl)amino-1,3,4-octadecanetriol (6)
[0234] Alcohol 5b (1.50 g, 3.91 mmol) was dissolved in t-BuOH/water (38 mL total, ratio 1:1) and methanesulfonamide (371 mg, 3.91 mmol) was added. The reaction mixture was cooled to 0 C and AD-mix-β (5.48 g) was added. The resulting mixture was stirred at 0° C. for 41 h and another 7 h at r.t., then it was quenched by the addition of solid Na 2 SO 3 (6.0 g) and left to stir for 30 min. Extraction with EtOAc (3×40 mL) followed. The organic extracts were washed with NaOH (1 M, 20 mL), water (20 mL) and sat. aq. NaCl solution (20 mL), dried over MgSO 4 and solvents were removed in vacuo. Purification by flash column chromatography on silica gel (gradient EtOAc/cyclohexane=1:1→2:1) provided triol 6 as a white solid (1.05 g, 64%).
Phytosphingosine (7)
[0235] Triol 6 (60 mg, 0.14 mmol) was dissolved in TFA (0.6 mL) and stirred at r.t. for 30 min. The solution was diluted with CH 2 Cl 2 (1.5 mL) and then carefully neutralized (to pH ˜8) with sat. aq. NaHCO 3 solution (10 mL) upon which precipitation of a white solid occurred. The white solid removed by filtration, washed with water (3×10 mL) and dried under reduced pressure. Recrystallization from MeCN yielded phytosphingosine 7 as a white powder (20 mg, 43%).
Ceramide (8)
[0236] To a solution of phytosphingosine 7 (15 mg, 0.047 mmol) in anhydrous THF (1 mL) was added hexacosanoic acid succinimidyl ester 11 (34 mg, 0.071 mmol) and Et 3 N (24 μL, 0.14 mmol). The solution was heated to 50° C. and stirred for 20 h. EtOAc (5 mL) was added and the resulting suspension was centrifuged (30 min., 3000 rpm). The white precipitate was removed by filtration and dried under reduced pressure to yield amide 8 (29 mg, 88%).
Hexacosanoic N-Hydroxysuccinimidyl Ester (11)
[0237] To a solution of hexacosanoic acid (121 mg, 0.304 mmol) in CH 2 Cl 2 (4 mL) were added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (0.058 mL, 0.33 mmol) and N-hydroxysuccinimide (42 mg, 0.37 mmol). The reaction mixture was heated to 40° C., stirred for 3 h and then quenched with water (4 mL). The solution was diluted with Et 2 O (8 mL) and the two layers were separated. The aqueous phase was extracted with Et 2 O (8 mL) and the combined organic layers were washed with sat aq. NaCl solution (5 mL), dried over MgSO 4 and filtered. After removal of the solvent in vacuo, N-hydroxysuccinimidyl ester 11 was obtained as a white solid (85 mg, 57%).
(2S,3S,4R)-1,3,4-Tri-t-butyl-dimethylsilyloxy-2-hexacosanoylamino-1-octadecane (9)
[0238] To a stirred suspension of amide 8 (25 mg, 0.036 mmol) in CH 2 Cl 2 (1.2 mL) was added TBSOTf (43 μL, 0.18 mmol) and 2,6-lutidine (65 μL, 0.054 mmol) at 0° C. The reaction mixture was stirred at r.t. for 2 h. The reaction was quenched with MeOH (0.2 mL). The mixture was diluted with Et 2 O (2 mL) and washed with sat. aq. NaHCO 3 solution (1 mL) and sat. aq. NaCl solution (1 mL). The organic layer was dried over MgSO 4 , filtered and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (cyclohexane/Et 2 O=15:1) to give TBS protected ceramide 9 as a colorless oil (27 mg, 71%).
(2S,3S,4R)-3,4-Bis-tert-butyldimethylsilyloxy-2-hexacosanoylamino-4-octadecanol (10)
[0239] To a solution of ceramide 9 (90 mg, 0,087 mmol) in THF (2 mL) was added TFA (40 μL, 0.519 mmol) in water (0.5 mL, 27.8 mmol) at −10° C. The reaction mixture was left to warm to 10° C. over a period of 2 h. Then, the reaction mixture was quenched by the addition of sat. aq. NaHCO 3 solution until neutral pH was reached. The resulting mixture was diluted with Et 2 O (10 mL), washed with water (10 mL), sat. aq. NaHCO 3 (10 mL), sat. aq. NaCl solution (10 mL), and dried over MgSO 4 . The solvent was removed in vacuo and the crude product was purified by flash column chromatography on silica gel (gradient EtOAc/cyclohexane=10:1→5:1) to yield alcohol 10 (68 mg, 85%) as a colorless oil. [α] D r.t. =−11.6 (c=1, CHCl 3 ); R f =0.3 (cyclohexane/EtOAc=4:1); IR (film) ν max 3285, 2920, 2851, 1645, 1465, 1253, 1034, 835, 776, 721, 680 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 6.27 (d, J=7.8 Hz, 1H), 4.21 (dd, J=11.3, 3.0 Hz, 1H), 4.06 (td, J=6.5, 3.2 Hz, 1H), 3.91 (t, J=2.8 Hz, 1H), 3.76 (td, J=6.4, 2.6 Hz, 1H), 3.59 (dd, J=11.3, 3.7 Hz, 1H), 2.24-2.14 (m, 2H), 1.69-1.45 (m, 4H), 1.45-1.16 (m, 68H), 0.92 (s, 9H), 0.90 (s, 9H), 0.87 (t, J=6.9 Hz, 6H), 0.11 (s, 6H), 0.08 (s, 6H); 13 C NMR (126 MHz, CDCl 3 ) b 172.8, 77.6, 76.6, 63.8, 51.4, 37.1, 34.6, 32.1, 30.0, 29.9, 29.8, 29.8, 29.7, 29.6, 29.5, 26.2, 26.1, 26.0, 25.8, 22.8, 18.3, 18.3, 14.3, -3.6, -3.9, -4.4, -4.8; HR ESI Calcd for C 56 H 117 NO 4 Si 2 [M+Na + ]: 924.8594. found: 924.8604.
[0240] According to the synthetic procedure for compound 10 starting from compound 2 derivatives 10a to 10o were prepared accordingly using the respective triphenylphosphonium bromides in the reaction of compound 4 to compound 5 and the corresponding compounds 11 in the conversion of compounds 7 to compounds 8:
[0000]
comp.
structure
mass spec
10a
C 35 H 75 NO 4 Si 2 Calc.: 631.1544 [M + H + ] Found: 631.1521
10b
C 45 H 95 NO 4 Si 2 Calc.: 771.4206 [M + H + ] Found: 771.4181
10c
C 38 H 73 NO 4 Si 2 Calc.: 665.1707 [M + H + ] Found: 665.1733
10d
C 43 H 83 NO 4 Si 2 Calc.: 735.3038 [M + H + ] Found: 735.3001
10e
C 50 H 97 NO 4 Si 2 Calc.: 833.4901 [M + H + ] Found: 833.4887
10f
C 56 H 109 NO 4 Si 2 Calc.: 917.6498 [M + H + ] Found: 917.6528
10g
C 37 H 69 F 2 NO 4 Si 2 Calc.: 687.1250 [M + H + ] Found: 687.1212
10h
C 47 H 99 NO 4 Si 2 Calc.: 799.4738 [M + H + ] Found: 799.4791
10i
C 48 H 101 NO 4 Si 2 Calc.: 813.5004 [M + H + ] Found: 813.4962
10j
C 50 H 97 NO 4 Si 2 Calc.: 833.4901 [M + H + ] Found: 833.4913
10k
C 39 H 67 NO 4 Si 2 Calc.: 671.1338 [M + H + ] Found: 671.1306
10l
C 49 H 87 NO 4 Si 2 Calc.: 811.4000 [M + H + ] Found: 811.4063
10m
C 57 H 103 NO 4 Si 2 Calc.: 923.6129 [M + H + ] Found: 923.6097
10n
C 46 H 95 NO 4 Si 2 Calc.: 783.4313 [M + H + ] Found: 783.4281
10o
C 51 H 105 NO 5 Si 2 Calc.: 869.5638 [M + H + ] Found: 869.5604
1-O-Allyl α-D-galactopyranoside (13)
[0241] To a stirred suspension of D-galactose 12 (22.2 g, 123 mmol) in allyl alcohol (250 mL) was added para-toluenesulfonic acid (2.3 g, 12.09 mmol). The mixture was heated to 100° C. and stirred for 24 h after which it was cooled to r.t. and quenched by the addition of NEt 3 . The solvent was removed in vacuo and the crude product was co-evaporated twice with toluene and purified by flash column chromatography on silica gel (gradient CH 2 Cl 2 /MeOH=9:1→4:1). Recrystalization from EtOAc yielded galactoside 13 (22.2 g, 88%) as a white solid.
1-O-Allyl 6-O-trityl-α-D-galactopyranoside (14)
[0242] 1-O-Allyl-galactoside 13 (4 g, 18.2 mmol) was dissolved in pyridine (18 mL). To the solution was added trityl chloride (6.58 g, 23.6 mmol) and the mixture was stirred at r.t. for 18 h after which the solvent was removed in vacuo. The crude product was purified by flash column chromatography on silica gel (CH 2 Cl 2 /MeOH=10:1) to yield pyranoside 14 (7.0 g, 83%) as colorless oil. [α] D r.t. =+60.0 (c=1, CHCl 3 ); R f =0.8 (CH 2 Cl 2 /MeOH=5:1); IR (film) ν max 3402, 2929, 1491, 1449, 1218, 1152, 1070, 1032, 746, 703 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 7.51-7.18 (m, 15H), 5.99-5.88 (m, 1H), 5.25 (ddq, J=35.9, 10.4, 1.4 Hz, 2H), 4.95 (d, J=3.8 Hz, 1H), 4.25 (ddt, J=12.8, 5.4, 1.4 Hz, 1H), 4.05 (ddt, J=12.8, 6.3, 1.3 Hz, 1H), 3.96 (s, 1H), 3.89 (t, J=5.8 Hz, 1H), 3.81 (d, J=5.7 Hz, 1H), 3.75 (d, J=9.8 Hz, 1H), 3.47 (s, 1H), 3.43 (dd, J=9.8, 6.1 Hz, 1H), 3.32 (dd, J=9.8, 5.3 Hz, 1H), 2.86 (d, J=2.1 Hz, 1H), 2.71 (d, J=8.1 Hz, 1H); 13 C NMR (75 MHz, CDCl 3 ) δ 143.8, 133.7, 128.6, 127.8, 127.1, 117.8, 97.5, 86.9, 71.2, 69.8, 69.5, 69.5, 68.5, 63.3; HR ESI Calcd for C 25 H 25 O 5 [M+Na + ]: 485.1935. found: 485.1941.
1-O-Allyl 2,3,4-tri-O-benzyl-6-O-trityl-α-D-galactopyranoside (15)
[0243] To a solution of allyl 6-O-trityl-α/β-D-galactopyranoside 14 (3.7 g, 8.0 mmol) in DMF (32 mL) was added sodium hydride (60% in mineral oil, 1.50 g, 36.0 mmol) portionwise at r.t. After 1 h benzyl bromide (4.2 mL, 35.2 mmol) was added. The reaction mixture was left to stir for 48 h after which it was quenched by the addition of MeOH (5 mL). The mixture was diluted with Et 2 O and extracted twice from sat. aq. NaHCO 3 . The combined organic layer was washed with water (3×100 mL) and sat. aq. NaCl solution and dried over MgSO 4 . The solvent was removed in vacuo and the crude product was over a plug of silica gel (hexanes/EtOAc=2:1, silica gel was neutralized with 1% NEt 3 ) to yield the benzyl ether 15 (5.5 g) as a pale yellow oil which was used in the subsequent step without further purification.
1-O-Allyl 2,3,4-tri-O-benzyl-α-D-galactopyranoside (16)
[0244] A solution of allyl 2,3,4-tri-O-benzyl-6-O-trityl-α-D-galactopyranoside 15 (5.00 g, 6.82 mmol) and triethyl silane (5.45 mL, 34.1 mmol) in CH 2 Cl 2 (68 mL) was cooled to 0° C. To the stirred solution was added trifluoroacetic acid (2.6 mL, 34.1 mmol) dropwise. The mixture was quenched after 15 min. with sat. aq. NaHCO 3 solution and extracted with CH 2 Cl 2 . The crude product was filtered over a plug of silica gel. All silane and trityl residues were removed with 10:1 hexanes/EtOAc and the product was eluted with EtOAc to yield 16 (3.0 g) as a pale yellow oil which was used without further purification in the subsequent reaction.
1-O-Allyl 6-(6′-azidohexyl)-2,3,4-tri-O-benzyl-α-D-galactopyranoside (17)
[0245] To a solution of allyl 2,3,4-tri-O-benzyl-α-D-galactopyranoside 16 (1.0 g, 2.04 mmol) in DMF (10 mL) was added sodium hydride (60% in mineral oil, 0.12 g, 3.1 mmol) at 0° C. After 15 min, the mixture was warmed to r.t. and stirred for another 1 h. Then, 6-azidohexyl 4-methylbenzenesulfonate 23 (0.9 g, 3.1 mmol) was added and the reaction mixture was stirred at r.t. for a further 8 h after which the mixture was quenched by the addition of MeOH (2 mL). After dilution with CH 2 Cl 2 , sat. aq. NH 4 Cl solution was added and the mixture was extracted with CH 2 Cl 2 (3×). The combined organic layer was washed with water and sat. aq. NaCl solution. The organic layer was dried over MgSO 4 , the solvent was removed in vacuo and the crude product was purified by flash column chromatography on silica gel (gradient hexanes/EtOAc=1:0→1:1) to yield azide 17 (1.0 g, 68% over three steps) as a colorless oil. [α] D r.t. =+25.4 (c=1, CHCl 3 ); R f =0.65 (Hexanes/EtOAc=4:1); IR (film) ν max 2933, 2863, 2094, 1497, 1454, 1358, 1177, 1098, 1059, 926, 816, 736, 697 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 7.94-7.16 (m, 15H), 5.95 (dddd, J=17.1, 10.3, 6.6, 5.2 Hz, 1H), 5.31 (dq, J=17.2, 1.6 Hz, 1H), 5.21 (ddd, J=10.3, 2.8, 1.1 Hz, 1H), 5.01-4.58 (m, 7H), 4.17 (ddt, J=13.0, 5.2, 1.4 Hz, 1H), 4.09-3.99 (m, 3H), 3.98-3.90 (m, 2H), 3.50-3.18 (m, 6H), 1.72-1.47 (m, 4H), 1.44-1.30 (m, 4H); 13 C NMR (75 MHz, CDCl 3 ) δ 138.9, 138.8, 138.6, 134.0, 129.8, 128.3, 128.3, 128.2, 128.1, 128.0, 127.9, 127.6, 127.5, 127.4, 117.9, 96.3, 79.1, 76.5, 75.3, 74.7, 73.3, 73.3, 71.3, 70.3, 69.5, 69.4, 68.2, 51.4, 51.2, 29.6, 28.8, 28.7, 28.6, 26.6, 26.1, 25.7, 25.0, 21.6. HR ESI Calcd for C 36 H 45 N 3 O 6 [M+Na + ]: 638.3201. found: 638.3229.
[0246] The below compounds were prepared according to the synthetic procedure above with the corresponding compounds 23 in moderate to high yields:
[0000]
comp.
structure
mass spec
17a
C 38 H 50 N 3 O 9 Calc.: 693.8278 [M + H + ] Found: 693.8241
17b
C 36 H 46 N 3 O 6 Calc.: 617.7764 [M + H + ] Found: 617.7721
17c
C 34 H 42 N 3 O 6 Calc.: 589.7231 [M + H + ] Found: 589.7274
17d
C 42 H 58 N 3 O 6 Calc.: 701.9361 [M + H + ] Found: 701.9400
17e
C 38 H 50 N 3 S 2 O 6 Calc.: 709.9618 [M + H + ] Found: 709.9651
17f
C 32 H 38 N 3 S 2 O 6 Calc.: 625.8021 [M + H + ] Found: 625.7996
6-(6′-Azidohexyl)-2,3,4-tri-O-benzyl-α/β-D-galactopyranose (18)
[0247] Allyl 6-(6′-azidohexyl)-2,3,4-tri-O-benzyl-α-D-galactopyranoside 17 (1.4 g, 2.3 mmol) was dissolved in MeOH (16 mL) and PdCl 2 (0.21 g, 1.17 mmol) was added to the solution at r.t. The mixture was stirred at for 4 h after which the mixture was filtered over celite and the solvent was removed in vacuo. The crude product was purified by flash column chromatography (gradient hexanes/EtOAc=1:0→1:1) to yield lactol 18 (1.2 g, 88%) as a colorless oil. R f =0.50 (Hexanes/EtOAc=2:1); IR (film) ν max 3414, 2933, 2862, 2093, 1454, 1255, 1060, 910, 733, 696 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 7.45-7.20 (m, 30H), 5.33-5.27 (m, 1H), 5.01-4.90 (m, 3H), 4.85-4.71 (m, 7H), 4.66 (ddd, J=16.7, 11.5, 6.0 Hz, 3H), 4.18-4.09 (m, 1H), 4.05 (dd, J=9.2, 3.6 Hz, 1H), 3.96 (s, 2H), 3.93 (d, J=2.8 Hz, 1H), 3.88 (d, J=2.8 Hz, 1H), 3.78 (dd, J=9.6, 7.5 Hz, 1H), 3.63-3.52 (m, 3H), 3.52-3.37 (m, 5H), 3.37-3.28 (m, 2H), 3.28-3.21 (m, 5H), 1.65-1.49 (m, 8H), 1.42-1.24 (m, 8H); 13 C NMR (101 MHz, CDCl 3 ) δ 138.8, 138.7, 138.5, 138.4, 128.5, 128.5, 128.4, 128.3, 128.3, 128.3, 128.3, 128.1, 127.9, 127.7, 127.7, 127.7, 127.6, 127.6, 97.9, 92.0, 82.3, 80.9, 78.8, 76.7, 75.2, 74.9, 74.8, 74.7, 73.8, 73.7, 73.6, 73.1, 73.1, 71.5, 71.4, 69.6, 69.6, 69.5, 51.5, 29.5, 28.9, 26.6, 25.8; HR ESI Calcd for C 33 H 41 N 3 O 6 [M+Na + ]: 598.2883. found: 598.2869.
[0248] The below compounds were prepared according to the synthetic procedure above with the corresponding compounds 17 in average good yields:
[0000]
comp.
structure
mass spec
18a
C 35 H 46 N 3 O 9 Calc.: 653.7638 [M + H + ] Found: 653.7601
18b
C 33 H 42 N 3 O 6 Calc.: 577.7124 [M + H + ] Found: 577.7193
18c
C 31 H 38 N 3 O 6 Calc.: 549.6592 [M + H + ] Found: 549.6556
18d
C 39 H 54 N 3 O 6 Calc.: 661.8721 [M + H + ] Found: 661.8791
18e
C 35 H 46 N 3 S 2 O 6 Calc.: 669.8978 [M + H + ] Found: 669.9003
18f
C 29 H 34 N 3 S 2 O 6 Calc.: 585.7381 [M + H + ] Found: 585.7323
6-(6′-Azidohexyl)-2,3,4-tri-O-benzyl-1-D-galactopyranosyl N-phenyl trifluoroacetimidate (19)
[0249] To a solution of 6-(6′-azidohexyl)-2,3,4-tri-O-benzyl-α/β-D-galactopyranose 18 (400 mg, 0.70 mmol) in CH 2 Cl 2 (7 mL) was added cesium carbonate (340 mg, 1.04 mmol). To the mixture was added 2,2,2-trifluoro-N-phenylacetimidoyl chloride 24 (216 mg, 1.04 mmol) and the reaction mixture was stirred at r.t. for 3.5 h after which it was filtered over celite and washed with CH 2 Cl 2 . The solvent was removed in vacuo and the crude product was purified by flash column chromatography on silica gel (gradient hexanes/EtOAc=10:1→1:1) to yield the imidate 19 (490 mg, 94%) as a colorless oil. [α] D r.t. =+60.8 (c=0.4, CHCl 3 ); R f =0.80 (Hexanes/EtOAc=2:1); IR (film) ν max 3064, 2934, 2865, 2094, 1717, 1598, 1454, 1321, 1207, 1099, 1027, 910, 734, 696 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 7.45-6.60 (m, 20H), 5.56 (s, 1H), 4.90 (d, J=11.5 Hz, 1H), 4.75 (s, J=1.5 Hz, 2H), 4.68 (s, J=12.4 Hz, 2H), 4.58 (d, J=11.6 Hz, 1H), 4.00 (t, J=8.7 Hz, 1H), 3.84 (d, J=2.4 Hz, 1H), 3.58-3.39 (m, 4H), 3.34 (dt, J=9.3, 6.5 Hz, 1H), 3.23 (dt, J=9.3, 6.5 Hz, 1H), 3.14 (t, J=6.9 Hz, 2H), 1.52-1.38 (m, 4H), 1.32-1.16 (m, 4H); 13 C NMR (101 MHz, CDCl 3 ) δ 138.6, 138.3, 138.2, 128.8, 128.6, 128.5, 128.4, 128.4, 128.3, 128.0, 127.9, 127.8, 127.7, 124.3, 119.4, 82.3, 78.3, 77.4, 77.2, 76.8, 75.7, 74.9, 74.6, 73.4, 73.2, 71.4, 68.7, 51.5, 29.7, 28.9, 26.7, 25.8; HR ESI Calcd for C 41 H 45 F 3 N 4 O 6 [M+Na + ]: 769.3183. found: 769.3239.
[0250] The below compounds were prepared according to the synthetic procedure above with the corresponding compounds 18 in average moderate to good yields:
[0000]
comp.
structure
mass spec
19a
C 43 H 50 F 3 N 4 O 9 Calc.: 824.8834 [M + H + ] Found: 824.8804
19b
C 41 H 46 F 3 N 4 O 6 Calc.: 748.8320 [M + H + ] Found: 748.8299
19c
C 39 H 42 F 3 N 4 O 6 Calc.: 720.7788 [M + H + ] Found: 720.7712
19d
C 47 H 58 F 3 N 4 O 6 Calc.: 832.9917 [M + H + ] Found: 832.9977
19e
C 43 H 50 F 3 N 4 S 2 O 6 Calc.: 841.0174 [M + H + ] Found: 841.0108
19f
C 37 H 38 F 3 N 4 S 2 O 6 Calc.: 756.8577 [M + H + ] Found: 756.8506
6-Hydroxyhexyl 4-methylbenzenesulfonate (21)
[0251] To a solution of hexane-1,6-diol 20 (10.0 g, 85 mmol) in CH 2 Cl 2 (200 mL) was added 4-methylbenzene-1-sulfonyl chloride (17.8 g, 93 mmol) dissolved in pyridine (100 mL) at 5° C. dropwise over 15 min. The reaction mixture was warmed to r.t. over the period of 5 h. Solvents were removed in vacuo and the crude was purified by silica flash column chromatography (gradient hexanes/EtOAc=1:0→1:1) to afford monotosylated hexanediol 21 (6.5 g, 28%) as a colorless oil. R f =0.55 (Hexanes/EtOAc=1:1); IR (film) ν max 3381, 2935, 2862, 1598, 1461, 1352, 1172, 959, 921, 813, 661 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 7.76-7.71 (m, 2H), 7.29 (dt, J=4.3, 1.2 Hz, 2H), 3.97 (t, J=6.5 Hz, 2H), 3.55 (t, J=6.5 Hz, 2H), 2.40 (s, 3H), 1.65-1.56 (m, 2H), 1.55 (s, 1H), 1.52-1.41 (m, 2H), 1.36-1.18 (m, 4H); 13 C NMR (101 MHz, CDCl 3 ) δ 144.7, 133.1, 129.8, 127.8, 70.5, 62.6, 32.4, 28.7, 25.1, 25.0, 21.6; HR ESI Calcd for C 13 H 20 O 4 S [M+Na + ]: 295.0975. found: 295.0968.
6-Azidohexan-1-ol (22)
[0252] 6-Hydroxyhexyl 4-methylbenzenesulfonate 21 (4.3 g, 15.79 mmol) was dissolved in DMF (23 mL) and sodium azide (1.75 g, 26.8 mmol) was added. The mixture was heated to 55° C. and after 16 h it was cooled to r.t. and diluted with water (150 mL). The mixture was extracted three times with CH 2 Cl 2 and washed with sat. aq. NaCl solution. The organic layer was dried over MgSO 4 and solvents were removed in vacuo. The crude product was purified by silica flash column chromatography on silica gel (gradient hexanes/EtOAc=1:0→1:1) to afford 6-azidohexan-1-ol 22 (2.2 g, 97%) as a colorless oil. R f =0.50 (Hexanes/EtOAc=2:1); IR (film) ν max 3329, 2935, 2891, 2090, 1256, 1349, 1258, 1055, 910, 731 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 3.63 (t, J=6.5 Hz, 2H), 3.25 (t, J=6.9 Hz, 2H), 1.64-1.51 (m, 4H), 1.43-1.32 (m, 4H); 13 C NMR (101 MHz, CDCl 3 ) δ2.8, 51.5, 32.6, 28.9, 26.6, 25.4; HR ESI Calcd for C 6 H 13 N 3 O[M+Na + ]: 166.0951. found: 166.0945.
6-Azidohexyl 4-methylbenzenesulfonate (23)
[0253] To a solution of 6-azidohexan-1-ol 22 (2.7 g, 18.9 mmol) in pyridine (70 mL) was added 4-methylbenzene-1-sulfonyl chloride (4.0 g, 21.0 mmol). The reaction mixture was left to stir for 5 h at r.t. after which the solvent was removed in vacuo and the crude product was dissolved in CH 2 Cl 2 , washed with water and dried over MgSO 4 . Solvents were removed in vacuo and the crude product was purified by silica flash column chromatography on silica gel (gradient hexanes/EtOAc=1:0→1:1) to afford azide 23 (5.0 g, 89%) as a colorless oil. R f =0.50 (Hexanes/EtOAc=3:1); IR (film) ν max 2938, 2863, 2092, 1598, 1455, 1356, 1258, 1174, 1097, 956, 919, 813, 724, 662 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ; 7.85-7.67 (m, 2H), 7.33 (dd, J=8.5, 0.6 Hz, 2H), 4.01 (t, J=6.4 Hz, 2H), 3.21 (t, J=6.9 Hz, 2H), 2.43 (s, 3H), 1.71-1.57 (m, 2H), 1.52 (dd, J=9.1, 4.9 Hz, 2H), 1.38-1.12 (m, 4H); 13 C NMR (101 MHz, CDCl 3 ) δ 144.8, 133.2, 129.9, 127.9, 70.4, 51.3, 28.7, 28.7, 26.1, 25.0, 21.7; HR ESI Calcd for C 13 H 19 N 3 O 3 S [M+Na + ]: 320.1045. found: 320.1057.
[0254] According to the synthetic route set forth above for compounds 20 to compounds 23 various starting materials have been tried out and successfully converted to corresponding compounds 23. For these syntheses Tetraethylenglycol was purchased at Merck, Germany; 2-(4-(2-hydroxyeth-1-yl)phenyl)ethanol was purchased at Sigma Aldrich; 2-methyl-1,3-propanol was purchased at Sigma Aldrich; dodecandiol was purchased by Sigma Aldrich; 2-Methypropane-1,3-bis(2-hydroxyethysulfide) was prepared according to the procedure disclosed in US2012/0295228.
[0000]
comp.
structure
mass spec
23a
C 15 H 23 N 3 SO 6 Calc.: 374.4344 [M + H + ] Found: 374.4388
23b
C 17 H 19 N 3 SO 3 Calc.: 346.4259 [M + H + ] Found: 346.4212
23c
C 11 H 15 N 3 SO 3 Calc.: 270.3297 [M + H + ] Found: 270.3229
23d
C 19 H 31 N 3 SO 3 Calc.: 382.5426 [M + H + ] Found: 382.5461
23e
C 15 H 23 N 3 S 3 O 3 Calc.: 390.5683 [M + H + ] Found: 390.5662
23f
C 9 H 11 N 3 S 3 O 3 Calc.: 306.4086 [M + H + ] Found: 306.4041
(2S,3S,4R)-3,4-Bis-tert-butyldimethylsilyloxy-2-hexacosanoylamino-1-(6-(6′-azidohexyl)-2,3,4-tri-O-benzyl)-α-D-galactopyranosyl)octadecane (25)
[0255] Nucleophile 10 (156 mg, 0.169 mmol) and glycosylating agent 19 (189 mg, 0.253 mmol) were co-evaporated with toluene three times and dried on high vacuum for 3 h after which they were dissolved in Et 2 O (2 mL) and THF (0.4 mL) and cooled to −40° C. To the mixture was added TMSOTf (9.0 μL, 0.051 mmol) and the solution was warmed to −10° C. over the period of 3 h. The reaction was quenched by the addition of NEt 3 (0.05 mL) and solvents were removed in vacuo and the crude product was purified by silica flash column chromatography (gradient hexanes/EtOAc=10:1→4:1) to afford glycoside 25 (180 mg, 72% α-anomer) as a white foam. [α] D r.t. =+18.9 (c=1, CHCl 3 ); R f =0.46 (Hexanes/EtOAc=6.5:1); IR (film) ν max 3328, 2925, 2854, 2096, 1731, 1656, 1452, 1348, 1246, 1156, 1099, 1058, 835, 777, 696 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 7.64-7.09 (m, 15H), 6.07 (d, J=7.1 Hz, 1H), 4.94 (d, J=11.5 Hz, 1H), 4.82 (d, J=3.7 Hz, 1H), 4.80-4.56 (m, 5H), 4.09 (td, J=7.6, 4.2 Hz, 1H), 4.03 (dd, J=10.1, 3.6 Hz, 1H), 3.97-3.85 (m, 5H), 3.82 (dd, J=10.9, 8.2 Hz, 1H), 3.66-3.61 (m, 1H), 3.50-3.42 (m, 1H), 3.38 (ddd, J=13.6, 8.1, 6.2 Hz, 2H), 3.29 (dt, J=9.4, 6.8 Hz, 1H), 3.22 (t, J=6.9 Hz, 2H), 1.99 (dd, J=16.6, 9.2 Hz, 2H), 1.60-1.45 (m, 8H), 1.39-1.15 (m, 70H), 0.91-0.84 (m, 26H), 0.06 (s, 3H), 0.05 (s, 3H), 0.02 (s, 6H). 13 C NMR (101 MHz, CDCl 3 ) δ 173.2, 138.6, 138.5, 138.0, 128.6, 128.6, 128.4, 128.3, 128.3, 128.1, 127.8, 127.8, 127.6, 99.3, 79.5, 76.4, 76.2, 74.9, 74.6, 74.4, 73.5, 72.9, 71.56, 70.1, 70.0, 69.4, 51.5, 49.6, 36.9, 33.5, 32.1, 29.9, 29.8, 29.7, 29.6, 29.6, 29.5, 29.5, 28.9, 26.7, 26.1, 25.9, 25.9, 22.8, 14.3; HR ESI Calcd for C 89 H 156 N 4 O 9 Si 2 [M+Na + ]: 1505.1333. found: 1505.1388.
[0256] The below compounds 25c-h were prepared according to the synthetic procedure above with the corresponding compounds 10 and 19 in average moderate to good yields:
[0000]
comp.
structure
mass spec
25c
C 70 H 119 N 4 O 9 S 2 Si 2 Calc.: 1282.0290 [M + H + ] Found: 1282.0317
25d
C 76 H 123 N 4 O 9 Si 2 Calc.: 1293.9930 [M + H + ] Found: 1293.9903
25e
C 84 H 131 N 4 O 12 Si 2 Calc.: 1446.1406 [M + H + ] Found: 1446.1458
25f
C 80 H 137 N 4 O 10 S 2 Si 2 Calc.: 1436.2787 [M + H + ] Found: 1436.2744
25g
C 68 H 105 F 2 N 4 O 9 Si 2 Calc.: 1217.7610 [M + H + ] Found: 1217.7588
25h
C 85 H 147 N 4 O 9 Si 2 Calc.: 1426.2802 [M + H + ] Found: 1426.2826
(2S,3S,4R)-2-Hexacosanoylamino-1-(6-(6′-azidohexyl)-2,3,4-tri-O-benzyl-α-D-galactopyranosyl)octadecane-3,4-diol (26)
[0257] To a solution of bis-TBS ether 25 (16.0 mg, 10.8 μmol) in THF (1 mL) was added a solution of TBAF (1 M in THF, 0.150 mL, 0.15 mmol) slowly. After 3.5 h the reaction mixture was diluted with CH 2 Cl 2 (10 mL). Solvents were removed in vacuo and crude product was purified by silica flash column chromatography (gradient hexanes/EtOAc=1:0→1:1) to afford diol 26 (10.5 mg, 78%) as a clear oil. [α] D r.t. =+121.9 (c=0.2, CHCl 3 ); R f =0.40 (Hexanes/EtOAc=2:1); IR (film) ν max 3329, 2919, 2851, 2096, 1640, 1543, 1467, 1455, 1350, 1094, 1046, 907, 730, 696 cm −1 ; 1 H NMR (400 MHz, CDCl 3 ) δ 7.58-7.08 (m, 15H), 6.37 (d, J=8.4 Hz, 1H), 4.94 (d, J=11.4 Hz, 1H), 4.88 (d, J=11.6 Hz, 1H), 4.85 (d, J=3.8 Hz, 1H), 4.82-4.73 (m, 2H), 4.68 (d, J=11.6 Hz, 1H), 4.60 (d, J=11.5 Hz, 1H), 4.22 (dq, J=6.8, 3.3 Hz, 1H), 4.05 (dd, J=10.0, 3.8 Hz, 1H), 3.95 (d, J=1.8 Hz, 1H), 3.88 (d, J=2.7 Hz, 2H), 3.87-3.75 (m, 2H), 3.55-3.36 (m, 5H), 3.31 (dt, J=9.4, 6.7 Hz, 1H), 3.25 (t, J=6.9 Hz, 2H), 2.20-2.11 (m, 3H), 1.70-1.44 (m, 8H), 1.41-1.17 (m, 73H), 0.88 (t, J=6.9 Hz, 6H); 10 13 C NMR (101 MHz, CDCl 3 ) δ 173.2, 138.6, 138.5, 130.0, 128.6, 128.6, 128.4, 128.3, 128.2, 128.1, 127.8, 127.8, 127.6, 99.3, 79.5, 76.4, 76.2, 74.9, 74.6, 74.4, 73.5, 72.9, 71.6, 70.1, 70.0, 69.4, 51.5, 49.6, 36.9, 33.5, 32.1, 29.9, 29.8, 29.7, 29.6, 29.6, 29.5, 29.5, 28.9, 26.7, 26.1, 25.9, 25.9, 22.8, 14.3; HR ESI Calcd for C 77 H 128 N 4 O 9 [M+Na + ]: 1275.9574. found: 1275.9536.
[0258] The below compounds 26c-h were prepared according to the synthetic procedure above for compound 26 in average moderate to good yields:
[0000]
comp.
structure
mass spec
26c
C 58 H 91 N 4 O 9 S 2 Calc.: 1053.5070 [M + H + ] Found: 1053.5046
26d
C 64 H 95 N 4 O 9 Calc.: 1065.4710 [M + H + ] Found: 1065.4677
26e
C 72 H 103 N 4 O 12 Calc.: 1217.6187 [M + H + ] Found: 1217.6203
26f
C 68 H 109 N 4 O 10 S 2 Calc.: 1207.7567 [M + H + ] Found: 1207.7532
26g
C 56 H 77 F 2 N 4 O 9 Calc.: 989.2390 [M + H + ] Found: 989.2371
26h
C 73 H 119 N 4 O 9 Calc.: 1197.7582 [M + H + ] Found: 1197.7614
(2S,3S,4R)-1-(6-(6′-Aminohexyl)-α-D-galactopyranosyl)-2-hexacosanoylaminooctadecane-3,4-diol (27)
[0259] To a solution diol 26 (55 mg, 0.044 mmol) in EtOH (0.5 mL) and chloroform (0.15 mL) was added Pd(OH) 2 on charcoal (10% w/w, wet 38 mg). The solution was stirred at r.t. under an atmosphere of Ar for 15 min. after which H 2 gas was inserted into the suspension and the mixture was hydrogenated for 12 h. The mixture was filtered over celite and thoroughly washed with CH 2 Cl 2 , THF and MeOH. Solvents were removed in vacuo and the crude was purified by silica flash column chromatography on silica gel (CH 2 Cl 2 /MeOH=4:1) to afford linker equipped GSL 27 (38 mg, 90%) as a pale yellow powder. [α] D r.t. =+66.1 (c=1.0, Pyridine); R f =0.44 (CH 2 Cl 2 /MeOH=4:1); IR (film) ν max 3292, 2918, 2850, 1640, 1539, 1468, 1304, 1073, 1038, 970, 721 cm −1 ; 1 H NMR (400 MHz, d-pyr) δ 8.66 (d, J=8.6 Hz, 1H), 5.48 (d, J=3.8 Hz, 1H), 4.59 (dd, J=10.6, 5.9 Hz, 1H), 4.49 (dd, J=9.7, 3.8 Hz, 1H), 4.39-4.15 (m, 1H), 3.91 (ddd, J=15.3, 10.4, 5.9 Hz, 1H), 3.74 (q, J=7.0 Hz, 1H), 3.44-3.31 (m, 2H), 3.17 (dd, J=13.1, 5.2 Hz, 2H), 2.42 (t, J=6.6 Hz, 2H), 2.17 (s, 1H), 1.89 (s, 2H), 1.84-1.65 (m, 4H), 1.65-0.97 (m, 75H), 0.75 (t, J=6.7 Hz, 6H); 13 C NMR (101 MHz, d-pyr) δ 171.9, 99.7, 75.5, 70.9, 70.1, 70.0, 69.6, 68.7, 66.7, 55.9, 49.9, 38.4, 35.4, 33.1, 30.7, 30.7, 29.0, 28.8, 28.6, 28.6, 28.6, 28.6, 28.5, 28.5, 28.4, 28.4, 28.2, 28.2, 26.8, 25.3, 25.1, 25.1, 24.7, 21.5, 17.8, 12.9; HR ESI Calcd for C 56 H 112 N 2 O 9 [M+H + ]: 957.8441. found: 957.8468.
[0260] The below compounds 26c-h were prepared according to the synthetic procedure above for compound 27 in average moderate to good yields:
[0000]
comp.
structure
mass spec
27c
C 37 H 75 N 2 O 9 S 2 Calc.: 757.1410 [M + H + ] Found: 757.1437
27d
C 43 H 79 N 2 O 9 Calc.: 769.1050 [M + H + ] Found: 769.1078
27e
C 51 H 87 N 2 O 12 Calc.: 921.2527 [M + H + ] Found: 921.2500
27f
C 47 H 93 N 2 O 10 S 2 Calc.: 911.3907 [M + H + ] Found: 911.3934
27g
C 35 H 61 F 2 N 2 O 9 Calc.: 692.8730 [M + H + ] Found: 692.8707
27h
C 52 H 103 N 2 O 9 Calc.: 901.3922 [M + H + ] Found: 901.3958
[0261] 2,3-Di-O-benzyl-4,6-O-benzylidene-D-galactose (33) was prepared according to ChemBioChem 2012, 1349.
2,3-di-O-benzyl-4,6-O-benzylidene-α-D-galactosyl trifluoroacetimidate (34)
[0262] To a solution of 2,3-Di-O-benzyl-4,6-O-benzylidene-D-galactose (800 mg, 1.786 mmol, coevaporated 3 times with dry toluene) 33 in CH 2 Cl 2 (7 mL) was added cesium carbonate (867 mg, 2.65 mmol). To the mixture was added 2,2,2-trifluoro-N-phenylacetimidoyl chloride 24 (551 mg, 2.65 mmol) and the reaction mixture was stirred at r.t. overnight after which it was filtered over celite and washed with CH 2 Cl 2 . The solvent was removed in vacuo and the crude product was purified by flash column chromatography on silica gel (gradient hexanes/EtOAc=8:1→1:1) to yield the imidate 34 (1.02 g, 92%) as a colorless oil. HR ESI Calcd for C 35 H 32 F 3 NO 6 [M+H + ]: 620.6362. found: 620.6327.
(2S,3S,4R)-3,4-Bis-tert-butyldimethylsilyloxy-2-hexacosanoylamino-1-(2,3-di-O-benzyl-4,6-O-benzylidene-α-D-galactopyranosyl)octadecane (35)
[0263] Nucleophile 10 (150 mg, 0.162 mmol) and glycosylating agent 34 (151 mg, 0.243 mmol) were co-evaporated with toluene three times and dried on high vacuum for 3 h after which they were dissolved in Et 2 O (2 mL) and THF (0.4 mL) and cooled to −40° C. To the mixture was added TMSOTf (8.0 μL, 0.043 mmol) and the solution was warmed to −10° C. over the period of 3 h. The reaction was quenched by the addition of NEt 3 (0.05 mL) and solvents were removed in vacuo and the crude product was purified by silica flash column chromatography (gradient hexanes/EtOAc=10:1-4:1) to afford glycoside 35 (140 mg, 64% α-anomer) as a white oil. HR ESI Calcd for C 83 H 143 NO 9 Si 2 [M+H + ]: 1356.2067. found: 1356.2098.
(2S,3S,4R)-3,4-Bis-tert-butyldimethylsilyloxy-2-hexacosanoylamino-1-(2,3,4-tri-O-benzyl-6-hydroxy-α-D-galactopyranosyl)octadecane (36)
[0264] To a solution of 35 (80 mg, 0.06 mmol) in anhydrous CH 2 Cl 2 (2 mL) under argon atmosphere were added copper(II) triflate (2 mg, 0.006 mmol) and BH 3 .THF (0.30 mL, 0.30 mmol). After stirring for 2 h at room temperature, the yellow reaction mixture was quenched with methanol. Subsequently the mixture was diluted with EtOAc and washed with sat. NaHCO 3 , water and brine. The organic layer was dried over Na 2 SO 4 and the solvent was removed in vacuo and the crude product was purified by silica flash column chromatography (gradient hexanes/EtOAc: 8.5/1.5) to afford glycoside 36 (62 mg, 78%) as a yellowish foam. HR ESI Calcd for C 83 H 145 NO 9 Si 2 [M+H + ]: 1358.2226. found: 1358.2196.
[0265] The Boc-protected PEG derivative 38 was purchased at Creative PEGWorks, Winston Salen, N.C., USA.
(2S,3S,4R)-3,4-Bis-tert-butyldimethylsilyloxy-2-hexacosanoylamino-1-(2,3,4-tri-O-benzyl-6-(carbonyl-1-ethyl-2-(tri(1-ethanoyl)1-ethanoyl-2-(tert-butoxy-carbonyl)amino)-α-D-galactopyranosyl)octadecane (37)
[0266] To a solution of 38 (18 mg, 0.05 mmol) in DMF (5 mL) was added O-(Benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate TBTU (16.1 mg, 0.05) and diisopropylethylamine (12.9 mg, 17 μl, 0.1 mmol). The mixture was stirred for 30 min at r.t. Then a mixture of 36 (50 mg, 0.04 mmol) in DMF (1 ml) was added to the reaction mixture and stirred for 5 hours. Subsequently, the reaction mixture was diluted with CH 2 Cl 2 (15 mL) and the resulting mixture was washed with 5% HCl (2×3 mL), 1M NaHCO 3 (3×3 mL) and water (2×3 mL). The organic layer was collected, dried (MgSO 4 ), filtered and concentrated to give the crude ester product which was purified by flash column chromatography on silica gel (gradient hexanes/EtOAc=8:1→1:1) to yield the linker-equipped glycolipid 37 (40 mg, 63%) as a colorless oil. HR ESI Calcd for C 99 H 174 N 2 O 16 Si 2 [M+H + ]: 1705.6272. found: 1705.6231.
[0267] Mono-tert.-butyl suberic acid was prepared according to Chem. Commun. 1999, 823.
[0268] Compound 37a was prepared according to the above reaction procedure in 53% yield.
[0000]
comp.
structure
mass spec
39
C 95 H 167 NO 12 Si 2 Calc.: 1572.5243 [M + H + ] Found: 1572.5216
(2S,3S,4R)-3,4-Bis-tert-butyldimethylsilyloxy-2-hexacosanoylamino-1-(2,3,4-tri-O-benzyl-6-(carbonyl-1-ethyl-2-(tri(1-ethanoyl)1-ethanoyl-2-amino)-α-D-galactopyranosyl)octadecane (25a)
[0269] 37 (40 mg, 0.02 mmol) was dissolved in TFA (1 mL) and stirred at r.t. for 30 min. The solution was diluted with CH 2 Cl 2 (2 mL) and then carefully neutralized (to pH ˜8) with sat. aq. NaHCO 3 solution (8 mL). Additional CH 2 Cl 2 . was added and the organic layer was dried over Na 2 SO 4 and the solvent was removed in vacuo and the crude product was purified by silica flash column chromatography (gradient hexanes/EtOAc: 10:1-1:1) to afford the linker-equipped glycolipid 25a (33 mg, 89%) as a yellowish oil. HR ESI Calcd for C 94 H 166 N 2 O 14 Si 2 [M+H + ]: 1605.5112. found: 1605.5088.
[0270] Compound 25b was prepared accordingly from compound 39:
[0000]
comp.
structure
mass spec
25b
C 91 H 159 NO 12 Si 2 Calc.: 1516.4179 [M + H + ] Found: 1516.4223
(2S,3S,4R)-2-Hexacosanoylamino-1-(2,3,4-tri-O-benzyl-6-(carbonyl-1-ethyl-2-(tri(1-ethanoyl)1-ethanoyl-2-amino)-α-D-galactopyranosyl)octadecane-3,4-diol (26a)
[0271] To a solution of bis-TBS ether 25a (33.0 mg, 20.7 μmol) in THF (1 mL) was added a solution of TBAF (1 M in THF, 0.150 mL, 0.15 mmol) slowly. After 3.5 h the reaction mixture was diluted with CH 2 Cl 2 (10 mL). Solvents were removed in vacuo and crude product was purified by silica flash column chromatography (gradient hexanes/EtOAc=1:0→1:1) to afford diol 26a (24.5 mg, 86%) as a clear oil. HR ESI Calcd for C 82 H 138 N 2 O 14 [M+H + ]: 1376.9893. found: 1376.9876.
[0272] Compound 26b was prepared accordingly from compound 25b:
[0000]
comp.
structure
mass spec
26b
C 79 H 131 NO 12 Calc.: 1287.8959 [M + H + ] Found: 1287.8914
(2S,3S,4R)-1-(6-(Carbonyl-1-ethyl-2-(tri(1-ethanoyl)1-ethanoyl-2-amino)-α-D-galactopyranosyl)-2-hexacosanoylaminooctadecane-3,4-diol (27a)
[0273] To a solution diol 26a (25 mg, 17.7 μmol) in EtOH (0.5 mL) and chloroform (0.15 mL) was added Pd(OH) 2 on charcoal (10% w/w, wet 35 mg). The solution was stirred at r.t. under an atmosphere of Ar for 15 min. after which H 2 gas was inserted into the suspension and the mixture was hydrogenated for 12 h. The mixture was filtered over celite and thoroughly washed with CH 2 Cl 2 , THF and MeOH. Solvents were removed in vacuo and the crude was purified by silica flash column chromatography on silica gel (CH 2 Cl 2 /MeOH=4:1) to afford linker equipped GSL 27a (18 mg, 92%) as a colorless oil. HR ESI Calcd for C 61 H 120 N 2 O 14 [M+H + ]: 1106.6209. found: 1106.6177.
[0274] Compound 27b was prepared accordingly from compound 26b:
[0000]
comp.
structure
mass spec
27b
C 58 H 113 NO 12 Calc.: 1017.5275 [M + H + ] Found: 1017.5231
5-((6-(((2R,3R,4S,5R,6S)-6-(((2S,3S4R)-2-hexacosanamido-3,4-dihydroxyoctadecyl)oxy)-3,4,5-trihydroxytetrahydro-2H-pyran-2-yl)methoxy)hexyl)amino)-5-oxopentanoic acid (40)
[0275] To gylocolipid 27 (10 mg, 10.44 μmol) in chloroform:methanol:triethylamine mixture (1:1:0.1, 7 ml) was added excess glutaric anhydride (14.9 mg, 131 μmol) in on eportion and left to stir at room temperature. After three days the completion of the reaction was indicated by the disappearance of the starting material mass on LCMS. The reaction was then evaporated to dryness and the resultant residue was triturated with dichloromethane to give the desired product 40 (8 mg, 72%) as a white solid.
[0000]
comp.
structure
mass spec
40
C 61 H 118 N 2 O 12 Calc.: 1069.861 [M + H + ] Found: 1069.642
Synthesis of the Antigen-Carbohydrate Glycolipid Conjugate:
[0276]
[0277] PS4 (1 mg) was dissolved in aq. NaOH solution (pH 10.95) to a final concentration of 10 mg/mL. The PS4 was activated with 15 μL of cyanogen bromide (10 mg/mL in acetonitrile) and left to stir at the room temperature for 10 min. To the activated PS4, μL of 27 was added (10 mg/2 mL in DMSO:THF, 1:1) and the mixture was incubated for 18 h at room temperature. After adjusting the pH to 6 with 0.1M aq. HCl, the mixture was dialyzed (12-14 k MWCO) against double distilled water, concentrated via ultrafiltration (10 k MWCO) then lyophilized.
[0278] Compounds 27a and 27c-h have been conjugated to PS4 accordingly and also showed immunogenic activity.
[0000]
[0279] Methyl ester 4.57 (provided by Dr. M. Oberli) (10 mg, 0,018 mmol) was dissolved in a mixture of THF (1.0 mL) and NaOH (0.1 M, 1 mL). The reaction mixture was stirred at r.t. for 1 h after which it was neutralized by the addition of Amberlite IR-120 (H+) resin. The resin was removed by filtration and solvents were removed in vacuo. The crude product was purified by silica gel chromatography (20% MeOH in CH2Cl2) to yield a white powder which was dissolved in THF (1.0 ml), water (1.0 mL) and MeOH (1.0 mL). To the mixture was added Pd on charcoal (20 mg). A stream of hydrogen was passed through the suspension for 20 min., after which the suspension was stirred for another 18 h under an H2 atmosphere. The suspension was filtered over celite and washed with MeOH and water (2×). Solvents were removed in vacuo and the crude product was purified by Sephadex G25 size-exclusion chromatography (eluent: 5% EtOH in water) to yield acid 4.13 (5.0 mg, 85% over two steps) a white powder. [α]D r.t.=−14.2 (c=1.0, water); Rf=0.67 (Isopropanol/1M aq. NH4OAc=2:1); IR (film) vmax 3256, 2938, 1571, 1410, 1050, 830 cm-1; 1H NMR (400 MHz, D2O) δ 4.00-3.84 (m, 3H), 3.74 (dd, J=19.7, 9.9 Hz, 3H), 3.63 (d, J=8.9 Hz, 1H), 3.46 (dd, J=15.8, 6.5 Hz, 1H), 3.01 (t, J=7.5 Hz, 2H), 2.43 (dd, J=12.1, 4.6 Hz, 1H), 1.79 (t, J=12.3 Hz, 1H), 1.67 (dd, J=14.0, 6.5 Hz, 2H), 1.63-1.57 (m, 2H), 1.44 (dd, J=15.2, 7.9 Hz, 2H); 13C NMR (101 MHz, D2O) δ 181.4, 173.9, 101.1, 73.3, 69.0, 67.4, 65.2, 64.1, 39.3, 34.7, 28.2, 26.3, 23.2, 22.0; HR ESI Calcd for C13H25NO8 [M−H+]: 322.1507. found: 322.1502.
[0000]
(2S,3S,4R)-1-(6-(6′-Hexanyl succinamido ethyleneglycol succinimidamido 5″-pentanyl α-3′″-deoxy-D-manno-oct-2′″-ulosonic acid pyranoside)-α-D-galactopyranosyl)-2-hexacosanoylaminooctadecane-3,4-diol (Glycoconjugate 43)
[0280] To a solution of linker-equipped KDO 42 (1.5 mg, 4.6 μmol) and glycolipid 27 (4.4 mg, 4.6 μmol) in DMSO/pyridine (0.1 mL, ratio=1:1 v/v) was added ethyleneglycol bissuccinimidyl succinate (EGS) (2.1 mg, 4.6 μmol) dissolved in DMF (0.1 mL). The reaction mixture was stirred at r.t. for 24 h after which solvents were removed by lyophilization. The crude product was purified by LH-20 size exclusion chromatography (eluent: MeOH/CH2Cl2=1:1) to yield conjugate 43 (3.0 mg, 42%) as a pale yellow powder. [α]D r.t.=+43.9 (c=0.2, Pyridine); Rf=0.54 (CH2Cl2/MeOH=85:15); IR (film) vmax 3308, 2918, 2850, 1781, 1709, 1645, 1548, 1467, 1378, 1211, 1157, 1071, 1020, 952, 816, 719 cm-1; 1H NMR (400 MHz, d-pyr) 8.52 (m, 2H), 8.44 (d, J=8.7 Hz, 1H), 5.56 (d, J=3.9 Hz, 1H), 5.26 (s, 1H), 4.88 (s, 1H), 4.66 (ddd, J=13.1, 9.9, 4.4 Hz, 2H), 4.55 (d, J=4.6 Hz, 1H), 4.52-4.39 (m, 5H), 4.39-4.31 (m, 7H), 4.20-3.93 (m, 2H), 3.85 (d, J=7.3 Hz, 1H), 3.79-3.72 (m, 1H), 3.47 (ddd, J=20.0, 14.8, 8.3 Hz, 3H), 3.39-3.32 (m, 1H), 3.22 (dd, J=11.9, 4.5 Hz, 1H), 3.08 (ddd, J=6.7, 5.8, 2.5 Hz, 1H), 2.94-2.84 (m, 4H), 2.79 (dd, J=8.5, 5.0 Hz, 3H), 2.73 (t, J=4.8 Hz, 2H), 2.53-2.49 (m, 18H), 2.33 (t, J=6.9 Hz, 1H), 1.99-1.66 (m, 4H), 1.66-1.47 (m, 6H), 1.42-1.20 (m, 71H), 0.89 (t, J=6.3 Hz, 6H). δ; 13C NMR (151 MHz, d-pyr) δ 173.6, 171.7, 170.5, 169.3, 101.9, 101.0, 77.1, 76.8, 72.9, 71.9, 71.9, 71.6, 71.4, 71.2, 71.1, 70.6, 69.5, 69.1, 67.8, 66.5, 64.4, 63.4, 63.3, 62.9, 62.8, 61.9, 51.7, 43.5, 41.5, 40.2, 40.1, 37.2, 37.2, 34.8, 32.6, 32.5, 31.3, 30.8, 30.6, 30.5, 30.5, 30.5, 30.4, 30.4, 30.4, 30.4, 30.3, 30.3, 30.3, 30.2, 30.0, 30.0, 29.3, 27.6, 27.0, 26.5, 26.5, 24.3, 23.4, 14.7; HR ESI Calcd for C79H147N3O23 [M+Na+]: 1529.0318. found: 1529.0363.
DESCRIPTION OF THE FIGURES
[0281] FIG. 1 . Model of glycoconjugate vaccine action.
[0282] The mode of action is illustrated by the antigen of invasive pneumococcal disease: the pneumococcal capsule polysaccharide (CPS) is covalently attached to a glycolipid. B cells specific for CPS will internalize the conjugate by receptor-mediated endocytosis and the conjugate will be cleaved in late endosomes, generating free αGalCer. In the late endosomal compartment, αGalCer will be complexed with CD1d antigen-presenting molecules and upon plasmamembrane recycling of CD1d be presented to invariant natural killer T (iNKT) cells.
[0283] Stimulation of iNKT cells by the αGalCer:CD1d complex on the surface of the antigen-presenting B cell will induce the release of soluble cytokines necessary for B cell help and memory generation. By this strategy a final long term immunological memory is induced, leading to the production of memory B-cells and the supply of high affinity IgG antibodies.
[0284] FIG. 2 . Glycoconjugate vaccine 1 containing the antigenic capsular polysaccharide portion PS4.
[0285] FIG. 3 . In vitro activity of the conjugate vaccine. αGalCer-CPS-pulsed CD1d-positive APC stimulate iNKT cells. Different batches of αGalCer-CPS type 4 conjugate vaccine (diamonds) are active in vitro when αGalCer is freed from CPS in living cells (A). αGalCer is entirely conjugated to CPS as remaining activity is not found when activating iNKT cells in a cell-free system (B). Unconjugated CPS type 4 (open circles) or αGalCer (closed circles) alone as control.
[0286] FIG. 4 . In vivo activity of the conjugate vaccine. Only αGalCer-CPS increases Abs response in C57BL/6 mice and the Abs response is dependent on NKT cells/CD1d. (A) WT C57BL/6 mice vaccinated with αGalCer-CPS (closed symbols) or CPS alone (open symbols) are bled after immunization and the CPS-specific Abs are assessed by ELISA. (B) WT C57BL/6 (WT, closed symbols) or CD1d-deficient (CD1d−/−, open symbols) mice immunized with αGalCer-CPS are bled after vaccination and the CPS-specific Abs are measured by ELISA.
[0287] FIG. 5 . In vivo antibody response after vaccination. The Abs response includes IgG subclasses and shows reactivity to common epitopes on different S. pneumoniae CPS. (A) WT C57BL/6 (WT, closed symbols) or CD1d-deficient (CD1d−/−, open symbols) mice immunized with αGalCer-CPS are bled after vaccination and the CPS-specific Abs subclasses are measured by ELISA (IgG1 given as representative example). (B) C57BL/6 mice vaccinated with αGalCer-CPS are bled after immunization and the CPS type 4 (closed symbols) or CPS type 2 (open symbols)-specific Abs are assessed by ELISA.
[0288] FIG. 6 . CPS-specific hybridomas express affinity matured IgM and all IgG subclasses with some preferential V, D, J segment usage. Hybridomas from αGalCer-CPS-immunized mice were established and classified by ELISA and sequencing. * aminoacid (aa) or nucleotide (nuc) substitutions in comparison to germ-line sequence.
[0289] FIG. 7 . Protection from infection with S. pneumoniae in a mouse model. CSP-specific mAbs promote bacterial opsonization. Uptake of fluorescently labeled S. pneumoniae serotype 4 into APC alone, in the presence of complement (C′) and/or mAbs 12F10 (CPS-specific hybridoma purified) or C15 (anti-human TCRAV24). Percent of positive cells according to background (OPA marker) is given in a table.
[0290] FIG. 8 . αGalCer-CPS-vaccinated C57BL/6 mice show long-term protection to challenge with S. pneumoniae . Mice vaccinated with αGalCer-CPS (A: closed symbols; B: line) or CPS alone (A: open symbols; B: dashed line) are infected with S. pneumoniae one week (A) or up to 3 months (B) after the last immunization. Mice are scored for disease, weight and survival over several days (given in hours). All αGalCer-CPS injected mice survived (B) without disease symptoms. Severe weight loss (A) is just observed for the CPS alone condition independently of the animal's survival (B).
[0291] FIGS. 9 and 10 . Isotype and specificity of anti-polysaccharide Abs (IgG, FIG. 9 ; IgM, FIG. 10 ).
|
The present invention relates to the field of synthesizing and biologically evaluating of a novel class of carbohydrate-based vaccines. The new vaccines consist of a multi-modular structure which allows applying the vaccine to a whole variety of pathogenes. This method allows preparing vaccines against all pathogens expressing immunogenic carbohydrate antigens. As conjugation of antigenic carbohydrates to proteins is not required the conjugate vaccine is particularly heat stable. No refrigeration is required, a major drawback of protein-based vaccines.
| 0
|
CROSS-REFERENCE TO RELATED APPLICATIONS
The present application is a continuation application to non-provisional application Ser. No. 13/671,534 filed Nov. 7, 2012 which is currently pending and related to and claimed priority from prior provisional application Ser. No. 61/628,996 filed Nov. 10, 2011.
FIELD OF THE INVENTION
This invention relates generally to the field of protecting secured assets, and particularly a method and system for creating a passcode to allow a user access to controlled assets and a passcode recovery process for when the source of the passcode fails to function.
BACKGROUND OF THE INVENTION
The protection of valuable assets is vital for government, private entities and individuals. Valuable assets are commonly protected by various access control systems to ensure that access to the assets are limited to only authorized persons. This includes protecting physical assets such as research labs with expensive equipment and file cabinets containing sensitive private information stored in the human resource department of a corporate office. Applications also include protecting electronic assets in the form of electronic data stored in computer and electronic systems. Access control systems use various authentication methods to control access to the physical and electronic assets. Typical authentication methods include passwords, tokens, access cards, biometrics, or other passcodes that ensure only authorized persons have access to the valuable assets.
Several problems arise when the authentication process malfunctions, such as when a user forgets a password, a token fails to work, or biometric match failure. Furthermore with respect to electronic data, stored and encrypted data will be lost, when a security system uses the passcode as an input for a data encryption algorithm or other secure transformation function. Users are encumbered with security features that require users to remember passwords, carry tokens, or utilize biometric features, so it is inevitable that such authentication methods regularly malfunction.
Existing authentication methods are vulnerable to misuse when a user attempts to recover a passcode after the authentication method fails to function, such as when the user forgets a password, has a malfunctioning token, or experiences a biometric match failure. For example, to reset a password the access control system must keep a record of the password in a database and send a copy to the user upon request. Alternatively, the access control system may establish a new random password and send a copy to the user. In both cases, the access control system knows the user's password. The password is thus vulnerable to disclosure to unauthorized users by means of attacks on the server, database, or the copy sent to the user. The password is also vulnerable to disclosure by unauthorized users from insider threats that lookup or reset the password from within the access control system. Furthermore, stored encrypted data will be permanently lost if the security system used the password as an input to the encryption algorithm and the original password was not stored in backup, or the user's stored encrypted data is susceptible to decryption by an unauthorized user with access to the stored password in backup.
This invention provides a novel method allowing an authorized user access to controlled assets when a passcode method malfunctions, such as when a user forgets a password, a token malfunction, or a biometric mismatch. For example, the invention allows temporary access to an access control system without knowing the password and without sending the user the password or a new random password. The user is able to set a new password without knowing the previous password. Furthermore, stored encrypted data is preserved and made accessible once again via the new password. This invention works for many authentication methods such as restoring access when a password, token, access card, or biometric method is used.
BRIEF SUMMARY OF THE INVENTION
In one embodiment of the invention a method for creating a passcode which may be derived from a password, token or biometric sample to allow a user access to controlled assets and a passcode code recovery process for when the source of the passcode (i.e. password, token, or biometric sample) fails to function comprises the first step of creating a passcode. Next, if needed, the passcode is converted into a numeric value. Next, either a predetermined value or a generated random code that is at least the same order of magnitude as the passcode or its numeric conversion is used as the first cryptographic recovery split. Next, the passcode and random code are used as inputs in a cryptographic derivation function to form a second cryptographic recovery split. More recovery splits may be generated if needed, but two is the minimum required. Next, the first cryptographic recovery split is stored in one repository and the second cryptographic recovery split is stored in a second repository that is isolated from the first repository. Next, when the source of the passcode fails to function, the first cryptographic recovery split is retrieved from the first repository and the second cryptographic recovery split is retrieved from the second repository. Next, the two cryptographic recovery split values are recombined in a reverse operation to reproduce the original passcode. Next, a new source of the passcode is supplied (i.e. a new password, new token, or new biometric sample) and cryptographically reconciled with the cryptographic derivation function to produce the same passcode. Alternatively, a new passcode can be generated and all existing electronic data may be encrypted using the new passcode instead of the original passcode. Next, a new random code is created that is at least the same size as the new passcode. Finally, the new passcode and new random code are used as inputs in a cryptographic derivation function to form a new second cryptographic recovery split with the new first cryptographic recovery split stored in a first repository and the new second cryptographic recovery split stored in a second repository.
In another embodiment of the invention a system for creating a passcode which may be derived from a password, token or biometric sample to allow a user access to controlled assets and a passcode code recovery process for when the source of the passcode (i.e. password, token, or biometric sample) fails to function comprises a first device for creating a passcode. The passcode creation device is coupled to a random code generation device that uses a predetermined value or creates a random code of at least the same order of magnitude as the passcode to be used as a first cryptographic recovery split. Next a cryptographic derivation function device executes a cryptographic split operation using the passcode and random code as inputs to form a second cryptographic recovery split. The cryptographic derivation function device is coupled to at least two repositories. The random code is stored in the first repository as one cryptographic recovery split. The output of the cryptographic derivation function is stored in a second repository as the second cryptographic split. The source of the passcode (i.e. password, token, or biometric sample) is not stored in the first or second repositories; instead it is either stored in the user's memory, on an access card or another type of storage device separate from the first or second repositories. Next, when the source of the passcode (i.e. password, token, or biometric sample) fails to function the user initiates the passcode code recovery device which retrieves the random code from the first repository and the output of the cryptographic derivation function from the second repository then the two cryptographic recovery split values are recombined in a reverse operation to reproduce the original passcode. Next, a new source of the passcode is supplied (i.e. a new password, new token, or new biometric sample) and cryptographically reconciled with the cryptographic derivation function to produce the same passcode. Alternatively, a new passcode can be generated and all existing electronic data may be encrypted using the new passcode instead of the original passcode. Finally, the devices of this system are used again to repeat the steps required creating a new random code and new cryptographic recovery splits.
BRIEF DESCRIPTION OF THE DRAWINGS
Features and advantages of the claimed subject matter will be apparent from the following detailed description of embodiments consistent therewith, which description should be considered with reference to the accompanying drawings, wherein:
FIG. 1 is a diagram of an exemplary embodiment for creating a passcode and the cryptographic recovery splits needed for the passcode recovery process in accordance with the teachings of the present invention;
FIG. 2 is a diagram of an exemplary embodiment for a passcode recovery process needed when the source of the passcode fails to function in accordance with the teachings of the present invention;
FIG. 3 is a diagram of an exemplary embodiment for a system to create a passcode and the cryptographic recovery splits needed for the passcode recovery process in accordance with the teachings of the present invention;
FIG. 4 is a diagram of an exemplary embodiment for a system that uses the source of the passcode to gain access to the controlled assets being protected by the access control system in accordance with the teachings of the present invention;
FIG. 5 is a diagram of an exemplary embodiment for a system including a passcode recovery device needed when the source of the passcode fails to function in accordance with the teachings of the present invention;
FIG. 6 is a diagram of an exemplary embodiment for an apparatus incorporating components that function in accordance with the teachings of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The following describes the details of the invention. Although the following description will proceed with reference being made to illustrative embodiments, many alternatives, modifications, and variations thereof will be apparent to those skilled in the art. Accordingly, it is intended that the claimed subject matter be viewed broadly. Examples are provided as reference and should not be construed as limiting. The term “such as” when used should be interpreted as “such as, but not limited to.”
FIG. 1 is a diagram of an exemplary embodiment for a method 100 to create a passcode 105 allowing a user 110 access to controlled assets 120 within an access control system 130 . The user 110 described throughout this specification may include a person, or an automated system controlled by computer software or other artificial intelligence. The controlled assets 120 may be physical assets such as a building, locked room, safe, or file cabinet; or an electronic asset such as data stored on a computer or electronic system. Furthermore, the passcode 105 and access control system 130 may comprise any type of system intended to control access to controlled assets 120 such as a direct passcode system, a token system which essentially stores the source of the passcode on a token device such as an RF chip within a fob or an access card, or a biometric system which essentially associates a passcode to the unique biometric features of a person, or thing, or any type of access control system that essentially uses a passcode. Examples of this invention are provided as reference throughout the specification using various passcode and access control systems, but any passcode and access control system may be substituted in the examples to exemplify this invention.
First the source for the passcode 101 is used as an input to create the passcode 140 . For example, a user 110 uses a numerical input console 115 to create a source for the passcode 101 that is used as the input to create a passcode 105 which allows the user 110 to access the controlled assets 120 within the access control system 130 . In some circumstances, the access control system 130 may allow use of a non-numeric passcode 151 such as a code using letters or special characters. In such a circumstance, the non-numeric passcode 151 is converted 150 to the passcode 105 with a numerical value. Next either a predetermined value or numerical random code 161 is created that is the same order of magnitude or greater as the value of the passcode's 105 numeric value. For example, if the passcode 105 comprises a number with six digits, the random code 161 will also comprise at least six digits.
Next the random code 161 and the passcode 105 are used as inputs for a cryptographic derivation function 170 to form a second cryptographic recovery split 171 . More recovery splits may be generated if needed, but two is the minimum required. The cryptographic derivation function 170 may be accomplished by using a reversible algorithm such as the Exclusive-OR (“XOR”) binary Boolean algebraic operation. The passcode 105 and random code 161 are used as inputs in the cryptographic derivation function 170 to form a second cryptographic recovery split 171 with the first encrypted split 161 stored in one repository 180 and the second encrypted split 171 stored in a second repository 190 . For example, the random code 161 is stored on a first storage device as one cryptographic split and the output of the cryptographic split 171 is stored on a second storage device as the second cryptographic split component 171 . The order in which the encrypted splits 161 and 171 are stored is not significant. The output from the XOR operation 171 could be stored in the first repository and the random code 161 could be stored in the second repository.
The passcode 105 is not stored on the first or second repositories; instead it is stored in a repository separate from the first or second repositories 180 and 190 that contain the recovery splits 161 and 171 . Alternatively, one of the cryptographic recovery splits 161 or 171 may be stored on the asset control system 130 or the same device that contains the user's encrypted data. The source of the passcode such as the password, token, or biometric sample is not stored in the first or second repositories; instead it is either stored in the user's memory, on an access card or another type of storage device separate from the first or second repositories 195 .
The XOR operation is ideal for encryption since it is virtually impossible to reverse without knowing the initial value of one of the two binary arguments and the output from the XOR operation; however any other type of reversible cryptographic split operation may be used. In other words, using the XOR operation the passcode 105 cannot be recovered without the random code 161 and the output of the XOR operation 171 . The random code 161 and the output of the XOR operation 171 are each useless by themselves because they individually cannot be used to recover the passcode 105 . However, the passcode 105 can be recovered when the random code 161 and the output of the XOR operation 171 are subjected to the inverse XOR operation.
FIG. 2 is a diagram of an exemplary embodiment for a method 200 to recover the passcode 222 when the source of the passcode 201 fails to function. First, the first cryptographic recovery split 207 is retrieved from the first repository 205 and the second cryptographic recovery split 212 is retrieved from the second repository 210 . In other words, the random passcode 207 is retrieved from the first repository 205 and the output from the XOR operation 212 is retrieved from the second repository 210 . The user 201 can have access to the first repository 205 and can readily obtain the first cryptographic recovery split 207 . The first repository 205 is available from the access control system 202 , is in the user's possession, or is otherwise directly available to the user through a third party.
The output from the XOR operation 212 (or 540 referring to FIG. 5 ), however, is not directly available to the user 201 (or 515 referring to FIG. 5 ). Instead, the user 515 must request the output from the XOR operation 540 from a separately controlled second repository 550 , referring to FIG. 5 . For example, the second repository 550 may be a central database under the control of a custodian 560 . To gain access to the output from the XOR operation 540 the user 565 must first authenticate his/her identity, such as by answering questions that only the user 565 would be able to answer or other alternative means of identification commensurate with the security policy of the asset control system 590 . This may be accomplished by human interaction, or with an automated system coupled to the central database. Once the user 565 correctly authenticates his/her identity to the custodian 560 , the output from XOR operation 540 is released to the user 565 , or the access control system 590 .
Next referring to FIG. 2 , the two cryptographic recovery splits 207 and 212 are recombined by performing a reverse cryptographic derivation function 220 to recover the passcode 222 . The XOR operation 220 may be done by a component of the access control system 202 , such as a passcode recovery device 570 , referring to FIG. 5 , or a computer 580 coupled 585 to the access control system 590 . The reverse XOR operation 220 uses the random code 207 and the output of the XOR operation 212 as inputs to recover the passcode 222 .
With the recovered passcode 222 , the user 201 is able to gain temporary access to the access control system 202 . Next, a new source of the passcode 206 is supplied such as a new password, new token, or new biometric sample and cryptographically reconciled with the cryptographic derivation function 220 to produce a new passcode 209 . The new passcode 209 may be identical to the original passcode 222 . Now any encrypted electronic data requiring the recovered passcode 222 may be decrypted 240 to prevent the loss of stored encrypted data. Alternatively the new passcode 209 can be generated with a unique value.
The method described in FIG. 1 can now be repeated 250 . Referring to FIG. 1 , for example if needed, the new passcode 105 may be converted into a numeric value 151 . Next, a new random code 161 is created that is at least the same order of magnitude as the original passcode or new passcode 105 . Finally the new passcode 105 and new random code 161 are used as inputs in the cryptographic derivation function 170 to form a second cryptographic recovery split 171 with the first cryptographic recovery split 161 stored in one repository 180 and the second cryptographic recovery split 171 stored in a second repository 190 .
FIG. 3 is an embodiment of the invention for a system 300 used to create a passcode 325 which may be derived from a source of the passcode 303 such as a password, token, or biometric sample to allow a user 301 access to controlled assets 380 in an access control system 370 . The system 300 comprises a passcode creation device 305 . In one embodiment, the passcode creation device 305 comprises a numerical input console 310 such as a keyboard, or other type of numeric console for inputting the source of the passcode 303 . The source of the passcode 303 may include a password, token, or biometric sample. In some circumstances, the passcode creation device 305 may comprise an input console 310 that creates a non-numeric passcode 315 such as a code using letters or special characters. In such a circumstance, the non-numeric passcode 315 must be converted to a numerical passcode 325 using a numeric code conversion device 320 . Next, the passcode creation device 305 is coupled to a random code generation device 330 that uses a predetermined value or creates a random code 335 of at least the same order of magnitude as the passcode 325 to be used as a first cryptographic recovery split. For example, if the passcode 325 comprises a number with six digits, the random code generation device 330 will create a random code 335 also comprising at least six digits. It is important for the random code 335 to have the same order of magnitude or greater than the passcode 325 so the two binary components can be used as inputs to a cryptographic derivation function device 340 .
Next the system comprises a cryptographic derivation function device 340 that executes a cryptographic split operation using the passcode 325 and random code 335 as inputs to form a second cryptographic recovery split 350 . The cryptographic derivation function device 340 accomplishes the cryptographic split by using a reversible algorithm such as the Exclusive-OR (“XOR”) binary Boolean algebraic operation. The random code 335 and the passcode 325 are used as inputs for a cryptographic derivation function to form a second cryptographic recovery split 350 . More cryptographic recovery splits may be generated if needed, but two is the minimum required. The first cryptographic recovery split, i.e. the random code 335 , is stored in one repository 355 and the second cryptographic recovery split, i.e. the output to the XOR operation 350 , is stored in a second repository 360 . The order in which the cryptographic recovery splits are stored is not significant. In other words, the output from the XOR operation 350 could be stored in the first repository 355 and the random code 335 could be stored in the second repository 360 . The repositories 355 and 360 may include any type of permanent or semi-permanent storage device capable of retaining the cryptographic recovery split such as random access memory (RAM) and read only memory (ROM) in a computer, server, network, and electronic database; printed on paper; or output onto a punch card.
The source of the passcode 303 is not stored in the first or second repositories 355 and 360 ; instead it is either stored in the user's memory, on an access card or another type of storage device 303 separate from the first or second repositories 355 and 360 . The passcode 325 is also not stored on the first or second repositories 355 and 360 ; instead it is stored in a passcode repository 365 separate from the first or second repositories 355 and 360 .
FIG. 4 is a diagram of the invention 400 illustrating a typical use in which the user 405 retrieves the source of the passcode 415 from the source of the passcode repository 418 which in turn enables the passcode 420 to be retrieved from the passcode repository 410 and passed to the access control system 430 to gain access to the controlled assets 420 within the access control system 430 . To access the source of the passcode, the user may use some source 408 such as a password entered with a console, via a token, or from a biometric sample. The access control system 430 authenticates the passcode 420 and then allows the user 405 access to the controlled assets 420 .
FIG. 5 is a diagram of an exemplary embodiment of the invention for a system 500 used to recover a passcode 570 when the source of the passcode 303 (referring to FIG. 3 ) such as a password, token, or biometric sample fails to function comprising a first passcode recovery device 510 . The passcode recovery device 510 retrieves the random code 520 from the first repository 530 and the output from the XOR operation 540 from the second repository 550 . The first repository 530 is situated such that the user 565 has ready access to the first repository 530 to obtain the random code 520 . For example, the first repository 530 may be coupled 535 to the access control system 590 , the user's computer, local system, server, or network 568 in the user's possession, or otherwise directly available to the user 565 .
The output from the XOR operation 540 , however, is not directly available to the user 565 . The user 565 must request the output from the XOR operation 540 from a separately controlled second repository 550 . For example, the second repository 550 may be a central database, server, computer, or network under the control of a custodian 560 . To gain access to the output from the XOR operation 540 , the user 565 must first authenticate his/her identity by answering questions that only the user 565 would be able to answer. This may be accomplished by human interaction, or with an automated system coupled to the separately controlled second repository 550 . Once the user 565 correctly authenticates his/her identity to the custodian 560 , the output from XOR operation 540 is released to the passcode recovery device 510 .
The passcode recovery device 510 then executes an inverse cryptographic split operation using the random code 520 and the output of the XOR operation 540 as inputs to reproduce the original passcode 570 . The passcode recovery device 510 may be a component of the access control system 590 , such as a computer 580 coupled 585 to the access control system 590 .
The user 565 is thus able to gain temporary access to the access control system 590 once the passcode 570 has been recovered. The process and devices used to create the passcode and recovery features can again be repeated. Referring to FIG. 1 , the user 301 then supplies a new source for the passcode 303 such as a new password, new token, or new biometric sample that is cryptographically reconciled with the cryptographic derivation device 340 . Any electrical data encrypted with the passcode may be decrypted preventing loss of stored encrypted data. Finally, the devices comprising this system described in FIG. 1 through FIG. 5 may be used again to create new cryptographic recovery splits.
Throughout this description reference was made to several discreet devices, such as the passcode creation device 601 , random code generation device 602 , numeric passcode conversion device 603 , passcode repository 604 , first and second cryptographic recovery split repositories 605 and 606 , access control system 607 , and a passcode recovery device 607 . An apparatus such as a computer, electronic, or security apparatus may be devised where such discreet devices are combined into fewer devices, or designed with components and programed to execute the steps and incorporate the features described in this invention. FIG. 6 illustrates an example, where the hardware 610 and software 620 of a computer, electronic system, or security system 600 could be designed to perform many, and possibly all of the functions and features described by this invention.
Several devices described throughout this invention may be coupled in a manner that allows the exchange and interaction of data, such that the operations and processes described may be carried out. For example, the devices may be coupled with electrical circuitry, or through wireless networks that allow the devices to transfer data, receive power, execute the operations described, and provide structural integrity.
The terms and expressions which have been employed herein are used as terms of description and not of limitation, and there is no intention, in the use of such terms and expressions, of excluding any equivalents of the features shown and described (or portions thereof), and it is recognized that various modifications are possible within the scope of the claims. Other modifications, variations, and alternatives are also possible. Accordingly, the claims are intended to cover all such equivalents.
|
This invention provides a novel method, system, and apparatus allowing an authorized user access to controlled assets when a passcode method malfunctions, such as when a user forgets a password, a token malfunction, or a biometric mismatch. The invention allows temporary access to an access control system without knowing the password and without sending the user the password or a new random password. The user is able to set a new password without knowing the previous password. Furthermore, stored encrypted data is preserved and made accessible once again via the new passcode. This invention works for many authentication methods such as restoring access when a password, token, access card, or biometric sample is used.
| 7
|
FIELD OF THE INVENTION
[0001] The present invention relates generally to the field of Universal Description, Discovery and Integration (UDDI) systems, and more particularly to a UDDI system that includes a performance monitoring system that makes available to a UDDI registry performance attributes for Web services registered with the UDDI registry.
BACKGROUND OF THE INVENTION
[0002] Universal Description, Discovery and Integration (UDDI) is a standards-based set of services supporting the description and discovery of Web service providers, the services the Web service providers make available, and the technical interfaces that may be used to access the services. Web services typically include data and/or small applications that may be used by Web service consumers or integrated into Web service consumers' solutions. Examples of Web services include stock quotes, local weather, Body Mass Index (BMI) calculators, and the like. Using common industry standards, such as HTTP, XML and SOAP, UDDI provides an interoperable infrastructure for a Web services-based software environment for both public available services and services exposed only internally within an organization.
[0003] A key component of the UDDI system is a UDDI registry. A UDDI registry allows Web service providers to register information about the Web services they offer so that Web service consumers can find them and use their services. A UDDI registry stores Web Service Definition Language (WSDL) files. WSDL is an XML-based language that describes an interface of a Web service together with information on how to call the Web service and where to find it.
[0004] A Web service provider can register three types of information in a UDDI registry. These types of information are commonly referred to as White Pages, Yellow Pages, and Green Pages. The White Pages contain basic identification information such as name, address, or other identifiers, such as Dun & Bradstreet's D-U-N-S numbers. The White Pages allow consumers to find a Web service provider based upon its identity. The Yellow Pages describe Web services using different categories or taxonomies. The Yellow pages allow consumers to find Web service providers based upon the categories of services they provide. The Green Pages provide technical information about how to interface with the Web service provider's services.
[0005] UDDI allows a consumer to find a Web service using means such as database look-ups, configuration files, or by making a Web service call to an ad hoc broker service. UDDI supports a very flexible taxonomy-based query mechanism that allows a consumer to select Web service based on classification schemes, such as physical location, cost of use, Quality of Service (QOS) guarantees, and the like. Though the provider of a Web service may claim a QOS guarantee, there is no feedback mechanism in place by which a UDDI registry can receive input from a third party regarding the delivery of a Web service.
SUMMARY OF THE INVENTION
[0006] In one of its aspects, the present invention provides a method of providing performance information in a Universal Description, Discovery and Integration (UDDI) system. A method according to the present invention requests data from a Web service provider that is registered in a UDDI registry. The method determines at least one performance attribute for the Web service provider based upon the requested data. Then, the method stores the at least one performance attribute in a performance metric store that is accessible by the UDDI registry.
[0007] Preferably, the method periodically requests data from a plurality of Web service providers, each of which is registered with the UDDI registry. The method stores the latest, or most currently determined, performance attribute for each of the Web service providers in the performance metric store. Thus, the method dynamically updates the performance attributes stored in the performance metric store.
[0008] The UDDI registry receives requests from Web service consumers for lists of Web service providers that provide specified Web services. According to a method of the present invention, the UDDI registry may access the performance metric store to obtain performance attributes for the listed Web service providers. The UDDI registry may return the performance attributes either along with the list or in response to a separate request from the Web service consumer.
[0009] The UDDI registry and performance monitoring processes of a method according to the present invention may run independently of each other. The performance monitoring process goes about its work of dynamically updating the contents of the performance metric store with currently determined performance attributes. At the same time, the UDDI registry services requests from Web service consumers with current performance attributes stored in the performance metric store.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a block diagram of a system according to the present invention.
[0011] FIG. 2 is a flow chart of an embodiment of performance monitor processing according to the present invention.
[0012] FIG. 3 is a message flow diagram according an embodiment of the present invention.
[0013] FIG. 4 is a message flow diagram according to an alternate embodiment of the present invention.
[0014] FIG. 5 is a block diagram of an information handling system adapted to implement components of a system according to the present invention.
DETAILED DESCRIPTION
[0015] Referring now to the drawings, and first to FIG. 1 , an embodiment of a system according to the present invention is designated generally by the numeral 101 . System 101 is preferably implemented in a network environment. A Web service client computer 103 is connected to the Internet 105 . A plurality of Web service provider computers, including Web service providers 107 a , 107 b , and 107 n , are also connected to Internet 105 . Web service client 103 and Web service providers 107 a - n may thus communicate with each other using well known protocols. Although FIG. 1 illustrates a network comprising the Internet, it will be recognized that other networks, such as internal intranets, may be used according to the present invention.
[0016] As is known by those skilled in the art, Web service providers 107 a - n are adapted to provide Web services. Web services typically include data and/or small applications that may be used by Web service consumers or integrated into Web service consumers' solutions. Examples of Web services include stock quotes, local weather, Body Mass Index (BMI) calculators, and the like.
[0017] When a Web service consumer integrates a Web service into its solution, the Web service consumer wants the Web service to provide accurate, reliable and timely information. It is therefore important to Web service consumers that Web services meet certain quality of service (QOS) standards. Additionally, a Web service consumer may want to use the Web service that provides the most accurate, reliable and timely information. Accordingly, the system of the present invention provides to Web service consumers performance information obtained by a trusted third-party provider.
[0018] A local area network (LAN) 109 is also connected to Internet 105 . LAN 109 may be of any topology. A Universal Description, Discovery and Integration (UDDI) server computer 111 is connected to LAN 109 . UDDI server 111 operates in a manner well known to those skilled in the art; however UDDI server 111 includes additional features according to the present invention that will be described in detail hereinafter. Also, connected to LAN 109 is a performance monitor computer 113 , the operation of which will be described in detail hereinafter. Finally, a performance metric store 115 is connected to LAN 109 . While UDDI server 111 and performance monitor 113 are illustrated as separate machines, it will be recognized that their functions may be implemented as separate processes running on a single machine.
[0019] UDDI server 111 and performance monitor 113 may communicate with each other and with performance metric store over LAN 109 . UDDI server 111 and performance monitor 113 may also communicate with Web service client 103 and Web service providers 107 a - n over Internet 105 .
[0020] Briefly, performance monitor 113 is adapted to collect information from Web service providers and, from the collected information, determine performance attributes. Performance monitor 113 stores the performance attributes in the performance metric store 115 for use by UDDI server 111 . Referring to FIG. 2 , which comprises a flow chart of an implementation of performance monitor processing according to the present invention, performance monitor processing is initialized at block 201 by setting an index n equal to 1. Each Web service provider 107 is assigned an identifier n from 1 to N. The performance monitor requests data from service provider n, at block 203 , according to the interface appropriate for service provider n. The performance monitor receives the data returned from Web service provider n and, at block 205 , determines a performance attribute, or attributes, for Web service provider n. A performance attribute may simply be response time measured from the time of the request to the time of the receipt of the return. Other examples of performance attributes will be apparent to those skilled in the art. For example, a performance attribute may be mean response time over a particular period, maximum response time over the period, standard deviation of response times, or the like.
[0021] After the performance monitor has determined the performance attribute or attributes, the performance monitor enters the performance attribute or attributes determined for Web service provider n in the performance metric store, at block 207 . Typically, the performance monitor overwrites any performance attribute previously stored in performance metric store for Web service provider n. Then, the performance monitor tests, at decision block 209 , if n is equal to N. If not, the performance monitor sets n equal to n plus 1, at block 211 , and processing returns to block 203 . If, as determined at decision block 209 , index n is equal to N, then the performance monitor waits for the next data collection cycle, at block 213 . Data collection cycles may be performed on any time period desired by the system designer. After having waited for the next data collection cycle, performance monitor processing returns to block 201 .
[0022] Referring now to FIG. 3 , there is illustrated a message flow diagram according to one embodiment of a system according to the present invention. Services 301 a , 301 b and 301 n each register with a UDDI registry 303 by sending register messages 305 a , 305 b and 305 n , respectively. The registration of services may occur at any time and in any order. Performance monitoring service 307 requests data from each registered service 301 a , 301 b and 301 n by sending data requests 309 a , 309 b and 309 n , respectively. Services 301 a , 301 b and 301 n respond to the data requests by returning data, as indicated at 311 a , 311 b and 311 n , respectively. As described with respect to FIG. 2 , performance monitoring service 307 determines performance attributes from the data returned from services 301 a , 301 b and 301 n. Performance monitoring service 307 enters the performance attributes in performance metric store 315 , as indicated at 313 .
[0023] A service consumer 317 requests a list of services from UDDI registry 303 , as indicated at 319 , according to the UDDI standard. UDDI registry returns a list of services, as indicated at 321 . Service consumer 317 may request additional attributes for the services listed in the return from UDDI registry 303 , as indicated at 325 . Additional attributes may include attributes registered by services 301 a - n as well as performance attributes determined by performance monitoring service 307 . UDDI registry 303 requests performance attributes from performance metric store 315 , as indicated at 325 . Performance metric store returns performance attributes, at 327 , to UDDI registry 303 . UDDI registry in turn returns additional attributes including the performance attributes to service consumer 317 , as indicated at 329 . Service consumer 317 uses the additional attributes, including the performance attributes, to determine which service 301 a - n to use. After having selected a service, service consumer 317 requests data from selected service 301 a , as indicated at 331 . The service 301 a services the request, as indicated at 333 .
[0024] It should be recognized that the processes illustrated in FIG. 3 are performed at least partially independent of each other. For example, registration of services with UDDI registry, indicated at 305 a - n , occurs essentially once, while performance monitoring service processing, indicated at 309 a - 313 , and service consumer processing, indicated at 319 - 333 , may occur more frequently, but independent of each other.
[0025] Referring now to FIG. 4 , there is illustrated a message flow diagram according to a second embodiment of a system according to the present invention. Services 401 a , 401 b and 401 n each register with a UDDI registry 403 by sending register messages 405 a , 405 b and 405 n , respectively. The registration of services may occur at any time and in any order. Performance monitoring service 407 requests data from each registered service 401 a , 401 b and 401 n by sending data requests 409 a , 409 b and 409 n , respectively. Services 401 a , 401 b and 401 n respond to the data requests by returning date, as indicated at 411 a, 411 b and 411 n, respectively. As described with respect to FIG. 2 , performance monitoring service 407 determines performance attributes from the data returned from services 401 a , 401 b and 401 n. Performance monitoring service 407 enters the performance attributes in performance metric store 415 , as indicated at 413 .
[0026] A service consumer 417 requests a list of services from UDDI registry 403 , as indicated at 419 , according to the UDDI standard. Processing according to FIG. 4 differs from that of FIG. 3 in that UDDI registry 403 , rather than simply returning a list of registered services satisfying request 419 , requests performance attributes from performance metric store 415 , as indicated at 421 . Performance metric store 415 returns performance attributes, at 423 , to UDDI registry 403 . UDDI registry 403 then returns a list of services satisfying the query of service consumer 417 together with additional attributes including the performance attributes, as indicated at 425 . Service consumer 417 then determines which service 401 a - n to use. After having selected a service, service consumer 417 requests data from selected service 401 a , as indicated at 427 . The service 401 a services the request, as indicated at 429 .
[0027] Referring now to FIG. 5 , there is illustrated a block diagram of a generic information handling system 500 capable of performing the server and client operations described herein. Computer system 500 includes processor 501 which is coupled to host bus 503 . Processor 501 preferably includes an onboard cache memory. A level two (L2) cache memory 505 is also coupled to host bus 503 . A Host-to-PCI bridge 507 is coupled to host bus 503 . Host-to-PCI bridge 507 , which is coupled to main memory 509 , includes its own cache memory and main memory control functions. Host-to-PCI bridge 507 provides bus control to handle transfers among a PCI bus 511 , processor 501 , L2 cache 505 , main memory 509 , and host bus 503 . PCI bus 511 provides an interface for a variety of devices including, for example, a local area network (LAN) card 513 , a PCI-to-ISA bridge 515 , which provides bus control to handle transfers between PCI bus 511 and an ISA bus 517 , a universal serial bus (USB) 519 , and an IDE device 521 . PCI-to-ISA bridge 515 also includes onboard power management functionality. PCI-to-ISA bridge 515 can include other functional elements not shown, such as a real-time clock (RTC), DMA control, interrupt support, and system management bus support.
[0028] Peripheral devices and input/output (I/O) devices can be attached to various interfaces or ports coupled to ISA bus 517 . Such interfaces or ports may include a parallel port 523 , a serial port 525 , an infrared (IR) interface 527 , a keyboard interface 529 , a mouse interface 531 , and a hard disk drive (HDD) 533 .
[0029] A BIOS 535 is coupled to ISA bus 517 . BIOS 535 incorporates the necessary processor executable code for a variety of low-level system functions and system boot functions. BIOS 535 can be stored in any computer readable medium, including magnetic storage media, optical storage media, flash memory, random access memory, read only memory, and communications media conveying signals encoding the instructions (e.g., signals from a network). In order to couple computer system 500 to another computer system to copy files or send and receive messages over a network, LAN card 513 may be coupled to PCI bus 511 . Similarly, a Fibre Channel card may be coupled to PCI bus 513 . Additionally, a modem 539 may be coupled to ISA bus 517 through serial port 525 to support dial-up connections.
[0030] While the computer system described in FIG. 5 is capable of executing the invention described herein, the illustrated system is simply one example of a computer system. Those skilled in the art will appreciate that many other computer system designs are capable of performing the invention described herein.
[0031] One of the preferred implementations of the invention is an application, namely, a set of instructions (program code) in a code module that may, for example, be in the random access memory of the computer. Until required by the computer, the set of instructions may be stored in another computer memory, for example, on a hard disk drive, or in removable storage such as an optical disk (for eventual use in a CD ROM) or floppy disk (for eventual use in a floppy disk drive), or downloaded via the Internet or other computer network. Thus, the present invention may be implemented as a computer program product for use in a computer. In addition, although the various methods described are conveniently implemented in a general purpose computer selectively activated or reconfigured by software, one of ordinary skill in the art would also recognize that such methods may be carried out in hardware, in firmware, or in more specialized apparatus constructed to perform the required method steps.
[0032] From the foregoing, it may be seen that processes and systems according to the present invention are well adapted to overcome the shortcomings of the prior art. The processes and systems of the present invention provide performance attributes from a trusted third-party that may be useful to a Web service consumer in selecting a Web service. While the present invention has been illustrated and described with reference to exemplary embodiments, those skilled in the art will recognize alternate embodiments. Accordingly, the foregoing description is intended for purposes of illustration rather than limitation.
|
A method of and system for providing performance information in a Universal Description, Discovery and Integration (UDDI) system periodically requests data from Web service providers that are registered in a UDDI registry. The method and system determine performance attributes for the Web service providers based upon the requested data. The method stores the latest, or most current, performance attributes in a performance metric store that is accessible by the UDDI registry. The UDDI registry services requests from Web service consumers for performance attributes of service providers that provide specified Web services. The UDDI registry accesses the performance metric store to obtain current performance attributes for the Web service providers and returns the performance attributes to the Web service consumer. The Web service consumer can use the performance attributes to select a Web service.
| 7
|
BACKGROUND OF THE INVENTION
The present invention relates to a method of and an apparatus for setting a projectile time fuse.
The method according to the invention is particularly applicable to high-acceleration resistant, high-accuracy, time fuzes, especially electronic-type time fuzes, or enables the use of these fuzes and improves their accuracy.
The projectile fuze's event times are set at appropriate devices prior to firing, e.g., by programming, on the basis of a number of factors such as the distance to the target.
The time fuzes of the hitherto used mechanical-clockwork type have a relatively low setting accuracy on the order of 50 msec. Thus, event time dispersion is very large, particularly as far as high-velocity projectiles are concerned. Because of this, electronic time fuzes which generally achieve a much higher accuracy are preferred.
The most accurate time fuzes at present are based on the use of crystal clocks that serve as time measuring instruments. Because of their special construction, crystal units withstand acceleration loads to a limit extent only. They are destroyed by acceleration loads of 5,000 to 10,000 g, and change their frequency even at lower accelerations. This results in crystal clocks being used in rocket fuzes only, since the maximum rocket acceleration is only a few thousand g. Projectiles fired from guns are subjected to accelerations of 50,000 g and above. Thus, the installation of crystal clocks into projectiles is not possible. This is one of the reasons why the accuracy of standard projectile time fuzes is quite insufficient; the event time dispersion as related to the firing range is generally larger than 1 percent.
SUMMARY OF THE INVENTION:
Hence, an object of the invention is to improve methods and means for setting fuzes. Another object is to create a method and means which can improve the accuracy of the event time.
According to the invention, this is achieved by measuring the muzzle velocity of the projectile and correcting the fuze operating time by applying the measured muzzle velocity to it.
When using this method, the fuze operating time is preferably selected to be directly proportional to the muzzle velocity measured.
On the whole, a variety of ways and means for determining the muzzle velocity are known. Most of these are not suitable for the operating time correction of time fuzes, because they are not accurate enough. German patent document DE-OS 20 23 938 of the applicant discloses a very accurate method of muzzle velocity measurement which can be advantageously applied to the method of the invention.
The invention has the following advantages: By measuring the muzzle velocity and applying it to the correction of the set fuze time, a major source of error is eliminated. If a fixed fuze operating time is set before firing, the distance traveled until initiation of the projectile main charge may vary significantly from round to round, since the muzzle velocity standard deviation is as large as 1% (assuming a constant temperature). The error due to these variations is often added to faulty temperature measurements. This is a source of error which, by the way, could not be eliminated by the use of highly accurate, e.g. crystal-stabilized clocks, since they are highly accurate in setting and measuring a fixed fuze operating time only. When using the measured value in such a way that the fuze operating time is directly proportional to the muzzle velocity of the projectile, all deviations of the muzzle velocity from the mean value (v 0 ) are applied to the fuze operating time and completely compensated for by measuring the projectile velocity at firing.
Measurement of the muzzle velocity inside the projectile is particularly preferred. The main advantage of this method is that no measured values have to be transmitted to the projectile after firing.
An alternative, particularly preferred, embodiment provides measurement of the muzzle velocity at the gun barrel. The main advantage of this method is that costly and sophisticated measuring devices are not lost with the projectile, but can be reused in other projectiles many times.
A particularly preferred embodiment is the measurement of the muzzle velocity with the use of an oscillator the frequency of which is detuned by the projectile flying past a measuring station located inside or in front of the gun tube.
A particularly advantageous measuring method is known from the above-mentioned DE-OS 20 23 938 which should also be referred to with regard to details that are not given in this specification. The measuring method described in DE-OS 20 23 938, though, does not include the installation of the measuring device inside the projectile.
The particularly preferred method of making the correction of the fuze operating time is by wireless radio frequency transmission. In particular, this has the advantage that the measuring basis or components thereof can be located at the gun tube, and that secure transmission is nevertheless guaranteed.
In accordance with a particular aspect of the invention, the radio frequency transmission used for correcting the fuze operating time is also employed for setting the fuze prior to firing. Present methods of programming electronic time fuzes prior to firing use an electric contact between the projectile and the data line of the fire control computer. Data are fed via the firing knob of the electrical primer. However, this well-known method poses great safety problems.
The tansmission of the measured value via an optical relay connection is alternatively preferred. This exhibits the aforementioned advantages of the radio frequency transmission, and is particularly advantageous in cases where radio-frequency interference may occur. In accordance with another aspect of the invention, this method may also be used for the time setting of the fuze prior to firing.
A particularly preferred measuring and correcting apparatus is a bidirectional counter used in combination with an adjustable frequency divider. This apparatus can substantially improve the accuracy of the time fuze, since a complete compensation for all systematic errors in the clock signal generator frequency is achieved. The accuracy of the event time with respect to the firing range can be improved by a power of ten. Then the dispersion is only 1 to 2 per mil of the range.
With the use of the adjustable frequency divider, the fuze can be preset on the basis of the individual characteristics of the short, the target range in particular.
Another advantage of the method and apparatus in accordance with the invention results from the fact that the zero point for time measurement can be fixed exactly because of the projectile passage or movement of the probe relative to the measuring basis. In previous methods using the ignition process of the propelling charge, the statistical variations of the ignition delays resulted in the disperion of the point of initiation. When acceleration switches are used, the different acceleration curve courses as well as the switch tolerances have an effect on that dispersion.
In addition to the above-mentioned, the invention provides an apparatus for setting a projectile time fuze. This apparatus is used in particular for carrying out the method specified in this patent application. The apparatus is cnaracterized by means for measuring the muzzle velocity of the projectile and by a device for correcting the fuze operating time with respect to the muzzle velocity measured. The advantages of such a solution are apparent from the description of the advantages of the corresponding method.
The preferred location of the means for measuring the muzzle velocity inside the projectile. In particular, this has the advantage that no data have to be transmitted to the projectile after firing.
An alternatively preferred embodiment of the apparatus includes the means for measuring the muzzle velocity being located at the gun barrel, at least partially. In particular, this has the advantage that components of the costly measuring device are reusable.
Preferably, the measuring device is fitted with an oscillator which is located such that its frequency is detuned to a large extent by the projectile traveling along the gun tube.
For this purpose, the arrangement known from DE-OS 20 23 938 and further described in the following can be used, the advantages of which have already been stated.
Preferably, the apparatus is equipped with a measuring base or station located inside or in front of the gun barrel. This measuring station detunes the oscillator frequency as the projectile travels along the station. On the basis of the (given, known) length of the measuring station and of the time interval of the signals generated by detuning, the muzzle velocity can be determined and used advantageously for the correction of the fuze operating time.
Preferably, the measuring station is fitted with one or two annular grooves located in the gun barrel wall. These grooves can be easily cut and their spacing from each other or from corresponding edges can be accurately fixed, so that an especially accurate measuring station will be achieved.
Alternatively, a measuring station with one or two annular grooves located in front of the gun barrel, the measuring station preferably being securely connected with the gun barrel. Such a solution has the advantage that no modifications of the gun barrel are required. Furthermore, acceleration is even nearer completion in front of the gun barrel, so that a nearly final velocity value can be determined. The secure but, if required, separable connection ensures that accurate measurements to be obtained at all times.
Preferably, the apparatus comprises a device for wireless transmission of the measured value for correcting the fuze operating time via radio frequency. The advantages of such a device are as stated above. In particular, this device can be used at an early stage for the transmission of data inputs prior to firing.
Preferably, the apparatus comprises a optical relay coupling or optical coupling for the transmission of the measured value. Such a coupling can also be used for the input of data prior to firing, presenting the intrinsic advantages as described at the beginning.
The device being equipped with a bidirectional counter in combination with an adjustable frequency divider is particularly preferred. By use of the bidirectional counter, systematic errors can be avoided, a value in proportion to the muzzle velocity can be recorded reliably and in a way to be easily utilized, and with the use of the adjustable frequency divider, the value pertaining to the respective range can be applied and set without difficulty.
The invention, both as to its construction and its method of operation, will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings, which are referred to in particular with regard to the disclosure.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows the arrangement of the different components, the invention being used with a full bore projectile;
FIG. 2 shows the arrangement of the different components, the invention being used with a subcaliber projectile with sabot;
FIG. 3A and 3B show the relationship between the measuring station shape and the oscillator frequency of the probe, according to the invention;
FIG. 4 shows a block diagram of an electronic fuze with operating time correction achieved by measuring the muzzle velocity;
FIGS. 5A and 5B show two means for setting or programming of the fuze inside the gun tube;
FIGS. 6A and 6B show two means for setting or programming of the fuze and operating time correction along the projectile trajectory.
FIGS. 7, 8, and 9 illustrate further embodiments of the invention using removable measuring stations.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
In FIG. 1 and 2, a projectile 1 is illustrated in its passage from its initial position (at the far left of that shown and) in the breech of a gun barrel 2, to the muzzle at the right end of the barrel 2. A measuring station is composed of two annular grooves 5 spaced a distance D on the inner wall of a gun barrel 2. According to an embodiment of the invention the measuring station is composed of a simple annular groove and the gun muzzle. According to yet another embodiment of the invention an additional measuring station is located in front of the muzzle gun barrel.
A probe 3, 4 is located inside the projectile or barrel in this case. The probe 3, 4 includes a coil 3 of an RF oscillator 4. The coil 3 is located directly at the interface of gun barrel and case of the projectile. The oscillator 4, together with the coil 3, is installed into an adapter housing which is screwed into a cavity in the case of the projectile. According to another embodiment of the invention the adapter housing is located inside the gun barrel. The frequency of the oscillator 4 varies (see FIG. 3) depending on whether there is metal above the upper side of the coil or not. The absolute frequency value of the oscillator can be freely selected. If there is a metal surface above the coil, the oscillator frequency is higher than it is in the air or with a plastic surface above the coil. The adaptor housing also includes a control circuit 6 and a power source 7.
At firing, the probe which is located inside the projectile moves past grooves 5 of the measuring station in the gun barrel. During passages of the groove edges, the oscillator circuit frequency changes. This frequency change is within the range of 40 to 50 MHz for the experimental models tested. As shown in FIG. 4, the oscillator 4 supplies its RF output signal to the circuit 6. In the circuit 6, the RF signal is fed to a narrow band receiver 8 (Δf=1 MHz) whose receiving frequency f E is adjusted to a value between the two extremes (FIGS. 3A and 3B). Because of the narrow band width, the projectile position is determined with great accuracy. FIG. 3A shows the coil 3 passing the grooves 5. FIG. 3B shows the frequency changes resulting from the effect of the grooves 5 on the coil 3 and oscillation 4 as the coil 3 progresses in the direction x. The receiver 8 is turned to the frequency 220 MHz as the frequency of oscillation 4 varies from 250 MHz to 200 MHz and back.
A frequency change such as 40 MHz applies to a distance of 4 mm for the embodiments tested. For a receiver band width of Δf=1 MHz, this results in a local resolution of ΔD=4 mm/40=0.1 mm. For a measuring station lens of D>10 cm, the resolution is ΔD/D<1 per mil. The output side of the receiver is fitted with a rectifier generating pulses at those instants when the probe passes the edge of a groove.
The projectile velocity can be determined from the intervals between the individual pulses.
As shown in FIG. 4, the pulses are used for the fuze operating time correction as follows:
The first pulse generated by the receiver on a line 15 at the beginning of the measuring station starts count-up in a bidirectional counter 9. A clock signal generator 10 with a very high frequency f c provides pulses to the counter a which counts approximately 1,000 pulses during count-up. As soon as the probe 3, 4 passes the end of the measuring station (second groove 5 or the muzzle), a stop pulse that ends the count-up is generated. Control logic 11 now uses the line 18 to set the counter to countdown, and at the same time, a divided frequency fd is fed to the counter 9 by an electronic switch 14. The divided frequency fd required for countdown is generated by an adjustable, e.g., programmable frequency divider 12 with a division ratio depending upon the time of flight (and, thus, upon the range). At zero count, a fuze firing pulse is generated. This is accomplished by the control logic 11 using a line 20 to cause a detector 13 to interrogate the condition of the counter 9 via a line 21, and to produce the firing pulse on a line 22 when the count is zero.
Example: The counter is assumed to have counter 1,000 pulses in countup.
Frequency for countdown: ν=1,000 Hz.
Hence, the counter "zero" is reached after 1 sec.
This method has the following effects and advantages:
At a constant frequency of the clock signal generator during projectile flight, there is a linear relationship between the event time and the time of projectile passage along the measuring station.
At a lower projectile velocity, more pulses are counted, so that the time required for the countdown to zero is prolonged. This is the next compensation for the projectile time of flight prolongation at lower muzzle velocities. For higher projectile velocities, the time until initiation of the projectile charge is shortened accordingly.
The frequency divider is set, e.g. programmed, by the fire control computer. The division ratio N results from the mean time of flight of the projectile at the respective range (=initiation range) as follows: ##EQU1## where
x=firing range;
T F =(mean) time of projectile flight;
n=number of pulses in counter at mean MV (v 0 );
ν=countdown frequency;
f c =undivided frequency of clock signal generator (count-up frequency);
N=division ratio.
Because of the 1,000 pulse counted in count-up, the inaccuracy of the event time with respect to the firing range is within 1 to 2 per mil only.
The accuracy of the method is dependent mainly upon the number of clock pulses counted in count-up. The larger their number n, the greater the accuracy of the fuze. The number n is dependent upon the length D of the measuring station and the frequency f c .
The stability requirements for the clock signal generator frequency are only minor and easy to meet. During projectile flight only, the clock signal generator frequency has to meet the stability requirement give by: ##EQU2##
The frequency f c can vary largely (several per cent) from projectile to projectile without any influence on the accuracy of the fuze.
Frequency changes due to temperature are also of minor importance, as long as the temperature in the vicinity of the clock signal generator inside the fuze remains constant from the time the projectile leaves the muzzle to the time of initiation.
Slightly modified, the method and the apparatus can be used with the same electronic fuze, the MV probe being located at the gun tube instead of inside the projectile, and the projectile being used as the measuring basis.
In this case, the measured value has to be transmitted to the projectile via a wireless radio or an optronic data transmission line.
The setting or programming of the frequency divider located inside the projectile can be carried out in one of the following ways.
1. Prior to firing, via a cable led through the breech and the cartridge case (known method);
2. prior to firing, by induction, with the use of RF directly transmitted to the projectile, with the MV probe inside the projectile being used as a receiving sytem as in FIG. 5A; this involves grooves 24 in the projectile;
3. prior to firing, optically via a fiber optic cable 30 located in a hole in the gun tube wall, with the projectile being equipped with an optical receiving system 25 (FIG. 5B);
4. after firing, on the trajectory via radio with an antenna 26 as in FIG. 6A;
5. after firing, on the trajectory via an optronic transceiver system (FIG. 6B) using a pulser 27 with the beam 28 being collected by an optical receiving system 29 located inside the projectile 1.
FIG. 7 illustrates a measuring station 71 screwed to the end of the gun barrel 2. Here, as in FIG. 1, grooves 75 corresponding to the grooves 5 of FIG. 1 produce changes in the oscillator frequency. These changes are processed the same manner as in FIG. 1. The station 71 is removable after wear has made it unusable and replaceable with another station 71.
According to another embodiment of the invention, the muzzle velocity is measured by the device shown in FIG. 8 which corresponds to that in the aforementioned German patent specification DE-OS 20 23 938. Here, the muzzle of a gun barrel 81 has a metal sleeve 82 mounted thereon such as by means of threads. An insulated circular carrier 83 mounted on the sleeve holds a metallic ring 84. A conductor 85 connects the metallic ring to a transistor oscillator 86. A battery 87 which may be 6 volts or 12 volts energizes the oscillator.
The projectile 88 shown by dotted lines and passing through the metal ring produces changes in a receiver (not shown) connected to the oscillator 86.
In the example shown the oscillator 86 has an oscillator circuit inductance that produces a frequency stabilized oscillation of approximately 110 mHz. When the projectile emerges from the muzzle and passes through the ring 84, the projectile is coupled to the ring and raises the frequency of the oscillator. The magnitude of the frequency change depends upon the diameter ratio of the ring 84 and projectile 88.
The passage of the projectile through the slit ring 84 produces a change in frequency and amplitude which can be used to determine the muzzle velocity of the projectile. Further details are available from the aforementioned German Patent Publication DE-OS 20 23938.
In FIG. 4 the programmable divider 12 is programmed in bit parallel fashion by a 16 bit word. This 16 bit word is transferred to the divider by a 16 bit shift register. The shift register is set with a 16 bit word by the fire control system via a programming interface.
The control orders for the counter 9 and the switch 14 in FIG. 4, such as count-up pulses along line 18 and switch control line 19, are derived from measuring pulses 15 within the control logic 11.
While embodiments of the invention have been described in detail it will be evident to those skilled in the art that the invention may be embodied otherwise without departing from its spirit and scope.
|
Disclosed is a high-acceleration resistant, programmable, electronic time fuze and a method of an apparatus for the correction of the operating time of this time fuze by muzzle velocity measurement carried out inside the projectile or at the gun tube. The time fuze uses the muzzle velocity measured at firing to adjust its operating time. Thus, range dispersion of the event time is substantially reduced. The muzzle velocity is measured with a metal sensitive probe installed inside the projectile. When the probe passes annular grooves in the gun wall, an oscillator is detuned and generates pulses for determination of the projectile muzzle velocity. A bidirectional counter responds to the pulses in one direction, to other information in the other direction and sets off the fuze at a predetermined count such as zero.
| 5
|
FIELD OF THE INVENTION
[0001] The present invention relates to various treatments of textiles, more particularly to plasma-treatments of textiles, and even more particularly to a plasma-treatment method for obtaining multifunctional technical textiles.
BACKGROUND OF THE INVENTION
[0002] Technical textiles are a specialized textile product used primarily for their function rather than for their aesthetic purposes. Some of the functions of the technical textiles are EMI shielding, water-proofing, fire and flame resistance, antistatic function, antimicrobial function, fire-resistance, and anti-odor function. The clothing made from the technical textiles is commonly referred to as protective clothing, which is used for various applications. For example, the protective clothing with an antistatic property or characteristic is used by the operators of a gas station, firefighters, and the like, as such clothing prevents the accumulation of electric charges on the surface thereof. Protective clothing with antimicrobial function is another product of technical textiles which helps in preventing the cross-transmission of infectious diseases, and is therefore used in hospitals, medical laboratories, and so on. Yet another example would be fire-resistant clothing typically worn by firefighters while performing firefighting operations.
[0003] In spite of various types of protective clothing known in the prior art, there's still a need for technical textiles that exhibit more than one function. For example, a protective clothing used in medical facilities might need to be water-proof while being anti-microbial. Similarly, another example would be a sportswear which needs to have an anti-odor function while exhibiting an anti-UV property. Several attempts have been made in the art to address the need for multifunctional technical textiles, however, the multifunctional textiles made out of these attempts comprises more than one layer of cloth and is therefore bulky and heavy causing inconvenience to the wearer. Therefore, there exists a need for a multifunctional technical textile which is light and single or uni-layered.
[0004] Further, the technical textiles are typically manufactured by a multi-stage wet process which consumes a lot of time. And on top of that, these wet processes are not eco-friendly as they produce a lot of wastewater which is hazardous to the environment. Hence, it is desirable to manufacture light, single-layered, multifunctional technical textiles from a dry, quick, eco-friendly method.
SUMMARY OF THE INVENTION
[0005] It is a primary object of the present invention to provide a method of treatment of textiles in order to obtain light, single-layered multifunctional technical textiles.
[0006] It is another object of the present invention to provide such a method of treatment which is dry and eco-friendly.
[0007] It is yet another object of the present invention to provide such a method of treatment which is a single-stage process.
[0008] It is still yet another objective of the present invention to provide such a method of treatment which is less time-consuming compared to conventional methods that are employed for obtaining technical textiles.
[0009] It should also be understood that many other advantages and alternatives for practicing the invention will become apparent from the following detailed description of the preferred embodiments and the appended drawings.
BRIEF DESCRIPTIONS OF THE DRAWINGS
[0010] FIG. 1 is an illustration of the reaction chamber employed for low-pressure plasma treatment of the textile product in accordance with the present invention.
[0011] FIG. 2 is an illustration of the reaction chamber employed for atmospheric-pressure plasma treatment of the textile product in accordance with the present invention.
FIGURES—REFERENCE NUMERALS
[0000]
10 . . . Reaction Chamber for Low-Pressure Plasma Treatment
12 . . . Anode
14 . . . Cathode
16 . . . Guide Roll
18 . . . Reaction Chamber for Atmospheric-Pressure Plasma Treatment
20 . . . Electrode
22 . . . Trolley
24 . . . Textile Product
26 . . . Precursor Material
DETAILED DESCRIPTION OF THE INVENTION
[0021] The present invention is a method of treatment of textiles with plasma for obtaining multifunctional technical textiles. The method of plasma-treatment of the present invention is clean, dry and eco-friendly as it doesn't involve treatment with chemicals, liquids including water. Also, the plasma-treatment method is a single-stage method and is therefore less time-consuming compared to the treatments directed to the same end as the plasma-treatment method of the present invention. In fact, the time required for the completion of the method of plasma-treatment of the present invention does not exceed five minutes. The final product of the plasma-treatment method is a multifunctional textile is a technical textile that is single-layered and exhibits more than one property or characteristic. Multifunctional textile so obtained, similar to a conventional technical textile, is used in various fields of application. For example, the multifunctional textile can be used as a medical textile as the multifunctional textile is both water-proof and antimicrobial. Similarly, the multifunctional textile can be used as a sportswear as exhibits both odor-free and anti-UV characteristics.
[0022] Prior to the initiation of the plasma-treatment method of the present invention, a textile product is washed in a solution comprising water mixed with non-ionic detergent water following the ratio of 1 gram per liter of water. More particularly, the textile product is washed at 40° C. for 10 minutes. Once washed, the textile product is stored at 20° C. and at 65% relative humidity. The textile product, such as a cloth, may be woven, knitted, non-woven, and so on.
[0023] The plasma used for the present invention can pertain to inert gases, particularly argon, or to reactive gases such as oxygen, nitrogen or nitrogen containing polymeric gases, and so on, with nitrogen plasma being preferable. Both low-pressure and atmospheric pressure plasma discharges can be used for the plasma-treatment. It is to be noted that the gases used for the plasma-treatment are pure grade.
[0024] Referring to FIG. 1 , for the low-pressure plasma treatment, a cylindrical reaction chamber 10 made of glass is employed for generating the low-pressure plasma from a gas. A rotary pump is employed for evacuating the reaction chamber 10 before filling up the same with a gas from which plasma is generated. The gas within the reaction chamber 10 , which is preferably nitrogen, is maintained at a pressure of 10 −2 Torr. The reaction chamber 10 further comprises a pair of electrodes, viz., an anode 12 and a cathode 14 wherein, when the electrodes are powered, a glow discharge is radially produced between the same. The gas between the electrodes is subjected to electromagnetic force resulting in the generation of plasma. An axial magnetic field formed within the reaction chamber 10 ensures uniform distribution of the plasma medium. The textile product 24 is placed on the anode 12 so as to be exposed to the plasma. In one embodiment, the reaction chamber 10 comprises a plurality of guide rolls 16 whereon the textile product 24 is transported in and out of the reaction chamber 10 . The surface of the textile product 24 reacts with the plasma so as become a multifunctional textile.
[0025] In one embodiment, argon plasma is used in the reaction chamber instead of nitrogen plasma. In this case, metallic particles are attached to the surface electrodes, whereby, upon the initiation of the plasma-treatment, the metallic particles are sputtered over the surface of the textile product forming a nano-layer of the metallic particles thereon. The antimicrobial property of the multifunctional textile is substantially increased with the deposition of metallic particles. The thickness of the nano-layer of the metallic nanoparticles depends on the electrodes, their shape and size, voltage supplied to the electrodes, and so on. In another embodiment, copper, silver, gold, and titanium are used as electrodes, which also enhance the antimicrobial properties of the multifunctional textile.
[0026] Referring to FIG. 2 , the reaction chamber 18 comprises a high power supply unit when atmospheric-pressure plasma is used in for the plasma-treatment of the textile product 24 . The reaction chamber 18 is set to operate at 300 W. The electrodes 20 employed within the reaction chamber 18 are made of ceramic containing aluminum oxide (Al 2 O 3 ) essentially. An alternating current of 20 kV is supplied to the electrodes 20 , as a result of which, a substantial amount of heat is generated by the electrodes 20 during the course of the plasma-treatment. An oil circulation system operated by a pump is employed for cooling the electrodes 20 at regular intervals in order to help prevent the same from overheating.
[0027] The distance between the electrodes 20 is adjustable within a range of 0.5 to 2.5 mm. Nitrogen is preferable although air and other gases including oxygen, argon can also be used for generating plasma. The reaction chamber 18 further comprises a trolley 22 whereon the textile product 24 is placed for uniform plasma exposure. More particularly, a vacuum sucker is employed for holding the textile product 24 in place as the trolley 22 imparts linear movement to the textile product. In one embodiment, a plurality of guide rolls is employed instead of the trolley 22 for transporting the textile product through the reaction chamber 18 .
[0028] Apart from the plasma produced from the ceramic electrodes 20 , a precursor material 26 is discharged into the plasma medium. The state of matter of the precursor material 26 may be liquid or powered. The precursor material 26 is atomized as the same is released into the plasma thereby enabling precursor material 26 to uniformly mix with the plasma.
[0029] N—H groups are formed over the surface of the textile product as the same is subjected nitrogen plasma mixed with the precursor material. The N—H functional groups cause the textile product exhibit antimicrobial property, anti-creasing property, anti-soiling property, UV protective property, and so on. The Limited Oxygen Index (LOI) of the finished multifunctional textile is substantially more than that of the textile product and hence, the multifunctional textile is highly fire and flame-retardant. Also, the UV Protection Factor (UPF) of the finished multifunctional textile is nearly 2000 thus making it highly protective against UV radiation. The multifunctional textile can be used for filtering metals from wastewater. Compared to the input textile product, the dyeability of the finished multifunctional textile is substantially higher.
[0030] In both the cases of low-pressure plasma and atmospheric pressure plasma, the time of exposure of the plasma is not more than 5 minutes. However, the exposure time may vary depending on the plasma, the purity of gas, the textile product and its shape, and so on. The finished multifunctional textiles are antimicrobial, wrinkle-free, breathable, fire and flame-resistant, water-proof, UV-protective, dyeable, EMI shielding, oil repellant, and so on. The multifunctional textile exhibits anti-soiling function when the surface thereof is added with a layer of titanium oxide nanoparticles.
[0031] The foregoing description of the specific embodiments will so fully reveal the general nature of the embodiments herein that others can, by applying current knowledge, readily modify and/or adapt for various applications such specific embodiments without departing from the generic concept, and, therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments herein have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the appended claims.
[0032] Although the embodiments herein are described with various specific embodiments, it will be obvious for a person skilled in the art to practice the invention with modifications. However, all such modifications are deemed to be within the scope of the claims.
[0033] It is also to be understood that the following claims are intended to cover all of the generic and specific features of the embodiments described herein and all the statements of the scope of the embodiments which as a matter of language might be said to fall therebetween.
|
Disclosed is a method for preparing a multifunctional technical textile that exhibits multiple functional properties comprising flame or fire-retardancy, EMI shielding, anti-odorous property, UV protection, oil-repellency, anti-soiling property, antimicrobial property, anti-creasing property, water-proof, and antistatic property. The method comprises washing a textile product in a water solution comprising water mixed with a predetermined quantity of non-ionic detergent, storing the textile product at a predetermined temperature and a predetermined relative humidity, and subjecting the textile product to plasma treatment by placing the same in a plasma stream within a reaction chamber.
| 3
|
BACKGROUND
[0001] 1. Field of the Invention
[0002] This invention is related to the field of integrated circuits and, more particularly, to detection of power on reset in an integrated circuit.
[0003] 2. Description of the Related Art
[0004] Integrated circuits continue to increase in complexity and the number of high level component functions that are included in the integrated circuit also continues to increase. The system on a chip (SOC) is an example of the high level of integration, including one or more processors and various peripheral components, memory controllers, peripheral interface controllers, etc. on a single integrated circuit “chip.” To ensure that the integrated circuits have been manufactured correctly, and to support debugging of hardware and software (which is complicated by the high level of integration), the integrated circuits typically support test modes in addition to the normal functional operation mode. The test modes may permit state to be scanned into and out of the integrated circuit.
[0005] The highly integrated circuits, such as SOCs, may be used in various devices that carry a user's personal data. For example, the integrated circuits may be used in smart phones, personal digital assistants, and other computing devices that a user may incorporate into his/her daily life and thus may carry significant amounts of personal data such as account numbers, passwords, and other personally-identifiable information. Similarly, such devices are increasingly being expected to maintain the digital rights of intellectual property owners (e.g. owners of audio and video data that a user is permitted to enjoy but is not permitted to copy or redistribute). Accordingly, the integrated circuits need to be secure for such data. Integrated circuits that can switch between test mode and normal functional mode may have potential insecurity (or may have a so-called “security hole”) if data from the functional mode is accessible in test mode or vice-versa.
SUMMARY
[0006] In an embodiment, an integrated circuit such may require that a full reset of the integrated circuit occur before the integrated circuit enters either a test mode or a functional mode. The integrated circuit may include a reset detector to detect that the reset has occurred, and the integrated circuit may not transition to the test mode or the functional mode unless the reset detector detects that the reset has occurred. Accordingly, if test mode is being entered, any user data or other private data that may have been stored in the integrated circuit during a preceding functional mode may have been cleared via the reset. Similarly, if functional mode is being entered, any test data that may have been stored in the integrated circuit in a preceding test mode may have been cleared via the reset. The reset may be referred to as a “power on reset,” or POR, because the reset may ensure a clean, empty state of the integrated circuit similar to a state that might be generated by resetting the integrated circuit at the time of power on.
[0007] In one embodiment, the reset detector may include a set of flops that are reset to a known state. If the reset has not occurred, the flops may have a random state that they acquired at power up. The random state may have a low probability of matching the known state. For example, if there are N flops (N is an integer), the probability that the random state matches the known state may be 1 in at least 2 N .
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The following detailed description makes reference to the accompanying drawings, which are now briefly described.
[0009] FIG. 1 is a block diagram of one embodiment of an integrated circuit.
[0010] FIG. 2 is a block diagram of one embodiment of a reset detector.
[0011] FIG. 3 is a block diagram of another embodiment of a reset detector.
[0012] FIG. 4 is a block diagram of one embodiment of a state machine for an initialization control unit shown in FIG. 1 .
[0013] FIG. 5 is a block diagram of one embodiment of a system including the integrated circuit of FIG. 1 .
[0014] While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that the drawings and detailed description thereto are not intended to limit the invention to the particular form disclosed, but on the contrary, the intention is to cover all modifications, equivalents and alternatives falling within the spirit and scope of the present invention as defined by the appended claims. The headings used herein are for organizational purposes only and are not meant to be used to limit the scope of the description. As used throughout this application, the word “may” is used in a permissive sense (i.e., meaning having the potential to), rather than the mandatory sense (i.e., meaning must). Similarly, the words “include”, “including”, and “includes” mean including, but not limited to.
[0015] Various units, circuits, or other components may be described as “configured to” perform a task or tasks. In such contexts, “configured to” is a broad recitation of structure generally meaning “having circuitry that” performs the task or tasks during operation. As such, the unit/circuit/component can be configured to perform the task even when the unit/circuit/component is not currently on. In general, the circuitry that forms the structure corresponding to “configured to” may include hardware circuits that implement the operation. Similarly, various units/circuits/components may be described as performing a task or tasks, for convenience in the description. Such descriptions should be interpreted as including the phrase “configured to.” Reciting a unit/circuit/component that is configured to perform one or more tasks is expressly intended not to invoke 35 U.S.C. §112, paragraph six interpretation for that unit/circuit/component.
DETAILED DESCRIPTION OF EMBODIMENTS
[0016] Turning now to FIG. 1 , a block diagram of one embodiment of an integrated circuit (IC) 10 is shown. In the illustrated embodiment, the IC 10 includes one or more component blocks 12 A- 12 B, an initialization control circuit 14 , and a set of fuses 18 . The component blocks 12 A- 12 B may include various clocked storage devices 16 A- 16 B (e.g. registers, flops, latches, etc.), some of which may store user state corresponding to a user of a system that includes the IC 10 (or other private state, such as unencrypted video, keys for video, keys for other encryption, etc.). The clocked storage devices 16 A- 16 B may be coupled to receive a reset input to the IC 10 . The initialization control circuit 14 may include a POR detect circuit 20 that is coupled to receive the reset input as well. The initialization control circuit 14 is coupled to the fuses 18 and a test port input to the IC 10 .
[0017] As mentioned above, various storage devices 16 A- 16 B may store user state or other private state during normal functional operation. To prevent such state from being available in test mode, which may permit the user/private state to be scanned out of the IC 10 or to otherwise be accessed from the IC 10 , potentially for nefarious purposes, the initialization control circuit 14 may prevent entry into test mode unless a reset has been detected by the POR detector 20 . Similarly, in an embodiment, the initialization control circuit 14 may prevent entry into normal functional mode (i.e. non-test) mode unless a reset has been detected by the POR detector 20 . Generally, a test mode may be a mode in which the state of the IC 10 is accessible to a test controller (e.g. via the test port on the IC 10 ). The state may be scanned out for analysis, or scanned in to test the circuitry in the IC 10 . The test port may be any type of test connection (e.g. the test port may be compatible with the joint test access group (JTAG) specification, Institute of Electrical and Electronic Engineers (IEEE) 1149.1 and follow-ons, or any other test port specification). The normal functional mode (or simply functional mode) may be a mode in which the IC 10 operates within the system to perform the operations that the system is designed for (e.g. computing, communication, etc.).
[0018] The POR detector 20 may include circuitry to detect that the reset has been performed. For example, in one embodiment, the POR detector 20 may include multiple storage devices that are coupled to the reset input. Each storage device may have a predefined reset state that the storage device acquires in response to assertion of the reset. Some of the storage devices may reset to a binary one, and others may reset to a binary zero. If IC 10 is powered up and the reset is not asserted, the storage devices may acquire a random state of either one or zero. Accordingly, by examining the state of the storage devices, the POR detector 20 may determine (which reasonable accuracy) whether or not a reset has been performed. For example, if there are N storage devices (where N is a positive integer) and if the storage devices are equally likely to have a one or a zero state in response to no reset, the odds of each storage device having the predefined state (and thus detecting a reset when no reset has occurred) is 1 in 2 N . The probability may be further improved by altering the design of the storage devices so that the “non-reset” state is more likely to occur than the predefined reset state if the reset is not asserted. For example, if cross coupled inverters are used to form the storage device, the N-type metal-oxide-semiconductor (NMOS) transistor in one inverter and the P-type MOS (PMOS) transistor in the other inverter may be made larger than the remaining two transistors to make it likely that a binary one will appear on the output of the inverter having the larger PMOS transistor. The predefined reset state may include having a binary zero on the output of that inverter. In such a case, the probability of N storage devices having states that indicate a reset when no reset has occurred may be less probable than 1 in 2 N .
[0019] The initialization control circuit 14 may be coupled to the fuses 18 . The fuses 18 may be selectively blown at manufacture of the IC 10 , to provide some instance-specific values (e.g. a private key or keys for the instance, a serial number or other instance identifier, permissible voltage and/or frequency combinations based on characterization testing, etc.). A fuse may also be used to indicate whether or not entry into test mode is permitted. That is, the fuse may have a first state (e.g. corresponding to a binary one) indicating that entry into the test mode is permitted and a second state different from the first state (e.g. corresponding to a binary zero) indicating that entry into the test mode is not permitted. The initialization control circuit 14 may be configured to read the fuses in response to detection of a reset by the POR detector 20 , and may initialize various state within the IC 10 based on the fuses.
[0020] The component blocks 12 A- 12 B may implement the operations for which the IC 10 is designed. For example, if the IC 10 includes processors, one or more of the component blocks 12 A- 12 B may be processors. In an SOC implementation, one or more component blocks 12 A- 12 B may include one or more memory controllers to communicate with a memory system (e.g. one or more dynamic random access memories). An SOC implementation may further include peripheral components such as audio and/or video processing components, graphics processing components, image processing components, networking components, peripheral interface controllers such as universal serial bus (USB), peripheral component interconnect (PCI), PCI express (PCIe), parallel or serial ports, universal asynchronous receiver/transceiver (UARTs), etc.
[0021] The test port and the reset input may be external inputs to the IC 10 . That is, the test port may be connected to one or more pins on the package of the IC 10 , which may be electrically connected to pads on the IC 10 itself. Similarly, the reset input may be received on an input pin of the package. In some cases, an internal reset may be supported (e.g. via a register written by software to cause a reset). The internal reset and the external reset may be logically combined to form the reset input to the POR detector 20 and the storage devices 16 A- 16 B. Alternatively, the internal reset may be treated differently than the external reset (e.g. it may be a “soft” reset that resets selected storage devices).
[0022] FIG. 2 is a block diagram of one embodiment of the POR detect unit 20 is shown. In the illustrated embodiment, the POR detect unit 20 includes a set of flops including flops 30 A- 30 D coupled to a decoder circuit 32 . The decoder circuit 32 is configured to output a reset detected signal, and the flops 30 A- 30 D are coupled to receive the reset signal on reset ports of the flops 30 A- 30 D.
[0023] The flops 30 A- 30 D may be representative of a set of flops that may be included in the POR detect circuit 20 . There may be more flops than the flops 30 A- 30 D. For example, a set of 32, 64, or 128 flops may be used. Some of the flops are reset to zero (e.g. the flops 30 A- 30 B) and others are reset to one (e.g. the flops 30 C- 30 D). In an embodiment, half of the flops may be reset to zero and the remaining half may be reset to one.
[0024] The decoder circuit 32 may be coupled to receive the state of each flop, and may be configured to decode the state based on the predefined reset state. For example, the decoder circuit 32 may logically NOR the states of the flops 30 A- 30 B that are reset to zero, logically AND the states of the flops 30 C- 30 D that are reset to one, and logically AND the result to generate the reset detected signal. Any Boolean equivalent of the above logic may be implemented in various embodiments of the decoder circuit 32 .
[0025] Viewed in another way, the expected reset states of the flops 30 A- 30 D may be viewed as a multibit value, and the decoder circuit 32 may decode the multibit value to generate the reset detected signal. In general, the decoder circuit 32 may be a control circuit configured to assert the reset detected signal responsive to the predetermined reset state appearing in the flops 30 A- 30 D.
[0026] In the embodiment of FIG. 2 , the flops 30 A- 30 D may be D-type flops. D-flops have a data input (D), and capture the data input responsive to a clock input. The data input is output from the flop as well (Q). In the embodiment of FIG. 2 , some of the D-flops are reset to zero flops (e.g. the flops 30 A- 30 B), which are designed to reset to a binary zero on the Q output responsive to the assertion of the reset. Similarly, other D-flops are reset to one flops (e.g. the flops 30 C- 30 D), which are designed to reset to a binary one on the Q output responsive to the assertion of the reset. The flops 30 A- 30 D have a reset port (R) coupled to the reset input and the flops are configured to reset to zero or one (as appropriate) in response to assertion of the reset on the reset input.
[0027] In the embodiment of FIG. 2 , the clock input to the flops 30 A- 30 D is tied to a constant value. The constant value may be selected to ensure that the flops 30 A- 30 D do not capture the D input, since the flops 30 A- 30 D are provided to detect the reset. In the illustrated embodiment, the clock input is tied to zero. The D flops 30 A- 30 D may be rising edge-triggered flops, for example, and a clock input of zero prevents a rising edge.
[0028] Additionally in FIG. 2 , the D inputs of the flops 30 A- 30 D are illustrated as being tied to a constant that is the opposite of the reset state. That is, the reset to zero flops 30 A- 30 B have the D inputs tied to one, and the reset to one flops 30 C- 30 D have their D inputs tied to zero. In this fashion, if the D inputs have some effect on the flops 30 A- 30 D, the effect may be to change the state to the opposite (or logical complement) of the reset state.
[0029] FIG. 3 is a block diagram illustrating another embodiment of the POR detector 20 . The embodiment of FIG. 3 includes the decoder 32 and a set of set-reset (S-R) flops 40 A- 40 D in place of the flops 30 A- 30 D. The flops 40 A- 40 D may be representative of a set of flops that may be included in the POR detect circuit 20 . There may be more flops than the flops 40 A- 40 D. For example, a set of 32, 64, or 128 flops may be used. Some of the flops have a set port (S) coupled to receive the reset input (e.g. the flops 40 C- 40 D), while others have a reset port (R) coupled to receive the reset input (e.g. the flops 40 A- 40 B). Flops having the set port coupled to receive the reset input are set (binary one) on their Q outputs in response to an assertion of reset. Flops having the reset port coupled to receive the reset input are reset (binary zero) on their Q outputs in response to an assertion of reset. In an embodiment, half of the S-R flops 40 A- 40 D may have the reset input coupled to the set port of the flops, and the other half of the S-R flops 40 A- 40 D may have the reset port coupled to the reset input.
[0030] The embodiments of FIGS. 2 and 3 are merely examples. Other embodiments may use any type of flop or any type of storage device for the POR detector 20 .
[0031] FIG. 4 is a state machine that may be implemented by one embodiment of the initialization control circuit 14 . Generally, the state machine may remain in a particular state unless the conditions for a state transition from that state to another state (as shown in FIG. 4 ) are met. In the illustrated embodiment, the state machine includes a reset state 50 , a fuse state 52 , a test mode state 54 , and a normal functional mode state 56 .
[0032] In response to a reset assertion while in any state (e.g. the test mode state 54 , the normal functional mode state 56 , the fuse state 52 , or any other state), the state machine transitions to the reset state 50 . The state machine may remain in the reset state 50 until the reset is deasserted and the reset detected output from the POR detector 20 is asserted. The state machine may then transition to the fuse state 52 , during which the initialization control circuit 14 may be configured to read the fuses 18 . Reading the fuses may include reading private or secure state, such as instance-specific keys or other values. Accordingly, preventing entry into the fuse state 62 may prevent reading of private or secure data until a POR has been detected. Once the fuse read (and corresponding initialization in the IC 10 ) is complete, the state machine may transition from the fuse state 52 to one of the test mode state 54 or the normal (functional) mode state 56 . In the test mode state 54 , test access to the component blocks 12 A- 12 B may be permitted from the test port. In the normal functional mode state 56 , test access is not permitted and the IC 10 (component blocks 12 A- 12 B) operates in functional mode. The state machine may transition to the test mode state 54 from the fuse state 52 if the fuse read is complete and the test mode is selected. The test mode selection may be controlled by requests from the test port and/or from a fuse that indicates whether test mode entry is permitted. That is, test mode may be selected, e.g., if the fuse is in the first state and communication on the test port has been received requesting test mode. The normal functional mode may be selected, e.g., if the fuse is in the second state or no communication on the test port has been received requesting the test mode. If test mode is not selected and the fuse read is complete, the state machine may transition to the normal mode state 56 from the fuse state 52 .
[0033] As can be seen in FIG. 4 , once the test mode state 54 has been entered, it is not possible to enter the normal functional mode state 56 without detection of at least one reset by the POR circuit 20 since the integrated circuit 10 has been powered up. Similarly, once the normal functional mode 56 has been entered, it is not possible to enter the test mode state 54 without detection of at least one reset by the POR circuit 20 since the integrated circuit 10 has been powered up. Even though the reset state 50 is entered in response to assertion of reset, exiting the reset state 50 includes detecting that the reset has occurred (i.e. that the reset remained asserted long enough to actually reset the storage devices).
[0034] Turning now to FIG. 5 , a block diagram of one embodiment of a system 150 is shown. In the illustrated embodiment, the system 150 includes at least one instance of the integrated circuit 10 (from FIG. 1 ) coupled to one or more peripherals 154 and an external memory 158 . A power supply 156 is also provided which supplies the supply voltages to the integrated circuit 10 as well as one or more supply voltages to the memory 158 and/or the peripherals 154 . In some embodiments, more than one instance of the integrated circuit 10 may be included (and more than one external memory 158 may be included as well).
[0035] The peripherals 154 may include any desired circuitry, depending on the type of system 150 . For example, in one embodiment, the system 150 may be a mobile device (e.g. personal digital assistant (PDA), smart phone, etc.) and the peripherals 154 may include devices for various types of wireless communication, such as wifi, Bluetooth, cellular, global positioning system, etc. The peripherals 154 may also include additional storage, including RAM storage, solid state storage, or disk storage. The peripherals 154 may include user interface devices such as a display screen, including touch display screens or multitouch display screens, keyboard or other input devices, microphones, speakers, etc. In other embodiments, the system 150 may be any type of computing system (e.g. desktop personal computer, laptop, workstation, net top etc.).
[0036] The external memory 158 may include any type of memory. For example, the external memory 158 may be SRAM, dynamic RAM (DRAM) such as synchronous DRAM (SDRAM), double data rate (DDR, DDR2, DDR3, etc.) SDRAM, RAMBUS DRAM, etc. The external memory 158 may include one or more memory modules to which the memory devices are mounted, such as single inline memory modules (SIMMs), dual inline memory modules (DIMMs), etc. Alternatively, the external memory 158 may include one or more memory devices that are mounted on the integrated circuit 10 in a chip-on-chip or package-on-package implementation.
[0037] Numerous variations and modifications will become apparent to those skilled in the art once the above disclosure is fully appreciated. It is intended that the following claims be interpreted to embrace all such variations and modifications.
|
In an embodiment, an integrated circuit such may require that a full reset of the integrated circuit occur before the integrated circuit enters either a test mode or a functional mode. The integrated circuit may include a reset detector to detect that the reset has occurred, and the integrated circuit may not progress to the test mode or the functional mode unless the reset detector detects that the reset has occurred. Accordingly, if test mode is being entered, any user data that may have been stored in the integrated circuit during a preceding functional mode may have been cleared via the reset. Similarly, if normal mode is being entered, any test data that may have been stored in the integrated circuit in a preceding test mode may have been cleared via the reset.
| 6
|
The patent application is a continuation in part of patent application Ser. No. 600,747 filed July 30, 1975, now abandoned.
BACKGROUND OF THE INVENTION
In effecting a fluid seal between a stationary member (such as a wall or housing) and a rotating member (such as a shaft passing through an opening in the wall or housing), it is common to bridge the rotating and stationary members with a sealing member in contact with both to block the leakage of any substance through the opening in the wall or housing through which the shaft passes. Usually, the sealing member is secured to one of the bridged members (either the rotating member or the stationary member) and makes rubbing contact with the other member. With this arrangement, the seal continuously acts as a barrier to the passage of material (either into or out of the housing or through the wall) through the shaft opening.
It is essential that the sealing member maintain continuous contact with both the stationary member and the rotating member if continuous sealing between the two members is to be effected. Although the contact of the sealing member with the member to which it is secured presents no particular problems, the continuous rubbing contact of the sealing member with the other member produces rapid wear which, eventually, will render the sealing member ineffective to perform its sealing function. With such continuous rubbing contact of the seal member, frequent inspection, and periodic replacement, is necessary to avoid leakage.
Sometimes, of course, it is necessary to provide a continuous contact-type seal because the fluid which it is necessary to block is continuously present. However, there are other applications where the fluid which it is desired to block is present only on infrequent occasions. For example, many ships are divided by bulkheads into water-tight compartments. Rotating shafts of the ship's machinery frequently extend through two or more compartments and, accordingly, must pass through openings in the bulkhead separating two compartments. Ordinarily, there is no fluid in either compartment, and sealing is not necessary under normal conditions. It is necessary, however, to seal the openings around the shaft to prevent leakage of water from one compartment to the next in the unusual event that one compartment becomes flooded.
In order to eliminate the continuous wear caused by the continuous rubbing of a sealing member, it is known to provide a seal between a stationary member and a rotating member in which the sealing member is mounted on one of said members and normally out of contact with the other of said members, and in which the sealing member contacts said other of said members in rubbing engagement only in the infrequent event that fluid attempts to penetrate the seal.
SUMMARY OF THE INVENTION
The present invention relates to apparatus for effecting a fluid seal between a stationary member and a rotating member, and, more particularly, to apparatus which provides a bi-directional seal between these two members wherein the seal is effective only during an infrequent presence of fluid.
Although there are many applications where the bi-directional non-contact fluid seal of the present invention can be used to block leakage resulting from the occasional presence of water or other fluid, we have illustrated the seal apparatus of the present invention to prevent water from leaking from one flooded ship compartment to the next compartment (and alternatively from said next compartment to said one compartment) through a shaft opening in the partition, or bulkhead separating the two compartments. In the preferred form of the invention, a sealing member is secured to the rotatable shaft for rotation with the shaft. A stationary housing, which forms a part of the partition, has two aligned openings through which the rotating shaft extends. The sealing member has two, spaced apart, flexible radial flanges which rotate inside the housing. In their normal, relaxed state, the rotating flexible flanges are spaced from the walls of the housing so that, under normal operating conditions of the ship, there is no rubbing contact of the rotating sealing member with the stationary housing or bulkhead. Consequently, under normal operating conditions, there is no wear of the sealing member, and the necessity of frequent inspections and/or replacement of the seal is virtually eliminated.
When either compartment becomes flooded, the fluid from the flooded compartment attempts to flow out of that compartment to the next compartment through the openings through which the shaft passes. Since the sealing member is secured to the shaft to block the flow of water between the seal member and the shaft, the water will attempt to flow around the sealing member. Consequently, the water flows into the housing past the flange adjacent the flooded compartment, and pressure is exerted on the other flange by this flow which presses the other flange into sealing engagement with the wall of the housing adjacent said other flange.
It will therefore be seen that it is the presence of the liquid to be blocked which converts the seal of the present invention from a non-rubbing (and non-wearing) condition to a rubbing (and sealing) condition.
It is an object of the present invention to provide a seal between a stationary member and a rotating member which is effective only in the presence of fluid to be blocked and which then prevents the flow of fluid in either direction.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view, partly in cross-section, showing the sealing apparatus of the present invention mounted in a bulkhead of a ship.
FIG. 2 is a view taken on the line 2--2 of FIG. 1.
FIG. 3A is an enlarged view, taken on the line 3--3 of FIG. 2.
FIG. 3B is a view similar to FIG. 3A, but showing a different embodiment of the invention.
FIG. 4 is a view taken on the line 4--4 of FIG. 1.
FIG. 5 is a view taken on the line 5--5 of FIG. 3B.
FIG. 6 is a view taken on the line 6--6 of FIG. 5.
FIG. 7 is a view taken on the line 7--7 of FIG. 3A.
FIG. 8A is a view similar to FIG. 3A (and showing the same embodiment of the invention) but showing the conformation of the sealing member as water from a flooded compartment initially rushes into the housing.
FIG. 8B is a view similar to FIG. 3B (and showing the same embodiment of the invention) but showing the conformation of the sealing member as water from a flooded compartment initially rushes into the housing.
FIG. 9A is a view similar to FIG. 8A (and showing the same embodiment of the invention) but showing the conformation of the sealing member after the water has filled the portion of the housing in communication with the flooded compartment.
FIG. 9B is a view similar to FIG. 8B (and showing the same embodiment of the invention) but showing the conformation of the sealing member after the water has filled the portion of the housing in communication with the flooded compartment.
FIG. 10 is an exploded, perspective view of the sealing apparatus of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
There is shown in FIGS. 1, 2 and 10 the bulkhead 12 of a ship having compartments or zones 14 and 16 separated by the bulkhead. A rotating shaft 18 of the ship's machinery extends between the two compartments and passes through an opening 20 in the bulkhead.
In the normal course of the ship's operation, there is no need to seal the opening 20 in the bulkhead around the shaft because neither compartment contains a liquid, or other substance, which must be blocked from the adjacent compartment. However, in the event of damage to the ship so that one of the compartments, 14 or 16, becomes flooded, it is desirable to seal the opening 20 in the bulkhead around the shaft to prevent the escape of water from the flooded compartment to the adjacent compartment.
To this end, a housing 22 is secured to the bulkhead 12 over opening 20. The housing has a circular base 24 and a central circular wall 26 extending outwardly therefrom. The outer edge of the base 24 is bolted to the bulkhead 12 by bolts 28, and an O-ring 30, mounted in a groove in the base, is pressed into sealing engagement with the bulkhead when the bolts 28 are drawn up tight. The wall 26 has a cover 32 bolted thereto, by bolts 34, with an O-ring 36, mounted in a groove in the wall, between the cover and the wall to seal the joint against seepage of water. The base 24 and cover 32 have central openings 38 and 40, respectively, through which the rotating shaft 18 passes, defining gaps G14 and G16, respectively. To facilitate installation, the housing 22 and cover 32 are split at a central bisecting plane, as shown in FIGS. 2 and 10. Each half of the housing has protruding pads 37 at that plane, on opposite sides of opening 38, to receive securing bolts 39. Each half of the cover 32 has protruding pads 41 at that plane, on opposite sides of opening 40, to receive securing bolts 43. The housing and cover, when the halves thereof are secured together, define an internal annular chamber 42 around the shaft 18.
In the preferred form of the invention (see FIG. 3A), a sealing member 44 is secured to the shaft 18 for rotation in the chamber 42 as the shaft rotates. The sealing member 44 has a hub portion 46 with radially outwardly extending, spaced apart, circular flanges 48 and 50. The hub portion 46 has a central bore 52 through which the shaft 18 passes, the outer portions of the bore being tapered (as at 53) to accommodate deflection of the shaft, which might occur in the event of an accident, without a corresponding cocking of the sealing member 44 in the housing chamber 42. The hub and flanges constitute an annular ring which is split, as at 45 (FIG. 4), to facilitate installation. The hub portion 46 has end surfaces 46a, 46b, respectively, normal to the central axis A of the shaft. The two flanges 48 and 50, which extend generally radially outward in spaced relation to each other, are slightly inclined away from a center plane B (which extends through the sealing member 44 normal to axis A of the shaft) as the flanges extend outwardly. The flanges, at their outer ends, terminate in sealing surfaces 52, 54, which are radially beyond the boundary, or periphery, of openings 38, 40. The sealing member 44 is made of a flexible, resilient material, such as rubber.
We have heretofore employed a sealing member secured to a rotating shaft, which sealing member is received in a housing for rotation therein to seal the opening between the shaft and a bulkhead. However, in this previous sealing apparatus, we had the outwardly extending flanges continuously pressed into sealing engagement with the walls of the housing in which the sealing member rotated. The continuous rubbing engagement of the flanges with the walls of the housing required frequent inspections to assure that the sealing member flanges had not worn to the point where they could not effectively seal against the seepage of water in the event one of the compartments became flooded. Replacement of the sealing member because of wear was also required on occasion, even though no flooding had yet occurred. In other words, the sealing member would become too worn for effective use, even though it had not yet been called upon to do the sealing job for which it was designed.
In the present invention, in order to overcome excessive wear of the sealing member before an actual sealing is required, we have provided flanges 48, 50 (FIGS. 3A or 3B) which are normally spaced from the parallel end, or wall, surfaces (designated as 56, 58, respectively) of chamber 42 (FIGS. 3A or 3B) to define a gap or gaps 60, 62 therebetween. We have thus provided, in the present invention, a sealing member which rotates with the shaft (as our previous sealing member) but which (unlike our previous sealing member) makes no rubbing contact with the housing (or with any other member).
As shown in FIG. 3A, the sealing member 44 is secured tightly to the shaft 18 for rotation therewith by means of a band 64 which is received between the spaced apart flanges 48, 50 and completely encircles the hub 46 of the sealing member. As shown best in FIG. 7, blocks 66, 68 are secured, respectively, at one end of the band and close to the other end of the band. A screw 70, extending through block 68, is threadedly received in block 66. A spring 72 is received on the screw 70 between block 68 and the head 70a of the screw to draw the band up tight on the hub 46 of the sealing member when the screw 70 is drawn up tight. The sealing member, which is made of a flexible resilient material such as rubber, is squeezed down on the shaft by the band to grip the shaft tightly for rotation with the shaft. The band holds the sealing member tightly enough on the shaft to prevent the seepage of water (if one of the compartments 14 or 16 becomes flooded) along the shaft and under the sealing member.
Although not necessary to the effective operation of the invention, we, preferably, provide thrust shoulders, indicated generally at 74 and 76, secured to the sides of the sealing member hub 46. The thrust shoulders, which are ring shaped members secured, respectively, to the ends 46a, 46b of sealing member 44, are each composed of four segments (such as the four segments 76a, 76b, 76c and 76d) shown in FIG. 4. These segments are made of carbon, or a hard plastic such as Teflon, to provide a bearing surface in the event that the bulkhead, or the shaft, is shifted in an axial direction because of some abnormal condition. Normally, the sealing member 44 is centered in the housing chamber 42 (as viewed in FIG. 3A) so that the thrust shoulders 74 and 76 are spaced from the inner walls 56, 58 of the chamber 42.
Although not normally necessary, a stabilizing ring member 78 may be provided, as shown in FIG. 3B, to prevent buckling of the flanges and to provide a force transfer between the flanges. The ring member 78 is made up of two segments 80 and 82, each of which comprises two half-rings (such as 82a, 82b of FIG. 5) held together by links 84 which are pinned, as at 86, to the two half-rings. The two ring segments 80 and 82 are held together by retaining rivets 88 (FIG. 6), having a head 88a at one end received in a bore 90 in segment 82, and having a shank 88b received in a bore 92 in segment 80. The bores 90 and 92 are restricted at their inner ends to hold the heads 88a and the peened ends of shanks 88b so that the segments, after the retaining pins 88 have been installed, cannot be separated beyond the limits defined by the space between the heads and peened ends of the retaining rivets. The segments are normally held in their extreme spaced apart positions by compression springs 94 (FIG. 3B) which are received in bores 91 and 93 of the members 80 and 92, respectively.
As shown in FIG. 3B, the stabilizing member 78 has a body 78a with a frusto-conical portion 78b, and has flanges 78c and 78d extending from the sides of the body at its outer surface. When the stabilizing ring member is installed, as shown in FIG. 3B, it seats between the outer ends of flanges 48, 50 of the sealing member, with the sides of the body 78a engaged in complementary relation to the inclined inner surfaces 48a and 50a of the flanges. The stabilizing member, in its normal position between the flanges of the sealing member, does not urge the flanges into engagement with the inner walls 56, 58 of chamber 42. Thus, the gaps 60, 62 between surfaces 52, 54 of the flanges and the walls 56, 58 are preserved even with the stabilizing member in place. The stabilizing member, however, does serve to prevent the flanges from buckling inward beyond a limited amount as will be more fully explained hereafter.
Members similar to the band 64, the thrust shoulder 74, 76, and the stabilizing member 78 have been used before by us in our earlier seal. However, in our earlier seal, the stabilizing member served to urge the sealing member flanges into continuous rubbing engagement with the walls of the housing.
In normal operation of the ship, the compartments 14 and 16 are not under water, and no sealing between the compartments is required. The sealing member 44 is rotating (in chamber 42) with the shaft 18, but no part of the sealing member is engaged with any part of the stationary housing, or any other stationary member. Consequently, no part of the resilient rubber sealing member will undergo wear, and frequent inspection and/or replacement of the seal is not necessary.
In the event that one compartment, say compartment 16, becomes flooded, the seal will act, in response to the pressure of the water in compartment 16 (which exceeds the pressure in chamber 42), to automatically effect a water-tight seal between the two compartments. The water in compartment 16, which cannot pass between the sealing member 44 and the shaft 18, will enter gap G16 and rise between the flange 50 and wall 58, and pass through the circular gap 62 into chamber 42, as shown in FIG. 8A. The flow of water into chamber 42 will initially deflect the flange 50 inwardly (that is, to the left, as shown in FIG. 8A) to widen gap 62 and quickly fill chamber 42. The water enters chamber 42 past flange 50 (through gap 62 which is now expanded) faster than it can escape past flange 48 (through gap 60) so the pressure in chamber 42 rises quickly. The rising pressure in chamber 42 urges flange 48 (which may still be rotating) into sealing engagement with wall 56 (FIG. 9A), thereby closing gap 52 and blocking flow through gap G14. When the pressure in chamber 42 matches the pressure in compartment 16, the flange 50 returns to its normal position (FIG. 3A). A similar operation occurs, except in the reverse manner, if the flooding occurs in compartment 14 instead of compartment 16. If the stabilizing member 78 is used, as shown in FIG. 8B, the force exerted on flange 50 will be transmitted through the stabilizing member 78 to the flange 48, which is then also deflected to the left to press the rotating sealing surface 52 into sealing relation with stationary wall 56. After the water has filled chamber 42, the force of the pressure bearing against the inner surface 48a of the flange 48 will retain the sealing surface 52 of the flange against wall 56, as shown in FIG. 9B. At that time, however, the pressure on opposite sides of flange 50 has equalized, so flange 50 returns to its initial, normal position. Without the stabilizing member 78, the flange 50 might buckle inwardly under the force of the inrushing water and the sealing surface 52 of flange 48 would not be initially pressed against surface 56 until the pressure had built up in chamber 42.
It should be noted that if the flange 50 were eliminated, the flange 48 would still be deflected from its normal position to its sealing position, by the pressure of the fluid in compartment 16, but probably only after a significant quantity of water had escaped through gap 60 into compartment 14. The use of two flanges 48, 50, and a bridging ring 78, assures a quicker closing of gap 60 since the flange 50, and hence (by virtue of ring 78) the flange 48, will be deflected by the initial flow of water rushing into the chamber 42. Moreover, the use of two flanges 48 and 50 insures a sealing action regardless of whether compartment 16 or 14 is flooded. The use of a single flange, such as only flange 48, will seal if the flooding water enters compartment 16, but will not seal if the flooding water enters compartment 14. This is because in the former case, the flange is deflected into sealing engagement with wall 56, while in the latter case, the flange is deflected away from wall 56.
Thus, it will be seen that the sealing member 44 suffers no wear under normal conditions of operation of the ship, even though the ship is in operation for years, because there is normally no rubbing engagement between the flexible resilient sealing member (which is made of rubber or other soft material) and the stationary housing. However, when one compartment becomes flooded, a portion of the seal is pressed into rubbing engagement with a stationary member to form a seal between the flooded compartment and the adjacent compartment.
Although the best mode contemplated for carrying out the present invention has been herein shown and described, it will be apparent that modification and variation may be made without departing from what is regarded to be the subject matter of the invention.
|
A normally non-contacting rotary seal is disclosed which prevents fluid from leaking from one zone, or compartment, to the next through an opening in the compartment separating wall, or bulkhead, through which a rotating shaft passes. The passage of fluid through the wall opening is prevented regardless of which side of the wall becomes flooded. An annular resilient seal, having spaced apart radial flanges, is secured around the shaft for rotation therewith in an annular chamber at the separating wall. No part of the seal normally contacts the stationary walls of the chamber. In the event one compartment becomes flooded, liquid flows past the seal flange adjacent that compartment into the chamber, forcing the other seal flange into sealing contact with the wall of the chamber to block the flow of the liquid into the adjacent compartment. In another embodiment, a stabilizing ring is mounted between the flanges.
| 5
|
CROSS REFERENCE TO RELATED APPLICATION
This application claims the benefit under 35 U.S.C. § 119(e) of U.S. Provisional Patent Application No. 60/502,364, filed Sep. 12, 2003, which is hereby incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
This invention relates generally to the field of measurement of size and volume, and, in particular, to the measurement of size and volume of features such as tumors, lesions, sores, wounds on the surface of animals, plants and humans using 3D image construction from 2D images of the object and patterned light superimposed over the object.
BACKGROUND
The identification and selection of potentially active drugs for use in treatment of diseases, (for example, cancer) has largely been based on the screening of large numbers of compounds and rational drug design (when the molecular structure of the target such as tumor is known). Once compounds have been chosen based on selectivity to the target and desired functional effect, the ultimate test for advancement of a compound to clinical testing is to show its safety and its efficacy in multiple animal models.
There are several current methods and devices that are used to assess the growth of abnormal external features such as tumors, lesions, sores, port stains and wounds in such animal models. The simplest is to measure a feature in two dimensions, length and width, with the aid of a mechanical or electronic caliper that is manually operated. An approximate volume formula is then used to calculate the area or the volume of the object by assuming an ellipsoid shape of the mass. This is the most commonly used method, since it is simple and the calipers cost very little.
Unfortunately, this approach has obvious pitfalls related to the instrument and methodology used to calculate volume as well as operator-related errors. First, a major source of inaccuracy or variability is caused by the operator's judgment on the choice of the ellipsoid axes. For example, in making a measurement, a different operator may select a different choice of ellipsoid axes. Second, this approach is fairly time consuming. In the case of cancer studies, for example, a single study may involve hundreds of animals, and because the tumor volume measurements have to be done at least twice a week and take a given amount of investigator time per measurement, there is a limit in the number of studies that a single investigator can handle at once. Therefore, a different approach is needed to eliminate the inaccuracies of the methodology and instrumentation used and the subjectivity introduced by the operator.
Other mechanical volume measuring devices come closer to being an automated volume measurement system. These mechanical devices include a cylindrical chamber filled with elongated pins or filaments which, when pressed over a tumor or any other mass, convert the shape of the mass into volume information. Such devices require direct contact to features such as tumors, however.
The most sophisticated methods for measuring a mass include Computer Aided Tomography (CAT) using X-rays, Magnetic Resonance Imaging (MRI) using magnetic scans, Positron Emission Tomography (PET) using electrons and Single Photon Emission Computer Tomography (SPECT) using gamma rays. Such methods are capable of obtaining more accurate size and volume information about both external and internal features such as tumors and organs. The use of such methods is not feasible in many cases, however, due to long and costly preparation times, the unwanted effects of the contrast agents and radioactive compounds and the necessity to anesthetize animals during measurement.
Notwithstanding the availability of the foregoing techniques, there is no method or device for non-contact and fast measurement of the volume of surface features of small animals that can be used in, for example, pre-clinical cancer and inflammation studies. All the methods discussed above suffer from a number of disadvantages. For example, manual caliper measurements are prone to significant subjective operator errors; CAT, PET, MRI and SPECT methods are unacceptably time consuming and expensive; and caliper and cylindrical chamber methods require direct contact with the object under measurement, which is a potential source of feature deformation and contamination that may negatively effect the measurements being made.
As a result there is a need for methods and systems that accurately and quickly measure the volume/size of surface features such as wounds on the surface of animals, plants and humans.
SUMMARY OF INVENTION
The methods and systems of the present invention utilize a 3D structured light scanner and geometry based feature recognition logic to obtain shape, size and/or volume of the animal surface features observed in clinical studies. Such features may include tumors, lesions, sores, and wounds and any other suitable feature on the surface of animals, plants and humans, and any other suitable surface. The invention may obtain a number of 2D images of the surface feature, such as a tumor, with patterns of structured light projected on the feature. The parallax between a camera and a light source is used to compute a 3D point cloud of the feature's surface. The point cloud is a collection of (x, y, z) coordinates of the surface feature points. Recognition algorithm separates the feature points from the healthy points by minimizing the standard deviation of the point cloud points from the suggested shape. After the separation is achieved, the feature size and volume may be calculated.
In one embodiment, a system in accordance with the invention includes a 3D structured light scanner, controlled by a processor. The scanner obtains a set of 2D images of structured light, projected to the scanned object, and, in some implementations, extracts the structured light coordinates from these images. The processor obtains the images and/or structured light coordinates from the scanner. Using this data, the processor calculates the point cloud, separates the feature shape, finds its sizes and/or volume, and records the results in a measurement database
In this way, the invention provides for fast, non-contact, automated measurements of external features such as tumors, lesions, sores, wounds shape, size and volume on the surface of animals, plants and humans.
The invention also provides time savings, which are extremely important when measuring, for example, tumor progress using large animal sets. For example, the 3D scanner of the present invention is many times faster than CAT methods. Compared to caliper method, the 3D scanner measurements are also faster. In addition, the 3D scanner method may be completely automated (i.e., measurement data may be electronically transferred to a computer from a measuring device, eliminating extra time needed to record and transfer paper recorded data to computers).
The invention may further be totally non-invasive (i.e., no part of the device touches the animal). This leads to three important consequences, for example, for making tumor volume measurements: i) animals are not stressed as much, which less affects the tumor growth; ii) there is no need to sterilize the device; and iii) tumors are not deformed by the measuring equipment. Only the 3D scanner light touches the animals. The 3D scanner method does not involve injecting contrast agents or radioactive substances into animals. Since it takes a very short time, around a few seconds, to complete the measurement, the 3D scanner method is less stressful to animals and preferably does not require anesthetizing them.
Thus, in accordance with certain embodiments of the invention, methods and systems for measuring characteristics of a feature portion on the surface of living tissue also having a non-feature portion are provided. These methods and systems obtain a set of 3-dimensional coordinates corresponding to points on the surface of the living tissue using a 3-dimensional scanner, separate a feature portion of the set, which corresponds to the feature portion of the surface, from a non-feature portion of the set, which corresponds to the non-feature portion of the surface, and calculate the size of the feature based on the feature portion of the set.
Further in accordance with the invention, certain embodiments also include: basing the separation and calculation upon the feature portion of the surface having a predetermined feature shape and the non-feature portion of the surface having predetermined non-feature shape; the: predetermined feature shape and the predetermined non-feature shape being described by a finite set of parameters; performing successive approximations to find the set of parameters; selecting an arbitrary initial choice of the set of parameters for the successive approximations; calculating distances between coordinates in the set and each of the predetermined feature shape and the predetermined non-feature shape; assigning the coordinates in the set to the feature portion of the set when the coordinates are closer to the predetermined feature shape than to the predetermined non-feature shape, and to the non-feature portion of the set when the coordinates are closer to the predetermined non-feature shape than to the predetermined feature shape; finding the set of parameters by minimizing the standard deviation of the feature portion of the set from the predetermined feature shape and by minimizing the standard deviation of the non-feature portion of the set from the predetermined non-feature shape; and calculating the size of the predetermined feature shape based on the set of parameters and estimating the size of the feature portion of the surface to be the size of the predetermined feature shape.
BRIEF DESCRIPTION OF THE DRAWINGS
The preferred embodiments of the invention are described below in connection with the accompanying drawings, in which like reference numerals refer to like parts throughout and in which:
FIG. 1 is a block diagram of a system using a Personal Computer (PC) for image processing in accordance with certain embodiments of the present invention;
FIG. 2 is a flow chart of a process using a PC for image processing in accordance with certain embodiments of the present invention;
FIG. 3 is a block diagram of another system using a DSP for image processing in accordance with certain embodiments of the present invention;
FIG. 4 is a flow chart of another process using a DSP for image processing in accordance with certain embodiments of the present invention; and
FIG. 5 illustrates a mathematical model of a 3D scanner in accordance with certain embodiments of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the following detailed description, numerous specific details are set forth regarding the methods and systems of the present invention and the environments in which the methods and systems may operate in order to provide a thorough understanding of the present invention. It will be apparent to one skilled in the art, however, that the present invention may be practiced without such specific details. In other instances, well-known components, structures and techniques have not been shown in detail to avoid unnecessarily obscuring the subject matter of the present invention. Moreover, various examples are provided to explain the operation of the present invention. It should be understood that these examples are merely illustrative and various modifications may be made in accordance with the invention. It is contemplated that there are other methods and systems that are within the scope of the present invention.
Many designs of the 3D structured light scanners are known, and some of them are available commercially. While many 3D scanner capable of providing point cloud that is the collection of (x, y, z) coordinates of the surface feature points, may be used by the methods and systems of the present invention, not all known designs provide combination of accuracy and speed, suitable for scanning of live animal surface features. For this reason, different illustrative embodiments of a 3D scanner of the present invention are described below.
Both illustrative embodiments use the scanning by one moving stripe of light, projected on the scanned object. The motion of the stripe is synchronized with the video stream of stripe images on the scanned object.
Each video field of this video stream captures one stripe image position. These images are used either by a customized video Digital Signal Processor DSP, or by PC based software to extract the (x p , y p ) pixel coordinates of the stripe in the images. These (x p , y p ) pixel coordinates, together with the video field number N, identify the stripe point in 3-dimensional parameter space (x p , y p , N). A PC software program is used, as described later, to convert from this parameter space to (x o , y o , z o ) coordinates of the object points in the real world.
Turning to FIG. 1 , a system 100 in accordance with one embodiment of the invention is shown. As illustrated, system 100 may include a PC 102 , a microcontroller 104 , a data link 106 , a camera 108 , a camera link 110 , a stripe positioning system 112 , a control link 114 , and a control link 116 . The scanner operation is controlled by the PC 102 . The PC may be any suitable hardware and/or software for controlling system 100 , such as a personal computer, a processor, dedicated logic, etc. The PC is connected to microcontroller 104 using data link 106 . Microcontroller 104 may be any suitable hardware for controlling stripe positioning system 112 and/or camera 108 , and maybe incorporated for hardware and/or software in PC 102 . When running a non-real-time operating system, a separate microcontroller may be necessary. Link 106 may be a USB connection, an IEEE 1394 connection, or any other suitable connection that is used to send commands to set the scan parameters, to start the scan, to get the information that the scan is completed and for any other suitable purpose. The PC 102 also connected to the video camera 108 by the camera link 110 . Camera 108 may be any suitable device for capturing a light stripe 118 image on the scanned object and may be connected to microcontroller 104 by control link 114 . Control link 114 may be any suitable control link for controlling camera 108 . Camera link 110 may be an analog or digital link such as a USB connection, an IEEE 1394 connection, a Camera Link connection, or any other suitable connection. Link 110 may be used to transfer a video signal from camera 108 to PC 102 . When this signal is an analog signal, suitable circuitry in PC 102 , such as a frame grabber, may be used to digitize the signal for processing. The video signal contains information about the stripe light 118 , on the scanned object 120 . This information may be used to find a surface point cloud corresponding to the surface of scanned object 120 , as explained below. The video signal may also used for a video preview of subsequent scanning.
As also shown in FIG. 1 , stripe positioning system 112 may include a source 122 and a controllable mirror 124 . Source 122 may be any suitable source of a detectable stripe 126 , such as a laser, a focused non-laser light source, or other form of suitable energy, etc. Mirror 124 may be any mechanism suitable for positioning stripe 128 . Source 122 and mirror 124 may be controlled via control link 116 , which may be any suitable link for controlling source 122 and mirror 124 . The light that is reflected off object 120 forms reflected light 118 .
A process 200 for operating system 100 is shown in FIG. 2 . As illustrated, before any feature scans are performed, at step 202 , video camera 108 and stripe positioning system 112 are calibrated by extracting information from video images of a stripe 128 , taken at different positions on objects of known shape and size. In step 204 and 206 , microcontroller 104 , synchronizes the light 126 and the mirror 124 movements with the video camera 108 field sync signals through the control link 114 . Microcontroller 104 controls mirror 124 through an electronic link 116 so that stripe 126 takes different positions on object 120 , while camera 108 takes images of the stripe at these positions as part of a video sequence. At step 206 , the video sequence, consisting of several video frames, is captured by using the data video link 110 . Each video field has an image of one stripe position at different location. At step 208 , pixel coordinates (x p , y p ) of the stripe 128 image are extracted from the video data, and the stripe line number N is assigned according to the field number after the camera sync. At step 210 , the (x p , y p , N) array, and the calibration data, obtained earlier at step 202 , are used to calculate scanned object point cloud, as described below. Feature shape identification in step 212 is also described below. After the feature is identified, the volume calculation 214 is done as described below.
Turning to FIG. 3 , an alternate form of the embodiment of the invention in FIG. 1 is shown as system 300 . Except as set forth below, system 300 is substantially identical to system 100 . However, as illustrated, unlike system 100 , system 300 includes a DSP 302 connected between camera 108 and microcontroller 312 by links 304 , 306 , and 308 . As in the previous implementation, the scanner operation is controlled by the PC 102 . The PC is connected to microcontroller 302 using the data link 310 , which may be USB or IEEE 1394 cable. This link 310 is used to send commands to set the scan parameters, to start the scan, and to get the information that the scan is completed. It is also used to read the scan data from the DSP 302 output memory. The PC 102 also connected to the video camera 108 by the video link 110 , which may be analog cable carrying analog video signal to be digitized by the frame grabber inside the PC. It also may be digital link, such as USB, IEEE 1394, or Camera Link. In any case, this link 110 is used to get the video signal form the camera into PC. Unlike in the previous implementation, this video signal is not used to extract the geometry information from the video stream. Instead, it is used for the video preview and, possibly, for color still image, which may be necessary for documentation purposes.
The stripe light 118 , reflected from the scanned object 120 , carries information about the scanned object geometry. The video signal of this light is captured by the video camera 108 . The output signal 308 of this camera may be analog signal. In such a case it is digitized inside the DSP 302 . It also may be digital signal, supplied immediately to the logic part of the DSP 302 .
Turning to FIG. 4 , a process 400 for operating system 300 is shown. Beginning at step 402 , long before any feature scans are performed, the video camera 108 and the light positioning system 112 are calibrated by obtaining (x p , y p , N) arrays by the DSP from the scans of the objects of exactly known shape and size. At step 404 , a microcontroller 312 , programmable by PC 102 , synchronizes the light 120 provided by a light source 122 and the mirror 124 movement with the video camera field sync signals in the video signal on link 308 . The communication between microcontroller 300 and the light positioning system 112 is established through an electronic link 116 . In step 406 , an analog camera output is captured by a digitizer which is part of DSP chip 302 , and fed to DSP 302 , logic part of which may be implemented in a FPGA. Obviously, when camera 108 outputs to DSP 302 a digital signal instead of an analog signal, step 406 may be omitted. At step 408 , DSP 302 does background subtraction by subtracting the video fields obtained with structured light off from the fields with structured light on. The subtraction operation is done by using the background memory, which is part of the DSP 302 . Also in step 408 , the pixel coordinates (x p , y p ) of all stripe points are found, the stripe number N is assigned to each point, and the array (x p , y p , N) are written to an output buffer. In step 410 , the microcontroller 300 reads the (x p , y p , N) from the DSP output buffer through an electronic data bus 110 , and sends it to the host PC. Microcontroller 300 controls DSP 302 through a bus 304 to send necessary commands and processing parameters. Further processing is done by the host PC. So, the steps 412 , 414 and 416 are the same as steps 210 , 212 and 214 of the previous implementation.
Step 412 which is substantially identical to step 210 is performed next. At this step, the processes convert coordinates (x p , y p , N) into real 3-dimensional object coordinates (x o , y o , z o ). This step is performed using a mathematical model of the 3D scanner, which consists of the camera model, and the model describing positions of the light plane relative to the camera 108 .
FIG. 5 illustrates a scanner model 500 . As shown, in standard pinhole camera model, the camera lens is replaced by a pinhole 512 , located at a focal distance length f 502 from the image plane 504 defined by a Charged Coupled Device CCD, in camera 108 . The stripe image coordinates (x p , y p ) refer to this plane. If the beginning of the 3D coordinate system is placed at the pin hole 512 , then the stripe image point position vector {right arrow over (r)} p 506 is equal to “−(f, x p , y p )”.
As can be seen from FIG. 5 , the CCD image point {right arrow over (r)} p 506 and the object point {right arrow over (r)} o 508 lie on the same line, which passes through the pinhole 512 . This co-linearity is described as {right arrow over (r)} o =η·{right arrow over (r)} p , where ηis a scalar coefficient. To find η, one more condition is needed. It is provided by the observation that the object point is also the light plane point. The light plane 510 is described by the equation {right arrow over (r)} light — plane ·{right arrow over (n)} light — plane =1. So, for the point of the object intersection with light plane we have η=1/({right arrow over (r)} p ·{right arrow over (n)} light — plane ). Thus, the object (x o , y o , z o ) vector is given by the following equation
r
⇀
0
=
r
⇀
p
r
⇀
p
·
n
⇀
light_plane
This formula may be used to calculate object coordinates in steps 210 or 410 . The parameters {right arrow over (n)} light — plane plane for each light plane, as well as the focal length f, are found by calibration during the step 202 or 402 .
The calibration steps 202 or 402 are also used to find lens distortions. Standard axial symmetric lenses have distortions proportional to the square of distance of the image point from the optical axis. The coefficients of proportionality, found as a result of calibration, provide the necessary corrections to the above formulae, based on the pinhole model.
It should be emphasized here that the calculations according to the formulae above are necessary only in certain embodiments, where custom 3D stripe scanners are used. In general, any 3D scanner, including those that are commercially available, may be used to get the scanned object point cloud in accordance with the invention.
Next at steps 212 and 412 , the feature points are separated from the healthy skin points in the point cloud provided by the 3D scanner. This is in essence a further explanation step 212 or 414 of the method described in FIGS. 2 and 4 . For purposes of this explanation, it is assumed that the feature (such as tumor bump on the healthy skin) can be reasonably described by a limited number of parameters. In accordance with the invention, the standard deviation of the point cloud points from the assumed shape is minimized by adjusting these shape defining parameters.
For example, a feature (such as tumor) may be modeled as part of an ellipsoid cut off by a plane. The plane simulates healthy skin surface. The feature volume may be calculated as the volume of the part of the ellipsoid that is cut off by this plane. The calculation of the volume of the ellipsoid may be made by defining the parameters such as plane's position and the ellipsoid's position and orientation.
The healthy skin plane, as any plane, can be described by the following formula {right arrow over (n)}·{right arrow over (r)}=1, where {right arrow over (r)}=(x, y, z) is the position of a point on the plane, and {right arrow over (n)}=(n x , n y , n z ) is vector of a set of parameters describing the plane.
The scanner gives us a set of points {right arrow over (r)} i , where i is the index of the scan point. If an ideal plane is available, just three points would have been sufficient to define the position of the plane. Unfortunately, the coordinate set, provided by the scanner, represents the healthy feature skin, and this is not an ideal plane. So the best possible approximation of the healthy feature skin by a plane is used. The reasonable approach is to look for the plane which provides least possible standard deviation of the healthy feature skin points from this plane. More accurately, the distance between the plane and the point {right arrow over (r)} i is given by the formula
n ⇀ · r ⇀ i - 1 n ⇀ .
To find the plane position {right arrow over (n)}, the sum of squares of such distances for all the points, which should be approximated by the plane, is minimized. In other words, the expression
∑ i ( n x · x i + n y · y i + n z · z i - 1 ) 2 ( n x 2 + n y 2 + n z 2 )
is minimized as a function of three variables n x , n y and n z . The problem then is reduced to a nonlinear minimization problem which can be solved by standard methods.
There is still a need to distinguish between the points belonging to the healthy skin, whose coordinates should be included into the sum, and the feature such as tumor points, whose coordinates should be included in the ellipsoid parameter calculations, and therefore should not be included in the plane parameter calculations. Before describing the method to do that, a method to find ellipsoid parameters should be considered.
For the sake of simplicity, consider first the simplest version of an ellipsoid: a sphere. A sphere is defined by four parameters: the three coordinates of the sphere center {right arrow over (r)} center =(x center , y center , z center ), and the sphere radius R. The distance between the approximating sphere surface and the scanner-provided point {right arrow over (r)} i is given by the formula ∥{right arrow over (r)} i −{right arrow over (r)} center |−R|.
To find the sphere parameters, the sum of squares of such distances for all the points, which should be approximated by the sphere, is minimized. In other words, the following sum
∑ i ( ( x i - x center ) 2 + ( y i - y center ) 2 + ( z i - z center ) 2 - R ) 2
is minimized as a function of (x center , y center , z center ) and R. This nonlinear minimization problem is treated the same way as the problem of finding plane parameters.
For an ellipsoid, the square of the distance between the scanner-provided point {right arrow over (r)} i and the ellipsoid surface is equal to (x i −x ell ) 2 +(y i −y ell ) 2 +(z i −z ell ) 2 . Here (x ell , y ell , z ell ) are the coordinates of the point on the ellipsoid, closest to the scanner-provided point {right arrow over (r)} i . To find this ellipsoid point, it is convenient to use the new coordinate system, related to the main axes of the ellipsoid. The transformation to such coordinate system is achieved by one translation and one rotation in the 3-dimensional space. The translation and rotation parameters should be regarded as the parameters to be found as a result of minimization, as described below.
In the coordinate system, defined by the main axes of the ellipsoid, coordinates of any point of the ellipsoid surface satisfy the equation
x ell 2 a 2 + y ell 2 b 2 + z ell 2 c 2 = 1 ,
where a, b, and c define ellipsoid sizes. The normal vector to the ellipsoid surface is proportional to gradient of the ellipsoid equation, which is given by the vector
[ x ell a 2 , y ell b 2 , z ell c 2 ] .
The vector between the scanner-provided point {right arrow over (r)} i and the closest ellipsoid point should be proportional to the normal vector. That means the following equation should be satisfied:
( ( x i - x ell ) , ( y i - y ell ) , ( z i - z ell ) ) = λ i [ x ell a 2 , y ell b 2 , z ell c 2 ]
where λ i is some scalar coefficient. This equation can be used to express (x ell , y ell , z ell ) as functions of λ i and of coordinates of scanner-provided point {right arrow over (r)} i . These expressions may be put back to the equation of the ellipsoid, giving the following equation for the λ i :
x
i
2
·
[
a
λ
i
+
a
2
]
2
+
y
i
2
·
[
b
λ
i
+
b
2
]
2
+
z
i
2
·
[
c
λ
i
+
c
2
]
2
=
1
After λ i is found as solution of this equation, it should be used to calculate the distance between the scanner-provided point {right arrow over (r)} i and the ellipsoid. The minimization should include sum of squares of such distances for all scan points assigned to the ellipsoid:
∑
i
λ
i
2
·
[
[
x
i
λ
i
+
a
2
]
2
+
[
y
i
λ
i
+
b
2
]
2
+
[
z
i
λ
i
+
c
2
]
2
]
To distinguish the healthy skin plane points from feature ellipsoid points, an optimization in the space of the plane and ellipsoid parameters is used: First, some initial set of the plane and the ellipsoid parameters is chosen. Using these parameters, the distance between any point and the plane and between the same point and ellipsoid can be calculated. Accordingly, the scan points, which are closer to the plane, are assigned to the plane, and the rest are assigned to the ellipsoid. Then the standard deviation for the complete point cloud is calculated. This standard deviation, as a function of the plane and ellipsoid parameters is the target function to be minimized. Standard nonlinear minimization methods, such as described in the book Numerical Recipes in C, Cambridge University Press, ISBN 0521 43108 5, Chapter 10.5 Direction Set (Powell's) Methods in Multidimensions, pp 412-420, which is hereby incorporated by reference herein in its entirety, can be used to find the minimum.
The set of parameters, providing the minimum, gives the plane position and the ellipsoid shape, sizes, and position relative to the plane. Having these parameters, the feature size or volume is calculated in step 214 or 416 as described below.
Volume Calculation:
Minimization provides the ellipsoid and the plane parameters. It is convenient to perform volume calculations in the ellipsoid-related coordinate system. In this coordinate system, the ellipsoid is described by the equation
x ell 2 a 2 + y ell 2 b 2 + z ell 2 c 2 = 1 ,
and the plane is described by the equation {right arrow over (n)}·{right arrow over (r)}=1. Standard geometry calculations may be used to determine if there is an intersection between the ellipsoid and the plane. If there is no such intersection, then the feature (tumor) volume is given by the ellipsoid volume:
4
3
·
π
·
a
·
b
·
c
On the other hand, if there is the intersection between the ellipsoid and the plane, then the ellipsoid volume is divided into two parts, and only the volume of one of these parts is the volume of the feature. While the numerical volume calculation is trivial, the volume calculation formulae are complex. To avoid complicated formulae, we show only the analytic result for the case when the feature is represented by a small part of the ellipsoid that is cut off by the plane, and the plane is orthogonal to one of the main axes of the ellipsoid. If the z-axis is chosen as such axis, then the plane equation can be written as h·z=1. For this case the feature volume is equal to
π
·
a
·
b
·
c
·
(
Δ
2
-
Δ
3
3
)
where
Δ
=
1
-
h
c
.
Although the invention has been described and illustrated in the foregoing illustrative embodiments, it should be understood that the present disclosure has been made only by way of example, and that numerous changes in the details of construction and combination and arrangement of processes and equipment may be made without departing from the spirit and scope of the invention.
|
Methods and systems for measuring volume and size of features such as lesions, tumors, sores, and wounds external to animal, human and plant skin, using 3D structured light scanners are provided. These methods and systems obtain a point cloud of the scanned feature, and employ algorithms to adjust the suggested feature geometry parameters to minimize deviations of the point cloud from suggested feature geometry. Obtained geometry parameters permit the calculation of the features' sizes and volumes.
| 0
|
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The present application claims priority to and the benefit of the filing date of U.S. Provisional App. No. 61/730,395 filed on Nov. 27, 2012, which is incorporated herein by reference in its entirety for all purposes.
TECHNICAL FIELD
[0002] This invention relates to a reset actuation device which uses a cam profile to reduce and control reset pin motion for a compression relief brake.
BACKGROUND
[0003] Compression braking is known in the art and is used for many applications, including braking heavy vehicles. Compression brakes convert an internal combustion engine cylinder to a compressor by cutting off the fuel flow and opening an exhaust valve of the cylinder near the end of the compression stroke. This allows the power generated in the piston to escape to the atmosphere, rather than continuing to power the vehicle. One type of compression braking system is shown in U.S. Pat. No. 6,253,730 to Gustafson.
[0004] An early technique for accomplishing compression braking is disclosed in U.S. Pat. No. 3,220,392 to Cummins, where a slave hydraulic piston located over an exhaust valve opens the exhaust valve near the end of the compression stroke of an engine piston with which the exhaust valve is associated. To place the engine into braking mode, solenoids are energized which cause pressurized lubricating oil to flow through a control valve, creating a hydraulic link between a master piston and a slave piston. The master piston is displaced inward by an engine element (such as a camshaft mechanism) periodically in timed relationship with the compression stroke of the engine. A typical modern compression braking system may include exhaust valves operated during the engine's power mode by an exhaust rocker lever.
[0005] The system may also include a reset valve which operates to cause the slave piston to retract after an initial opening of the exhaust valve during braking. As a result, the exhaust valve is closed prior to the end of the expansion stroke and before the hydraulic pressure drops due to a return motion of the master piston. This design advantageously avoids shock or asymmetric loading of the valve or valve crosshead by the exhaust rocker arm at the start of the main opening event of the exhaust valve following the initial opening event.
[0006] The modern compression braking system has been further improved by the system disclosed in Gustafson, wherein the engine compression braking system has an integral rocker lever and reset valve capable of effectively avoiding asymmetric loading of a valve crosshead while providing accurate and predictable compression braking. However, further improvements in this technological area are desired.
SUMMARY
[0007] Systems, apparatus, and methods are disclosed herein to improve the operation of a reset pin in a compression brake assembly.
[0008] The systems, apparatus and methods disclosed herein present an alternative approach and enhancement to the rocker lever compression brake disclosed in U.S. Pat. No. 6,253,730 to Gustafson, the entire contents of which are hereby incorporated by reference. Although the function is similar to the device disclosed in U.S. Pat. No. 6,253,730, such as shown in FIGS. 1 a and 1 b , the reset actuation device of the present disclosure includes a reset pin that is actuated via a cam shaped surface on the rocker shaft, such as shown in the rocker lever of FIGS. 2-11 of the present disclosure.
[0009] Controlling motion of the reset pin by the cam surface on the rocker shaft separates the reset pin motion from the base camshaft profile lift. Shorter lift reduces the reset ball total travel and allows for improved reset spring design. In addition, the cam surface can increase the lift of the reset pin after the reset event and exhaust valve closure to enhance filling of the slave piston.
[0010] This summary is provided to introduce a selection of concepts that are further described below in the illustrative embodiments. This summary is not intended to identify key or essential features of the claimed subject matter, nor is it intended to be used as an aid in limiting the scope of the claimed subject matter. Further embodiments, forms, objects, features, advantages, aspects, and benefits shall become apparent from the following description and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIGS. 1A and 1B are cross-sectional illustrations of a prior art compression relief brake reset mechanism with an integral rocker lever and reset valve operated by a reset pin in conjunction with a reset pin contact pad on a pedestal mount.
[0012] FIG. 2 is a cross-sectional illustration of a rocker lever assembly with a rocket lever connected with a cam at one end and an exhaust valve of a cylinder at an opposite end, the rocker lever being pivotally mounted about a support shaft with a cam surface that contacts a reset pin of a reset actuation device for compression relief braking.
[0013] FIG. 3 is a cross-sectional illustration of the rocker lever of FIG. 2 with the position of the rocker lever and reset pin at zero lift.
[0014] FIG. 4 is a cross-sectional illustration of the rocker lever of FIG. 2 with the position of the rocker lever and reset pin at peak lift.
[0015] FIG. 5 is a cross-sectional illustration of the rocker lever of FIG. 2 .
[0016] FIG. 6 is a cross sectional view of the rocker lever along line 6 - 6 of FIG. 5 with reset pin in the brake on position.
[0017] FIG. 7 is the cross sectional view of the rocker lever of FIG. 6 with reset valve in the brake off position.
[0018] FIGS. 8 and 9 are perspective view illustrations of the rocker lever.
[0019] FIG. 10 is a perspective view of the support shaft of the rocker lever.
[0020] FIG. 11 is a top elevation view of the rocker lever.
DETAILED DESCRIPTION
[0021] For the purposes of promoting an understanding of the principles of the invention, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the invention is thereby intended, any alterations and further modifications in the illustrated embodiments, and any further applications of the principles of the invention as illustrated therein as would normally occur to one skilled in the art to which the invention relates are contemplated herein.
[0022] Referring to FIGS. 1A and 1B , a compression relief braking system 120 is shown similar to that disclosed in U.S. Pat. No. 6,253,730 to Gustafson. In this system, a rocker lever 140 is provided on a support shaft 170 . Rocker lever 140 includes a reset pin 192 slidably mounted in a bore 190 , where the upper end of reset pin 192 is immediately adjacent the valve seat for abutment by reset valve head 194 . Reset pin 192 is positioned to contact and move valve head 194 against the force of bias spring 196 . Valve head 194 is positioned to open and close bore 190 , which separates low pressure fluid circuit 164 from high pressure fluid circuit 166 . A reset pin contact pad 122 is mounted on an engine component, for example a pedestal 124 , immediately adjacent a lower end of reset pin 192 . During the initial pivoting movement of rocker lever 140 , reset pin 192 will contact reset pin contact pad 122 mounted on pedestal mount 124 , causing reset pin 192 to move upwardly, thereby moving reset valve head 194 off its seat from a closed position into an open position, shown in FIG. 1B . In this prior art embodiment, the amount of travel of the reset pin 192 at peak lift is shown in FIG. 1B .
[0023] FIG. 2 illustrates an embodiment of the compression relief brake apparatus 20 of the present invention. Apparatus 20 includes a rocker lever 40 operably connected at one end to a cam 30 that pivots or rotates rocker lever 40 about a support shaft 70 to control opening and closing of at least one exhaust valve 26 of engine cylinder 28 . A reset valve assembly 90 is housed in an obliquely oriented bore 98 of the rocker lever 40 , and a portion of bore 98 also serves as a fluid passage 62 . Passage 62 is in flow communication with a slave piston 32 , which is coupled to exhaust valve 26 , and a fluid supply 86 . Slave piston 32 reciprocates between a lower position, in which exhaust valve 26 is open and an upper position, in which exhaust valve 26 is closed, the distance between the lower and upper positions of slave piston 32 is represented schematically as a distance D in FIG. 2 . Slave piston 32 may also be connected to crosshead 22 that is connected to a second exhaust valve of cylinder 28 .
[0024] Reset valve assembly 90 includes a reset pin 92 slidably mounted in bore 98 , where a second or upper end of reset pin 92 is immediately adjacent the valve seat 78 for abutment by reset valve head 94 . In the illustrated embodiment, reset valve head 94 is a ball valve, although other valve types are not precluded. Reset pin 92 is positioned to contact and move valve head 94 against the force of bias spring 96 . When the reset valve 90 is in the closed position, with reset valve head 94 seated in the valve seat 78 , fluid is trapped in the slave piston 32 under high pressure, which enables slave piston 32 to hold exhaust valve 26 open, which in turn enables a compression brake event in a compression braking mode of operation.
[0025] FIGS. 3 and 4 show the effect on reset pin 92 of the rotation or pivoting of rocker lever 40 around support shaft 70 . Cam surface 72 of support shaft 70 has a concave surface portion 74 and a convex surface portion 76 . It should be understood that other profiles of cam surface 72 are also possible in order to achieve the objectives stated herein. When in a compression braking mode of operation, cam surface 72 of support shaft 70 contacts a first end of reset pin 92 and rotation of rocker lever 40 around support shaft 70 causes movement of the first end of reset pin 92 along cam surface 72 . When the first end of reset pin 92 is in contact with the concave surface portion 74 of support shaft 70 , the position of the second end of reset pin 92 adjacent valve head 94 allows valve head 94 to be seated against the valve seat 78 , in a closed position, as shown in FIG. 3 . When the first end of reset pin 92 is in contact with the convex surface portion 76 of support shaft 70 , the second end of reset pin 92 pushes valve head 94 off of valve seat 78 to an open position, overcoming the force of the reset valve bias spring 96 and any force due to a difference in hydraulic pressure on either side of the valve head 94 , as shown in FIG. 4 .
[0026] FIG. 5 is a cross sectional illustration of the rocker lever 40 in a closed position with valve head 94 against valve seat 78 . FIG. 6 is a cross sectional view of the rocker lever 40 along line 6 - 6 of FIG. 5 with the reset valve assembly 90 in the brake on position. A detent mechanism 50 includes a detent ball 51 and corresponding spring 52 , which are arranged within a receptacle 53 of rocker lever 40 , which is transverse to bore 98 housing reset pin 92 . There is a recess 56 around reset pin 92 , which provides a seat for detent ball 51 to lock reset pin 92 in an open position when compression braking mode is off, as shown in FIG. 7 . In an open position, fluid flows from slave piston 32 through fluid passage 62 of bore 98 to and from a fluid supply passage 84 that is connected to a fluid supply 86 . When a compression braking mode of operation is on, as shown in FIG. 6 , a control fluid pressure 54 pushes detent ball 51 away from recess 56 on the side of reset pin 92 . When detent ball 51 is not seated in recess 56 , reset pin 92 can move freely in bore 98 under bias of spring 96 and in response to a position of cam surface 72 of support shaft 70 relative to the first end of reset pin 90 when rocker lever 40 rotates around support shaft 70 . This allows reset valve head 94 to seat, thereby sealing to valve seat 78 and trapping fluid in slave piston 32 , enabling a compression braking event. It should be noted that in an alternative embodiment, detent ball 51 may be alternatively replaced by a cylindrical detent as disclosed in U.S. Pat. No. 6,253,730 to Gustafson.
[0027] FIG. 7 shows the position of detent ball 51 and corresponding spring 52 when compression braking mode is off. In this mode control fluid pressure 54 is reduced so detent ball 51 is spring biased into engagement with reset pin recess 56 . Reset pin 92 is thereby locked into a position where it is pushing reset valve head 94 off the valve seat 78 and maintaining the valve head 94 in an open position, regardless of the motion of rocker lever 40 around support shaft 70 . This does not allow fluid pressure to build up in slave piston 32 , allowing exhaust valve 26 to open and close freely in response to the movement of rocker lever 40 in normal operation.
[0028] FIGS. 8-9 are perspective view illustrations of the rocker lever 40 mounted to support shaft 70 . FIG. 10 is a perspective view of the rocker lever support shaft 70 showing cam surface 72 formed into an outer surface of support shaft 70 to define concave and convex cam surface portions 74 , 76 . FIG. 11 is a top elevation view of the rocker lever 40 mounted about support shaft 70 .
[0029] The present invention described above advantageously permits the lift of reset pin 92 to be limited as desired by the cam surface 72 formed on support shaft 70 . This has the further advantage of reducing the design requirements of the reset valve bias spring 96 . Moreover, the present brake reset mechanism incorporates an initial negative curvature 74 on the cam surface 72 , which lowers stress when lifting the reset valve head 94 off of the valve seat 78 at high brake cavity pressures at the start of the reset operation.
[0030] Many aspects of the present invention are envisioned. For example, one aspect is directed to a system comprising a compression relief brake apparatus with a rocker lever pivotally mounted on a support shaft with a cam surface and a reset valve assembly. The rocker lever is connected to an exhaust valve of an internal combustion engine cylinder at one end and connected to a cam member that pivots the rocker lever about the support shaft at the other end. The reset valve assembly is housed in a passage of the rocker lever and the passage is in flow communication with a slave piston coupled to the exhaust valve. The passage is also in flow communication with a fluid supply and a reset valve assembly opens and closes the passage with a reset pin. In a compression braking mode of operation, the cam surface of the support shaft contacts one end of the reset pin and rotation of the rocker lever around the support shaft causes movement of the end of the reset pin along the cam surface. This movement positions the reset valve assembly to close the passage and isolate the slave piston from the fluid supply.
[0031] In one embodiment, one end of the reset pin rides the cam surface of the support shaft to displace the reset pin along the passage to open and close the reset valve assembly. In one refinement of this embodiment, the reset valve assembly includes a reset ball that is positionable with the reset pin to open and close the passage and one end of the reset pin is in contact with the reset ball. In a further refinement, the reset ball is spring biased toward the second end of the reset pin.
[0032] In another embodiment, closing the reset valve assembly traps fluid in the slave piston to maintain the exhaust valve in an open position for compression braking. In a further embodiment, the cam surface of the rocker lever support shaft includes a concave and a convex portion. One end of the reset pin contacts the concave portion when the reset valve assembly is in a closed position and the end of the reset pin contacts the convex portion when the reset valve assembly is in an open position. In yet a further embodiment, the reset valve assembly is normally locked in the open position with a detent mechanism when the compression mode of braking is off.
[0033] In one embodiment, the support shaft includes a cylindrical body and the cam surface is formed in an outer surface of the cylindrical body. In another embodiment, the passage includes a first portion between the reset valve assembly and the slave piston and a second portion that houses the reset pin. A fluid supply passage extends from the second portion of the passage to a fluid supply. In one refinement of this embodiment, there is a receptacle in the rocker lever that houses a detent locking mechanism that locks the reset pin and a second fluid supply passage between the receptacle and a fluid supply to unlock the detent mechanism from the reset pin.
[0034] According to another aspect, the system comprises a compression relief brake apparatus with a rocker lever pivotally mounted on a support shaft with a cam surface and a reset valve assembly. The rocker lever is connected to an exhaust valve of an internal combustion engine cylinder at one end and connected to a cam member that pivots the rocker lever about the support shaft at the other end. The reset valve assembly is housed in a passage of the rocker lever and the passage is in flow communication with a slave piston coupled to the exhaust valve. The passage is also in flow communication with a fluid supply and a reset valve assembly opens and closes the passage with a reset pin. A detent mechanism has a position in engagement with the reset pin to lock the reset valve assembly in an open position when compression mode of braking is off and in a second position disengaged with the reset pin when compression mode of braking is on to allow movement of the reset pin within the passage. In a compression braking mode of operation, the cam surface of the support shaft contacts one end of the reset pin and rotation of the rocker lever around the support shaft causes movement of the end of the reset pin along the cam surface. This movement positions the reset valve assembly to close the passage and isolate the slave piston from the fluid supply.
[0035] In one embodiment, one end of the reset pin rides the cam surface of the support shaft to displace the reset pin along the passage to open and close the reset valve assembly. In another embodiment, the reset valve assembly includes a reset ball that is spring biased toward contact with the end of the reset pin that is not in contact with the cam surface. In a further embodiment, the detent mechanism is housed in a receptacle of the rocker lever that is in fluid communication with a control fluid. In one refinement of this embodiment, the detent mechanism includes a ball member spring biased into engagement with a recess in the reset pin when compression braking mode is off to maintain the reset valve assembly in an open position. In a further refinement, control fluid is provided to the receptacle to force the ball member out of the recess to unlock the reset pin in the compression braking mode of operation.
[0036] While the invention has been illustrated and described in detail in the drawings and foregoing description, the same is to be considered as illustrative and not restrictive in character, it being understood that only certain exemplary embodiments have been shown and described. Those skilled in the art will appreciate that many modifications are possible in the example embodiments without materially departing from this invention. Accordingly, all such modifications are intended to be included within the scope of this disclosure as defined in the following claims. In reading the claims, it is intended that when words such as “a,” “an,” “at least one,” or “at least one portion” are used there is no intention to limit the claim to only one item unless specifically stated to the contrary in the claim. When the language “at least a portion” and/or “a portion” is used the item can include a portion and/or the entire item unless specifically stated to the contrary.
|
An engine compression braking system having a rocker lever and reset valve assembly to operate an engine in both normal power and braking modes while effectively controlling opening and closing of the exhaust valve for compression braking. The reset valve assembly includes a reset pin mounted in a passage of the rocker arm and movement of the reset pin in the compression mode of braking is controlled by contact of the reset pin with a support shaft which the rocker arm rotates around.
| 5
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a process for converting and printing on paper webs, and to a printing machine for printing on converted webs to carry out this process.
2. Discussion of the Related Art
Frequently, the base paper that exits a paper machine requires an additional conversion to account for the different requirements so that the paper can be printed on. The principle conversion processes are coating and calendering.
In coating, a coating dye that consists of pigments and fixing agents is applied, with the aid of a coating machine, to the base paper on one or both sides of the paper. Coating a base paper produces a closed and smooth, easily printable paper surface.
In calendering, smoothness and/or gloss are created, with the aid of a calender, on the surface of the base paper. Calendering a base paper increases the ability to apply ink during the printing process. Calenders typically have at least one roller gap, and preferably have several roller gaps. The roller gaps are defined by the juncture of a hard and soft roller. The hard rollers are preferably heatable rollers that are made of chill casting or steel. The soft rollers are preferably provided with a flexible outer covering. The web (e.g., the base paper) is subjected to a pressure treatment and, in most cases, a temperature treatment in these roll gaps, which create the desired smoothing of the web. Such calenders are generally well known. An example of such a calender is disclosed, for example, in German Reference DE-U-295 04 034.3.
Coating machines and calenders have conventionally been set up in paper factories and have been placed behind (i.e., downstream) with respect to a paper machine in the work sequence, either in-line or off-line. The converted web, which has a width corresponding to the paper machine, is formed into a roll in a wind-up device. During the winding-up process, there is a great deal of difficulty in creating a uniformly wound roll, particularly due to the fact that the web, because of its great surface smoothness, tends to slip sideways on a cushion of air that is present during the winding-up process.
To further process the web of paper in a printing plant, the rolls are usually cut, while still in the paper factory, into narrower rolls that match the width of the printing machines. The cutting of the roll is typically done by a roll-slitting machine, which divides the wide web that is unwound from a roll into separate partial webs by means of longitudinal cutters. Each of these separate partial webs are wound into a separate roll of lesser width in a winding station. With this second winding-up process there is still a tendency for the webs to slip sideways because of their relatively smooth surfaces.
The individual rolls that are made from the converted webs of paper must subsequently be individually packaged so that they can be transported to a printing plant in a protected manner. Additionally by packaging the individual rolls, the paper's moisture can be retained. Of course, this packaging of each individual roll is quite expensive.
Accordingly, it is an object of the present invention to improve the preparation of converted paper for printing.
SUMMARY OF THE INVENTION
This object is achieved in accordance with the present invention by converting the running web and subsequently printing thereon with no intermediate winding up process.
Thus, the method according to the present invention dispenses with the requirement of winding the converted paper into a roll. Shortly after the completion of the conversion treatment, the running web enters into the printing area. The individual rolling-up process in the paper factory is, thus, made substantially simpler because only the base paper has to be formed into a roll (i.e., wound-up). Because of the relatively rough surface and the greater volume of the base paper, it can be wound significantly more easily than paper that has been converted and is, therefore, smooth.
A further advantage of the present invention is the improved printing quality that can be achieved. Conventionally, it is practically impossible to avoid losing smoothness in the converted web of material during the long periods of storage and transport before the web was printed on in the printing process. This loss of smoothness can be attributed to the fact that the fibers, which have been leveled on the surface of the web, relax and stand up again over time. In accordance with the present invention, however, only a very short period of time exists between the conversion and the printing of the web. Thus, it is practically impossible for the surface fibers to stand up again during this relatively very short period of time. Thus, it is also possible to adjust or regulate the surface smoothness of the base paper so that it is optimally matched to the application of ink during printing.
The yet unconverted web is preferably cut to the width required for printing, formed into a roll, and drawn off this roll for conversion and printing. Thus, a wide web is cut into several partial webs in the paper factory as usual, but these partial webs have yet to be converted. Thus, the partial webs can be wound up easily. In addition, less expensive packaging can be used because the web has not yet reached its final conversion stage, and because the moisture content can still be used during the coating or calendering processing.
The converted web is optionally tempered before the printing step to achieve an especially good adapting of the web to the printing process.
The conversion can be achieved by calendering or coating, or through coating and subsequent calendering. The entire conversion is preferably carried out in the printing plant. But substantial advantages of the present invention can still be achieved even if only the concluding conversion treatment is carried out together with the printing during a single pass (in other words, a portion of the conversion has already been carried out in the paper factory).
In accordance with the present invention, a facility for the conversion of the web of paper is disposed in front of the entrance to the printing machine. The pass-through speed of the conversion facility matches that of the printing machine.
The conversion facility can be a coating device and/or a satinizing calender. In both cases, the surface of the web of paper is smoothed, which improves the printing process.
Because the pass-through speed of the conversion facility matches the pass-through speed of the printing machine, the conversion facility works comparatively slowly. In the case of a coating machine, the coating dye can be carefully applied with little effort. In the case of a calender, longer hold or dwell times of the web in the roller gap result, which leads to higher smoothness values. In addition, a calender that runs slower than calenders that are commonly used in paper factories is easier to manufacture and operate, and is less expensive to produce and operate.
The working width of the conversion facility is equal to or slightly greater than (i.e., is approximately equal to) that of the printing machine. Because the conversion facility can be allocated to a specific printing machine, the working width of the conversion facility can be matched to that of the printing machine. Thus, the conversion facility has a lesser width in comparison with the coating machines and calenders that have been commonly used in paper factories. Because of the smaller width, in combination with the slower speed, the conversion facility according to the present invention has markedly lower production costs.
In a further embodiment, a tempering facility, which affects the web temperature, is disposed between the exit of the conversion facility and the entrance to the printing machine.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
The above and still further objects, features and advantages of the present invention will become apparent upon consideration of the following detailed description of a specific embodiment thereof, especially when taken in conjunction with the accompanying drawings wherein like reference numerals in the various figures are utilized to designate like components, and wherein:
FIG. 1 is a schematic illustration of a combination calender and printing machine;
FIG. 2 is a schematic illustration of a combination coating machine and printing machine; and
FIG. 3 is a logic diagram showing the process sequence.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1, a winding off station 1 is illustrated. Wind-off station 1 includes a roll 2, which contains a web 3 of uncalendered (i.e., unconverted) paper. Web 3 runs through a calender 4. Web 3 leaves an exit 5 of the calender as a calendered web (i.e., a converted web 3'). Converted web 3' then winds, by an angle of more than 180°, around a tempering roller 6, which determines the web temperature. Thereafter, converted web 3' enters into an entrance 7 of a printing machine 8. Thereafter, converted web 3' enters into a folding apparatus 9, which is disposed at the end of the printing machine 8.
Calender 4 is comprised of hard rollers 10 and soft rollers 11. Hard rollers 10 are made of steel or chilled casting and are heated. Soft rollers 11 have a flexible outer covering 12. The rollers 10 and 11 are pressed in their working directions against each other by a device (not shown) so that the web 3 is affected by pressure and temperature in the roller gaps 13, and is smoothed as a result.
Printing machine 8 has four printing couples 14-17 for the first printing and four printing couples 18-21 for the second printing. Thus, printing machine 8 is an eight-color gravure, web-fed rotary press. The individual printing couples 14-21 each have engraved cylinders 23, which dip into ink troughs 22, in a conventional manner. In each printing couple, web 3' is guided between engraved cylinder 23 and an adjacent rubber impression cylinder 24, and, with the aid of tensioning means 25, is subsequently directed over at least one drying cylinder 26. Printing machine 8 has a common drive shaft 27, which drives the engraved cylinders 23 by means of appropriate transmissions 28 or 29.
A matching of the smoothness or gloss values to the requirements that have to be met for optimum printing in the printing machine 8 can be attained by regulating the pressure in the roll gap and/or the temperature of the hard rollers 10.
Referring now to FIG. 2, a coating machine 30 is illustrated. A winding-off station 31 is disposed upstream of (or in front of) coating machine 30 as viewed from the direction of movement of web 32. A printing machine 8 is disposed downstream from coating machine 30. Printing machine 8 corresponds to the printing machine 8 illustrated in FIG. 1, and terminates with a folding apparatus 9. Web 32 is unwound from winding off station 31 and enters into coating machine 30. Web 32 runs through a path, which is defined by guide rollers 33. Coating dyes are applied at a coating basin 34, and the excess is stripped off by means of a wiping blade 35. Subsequently, a first drying step is carried out in an infrared heating facility 36, and a second drying step is carried out in a hot-air drying facility 37. The now coated web 32' (i.e., a converted web 32') next winds partly around heating roller 6, and then enters printing machine 8. The web of paper is, thus, taken from a stored roll in an unwinding station 31, directed through a converting facility, namely, coating machine 30, and is then guided directly into printing machine 8.
Referring now to FIG. 3a, a logic diagram is illustrated. A roll cutting and winding facility 39 is disposed at the exit of a paper machine 38. The web of base paper, which has the same width as the paper machine, is cut into narrower webs in the roll cutting and winding facility. The cut narrower webs are then wound into individual rolls. These rolls, which have a lesser width than the base paper, are packaged in a packaging station 40. A dashed line 41 schematically represents the border between a paper factory 42 and a printing plant 43, which can be at any distance from one another. In the printing plant 43, the web is unwound in an unwinding station 31, directed through a coating machine 30 and a calender 4, and is directed to a printing machine 8, without any kind of intermediate winding. In this case, web 32 undergoes the effects of a coating machine 30, and then directly undergoes the effects of a calender 4.
Printing machines other than the illustrated eight-color gravure, web-fed rotary press can be used. For example, printing machines that work by means of high-pressure or planographic printing can be used. Additionally, calenders other than the illustrated seven roller gap calender 4 can be used. For example, a calender having a stack that is comprised of a greater number of rollers, or a calender with a smaller number of rollers can be used. Thus, for example, a soft calender that has one roller gap or two roller gaps connected one after the other could be used without departing from the spirit of the present invention.
Having described the presently preferred exemplary embodiment of a process for converting and printing on webs, and a printing machine for carrying out this process in accordance with the present invention, it is believed that other modifications, variations and changes will be suggested to those skilled in the art in view of the teachings set forth herein. It is, therefore, to be understood that all such modifications, variations, and changes are believed to fall within the scope of the present invention as defined by the appended claims.
|
A process of converting and printing on paper webs includes converting the running web by coating and/or calendering the web. Printing of the web occurs directly after the converting step. Thus, the converted web is not wound into a roll between the converting step and the printing step. A facility for converting the web of paper is placed in front of the entrance to a printing machine. The pass-through speed of the converting facility matches that of the printing machine.
| 3
|
CROSS-REFERENCE TO RELATED APPLICATION
The present application claims the benefit of European Patent Application No. 09160445.4, filed May 15, 2009, entitled Fixation Clamp, the disclosure of which is hereby incorporated herein by reference.
BACKGROUND OF THE INVENTION
The present invention relates to a fixation clamp and, more particularly, to a fixation clamp for use in an external fixation system for holding bone fragments adjacent to each other.
External fixation systems are widely used to connect two or more bone fragments to each other. Such systems comprise bone screws, pins, wires which are inserted directly into the bone material and these systems use external structural elements as fixation rods, bars and rings. In order to connect the rods and bars to form a rigid frame, fixation clamps are used. Furthermore, fixation clamps are used to connect this screws and pins to the rigid frame to specifically hold bone fragments at an intended place.
One adjustable fixation clamp is known from U.S. Pat. Nos. 5,752,954 and 6,080,153, the disclosures of which are incorporated herein by reference, comprising two pairs of jaws allowing clamping of a rod as well as of a pin.
A clamp for multiple rod-shaped elements is known from U.S. Pat. No. 7,618,417, the disclosure of which is incorporated herein by reference, having one single pair of jaws. However, such a clamp allows clamping more than two, e.g. three or four rod-shaped elements such as pins with one single clamp, thus reducing the number of clamps. However, one further fixation clamp is necessary to fix the rod of said clamp to the frame of the fixation system.
U.S. Patent Publication No. 20060287652 discloses that the usual fixation clamps as e.g. known from U.S. Pat. No. 6,080,153 allow clamping of one single screw or pin to the frame and that this way to attach pins or rods leads to bulky fixation systems. Therefore U.S. Patent Publication No. 20060287652 discloses a fixation clamp addressing this problem and comprises two pairs of jaws within which each pair of jaws allows the introduction and clamping of two rods or pins etc. at the same time.
These clamps according to the prior art either provide different diameters of the reception cavities, such as grooves, provided by the jaws to introduce different sizes of rods, pins or wires, or they rely on additional inserts as e.g. disclosed in U.S. Patent Publication No. 20080065068. Such inserts reduce the diameter of the reception cavities to allow a secure fixing of differently sized rods, pins or wires.
BRIEF SUMMARY OF THE INVENTION
Solutions according to the prior art providing different diameter reception cavities necessitate provision of either a variety of different clamps or additional inserts.
It is one aspect of the invention to overcome this problem and to provide the practitioner with a fixation clamp, especially for use in an external fixation system, which clamp can directly be used with a variety of differently sized rods, pins, screws and wires.
A fixation clamp for use in an external fixation system for holding bone fragments adjacent to each other with the help of fixation elements includes at least one clamping assembly, and a central locking shaft extending through the one or more clamping assemblies for blocking the position of the clamping assemblies in a defined angular position; wherein each clamping assembly comprises two jaws, wherein each jaw comprises three grooves. The longitudinal axis of each groove is perpendicular to the locking shaft. One groove of one jaw corresponds to one groove of the other jaw to form a cavity to accommodate a bone fixation element. The longitudinal axes of the grooves may span a triangle, and wherein at least two grooves have a different size adapted to accommodate a correspondingly sized fixation element. The fixation clamp groove may have a different size. The fixation clamp for use in an external fixation system for holding bone fragments adjacent to each other with the help of fixation elements also may include at least one clamping assembly having jaws mounted on a locking shaft, each jaw having four grooves forming a cavity to accommodate a bone fixation element along the longitudinal axis of the groove. The longitudinal axes of these grooves form a quadrilateral. At least two grooves have a different size adapted to accommodate a correspondingly sized fixation element. Each groove of the fixation clamp has a different size wherein two opposite grooves have the same size. The fixation clamp for use in an external fixation system for holding bone fragments adjacent to each other with the help of fixation elements may have at least one clamping assembly including at least one pair of jaws mounted on a locking shaft having five grooves to accommodate a bone fixation element along the longitudinal axis of the grooves. The longitudinal axes of the grooves form a pentagon, and in that at least two grooves have a different size adapted to form a cavity to accommodate a correspondingly sized fixation element. Each groove set forms a different size cavity. The grooves of all clamping elements may be circular or triangular in crossection and may comprise longitudinal ribs. Each clamping assembly preferably comprises an anti-rotation pin extending from a first jaw into a complementary recess in an opposite jaw. The grooves may be provided within outer side walls of each jaw in a way that the surface of a fixation element pointing away from the locking shaft when inserted into one groove is flush with the corresponding side wall.
A fixation clamp for use in an external fixation system for holding bone fragments adjacent to each other with the help of fixation elements includes a first and a second jaw member. A central locking shaft extends through the first and second jaw members wherein each jaw member comprises at least three grooves. The longitudinal axis of each groove lies in a plane perpendicular to a longitudinal axis of the locking shaft. One groove of the first jaw member corresponds to one groove of the second jaw member to form a cavity to accommodate a bone fixation element. The longitudinal axes of the grooves are all non-parallel in the plane. The first and second jaw members have a face parallel to the plane containing the longitudinal axis of the at least three grooves. An anti-rotation pin extends perpendicular to the plane of the face of the first jaw extends into a bore in the planar face of the second jaw member. The pin and bore are located within a geometric shape formed by the grooves. The fixation clamp for use in an external fixation system for holding bone fragments adjacent to each other with the help of fixation elements may have first and second jaw members having four grooves to accommodate a fixation element along the longitudinal axis of the groove wherein the longitudinal axes of said grooves form a quadrilateral. At least two grooves have a different size adapted to accommodate a correspondingly sized fixation element.
The fixation clamp for use in an external fixation system for holding bone fragments adjacent to each other with the help of fixation elements may include first and second jaw members having five grooves to accommodate a fixation element along the longitudinal axis of the grooves. The longitudinal axes of the grooves form a pentagon, and in that at least two grooves have a different size adapted to form a cavity to accommodate a correspondingly sized fixation element.
The clamp according to the invention allows readily treating different types of fractures or connecting bones of different sizes to each other, since usually different pin diameters are required. The clamp provides a plurality of different couplings possibilities which is an advantage, avoiding mismatching of components, which can lead to insufficient connecting strength. The clamp according to the invention also allows for clicking in rods from the side. The clamp can be built based on the usual metallic components and can comprise non-magnetic and non conductive materials, which are safe for temporary exposition in a MRI scanner, and can furthermore comprise plastic or composite materials or have electrical insulating cover surfaces.
It is an advantage of the clamp according to the invention that after having clamped a bone screw with one clamping assembly, a practitioner attaching subsequently a rod of an external fixator to the other clamping assembly can check the robustness of the external fixator, and if the practitioner finds that the rod used is not stiff enough, one simply opens the other clamping assembly, removes the thinner rod, turns the other clamping assembly e.g. 60 degrees into one direction or the other around the longitudinal axis to align a larger reception cavity with the new thicker rod and replaces said rod. This change does not necessitate the replacement of the clamp itself and is thus faster and more reliable since the clamping of the bone screw is not changed, and the use of a second sterile clamp at said time is avoided.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiments of the invention are described in the following description with reference to the drawings, which are provided for the purpose of illustrating the present preferred embodiments of the invention and not for the purpose of limiting the same. In the drawings,
FIG. 1 is an exploded view of a first embodiment of the clamp of the present invention;
FIG. 2 is a top view of the clamp according to FIG. 1 ;
FIG. 3 is a first side view of the assembled clamp of FIG. 1 ;
FIG. 4 is a second side view of the assembled clamp of FIG. 1 from a different direction than FIG. 3 ;
FIG. 5 is a top view of an inner jaw portion of the clamp according to FIG. 1 ;
FIG. 6 is a top view of an outer jaw portion of the clamp according to FIG. 1 ;
FIG. 7 is a cross-section of the clamp shown in FIG. 4 ;
FIG. 8 is an exploded view of a second embodiment of the clamp of the present invention;
FIG. 9 is a top view of the clamp shown in FIG. 8 ;
FIG. 10 is a cross-section of the clamp of FIG. 8 along line X-X of FIG. 9 ;
FIG. 11 is a top view of the clamp of the present invention with two attached fixation elements;
FIG. 12 is a front view of the clamp with two attached fixation elements according to FIG. 11 ; and
FIG. 13 is a right side view of the clamp of FIG. 11 with two attached fixation elements.
DETAILED DESCRIPTION
Referring to FIG. 1 there is shown a perspective exploded view of a preferred first embodiment of a clamp 10 pursuant to the invention. The clamp 10 consists of a first clamping assembly 20 and a second clamping assembly 30 and a shaft 40 which is positioned through bores 21 , 31 within the two clamp assemblies 20 , 30 along the longitudinal axis of shaft 40 . Each clamping assembly has a first jaw 11 and a second jaw 12 . Shaft 40 is preferably a locking element adapted to allow the closing the clamp assemblies 20 and 30 . Shaft 40 enters a first jaw 11 through a washer 41 . Washer 41 may have a part-spherical shape for receipt on a part-spherical surface of bore 21 . The shaft 40 comprises a proximal portion 42 and a reduced diameter portion 43 which is followed by a threaded portion 49 . The outer threaded portion 49 is adapted to be screwed into a complementary inner thread which may be formed within the distal most jaw 11 (bottom jaw of FIG. 1 ) so that turning the head of the shaft 40 changes the longitudinal position of the shaft 40 against the bottom jaw 11 . This allows for opening or closing the entire clamp 10 against the force of a spring 15 provided between the two clamp assemblies 20 and 30 . Obviously a separate nut could be provided rather than threading the bore in lowermost jaw 11 of FIG. 1 . Spring 15 is preferably positioned in corresponding reception cavities in jaws 12 . Instead of a spring 15 , provided around shaft 40 , it is possible to provide a different spring means as Belleville washers or an elastic compressible solid or foam. Upon closing of the clamp assemblies 20 and 30 the jaws 12 adjacent spring 15 can eventually come into contact and then the anti-rotation surface 44 which is provided in both surfaces of the jaws, fixes the angular orientation of each clamping assembly 20 and 30 against each other.
Preferably after having mounted the shaft 40 with the thread 49 within the bottom jaw 11 , the end portion of the thread 49 is deformed or destroyed through pressure to ensure that the shaft 40 cannot be removed from the clamping assemblies 20 , 30 to maintain the clamp as one single piece.
As discussed above, each clamping assembly 20 or 30 comprises two opposing clamping jaws 11 and 12 . These jaws 11 and 12 are essentially similarly shaped on the sides facing each other except for a pin 13 which extends into a corresponding bore 14 in clamping jaw 12 . This pin-bore connection which is oriented along or parallel to the longitudinal axis of the clamping device is an anti-rotation device for jaws 11 and 12 . Once engaged jaws 11 , 12 cannot change their mutual angular orientation. The plane surface of jaw 11 facing the plane surface of jaw 12 is provided with three spacers 17 arranged in the corners of the surface. The spacers 17 have a mostly triangular form and a height to allow the function of a counter bearing as explained below. Additionally, the spacers 17 result in the two plane surfaces of jaws 11 and 12 being spaced so that the open areas between these surfaces can be cleaned.
The jaws 11 and 12 are provided with three grooves 51 , 52 and 53 . Grooves 51 , 52 and 53 are all provided in a same plane perpendicular to the longitudinal axis of shaft 40 . In that plane they are oriented perpendicular to the radial direction from the center of the bore 21 or 31 . As such the grooves 51 , 52 and 53 are parallel to outer side wall 61 , 62 or 63 of each pair of triangularly shaped jaws 11 and 12 .
Each pair of grooves 51 , 52 or 53 , respectively, in each jaw 11 and 12 , define one reception cavity, i.e. a first reception cavity 71 , a second reception cavity 72 and a third reception cavity 73 . The grooves 51 , 52 and 53 are each formed as a rounded semi-spherical recess in section to provide reception cavities 71 , 72 and 73 which accommodate cylindrical pins or rods 100 with a defined diameter (see FIGS. 11 to 13 ), if the clamp is closed. The outer side walls 61 , 62 or 63 can comprise an inclined sliding surface to allow for easy clipping or snapping in of such pins or rods 100 into the corresponding cavities. The grooves 51 , 52 , 53 are formed as rounded semi-spherical recesses in a section. This means that the recesses provided by the grooves 51 , 52 , 53 have a hollow cylindrical shape to accommodate rod-shaped elements.
All three grooves 51 , 52 and 53 have different sizes so that the corresponding reception cavities 71 , 72 and 73 have three different sizes. In other words each reception cavities 71 , 72 or 73 is adapted to accept a different fixation element, i.e. a rod, screw, pin or wire having a different diameter. One preferred embodiment of the first clamping assembly 20 has grooves to accept fixation elements having a diameter of 12 mm, 8 mm and 5 mm, respectively. A different embodiment may have a sequence of diameters of 8 mm, 6 mm and 4 mm, respectively.
The second clamping assembly 30 according to the embodiment of FIG. 1 also comprises two jaw portions 11 and 12 and these comprise three grooves 51 , 52 , 53 . These grooves 51 , 52 , 53 also comprise a sequence of different sizes. In the embodiment shown the inner jaws portion 12 have an identical structure as have the outer jaws 11 , especially in view of the anti-rotation device 44 , the second bore for a spring 15 as well as ribs 45 inside the grooves 51 , 52 , and 53 .
Within a preferred embodiment the first clamping assembly 20 may comprise a sequence of smaller size cavities, e.g. 7 mm, 5 mm and 3 mm; or 6 mm, 5 mm and 4 mm; and the second clamping assembly 30 may comprise a sequence of larger sizes, e.g. 13.5 mm, 12 mm and 10 mm. Different sizes are possible, usually for wires starting from 2 mm diameter up to thicker rods with a diameter of 30 mm are used within such a clamp 10 . Such a clamp 10 allows the use of one single versatile clamp, wherein the first clamping assembly 20 is used to fix a specific pin or screw or wire having a diameter for which one of the reception cavities 71 , 72 or 73 is adapted. The user takes the clamp 10 and orients or rotates the first clamping assembly 20 into the correct alignment so that the pin or screw can be clipped into the corresponding reception cavity.
Then the clamp 10 can be clamped on a rod of an external fixator with the help of the second clamping assembly 30 . The second clamping assembly 30 can be oriented in a way so that the rod can be clipped into the corresponding reception cavity. It is an advantage of the clamp 10 having two clamping assemblies 20 and 30 according to the invention, that a practitioner attaching such a clamp at a bone screw with one clamping assembly 20 and subsequently a rod of an external fixator to the other clamping assembly 30 can check the robustness of his external fixator, and if it is found that the rod used is not stiff enough, one simply opens the second clamping assembly 30 , removes the thinner rod, turns the second clamping assembly 30 e.g. 60 degrees in one direction or the other around the longitudinal axis, to align the larger reception cavity with the new thicker rod and replaces it. This change does not necessitate the replacement of the clamp 10 itself as necessary with prior art systems. The method to replace such a rod 100 is faster and more reliable since the clamping of the bone screw is not changed, and at the same time avoids use of a second sterile clamp.
It is of course also possible that the second clamping assembly 30 is a traditional clamping assembly or even any other element known in the prior art with clamping elements. The object of a versatile clamping assembly is already achieved through one first clamping assembly 20 , since it allows clamping one of three different sizes of screws, pins of wires through simple reorientation of the first clamping assembly 20 .
FIG. 2 shows a top view of the clamp according to FIG. 1 . Since the embodiment of FIG. 1 comprises three grooves 51 , 52 and 53 , there are three side walls 61 , 62 and 63 , which provide, when looked from above as in FIG. 2 a triangular shape of each clamping assembly 20 or 30 .
FIG. 3 shows a first side view of the clamp of FIG. 1 and FIG. 4 shows a second different side view of the clamp 10 of FIG. 1 from a different direction. Identical reference signs are used for identical features within the same embodiment and are used for identical or similar features in further embodiments.
It is clear from FIG. 3 that the first reception cavity 71 is identical in size and allows for insertion of a large rod. From FIG. 4 it can be seen that the third reception cavity 73 are small cavities, e.g. for a pin. In this embodiment, second cavities 72 have an intermediate size. From FIG. 4 it can be seen that the depicted embodiment has a decreasing size sequence of reception cavities 71 , 72 and 73 in the upper first clamping assembly 20 in clockwise direction whereas the depicted embodiment has a decreasing size sequence of the reception cavities 71 , 72 and 73 in the lower second clamping assembly 30 in counter-clockwise direction.
Referring to FIG. 5 there is shown a top view of an inner jaw portion 12 , whereas FIG. 6 shows a similar view on a corresponding outer jaw portion 11 . It is clear that each jaw portion 11 or 12 of any clamping assembly 20 , 30 according to the invention comprises three differently sized grooves 51 , 52 and 53 , respectively. The longitudinal axes of these grooves 51 , 52 and 53 are oriented in an angle of 60 degree one to another. However, these angles of 60 degree are not mandatory. It is only necessary that the total internal angle of the triangle provided by these three grooves 51 , 52 and 53 is 180 degrees. The grooves are also in the same median plane which indicates that only one pin, screw or rod can usually be introduced in one of the grooves 51 , 52 or 53 and such an introduction blocks the other empty grooves. It is an aim of this orientation to provide a simpler mounting of a fixation device, since based on the chosen pin or screw a clamp of the invention can be chosen and through rotation of the clamping assembly the correct sized reception cavities 71 , 72 or 73 is usable for a well clamped connection, wherein the clipping of the pin or screw from the open side further facilitates their introduction.
It is clear from FIGS. 5 and 6 that the grooves 51 , 52 and 53 mutually intersect. The inner jaw portion 12 shown in FIG. 5 comprises ribs 45 which are oriented in the longitudinal direction of the grooves 51 , 52 and 53 . Each groove is provided with two lines of ribs 45 , which are arranged one behind the other and thus can also be described to be a single line interrupted in the middle part. Of course there may be one or no ribs 45 , or there may be more than two lines, and these lines can be provided uninterrupted, although the embodiment with interrupted ribs 45 as well as two lines of these ribs 45 is preferred.
It is possible to deviate from the correct triangular orientation of the grooves; especially the angle between the largest groove 51 and the neighboring grooves can be less than 60 degree, so that the angle between the longitudinal axes of the grooves 52 and 53 is greater then 60 degrees.
It is also possible, in different embodiments, not shown in the figures, to provide four, five or more grooves. If four grooves are provided, then the form of such a clamping assembly 20 seen from above is a square and each jaw comprises four grooves joining in the corners in at preferably a right angle. Then a sequence of four sizes of the reception cavities is possible as 12 mm, 8 mm, 6 mm and 4 mm. If five grooves are provided, then the form of such a clamping assembly 20 seen from above is a pentagon and each jaw comprises five grooves joining in the corners, preferably at an angle of around 108 degrees. Then a sequence of five sizes of the reception cavities is possible as 12 mm, 20 mm, 8 mm, 6 mm and 4 mm. Of course deviations from such a symmetrical polygon are possible.
It is noted that the spacers 17 and thus the counter bearings as well as the corners of the jaw planes are not symmetrically positioned in view of the central bore 21 of a jaw. The deviation from the symmetric form is smaller for the largest reception cavity 71 and larger for the smallest reception cavity 73 . However, this is not problematic, since the largest reception cavity 71 with the smallest deviation accepts the largest rod and thus the largest forces, wherein the largest deviation occurs for the smallest reception cavity and the function of such a small reception cavity resides in accepting a limited force.
FIG. 7 shows a cross-section of the clamp according to FIG. 4 , wherein the clamp 10 is shown in a premounted state, i.e. the spring 15 is under tension. The upper jaw 11 of the first clamping assembly 20 is therefore pushing the rounded counter piece 41 against a flange 40 a of the head of shaft 40 . The jaw 11 has around its bore 21 a rounded part-spherical recess to accommodate the washer 41 . This enables a pivoting movement of the upper jaw 11 against the axis of the shaft 40 , since the shaft 40 comprises a reduced diameter portion 43 extending over the whole length of the jaws 11 and in both assemblies. It is also possible that there is no play between shaft 40 and jaw 11 ; the bore 21 just allows the introduction of the shaft 40 . Then jaw 11 and jaw 12 can only effect a translatory movement.
The pin 13 of the upper jaw 11 is lodged in a recess 16 in the bore 14 . It is possible but not necessary that the pin 13 or the recess 16 receives an elastic fitting piece allowing elastic movements of the pin within the recess 16 .
The shaft 40 as part of a locking element is threaded into the lower jaw 11 of the second clamping assembly 30 and is further connected with a counter nut 46 , which is fixedly lodged on shaft 40 . Therefore the two clamp assemblies 20 , 30 can be opened and closed through turning the head of shaft 40 and thus turning shaft 40 with the blocking counter nut 46 and in the jaw thread. The counter nut 46 can then be used to lock shaft 40 from further rotation
The combination of shaft 40 and counter nut 46 can also be replaced by a single screw to be screwed into the lower jaw 11 of the second clamping assembly 30 . Threading may be provided in the bore or the screw may exhibit self-tapping threading. Quite generally, a locking element may be provided which may be a lever locking element or a bayonet lock. Among these locking elements may also be supporting disks or toothed disks, which, for the sake of simplicity, are not shown in the drawings.
FIG. 8 shows an exploded view of a second embodiment of a clamp 10 a of the present invention; FIG. 9 shows a top view of the clamp and FIG. 10 shows a cross-section of the clamp along line X-X in FIG. 9 . The sequence of sizes for the first clamping assembly 20 a is 13.5 mm, 8 mm and 5 mm. The choice of this sequence depends on the intended application (e.g. which limb is to be treated) of the external fixator set and follows the needs of the application.
The clamping assemblies 20 a , 30 a of the embodiment have a triangular form, as can be seen from FIG. 9 , having defined straight side walls 61 , 62 and 63 and identically curved transitory portions. For a description of features which are identical to the clamp of FIG. 1 reference is made to that description.
Instead of spacers 17 in the corners of the plane surface of the jaws 11 a there are provided two flattened semi-spherical spacers 27 on the surface. As mentioned above, the first clamping assembly 20 a comprises a sequence of larger sized reception cavities 71 , 72 , 73 . The lower second clamping assembly 30 comprises a different sequence of smaller sized reception cavities 71 , 72 , 73 . The corresponding grooves 51 , 52 and 53 within the lower jaw 11 a are not semi-spherical as with the clamp of FIG. 1 but are triangular or v-shaped grooves 51 , 52 , 53 having a bottom line 54 of a v-shaped groove. The corresponding groove portion in the opposite jaw 12 a is a rounded groove, in FIG. 10 receiving the numeral 55 , so that slightly different sizes of elements can be clamped. However, the sizes of the grooves 51 , 52 and 53 are nevertheless different one from the other.
Usually the rounded grooves are intended to be used especially with carbon rods and allow high precision clamping under all circumstances, whereas the triangular grooves are more flexible. They usually provide two sizes with one groove, e.g. 4-5 mm, 5-6 mm and 7-8 mm for three grooves.
Element 47 is a steel helicoil inserted into an aluminum jaw 11 a to provide a better counter thread for the thread 49 of shaft 40 . The end portion 49 of shaft 40 is hollow with an additional inner thread to accommodate the outer thread 58 of a counter nut 48 .
FIG. 11 shows a top view of the clamp 10 a of the present invention with two attached fixation elements 100 and 101 . FIG. 12 shows a front view of the clamp according to FIG. 11 ; and FIG. 13 shows a view from the right.
The fixation elements shown here are small-sized rods. Fixation element 100 is introduced in the smallest size reception cavity 73 of the first clamping assembly 20 leaving the middle-sized reception cavity 72 and the large-size reception cavity 71 empty. From FIG. 12 it can be seen that the introduction of rod 100 blocks the section of reception cavity 72 . From FIG. 13 it can be seen that the introduction of rod 100 also blocks the section of reception cavity 73 . Therefore a clamping assembly 20 is usable for one single rod or pin at the same time, here rod 100 .
The same is true for rod 101 used in connection with the second clamping assembly 30 a . In this embodiment, the two clamping assemblies have an identical sequence of reception cavity sizes, i.e. there are three sizes of reception cavities twice in the clamp 10 a . As mentioned above it is possible to provide different reception cavity sizes in the two clamping assemblies 20 , 20 a and 30 , 30 a . Therefore it is possible to have up to six different sizes of reception cavities within one clamp consisting of two clamping assemblies according to the invention, e.g. 3 mm, 4 mm, 5 mm, 6 mm, 8 mm, and 10 mm. It has to be noted that the sequence is not necessarily distributed according to size. One clamping assembly can have sizes 3 mm, 5 mm and 8 mm, whereas the complementary assembly has the sizes 4 mm, 6 mm and 10 mm, showing a mixed sequence.
It is also possible to use two rods 100 and 101 with one single clamping assembly 20 , 20 a , if the rods are shorter so that the rods 100 , 101 cannot intersect behind the clamp 10 . This allows providing a so-called Y-frame with one single clamping assembly, wherein the two rods or bone screws are oriented within an angle of 60 degrees.
It is noted that the grooves 51 , 52 and 53 are preferably provided at a distance from the center of the clamp 10 so that the rods, pins or screws which are to be inserted in the created reception cavities are flush with the side walls 61 , 62 or 63 as it can be seen in FIG. 11 .
The single clamping assemblies 20 , 20 a or 30 , 30 a can be combined in different ways. If a clamping assembly having round grooves is called a rod clamping assembly and a clamping assembly having triangular grooves is called a pin clamping assembly then several clamps having two single clamping assemblies 20 , 20 a or 30 . 30 a are possible, i.e. pin-pin, rod-pin or rod-rod.
The clamp or articulation element according to the invention has at least two opposing first and second clamping jaws 11 , 11 a and 12 , 12 a , providing one lateral open free space for laterally receiving a rod-shaped element 100 . The lateral open free space is formed through grooves and is in the form of an open slot. It is also possible to accommodate inserts, i.e. a jacket element adapted to be inserted in one jaw of the clamp to modify the space available for the rod-shaped element. Such an insert can be built according to e.g. U.S. Patent Publication No. 20080065068 and introduced into the reception cavities to have additional versatility. On the other side it is also possible that a triangular clamp 10 , 10 a according to the invention comprises a clamping assembly 20 , 20 a or 30 , 30 a having two identical grooves within the three grooves. This is especially true, if according to a different embodiment, four, five or more grooves are provided.
For four grooves it is possible to combine the advantage of using two sizes of reception cavities which are provided one opposite to the other. Then—in clockwise direction—the four cavities may be: small, large, small, large; which allows the parallel introduction and fixation of two small pins or two large rods, since the square disposition do not hinder the simultaneous introduction of two pins or rods. The same is true, if five grooves/reception cavities are provided, since an angle of around 108 degrees, two out of the five reception cavities can be used.
Within a preferred embodiment it is contemplated that at least the lower jaw 11 , 11 a of the second assembly 30 , 30 a has a different color then the other jaws to indicate that there is a specific sequence of sizes. It is e.g. possible that said lower jaw is green, indicating that said clamping assembly 30 , 30 a provides a sequence of larger reception cavities (13.5 mm, 10 mm, 8 mm) whereas the other clamping assembly 20 , 20 a provide smaller reception cavities (e.g. 6 mm, 5 mm and 4 mm). It is also possible to provide the upper most jaw 11 , 11 a of the first clamping assembly 20 , 20 a with a different color, e.g. blue to indicate that said clamping assembly 20 provides the smaller reception cavities. Then of course, blue-blue, blue-green and green-green combinations of clamps 10 , 10 a would provide a high usability of use with direct indication for the user, which clamp he should choose. This color model can be extended to a third of fourth color according to the above mentioned sequences of reception cavity sizes.
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 fixation clamp for use in an external fixation system for holding bone fragments adjacent to each other with the help of fixation elements has at least one clamping assembly having a pair of jaws with at least two different size grooves to accommodate a bone fixation element such as a pin or rod. An alternate clamping assembly has at least three grooves wherein at least two of the grooves have a different size adapted to accommodate a correspondingly sized bone fixation element such as a bone pin. The longitudinal axes of the grooves define a polygon. The jaw pairs can be rotated about a central longitudinal axis to present different size reception cavities towards the pins or rocks depending on their diameter.
| 5
|
BACKGROUND AND SUMMARY
The present invention relates to a method of composite casting of a one-piece cast tool which comprises at least a first portion which comprises the working component of the tool and which is manufactured from steel, and a second portion which comprises the body component of the tool and which consists of or comprises grey iron, there being formed an interconnection zone between the steel and the grey iron.
In the production of tools for sheet metal working, for example cutting, hole making, bending or other shaping, previous practice has generally been to separately produce a tool body by casting of grey iron. The cast tool body has often required heat treatment and thereafter machining in order to create the requisite seats, holes for guide stub shafts, bolt holes etc., so that securing is made possible of working components, for example steel cutters, for carrying out the working operations proper for which the tool is intended. These working components have been manufactured from steel and the point of departure has often been bar material, the working components having been machined to the correct configuration, provided with apertures for guide stub shafts, fixing bolts and the like. This has been often followed by heat treatment, whereafter additional machining, for example grinding, has been carried out.
To produce a tool in the above-outlined manner is extremely time-consuming and expensive, and is often therefore determinative of the time consumption that is required for the new production of different sheet metal products.
WO 03/041895 discloses a one-piece cast composite tool which consists of two different material qualities, as well as a method of manufacturing such a tool.
According to the prior art technology, two different material qualities are cast in one and the same mould, steel being cast for forming working components in the tool, while grey iron has been cast for producing the tool body proper. Between the two material qualities, an interconnection zone is formed where, to some degree, mixing of the two material qualities may take place. The prior art technology suffers from numerous problems since it does not offer any possibility of positioning the interconnection zone in the tool in such a manner that the mechanical strength of the interconnection zone can be optimised.
In order for the interconnection zone to achieve the requisite quality, careful and accurate control is required of the temperature of the material which is cast first, before casting can take place of the material which is cast last. The prior art technology offers no such possibilities.
Finally, the prior art technology otters no possibility of orienting, in a suitable manner, the interconnection zone in a mould for producing the tool.
It is desirable to design the method intimated by way of introduction so that it obviates the drawbacks inherent in the prior art technology. In particular, it is desirable to design the method according to the invention so that the position of the interconnection zone may be optimised in view of mechanical strength aspects. It is also desirable to design the method according to the invention so that a superior control of the temperature conditions in and at the interconnection zone is created on casting of the last cast material. It is also desirable to design the method according to the invention in such a manner that the orientation of the interconnection zone in a mould may readily be controlled.
According to an aspect of the present invention, a method is characterised in that the casting process is carried out in a single mould which is kept unchanged and closed throughout the entire casting process, that the steel is cast first and in a direction from beneath and upwards, that after the casting of the steel a pause is made, and that the casting of the grey iron is carried out only when the temperature of the steel in the intended interconnection zone has fallen to a first temperature corresponding to the liquidus temperature of the steel minus approx. 30° to 150° C.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
The present invention will now be described in greater detail hereinbelow, with reference to the accompanying Drawings. In the accompanying Drawings:
FIG. 1 is a schematic cross section through a mould for reducing the method according to the present invention into practice;
FIG. 2 is a schematic cross section of a modified embodiment of a mould for reducing the method according to the present invention into practice;
FIG. 3 is a detailed section through a mould for applying the method according to the present invention;
FIG. 4 shows a tool cast according to the method according to the present invention, seen in perspective obliquely from beneath, compared with the position during the casting process;
FIG. 5 is an alternative view corresponding to that of FIG. 4 ; and
FIG. 6 is a top plan view of a tool cast according to the present invention.
DETAILED DESCRIPTION
Referring to the Drawings, in FIG. 1 , reference numeral 1 relates to a substrate on which rests a mould 2 for reducing the present invention into practice. The substrate 1 is preferably a horizontal floor. If no such floor is available, some equalisation platform or the like must be placed on the substrate so that its upper surface will be horizontal and the mould thus rests on a horizontal substrate.
The moulding consists of or comprises a moulding box or flask 3 , which encloses in itself a first model section 4 and a second model section 5 . In such instance, the first model section 4 is designed for casting of the working component of the tool by casting of steel. It should be emphasised already at this stage that the tool may very well have more than one working component and thus the mould may have several first model sections 4 .
Above the first model section 4 , there is disposed a second model section 5 which is intended for the casting of grey iron, so that a tool body is formed. The second model section may, in the conventional manner, be provided with mould cores so that cavities 6 are formed in the tool body cast from grey iron. In addition, the mould box 3 is, in the conventional manner, filled with foundry or moulding sand 7 which has tamped, packed and set.
Both of the model sections 4 and 5 have a planar contact surface where they are in contact with one another, or where they are united. This contact surface 8 is the desired position of the interconnection zone which is formed in the interface region between the steel which is cast in the first model section 4 and the grey iron which is cast in the second model section 5 . The contact surface 8 is parallel with the lower edge 9 of the moulding box 3 so that the contact surface 8 will be horizontal when the moulding box rests on a horizontal substrate.
In the production of the mould according to FIG. 1 , an upper portion 12 of the moulding box is first removed and the moulding box 3 is placed on a planar, horizontal substrate with its upper edge turned to face downwards. Thereafter, the total model, which hence consists of or comprises two or more first sections 4 and one second section 5 is placed on a substrate 1 on which the upper edge of the moulding box 3 rests. This presupposes however that the contact plane 8 is parallel with the upper surface of the second model section 5 . The important feature is that the contact plane 8 will be horizontal in the casting position of the mould, in the mould illustrated in FIG. 1 , parallel with the lower edge 9 of the moulding box.
It may be appropriate to join together the second model section 5 with the first model section or sections 4 , so that they together form a manageable unit.
Thereafter, the moulding box 3 is filled with foundry or moulding sand of suitable quality, and it should here be emphasised that this moulding sand need not be of the same quality around the second model section 5 and around the first model section or sections 4 . When the moulding box 3 has been filled in this manner with moulding sand and the sand has been tamped, packed and permitted to set, the moulding box 3 is inverted to the moulding position, it being ensured that the contact plane 8 is horizontal in that the substrate on which the moulding box is placed is also horizontal. Thereafter, the upper portion 12 is placed on the moulding box 3 and the mould is completed with the ingates 10 and 11 .
If the second section 5 of the model were not to have its upper side 5 (according to FIG. 1 ) parallel with the contact plane 8 , the second model section 5 must be chocked up to a correct inclination which compensates for the non-parallelism between the contact plane 8 and the upper surface, so that thereby, in the finished mould 2 , the contact plane 8 will always be horizontal when the moulding box 3 is on a horizontal substrate.
In FIG. 1 , reference numeral 10 relates, as was intimated above, to an ingate for the steel which is to be cast in the first model section 4 . While not being apparent from FIG. 1 , the ingate system that is employed for casting of the steel is formed in such a manner that it at least partly extends in under the first model section 4 and connects to it in order to give a casting direction for the steel from beneath and upwards towards the contact surface 8 , which represents the desired position of the interconnection zone which is to be formed between the two different material qualities.
The design of the ingate system for the grey iron may be made in a conventional manner. In order to close the mould box 3 upwardly and accommodate parts of the ingate systems, there is provided an upper portion 12 above the moulding box 3 which includes moulding or foundry sand 7 .
Both of the model sections 4 and 5 , which are included in the total mould model in FIG. 1 , are destructible models on casting, for example produced from expanded polystyrene. In a conventional manner they are also provided with blacking to improve the surface finish on the cast material.
FIG. 2 shows an alternative embodiment of a mould 2 for reducing the present invention into practice. The reference numerals in this Figure correspond to the reference numerals in FIG. 1 , but it will be clearly apparent that both of the model sections 4 and 5 have completely different appearances. Also in the embodiment according to FIG. 2 , there may occur a plurality of first model sections 4 , which are connected either directly to the ingate system 10 or indirectly via communications between the different first model sections.
It will be apparent from both FIG. 1 and FIG. 2 that, on casting of the steel in the first model section or sections 4 , these will be destroyed by the steel melt, since the model sections are produced from expanded polystyrene. However, this also applies to a part of the second model section 5 , at least in the area straight above the first model section 4 . This implies that, after the casting of the steel, those portions of the foundry sand that are exposed downwards towards the first model section or sections 4 will be exposed to an extremely powerful thermal radiation which possibly could break down the binder in the foundry sand. For this reason, the second model section 5 , at least on those parts which are exposed to this thermal radiation, are provided with extra protection in the form or one or more extra layers of blacking.
Regardless of whether the mould 2 has the appearance as illustrated in FIG. 1 or FIG. 2 , the steel is always cast first at a temperature of the order of magnitude or 1550° C. Once the steel casting has been completed and the upper surface of the steel has reached the level of the contact surface 8 , a pause is made in the casting process, so that the cast steel is permitted to cool. In such instance, it has been ensured that the steel cools last in the region of the contact surface or plane 8 in that the first model section has been given a form which entails that, to some degree, it tapers downwards (according to FIGS. 1 and 2 ) in a direction away from the contact surface or plane 8 . As a result, a directed cooling will be obtained, where the cooling first takes place in the lower parts of the first model section 4 and last in the region at the contact surface or plane 8 .
At the contact surface 8 , parts of the first and the second model sections 4 and 5 , respectively, have been given uniform thickness throughout their entire length (the length in the direction from left to right in FIGS. 1 and 2 ). The uniform thickness implies that the temperature distribution throughout the entire contact surface 8 where the model sections meet one another, will relatively uniform, which is an important precondition for good quality in the interconnection zone. In actual fact, it is the case that, by computer simulation, the parts 16 , 17 of the two model sections, lying in the proximity of the contact surface, are formed in such a manner that the steel cast in the lower model section will have as uniform a temperature distribution at the contact surface 8 as is humanly possible to achieve. In the same manner, by means of a computer simulation, a calculation is made of the time that is needed for achieving a temperature in the steel cast in the first model section 4 at the contact surface 8 , a first temperature corresponding to the liquidus temperature of the selected steel quality minus approx. 30° to 150° C., often in the region of 1440° to 1320° C.
This pause or stay time in the casting process may amount to one or a few minutes, but it may also be as long as between 15 and 20 minutes, depending overall on the size of the first model section or sections 4 .
The casting of the grey iron is carried out when the computed pause or stay time has elapsed at a second temperature, which corresponds to the liquidus temperature of the grey iron plus approx. 100° to 150° C., often approx. 1320° C.
At the interconnection zone, if the casting of the grey iron takes place at an elevated first temperature, i.e. at or above the upper end of the exemplified temperature range of approx. 1440° to 1320° C., a certain intermixing of the two materials may occur at the same time as a diffusion process occurs, where parts of the one material migrate into the other and vice versa. If, on the other hand, the casting takes place at a low first temperature, i.e. at or below the lower end of the exemplified temperature range, a diffusion process still occurs, which implies that the interconnection zone will also have a certain intermixing of the two materials, and still a thickness of at least a millimeter or so, but preferably slightly more, possibly up to 2.5-3.0 mm.
In practical strength trials which have been conducted, no breakage, either in tensile or bending tests, has occurred in the interconnection zone proper, but always occurred in the grey iron.
As was mentioned above, the contact surface 8 , i.e. the theoretical position of the interconnection zone in the vertical direction, is horizontal. Since the interconnection zone is defined by the upper, free surface of the steel melt, it will readily be perceived that this will planar and also horizontal.
There are certain problems in accurately computing the quantity of steel melt which is to be cast in the mould 2 . For this reason, the mould has been provided with one or more accommodation spaces 13 to which any possible surplus of steel will be permitted to run so that, thereby, the level of the cast steel will always be at the contact surface 8 . FIG. 3 shows in cross section a detail through a mould, where such an accommodation space 13 is provided. The accommodation space 13 is connected via a duct 14 to the mould cavity of the mould in the region of the contact surface 8 . The duct 14 has a lower wall 15 which, in the mould cavity, discharges on the level of the contact surface 8 . The cross-sectional area of the duct 14 is so large that it exceeds the total cross sectional area of the ingate system for steel, preferably by at least a factor of 1.5. It will also be apparent from FIG. 3 that the lower duct wall 15 slants from the contact surface 8 in a downward direction towards the accommodation space 13 .
Depending on the form, size and the number of the first model sections 4 , a plurality of different accommodation spaces 13 may be employed. In such instance, one accommodation space may directly or indirectly, via ducts, serve two or more first model sections 4 , but the reverse is also possible.
In order to give the interconnection zone the correct formation, i.e. uniform width throughout its entire extent, the first model section 4 has an upper region 16 which forms a uniformly thick wall or projection, which is directed in the vertical direction in the mould 2 and which extends up towards the second model section 5 . Correspondingly, the second model section 5 has a uniformly thick wall 17 or projection which extends downwards in a direction towards the first model section 4 . The interconnection zone is placed between both of these wall portions 16 and 17 displaying substantially constant cross-sectional area in the region of the interconnection zone, i.e. the contact surface 8 . Further, the lower end surface (in FIGS. 1 and 2 ) of the upper wall 17 abuts against the upper end surface of the lower wall 16 and further these end surfaces coincide substantially as regards size and configuration.
FIG. 4 shows (in a position inverted in relation to the position during casting) in perspective a tool cast according to the invention, and it will be apparent that this has a steel portion 18 which is cast in the first model section 4 , and a grey iron portion 19 which is cast in the second model section 5 . The Figure also shows an accommodation space 13 and two ducts 14 , by means of which it is connected to the first model section 4 (the steel portion 18 ).
That steel which may possibly arrive in the accommodation space or spaces 13 disposed in the mould is removed gradually, according as the casting of the complete tool proceeds.
FIG. 5 shows (in a position inverted in relation to the position during casting) in perspective a tool cast according to the present invention. It will be clearly apparent that the grey iron portion 19 has a wall 17 upwardly directed towards the steel portion 18 , the wall being of uniform thickness throughout its entire extent. Correspondingly, it will be apparent that the steel portion 18 has a wall 16 directed towards the grey iron portion 19 and having the same size and extent as the wall 17 .
FIG. 6 shows a further embodiment of a composite tool cast according to the present invention, which is shown in the same position as it has on casting in the mould. It will be apparent that the contact surface 8 , i.e. the interconnection zone in the finished tool, is horizontal. It will further be clearly apparent from the Figure that the grey iron portion 19 of the tool has a downwardly directed wall 17 which has its counterpart in an upwardly directed wall 16 on the steel portion 18 of the tool. Also in this embodiment, there is a number of cutting edges 20 on the steel portion.
As was mentioned above, the steel is cast from beneath and upwards as first component before the grey iron is cast. Since the model 4 , 5 is produced from expanded polystyrene, this will be destroyed, be vaporised and combust already during the casting of the steel. This implies quite a voluminous development of gas which would have as a consequence an uncontrolled and rapid gas outflow and combustion of the gases in the ingate 11 to the grey iron portion. In order to realise a better controlled casting process for the steel, but above all for reasons of working environment health, the ingate 11 to the grey iron is kept blocked while the steel is cast, so that the gases thus generated are forced to depart via other routes, for example via a ventilation system or quite simply through the foundry sand in the moulding box.
|
A method of one-piece casting of a tool with a working component of steel and a body of grey iron, and an interconnection zone therebetween is carried out in a single mold which is kept closed and unchanged during the casting. The steel is cast first from beneath and upwards, whereafter a pause is made. The casting of the grey iron is only carried out when the temperature of the steel in the intended interconnection zone has fallen to a temperature corresponding to the liquidus temperature of the steel minus approx. 30° to 150° C.
| 1
|
CROSS REFERENCE TO RELATED APPLICATION
This application is based upon and claims the benefit of priority from the prior Japanese Patent Application No. 2005-164603, filed on Jun. 3, 2005, the entire contents of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an image measuring method, image measuring system and image measuring program, having a non-stop measurement mode for image measurement, in which an imaging means moves relative to a measurement target supported on a measurement stage and captures instantaneous image information at designated measurement positions without making a stop.
2. Description of the Related Art
A conventional CNC image measuring machine comprises a measurement stage, which is moved relative to an imaging means such as a CCD camera and stopped at a measurement position as shown in FIG. 8 . Then, the amount of illuminating light is adjusted to acquire image information about a measurement target. To the acquired image information, image processing such as setting of a measuring tool and edge detection is applied, thereby executing a measurement at one measurement position. This measurement is repeated as Measurement 1 , Measurement 2 , . . . and so on for all measurement positions to achieve measurements at required positions (hereinafter, such the measurement mode is referred to as a “standard measurement mode”).
In contrast, for the purpose of improving the throughput of measurement, a measurement may be performed without making a stop of the measurement stage relative to the imaging means even at a measurement position in a measurement mode (hereinafter, such the measurement mode is referred to as a “non-stop measurement mode”). An image measuring machine having such the non-stop measurement mode has been proposed (see JP-A 2004-535587, paragraphs 0005-0006, FIG. 2). This image measuring machine irradiates the measurement target with strobe illumination, as shown in FIG. 9 , without making a stop of the measurement stage at measurement positions. Alternatively, it captures instantaneous image information imaged using a shuttered CCD camera, for image measurement. In the image measuring machine, the CCD camera is roughly positioned in a measurement region at high speeds and then decelerated to capture images within a predetermined constant speed region.
The above-described conventional image measuring machine has no problem if multiple positions to be measured are arranged in a straight line. In contrast, if the multiple positions are not arrayed in a straight line, on measurement in a non-stop measurement mode, a measurement position may appear at a folded point on a movement path of the imaging means. Therefore, a movement mechanism is overloaded and a problem may arise associated with a blown protective fuse depending on the case. In addition, the movement mechanism may cause vibrations and worsen the measurement accuracy as a problem.
SUMMARY OF THE INVENTION
The present invention has been made in consideration of such the problems and has an object to provide an image measuring method, image measuring system and image measuring program capable of preventing the measurement accuracy from lowering and the movement mechanism from being overloaded.
To achieve the above object, the present invention provides an image measuring method for image measurement including moving an imaging means relative to a measurement target supported on a measurement stage and capturing instantaneous image information about the measurement target at each of multiple measurement positions without making a stop of the imaging means. The method comprises forming an overshoot path, when the imaging means moves in a first direction to a first measurement position to be measured next and in a second direction from the first measurement position to a next measurement position or a second measurement position, and if an angle formed between the first direction and the second direction exceeds a certain angle, such that the imaging means, after passing through the first measurement position in the first direction, moves a certain distance in the first direction; and lowering a relative movement speed of the imaging means to the measurement stage at the first measurement position as the angle formed between the first direction and the second direction becomes larger.
The present invention also provides an image measuring system for image measurement including moving an imaging means relative to a measurement target supported on a measurement stage and capturing instantaneous image information about the measurement target at each of multiple measurement positions without making a stop of the imaging means. The system comprises a means operative to indicate the multiple measurement positions; a movement path/speed determining means operative to determine a relative movement path and a relative movement speed of the imaging means to the measurement stage based on the multiple measurement positions indicated by the preceding means; and a means operative to move the imaging means relative to the measurement stage based on the relative movement path and the relative movement speed determined at the movement path/speed determining means. The movement path/speed determining means determines the relative movement path and the relative movement speed so as to form an overshoot path, when the imaging means moves in a first direction to a first measurement position to be measured next and in a second direction from the first measurement position to a next measurement position or a second measurement position, and if an angle formed between the first direction and the second direction exceeds a certain angle, such that the imaging means, after passing through the first measurement position in the first direction, moves a certain distance in the first direction, and to lower the relative movement speed of the imaging means to the measurement stage at the first measurement position as the angle formed between the first direction and the second direction becomes larger.
The present invention further provides an image measuring program for instructing a computer to execute image measurement including moving an imaging means relative to a measurement target supported on a measurement stage and capturing instantaneous image information about the measurement target at each of multiple measurement positions without making a stop of the imaging means. The program comprises steps of forming an overshoot path, when the imaging means moves in a first direction to a first measurement position to be measured next and in a second direction from the first measurement position to a next measurement position or a second measurement position, and if an angle formed between the first direction and the second direction exceeds a certain angle, such that the imaging means, after passing through the first measurement position in the first direction, moves a certain distance in the first direction; and lowering a relative movement speed of the imaging means to the measurement stage at the first measurement position as the angle formed between the first direction and the second direction becomes larger.
In the present invention, the imaging means may move in a first direction to a first measurement position to be measured next and in a second direction from the first measurement position to a next measurement position or a second measurement position. In this case, if an angle formed between the first direction and the second direction exceeds a certain angle, an overshoot path is formed from the first measurement position in the first direction. Therefore, it is possible to prevent the first measurement position from appearing at a folded point on a movement path, thereby preventing the measurement accuracy from worsening.
In the present invention, the relative movement speed of the imaging means to the measurement stage at the first measurement position is lowered as the angle formed between the first direction and the second direction becomes larger. Therefore, it is possible to prevent the movement mechanism from being overloaded at a folded point on the movement path.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiments of the present invention will now be described below with reference to the accompanying drawings, in which:
FIG. 1 is an external perspective view showing a configuration of an image measuring system according to an embodiment of the present invention;
FIG. 2 is a functional block diagram of a computer in the same measuring system;
FIG. 3 shows an example of a measurement path in the same measuring system;
FIG. 4 shows an example of a speed pattern on the same measurement path;
FIG. 5 shows an example of a path/speed table in the same system;
FIG. 6A and FIG. 6B show an example of a measurement path in another embodiment of the present invention;
FIG. 7 shows a speed pattern on the same measurement path;
FIG. 8 is an illustrative view of measurement in a standard measurement mode; and
FIG. 9 is an illustrative view of measurement in a non-stop measurement mode.
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the present invention will be described next based on the accompanying drawings.
EMBODIMENT 1
FIG. 1 is a perspective view showing an entire configuration of an image measuring system according to an embodiment of the present invention. This system comprises a non-contact image measuring machine 1 , a computer system 2 operative to drive/control the image measuring machine 1 and execute required data processing, and a printer 3 operative to print out a measurement result.
The image measuring machine 1 is configured as follows. A table 11 is provided and a measurement stage 13 is installed thereon to receive a measurement target (hereinafter referred to as a work) 12 mounted thereon. The measurement stage 13 is driven in the Y-axis direction by a Y-axis drive mechanism, not shown. Fixed at the central portion between both edges of the table 11 are support arms 14 , 15 extending upward. An X-axis guide 16 is fixed to the support arms 14 , 15 to link both upper ends thereof. An imaging unit 17 is supported on the X-axis guide 16 . The imaging unit 17 is driven along the X-axis guide 16 by an X-axis drive mechanism, not shown. A CCD camera 18 is installed on a lower end of the imaging unit 17 as opposed to the measurement stage 13 . The imaging unit 17 contains an illuminator and a focusing mechanism, not shown, as well as a Z-axis drive mechanism operative to shift the position of the CCD camera 18 in the Z-axis direction.
The computer system 2 includes a computer body 21 , a keyboard 22 , a joystick box (hereinafter referred to as J/S) 23 , a mouse 24 , and a display unit 25 . The computer body 21 realizes various functions as shown in FIG. 2 together with certain programs stored therein.
It includes a stage movement processor 31 for controlling the image measuring machine 1 based on an instruction input from input means such as the keyboard 22 , the J/S 23 and the mouse 24 ; an illumination adjustment processor 32 ; and an other measurement condition adjustment processor 33 . The stage movement processor 31 controls the XYZ-axes drive mechanisms in the image measuring machine 1 based on a stage movement instruction input from input means to shift the position of the CCD cameral 18 relative to the measurement stage 13 . At the time of teaching, the illumination adjustment processor 32 flashes the illuminator in the image measuring machine 1 as a strobe light at a certain cycle successively and adjusts the pulse width of the strobe light based on an illumination adjustment instruction input from input means. In a non-stop measurement mode, it flashes the strobe light with a predetermined pulse width at designated measurement positions. The other measurement condition adjustment processor 33 adjusts other measurement conditions such as lens magnification and focusing adjustment based on instruction inputs for other measurement condition adjustments.
The stage position, the information about the pulse width of the strobe light and the information about the other measurement conditions adjusted at the processors 31 - 33 are fetched into a parameter input unit 34 based on a certain instruction input from input means. The parameter fetched in the parameter input unit 34 is stored in a parameter memory 35 . A part program generator 36 uses the parameter stored in the parameter memory 35 to generate a part program for measurement. If input means instructs a non-stop measurement mode, the part program generator 36 generates a part program for the non-stop measurement mode. The generated part program is stored in a part program memory 37 .
A part program executor 38 is operative to read a required part program out of the part program memory 37 and execute it. In accordance with various commands described in the part program, the part program executor drives the stage movement processor 31 , the illumination adjustment processor 32 , the other measurement condition adjustment processor 33 , an image acquisition unit 42 and an image processor 43 appropriately. The pieces of image information imaged at the CCD camera 18 are sequentially stored in an image memory 41 . The pieces of image information stored in image memory 41 are sequentially displayed on the display unit 25 and captured by the image acquisition unit 42 as still images based on the part program. To the image information acquired at the image acquisition unit 42 , the image processor 43 executes image processing for image measurement, such as setting of a measuring tool, detection of edges, and detection of coordinates.
A measurement operation of the image measuring system according to the embodiment thus configured is described next.
FIG. 3 shows an example of a movement path of the measurement stage 13 in the presence of three measurement positions (MP 1 , MP 2 , MP 3 ). The three measurement positions MP 1 -MP 3 are not arrayed in a straight line. A direction of movement from the current position of the CCD camera 18 relative to the measurement stage 13 toward the measurement position MP 1 and a direction of movement from the measurement position MP 1 toward the next measurement position MP 2 form an angle of 45° therebetween. Similarly, the direction of movement from the measurement position MP 1 toward the next measurement position MP 2 and a direction from the measurement position MP 2 toward the next measurement position MP 3 form an angle of 90° therebetween.
FIG. 4 shows an example of a speed pattern of the measurement table 13 on the above movement path.
This system limits the maximum speed depending on the angle at a folded point. For example, a speed pattern may be set as partly speed-limited as including an initial measurement speed unchanged at a 0° angle (straight line), 10 mm/s at the 45° angle corner, and 5 mm/s at the 90° angle corner.
The overshoots beyond the measurement positions MP 1 , MP 2 , MP 3 are made variable depending on the angle at the folded point. For example, the overshoot may be set at 0.3 mm beyond the 45° angle corner, and 0.5 mm beyond the 90° angle corner. Therefore, a practical measurement path shapes a path folded at overshoot points OP 1 , OP 2 as shown with the dotted line in FIG. 3 .
This makes it possible to prevent the vibrations of the measurement positions MP 1 , MP 2 , MP 3 and perform accurate measurements.
To realize the above operation, the part program generator 36 includes a movement path/speed determining means (routine). The movement path/speed determining means contains a path/speed table as shown in FIG. 5 , which may be used to previously register maximum speeds and overshoots relative to corner angles (angles at folded points) on a movement path. When input means indicates measurement positions, the movement path/speed determining means interconnects the measurement positions to create a movement path, calculates angles at the measurement positions on the movement path, and refers to the path/speed table by the angles for the maximum speeds and overshoots. In this embodiment, when the angle is less than 5°, the speed is determined limitless and the overshoot zero, for example.
For convenience of description, a “movement speed” in a fast movement region other than the measurement region is herein distinguished from the “measurement speed” in the measurement region. This system controls the speed as shown in FIG. 4 by decelerating from the movement speed to the measurement speed for passing through the measurement positions MP 1 -MP 3 , then maintaining the measurement speed also in the period of overshoot, thereby achieving zero acceleration at the measurement positions MP 1 -MP 3 . This makes it possible to achieve a high-accuracy measurement. An approach distance is determined at the movement path/speed determining means taking the movement speed and the measurement speed into account.
EMBODIMENT 2
Each of FIG. 6A and FIG. 6B is an illustrative view of another embodiment of the present invention.
FIG. 6A shows an example of the measurement path, which is shaped zigzag in consideration of overshoots because the measurement positions MP 1 -MP 3 are arrayed in a straight line though a measurement starting point SP is not arrayed in the same straight line accidentally.
In such the case, as shown in FIG. 6B , a way point (a passing point) WP can be set, which is not involved in the measurement operation. To the way point WP, no overshoot path is added. The maximum speed at the way point WP can be limited, if required, thereby allowing the measurement path to run in a straight line. Such the setting allows a measurement to be performed with no deceleration at all the measurement positions MP 1 -MP 3 (that is, at the measurement speed) as shown in FIG. 7 . The instruction of such the way point WP is also effective in the presence of a position where it is intended to avoid an interference on the measurement stage.
The above system requires no limitation to be imposed on the arrangement locations of the measurement positions and the order of measurement. In addition, regardless of arrangement of the measurement positions, the angle formed between a path determined from a measurement position and a next measurement position and a next path is used to automatically calculate the speed and the overshoot. Therefore, a measurement can be performed accurately without overloading the machine. Further, a stable and accurate measurement can be achieved effectively within one path.
|
An image measuring method comprises making no stop of an imaging means relative to a measurement stage at measurement positions (MP 1 -MP 3 ), and capturing instantaneous images to acquire information required for measurement. A first direction to a measurement position (MP 1 ) to be measured next and a second direction from the measurement position (MP 1 ) to a next measurement position (MP 2 ) form an angle therebetween. If this angle exceeds a certain angle, an overshoot path is formed at a location beyond the measurement position (MP 1 ) in the first direction. The larger the angle formed between the first direction and the second direction, the lower the measurement speed at the measurement position (MP 1 ) is made.
| 6
|
BACKGROUND
[0001] Automatic reading tutoring has been a growing application for natural language processing and automatic speech recognition tools. An automatic reading tutoring system can provide a story or other text for a student to read out loud, and track the student's reading and any errors the student makes. It can diagnose particular kinds of systematic errors the student makes, respond to errors by providing assistance to the student, and evaluate d student's reading aptitude.
[0002] Automatic reading tutoring systems typically involve building a language model for a given story or other text prior to presenting the text to the student to begin a reading tutoring episode. Building the language model for the story or other text typically involves preparing to accommodate all possible words in the text being used, as well as all possible mistaken words the student might utter, to the best that these can be foreseen. This is particularly difficult for reading tutoring systems since one of their main audiences is children learning to read their native language, and children tend not only to make many unpredictable mistakes in reading, but also to get distracted and make frequent utterances that have nothing to do with the displayed text.
[0003] Building the language model for the text also typically involves accessing a large corpus and requires a significant amount of time to prepare. It also presents a large processing burden during runtime, which tends to translate into processing delays between when the student reads a line and when the computer is able to respond. Such delays tend to strain the student's patience and interrupt the student's attention. Additionally, the reading tutoring system cannot flag all possible reading errors, and may erroneously indicate the student has made an error when the student reads a portion of text correctly. Trying to improve the system's ability to catch errors and not indicate false alarms typically involves raising the time spent processing and further stretching out the delays in the system's responsiveness, while trying to reduce the system's lag time in responding conversely tends to degrade performance in error detection and false alarms.
[0004] The discussion above is merely provided for general background information and is not intended to be used as an aid in determining the scope of the claimed subject matter.
SUMMARY
[0005] A novel system for automatic reading tutoring is disclosed herein, that naturally provides effective error detection and reduced false alarms combined with low processing time burdens and response times short enough to maintain a natural, engaging flow of interaction. According to one illustrative embodiment, an automatic reading tutoring method includes displaying a text output and receiving an acoustic input. The acoustic input is modeled with a domain-specific target language model specific to the text output, and with a general-domain garbage language model. User-perceptible feedback is provided based on the target language model and the garbage language model.
[0006] This Summary is provided to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This Summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used as an aid in determining the scope of the claimed subject matter. The claimed subject matter is not limited to implementations that solve any or all disadvantages noted in the background.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1 depicts a flow diagram of a method for automatic reading tutoring, according to an illustrative embodiment.
[0008] FIG. 2 depicts a block diagram of a language modeling system, according to an illustrative embodiment.
[0009] FIG. 3 depicts a block diagram of a language modeling system, according to an illustrative embodiment.
[0010] FIG. 4 depicts a block diagram of a language modeling system, according to an illustrative embodiment.
[0011] FIG. 5 depicts a graph illustrating a feature of an automatic reading tutoring system, according to an illustrative embodiment.
[0012] FIG. 6 depicts a block diagram of one computing environment in which some embodiments may be practiced, according to an illustrative embodiment.
[0013] FIG. 7 depicts a block diagram of a mobile computing environment in which some embodiments may be practiced, according to an illustrative embodiment.
DETAILED DESCRIPTION
[0014] FIG. 1 depicts a flow diagram of an automatic reading tutoring method 100 . Automatic reading tutoring method 100 may be implemented in any of a wide variety of software and computing implementations, as will be familiar to those skilled in the art, and which are surveyed below. FIGS. 2-4 depict block diagrams of automatic reading tutoring systems 200 , 300 , 400 according to various illustrative embodiments that may be associated with automatic reading tutoring method 100 of FIG. 1 . Further details of various illustrative embodiments are provided below, which are illustrative and indicative of the broader meaning and variety associated with the disclosure and the claims provided herein.
[0015] Automatic reading tutoring method 100 includes step 102 , of displaying a text output, such as a sentence of a paragraph from within a larger story or other text. Method 100 next includes step 104 , of receiving an acoustic input, such as a spoken-word utterance from a student reading aloud the text output from step 102 . Method 100 further includes step 106 , of modeling the acoustic input with a domain-specific target language model specific to the text output; and step 108 , of further modeling the acoustic input with a general-domain garbage language model.
[0016] The target language model and the garbage language model may be used, for example, to detect elements of the acoustic model that do not correspond properly to the text output, and to identify these elements as miscues. The target language modeling and garbage language modeling are done in parallel and used together, although in an asymmetrical fashion, since the target language model is domain-specific while the garbage language model is general-domain, providing unique advantages. Because the speech inputs are compared between the parallel target language model and garbage language model, and assigned to the one or the other, the language modeling can be thought of as polarizing the speech inputs. The steps 106 , 108 of modeling the language models are further elaborated below.
[0017] Method 100 also includes step 110 , of providing user-perceptible feedback based on the target language model and the garbage language model. Such user-perceptible feedback may provide confirmation and/or encouragement when the student reads the texts correctly, and may include information on any miscues, such as by providing suggestions or other assistance, when the student makes a mistake in reading the text. Such assistance may take the form of audible corrections to the miscues, provided by the computing device in spoken word, for example. These spoken-word corrections may be pre-recorded, or may be generated by a text-to-speech tool, for example. The assistance may also take the form of displaying a phonetic representation of the portion of the text output corresponding to a miscue, on a monitor or other visual output, for example. Such user-perceptible feedback thereby provides automatic reading tutoring for the student.
[0018] The user-perceptible feedback may also take the form of an evaluation of how well the acoustic input corresponds to the text output, such as a score representing how much of the acoustic input is free of miscues. Such an evaluation can constitute a score on which the student is graded for a test, or it can be used by the student or the student's teacher or parent to keep track of the student's progress over time and set goals for further learning.
[0019] In an application in which the reading tutoring system is provided for students of a second language, as opposed to children learning to read their native language, the user-perceptible feedback may include displaying a translation into a different language, such as the student's native language, of a portion of the text output for which the acoustic input includes a miscue.
[0020] Such user-perceptible feedback may also be provided when the system evaluates the acoustic input to correctly correspond to the text output, indicating that the student has correctly read the text output. (“The system” here, and throughout the remaining disclosure, may be used as a shorthand reference to a computing system executing an illustrative embodiment, such as method 100 .) For example, the system may provide a low-key, unobtrusive running indicator of each of the student's spoken-word inputs that represents a correct reading of the corresponding text output. This might be, for example, a green light that lights up in a corner of a screen every time the student correctly reads a text output, in one illustrative embodiment.
[0021] Method 100 further includes decision node 112 , in which the system evaluates whether it is finished with a larger reading tutoring episode of which the text output of step 102 is part.
[0022] If the system is finished with a reading tutoring episode, the method may proceed to endpoint 114 . If it is not yet finished, the system may return to the beginning and iteratively repeat the process of displaying additional text outputs as in step 102 , receiving corresponding acoustic inputs as in step 104 , assembling additional domain-specific target language models respectively based on each of the additional text outputs as in step 106 , modeling the acoustic input with the general-domain garbage language model as in step 108 , and provide new user-perceptible feedback for that iteration, as in step 110 .
[0023] Step 106 , of modeling the acoustic input with a domain-specific target language model specific to the text input, may be performed within a restricted period of time relative to when its respective text output is displayed as in step 102 . That is, the system may calculate a language model score for the target words of the displayed text only once the target words are called up for display, which may be in a sentence or a paragraph at a time, for example. In this illustrative embodiment, therefore, a small language model is built just for an individual sentence or paragraph at the time that short text sample is brought up for display, for the student to read.
[0024] This provides a number of advantages. Because the text sample is so small, the system can process it in a very short time, short enough that the student will not experience any noticeable delay. This also allows the system to begin functioning, or to begin a tutoring episode based on a text or a position within a text just selected by the student, without having to then stop and process the entire text prior to allowing the student to continue.
[0025] A reading tutoring system such as this is illustratively depicted as language modeling system 200 in FIG. 2 . Language modeling system 200 involves a combination of general-domain garbage modeling and domain-specific target modeling, implemented in this illustrative embodiment with target language model 206 , a domain-specific statistical language model implemented as a Context-Free Grammar (CFG), in this embodiment; and garbage language model 210 , a general-domain N-gram statistical language model implemented as a Context-Free Grammar (CFG), in this embodiment. Target language model 206 is engaged through grammar entry node 202 , and leads to grammar exit node 204 , in this illustrative embodiment.
[0026] Ordinarily, a general-domain N-gram statistical language model has a low processing burden but poor modeling performance, while a domain-specific statistical language model ordinarily has high modeling performance but imposes a high processing burden involving significant delays.
[0027] Language modeling system 200 combines the best of both worlds, as an on-line interpolated language model, with the domain-specific target language model 206 at its core, which is trained on-the-fly from a limited set of training sentences, such as a then-current sentence or paragraph in a story or other text output. At the same time, the general-domain garbage language model 210 , which may be implemented as an N-Gram Filler, such as a restricted version of a dictation grammar, is attached to target language model 206 through a unigram back-off node 208 comprised in target language model 206 . Garbage language model 210 thereby provides robustness in that it is able to siphon off general miscues without having to have them defined in advance. The interpolation between target language model 206 and garbage language model 210 may be promoted by reserving some unigram counts for unforeseen garbage words, to get swept aside from target language model 206 by garbage language model 210 .
[0028] Beginning from the path from grammar entry node 202 to target language model 206 , target language model 206 then has a weight w 1 that controls the possibility of moving from within target language model 206 to unigram back-off node 208 . A second weight, w 2 , controls the possibility of moving from unigram back-off node 208 to garbage language model 210 . The target language model 206 is relatively small, such as enough to occupy a few kilobytes of memory in one embodiment, due to being based on only the text sample currently on display at a given time, such as a paragraph or a sentence. The garbage language model 210 is significantly larger—in the same embodiment, it may be enough to occupy several megabytes of memory—but this does not pose any significant processing burden or reaction time delay, because the one single garbage language model 210 may be shared for the purposes of all the text samples that are successively modeled with the target language model 206 . So, the only new language model that is built within the timeframe of providing the display text output, is the few kilobytes worth or so of the local-scale, on-the-fly target language model 206 .
[0029] FIG. 3 elaborates on the embodiment of FIG. 2 . FIG. 3 depicts language modeling system 300 , according to an illustrative embodiment which shares a number of common or analogous features with the illustrative embodiment of FIG. 2 . FIG. 3 includes grammar entry node 302 , grammar exit node 304 , target language model 306 , unigram back-off node 308 comprised in target language model 306 , and garbage language model 310 , implemented as an N-Gram Filler. Target language model 306 in this embodiment is built from a text output comprising a single sentence from a story. The sentence reads simply, “Giants are huge”. Target language model 306 includes a binary Context Free Grammar built from this single sentence.
[0030] In addition to the special nodes consisting of the grammar entry node 302 , grammar exit node 304 , and unigram back-off node 308 , target language model 306 includes three nodes corresponding to bigram states with one word each: bigram state node 312 for the word “Giants”, bigram state node 314 for the word “are”, and bigram state node 316 for the word “huge”. Running between the nodes are possible paths that may be taken, depending on the acoustic input. Each of grammar entry node 302 and bigram state nodes 312 , 314 , and 316 have possible paths leading to unigram back-off node 308 , and thence to garbage language model 310 and back, if any one of the nodes is followed by a miscue. Target language model 306 may also include more complex N-gram nodes to provide stronger robustness, such as trigram nodes “<s> Giants”, “Giants Are”, “Are Huge”, “Huge </s>” (not shown in FIG. 3 ), in the example sentence “Giants are huge”. The domain-specific target language model may therefore be constructed with different complexity ranging from simple unigrams, to more complex bigrams and trigrams, to more complicated higher-order N-grams, in order to provide different levels of robustness in the system. Using a relatively simpler unigram or bigram garbage language model may provide significant advantages in efficiency. The complexity of the domain-specific target language model may be user-selectable, and may be selected according to the nature of the applications being implemented and the user's reading ability.
[0031] Grammar entry node 302 , bigram state nodes 312 , 314 , and 316 , and grammar exit node 304 also have possible paths running in sequence between them, allowing for the potential match of the acoustic input with bigrams composed of the bigram state nodes 312 , 314 , if the student correctly reads aloud (as embodied in the acoustic input) the two-word sequence “Giants are”, as well as the potential match of the acoustic input with bigrams composed of the bigram state nodes 314 , 316 , if the student correctly reads aloud the two-word sequence “are huge”.
[0032] The garbage language model 310 is used to detect reading miscues, whether or not unforeseen, and without any need to predict in advance what the miscues will be like, to assemble and comb through a miscue database, or to try to decode miscues phonetically. This provides a particular advantage in a reading tutoring system for children, who are liable to say any variety of things or make any variety of sounds that have nothing to do with the displayed text output they are supposed to be reading. It is also advantageous for adult learners of a second language, as it detects the frequent miscues they may make such as by mispronouncing the words in the text output of the non-native language they are studying.
[0033] Garbage language model 310 may be obtained from a general-domain N-gram model, but restricted or trimmed down to a smaller selection from a dictation grammar, such as only the 1 , 600 most common words, for example. This is one example of a small selection that will reduce the processing burden on the system, that is nevertheless very effective. A small set of lexical features may be used by the garbage language model 310 , to save further on the processing burden. It has been found, for example, that basing the garbage language model 310 only on unigrams and bigrams provided very effective garbage language modeling, that was not substantially improved by trying to add additional, more burdensome lexical features to the language modeling. Garbage language model 310 with different complexity may be used, ranging from a simple unigram to more a more complex bigram or trigram, or higher order N-gram, although in some embodiments, higher orders of N-grams may provide diminishing returns in robustness while increasing the computational burden, such that building the garbage language model in a unigram or bigram form may provide the best efficiency for the goals for that embodiment.
[0034] Garbage language model 310 can thereby be built on-the-fly, during usage of the reading tutoring system; garbage language model 310 does not impose any burden to change decoding engines, and it can interface with any automatic speech recognition system; and it provides adjustable, tunable weighting parameters w 1 , w 2 that allow the sensitivity of the garbage language modeling, in terms of its Receiver Operating Characteristic (ROC) curve, to be freely adjusted, based on preference, the level of the student's knowledge, and so forth. FIG. 5 depicts just such an ROC curve for garbage language model 310 , based on further discussion on the weighting parameters provided below in connection with FIG. 4 .
[0035] FIG. 4 depicts a language modeling system 400 with analogous elements to those discussed above, although this one is directed to an equivalent two-path grammar for a single word. Language modeling system 400 includes grammar entry node 402 , grammar exit node 404 , target word node 406 , and garbage word node 410 . Language modeling system 400 also includes tunable weighting parameter w 0 , that applies to the path leading to garbage word node 410 . The weighting parameter w 0 can be calculated based on the weighting parameters w 1 , w 2 and the target language model 206 in FIG. 2 . Garbage word node 410 is not limited to modeling words per se, but may also output garbage words that are acoustically similar to subword-level miscues that are detected, such as a partial word, a hesitation or elongation, or background noise, for example.
[0036] Given a spoken word acoustic input X, a target word T, and a garbage word G, a hypothesis testing scenario can be obtained as follows:
[0037] H 0 : Target word T exists;
[0038] H 1 : Target word T does not exist;
[0039] Then the decision rule is given by:
[0000]
H
0
:
when
P
(
H
0
|
X
)
P
(
H
1
|
X
)
=
(
1
-
w
0
)
P
(
X
|
T
)
P
(
T
)
w
0
P
(
X
|
G
)
P
(
G
)
≻
1
[0040] H 1 : otherwise;
[0041] where P(X|T) and P(X|G) are the acoustic score for the target and garbage words, respectively, and P(T) and P(G) are language model scores for the target and garbage words, respectively. The above decision rule is equivalent to the following decision rule:
[0000]
H
0
:
when
P
(
X
|
T
)
P
(
T
)
P
(
X
|
G
)
P
(
G
)
≻
λ
=
w
0
1
-
w
0
[0042] H 1 : otherwise;
[0043] where λ is a threshold as an explicit function of the weighting parameter w 0 . This detection scenario is equivalent to regular hypothesis testing in an utterance verification problem.
[0044] When the garbage model weight is increased, therefore, the miscue detection rate also increases, along with some increase in the rate of false alarms. The relationship between the prevalence of the two factors according to one illustrative implementation can be seen in FIG. 5 , where the curve represents the rates of both detection and false alarm corresponding to a series of selected weighting parameters w 0 with a set of pre-trained acoustic model and language models. In general, it may often be desirable to train better acoustic and language models to obtain a curve towards the upper left corner of the graph, to work a good compromise between relatively high detection and relatively low false alarm rate.
[0045] For a fixed set of acoustic and language models, it may also be desired to adjust the weighting parameter to be more lenient, and occupy a spot on the curve more toward the lower left, such as for beginning students. This is to specifically avoid false alarms that might discourage these beginning students, at the expense of performance in the absolute detection rate. For more advanced students such as adult learners of a second language, and still assuming a fixed set of acoustic and language models, it may be preferable to adjust the weighting parameter w 0 to make the system more strict, i.e. to move the operating point toward the upper right portion of the curve in FIG. 5 , when the students might be expected to understand the false alarms as such or to have more patience with them, but be more interested in addressing as many errors in reading as possible.
[0046] The miscues may be identified with one or more miscue categories, and the user-perceptible feedback may be based in part on one of the miscue categories with which a miscue in the acoustic input is identified, so that it will correct a mispronunciation, for example, but simply continue to prompt for an acoustic input if the miscue is an interjection or background noise. The miscue categories may include, for example, word repetition, breath, partial word, pause, hesitation or elongation, wrong word, mispronunciation, background noise, interjection or insertion, non-speech sound, and hyperarticulation.
[0047] FIG. 6 illustrates an example of a suitable computing system environment 600 on which various embodiments may be implemented. For example, various embodiments may be implemented as software applications, modules, or other forms of instructions that are executable by computing system environment 600 and that configure computing system environment 600 to perform various tasks or methods involved in different embodiments. A software application or module associated with an illustrative implementation of an automatic reading tutoring system with parallel polarized language modeling may be developed in any of a variety of programming or scripting languages or environments. For example, it may be written in C#, F#, C++, C, Pascal, Visual Basic, Java, JavaScript, Delphi, Eiffel, Nemerle, Perl, PHP, Python, Ruby, Visual FoxPro, Lua, or any other programming language. It is also envisioned that new programming languages and other forms of creating executable instructions will continue to be developed, in which further embodiments may readily be developed.
[0048] Computing system environment 600 as depicted in FIG. 6 is only one example of a suitable computing environment for implementing various embodiments, and is not intended to suggest any limitation as to the scope of use or functionality of the claimed subject matter. Neither should the computing environment 600 be interpreted as having any dependency or requirement relating to any one or combination of components illustrated in the exemplary operating environment 600 .
[0049] Embodiments are operational with numerous other general purpose or special purpose computing system environments or configurations. Examples of well-known computing systems, environments, and/or configurations that may be suitable for use with various embodiments include, but are not limited to, personal computers, server computers, hand-held or laptop devices, multiprocessor systems, microprocessor-based systems, set top boxes, programmable consumer electronics, network PCs, minicomputers, mainframe computers, telephony systems, distributed computing environments that include any of the above systems or devices, and the like.
[0050] Embodiments may be described in the general context of computer-executable instructions, such as program modules, being executed by a computer. Generally, program modules include routines, programs, objects, components, data structures, etc. that perform particular tasks or implement particular abstract data types. Some embodiments are designed to be practiced in distributed computing environments where tasks are performed by remote processing devices that are linked through a communications network. In a distributed computing environment, program modules are located in both local and remote computer storage media including memory storage devices. As described herein, such executable instructions may be stored on a medium such that they are capable of being read and executed by one or more components of a computing system, thereby configuring the computing system with new capabilities.
[0051] With reference to FIG. 6 , an exemplary system for implementing some embodiments includes a general-purpose computing device in the form of a computer 610 . Components of computer 610 may include, but are not limited to, a processing unit 620 , a system memory 630 , and a system bus 621 that couples various system components including the system memory to the processing unit 620 . The system bus 621 may be any of several types of bus structures including a memory bus or memory controller, a peripheral bus, and a local bus using any of a variety of bus architectures. By way of example, and not limitation, such architectures include Industry Standard Architecture (ISA) bus, Micro Channel Architecture (MCA) bus, Enhanced ISA (EISA) bus, Video Electronics Standards Association (VESA) local bus, and Peripheral Component Interconnect (PCI) bus also known as Mezzanine bus.
[0052] Computer 610 typically includes a variety of computer readable media. Computer readable media can be any available media that can be accessed by computer 610 and includes both volatile and nonvolatile media, removable and non-removable media. By way of example, and not limitation, computer readable media may comprise computer storage media and communication media. Computer storage media include both volatile and nonvolatile, removable and non-removable media implemented in any method or technology for storage of information such as computer readable instructions, data structures, program modules or other data. Computer storage media include, but are not limited to, RAM, ROM, EEPROM, flash memory or other memory technology, CD-ROM, digital versatile disks (DVD) or other optical disk storage, magnetic cassettes, magnetic tape, magnetic disk storage or other magnetic storage devices, or any other medium which can be used to store the desired information and which can be accessed by computer 610 .
[0053] Communication media typically embody computer readable instructions, data structures, program modules or other data in a modulated data signal such as a carrier wave or other transport mechanism and include any information delivery media. The term “modulated data signal” means a signal that has one or more of its characteristics set or changed in such a manner as to encode information in the signal. By way of example, and not limitation, communication media include wired media such as a wired network or direct-wired connection, and wireless media such as acoustic, RF, infrared and other wireless media. Combinations of any of the above should also be included within the scope of computer readable media.
[0054] The system memory 630 includes computer storage media in the form of volatile and/or nonvolatile memory such as read only memory (ROM) 631 and random access memory (RAM) 632 . A basic input/output system 633 (BIOS), containing the basic routines that help to transfer information between elements within computer 610 , such as during start-up, is typically stored in ROM 631 . RAM 632 typically contains data and/or program modules that are immediately accessible to and/or presently being operated on by processing unit 620 . By way of example and not limitation, FIG. 6 illustrates operating system 634 , application programs 635 , other program modules 636 , and program data 637 .
[0055] The computer 610 may also include other removable/non-removable volatile/nonvolatile computer storage media. By way of example and not of limitation, FIG. 6 illustrates a hard disk drive 641 that reads from or writes to non-removable, nonvolatile magnetic media, a magnetic disk drive 651 that reads from or writes to a removable, nonvolatile magnetic disk 652 , and an optical disk drive 655 that reads from or writes to a removable, nonvolatile optical disk 656 such as a CD ROM or other optical media. Other removable/non-removable, volatile/nonvolatile computer storage media that can be used in the exemplary operating environment include, but are not limited to, magnetic tape cassettes, flash memory cards, digital versatile disks, digital video tape, solid state RAM, solid state ROM, and the like. The hard disk drive 641 is typically connected to the system bus 621 through a non-removable memory interface such as interface 640 , and magnetic disk drive 651 and optical disk drive 655 are typically connected to the system bus 621 by a removable memory interface, such as interface 650 .
[0056] The drives and their associated computer storage media discussed above and illustrated in FIG. 6 , provide storage of computer readable instructions, data structures, program modules and other data for the computer 610 . In FIG. 6 , for example, hard disk drive 641 is illustrated as storing operating system 644 , application programs 645 , other program modules 646 , and program data 647 . Note that these components can either be the same as or different from operating system 634 , application programs 635 , other program modules 636 , and program data 637 . Operating system 644 , application programs 645 , other program modules 646 , and program data 647 are given different numbers here to illustrate that, at a minimum, they may be different copies.
[0057] A user may enter commands and information into the computer 610 through input devices such as a keyboard 662 , a microphone 663 , and a pointing device 661 , such as a mouse, trackball or touch pad. Other input devices (not shown) may include a joystick, game pad, satellite dish, scanner, or the like. These and other input devices are often connected to the processing unit 620 through a user input interface 660 that is coupled to the system bus, but may be connected by other interface and bus structures, such as a parallel port, game port or a universal serial bus (USB). A monitor 691 or other type of display device is also connected to the system bus 621 via an interface, such as a video interface 690 . In addition to the monitor, computers may also include other peripheral output devices such as speakers 697 and printer 696 , which may be connected through an output peripheral interface 695 .
[0058] The computer 610 is operated in a networked environment using logical connections to one or more remote computers, such as a remote computer 680 . The remote computer 680 may be a personal computer, a hand-held device, a server, a router, a network PC, a peer device or other common network node, and typically includes many or all of the elements described above relative to the computer 610 . The logical connections depicted in FIG. 6 include a local area network (LAN) 671 and a wide area network (WAN) 673 , but may also include other networks. Such networking environments are commonplace in offices, enterprise-wide computer networks, intranets and the Internet.
[0059] When used in a LAN networking environment, the computer 610 is connected to the LAN 671 through a network interface or adapter 670 . When used in a WAN networking environment, the computer 610 typically includes a modem 672 or other means for establishing communications over the WAN 673 , such as the Internet. The modem 672 , which may be internal or external, may be connected to the system bus 621 via the user input interface 660 , or other appropriate mechanism. In a networked environment, program modules depicted relative to the computer 610 , or portions thereof, may be stored in the remote memory storage device. By way of example, and not limitation, FIG. 6 illustrates remote application programs 685 as residing on remote computer 680 . It will be appreciated that the network connections shown are exemplary and other means of establishing a communications link between the computers may be used.
[0060] FIG. 7 depicts a block diagram of a general mobile computing environment 700 , comprising a mobile computing device 701 and a medium, readable by the mobile computing device and comprising executable instructions that are executable by the mobile computing device, according to another illustrative embodiment. FIG. 7 depicts a block diagram of a mobile computing system 700 including mobile device 701 , according to an illustrative embodiment. Mobile device 701 includes a microprocessor 702 , memory 704 , input/output (I/O) components 706 , and a communication interface 708 for communicating with remote computers or other mobile devices. In one embodiment, the afore-mentioned components are coupled for communication with one another over a suitable bus 710 .
[0061] Memory 704 is implemented as non-volatile electronic memory such as random access memory (RAM) with a battery back-up module (not shown) such that information stored in memory 704 is not lost when the general power to mobile computing device 701 is shut down. A portion of memory 704 is illustratively allocated as addressable memory for program execution, while another portion of memory 704 is illustratively used for storage, such as to simulate storage on a disk drive.
[0062] Memory 704 includes an operating system 712 , application programs 714 as well as an object store 716 . During operation, operating system 712 is illustratively executed by processor 702 from memory 704 . Operating system 712 , in one illustrative embodiment, is a WINDOWS® CE brand operating system commercially available from Microsoft Corporation. Operating system 712 is illustratively designed for mobile devices, and implements database features that can be utilized by applications 714 through a set of exposed application programming interfaces and methods. The objects in object store 716 are maintained by applications 714 and operating system 712 , at least partially in response to calls to the exposed application programming interfaces and methods.
[0063] Communication interface 708 represents numerous devices and technologies that allow mobile computing device 701 to send and receive information. The devices include wired and wireless modems, satellite receivers and broadcast tuners to name a few. Mobile computing device 701 can also be directly connected to a computer to exchange data therewith. In such cases, communication interface 708 can be an infrared transceiver or a serial or parallel communication connection, all of which are capable of transmitting streaming information.
[0064] Input/output components 706 include a variety of input devices such as a touch-sensitive screen, buttons, rollers, and a microphone as well as a variety of output devices including an audio generator, a vibrating device, and a display. The devices listed above are by way of example and need not all be present on mobile computing device 701 . In addition, other input/output devices may be attached to or found with mobile computing device 701 .
[0065] Mobile computing environment 700 also includes network 720 . Mobile computing device 701 is illustratively in wireless communication with network 720 —which may be the Internet, a wide area network, or a local area network, for example—by sending and receiving electromagnetic signals 799 of a suitable protocol between communication interface 708 and wireless interface 722 . Wireless interface 722 may be a wireless hub or cellular antenna, for example, or any other signal interface. Wireless interface 722 in turn provides access via network 720 to a wide array of additional computing resources, illustratively represented by computing resources 724 and 726 . Naturally, any number of computing devices in any locations may be in communicative connection with network 720 . Mobile computing device 701 is enabled to make use of executable instructions stored on the media of memory component 704 , such as executable instructions that enable mobile computing device 701 to implement various functions of automatic reading tutoring with parallel polarized language modeling, in an illustrative embodiment.
[0066] Although the subject matter has been described in language specific to certain illustrative structural features and/or methodological acts, it is to be understood that the subject matter defined in the appended claims is not limited to the specific features or acts described above. Rather, the specific features and acts described above are disclosed as illustrative examples of ways in which the claims may be implemented. As a particular example, while the terms “computer”, “computing device”, or “computing system” may herein sometimes be used alone for convenience, it is well understood that each of these could refer to any computing device, computing system, computing environment, mobile device, or other information processing component or context, and is not limited to any individual interpretation. As another particular example, while many embodiments are presented with illustrative elements that are widely familiar at the time of filing the patent application, it is envisioned that many new innovations in computing technology will affect elements of different embodiments, in such aspects as user interfaces, user input methods, computing environments, and computing methods, and that the elements defined by the claims may be embodied according to these and other innovative advances in accordance with the developing understanding of those skilled in the art, while still remaining consistent with and encompassed by the subject matter defined by the claims herein.
|
A novel system for automatic reading tutoring provides effective error detection and reduced false alarms combined with low processing time burdens and response times short enough to maintain a natural, engaging flow of interaction. According to one illustrative embodiment, an automatic reading tutoring method includes displaying a text output and receiving an acoustic input. The acoustic input is modeled with a domain-specific target language model specific to the text output, and with a general-domain garbage language model, both of which may be efficiently constructed as context-free grammars. The domain-specific target language model may be built dynamically or “on-the-fly” based on the currently displayed text (e.g. the story to be read by the user), while the general-domain garbage language model is shared among all different text outputs. User-perceptible tutoring feedback is provided based on the target language model and the garbage language model.
| 6
|
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to cutting blades for shredders. Specifically, this invention teaches cutting blades and a rotary cutting assembly which reduce the power needed to shred paper, plastic, and other forms of media that hold information.
[0003] 2. Background Information
[0004] With increased privacy concerns, shredders have become an integral part in both homes and businesses. Though originally used to destroy paper products, shredders are now used to shred other forms of media that hold information, such as compact discs. In addition, credit cards and other plastic products are commonly shredded.
[0005] Conventional shredders use a plurality of cutting blades spaced apart along a rotary shaft to form a rotary cutting assembly. Articles are shredded when fed through two parallel and opposite rotating rotary cutting assemblies.
[0006] The first common conventional shredder, called the strip-cut shredder, cut paper into strips along the entire length of the paper. A drawback with this type of shredder is that the strips can be pieced together like a puzzle.
[0007] In order to decrease this likelihood, shredder manufacturers developed the cross-cut shredder which shreds paper into tiny rectangles. This is accomplished by again having two parallel and opposite rotating rotary cutting assemblies. Cutting blades are again spaced apart along the length of each rotary shaft. When paper is fed through the two rotary cutting assemblies, it is cut in a similar fashion as the strip cut shredder. However, the cutting blades also have teeth protruding from the blade which puncture the strips into small rectangles, for example into 4 mm×40 mm pieces.
[0008] The teeth of each cutting blade are offset in the longitudinal direction of the rotary shaft such that they form a helix around the rotary shaft. The teeth are offset in order to decrease the amount of power needed to cut the paper. If the teeth were aligned in a row, then they would punch the paper at the same time, thus requiring a more powerful motor to simultaneously punch through the paper.
[0009] The Diamond Cut shredder was the next innovation in shredders. Through the use of a unique and novel rotary cutting assembly utilizing round undulating blades, Diamond Cut shredders, are able to shred paper in a diamond shape, thus offering maximum security.
[0010] Irrespective of the type of cut, shredders may be generally categorized according to the maximum number of sheets that it can shred. For example, a 10 sheet cross-cut shredder is designed to shred a maximum of 10 sheets. A 16 sheet cross-cut shredder is designed to shred a maximum of 16 sheets. Logically, the size of the shredder motor increases as the maximum number of sheets that the shredder can shred increases. More powerful motors are needed to shred greater amounts of paper, and are heavier and use more energy than the motors requiring less torque.
[0011] In order to save energy and reduce the size of the motor currently employed in shredders, the present invention seeks to employ various cutting blades and configurations which more readily shred paper thus reducing the size of the motor and saving energy.
[0012] One preferred embodiment of the claimed invention provides this by adding an additional cutting blade between the two cutting blades that are typically employed in a cross-cut shredder. The additional cutting blade has a spear shaped tooth which, in conjunction with two adjacent teeth, more readily tears through and shreds the paper. From the preceding descriptions, it is apparent that the devices currently being used have significant disadvantages and/or limitations. Thus, important aspects of the technology used in the field of invention remain amenable to useful refinement.
SUMMARY OF THE INVENTION
[0013] The present invention relates to an apparatus that satisfies the need for a more efficient and power saving cutting blade incorporated into a rotary cutting assembly. In one preferred embodiment, an inner cutting blade having features of the present invention comprises a circular blade with at least two teeth that are spear shaped protruding from the blade. The inner cutting blade is then placed between two outer cutting blades with the same number of teeth, except the outer cutting blade teeth are flat and narrow. The blades are aligned such that the inner spear shaped tooth is sandwiched between the two outer, flat and narrow teeth. The blades are then spaced apart along the length of a rotary shaft and displaced along the longitudinal axis in order to form a helix around the rotary shaft. This novel rotary cutting assembly requires less power to shred. For instance, a 10 sheet shredder motor can now be used to shred 16 sheets.
[0014] All of the foregoing operational principles and advantages of the present invention will be more fully appreciated upon consideration of the following detailed description with reference to the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The features and advantages of this invention are better understood with regard to the following drawings, description, and claims. The drawings consist of the following:
[0016] FIG. 1 is a perspective view of prior art cutting blades.
[0017] FIG. 2 is a planar view of prior art cutting blades.
[0018] FIG. 3 is a perspective view of a rotary cutting assembly embodying features of this invention.
[0019] FIG. 4 is an elevation side view of a rotary cutting assembly.
[0020] FIG. 5 is an elevation front view of a rotary cutting assembly.
[0021] FIG. 6 is an elevation front view of the rotary shaft.
[0022] FIG. 7 is an elevation side view of the rotary shaft.
[0023] FIG. 8 is a perspective view of a blade embodying features of this invention.
[0024] FIG. 9 is a side elevation view of a cutting blade embodying features of this invention.
[0025] FIG. 10 is a front elevation view of a cutting blade embodying features of this invention.
[0026] FIG. 11 is a perspective view of a cutting blade embodying features of this invention.
[0027] FIG. 12 is a side elevation view of a cutting blade embodying features of this invention.
[0028] FIG. 13 is a front elevation view of a cutting blade embodying features of this invention.
[0029] FIG. 14 is a perspective view of three cutting blades embodying features of this invention.
[0030] FIG. 15 is a side elevation view of a three cutting blades embodying features of this invention.
[0031] FIG. 16 is a perspective view of a partially assembled rotary cutting assembly.
[0032] FIG. 17 is a front elevation view of a partially assembled rotary cutting assembly.
[0033] FIG. 18 is a side elevation view of a partially assembled rotary cutting assembly.
[0034] FIG. 19 is a perspective view of two rotary cutting assemblies.
[0035] FIG. 20 is a side elevation view of two rotary cutting assemblies.
[0036] FIG. 21 is a perspective view of three cutting blades embodying features of this invention.
[0037] FIG. 22 is a side elevation view of three cutting blades embodying features of this invention.
[0038] FIG. 23 is a front elevation view of a cutting blade embodying features of this invention.
[0039] FIG. 24 is a perspective view of three cutting blades embodying features of this invention.
[0040] FIG. 25 is a side elevation view of three cutting blades embodying features of this invention.
[0041] FIG. 26 is a perspective view of a partially assembled rotary cutting assembly with paper strippers.
[0042] FIG. 27 is a front elevation view of a partially assembled rotary cutting assembly with paper strippers.
[0043] FIG. 28 is a side elevation view of a partially assembled rotary cutting assembly with paper strippers.
[0044] FIG. 29 is a perspective view of a partially assembled rotary cutting assembly with paper strippers.
[0045] FIG. 30 is a perspective view of a partially assembled rotary cutting assembly with paper strippers.
[0046] FIG. 31 is a perspective view of a rotary cutting assembly with paper strippers.
[0047] FIG. 32 is a front elevation view of a rotary cutting assembly with paper strippers.
[0048] FIG. 33 is a side elevation view of a rotary cutting assembly with paper strippers.
DETAILED DESCRIPTION OF THE INVENTION
[0049] The essential elements of a shredder are comprised of a base, a housing, and a shredder mechanism which resides in the housing. The shredder mechanism contains two rotary cutting assemblies which shred paper as the paper is fed through the assemblies.
[0050] This invention discloses a rotary cutting assembly with a configuration that more efficiently shreds paper, thus requiring less power. The rotary cutting assembly is comprised of cutting blades spaced apart along the length of a rotary shaft. The cutting blade or blades are configured such that teeth protrude from it as described below.
[0051] FIGS. 3-20 disclose a first preferred embodiment of a rotary cutting assembly 1 with three cutting blades 2 forming a cutting blade assembly 5 . As shown in FIGS. 3 and 5 , the rotary cutting assembly 1 is comprised of cutting blade assemblies 5 spaced apart along the length of the rotary shaft 3 . Each cutting blade assembly 5 has a plurality of teeth 4 that protrude from the cutting blades 2 . As illustrated in FIGS. 6 and 7 , the rotary shaft 3 is preferably hexagon in shape and made of a durable metal alloy such as steel.
[0052] In one preferred embodiment, the three cutting blades are coupled together to form a cutting blade assembly 5 (see FIG. 14 ) and then spaced apart along the rotary shaft from other cutting blade assemblies 5 . FIGS. 8-10 illustrate the outer cutting blades 6 of the cutting blade assembly 5 . The outer cutting blades 6 have a hub 7 with polygonal hole 8 formed in the center of the hub 7 through which a rotary shaft 3 may pass. The polygonal shape locks into the hexagon shaped rotary shaft thereby securing the cutting blade such that it will not rotate around the rotary shaft.
[0053] It is preferable that the periphery 9 of the outer cutting blade is serrated, though not necessary. The serration may serve to pull the paper to be cut through the rotary cutting assemblies. Towards the periphery of the outer cutting blade 6 is a plurality of indentations or ribs 10 in the body 11 of the cutting blade. The ribs 10 serve to reinforce the cutting blade and prevent it from flexing. In addition, the ribs 10 hold the inner cutting blade 19 in place. Substantially perpendicular to the ribs are additional indentations or spokes 12 . The spokes 12 also serve as reinforcement for the cutting blade. In addition, the spokes 12 serve to support the inner cutting blade 19 .
[0054] The outer cutting blades 6 also have three flat, narrow teeth 13 located 120 degrees apart around the circumference of the cutting blade. It should be appreciated that for larger capacity shredders which require larger cutting blades with a greater circumference, four teeth can be placed 90 degrees apart around the periphery. For shredders with smaller capacities and thus smaller cutting blades, two teeth can be placed 180 degrees apart around the periphery. The distance between the teeth determines the size of the shredded material. If there is less distance, the material is shredded into smaller pieces.
[0055] The outer cutting blade tooth 13 is preferably the same width as the cutting blade along the serrated periphery, and maintains the same width from the base 14 of the tooth to its tip 15 . One side 16 of the outer cutting blade tooth is a few degrees from perpendicular to the tangent at the circumference of the cutting blade, while the other sloping side 17 is greater than 105 degrees from the tangent. The tooth is formed when the substantially perpendicular side 16 of the tooth and the sloping side 17 meet. The tooth also has an indented portion 18 which provides reinforcement in a similar manner that the ribs 10 and spokes 12 reinforce the overall structure of the blade.
[0056] The outer blade 6 is formed when sheet metal of a thickness of about 0.6 mm is punched by a die into the form of the outer cutting blade comprised of a polygonal hole, hub, ribs, spokes, serrated periphery, and teeth.
[0057] FIGS. 11-13 disclose the inner cutting blade 19 . Like the outer cutting blade 6 , the inner cutting blade 19 has a polygonal hole 20 formed in the center of it through which a rotary shaft may pass. The polygonal shape locks into the hexagon shaped rotary shaft thereby securing the cutting blade such that it will not rotate around the rotary shaft.
[0058] The inner cutting blade 19 has the same number of teeth around the periphery as the outer cutting blade. In this preferred embodiment, three teeth are located 120 degrees apart around the circumference of the inner cutting blade. As mentioned above, for larger capacity shredders which require larger cutting blades with a greater circumference, four teeth can be placed 90 degrees apart around the periphery. For shredders with smaller capacities and thus smaller cutting blades, two teeth can be placed 180 degrees apart around the periphery.
[0059] The inner cutting blade tooth 21 is preferably shaped like a spear at its tip 22 . It is formed by folding over the 0.6 mm metal sheet two times such that the approximate thickness of the tooth is 1.8 mm and then punched by a die into the form of the spear shaped tooth. The width of the inner cutting tooth 23 is therefore approximately three times greater than the width of the base 24 of the inner cutting blade 19 .
[0060] As seen in FIGS. 14 and 15 , the outer cutting blades 6 sandwich and flank the inner cutting blade 19 in a configuration such that the teeth are aligned. The ribs 10 and spokes 12 of the outer cutting blade 6 and the tooth indented portion 18 provide support and secure the inner cutting blade 19 to ensure proper alignment.
[0061] It should be appreciated that although this preferred embodiment discloses three blades coupled together to form a cutting blade assembly 5 , the same mechanism can be accomplished with less than three blades. For example, rather than have three blades, one blade can have a base of sufficient width to support two narrow teeth flanking a larger spear shaped tooth. In addition, in certain situations, more than three adjacent teeth may be advantageous. In such situations, one or more blades may be used to support the adjacent teeth.
[0062] Accordingly, this patent discloses a rotary cutting assembly comprised of a plurality of cutting blades; said cutting blades having at least two sets of at least three adjacent teeth wherein said adjacent teeth flank each other; said sets of adjacent teeth spaced apart from other sets of adjacent teeth along the circumference of the cutting blade. The adjacent teeth may be comprised of at least one inner tooth flanked by at least two outer teeth, wherein said outer teeth may be narrower than said inner tooth.
[0063] The patent also illustrates a rotary cutting assembly comprised of a plurality of cutting blade assemblies having at least two sets of at least three adjacent teeth, wherein said adjacent teeth flank each other, said sets of adjacent teeth being spaced apart along the circumference of the cutting blade assembly. The adjacent teeth may be comprised of at least one inner tooth flanked by at least two outer teeth, wherein said outer teeth may be narrower than said inner tooth. The cutting blade assemblies may be comprised of at least two cutting blades flanking each other.
[0064] The patent further discloses a rotary cutting assembly comprised of at least one cutting blade having at least two sets of at least three adjacent teeth wherein said adjacent teeth flank each other; said sets of adjacent teeth being spaced apart along the circumference of the cutting blade. The adjacent teeth may be comprised of at least one inner tooth flanked by at least two outer teeth, wherein said outer teeth may be narrower than said inner tooth.
[0065] FIGS. 16-18 show a partially assembled rotary cutting assembly 1 with the cutting blade assemblies 5 spaced apart. The cutting blade assemblies in this preferred embodiment are spaced apart by the hubs 7 in outer cutting blades 6 . The teeth 4 are displaced in the longitudinal direction to form a helix. If the teeth were aligned, then a greater force would be required to punch through paper. By displacing the teeth, a lesser, constant force is required. Though a helix is described herein, any configuration may be used such that the teeth are not aligned. In addition, it may be possible to have varying numbers of teeth around the circumference of each cutting assembly, such that some cutting assemblies have two sets of teeth around its periphery and others have three sets or more.
[0066] FIGS. 19 and 20 show the interaction between two rotary cutting assemblies 25 . As paper is fed between the two assemblies, it is shredded into rectangles. The width of the rectangle is determined by the space between the cutting blade assemblies created by the hubs. The length of the rectangle is determined by the distance between the teeth around the circumference of the cutting blade. Though the size can vary, an exemplar shredded piece of paper is 4 mm by 40 mm.
[0067] FIGS. 21-25 disclose another preferred embodiment of the present invention. In this embodiment the components are essentially the same as above, except that the cutting blade assembly does not have a hub protruding from it. Since there is no hub to create space between the cutting blade assemblies, a separate spacer 26 is needed to separate the cutting blade assemblies. (See FIGS. 29 & 30 .)
[0068] As seen in FIGS. 26-33 , this preferred embodiment also discloses paper strippers 27 which are coupled to the spacer 26 . Both the paper strippers 27 and the spacer 26 are commonly known to those skilled in the art. The paper strippers facilitate the papers shreds to fall downward into the shredder base, and also prevent the paper from accumulating between the cutting blade assemblies. Though the paper strippers were not shown in the previous embodiment, a fully assembled shredder utilizing the rotary cutting assembly above would preferably have the paper strippers coupled to the hubs between the cutting blade assemblies.
[0069] Other preferred embodiments are also possible. For example, the principle of three or more adjacent teeth can also be applied to Diamond Cut shredders.
[0070] Although the present invention has been described in detail with respect to certain preferred versions thereof, other versions are possible. Therefore, the scope of the claims should not be limited to the description of the preferred versions contained herein.
|
The present invention relates generally to cutting blades for shredders. Specifically, this invention teaches cutting blades and a rotary cutting assembly which reduce the power needed to shred paper, plastic, and other forms of media that hold information. This is accomplished by creating a cutting blade with at least three adjacent teeth. The formation of three or more adjacent teeth more readily tears through paper and other media thus reducing the amount of power necessary to drive a shredder.
| 1
|
PRIORITY CLAIM
[0001] This application is related to and claims priority under 35 U.S.C. §119(e) to a commonly assigned provisional patent application entitled “The Split Tank Toilet System” by Nicholas Nguyen, Attorney Docket Number NICK-P001P1, application Ser. No. 61/182,714, filed on May 30, 2009, which is incorporated by reference herein.
BACKGROUND OF THE INVENTION
[0002] The toilet is one of the most vital household items. The toilet is a china bowl and tank system designed to remove wastes and prevent sewer gases from entering the home, and the toilet does its job well.
[0003] A toilet's entire system is controlled by the flush lever. When the lever is pulled, a chain rises, lifting a flush valve (flap) and causing about three gallons of water to rush from the tank through a drain hole into the bowl. As the water rushes into the bowl, the force of the water cleans the bowl and forces the waste down and out into the sewers. The bowl's water is then replaced with water flowing from the tank to the bowl through an overflow tube.
[0004] As the water level of the tank lowers, a float ball attached to the ballcock lowers, and activates a ballcock. The ballcock is a mechanism that refills the toilet tank's water level. When the ballcock activates, water flows into the tank, and as the water level rises, so does the float ball. When the float ball is raised enough, the ballcock shuts off. The process repeats the next time someone flushes.
[0005] According to the United States Geological Survey, an average toilet tank of 3 gallons is flushed. This means that According to Aquacraft, Inc. and the American Waterworks Association Research Foundation, The average person uses around 18 gallons/day flushing the toilet. In the United States alone, that translates to about 2 trillion gallons of water being flushed “down the toilet” a year. If the water usage can be reduced, water can be conserved for future generation.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0006] The present invention is illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings and in which like reference numerals refer to similar elements and in which:
[0007] FIG. 1 shows, in an embodiment of the invention, a top view of the split-tank toilet system.
[0008] FIG. 2 shows, in an embodiment of the invention, a front view of the split tank toilet system (with both flaps open).
[0009] FIG. 3 shows, in an embodiment of the invention, a front view of the split tank toilet system with one flap opens.
[0010] FIG. 4 shows, in an embodiment of the invention, a front view of the split tank toilet system with all flaps close.
DETAILED DESCRIPTION OF EMBODIMENTS
[0011] The present invention will now be described in detail with reference to a few embodiments thereof as illustrated in the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without some or all of these specific details. In other instances, well known process steps and/or structures have not been described in detail in order to not unnecessarily obscure the present invention.
[0012] Various embodiments are described hereinbelow, including methods and techniques. It should be kept in mind that the invention might also cover articles of manufacture that includes a computer readable medium on which computer-readable instructions for carrying out embodiments of the inventive technique are stored. The computer readable medium may include, for example, semiconductor, magnetic, opto-magnetic, optical, or other forms of computer readable medium for storing computer readable code. Further, the invention may also cover apparatuses for practicing embodiments of the invention. Such apparatus may include circuits, dedicated and/or programmable, to carry out tasks pertaining to embodiments of the invention. Examples of such apparatus include a general-purpose computer and/or a dedicated computing device when appropriately programmed and may include a combination of a computer/computing device and dedicated/programmable circuits adapted for the various tasks pertaining to embodiments of the invention.
[0013] The inventor herein realized that liquid waste requires less water to flush away than solid waste. In accordance with embodiments of the invention, a split tank toilet system is provided for conserving water while providing sufficient water to remove waste from the toilet. Embodiments of the invention include a modified tank in which the tank is divided into two half-tanks. Embodiments of the invention also include modifying the lever unit to enable the half-tanks to be emptied according to usage.
[0014] In an embodiment of the invention, a split tank toilet system is provided for removing waste while conserving water. The split tank toilet system provides for a standard toilet to be divided into two half-tanks utilizing an internal wall (e.g., barrier), in an embodiment. The internal wall is a moldable component that may be inserted into the tank to split the tank into two half-tanks. To hold the internal wall in place, rubber edges may be positioned around the outside of the internal wall, thereby holding the internal wall in place when the internal wall is inserted into the tank. Since the internal wall is moldable, the internal wall may bend slightly as the two rubber edged sides of the internal wall pushes against the toilet tank wall. As can be appreciated from the foregoing, the standard toilet does not have to be divided into half-tank of equal size. Instead, the internal wall may be installed according to a user's configuration
[0015] When the lever is activated (e.g., pulled, pushed, etc.), the conventional refill system is activated. As the float ball lowers and the ballcock provides water to the tank, the first half-tank is refilled, in an embodiment. When the water reaches an overspill level, the water flows into the second half-tank. In an embodiment, the overspill level may be the top of the internal wall. In this embodiment, the internal wall is configured to be lower than the maximum water level, which is the level at which the ballcock shuts off. In an example, water will fill the first half-tank until it overflows over the top of the internal wall into the second half-tank. Once the water on both sides is above the top of the internal wall and has reached the maximum level, the float ball raises and the ballcock shuts off.
[0016] In another embodiment, the internal wall includes an overspill hole. When the internal wall is inserted into place within the tank, the overspill hole is positioned below the maximum water level, in an embodiment. As the tank is being refilled, the water flows into the first half-tank. When the water reaches the overspill hole, the water flow through the overspill hole into the second half-tank. The water will continue to spill into the second half-tank until the water level in both tanks is above the overspill hole. Once the water in at least the first half-tank has reached the maximum water level, the float ball raises and the ballcock shuts off.
[0017] When the toilet is used, water flows into the china bowl from the tank to flush away the waste. In an embodiment, a two-flap arrangement is provided. Each flap is located in each tank. In an example, the first flap is positioned in the first half-tank and is positioned over the drain hole. The second flap is positioned in the second half-tank and is positioned over a second drain hole.
[0018] Different arrangements for emptying at least part of the water from the tank to flush away the waste may be provided. In one embodiment, a three lift-arms lever arrangement may be provided. In a three lift-arms lever arrangement, a single rotating arm with three lift arms are attached to a handle, in an embodiment. The single rotating arm may extend from one side of the tank (at the handle side) to at least part of the second half-tank side. lithe tank includes an internal wall that has a height less than the maximum water level, the single rotating arm may rest on the top side of the internal wall. In an embodiment, the single rotating arm may be extended without resting on the top side of the internal wall for support if the single rotating arm is made of a more rigid material. If the tank includes an internal wall that has an overspill hole, the internal wall may also include a small gap for inserting the single rotating arm, thereby enabling the single rotating arm to extend from the handle into the second half-tank.
[0019] Unlike the prior art, the first flap (which may be the existing flap in a standard toilet tank) is connected to two chains, which are connected to two opposing lift arms (first lift arm and second lift arm). The two lift arms are attached to the single rotating arm. The second flap, in an embodiment, is connected to a chain, which is connected to a third lift arm. In an embodiment, the third lift arm is parallel to the first lift arm. Both the first and the third lift arm are facing in the direction toward the china bowl, in an embodiment. The second lift arm is positioned in the direction facing away from the china bowl.
[0020] Consider the situation wherein, for example, a user of a toilet needs to remove liquid waste from the china bowl. The user may move the handle in a first direction. The single rotating arm rotates causing the second lift arm to move in an upward position, thereby causing the first flap to open up and the water to flow from the first half-tank into the china bowl to flush away the liquid waste. Since only the water from the first half-tank has been emptied in this example, less water is utilized.
[0021] If the user needs to remove solid waste from the china bowl, the user may move the handle in a second direction. The single rotating arm rotates causing the first and third lift arms to move in an upward direction. The water from the second half-tank rushes into the first half-tank, thereby allowing water from both half-tanks to flow into the china bowl to flush away the solid waste.
[0022] In another embodiment, instead of having a single rotating arm, two rotating arms are' provided. Each rotating arm is attached to a handle. In an example, the first rotating arm is attached to a first handle and the second rotating arm is attached to a second handle. The first rotating arm is attached to the first flap and is employed to rotate the first flap upward to flush away liquid waste, in an embodiment. The second rotating arm is attached to both the first and second flaps and is employed to rotate both flaps to flush away solid waste, in an embodiment.
[0023] The features and advantages of the present invention may be better understood with reference to the figures and discussions that follow.
[0024] While the conventional toilet operates using one tank, the design of the new toilet uses a split-tank system operating upon the same principles as the conventional toilet. FIG. 1 shows, in an embodiment of the invention, a top view of the split-tank toilet system. FIG. 2 shows, in an embodiment of the invention, a front view of the split tank toilet system (with both flaps open). FIG. 3 shows, in an embodiment of the invention, a front view of the split tank toilet system with one flap opens. FIG. 4 shows, in an embodiment of the invention, a front view of the split tank toilet system with all flaps close.
[0025] The tank (A), however, is separated in half by a wall or barrier (B). More importantly, the new toilet can provide two different flush amounts of water: a smaller amount for liquid waste and a larger amount for solid waste.
[0026] When the lever (C) is pulled, the conventional refill system activates. However, when the float ball (conventional and not shown) lowers and the ballcock (conventional and not shown) provides water to one of the tanks (for example D), the water pours into the first tank (D), overflows, and fills the second tank (E), thereby leveling out the water levels above the barrier (B). When the water level in both tanks raises sufficiently, the float ball raises, and the ballcock shuts off.
[0027] Besides the changes mentioned above, the new toilet design has a two-flap system. One flap is located in each tank. A single rotating arm (F) is provided and is attached to the lever (C). This single rotating arm (F) has, on one side of rotating arm (F), two lift arms (G and H). On the other side of rotating arm (F) is another lift arm (I). One flap (J) is attached to lift arms (H) and (I) using chains (K) and (L) respectively. Another flap (M) is attached to lift arm (G) using a chain (N). If the lever (C) is turned one way, both flaps (J) and (M) will opened by lift arms (G) and (H), and if the lever (C) is turned the other way, only one flap (J) opens.
[0028] The split-tank system is very flexible. If there is no solid waste, then turn the lever one way to lift only one valve (J) and provide the half tank (D) flush. If the lever is turned the other way, both valves (J) and (M) lift, forcing both half tanks (D) and (E) out, providing enough force to flush solid waste. Then both half tanks (D) and (E) refill, and the toilet is ready for use again.
[0029] Best of all, the split tank does not require a new toilet or new tank. Only internal parts of the tank need to be changed, and these changes involve adding an internal wall (B) with a built-in flap seal seat (P), a flap (M), and a new rotating lever arm (F) with attached lift arms (G, H, and I), and chains (K, L, N) to connect to the flap valves (M and J).
[0030] According to the United States Geological Survey, the average person uses 80-100 gallons a day. Of that, flushing the toilet is the number one usage of water. As mentioned above, an average person uses around 18 gallons/day flushing the toilet with the conventional toilet. That is 6 flushes per day.
[0031] If a person only releases liquid waste for one day using a conventional toilet, based upon the facts above, he would have flushed 18 gallons of water that day, having used the toilet six times. Surely 18 gallons of fresh water is not needed to flush liquid waste!
[0032] Now, if that person uses a split-tank toilet, and only releases liquid waste, and the split tank contains two halves of a full tank, then he would use only half of a tank each time he flushes. Thus, he saves 9 gallons of water, even though he went the same six times. if everyone in San Diego (population est. 1.3 million), for example, uses a split-tank toilet, they would save over 10 million of water a day.
[0033] While this invention has been described in terms of several preferred embodiments, there are alterations, permutations, and equivalents, which fall within the scope of this invention. It should also be noted that there are many alternative ways of implementing the methods and apparatuses of the present invention. Although various examples are provided herein, it is intended that these examples be illustrative and not limiting with respect to the invention.
|
An toilet arrangement having two flow rates is provided. The toilet arrangement includes a lever having two positions, wherein said lever being disposed in a first location, a first amount of water is released by a valve, and wherein said lever is being disposed in a second location, a second amount of water is released by said valve.
| 4
|
This application is a continuation of application Ser. No. 808,787, filed 12/13/85, now abandoned.
BACKGROUND OF THE INVENTION
The invention is a telephone line interface employed for coupling an electronic device, hereinafter main module, to a public telephone (PT) network, and is, therefore, subject to a large set of telephone interconnect regulations. Examples of such main modules include modems, telephone message systems, video-text storage systems, or, as in the preferred embodiment, a text-to-speech device. In the United States and Canada, meeting these regulations is quite straightforward (the regulations in the United States and Canada are essentially the same). However, in the rest of the world, there are many countries with different (and frequently changing) regulations. Additionally, the regulations can be plain barrier regulations.
In general, the problem of PT interconnect is solved by modifying the main module to conform to a particular country's regulations. In every prior solution, the main module is involved in some way with making the system conform to the regulatory issues. This coupling is unpleasant. A dependency between the main module and an option module is disadvantageous because it means that the option module may have to be recertified any time a change to the the main module is made. Since the base module changes with each language, many different combinations of base module and option module are possible.
SUMMARY OF THE INVENTION
The invention eliminates the dependency between the main module and the interfacing option module. In a preferred embodiment, the option module employs a small computer, wherein the option module is made responsible for all of the details of the interface to the telephone network. If an option module is present, the main module defers all judgment about telephone interfacing to the option module.
The option module is an independent piece of hardware employing a programmable CPU. The option module can even be certified on a test fixture. The main module cannot do anything to make the option module do something illegal on the telephone line. The main module can be changed at will, and the telephone certification is not compromised. In addition, the telephone interface module can be re-used. Any time a telephone product is built, the standard option module for a given country is used, and a certified product is produced.
Uncoupling the two modules provides for independent development of telephone line interfaces and main modules. Developers of main modules can work without any concern for the details of the telephone line interface option modules. Developers of telephone line interfaces can also work in isolation. If a country changes its regulations, then the developer for that country's telephone line can react to it, without any effect on any other telephone line interface option.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram illustrating the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The invention is an apparatus (option module) for interfacing an electronic device (main module) to a telephone network. The invention contemplates that the main module, in a preferred embodiment, is a text-to-speech device. The interconnection of an electronic device with the telephone network is generally controlled by government regulations. Since there are many governments, there are many different sets of regulations. The option module is an implementation of a telephone line interface that isolates a main module, in particular, a text-to-speech device, from different and/or changing regulations.
FIG. 1 illustrates a main module 10, representing a text-to-speech device, coupled to a telephone network by a telephone line interface option module 50. The main module is shown to have a microprocessor 15, and the option module is shown to have a microprocessor 55; however, it would be possible to build both the main module 10 and option module 50 without microprocessors. The microprocessor 15, in the preferred embodiment, is an Intel 80186. Telephone line interface circuitry 51 is the physical connection between the phone system network and the option module. This circuitry ensures compliance with the electrical connection requirements of the telephone regulations.
The computer on the option module stores inputted microcode that is responsible for enforcing telephone regulations. The microcode can be changed so that the option module conforms to different or varying regulations. These regulations are usually in the form of escape sequences in which the main module is disconnected from the telephone network. The main module employs microcode, running on the microprocessor is, which determines if an option module is present. When the option module is connected, the main module relinquishes responsibility for handling these escape sequences to the option module.
There is also a channel in the reverse direction (from the option module to the main module) so that the option module can send replies to the host. The main module provides formatting services, but essentially nothing else.
The main module 10 and the option module 50 communicate with each other by sending information packets, with predefined formats, through a physical communication link. The packets are between 1 and 255 bytes in length. The physical communication link comprises a series of three bus structures, including a main module bus 25, an interconnect bus 30 and an option module bus 60. The transmission of the information packets is conducted in conformance with the stored regulations on the option module.
A bus buffer 20, located on the main module 10, couples the main module bus 25 to the interconnect bus 30. A buffer 61 comprising an outbound register 65 and an inbound register 70, both located on the option module 50, couple the option module bus 60 to the interconnect bus 30. This interface is implemented by two connectors located on the main module, wherein a pair of plugs located on the option module connect. The buffer 61 has an option port 63 coupled to the option module bus 60, a main port 64 coupled to the interconnect bus 30, and a control port 66 for coupling control signals from the microprocessor 15 and the microprocessor 55.
A protocol is used to actually transport data between the modules. This protocol initiates, as well as monitors, transfers of data. Microcode, stored in microprocessor 55, represents the telephone interconnect regulations for a particular country and ensures that the protocol is followed. The microprocessor 55, running the microcode, determines when information should be transmitted and generates control signals to implement the telephone regulations.
The outbound register 65 stores data that is flowing from the main module 10 to the option module 50. The data is written by the main module, and read by the option module. The main module initiates an outbound transfer after waiting until the outbound register 65 is empty. Waiting is necessary as the outbound register 65 may still contain the last byte of the last outbound transfer. There are some electronics, not illustrated, that generate a flag control signal. The flag signal is set TRUE when the main module writes data, and set FALSE by the option module when data is read by the option module. The flag serves to tell the option module microprocessor 55 that there is a packet size byte of data waiting in the outbound register 65 for reading.
The inbound register 70 stores data transmitted from the option module to the main module. The data is written by the option microprocessor 55 and read by the main microprocessor 15 through the bus buffer 20. There is a similar flag, a second control signal, set TRUE by an option module write and set FALSE by a main module read, which notifies the main module that there is data in the inbound register.
The option microprocessor 55, because it is dedicated to a control task, can poll the flag control signal associated with the outbound register 65, to determine if there is any data to be read. The main microprocessor 15 is not dedicated to control functions, and therefore, polling the inbound register is not feasible. The invention employs alert logic 75 for keeping both of the microprocessors 15 and 55 abreast of the status of information flow. The option microprocessor 55, having data for the main microprocessor 15, transfers the data to the inbound register 70. A request alert command signal 80 is then generated by the option microprocessor 55. This signal 80 is inputted to the alert logic 75. In response, the alert logic 75 sends an alert signal 35 to the main processor 15 to alert the main processor 15 that the data is present. The main processor is then interrupted. The main processor uses the "cancel alert command" signal 40 to make the alert signal go away (it has noticed it already), and then it reads the data from the inbound register, using the flag to decide when each byte in the packet is available.
The data packets are of variable length. The first data byte is always an opcode byte. This byte, in addition to specifying the function of the packet, implicitly determines the format of the remaining data in the packet.
The option module controls the rate at which the main module sends data to the telephone network. After an outbound packet is sent, the main module waits for a proceed packet before sending another outbound packet. This permits the option module to control the rate at which data is interfaced between the main module and the telephone network.
It is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described.
|
36 Telephone interface option module circuit for interfacing an electronic device to a telephone network. Most electronic devices, for example, modems, telephone message systems and text-to-speech systems, when coupled to a telephone network must conform to specific telephone interconnect regulations. These regulations generally vary from country to country, and therefore, the electronic device generally has to be modified to conform to a specific countries telephone regulations. The option module circuit contains the country specific telephone regulations, and when plugged into the electronic device, ensures that the electronic device conforms to those regulations.
| 8
|
[0001] This is a continuation-in-part of co-pending application Ser. No. 12/606,762 filed Oct. 27, 2009 which was a continuation-in-part of application Ser. No. 12/437,749 filed May 8, 2009 which was a continuation-in-part of co-pending application Ser. No. 12/151,899 filed May 9, 2008 which claimed priority to U.S. Provisional application No. 61/124,586 filed Apr. 17, 2008. Application Ser. No. 12/606,762 also claimed priority from U.S. Provisional application No. 61/135, 058 filed Jul. 16, 2009 and U.S. Provisional application No. 61/249,090 filed Oct. 6, 2009. Application Ser. Nos. 12/606,762, 12/437,749, 12/151,899, 61/124,586, 61/135,058 and 61/249,090 are hereby incorporated by reference.
BACKGROUND
[0002] 1. Field of the Invention
[0003] The present invention relates generally to the field of amines and more particularly to a classes of amines used as buffers in biological systems.
[0004] 2. Description of the Problem Solved by the Invention
[0005] Amines are very useful compounds in the buffering of biological systems. Each class of amine has various limitations which require choosing an amine based on multiple factors to select the best amine. For example, pH buffering range is typically most important, but issues of chelation, and pH range stability, and solubility also come into play. Typically, a suboptimal buffer will result in yields that are well below the potential yield. The invention disclosed improves the yields in fermentation and purification, and improves shelf stability of proteins and amino acids.
SUMMARY OF THE INVENTION
[0006] The present invention relates to amines and amine derivatives that improve the buffering range, and/or reduce the chelation and other negative interactions of the buffer and the system to be buffered. The reaction of amines or polyamines with various molecules to form polyamines with differing pKa's will extend the buffering range, derivatives that result in polyamines that have the same pKa yields a greater buffering capacity. Derivatives that result in zwitterionic buffers improve yield by allowing a greater range of stability.
DESCRIPTION OF THE FIGURES
[0007] Attention is now directed to the following figures that describe embodiments of the present invention:
[0008] FIG. 1 shows the derivation of polyamines and zwitterionic buffers from tromethamine.
[0009] FIG. 2 shows the derivation of zwitterionic buffers and polyamines from aminomethylpropanol.
[0010] FIG. 3 shows the reaction of 2-methyl-2-nitro-1-propanol with acrylonitrile and its derivatives.
[0011] FIG. 4 shows the reaction of 2-nitro-2-ethyl-1,3-propanediol with acrylonitrile and its derivatives where x,y,and n are all integers where x and y are chosen independently, such that x+y=n and n is greater than zero.
[0012] FIG. 5 shows the reaction of 2-nitro-2-methyl-1,3-propanediol with acrylonitrile and its derivatives where x,y,and n are all integers where x and y are chosen independently, such that x+y=n and n is greater than zero.
[0013] FIG. 6 shows the reaction of tris(hydroxymethyl)nitromethane with acrylonitrile and its derivatives where x,y, z, and n are all integers where x, y and z are chosen independently, such that x+y+z=n and n is greater than zero.
[0014] FIG. 7 shows the reaction of 2-nitro-1,3-propanediol with acrylonitrile and its derivatives where x,y,and n are all integers where x and y are chosen independently, such that x+y=n and n is greater than zero.
[0015] FIG. 8 shows the reaction of 2-nitro-1-butanol with acrylonitrile and its derivatives.
[0016] FIG. 9 shows FIG. 9 shows alkoxylation of aminomethylpropanol.
[0017] FIG. 10A shows the synthesis of a very mild, high foaming, surfactant derived from MCA.
[0018] FIG. 10B shows the synthesis of a very mild, high foaming, surfactant derived from SVS.
[0019] FIG. 11 shows the synthesis of a series of buffers with 2-nitropropane as the starting material.
[0020] FIG. 12 shows FIG. 12 shows the synthesis of a series of buffers with 1-nitropropane as a starting material where n and m are integers where m+n is greater than zero and n is greater than or equal to m.
[0021] FIG. 13 shows the synthesis of a series of buffers with nitroethane as a starting material where n and m are integers where m+n is greater than zero and n is greater than or equal to m.
[0022] FIG. 14 shows the synthesis of a series of buffers with nitromethane as a starting material where x,y,z and n are integers and x+y+z=n and n is greater than zero.
[0023] FIG. 15 shows the synthesis of a series of zwitterionic buffers based on acrylic acids.
[0024] FIG. 16 shows the synthesis of a zwitterionic sulfonate based on tromethamine.
[0025] FIG. 17 shows the synthesis of a zwitterionic sulfonate based on aminomethylpropanol.
[0026] FIG. 18-25 show the synthesis of families of zwitterionic buffers from nitroalcohols.
[0027] FIG. 26 shows the synthesis of zwitterionic buffers from morpholine.
[0028] FIG. 27 shows the synthesis of zwitterionic buffers from hydroxyethyl piperazine.
[0029] FIG. 28 shows the synthesis of zwitterionic buffers from piperazine.
[0030] FIG. 29 shows the synthesis of zwitterionic buffers from ethyleneamines.
[0031] FIG. 30 shows the synthesis of a zwitterionic buffer with primary, secondary, tertiary, or quaternary amine functionality.
[0032] FIGS. 31-33 show the synthesis of mild zwitterionic surfactants from nitroalcohols.
[0033] FIG. 34-37 show the synthesis of polyamines from nitroalcohols.
[0034] FIG. 38 shows the synthesis of diamines from nitroalcohols and aminoalcohols.
[0035] FIG. 39 shows the synthesis of isopropyl amine acrylate buffers and mild surfactants.
[0036] FIG. 40 shows the synthesis of zwitterionic buffers from SVS and MCA derived from isopropyl amine as well as mild surfactants and diamines.
[0037] FIG. 41 shows the synthesis of a sultaine zwittterionic buffer of isopropyl amine.
[0038] FIG. 42 shows the synthesis of zwitterionic buffers from amino alcohols and itaconic acid.
[0039] FIG. 43 shows the synthesis of nitro acids from nitroalcohols and itaconic acid.
[0040] FIG. 44 shows the synthesis of primary amino zwitterionic buffers from nitro acids.
[0041] FIG. 45 . shows the synthesis of a family of zwitterionic buffers from itaconic acid and amines.
[0042] FIG. 46 shows the synthesis of surfactants from amines and itaconic acid intermediates.
[0043] FIG. 47 shows the synthesis of nitroacids from nitroparaffins and itaconic acid.
[0044] FIG. 48 shows the synthesis of zwitterionic buffers from nitro acids.
[0045] FIG. 49 shows the synthesis of zwitterionic buffers from 4-aminopyridine.
[0046] FIG. 50 shows the synthesis zwitterionic buffers from the ketimine conformation of 4-aminopyridine.
[0047] FIG. 51 shows the synthesis of zwiiterionic sultaines from 4-aminopyridine.
[0048] Several drawings and illustrations have been presented to aid in understanding the invention. The scope of the present invention is not limited to what is shown in the figures.
DETAILED DESCRIPTION OF THE INVENTION
[0049] Combining amines with monochloroacetic acid (MCA)or sodium vinyl sulfonate (SVS) results in products are zwitterionic buffers that can buffer in both acidic and basic pH conditions. A limited number amines are currently used for this purpose, such as, tromethamine and ammonia. The reaction of amines, alcohols, and aminoalcohols with acrylonitrile (via the Michaels Addition), followed by reduction results in amines and polyamines that have a broad buffering range. The further derivatization of the amines and polyamines with MCA and SVS yields a further crop of amine buffers with desirable properties. One skilled in the art will recognize that MCA and sodium monochloroacetic acid (SMCA) can be used interchangeably.
[0050] The reaction of tromethamine as described above yields the products in FIG. 1 . In step 1 in FIG. 1 where the acrylonitrile is added to the amine a branched structure wherein the addition of acrylonitrile results in a tertiary amine is shown. In reality, particularly when n is greater than 1, a mixture of products is obtained that is both tertiary and secondary. For the invention disclosed herein, n may equal any integer greater than zero, including 1. Controlling the reaction temperature, pressure and agitation will allow the mixture to be predominately secondary (such as when m=n) or tertiary amine, m can be any integer less than or equal n. Furthermore, this selection can take place in adding acrylonitrile to the amine that results, allowing a progressively more branched product. It is within the scope of the invention disclosed herein to include these additional types of products and their subsequent derivatives described herein.
[0051] With regard to the reaction of the polyamine resulting from the second step in FIG. 1 . FIG. 1 shows the addition of only one mole of SVS or MCA, it is known in the art, that a second mole may be added to obtain a product with a second zwitterionic group. Furthermore, in the case where the product has repeated additions of acrylonitrile and reduction to the amines, the branched products may have many more zwitterionic groups. Also, it is to be noted that, while the sulfonates are shown as sodium salts, other salts and the free acids (non-salted form) are also within the scope of this invention.
[0052] Other amines that would make excellent starting materials in place of tromethamine are 2-amino-2-methyl-1-propanol, 2-amino-1-butanol, 2-amino-2-ethyl-1,3-propanediol, 2-amino-2-methyl-1,3-propanediol, and dihydroxymethylaminomethane.
[0053] Additionally, fatty amines, such as lauryl amine, coco amine, tallow amine, and oleoyl amine, and fatty ether amines, such as bis-(2-hydroxyethyl)isodecyloxypropylamine, when reacted with SVS produce mild surfactants that find utility where zwitterionic surfactants are desired, including personal care.
[0054] Other amines that are shown in FIG. 2 are produced via a similar series of reactions, except that FIG. 2 includes zwitterionic buffers from the amine 2-amino-2-methyl-1-propanol, as well as the polyamines derived from the reaction with acrylonitrile and the subsequent derivatives described above. Other amines can be utilized in addition to 2-amino-2-methyl-1-propanol to obtain excellent buffers are 2-amino-1-butanol, 2-amino-2-ethyl-1,3-propanediol, 2-amino-2-methyl-1,3-propanediol, and dihydroxymethylaminomethane. Reaction conditions could be created such that the alcohol groups on the amines listed above could be reacted with acrylonitrile as well, and then reduced to the amines and, if desired, reacted with SVS or MCA to impart zwitterionic character.
[0055] Polyamines with good properties for use in biological fermentations, purifications, storage and general handling can also be produced through the reaction of nitroalcohols and acrylonitrile, followed by reduction. Additional derivatization with SVS or MCA will result in zwitterionic buffers with a very large buffering range and capacity.
[0056] FIG. 3 shows the reaction of 2-methyl-2-nitro-1-propanol with acrylonitrile and its derivatives.
[0057] FIG. 4 shows the reaction of 2-nitro-2-ethyl-1,3-propanediol with acrylonitrile and its derivatives where x,y,and n are all integers where x and y are chosen independently, such that x+y=n and n is greater than zero.
[0058] FIG. 5 shows the reaction of 2-nitro-2-methyl-1,3-propanediol with acrylonitrile and its derivatives where x,y,and n are all integers where x and y are chosen independently, such that x+y=n and n is greater than zero.
[0059] FIG. 6 shows the reaction of tris(hydroxymethyl)nitromethane with acrylonitrile and its derivatives where x,y, z, and n are all integers where x, y and z are chosen independently, such that x+y+z=n and n is greater than zero.
[0060] FIG. 7 shows the reaction of 2-nitro-1,3-propanediol with acrylonitrile and its derivatives where x,y,and n are all integers where x and y are chosen independently, such that x+y=n and n is greater than zero.
[0061] FIG. 8 shows the reaction of 2-nitro-1-butanol with acrylonitrile and its derivatives.
[0062] FIGS. 2 through 8 are subject to the same clarifications as FIG. 1 with regard to the cyanoethylation and the formation of a more linear or branched structure as well as the addition of SVS or MCA in molar equivalents of primary amine groups or less than molar equivalents of primary amine groups present.
[0063] The buffers described thus far may also be ethoxylated, propoxylated, or butoxylated to modify their properties. Ethoxylation will tend to impart surfactancy to the resulting product. Propoxylation will add surfactancy, but also reduce the water solubility. This is useful in emulsion breaking and reverse emulsion breaking, this will also find utility in breaking up and dissolving biofilms. This is also desired in oil-field applications. Butoxylation will similarly shift the HLB to the hydrophobic. Combinations of ethoxylation, propoxylation, and butoxylation can be tailored to specific emulsion and reverse emulsion forming and breaking requirements. FIG. 9 shows alkoxylation of aminomethylpropanol. The direct 2 mole ethoxylation of 2-amino-2-methyl-1-propanol with 2 moles of ethylene oxide, as shown in FIG. 9 produces an excellent biological buffer with less chelation than 2-amino-2-methyl-1-propanol. The reaction of 2-amino-2-methyl-1-propanol with propylene oxide or butylene oxide yields a similarly less chelating product, as does the reaction with diethylene glycol. The reaction product of 2-amino-2-methyl-1-propanol with 1 mole of diethylene glycol as shown in FIG. 9 produces an ideal amine for gas scrubbing of H 2 S. This product is particularly useful because it does not bind to carbon dioxide and carbon monoxide in any appreciable amount. Thus making it ideal for tail gas scrubbing and maximizing the capacity of sulfur plants in refineries. Similar performance is seen with the reaction of the following amines 2-amino-1-butanol, 2-amino-2-methyl-1,3-propanediol, 2-amino-2-ethyl-1,3-propanediol, tris(hydroxylmethyl)aminomethane, and 2-amino-1,3-propanediol.
[0064] The buffers described herein also make excellent starting materials for surfactants. FIG. 10 shows the synthesis of 2 very mild, high foaming, surfactants that are well suited for personal care applications were irritation is problematic, such as baby shampoo and face cleansers. Similar results are seen when 2-amino-1-butanol, 2-amino-2-methyl-1,3-propanediol, 2-amino-2-ethyl-1,3-propanediol, tris(hydroxylmethyl)aminomethane, and 2-amino-1,3-propanediol are used as the starting material in place of 2-amino-2-methyl-1-propanol.
[0065] Polyamines with good properties for use in biological fermentations, purifications, storage and general handling can also be produced through the reaction of nitroalkanes and acrylonitrile, followed by reduction. Additional derivatization with SVS or MCA will result in zwitterionic buffers with a very large buffering range and capacity. FIG. 11 shows the synthesis of a series of buffers with 2-nitropropane as the starting material. FIG. 12 shows the synthesis of a series of buffers with 1-nitropropane as a starting material where n and m are integers where m+n is greater than zero and n is greater than or equal to m. Branching can be imparted on the buffers described in FIGS. 11 through 14 for the polyamines that have greater than 3 amine groups by reducing the resulting nitrile or polynitrile to the polyamine and then reacting with more acrylonitrile and then reducing the resulting nitrile groups to amine groups. This can be done repeatedly. As in FIG. 1 , conditions can be chosen such that a more branched product results. A more linear product is produced by simply adding all the acrylonitrile in one step, and then reducing the resulting polynitrile to the polyamine. For FIGS. 12 through 14 , the zwitterionic products can be made by adding MCA or SVS as shown in FIGS. 2 through 8 .
[0066] FIG. 13 shows the synthesis of a series of buffers with nitroethane as a starting material where n and m are integers where m+n is greater than zero and n is greater than or equal to m. FIG. 14 shows the synthesis of a series of buffers with nitromethane as a starting material where x,y,z and n are integers and x+y+z=n and n is greater than zero.
[0067] Several descriptions and illustrations have been presented to enhance understanding of the present invention. One skilled in the art will know that numerous changes and variations are possible without departing from the spirit of the invention. Each of these changes and variations are within the scope of the present invention.
[0068] Another embodiment of the present invention is the synthesis of zwitterionic buffers with vinyl acids. FIG. 15 shows the synthesis of a family of zwitterionic buffers based on members of the acrylic acid family. However, other vinyl acids may be used. Vinyl acids such as acrylic, 3-butenoic acid, 4-pentenoic acid, and other carboxcylic acids with a double bond at the terminus. Carboxcylic acids with a triple bond at the terminus also can be utilized, similarly, an acid where the multiple bond is not at the terminus, such as hex-4-enoic acid, can also be utilized. However, due to the reduced commercial availability of such compounds, the preferred embodiment is the vinyl acid with a double bond at the terminus. One very large benefit of utilizing vinyl acids to make zwitterionic buffers is that the product does not need to be ion exchanged to produce a non-ionized form. In the market, both ionized, or sometimes called salted, and non-ionized forms sometimes called free acid or free base, are required. In situations where ionic strength must be very closely controlled, the non-ionized forms are more popular. For cases where increased water solubility and ease of solution are desired, the salted forms are preferred. It is understood to one skilled in the art, the present invention covers both the ionized and non-ionized forms of the buffers disclosed herein.
[0069] Another embodiment of the present invention is the sulfonate zwitterionic buffers derived from the reaction of an amine with an epichlorohydrin and sodium bisulfate condensate as described in FIG. 16 . It is understood by one skilled in the art that other sulfate salts can be utilized to arrive at the desired molecular structure and is included in the present invention. FIGS. 17 through 25 teach the flexibility of the present invention to synthesize a series of a amine sulfonate or amino acid zwitterionic buffers from nitroalcohols or alkanolamines to produce zwitterionic buffers that have primary amino functionality or secondary amino functionality. In cases where there are more than one reactive group, amine, alcohol, or a combination, multiple sulfonate groups or acid groups can be reacted by adding more than one equivalent of the vinyl acid or the oxirane containing sulfonate.
[0070] Another embodiment of the current invention is to make zwitterionic buffers with cylcoamines as the starting material. The cycloamines result in a tertiary amino group that is less chelating and interferes less in biological functions. FIG. 26 shows the reaction of morpholine with a vinyl acid and morpholine with the oxirane sulfonate. FIG. 27 teaches similar products, but utilizing hydroxyethyl piperazine. FIG. 28 teaches the use of diamines as starting materials by using piperazine as the starting material. This is a good example of a synthesis of polyzwittterionic buffers as discussed earlier. FIG. 29 teaches the use of ethylene amines to make zwitterionic buffers through reaction with vinyl acids or oxirane sulfonates. One skilled in the art will recognize that similar compounds can be made by using ethylene amines, such as monoethanolamine and the higher homologs, such as diethylenetriamine and is part of the invention disclosed herein.
[0071] Another embodiment of the current invention is the synthesis of zwitterionic amines that have primary, secondary, tertiary, and quaternary amine functionality. FIG. 30 teaches this via oxirane sulfonate and amines. It is obvious to one in the art that any primary, secondary, or tertiary amine can be used in place of the methyamines in FIG. 30 . While not shown in the figure, it is obvious to one skilled in the art that the resulting amines can be reacted further with vinyl acids, monochloroacetic acid, sodium vinyl sulfonate, or an oxirane sulfonate to further add acidic character to the zwitterionic buffer.
[0072] Another embodiment of the current invention is the synthesis of mild surfactants from nitroalcohols. FIGS. 31 through 33 teach the synthesis of these mild surfactants. Lower molecular weight acids produce lower foaming mild surfactants, whereas higher molecular weight carboxcylic acids yield higher foam. Lauric acid is the preferred embodiment for a high foaming, mild surfact. Coconut fatty acid performs similarly, but at a lower cost. A good surfactant with low foam can be made using octanoic acid as the carboxcylic acid.
[0073] Another embodiment of the current invention is the synthesis of polyamines from nitroalcohols. FIGS. 34 and 35 teach the synthesis of diamines from nitroalcohols. FIG. 34 teaches the synthesis with several hydroxyl groups present. It is understood by one skilled in the art that additional amino groups can be added by reacting more than one equivalent of epichlorohydrin to the nitroalcohol, up to the number of hydroxyl groups, and then reacting the same number of equivalents of amine to the oxirane containing amine. In the case where the nitroalcohol is reduced to the amino alcohol in the beginning, the addition of base, such as caustic, to the amino alcohol will assist in the reaction of the epichlorohydrin with the hydroxyl groups. Without the base, the epichlorohydrin will preferably react with the amine as outlined in the 1 equivelent addition depicted in FIG. 34 and FIG. 35 . FIG. 26 demonstrates that tertiary amines can be used to make zwitterionic buffers with quaternary amine functionality from tertiary amines. While not explicitly shown, any other tertiary amine can be used as the starting material and is part of the invention described herein. FIG. 37 and FIG. 38 demonstrate that diamines can be made from nitroalcohols by reacting sequentially the nitroalcohol with epichlorohydrin and then the second equivalent of the nitroalcohol, followed by reduction. Also taught is that a reduction step can take place in the beginning to yield a diamine with two secondary amino groups. It is understood by one skilled in the art that the nitroalcohols or alkanolamines do not need to be symmetric, but others may be used in the synthesis of the diamine and is part of the invention disclosed herein.
[0074] FIG. 42 teaches the synthesis of zwitterionic biological buffers from amino alcohols and itaconic acid. These buffers have two acid groups and increased buffering in the acidic range of pH 3-6. FIGS. 43 and 44 show the synthesis of zwitterionic buffers with primary amine groups. These buffers are preferred in applications such as personal care where secondary amines are seen as undesirable. The nitro diacids of FIG. 44 also have great utility as chemical intermediates when synthesizing bioactive molecules.
[0075] FIG. 45 teaches the synthesis of a family of zwitterionic buffers from itaconic acid. The buffers in FIG. 45 are not limited to amino alcohols as starting materials and provide a wide range of molecular size and solubilities.
[0076] FIG. 46 teaches the synthesis of a family of amphoteric surfactants. These surfactants are preferred for there mildness, ability to perform in hard water conditions and persistent lather when in the fatty tail is approximately 10-12 carbons in length. The R group in FIG. 46 is to encompass the fatty acid family of carbon chain lengths, generally from about 6 to about 22 carbons. In the specific cases illustrated of lauric amine and lauric dimethyl amine reacted with itaconic acid, it is understood by one in the art that any chain length amine can be used and is in within the scope of the invention herein. Particularly, but not limited to the fatty amines (carbon lengths of about 6 to about 22 carbons, branched and linear, saturated and unsaturated), isopropyl amine and butyl amine. The lower carbon chain lengths produce low foaming hard surface cleaners, while the carbon chains of about 8 to 10 tend to produce the most foam. Higher chain lengths find utility as mineral collectors in floatation processes such as those employed in iron and potash mining.
[0077] FIG. 47 shows the synthesis of nitro acids from nitroparaffins. As stated early, these are very flexible intermediates, particularly when synthesizing bioactive molecules. Reduction of the nitro acids, as shown in FIG. 48 produces zwitterionic buffers with primary amine character. In the case of nitroparaffins that have more than one hydrogen bound to the nitro bound carbon, more than one addition of the itaconic acid can occur. The substitution can occur up to the number of hydrogen atoms bound to the nitro bound carbon.
[0078] FIG. 49 shows the synthesis of zwitterionic buffers from 4-aminopyridine, FIG. 50 shows using the less stable ketimine conformation as the starting material. FIG. 51 shows the synthesis of sultaine type buffers from 4-aminopyridine. Additional buffers can be made by propoxylating and butoxylating 4-aminopyridine. The ethoxylating and propoxylating will reduce the water solubility and reduce the bioavailability. This is one method of extending the time a material is bioavailable by making it available slowly, particularly if the molecule is metabolized. Additionally, a triamine can be made by reacting 2-aminopyridine with arcrylonitrile and reducing it to the triamine, or reacting with allylamine to keep the aromatic nature of the six membered ring. The resulting buffers are excellent buffers in their own right, but also have great promise in treatment of multiple sclerosis, and other conditions that can benefit from calcium or other cation inhibition. The anionic components, in particular, are all groups that can chelate cations.
[0079] As outlined earlier, it is obvious to one skilled in the art that the resulting amines can be reacted further with vinyl acids, monochloroacetic acid, sodium vinyl sulfonate, or an oxirane sulfonate to further add acidic character to the zwitterionic buffer.
[0080] Several descriptions and illustrations have been presented to enhance understanding of the present invention. One skilled in the art will know that numerous changes and variations are possible without departing from the spirit of the invention. Each of these changes and variations are within the scope of the present invention.
|
Amines and amine derivatives that improve the buffering range, and/or reduce the chelation and other negative interactions of the buffer and the system to be buffered. The reaction of amines or polyamines with various molecules to form polyamines with differing pKa's will extend the buffering range, derivatives that result in polyamines that have the same pKa yields a greater buffering capacity. Derivatives that result in zwitterionic buffers improve yield by allowing a greater range of stability.
| 2
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is based on and claims priority from Korean Patent Application No. 10-2016-0056216, filed on May 9, 2016, the disclosure of which is incorporated herein in its entirety by reference for all purposes.
TECHNICAL FIELD
[0002] The present disclosure relates to refrigerators, and more particularly, to ice making and dispensing mechanisms in refrigerators.
BACKGROUND
[0003] A refrigerator is an appliance for use in storing food at a low temperature and may be configured to store food (or other items) in a frozen state or a refrigerated state depending on the type of food to be stored. The inside of the refrigerator is cooled by circulating cold air that can be continuously generated through a heat exchange process by using a refrigerant. During operation, the refrigerant goes through repetitive cycles of compression, condensation, expansion and evaporation in a heat exchanger. The cold air supplied in the refrigerator is uniformly distributed by convection. Accordingly, the items placed in the refrigerator can be stored at a desired low temperature.
[0004] The heat exchanger is installed in one side of the refrigerator and is isolated from the storage spaces such as the refrigeration room (or the refrigeration compartment) and the freezer for storing food. For example, compression and condensation processes may be performed by a compressor and a condenser disposed within a machine room located at the lower side of a rear surface of the refrigerator. In an evaporation process, the refrigerant may evaporate and thereby absorb heat from ambient air. As a result, the ambient air is cooled down.
[0005] A main body of the refrigerator may have a rectangular parallel-piped shape with an open front surface. Typically, the main body encloses a refrigeration room and freezer, each with its own door. The refrigerator may include a plurality of drawers, shelves, vegetable compartments, etc., for sorting and storing different types of items.
[0006] Conventionally, top mount type refrigerators were popular, with a freezer located at an upper side and a refrigeration room located at a lower side. Recently, bottom freezer type refrigerators have been developed, where a freezer is located at the lower side. A bottom freezer type refrigerator provides the advantage that a user can conveniently access the refrigerator in general. However, a user often needs to lower down or bend down to access the freezer, e.g., for taking ice from it.
[0007] Some bottom freezer type refrigerators have an ice dispenser located at the refrigeration room compartment disposed at the upper side of the refrigerator. An ice-making device for making ice pieces may be disposed on the refrigeration room door or inside refrigeration room. The ice-making device may include an ice-making unit including an ice tray, and an ice storage part (ice bucket) for storing the ice pieces produced in the ice tray.
[0008] When a certain amount of ice or more is contained in the ice storage part of the ice-making device (e.g., when ice storage part is full), it is desirable to detect the fullness status to pause ice making promptly.
SUMMARY
[0009] Embodiments of the present disclosure provide an ice-making device capable of suspending ice production based on a determination that an ice storage capacity of the ice-making device has been reached.
[0010] According to the embodiments of the present disclosure, an ice-making device can detect a fullness status of an ice storage unit and accordingly suspend ice production therein.
[0011] According to an embodiment of the present invention, an ice-making device for a refrigerator includes an ice-making unit configured to receive water and to produce ice pieces; an ice-storing unit configured to store the ice pieces produced in and fed from the ice-making unit; a sensing unit configured to measure an amount of the ice pieces filled in the ice-storing unit; and an accommodation unit configured to accommodate the ice-making unit and the ice-storing unit therein. The ice-storing unit includes: a bucket configured to store the ice pieces delivered from the ice-making unit; and a support part configured to movably support the bucket, the sensing unit being configured to sense relative movement of the bucket with respect to the accommodation unit.
[0012] Further, the sensing unit includes a magnetic sensor.
[0013] Further, the sensing unit includes: a target part disposed in the bucket; and a recognition part disposed in the accommodation unit, the recognition part being configured to sense relative movement of the target part with respect to the recognition part.
[0014] Further, the target part is disposed in a central region of a bottom surface of the bucket, and the recognition part is disposed in a corresponding relationship with the target part.
[0015] Further, elastic members configured to support the bucket are disposed between the bucket and the support part.
[0016] Further, the bucket includes bucket guides, and the support part includes support part guides configured to guide up-down movement of the bucket guides.
[0017] Further, the bucket is disposed with first elastic member guides configured to guide the elastic members at one side thereof, and the support part is disposed with second elastic member guides configured to guide the elastic members at the other side thereof.
[0018] Further, a slot extending in an up-down direction is formed in the bucket, and the ice-storing unit further includes a delivery member rotated to discharge the ice pieces existing within the bucket and disposed to pass through the slot.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] FIG. 1 is a front view illustrating the configuration of an exemplary refrigerator having an ice-making device according to one embodiment of the present disclosure.
[0020] FIG. 2 is a side view illustrating the configuration of an exemplary ice-making device for a refrigerator according to one embodiment of the present disclosure.
[0021] FIG. 3 is an exploded perspective view illustrating the configuration of the exemplary ice-making device in FIG. 2 .
[0022] FIG. 4 is a bottom perspective view illustrating the configuration of an exemplary bucket in the ice-making device illustrated in FIG. 2 .
[0023] FIG. 5 illustrates an exemplary method of controlling the ice-making device for a refrigerator.
[0024] FIG. 6 is an exploded perspective view of the exemplary ice-making device according to another embodiment of the present disclosure.
[0025] FIG. 7 is a bottom perspective view of an exemplary bucket in the ice-making device in FIG. 6 .
[0026] FIG. 8 is a block diagram illustrating control logic of an exemplary control unit according to one embodiment of the present disclosure.
DETAILED DESCRIPTION
[0027] In the following detailed description, reference is made to the accompanying drawings, which form a part hereof. The illustrative embodiments described in the detailed description, drawings, and claims are not meant to be limiting. Other embodiments may be utilized, and other changes may be made, without departing from the spirit or scope of the subject matter presented here.
[0028] One or more exemplary embodiments of the present disclosure will be described more fully hereinafter with reference to the accompanying drawings, in which one or more exemplary embodiments of the disclosure can be easily determined by those skilled in the art. As those skilled in the art will realize, the described exemplary embodiments may be modified in various different ways, all without departing from the spirit or scope of the present disclosure, which is not limited to the exemplary embodiments described herein.
[0029] It is noted that the drawings are schematic and are not dimensionally illustrated. Relative sizes and proportions of parts in the drawings may be exaggerated or reduced in size, and a predetermined size is merely exemplary and not limiting. The same reference numerals designate the same structures, elements, or parts illustrated in two or more drawings in order to exhibit similar characteristics.
[0030] The exemplary drawings of the present disclosure illustrate ideal exemplary embodiments of the present disclosure in more detail. As a result, various modifications of the drawings are expected. Accordingly, the exemplary embodiments are not limited to a specific form of the illustrated region, and for example, include a modification of a form due to manufacturing.
[0031] The term “fullness of ice pieces” used herein is not limited to a situation that an ice storage part 200 is completely filled with ice pieces. Thus, in the present disclosure, the term “fullness of ice pieces” is intended to include a situation where an ice storage part 200 is filled with a predetermined amount or more of ice and ice production stops accordingly.
[0032] The configurations of an ice-making device for a refrigerator according to one embodiment of the present disclosure and a refrigerator including the same will now be described with reference to FIGS. 1 to 5 .
[0033] FIG. 1 is a front view illustrating the configuration of an exemplary refrigerator having an ice-making device according to one embodiment of the present disclosure. FIG. 2 is a side view illustrating the configuration of an exemplary ice-making device for a refrigerator according to one embodiment of the present disclosure. FIG. 3 is an exploded perspective view illustrating the configuration of the exemplary ice-making device in FIG. 2 . FIG. 4 is a bottom perspective view illustrating the configuration of an exemplary bucket in the ice-making device illustrated in FIG. 2 . FIG. 5 illustrates an exemplary method of controlling the ice-making device for a refrigerator.
[0034] Referring to FIGS. 1 to 5 , the refrigerator 1 according to one embodiment of the present disclosure may include a refrigerator storage room 10 and an ice-making device 30 for a refrigerator.
[0035] The refrigerator 1 may include a cooling system (not shown) configured to supply cold air to the refrigerator storage room 10 . The cooling system may include, for example, an evaporator, a compressor and a condenser. A gaseous refrigerant at high temperature exchanges heat with ambient air through the evaporator and then flows to the compressor to be compressed. The compressed gaseous refrigerant dissipates heat while it passes through the condenser and becomes a liquid refrigerant. The liquid refrigerant passed through the condenser flows back to the evaporator. The liquid refrigerant in the evaporator is evaporated by absorbing heat from ambient air. Thus, in the evaporator, the liquid refrigerant receives heat from the ambient air and becomes a gaseous refrigerant. The gaseous refrigerant is separated from the liquid refrigerant and introduced into the compressor again.
[0036] Air cooled by the evaporator is supplied to circulate through the refrigerator storage room 10 .
[0037] The ice-making device 30 for a refrigerator may include an ice-making unit 100 , an ice-storing unit 200 , an accommodation unit 300 , a sensing unit 400 and a control unit 500 . The ice-making unit 100 , the ice-storing unit 200 and the sensing unit 400 may be disposed within the accommodation unit 300 . The ice-making unit 100 may be disposed at the upper side and the ice-storing unit 200 may be disposed at the lower side of the ice-making unit 100 . Hereinafter, the configuration of the ice-making unit 100 is described.
[0038] The ice-making unit 100 may include an ice tray 110 , a cooling unit 120 , a heating unit 130 and a water supply unit (not shown).
[0039] The ice tray 110 is configured to receive water from the water supply unit. Water in the ice tray 110 freezes into ice pieces by the cooling unit 120 . The ice tray 110 may include: partition walls 111 configured to divide the ice pieces, ice cells 112 partitioned by the partition walls 111 , an ice-releasing member 113 configured to discharge ice pieces out of the ice tray 110 , and an ice-releasing member guide 114 configured to guide the ice-releasing member 113 . The number and shape of the partition walls 111 may vary in different embodiments.
[0040] The ice-releasing member 113 may be configured to be rotated by a drive device such as a motor or the like. The ice tray 110 may include a heat transfer member made of metal or the like. The heat transfer member enhances the heat transfer efficiency between the cooling unit 120 and the water. The heat transfer member may be disposed outside the ice tray 110 and may have a shape conformal to the shape of the ice tray 110 . However, the present disclosure is not limited thereto.
[0041] In the illustrated embodiment, the ice pieces of the ice tray 110 are discharged by the ice-releasing member 113 . However, the present disclosure is not limited thereto. For example, the ice pieces of the ice tray 110 may be discharged by rotating and twisting the ice tray 110 .
[0042] The cooling unit 120 may cool the ice tray 110 and freeze water therein. The cooling unit 120 may include a duct 121 disposed below the ice tray 110 . The duct 121 may receive cold air from the cooling unit 120 through an inflow portion 122 of the duct 121 . After cooling the ice tray 110 , cold air is discharged through an outflow portion 123 of the duct 121 and then flow toward the ice-storing unit 200 .
[0043] In the present embodiment, the cooling unit 120 uses the duct 121 for supplying the cold air. However, the present disclosure is not limited thereto. For example, the cooling unit 120 may be composed of a pipe through which refrigerant flows. The cooling unit 120 may receive the refrigerant from the condenser of the refrigerator cooling system and may contact the ice tray 110 .
[0044] The heating unit 130 is configured to heat the ice tray 110 . The surfaces of the ice pieces making contact with the ice tray 110 may be melted (e.g., partially) by heating of the heating unit 130 . This enables the ice pieces to be easily released from the ice tray 110 . The heating unit 130 may have a long strip shape. The heating unit 130 may be disposed around the ice tray 110 . For example, the heating unit 130 may be disposed under the ice tray 110 to make contact with the ice tray 110 . The heating unit 130 may include a pipe through which a heat medium flows. However, the present disclosure is not limited thereto. For example, the heating unit 130 may be an electric wire that generates heat from electric energy.
[0045] The ice-storing unit 200 may include a bucket 210 , a support part 220 and an ice discharge part 230 .
[0046] The bucket 210 is configured to receive ice pieces produced in the ice tray 110 . Furthermore, the bucket 210 may receive cold air from the cooling unit 120 . The bucket 210 may be, for example, a container with a top opening and a front side opening. Elastic members 213 may be disposed between the bucket 210 and the support part 220 to be described later. The bucket 210 may be supported by the elastic members 213 and can move up and down. For example, the elastic members 213 may support the lower portion of the bucket 210 . The number of the elastic members 213 may be four for example. A slot 212 extending along an up-down direction may be formed in the bucket 210 . A delivery member 231 to be described in greater detail below may penetrate the bucket 210 through the slot 212 .
[0047] The support part 220 is configured to support the movable bucket 210 . The support part 220 is configured so that the support part 220 can be removed from the accommodation unit 300 while supporting the bucket 210 . The support part 220 may be, for example, a case capable of accommodating the bucket 210 . The bucket 210 may move up and down while being supported by the support part 220 .
[0048] Guides may be disposed in the bucket 210 and the support part 220 to guide the up-down movement of the bucket 210 . For example, as illustrated in FIGS. 3 to 5 , the bucket 210 may include first elastic member guides 214 and the support part 220 may include second elastic member guides 215 . The first elastic member guides 214 are configured to guide the elastic members 213 at one side. The second elastic member guides 215 are configured to guide the elastic members 213 at the other side. For example, the first elastic member guides 214 may be disposed inside the elastic members 213 . The second elastic member guides 215 may be disposed outside the elastic members 213 . The first and second elastic member guides 214 and 215 may guide the movement of the elastic members 213 , thereby guiding the up-down movement of the bucket 210 .
[0049] As another example of the guides, as illustrated in FIGS. 6 and 7 , the bucket 210 may include the bucket guides 211 and the support part 220 may include the support part guides 221 corresponding to the bucket guides 211 . The bucket guides 211 and the support part guides 221 facilitate the up-down motion the bucket. The bucket guides 211 may be projections protruding from the side surface of the bucket 210 . The support part guides 221 may be slots formed on the side surface of the support part 220 and extend up and down. However, the present disclosure is not limited thereto.
[0050] The ice discharge part 230 may discharge ice pieces stored in the ice-storing unit 200 to the outside. The ice discharge part 230 may include a delivery member 231 and a drive device 232 . The delivery member 231 may be disposed in the ice storage part 210 and may discharge the ice pieces stored in the ice storage part 210 to the outside. The delivery member 231 may be a rotary member including a central shaft and a blade. However, the present disclosure is not limited thereto.
[0051] The drive device 232 is coupled to the delivery member 231 and is configured to drive the delivery member 231 . The drive device 232 may be disposed adjacent to the other end wall of the ice-making device 30 . As the delivery member 231 is rotated by the drive device 232 , the ice pieces around the delivery member 231 may be moved toward an exit of the ice-making device 30 . The drive device 232 may include, for example, an electric motor and the like. However, the present disclosure is not limited thereto.
[0052] The accommodation unit 300 may surround the ice-making unit 100 , the ice-storing unit 200 and the sensing unit 400 . The accommodation unit 300 may include a heat insulation member. The accommodation unit 300 may be coupled to the inner wall of the refrigerator storage room 10 . The sensing unit 400 to be described in greater detail later may be disposed in the accommodation unit 300 .
[0053] The sensing unit 400 is configured to sense relative positional information (movement or the like) of the bucket 210 with respect to the accommodation unit 300 . For example, the sensing unit 400 may include a target part 410 and a recognition part 420 . The target part 410 may be disposed in the bucket 210 . The recognition part 420 may be disposed in the accommodation unit 300 .
[0054] The recognition part 420 may be a sensor configured to sense the relative positional information of the target part 410 . For example, if the bucket 210 disposed with the target part 410 is moved downward by the weight of the ice therein, the recognition part 420 may sense a change in the distance between the recognition part 420 and the target part 410 and thereby may detect a movement of the target part 410 .
[0055] For example, if the target part 410 is disposed in a central region of a bottom surface of the bucket 210 , the recognition part 420 may be disposed in a central region of the bottom of the accommodation unit 300 to face the target part 410 .
[0056] The target part 410 and the recognition part 420 may be spaced apart from each other. Since the bucket 210 disposed with the target part 410 may be separated from the accommodation unit 300 disposed with the recognition part 420 , the target part 410 and the recognition part 420 can be separated from each other. In this way, the target part 410 and the recognition part 420 are spaced apart without direct contact. Thus, when the bucket 210 is coupled with the accommodation unit 300 again, the operation of the sensing unit 400 would not be interrupted even if the target part 410 and the recognition part 420 are not electrically coupled to each other. In other words, the bucket 210 may be easily decoupled from or coupled with the accommodation unit 300 without having to electrically connect or disconnect the target part 410 and the recognition part 420 . The target part 410 may be a magnetic material and the recognition part 420 may be a magnetic sensor capable of sensing movement of the magnetic material. However, the present disclosure is not limited thereto.
[0057] The control unit 500 , as illustrated in FIG. 8 , may receive positional information (related to movement and/or position) on the bucket 210 from the sensing unit 400 . Accordingly, the control unit 500 may determine whether to suspend ice production. For example, if the distance between the target part 410 and the recognition part 420 falls within a predetermined range, the control unit 500 may determine that the bucket 210 is filled with a sufficient amount of ice and therefore instructs the ice-making unit 100 to suspend ice production. The control unit 500 may be implemented using a microprocessor or microcontroller.
[0058] Hereinafter, the operation and effect of the ice-making device 30 for a refrigerator configured as above are described. Once water is introduced into the ice tray 110 from the outside, water in the ice tray 110 can freeze into ice pieces by the cooling unit 120 . The ice pieces existing in the ice-making unit 100 are fed to the bucket 210 of the ice-storing unit 200 . At this time, the ice-releasing member 113 and the heating unit 130 may be driven. For example, the heating unit 130 may heat the ice tray 110 prior to releasing the ice pieces. Thereafter, the ice-releasing member 113 is driven to transfer the ice pieces in the ice tray 110 to the bucket 210 .
[0059] When the bucket 210 is not full with ice pieces, the bucket 210 is supported by the elastic members 213 and the bucket 210 is not pressed downward. If bucket 210 is full, the bucket 210 is moved downward due to the weight of the ice pieces existing in the bucket 210 . At this time, the elastic members 213 are compressed by the weight of the ice pieces. The sensing unit 400 may sense the downward movement of the bucket 210 .
[0060] The ice-making operation in the ice-making unit 100 is repeatedly performed and the ice pieces accumulate in the bucket 210 . As ice pieces are filled in the bucket 210 , the elastic members 213 are further compressed and the bucket 210 is further moved downward. If the bucket 210 is full of ice, the bucket 210 is further moved downward. The sensing unit 400 senses such movement of the bucket 210 . In other words, the sensing unit 400 senses that the bucket 210 is moved downward by a predetermined distance or more. The sensing unit 400 transmits the sensing result to the control unit 500 . Accordingly, the control unit 500 determines that the bucket 210 is full of ice and controls the ice-making unit 100 to suspend ice production.
[0061] Although exemplary embodiments of the present disclosure are described above with reference to the accompanying drawings, those skilled in the art will understand that the present disclosure may be implemented in various ways without changing the necessary features or the spirit of the present disclosure.
[0062] Therefore, it should be understood that the exemplary embodiments described above are not limiting, but only an example in all respects. The scope of the present disclosure is expressed by claims below, not the detailed description, and it should be construed that all changes and modifications achieved from the meanings and scope of claims and equivalent concepts are included in the scope of the present disclosure.
[0063] From the foregoing, it will be appreciated that various embodiments of the present disclosure have been described herein for purposes of illustration, and that various modifications may be made without departing from the scope and spirit of the present disclosure. The exemplary embodiments disclosed in the specification of the present disclosure do not limit the present disclosure. The scope of the present disclosure will be interpreted by the claims below, and it will be construed that all techniques within the scope equivalent thereto belong to the scope of the present disclosure.
|
An ice-making device for a refrigerator capable of detecting ice fullness in the ice storing unit and suspending ice production accordingly. The ice-making device includes a sensing unit configured to measure the amount of ice in the ice-storing unit based on detected positional information of the ice-storing unit. An accommodation unit is configured to accommodate the ice-making unit and the ice-storing unit. The sensing unit can sense relative movement of the ice storage unit with respect to the accommodation unit.
| 5
|
BACKGROUND
[0001] The invention relates generally to motion detection and more specifically to a surveillance system and method, for use in security systems or the like, in which a moving camera can be used to detect motion in an area.
[0002] Conventional security systems typically protect an enclosed area using switches at doors, windows, and other potential entry points. When a switch is activated, an alarm is sounded, a message is generated, or some other means of notifying the appropriate persons and/or discouraging the persons breaching security is activated. It is also known to use passive infra red (PIR) sensors, which sense heat differences caused by animate objects such as humans or animals, to detect the presence of persons in unauthorized areas. Other sensors used in surveillance and security systems include vibration sensors, radio frequency sensors, laser sensors and microwave sensors. Sensors often can be activated erroneously by power surges or large electromagnetic fields, such as occur when lightening is present. Such activation of course can trigger a false alarm.
[0003] To increase the reliability of security and surveillance systems, video cameras have been used to monitor premises. However, with camera surveillance, a constant communications channel must be maintained with the operator at the monitoring site. It is known to combine video camera surveillance with another sensing mechanism, a PIR sensor, for example, so actuation of the video camera is initiated by activation of the other sensor and the operator's attention is focused by sounding an alarm or delivering a message. However, when monitoring continuous video, even for relatively short periods of time, the operator must maintain a constant vigilance. However, an operator's ability to pay attention to a video display generally diminishes rapidly to the point where the operator is essentially ineffective after several minutes. Accordingly, video surveillance is labor intensive, expensive, and not always effective.
[0004] More recently, video cameras have been used to monitor an area within a field of view and the resulting image signal is processed to detect any motion in the field of view. U.S. Pat. No. 4,408,224 is exemplary of such systems in which a video camera monitors an area, such as a parking lot, and produces a video signal. The video signal is digitized and stored in a memory and is compared with a previous video signal that has been digitized and stored in a memory. If any differences between the two signals exceeds a threshold, an output is generated and fed to an alarm generation circuit. Various algorithms can be used to compare video signals with one another to determine if motion has occurred in the monitored area. For example, U.S. Pat. No. 6,069,655 discloses comparing video signals on a pixel by pixel basis, generating a difference signal between the two signals, and interpreting any non-zero pixel in the difference signal to be a possible movement. U.S. Pat. No. 4,257,063 discloses a video monitoring system in which a video line from a camera is compared to the same video line viewed at an earlier time to detect motion. U.S. Pat. No. 4,161,750 teaches that changes in the average value of a video line can be used to detect motion.
[0005] While the use of video cameras for detecting motion has solved many problems associated with surveillance, some limitations still exist. Specifically, a video camera can only monitor an area within its field of view. The field of view can be increased by locating the camera at a position far away from the area or by using wide angle optics. In either case, each pixel of the imager in the camera will correspond to a larger portion of the area as the field of view is increased. Therefore as the field of view is increased, resolution of the image signal decreases and the ability of the camera to accurately detect motion is reduced. To increase the area covered by a video camera surveillance system, it is well known to provide multiple video cameras. Of course, this increases the cost and complexity of the surveillance system. It is also known to utilize a moving camera to increase the field of view. For example, U.S. Pat. No. 5,473,364 discloses a surveillance system having moving cameras. However, the system disclosed in U.S. Pat. No. 5,473,364 requires complex algorithms, such as affine transforms, for adjusting images for camera movement. Accordingly, such systems are complex and require a great deal of processing power.
SUMMARY OF THE INVENTION
[0006] An object of the invention is to improve surveillance systems. To achieve this and other objects, a first aspect of the invention is an apparatus for detecting motion in an area. The apparatus comprises an imaging device, such as a camera, having a field of view that is smaller than the area, means for moving the field of view to vary the portion of the area that is covered by the field of view, means for storing a first set of image data captured by the imaging device when the field of view covers a first portion of the area and for storing a second set of image data captured by the imaging device when the field of view covers a second portion of the area, means for determining a fixed object image portion in an overlapping area, means for adjusting at least one of the first set of image data and the second set of image data based on the fixed object image portion to obtain two sets of adjusted image data, and means for comparing the two sets of corrected image data to determine if any objects in the overlapping area have moved.
[0007] A second aspect of the invention is a method for detecting motion in an area of interest. The method comprises recording test image data of a portion of the area having a fixed object therein, selecting a portion of the test image data corresponding to the fixed object, storing the portion of the test image data as learned image data, recording first image data at a first field of view, changing the field of view to a second field of view including the fixed object, recording second image data at the second field of view, recognizing the fixed object in the first image data and the second image data, adjusting at least one of the first image data and the second image data for position based on the position of the fixed object in the first image data and the second image data, and comparing the first image data and the second image data after the adjusting step to determine if motion has occurred in an area encompassed by both the first field of view and the second field of view.
BRIEF DESCRIPTION OF THE DRAWING
[0008] The invention is described through a preferred embodiment and the attached drawing in which:
[0009] FIG. 1 is a black diagram of a surveillance system of the preferred embodiment;
[0010] FIG. 2 is a diagram illustrating the moving field of view of the preferred embodiment; and
[0011] FIG. 3 is a flow chart of the surveillance method of the preferred embodiment;
DETAILED DESCRIPTION
[0012] FIG. 1 illustrates a surveillance system in accordance with a preferred embodiment of the invention. Surveillance system 10 utilizes a single imaging device, camera 20 in the preferred embodiment, to detect motion over a large area. Camera 20 includes imaging section 22 and optics section 24 and has field of view F. The phrase “field of view,” as used herein, refers to the effective area of a scene that can be imaged on the image plane of camera 20 at a given time. Imaging section 22 includes an imager, such as a known solid state imager, for sensing light at a plurality of points in a scene. For example, the imager can be an active pixel Complementary Metal Oxide Semiconductor (CMOS) sensor, such as that described in U.S. Pat. No. 6,215,113, or the imager can be a Charge Coupled Device (CCD). Optics section 24 serves to focus light from the scene in the field of view of camera 20 onto the imager. For example, optics section 24 can include a lens system, aperture diaphragm, and the like for focusing the image and adjusting exposure. Imaging section 22 can include appropriate imaging electronics, such as an A/D converter, for outputting an image signal corresponding to light sensed by the imager. Optics section 24 can also include mirrors, prisms, or other elements as necessary to accomplish the functions set forth herein.
[0013] Imaging section 22 and/or optics section 24 are coupled to panning mechanism 30 which comprises a motive device to move the field of view as desired by moving camera 20 , imaging section 22 , or optic section 24 . For example, the motive device can be the output shaft of a transmission coupled to a motor to rotate camera 20 about an axis or move camera 20 linearly. Further, the motive device can be coupled to a mirror or other element of optics section 24 to change the field of view without the need to move imaging section 22 . Panning mechanism 30 can be any device or combination of devices for moving the field of view of camera 20 across a desired area.
[0014] Processor 40 of the preferred embodiment can comprise a microprocessor based device, such as a general purpose programmable computer. For example, processor 40 can be embodied in a personal computer, a server, or a dedicated programmable device. Processor 40 includes storage device 42 , determining module, 44 , adjusting module 46 , comparing module 48 , messaging layer 50 , and user interface 52 . The various components of processor 40 can be embodied as hardware and/or software, as will become apparent below. Such components are described as separate entities for the clarity. However, the components need not be embodied in separate hardware and/or software and the functionality thereof can be combined or further separated. For example, all of the modules can be embodied in a single executable program file of a control program running on processor 40 .
[0015] Camera 20 generates a set of image data as an image signal based on the image in the field of view and communicates the signal to processor 40 for processing. As the field of view changes, by virtue of panning mechanism 30 , the image signal changes accordingly.
[0016] Storage device 42 can include a Random Access Memory (RAM), a magnetic disk, such as a hard disk, or any other device capable of retaining image data. Image data corresponding to the image signal is stored in storage device 42 . The image data can be updated periodically, such as every second, every minute, or the like. Because the field of view is changing, the image signal will change over time. Storage device 42 preferably is capable of storing at least two sets of image data at a time for reasons which will become apparent below.
[0017] Determining module 44 can include any algorithm or other logic for determining a static portion of an image corresponding to an image signal stored in memory device 42 . For example, Principal Component Analysis (PCA) techniques can be used. PCA distributes image data of a multidimensional image space and converts the image data into feature space. The principal components of eigenvectors which serve to characterize such space are then used for processing. More specifically, the eigenvectors are defined respectively by the amount of change in pixel intensity corresponding to changes within the image group, and can thus be thought of as characteristic axes for explaining the image.
[0018] A large number of eigenvectors are required to accurately reproduce an image. However, if one only desires to express the characteristics of the outward appearance of an image, the image can be sufficiently expressed using a smaller number of eigenvectors to thereby reduce the required processing power. Known PCA techniques can be used to compare a “learned” image with a current image to recognize patterns in the present image that are similar or identical to the learned image. In the preferred embodiment, the learned image is a designated portion of a previous image signal taken by camera 20 as described in detail below.
[0019] The learned image can be obtained by directing camera 20 toward an area including a substantially fixed object, such as a tree, a sign, a building, or a portion of such an object. The resulting image can be displayed on a screen in user interface 52 , such as a CRT display or the like. The operator can then designate the portion of the image representing the fixed object by selecting that portion of the image with a mouse pointer or other input device in a known manner. The portion of the image data representing the fixed object is then stored as a learned image. This learned image can be recognized in subsequent images by determining module 44 , using PCA techniques for example, and the position of the learned image in the current image can be output to adjusting module 46 .
[0020] Alternatively a software algorithm of determining module 44 can automatically determine a portion of an image representing a fixed object using any known image analysis technique. For example, determining module 44 can determine a fixed object image portion by comparing successive image data of a test field of view to determine a reference image portion having a fixed object therein, i.e. a portion where data does not change in successive views. The reference image portion can then be compared with portions of the first and second image data to determine which portion of the first and second image data has the fixed object therein. Many reference images can be taken over time to eliminate false fixed objects, such as cars, that may appear fixed and then can be moved later on.
[0021] Adjusting module 46 includes logic for adjusting images based on the determination of determining module 44 . In particular, adjusting module 46 compares the position of the learned image in two sets of image data and offsets the image data of at least one set of image data to locate the learned image in the same place in each set of image data. This operation permits the adjusted image data to be compared notwithstanding the fact that the field of view is different for each set of image data.
[0022] The adjusted sets of image data are sent to comparing module 48 for comparison in a known manner to ascertain if an object in the area has moved, e.g., an animate object has entered the area of surveillance. Appropriate filters and other logic can be applied to the determination to reduce detection of motion caused by small animals, wind, or the like, in a known manner. In the case of motion detection, messaging layer 50 can send a message, or other signal, to annunciation device 60 which can include an audible alarm, an image display, a phone dialer, or the like, to notify the proper parties and provide the desired information thereto.
[0023] FIG. 2 Illustrates the ability of the preferred embodiment to provide surveillance of a large area with a small amount of cameras by moving the field of view. In this example, the area to be converted by surveillance system 10 is area A (designated by the solid line in FIG. 2 ). Field of view F 1 (designated by the dotted line in FIG. 2 ) of camera 20 at a first position does not cover the entirety of area A. However, field of view F 1 does encompass tree T as a fixed object. The image of tree T can be selected as the learned image to be used for position adjustment by adjusting module 46 . The field of view of camera 20 can then be changed by panning mechanism 30 to be field of view F 2 (designated by the dashed line in FIG. 2 ). Note that field of view F 2 also encompasses tree T. Accordingly, image data of overlapping portions of field of view F 1 and field of view F 2 can be compared after adjustment in the manner described above. It can be seen that the field of view can be changed incrementally to span the entirety of area A, as long as each field of view includes tree T, while comparing overlapping portions of successive sets of image data to thereby cover the entirety of area A with only camera 10 .
[0024] FIG. 3 illustrates the method of surveillance of the preferred embodiment. In step 100 , a test image of the area to be monitored is taken and stored in storage device 42 . The test image can have any field of view of the area as long as there is a fixed object therein. The fixed object can be any object that is at least partially visible in all fields of view of camera 20 throughout panning of the area and is reasonably still and distinct to be discerned by analyzing image data. In step 110 , the portion of the test image having the fixed object therein is selected. For example, the test image can be displayed to a user through user interface 52 and the user can demarcate the fixed image with a mouse pointer, touch screen device, or the like. The image of the fixed object is then stored as a learned image in storage device 42 .
[0025] In step 130 , a surveillance image N of the area is recorded with camera 20 at a first field of view and image N is stored in storage device 42 . In step 140 , the field of view of camera 20 is changed by an incremental amount by panning mechanism 30 , while still including the fixed object, and in step 150 , surveillance image N+1 is recorded at the new filed of view. In step 160 , adjusting module 46 adjusts one or both of images N and N+1 for position based on the position of the fixed object recognized by determining module 44 in each image. The images N and N+1 are compared after adjustment by comparing module 48 to determine if motion has occurred in the area based on a known algorithm. If it is determined that motion has occurred, annunciation device 60 is activated to sound an alarm or take any appropriate action to notify the proper persons or entities that motion has been detected.
[0026] At this time, the mode of surveillance can be changed in step 200 . For example, an operator may now be given control of panning mechanism 30 to selectively view portions of the area to ascertain the source of motion or the operator may be presented with various displays automatically. If no motion is detected in step 170 , N is set to N−1, i.e. image N+1 becomes image N and surveillance continues in step 140 in the manner described above. This process can continue until panning mechanism has taken the field of view of camera 20 to the edge of the area and can continue with panning mechanism moving in a reverse direction back across the area.
[0027] Note that steps 100 through 120 , i.e., the recording of the learned image, can be accomplished at the same time as step 130 . In other words, the learned image can be captured directly out of the first or subsequent surveillance images. Also, the learned image can be captured again periodically to improve performance. In fact, the learned image can be of plural objects as long as each successive surveillance image includes at least one fixed object in common.
[0028] The logic of and data manipulation of the invention can be accomplished by any device, such as a general purpose programmable computer or hardwired devices. The imaging device can be any type of sensor for capturing image data, such as a still camera, a video camera, an x-ray imager, an acoustic imager, an electromagnetic imager, or the like. The camera can sense visible light, infra red light, or any other radiation or characteristic. The panning mechanism can comprise any type of motors, transmissions, and the like and can be coupled to any appropriate element to change the field of view of the camera. Any type of comparison and adjustment algorithm can be used with the invention.
[0029] The invention has been described through a preferred embodiment. However, various modifications can be made without departing from the scope of the invention as defined by the appended claims and legal equivalents.
|
A method and apparatus for detecting motion in a large area with a single imaging device, such as a camera. A fixed object is located in the area and a camera is panned across the area with the fixed object remaining in the field of view of the camera. Successive images are adjusted based on the position of the fixed object within the image and the adjusted images are compared to detect movement with an area of overlap between the images.
| 6
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a recombinant electric storage battery which includes separators that retain a selected balanced quantity of electrolyte and has positive plates of high antimony content.
2. Description of the Prior Art
There has been considerable interest in developing recombinant electric storage batteries due to their maintenance-free capabilities, long life, and possible manufacturing economies. Recombinant batteries of the lead acid or nickel cadmium type which operate by recombining the gases generated during charging are known in the art.
Recombinant batteries usually operate on the oxygen cycle and are designed with an excess of negative material as compared with positive material. During charging the positive electrodes reach full charge and generate oxygen before the negative electrodes generate hydrogen. The batteries are designed for optimum oxygen movement to the negative electrodes for recombination with the negative material or with the generated hydrogen to form water. By recombining the oxygen the internal pressure in the battery is restrained, the cell can be sealed and the battery continuously charged.
Examples of prior art batteries are found in the following U.S. patents: Abramson No. 3,170,819; McClelland, et al. No. 3,704,173; McClelland, et al. No. 3,862,861; Peters, et al. No. 4,119,772; Habich, et al. No. 4,320,181; Peters, et al. No. 4,373,015; McClelland, et al. No. 4,383,011; and Pearson No. 4,525,438.
The use of antimony in the positive plates in a sealed lead acid battery is described in the Szymborski, et al. Patent No. 4,401,730 as an improvement where the antimony content of the positive plates is not more than 2 percent. The Szymborski patent also describes control cells which contain antimony of a 2.1 percent content, which cells are described as showing a marked decrease in capacity after 300 cycles, compared with the cells made by Szymborski, according to his invention, that contained 1.4 to 1.5 percent antimony.
It is known that adding antimony as a component of the positive plates of a lead acid battery improves performance, but it also increases the degree of gassing of the positive plates, and no satisfactory solution has been proposed in the prior art to accommodate the higher rate of gassing.
It has been found that lead acid batteries constructed with fibrous sheet plate separators, having first and second fibers of different absorbency relative to the electrolyte in order to control the recombination rate, can control the degree of gassing that occurs with antimony levels above 2 percent of total alloy weight.
SUMMARY OF THE INVENTION
This invention relates to a recombinant electric storage battery with separators of the type that contain a balanced amount of electrolyte, and positive plates of the battery which contain antimony above 2 percent of total alloy weight. Control of the recombinant rate controls the increased gassing of the plates which provides greater current capacity.
The principal object of the invention is to provide a recombinant lead acid storage battery of increased current capacity.
A further object of the invention is to provide a battery of the character aforesaid which is economical to construct and has a long service life.
A further object of the invention is to provide a battery of the character aforesaid which can be constructed in a large number of shapes and sizes.
A further object of the invention is to provide a battery of the character aforesaid which is of reduced weight.
Other objects and advantageous features of the invention will be apparent from the description and claims.
It should, of course, be understood that the description herein is illustrative merely and that various modifications and changes can be made in the structure disclosed without departing from the spirit of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Recombinant lead acid storage batteries in accordance with the invention include an outer sealed case with provisions for venting of excess internal gas pressure, separators, positive and negative plates and electrolyte absorbed and retained in the separators. The separators are in close contact with the plates to wet the plates and to permit oxygen generated by the positive plates to travel to the negative plates for recombination with the negative active material, or with hydrogen produced by the negative plates. Since it is known that antimony added to the positive plates improves cycle life and current capacity, positive plates of a lead alloy were constructed with the following content in addition to lead of:
______________________________________% Sb % As % Cu % Sn % S % Ca______________________________________2.30 0.20 0.08 0.23 0.01______________________________________
Negative lead alloy plates were constructed with the following content in addition to lead of:
______________________________________% Sb % As % Cu % Sn % S % Ca______________________________________<0.001 <0.001 <0.0005 0.2-0.4 <0.001 0.10______________________________________
The amount of electrolyte available in the separators must be carefully balanced since too much electrolyte reduces the gas transfer passageways in the separator, and reduces the area available for gas recombination at the negative plate surfaces in contact therewith. Too little electrolyte causes reduced battery performance due to increased resistance and insufficient sulphate ions. It is important to provide sufficient electrolyte so that the recombinant action overcomes the increased gassing caused by the higher percentage of antimony. In addition, it is important that the separators be in close contact with the plates. This objective can be obtained by improving the compression resiliency of the separators. Absorbent mat separators were fabricated of first and second fibers which are inert to a particular electrolyte to be used, the fibrous sheet separators used were constructed as disclosed in the U.S. patent application to Badger, Ser. No. 929,648, filed Nov. 12, 1986.
As described in the Badger specification: "The first fibers impart to the sheet a given absorbency greater than 90 percent relative to the particular electrolyte, when surfactant-free, while the second fibers impart to the sheet a different absorbency less than 80 percent relative to the electrolyte, when surfactant-free. The first and second fibers are present in the sheet in such proportions that the sheet has an absorbency with respect to that electrolyte, when surfactant-free, of from 75 to 95 percent. Preferably, the first fibers are glass fibers, most desirably glass fibers having an average diameter less than 5 um. In one preferred embodiment the second fibers are organic fibers that are hydrophobic relative to the electrolyte, when surfactant-free, most desirably polyethylene or polypropylene fibers. In another preferred embodiment the second fibers are coarse glass fibers, for example, having a diameter from 10 um to 20 um. In a third preferred embodiment there are both organic fibers that are hydrophobic relative to the electrolyte, when surfactant-free, and large diameter glass fibers, in addition to glass fibers having an average diameter less than 5 um."
A recombinant battery was constructed using the described badger plate and separator construction, and it was compared to a like recombinant battery constructed with an antimony content in the positive plates of 2.3 percent. The batteries constructed with 0 and 2.3% percent antimony content tested as shown in Table I.
TABLE 1__________________________________________________________________________Comparison of Performance and Life of a Group 22NF RecombinationBattery with 2.3% Antimony (Sb) Positive Versus 0.0% Antimony(Sb) Positive (PbCaSn Alloy) PbCaSn* 2.3% Sb Positive**Test Positive/Negative PbCaSn Negative % Increase__________________________________________________________________________3 Hours @ 8.7 Ampere 2.28 Hours 3.38 Hours 48%6 Hours @ 5.28 Ampere 4.03 Hours 5.41 Hours 34%1 Hour @ 25 Ampere 0.56 Hours 0.79 Hours 41%20 Hour (A.H.) 25.43 A.H. 35.20 A.H. 38%# Cycles B.C.I. 100 143 43%Life Cycle Test (Range 125-160)__________________________________________________________________________ *PbCaSn alloy typically contains .10% Ca, .25% Sn and Pb are remainder. **2.3% Sb alloy typically contains 2.2-2.4% Sb, .10-.25% Sn and various grain refining elements.
The battery of the invention with 2.3 percent antimony provided a markedly increased capacity in contrast to the 0% antimony battery and the examples disclosed by the Szymborski, et al. patent which indicated a gratly decreased capacity with an antimony content of greater than 2.1%.
It will thus be seen that the objects of the invention have been achieved.
|
A recombinant electric storage battery which includes separators of multiple fiber electrolyte absorbency that retain a balanced amount of absorbed electrolyte, for controlled recombination and which are in contact with positive and negative plates, the negative plates being antimony free and the positive plates containing antimony in amount of 2 to 4 percent of total alloy weight, which provides considerably greater capacity and cycling life.
| 7
|
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to data storage systems and more particularly to systems and methods for mapping storage volumes to servers or other devices mounted in a server chassis.
[0003] 2. Description of the Related Art
[0004] In a client/server computing model, files may be stored on a central computer or system (e.g., a file server or storage server) to allow data to be shared by computer systems or other devices connected to a network. This centralized approach often makes it easier to backup important files since they are contained within a common repository. This approach may also make it easier to control access to files and applications, thereby improving security.
[0005] A storage server may include one or more physical storage devices, such as hard drives, tape drives, or the like, which may be formatted to include one or more storage areas, or “volumes,” utilizing a single file system. When configuring these volumes, some configuration tools may allow storage volumes to be mapped to specific servers, computing devices, or other attached devices connected to a storage server, controlling which volumes can be seen and accessed by certain servers and computing devices. This capability may be used to protect sensitive information while still enabling authorized use.
[0006] Before volumes can be mapped to a specific server or computer system, some configuration tools may require a user to input a unique multi-digit alphanumeric number, such as a World Wide Node Name (WWNN), World Wide Port Name (WWPN), or other identifier used to provide addressing to a card connected to a server or computer device. These identifiers may be quite confusing as these identifiers may be completely different for different hardware manufacturers. These identifiers may also change as cards are replaced or swapped out of particular servers. In certain cases, retrieving these identifiers may require physically inspecting computer hardware or accessing the identifiers through a telnet session with a selected server or computer. In short, dealing with these identifiers can significantly complicate the process of volume mapping.
[0007] In view of the foregoing, what is needed is an improved system and method to reduce complexity when mapping storage volumes to servers or other devices mounted in a server chassis. Ideally, such a system and method would be able to perform volume mapping without requiring knowledge of identifiers such as WWNNs or WWPNs corresponding to particular servers or computing devices.
SUMMARY OF THE INVENTION
[0008] The present invention has been developed in response to the present state of the art, and in particular, in response to the problems and needs in the art that have not yet been fully solved by currently available systems and methods. Accordingly, the present invention has been developed to provide improved systems and methods for mapping storage volumes to servers or other devices mounted in a server chassis.
[0009] In a first aspect of the invention, a method in accordance with the invention includes providing a chassis comprising multiple slots, with each slot having a unique slot number assigned thereto. Multiple servers, each having at least one globally unique identifier associated therewith, are provided to plug into one or more of the slots. At least one storage device is provided having one or more storage volumes. To map volumes to specific servers, a volume may be assigned to a slot by identifying a slot number associated with the slot. This slot may then be mapped to a globally unique identifier associated with a server plugged into the slot. In selected embodiments, the globally unique identifier includes a WWNN, WWPN, or other unique identifier.
[0010] In a second aspect of the invention, a system in accordance with the invention includes a chassis having multiple slots, with each slot having a unique slot number assigned thereto. Multiple servers, each having a globally unique identifier, are provided to plug into one or more of the slots. At least one storage device having one or more storage volumes is also provided. An assignment module is provided to assign a storage volume to a specific slot by identifying the unique slot number associated with the slot. A mapping module is provided to map the slot to a globally unique identifier, such as a WWNN or WWPN associated with a server plugged into the slot.
[0011] The present invention provides a novel system and method for mapping storage volumes to servers or other devices mounted in a server chassis. The features and advantages 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
[0012] In order that the advantages of the invention will be readily understood, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments illustrated in the appended drawings. Understanding that these drawings depict only typical embodiments of the invention and are not therefore to be considered limiting of its scope, the invention will be described and explained with additional specificity and detail through the use of the accompanying drawings, in which:
[0013] FIG. 1 is a high-level block diagram illustrating one embodiment of a system for mapping storage volumes to servers mounted in a server chassis.
DETAILED DESCRIPTION OF THE INVENTION
[0014] It will be readily understood that the components of the present invention, as generally described and illustrated in the Figures herein, may be arranged and designed in a wide variety of different configurations. Thus, the following more detailed description of the embodiments of the systems and methods of the present invention, as represented in the Figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention.
[0015] Some of the functional units described in this specification have been labeled as modules, in order to more particularly emphasize their implementation independence. For example, a module may be implemented as a hardware circuit comprising custom VLSI circuits or gate arrays, off-the-shelf semiconductors such as logic chips, transistors, or other discrete components. A module may also be implemented in programmable hardware devices such as field programmable gate arrays, programmable array logic, programmable logic devices or the like.
[0016] Modules may also be implemented in software for execution by various types of processors. An identified module of executable code may, for instance, comprise one or more physical or logical blocks of computer instructions which may, for instance, be organized as an object, procedure, or function. Nevertheless, the executables of an identified module need not be physically located together, but may comprise disparate instructions stored in different locations which, when joined logically together, comprise the module and achieve the stated purpose for the module.
[0017] Indeed, a module of executable code could be a single instruction, or many instructions, and may even be distributed over several different code segments, among different programs, and across several memory devices. Similarly, operational data may be identified and illustrated herein within modules, and may be embodied in any suitable form and organized within any suitable type of data structure. The operational data may be collected as a single data set, or may be distributed over different locations including over different storage devices, and may exist, at least partially, merely as electronic signals on a system or network.
[0018] Reference throughout this specification to “one embodiment,” “an embodiment,” or similar language means that a particular feature, structure, or characteristic described in connection with the embodiment may be included in at least one embodiment of the present invention. Thus, appearances of the phrases “in one embodiment” or “in an embodiment” in various places throughout this specification are not necessarily all referring to the same embodiment.
[0019] Furthermore, the described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. One skilled in the relevant art will recognize, however, that the invention can be practiced without one or more of the specific details, or with other methods, components, etc. In other instances, well-known structures, or operations are not shown or described in detail to avoid obscuring aspects of the invention.
[0020] The illustrated embodiments of the invention will be best understood by reference to the drawings, wherein like parts are designated by like numerals throughout. The following description is intended only by way of example, and simply illustrates certain selected embodiments of apparatus and methods that are consistent with the invention as claimed herein.
[0021] Referring to FIG. 1 , in general, a system 100 in accordance with the invention may include a storage server 102 configured to contain or have access to multiple volumes 104 a - c. A storage server 102 , for example, may include various enterprise storage systems including but not limited to network attached storage (NAS) arrays, storage area network (SAN) arrays, servers connected to direct-attached storage (DAS) devices, or the like.
[0022] The system 100 may also include a server chassis 106 which may be used to accommodate one or more servers 108 a - c. As will be explained in more detail hereafter, one or more of the servers 108 a - c may be configured to “see” and access one or more of the volumes 104 a - c. In selected embodiments, the server chassis 106 may include multiple slots 110 a - e which may be used to connect the servers 108 a - c to the chassis 106 and provide various services to the servers 108 a - c. The servers 108 a - c, similarly, may occupy one or several slots 110 a - e of the chassis 106 . In certain embodiments, each of the slots 110 a - e may be identified by a unique slot number (e.g., 1, 2, 3, etc).
[0023] In selected embodiments, the chassis 106 may be a blade chassis 106 , one example of which is marketed under the BladeCenter® tradename. Similarly, the servers 108 a - c may be “blade servers” 108 a - c configured to plug into the blade chassis 106 . These servers 108 a - c may have various internal components removed to reduce their size and enable packing at higher densities. The blade chassis 106 , in selected embodiments, maybe used to provide services such as power, networking, cooling, storage, as well as various interconnects to the servers 108 a - c.
[0024] The servers 108 a - c may be configured to function as web servers, file servers, applications servers, database servers, or the like. For the purposes of this specification, the term “server” may include any type of device that is mapped to one or more of the logical volumes 104 a - c, and may include devices to provide switching, routing, storage, or other services.
[0025] In certain embodiments, a switch 112 may be provided to control communication between the servers 108 a - c and the logical volumes 104 a - c. The switch 112 may, in certain embodiments, be integrated into the server chassis 106 . In one embodiment, the switch 112 is a serially-attached SCSI (SAS) switch 112 or fiber-optic switch 112 . A SAS switch 112 , for example, may be used to control communication between multiple SAS-configured servers 108 a - c and SAS-configured storage arrays 102 .
[0026] In selected embodiments, the storage server 102 may include a GUI configuration front end 114 to configure the storage server 102 . This front end 114 may enable a user to map specific volumes 104 a - c to one or more of the servers 108 a - c and thereby control access to the volumes 104 a - c.
[0027] As previously mentioned, some prior configuration tools may require a user to input a unique multi-digit alphanumeric number, such as a World Wide Node Name (WWNN), World Wide Port Name (WWPN), or other identifier or address associated with a card on a server 108 a - c before a volume 104 a - c can be mapped to the server 108 a - c. These identifiers may be long (e.g., 16 bits) and confusing in that they may differ significantly for different manufacturers. These identifiers may also change when a card is replaced or swapped out of a particular server 108 a - c. In other cases, the identifiers may not be readily available and may require visiting the server 108 a - c or retrieving the identifiers through a telnet session.
[0028] In selected embodiments in accordance with the invention, an assignment module 116 and mapping module 118 may be provided to mask the complexity of the WWNN and WWPN identifiers from a user. Instead of requiring input of the WWNN and WWPN identifiers, the modules may allow a user to map volumes 104 a - c to specific slots 110 a - e in the chassis 106 . For example, in selected embodiments, an assignment module 116 may enable a user to assign volumes 104 a - c to slots 110 a - e of the chassis 106 . In selected embodiments, a user may make these assignments through the GUI configuration front end 114 . As shown by way of example, volume A may be assigned to slot 1 , volume B may be assigned to slot 3 , and volume C may be assigned to slot 5 . In effect, these assignments allocate the volumes 104 a - c to the servers 108 a - c inserted into the slots 110 a,
[0029] A mapping module 118 , by contrast, may be provided to correlate the slot numbers 110 a, 110 c, 110 e with the servers 108 a - c and their associated WWNN and WWPN identifiers 120 a - c. In selected embodiments, the mapping module 118 may be located in and executed by the switch 112 . The switch 112 may, in certain embodiments, be configured to discover the WWNN and WWPN identifiers of the servers 108 a - c or other devices 108 a - c installed in the slots 110 a - e. In this way, the switch 112 may be able to correlate the slots 110 a - e with the servers 108 a - c and corresponding WWNN and WWPN identifiers 120 a - c.
[0030] As shown by the example of FIG. 1 , slot 1 may be mapped to server 1 having WWPN 1 and WWPN 2 . Slot 3 may be mapped to server 2 having WWPN 3 and WWPN 4 . Similarly, slot 5 may be mapped to server 3 having WWPN 5 and WWPN 6 . Because the slot number is correlated with a specific server 108 a - c and WWNN and WWPN identifiers 120 a - c inside the switch 112 , the user can map volumes 104 a - c to these servers 108 a - c knowing only the slot number 110 a, 110 c, 110 e and without any knowledge of the WWNN and WWPN identifiers 120 a - c. This improvement simplifies and speeds up the volume mapping process.
[0031] The present invention may be embodied in other specific forms without departing from its spirit or essential characteristics. The described embodiments are to be considered in all respects only as illustrative and not restrictive. The scope of the invention is, therefore, indicated by the appended claims rather than by the foregoing description. All changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
|
A system and method includes providing a chassis comprising multiple slots, with each slot having a unique slot number assigned thereto. Multiple servers, each having at least one globally unique identifier associated therewith, are provided to plug into one or more of the slots. At least one storage device is provided having one or more storage volumes. To map volumes to specific servers, a volume may be assigned to a slot by identifying a slot number associated with the slot. This slot may then be mapped to a globally unique identifier associated with a server plugged into the slot. In selected embodiments, the globally unique identifier includes a WWNN, a WWPN, or other unique identifier.
| 7
|
PRIORITY CLAIM
This application claims priority from European patent application No. 01830765.2, filed Dec. 14, 2001, which is incorporated herein by reference.
TECHNICAL FIELD
An embodiment of the present invention generally concerns the acquisition and processing of digital images and, more particularly, relates to a compression method that can be advantageously used in digital image acquisition devices.
BACKGROUND
Digital images are at present used in several applications, digital photography being a case in point.
In normal usages digital images are generally made to undergo a compression and encoding procedure. This procedure, also referred to more simply as compression, reduces the occupied memory quantity and makes it possible, for example, to increase the maximum number of images that can be simultaneously stored in the memory unit of a digital still camera. Furthermore, compression promotes shorter transmission times when the images have to be transferred to some external peripheral device or, more generally, on telecommunication networks such as—for example—the Internet.
The most common and efficient compression methods at present employed are based on the transform of the images into the two-dimensional spatial frequency domain, especially the so-called discrete cosine transform (or DCT). An example of this type is represented by the system defined by the specifications of the JPEG (Joint Photographic Expert Group) international standard for the compression/encoding of images (ISO/CCITT).
Proposing a generic and flexible compression system, this standard really defines several compression methods that can all be derived from two basic methods. One of these, the so-called JPEG baseline, employs the DCT and compression of the “lossy” type, i.e. with loss of information. An embodiment of the present invention concerns this method and, more generally, compression methods that use the DCT or such similar two-dimensional spatial transforms as the discrete wavelet transform (DWT).
A digital image can be represented by means of a matrix of elements, known as pixels, each of which corresponds to an elementary portion of the image and comprises one or more digital values each associated with an optical component. In a monochromatic image, for example, just a single value is associated with each pixel, and in this case it is usually said that the image consists of just a single channel or plane.
In a coloured RGB image, on the other hand, associated with each pixel there are three digital values that correspond to the three components (red, green, blue) of additive chromatic synthesis. In this case the image can be decomposed into three distinct planes or channels, each of which contains the information relating to just a single chromatic component.
A compression algorithm that employs the DCT operates separately and independently on the planes that make up the image; these planes are subdivided into sub-matrices of size 8×8 pixels, each of which is then transformed by means of the DCT.
For each sub-matrix (or sub-block) there is obtained an 8×8 matrix of which the elements, the so-called DCT coefficients, correspond to the amplitudes of orthogonal waveforms that define the representation of the sub-block in the two-dimensional DCT spatial frequency domain. In practice, therefore, each DCT coefficient, identified by indices (i,j), represents the amplitude of the DCT spatial frequency identified by the indices (i,j) associated with the coefficient. In the spatial frequency domain the compression algorithm reduces the information content by selectively attenuating or eliminating certain frequencies.
The reduction of the information quantity is obtained by dividing the DCT coefficient matrices by an 8×8 matrix of integer quantization coefficients: in practice each DCT coefficient is divided by the corresponding quantization coefficient and the result is then rounded off to the nearest integer. Due to the division and rounding-off operations and depending also on the actual values of the quantization coefficients, the “quantized” matrices obtained in this way contain a certain number of zero elements. When these matrices, which generally contain many coefficients equal to zero, are encoded—as is the case, for example, in the JPEG standard—by means of a Run Length encoding and subsequently by means of a Huffmann encoding, the memory occupation becomes reduced without any further information losses being suffered.
Quantization essentially reduces the precision of the DCT coefficients. The greater the values of the coefficients of the quantization matrix, the greater will be the information reduction quantity. Since there is no way of restoring the eliminated original information, an inappropriate quantization can appreciably deteriorate the quality of the image.
Optimization of the quantization matrices makes it possible to improve the performance of the compression algorithm by introducing some kind of compromise between final image quality and compression efficiency.
A characterization of the quality deterioration introduced into a digital image by a compression algorithm is provided by the so-called PSNR (Peak-to-Peak Signal to Noise Ratio), which is a measure in dB of the quantity of noise introduced by the algorithm at a given compression ratio. The compression ratio of an algorithm, on the other hand, is measured in terms of bit rates. The bit rate represents the number of bits that are needed to represent a pixel in the compressed and encoded image.
The JPEG standard suggests the use of quantization matrices synthesized on the basis of perceptive criteria that take due account of the sensitivity of the human eye to the DCT spatial frequencies. It has been shown that the use of these matrices gives rise to considerable artifacts when the (decoded/decompressed) images are displayed on high-resolution displays.
The prior art includes numerous attempts that were made—using different approaches—with a view to pinpointing and synthesizing optimal quantization matrices. The best results were obtained with adaptive or iterative procedures that operate on the basis of statistical, contentual and perceptive criteria. These methods obtain the optimization—albeit in some cases with a considerable computational effort—by supposing that the operation is being performed in an ideal context, i.e. without taking account of the effective degradation introduced into the digital image during the acquisition phase and the processing phases that precede compression. For this reason, solutions that in an ideal context would constitute the best trade-off between perceptive quality of the decoded/decompressed image and compression efficiency will produce non-optimal results when applied in some real context such as a digital still camera or an image scanner.
SUMMARY
In one embodiment of the present invention an efficient method is proposed for producing compressed images that will make it possible to improve the results obtainable with any one of the quantization matrices synthesized by the prior art.
According to an embodiment of the invention, an approach is proposed that, basing itself on a statistical characterization of the errors introduced during the image processing phase that precedes compression, appropriately modifies the coefficients of an arbitrary initial quantization matrix—even one of the matrices suggested by the JPEG standard, for example—and obtains a greater compression efficiency than said initial matrix without introducing any further quality losses.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the invention will be understood more readily from the detailed description given below of a particular embodiment, the said embodiment being merely an example and should not therefore be regarded as in any way limitative, together with the accompanying drawings, of which:
FIG. 1 a shows the block logic scheme of the image acquisition and compression process in a common digital still camera,
FIG. 1 b shows the arrangement of the R, G, B filtering elements in a conventional Bayer-type sensor,
FIG. 2 shows the logic scheme of measuring the error introduced into the DCT coefficients by the processing method used in a common IGP in accordance with an embodiment of the invention,
FIG. 3 a shows experimental results that illustrate the performance improvement in terms of bit rate obtained by the method in accordance with an embodiment of the invention as compared with the prior art,
FIG. 3 b shows experimental results that illustrate the performance improvement in terms of percentage and average bit rate gain obtained by the method in accordance with an embodiment of the invention as compared with prior art, and
FIG. 4 shows experimental results that illustrate the comparison of perceptive quality in terms of PSNR between the method according to an embodiment of the invention and the prior art.
DETAILED DESCRIPTION
The following discussion is presented to enable a person skilled in the art to make and use the invention. Various modifications to the embodiments will be readily apparent to those skilled in the art, and the generic principles herein may be applied to other embodiments and applications without departing from the spirit and scope of the present invention. Thus, the present invention is not intended to be limited to the embodiments shown, but is to be accorded the widest scope consistent with the principles and features disclosed herein.
Referring to FIG. 1 a , a digital still camera includes an acquisition block 1 that, by means of a sensor 2 , acquires an image representing a real scene.
Irrespective of whether it is of the CCD (Charge Coupled Device) or the CMOS type, the sensor 2 is an integrated circuit comprising a matrix of photosensitive cells, each of which generates a voltage proportional to the light that strikes it.
In a typical sensor each pixel is associated with just a single photosensitive cell. The sensor is covered by an optical filter consisting of a matrix of filtering elements, each of which is associated with one photosensitive cell. Each filtering element transmits to the photosensitive cell associated with it the light radiation corresponding to the wavelength of nothing but red light, nothing but green light or nothing but blue light, of which it absorbs only a minimal part, and therefore detects only one component for each pixel.
The type of filter employed varies from one producer to another, but the one most commonly used is known as a Bayer filter. The element matrix shown in FIG. 1 b shows the arrangement of the filtering elements of this filter, the so-called Bayer pattern.
The voltage values acquired by the photosensitive cells in block 1 are converted into digital values by an A/D converter, which is not shown in the figure.
The image 3 representing the output of acquisition block 1 is an incomplete digital image, because it is constituted by just a single component (R, G or B) per pixel. The format of this image is conventionally known as CFA (Colour Filter Array).
The CFA image 3 is sent to block 4 , the so-called IGP (Image Generation Pipeline), which performs a complex processing phase in order to obtain an uncompressed high-resolution digital image 5 .
The core of the complex processing performed in the IGP is the reconstruction process that, using the incomplete digital CFA image as its starting point, produces a complete digital image, in KGB format for example, in which each pixel is associated with three digital values corresponding to the three components R, G, B. This transformation implies a passage from a representation of the image on just a single plane (Bayer), but containing information about the various chromatic components, to a representation on three channels (R, G, B). The reconstruction process, known as expansion to full resolution, is conventionally obtained with known interpolation algorithms or with algorithms that construct a weighted average of the information contained in the CFA image.
The expansion to full resolution, which henceforth will be referred to more simply as interpolation, though without thereby introducing any limitation at all, produces only an approximation of the image that would be obtained with a sensor capable of acquiring three optical components per pixel In this sense, therefore, the interpolation process introduces an error that depends on the particular algorithm used in the IGP. As will be explained further on, this error, which can be likened to a noise, is a random process that can be statistically characterized in the two-dimensional spatial frequency domain.
Various other functions for improving image quality are also performed within the IGP block 4 , among them exposure correction, filtering of the noise introduced by the sensor 2 , application of special effects and other functions that will generally vary in both number and type from one producer to another.
Lastly, the RGB image is converted into the corresponding YCrCb image 5 , in which each pixel is represented by a luminance component Y and two chrominance components Cr and Cb.
Image 5 in YCrCb format is compressed by block 6 , known as Compression Engine, which could be, for example, an encoding/compression block in conformity with the JPEG baseline standard. Block 6 could also receive as input an image in some format other than YCrCb, though the choice of this particular format is often preferred. Indeed, the JPEG compression algorithm operates separately on the three channels that make up the coloured image: a YCrCb format presents the luminance information (Y channel) already separate from the chrominance information (Cr and Cb channels). For this reason it is possible to discard a larger quantity of information from the chrominance channels Cr and Cb, to which the human eye is less sensitive.
Block 6 divides each plane (channel) of the image into sub-blocks sized 8×8 pixel. Each sub-block is then transformed into an 8×8 matrix of DCT coefficients F i,j , where i=0 . . . 7 and j=0 . . . 7. The first DCT coefficient F 0,0 is called the DC component and represents the mean value (in the sub-block) of the component associated with the plane under consideration. The other coefficients, the so-called AC components, are associated with gradually increasing spatial frequencies.
The transformation method employed is well known to persons skilled in the art and is not therefore explained in detail. It would also be possible, for example, to divide the image into sub-blocks of size M×N, where M an N can be any desired integers, or to transform the sub-blocks into any two-dimensional spatial frequency domain. If so desired, it would also be possible to sub-sample the chrominance planes in accordance with the known technique thus further reducing the information contained in these channels.
Once the DCT coefficients have been obtained, a start can be made with the quantization process, which is substantially performed in accordance with the known technique, but utilizes matrices, and even standard-type matrices, that have been further refined by means of a method in accordance with an embodiment of the present invention.
By way of example, we shall here describe the synthesis of a quantization matrix Q opt for the luminance channel Y, using as starting point an arbitrary quantization matrix Q st that could also be a standard-type matrix. An analogous procedure is adopted for the other channels, but it is also possible to utilize the quantization matrices that have not been optimized by means of a method in accordance with an embodiment of the invention.
The starting matrix Q st is optimized by measuring and statistically characterizing the error that the IGP block introduces into the DCT coefficients. A scheme of the method used to obtain a measure of this error is shown in FIG. 2 .
On the upper line an incomplete CFA-format image representing a real scene 7 is acquired by means of a common CCD sensor 2 , realized, for example as a Bayer filter, and is then processed (interpolated) by the IGP block 4 and converted into a complete YCrCb-format image. The plane Y is divided into 8×8 sub-blocks and each of these is then transformed into an 8×8 DCT coefficient matrix.
On the lower line an image representing the same real scene 7 is acquired directly in RGB format, i.e., with three components for each pixel, and with full resolution by means of a sensor 9 and then transformed into a YCrCb-format image by the block 10 . The plane Y is divided into 8×8 sub-blocks and each of these is then transformed into an 8×8 DCT coefficient matrix.
The sensor 9 is capable of directly acquiring a complete image and could be, for example, a trilinear sensor or a more complex system consisting of a series of prisms that first decompose the ray of light that enters the objective into its three chromatic components and then direct these components onto three separate common CCD sensors.
When a sensor of this type—in any case a very costly item of equipment—is not available, the same measurement can be easily obtained with the help of simulation software, using as a full-resolution image an image consisting of three digital values per pixel and subsequently obtaining therefrom the corresponding incomplete CFA image by discarding two values per pixel in accordance with the pattern in which the filtering elements are arranged in the Bayer matrix ( FIG. 1 b ).
The difference between the DCT coefficients of a sub-block of the image acquired in CFA format and the corresponding sub-block of the image acquired with full resolution is an 8×8 matrix that constitutes the representation in the DCT spatial frequency domain of the error introduced by the IGP into the sub-block.
When this measurement is repeated for a large number of images, one obtains a statistical characterization of the error introduced by the IGP (in this case concerning the plane Y) in the spatial frequency domain that does not depend on the position of the sub-block within the plane.
It has been noted that this error is a random process that, depending on the characteristics of the IGP, acts selectively in the spatial frequency domain, distorting some frequencies to a greater extent than others. For example, it has been noted that a characteristic common to many IGPs is the fact that they introduce a very great error into the DCT coefficients associated with high spatial frequencies.
A possible statistical measure of the error introduced by the IGP and associated with a DCT spatial frequency identified by the indices (i,j) is the mean M i,j of the modules of the errors measured at the frequency (i,j), that is to say, of the errors measured on the DCT coefficients of index (i,j) as calculated from a large number of images. The quantity
E i , j = M i , j ∑ i , j M i , j
i=0, . . . , 7 j=0, . . . , 7
represents for every index (i,j) the error rate of the spatial frequency identified by the indices (i,j) with respect to the overall error introduced by the IGP in the spatial frequency domain.
Once this quantity is known, it is possible to obtain for each DCT frequency identified by the indices (i,j) a correction factor (or weighting coefficient) w i,j that is given by:
w
i
,
j
=
-
S
log
2
E
i
,
j
so that greater weights will be associated with the spatial frequencies affected by more substantial errors. S is a normalization-constant and represents a gain factor, and its value is determined experimentally in such a manner as to optimize the PSNR of the compressed image.
Each element Q i,j opt of the new quantization matrix Q opt can be obtained from the elements Q i,j st of the standard matrix by multiplying these elements by the corresponding weights, i.e.:
Q i,j opt =w i,j Q i,j st .
The elements of the initial quantization matrix are thus modified in such a way as to increase the value of the elements that correspond to the spatial frequencies affected by the greatest errors. This enhances the compression efficiency and at the same time reduces or eliminates image information corrupted by noise (errors).
Many variants can be applied to this basic approach. For example, experimental measurements have shown that the best results may be obtained by forcing to unity the coefficients Q 0,0 st , Q 0,1 st , Q 1,0 st , Q 1,1 st corresponding to the lowest DCT frequencies. When this is done, one avoids the possibility of having lack of uniformity between the tonalities of adjacent sub-blocks in the decoded and decompressed image (blocking effect).
In order to avoid producing artifacts, moreover, the weights w i,j may be applied only to those frequencies for which the measured statistical error lay below a certain threshold (for example, half the statistical error measured on the DC component). Alternatively, the weights w i,j may be applied only to those frequencies for which the measured statistical error lay above a certain threshold.
Experiments have shown a significant increase of the compression ratio as compared with the compression ratio obtained with standard matrices when the quality of the decoded/decompressed image is kept constant.
The graphs reproduced in FIGS. 3 a and 3 b illustrate the performance increment in terms of bit rate. In particular, the graph of FIG. 3 a illustrates the bit rates (in abscissa) obtained with optimized matrices (Curve 10 ) and standard matrices (Curve 11 ) in the case of 36 images subjected to JPEG standard compression/encoding.
The percentage gain in terms of bit rate is illustrated by Curve 12 in FIG. 3 b , where Curve 13 represents the average gain (35%).
FIG. 4 shows a quality comparison in terms of PSNR between the method with standard matrices (Curve 14 ) and the method with optimized standard matrices (Curve 15 ).
The experimental results thus confirm that the method explained above, though employing only a single quantization matrix per plane, offers concrete advantages.
In this connection attention should also be drawn to the simplicity of this method as compared with others that, performing the optimization block by block, produce a different quantization matrix for each block and therefore do not comply with the JPEG baseline standard (which envisages the use of only one matrix per plane).
|
A method of compressing digital images acquired in CFA format that utilizes optimized quantization matrices. The method, basing itself on the statistical characterization of the error introduced during the processing phase that precedes compression, appropriately modifies the coefficients of any initial quantization matrix, even of a standard type, obtaining a greater compression efficiency without introducing further quality losses.
| 7
|
The Government has rights in this invention pursuant to Contract No. F33615-76-C-5151 awarded by the Department of the Air Force.
BACKGROUND OF THE INVENTION
This invention relates to gas turbine engines and, more specifically to methods for remanufacturing turbine vane clusters from salvageable vane components.
In a gas turbine engine of the type to which the present invention is directly applicable, working medium gases are burned in a combustion section and are expanded through a turbine section. Disposed within the turbine section are one or more rows of stator vanes which are adapted to direct the working medium gases to a preferred angle of approach into a downstream row of rotor blades.
The vanes of the turbine have a limited life and are among the most susceptible of gas turbine engine components to damage. The medium gases directed across the vanes are extremely hot and likely contain corrosive constituents. For example, the initial row of stator vanes in a modern turbine is exposed to gases having temperatures well in excess of two thousand degrees Fahrenheit (2000° F.). Corrosive constituents contained within the medium gases include unreacted oxygen and oxides of sulfur. Violent energy reactions upstream of the stator vanes make it nearly impossible to control the homogeneity of the medium gases approaching the vanes. Accordingly, the vanes do not wear evenly and individual vanes are likely to need replacement before the entire set.
For ease of installation of the vanes and for aerodynamic performance considerations, it is conventional practice to form a row of stator vanes from clusters comprising a plurality of individual vanes each. The clusters are disposed in end to end relationship circumferentially around the working medium flow path. Paired vanes such as those illustrated in the present drawing are commonly employed although each cluster may also comprise three or more vanes.
To reduce replacement costs of vanes, designers and manufacturers of gas turbine engines have sought techniques for salvaging reusable portions of vane clusters and combination of salvaged portions to form remanufactured components.
SUMMARY OF THE INVENTION
A primary object of the present invention is to provide a method for remanufacturing turbine vane clusters of the type utilized in gas turbine engines. Effective methods for salvaging undamaged vanes from a damaged vane cluster and combining the salvaged vanes to form a remanufactured cluster are sought.
According to the present invention vanes to be salvaged from a damaged vane cluster are stripped of coating materials and stress relieved prior to separation from the original vane cluster.
In accordance with one detailed embodiment of the invention, faying surfaces on the vanes to be joined are simultaneously machined in a coelectric discharge machining process wherein the workpieces to be machined serve as the electrodes in the discharge machining apparatus.
A primary feature of the invention is the step of stripping corrosion resistant coating materials from the surfaces of the vanes to be salvaged. Another feature is the step of relieving residual stresses from the damaged vane cluster prior to separation of the salvageable vane. Yet another feature in at least one embodiment is the step of machining faying surfaces on the vane components to be joined.
A principal advantage of the invention is the ability to produce low cost vane clusters from undamaged components of damaged clusters. High quality vane clusters are produced by avoiding incipient melting of the parent material during remanufacture and by avoiding distortion from residual stresses after the salvaged vanes are separated from the damaged clusters. Direct correspondence between the faying surfaces of the vanes to be joined is assured in one method by simultaneously machining the faying surfaces in a coelectric discharge machining process.
The foregoing, and other objects, features and advantages of the present invention will become more apparent in the light of the following detailed description of the preferred embodiment thereof as shown in the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a perspective view of a two-vane cluster to which the present method of remanufacture applies; and
FIG. 2 is a block diagram illustrating the sequence of steps employed in the present method of remanufacture.
DETAILED DESCRIPTION
The vane clusters to which the present methods of remanufacture applies are of the type utilized in the turbine section of a gas turbine engine to direct hot working medium gases to a preferred angle of approach into a downstream row of rotor blades. The methods are described with respect to a two-vane structure, however, the concepts are equally applicable to clusters having more than two vanes.
FIG. 1 illustrates such a two-vane cluster 10. The cluster shown has two vanes 12 which extend between an inner platform 14 and an outer platform 16. The vane typically has a plurality of cooling holes 18 disposed in the vanes and platforms of the cluster. A cooling tube 20 is employed to direct the cooling medium against the interior surfaces of the vanes. The vane cluster is typically fabricated from a high quality, nickel-base superalloy material and is coated with a corrosion resistant material. Notwithstanding the use of such materials, the vanes become cracked, corroded, and otherwise damaged during extended service and need be replaced during maintenance and overhaul of the engine. The methods of reconstruction disclosed herein contemplate the severance of undamaged vanes from a damaged vane cluster and combining complementary vanes to form a remanufactured vane cluster.
The methods employ the principle steps of: inspecting damaged vane clusters and selecting complementary vanes for combination into a reconstructed cluster; stripping coating materials from the selected vanes and from portions of the vane platforms contiguous thereto; relieving residual stresses in the entire vane cluster in which the selected vanes are contained; separating the selected vanes and contiguous portions of the platforms from the damaged vane clusters; machining bond faying surfaces in the platforms of the complementary vanes selected for combination; bonding the complementary vanes at the faying surfaces to form a vane cluster; solution heat treating the vane cluster; applying corrosion resistant coating material to surfaces of the vane cluster which are exposed to hot working medium gases; and precipitation hardening the coated vane cluster.
The salvageable vane is separated from the damaged vane cluster at a midpoint along the inner platform 14 and outer platform 16. Complementary vanes are joined at the bond plane A at the inner platform and at the bond plane B at the outer platform. The orientation of the bond plane A and the bond plane B is not critical as long as the bond integrity remains secure. An extra measure of safety is obtainable by orienting the bond planes in accordance with the teaching in U.S. patent application Ser. No. 920,583, filed on even date herewith. In such an embodiment the complementary vanes are capable of retention in an engine notwithstanding failure of the bond.
The step of stripping coating material from the vanes is one critical step in the described procedure. In areas where coatings are not removed incipient melting of the vane alloy is likely to occur during the bonding cycle and subsurface material voids may resultantly develop. It is, therefore, that all coating materials are preferably removed from surfaces of the vanes and platforms selected for salvage.
The step of relieving residual stresses in the vane cluster is performed prior to separation of a salvageable vane from its damaged vane cluster. Relieving the stresses with the discardable vane attached, holds the vane platforms at near print dimensions during stress relief without additional fixturing. Without stress relief subsequent machining and heating processes induce deformation and resultant mismatch at the platforms.
For one vane material system in which a two-vane structure of directionally solidified MAR-M-200+Hf alloy (nominal by weight: 9% Cr, 10% Co, 12.5% W, 1% Cb, 2% Ti, 5% Al, 0.015% B, 0.05% Zr, 0.15% C, 1.5% Hf, and Balance Ni) material is coated with an aluminide protective material such as the type known in the industry as PWA 73, the following detailed manufacturing method has proved successful:
(1) Inspect damaged vane clusters and identify salvageable vanes and their associated platforms. Select a pair of complementary vanes from the identified, salvageable vanes.
(2) Remove appendages, such as internal cooling tubes, from the cast material.
(3) Chemically strip the aluminide protective coating from the internal and external surfaces of the salvageable vane as follows:
a. Grit blast the external and internal coated surfaces of the vane cluster with No. 240 aluminum oxide grit.
b. Immerse the vane cluster in an agitated nitric acid solution (20% by volume of 42° Baume) at seventy-five to ninety degrees Fahrenheit (75°-90° F.) for four (4) hours.
c. Wet abrasive blast the external and internal surfaces with a No. 200 or finer soft type abrasive such as the silicon dioxide abrasive known in the industry as Novaculite (Chicago Wheel and Manufacturing Company, Chicago, Ill).
d. Immerse the vane cluster in an agitated nitric acid solution (20% by volume of 42° Baume) at seventy-five to ninety degrees Fahrenheit (75°-90° F.) for four (4) hours.
e. Wet abrasive blast the external and internal surfaces with a No. 200 or finer soft type abrasive such as the silicon dioxide abrasive known in the industry as Novaculite.
f. Immerse the vane cluster in an agitated nitric acid solution (20% by volume of 42° Baume) at seventy-five to ninety degrees Fahrenheit (75°-90° F.) for four (4) hours.
g. Wet abrasive blast the external and internal surfaces with a No. 200 or finer soft type abrasive such as the silicon dioxide abrasive known in the industry as Novaculite.
h. Rinse the vane cluster in clean cold water.
(4) Relieve residual stresses from the vane cluster by heating the cluster in argon at a partial pressure vacuum of one and one half to two (1.5-2.0) torr at two thousand two hundred degrees Fahrenheit (2200° F.) for two (2) hours.
(5) Separate the salvageable vane and contiguous inner and outer platforms from the vane cluster. Separation may include cutting by a convention aluminum oxide or, silicon carbon abrasive wheel. Alternatively, the vane may be cut by electrical discharge machining.
(6) Inspect the separated vane and platforms for distortion. Correct any distortion by mechanically deforming the vane. The vane may be heated during correction of distortion to temperatures up to two thousand degrees Fahrenheit (2000° F.).
(7) Grind platforms of the vanes to be joined to within thirteen to fifteen thousandths (0.013-0.015) of an inch extra stock at the bond planes.
(8) Coelectrical discharge machine the platform surfaces to be joined using one vane as the positive electrode in the discharge machining apparatus and using the complementary vane as the negative electrode in the discharge machining apparatus. After machining the platform surfaces to be joined, or faying surfaces, must be capable of complete contact with each other.
(9) Clean the bond faying surfaces using an effective process, such as the electrolyte alkaline process which follows:
a. Wet vapor blast the faying surfaces with a No. 200 or finer soft type abrasive such as the silicon dioxide abrasive known in the industry as Novaculite.
b. Immerse the faying surfaces in an alkali solution such as a water base solution of eighteen to twenty-four (18-24) ounces of Endox 114 (Ehthone, Inc., West Haven, Conn.) or equivalent and eight to fourteen (8-14) ounces of sodium cyanide per gallon of solution at one hundred twenty plus or minus ten degrees Fahrenheit (120°±10° F.) with periodic current reverse of ten (10) seconds anodic, ten (10) seconds cathodic, for two minutes plus or minus one-half minute (2 min.±1/2 min.) at twenty-five to thirty-five amperes per square foot (25 to 35 ASF).
c. Rinse in clean water.
d. Immerse in a hydrochloric acid solution (HCl 65% by volume of 20° Baume). Make anodic at sixty (60) ASF for one (1) minute.
e. Rinse in clean water.
f. Immerse in the alkali solution of step 9b at one hundred twenty plus or minus ten degrees Fahrenheit (120°±10° F.) and agitate for thirty (30) seconds.
g. Rinse in clean water.
h. Immerse in a hydrochloric acid solution (HCl 65% by volume of 20° Baume) for thirty (30) seconds.
i. Rinse in clear water.
j. Immerse in acid solution (HNO 3 at 40% by volume 42° Baume, HF at 2% of 70 molecular weight percent by volume) at room temperature for ten (10) seconds.
k. Rinse in hot demineralized water at one hundred eighty to two hundred degrees Fahrenheit (180°-200° F.) for ten (10) seconds.
l. Blow dry using argon or hot air.
m. Visually inspect the bond faying surfaces. Properly cleaned surfaces will exhibit a bright or gray color.
n. Repeat the cleaning as many times as required until the surfaces exhibit the bright or gray color of step 9m.
(10) Bond the complementary vanes at the faying surfaces employing a high quality bond technique such as the diffusion bonding TLP® process (United Technologies Corporation, Hartford, Conn.) disclosed in U.S. Pat. No. 3,678,570.
(11) Dress off excess bonding alloy and any joint mismatch on the bonded vanes.
(12) Optically inspect the bonded vanes at 10× magnification for complete bonding. No unbonded areas are allowed.
(13) Dimensionally inspect the bonded vanes. Remachining to remove extra material is allowed. Minor dimensional restoration may be performed on the vane platform machined surface areas using conventional plasma spray techniques with PWA 1347 alloy powder (nominally by weight: 6% Al, 18.5% Cr, and Balance Ni). Grit blast the surface using No. 30 grit silicon carbide prior to plasma spray. Deposits up to thirty thousandths (0.030) of an inch thick may be applied on the platform edges. Conventional gas tungsten-arc welding, direct current straight polarity, may also be utilized with Inconel 625 filler metal (nominally by weight: 0.05% C, 0.15% Nn, 0.3% Si, 22% Cr, 9% Co, 4% Cb, 0.2% Ti, 0.2% Al, 3% Fe, and Balance Ni). Weld deposits up to sixty thousandths (0.060) of an inch thick may be made on these machined surface areas. Machine the plasma spray and weld deposits to meet vane dimensional requirements.
(14) Solution heat treat the bonded vanes at two thousand two hundred degrees Fahrenheit (2200° F.) in a static partial pressure vacuum of argon at one and one-half to two (1.5-2.0) torr for two (2) hours. Cool by back filling argon at a rate equivalent to air cool.
(15) Reapply a corrosion resistant coating such as PWA 73 aluminide protective coating to the surfaces of the cluster which are exposed to the working medium gases of an operating engine.
(16) Reinstall cooling tubes as required.
(17) Precipitation heat treat at sixteen hundred degrees Fahrenheit (1600° F.) for thirty-two (32) hours in air.
(18) Final inspect and classify the vane cluster.
Although the invention has been shown and described with respect to preferred embodiments thereof, it should be understood by those skilled in the art that various changes and omissions in the form and detail thereof may be made therein without departing from the spirit and the scope of the invention.
|
A method for remanufacturing turbine vane clusters of gas turbine engines is disclosed. Concepts and techniques for salvaging undamaged vanes from a damaged vane cluster are developed. In accordance with the method taught, protective coatings on the vane clusters are removed and residual stresses in the vanes are relieved before salvageable vanes are separated from their original vane cluster.
| 8
|
This application claims priority and benefit under 35 U.S.C. §119(e) to U.S. Provisional Patent Application No. 61/136,518, entitled “Imprint Lithography”, filed on Sep. 11, 2008. The content of that application is incorporated herein in its entirety by reference.
FIELD
The present invention relates to imprint lithography.
BACKGROUND
In lithography, there is an ongoing desire to reduce the size of features in a lithographic pattern in order to increase the density of features on a given substrate area. In photolithography, the push for smaller features has resulted in the development of technologies such as immersion lithography and extreme ultraviolet (EUV) radiation lithography, which are however rather costly.
A potentially less costly road to smaller features that has gained increasing interest is so-called imprint lithography, which generally involves the use of a “stamp” (often referred to as an imprint template) to transfer a pattern onto a substrate. An advantage of imprint lithography is that the resolution of the features is not limited by, for example, the wavelength of a radiation source or the numerical aperture of a projection system. Instead, the resolution is mainly limited to the pattern density on the imprint template.
Lithography typically involves applying several patterns onto a substrate, the patterns being stacked on top of one another such that together they form a device such as an integrated circuit. Alignment of each pattern with a previously provided pattern is a significant consideration. If patterns are not aligned with each other sufficiently accurately, then this may result in some electrical connections between layers not being made. This, in turn, may cause the device to be non-functional. Lithographic apparatus therefore usually include an alignment apparatus which is intended to align each pattern with a previously provided pattern.
SUMMARY
Accordingly, it is advantageous, for example, to provide an imprint lithography alignment apparatus and method which is novel and inventive.
According to an aspect of the invention, there is provided a method of determining a position of a substrate relative to an imprint template, the imprint template having at least three gratings and the substrate having at least three gratings positioned such that each imprint template grating forms a composite grating with an associated substrate grating, the at least three imprint template gratings and associated substrate gratings having offsets relative to one another, the method comprising: detecting an intensity of radiation which is reflected by the three composite gratings; and using the detected intensities to determine displacement of the substrate or imprint template from a position.
According to an aspect of the invention, there is provided a lithographic apparatus comprising: an imprint template holder configured to hold an imprint template; a substrate table configured to hold a substrate to be imprinted by the imprint template; an alignment radiation beam source and a beam directing apparatus, arranged to direct an alignment radiation beam towards different locations on the imprint template; and a detector arranged to detect an intensity of alignment radiation reflected from gratings provided on the imprint template and the substrate.
BRIEF DESCRIPTION OF THE DRAWINGS
Specific embodiments of the invention will be described with reference to the accompanying figures, in which:
FIGS. 1 a - c schematically shows examples of, respectively, micro-contact printing, hot imprint, and ultraviolet (UV) radiation imprint;
FIG. 2 schematically shows a lithographic apparatus according to an embodiment of the invention;
FIG. 3 schematically shows alignment of an imprint template and substrate according to an embodiment of the invention;
FIG. 4 schematically shows other parts of the lithographic apparatus according to an embodiment of the invention; and
FIG. 5 schematically shows an alternative lithographic apparatus to which an embodiment of the invention may be applied.
DETAILED DESCRIPTION
Examples of three known approaches to imprint lithography are schematically depicted in FIGS. 1 a to 1 c.
FIG. 1 a shows an example of a type of imprint lithography that is often referred to as micro-contact printing. Micro-contact printing involves transferring a layer of molecules 11 (typically an ink such as a thiol) from a template 10 (e.g. a polydimethylsiloxane template) onto an imprintable medium layer 13 which is supported by a substrate 12 and planarization and transfer layer 12 ′. The template 10 has a pattern of features on its surface, the molecular layer being disposed upon the features. When the template is pressed against the imprintable medium layer, the layer of molecules 11 are transferred onto the imprintable medium. After removal of the template, the imprintable medium is etched such that the areas of the imprintable medium not covered by the transferred molecular layer are etched down to the substrate. For more information on micro-contact printing, see e.g. U.S. Pat. No. 6,180,239.
FIG. 1 b shows an example of so-called hot imprint lithography (or hot embossing). In a typical hot imprint process, a template 14 is imprinted into a thermosetting or a thermoplastic imprintable medium 15 which has been cast on the surface of a substrate 12 . The imprintable medium may, for example, be resin. The imprintable medium may, for instance, be spin coated and baked onto the substrate surface or, as in the example illustrated, onto a planarization and transfer layer 12 ′. When a thermosetting polymer resin is used, the resin is heated to a temperature such that, upon contact with the template, the resin is sufficiently flowable to flow into the pattern features defined on the template. The temperature of the resin is then increased to thermally cure (crosslink) the resin so that it solidifies and irreversibly adopts the desired pattern. The template may then be removed and the patterned resin cooled. In hot imprint lithography employing a layer of thermoplastic polymer resin, the thermoplastic resin is heated so that it is in a freely flowable state immediately prior to imprinting with the template. It may be necessary to heat a thermoplastic resin to a temperature considerably above the glass transition temperature of the resin. The template is pressed into the flowable resin and then cooled to below its glass transition temperature with the template in place to harden the pattern. Thereafter, the template is removed. The pattern will consist of the features in relief from a residual layer of the resin which residual layer may then be removed by an appropriate etch process to leave only the pattern features. Examples of thermoplastic polymer resins used in hot imprint lithography processes are poly (methyl methacrylate), polystyrene, poly (benzyl methacrylate) or poly (cyclohexyl methacrylate). For more information on hot imprint, see e.g. U.S. Pat. No. 4,731,155 and U.S. Pat. No. 5,772,905.
FIG. 1 c shows an example of UV radiation imprint lithography, which involves the use of a transparent template and a UV radiation-curable liquid as imprintable medium (the term “UV” is used here for convenience but should be interpreted as including any suitable actinic radiation for curing the imprintable medium). UV radiation curable liquids are often less viscous than the thermosetting and thermoplastic resins used in hot imprint lithography and consequently may move much faster to fill template pattern features. A quartz template 16 is applied to a UV radiation-curable resin 17 on substrate 12 (and optionally on a planarization and transfer layer 12 ′) in a similar manner to the process of FIG. 1 b . However, instead of using heat or temperature cycling as in hot imprint, the pattern is frozen by curing the imprintable medium with UV radiation that is applied through the quartz template onto the imprintable medium. Thereafter, the template is removed. The pattern will consist of the features in relief from a residual layer of the resin which residual layer may then be removed by an appropriate etch process to leave only the pattern features. A particular manner of patterning a substrate through UV radiation imprint lithography is so-called step and flash imprint lithography (SFIL), which may be used to pattern a substrate in small steps in a similar manner to optical steppers conventionally used in integrated circuit (IC) manufacture. For more information on UV radiation imprint, see e.g. U.S. patent application Publication No. US 2004-0124566, U.S. Pat. No. 6,334,960, PCT Patent Application Publication No. WO 02/067055, and the article by J. Haisma entitled “Mold-assisted nanolithography: A process for reliable pattern replication”, J. Vac. Sci. Technol. B14(6), November/December 1996.
Combinations of the above imprint techniques are possible. See, e.g., U.S. patent application Publication No. US 2005-0274693, which mentions a combination of heating and UV radiation curing an imprintable medium.
FIG. 2 shows schematically an imprint lithography apparatus according to an embodiment of the invention. Referring to FIG. 2 a , a substrate 20 bearing a layer of imprintable medium is provided on a substrate table 22 . An imprint template 24 is held by an imprint template holder 26 . A source of actinic radiation 28 (for example, a UV radiation source) is provided above the imprint template holder 26 . The radiation source 28 is configured to provide a converging beam of actinic radiation 29 which passes through a focal area or focal point 30 (focal area if the actinic radiation source 28 is an extended source; focal point if the actinic radiation source 28 is a point source). A lens 32 , which is located some distance beyond the focal point 30 is arranged to collimate the actinic radiation beam 29 , and to direct it through the imprint template holder 26 and imprint template 24 onto the substrate 20 .
The lithographic apparatus further comprises a source 34 of non-actinic radiation. This source, which will hereafter be referred to as the alignment beam source 34 , generates a collimated beam of radiation 35 which will hereafter be referred to as the alignment radiation beam. A tip-tilt mirror 36 is provided above the imprint template holder 26 . The tip-tilt mirror 36 can be tilted around two axes, and is arranged to be moved between a plurality of orientations. Different orientations of the rotatable mirror 36 may direct the alignment radiation beam towards different alignment targets 42 , 43 provided on the imprint template 24 (or towards different parts of those alignment targets). The axes about which the tip-tilt mirror 36 may be tilted may, for example, be parallel and normal to the surface of the substrate table 22 .
The lithographic apparatus further comprises a beam-splitter 38 and detector 40 . The beam-splitter 38 is arranged to direct towards the detector 40 a portion of the alignment radiation beam 35 which has been reflected from the substrate 20 or from the imprint template 24 , as is explained below. The detector 40 is connected to a processor 46 , which receives output from the detector and uses this output to align the substrate 20 with respect to the imprint template 24 (or to align the imprint template with respect to the substrate).
The actinic radiation beam 29 passes through the focal point or focal area 30 in order to allow the tip-tilt mirror 36 to be provided above the imprint template holder 26 without the actinic radiation beam 29 hitting the tip-tilt mirror. Other arrangements of the actinic radiation and the tip-tilt mirror 36 may be used. For example, the tip-tilt mirror may be provided in some other location, and/or a beam-directing apparatus other than a tip-tilt mirror may be used to direct the alignment radiation beam towards the imprint template. For example, a lens system, mirror array or other optical device may be used. The actinic radiation source may be provided in a different location, with the actinic radiation beam being directed to the imprint template, for example, by beam steering mirrors.
During alignment, the actinic radiation source 28 is switched off (or the actinic radiation beam is blocked) such that the actinic radiation beam 29 is not directed onto the imprint template 24 or substrate 20 . A substrate 20 which has been provided with a layer of imprintable medium is then placed on the substrate table 22 . The substrate table is moved until the substrate is positioned beneath the imprint template 24 , the imprint template alignment marks 42 , 43 being located over alignment targets 44 , 45 provided on the substrate. The imprint template 24 may be brought into contact with the imprintable medium provided on the substrate 20 . The substrate table 22 may be moved, for example, by motors. The position of the substrate table may be monitored, for example, by one or more interferometers, as is described further below.
The accuracy with which the substrate table is positioned in this initial alignment phase (sometimes referred to as coarse alignment) is such that the imprint template alignment marks 42 , 43 and substrate alignment marks 44 , 45 are aligned sufficiently closely to allow alignment (sometimes referred to as fine alignment) to be performed using the marks 42 - 45 . Once final alignment has taken place, the imprint template holder 26 is lowered (and/or the substrate table is raised) so that the imprintable medium flows into pattern recesses of the imprint template 24 . The actinic radiation beam 29 is then directed onto the imprintable medium in order to cure the imprintable medium (and thereby cause it to solidify). The imprint template 24 and substrate 20 are then separated, and the substrate 20 is removed from the lithographic apparatus for processing.
Alignment between the substrate 20 and the imprint template 24 is achieved as follows. The tip-tilt mirror 36 is oriented such that it directs the alignment radiation beam 35 towards part of a first imprint template alignment target 42 . A proportion of the alignment radiation beam 35 will be reflected from the imprint template alignment target 42 , and a proportion of the alignment radiation beam will pass onto the substrate alignment target 44 . A proportion of the alignment radiation beam 35 will then be reflected from the substrate alignment target 44 . The reflected alignment radiation (i.e. alignment radiation which has been reflected from the imprint template alignment target 42 and/or the substrate alignment target 44 ) passes back to the mirror 36 . The mirror 36 directs the reflected alignment radiation towards the beam-splitter, which in turn directs the reflected alignment radiation onto the detector 40 . The detector provides an output signal which passes to the processor 46 .
The tip-tilt mirror 36 is then moved to a new orientation (not shown) such that it directs the alignment radiation beam 35 towards a different part of the first imprint template alignment target 42 , and the detector 40 again provides an output signal which passes to the processor 46 . This may be repeated for other different parts of the first imprint template alignment target 42 .
Referring to FIG. 2 b , the tip-tilt mirror 36 is then moved to a new orientation, such that the alignment radiation beam 35 is directed towards part of a second imprint template alignment target 43 and associated substrate alignment target 45 . Again, a portion of the alignment radiation beam 35 is reflected back via the mirror 36 and beam-splitter 38 to the detector 40 . The detector 40 again provides an output signal which passes to the processor 46 .
The tip-tilt mirror 36 is then moved to other orientations in order to direct the alignment radiation beam 35 towards other parts of the second imprint template alignment target 43 .
The tip-tilt mirror 36 may be moved to other orientations in order to direct the alignment radiation beam 35 towards other imprint template alignment targets (not shown).
The processor 46 uses the signals output from the detector 40 to determine the distance of the substrate 20 (and/or the template 24 ) from a desired aligned position. The desired aligned position may, for example, be the position in which a pattern provided on the imprint template 24 is aligned with a pattern provided on the substrate 20 . The processor then causes movement of the substrate table 22 until the substrate 20 (and/or of the imprint template holder 26 until the imprint template 24 ) is in the desired aligned position.
The manner in which the imprint template alignment targets 42 , 43 and the substrate alignment targets 44 , 45 provide a signal which may be used to align the substrate 20 with respect to the imprint template 24 (or vice versa) is illustrated schematically in FIG. 3 .
FIG. 3 a shows in more detail a portion of the imprint template 24 and substrate 20 that is circled by a dotted line in FIG. 2 a . As can be seen from FIG. 3 a , the first imprint template alignment target 42 comprises at least three gratings 42 a - c provided on a lowermost surface of the imprint template 24 . The associated substrate alignment target 44 also comprises at least three gratings 44 a - c , provided on an uppermost surface of the substrate 20 . A layer of imprintable medium 50 is provided between the imprint template 24 and the substrate 20 .
The period of each grating 42 a - c , 44 a - c is the smile. However, the substrate gratings 44 a - c are offset relative to the imprint template gratings 42 a - c . In the example shown in FIG. 3 a , for ease of understanding the imprint template 24 and substrate 20 are aligned so that the central imprint grating 42 b and the central substrate grating 44 b are aligned. The offset of the right-hand substrate grating 44 a relative to the right-hand imprint template grating 42 a is a distance “−d”. The offset of the left-hand substrate grating 44 c relative to the left-hand imprint template grating 42 c is a distance “+d”.
Operation of an embodiment of the invention is described in relation to FIG. 3 b . Coarse alignment between the substrate 20 and the imprint template 24 is performed as described further above. As a result of this coarse alignment, the imprint template gratings 42 a - c are located over the substrate gratings 44 a - c . However, they are not aligned as shown in FIG. 3 a , but instead include a degree of misalignment.
The tip-tilt mirror 36 is used to direct the alignment radiation beam 35 towards the imprint template alignment target 42 . The alignment radiation beam 35 does not illuminate the entire alignment target 42 , but instead illuminates each of the imprint template gratings 42 a - c in turn.
The alignment radiation beam 35 is initially directed at the right-hand imprint template alignment mark 42 a (the alignment radiation beam is labeled here as 35 a ). The cross-sectional size (e.g., diameter or width) of the alignment radiation beam 35 a is sufficiently small, relative to the size of the imprint template grating 42 a , that the alignment radiation beam 35 a does not extend beyond edges of the grating. The imprint template grating 42 a and the substrate grating 44 a (as well as imprint template grating 42 b and substrate grating 44 b and imprint template grating 42 c and substrate grating 44 c ) may together be considered to form a composite grating. This composite grating reflects a proportion of the alignment radiation beam 35 a back to the detector (see FIG. 2 a ). The reflected alignment radiation may be considered to have undergone a zero-order diffraction which has reflected the alignment radiation. The detector 40 detects only zero-order alignment radiation. It does not detect a significant amount of 1 st order or higher order diffracted radiation.
The term composite grating may be interpreted as meaning two gratings which are configured such that a substantial proportion of radiation diffracted by one of the gratings is incident upon the other grating. The amount of radiation which is reflected by the composite grating depends upon the degree to which the respective imprint template grating and substrate grating are aligned. The pitch of the gratings may be of the same order as the wavelength of the alignment radiation beam, and as a result the physics which governs the reflection of radiation by the composite grating is complicated. In order to aid an intuitive understanding, the following is a simplified explanation based on geometrical optics.
Reflective lines of the substrate grating 44 a , 44 b and/or 44 c will reflect radiation upwards to the detector 40 , in addition to reflective lines of the respective imprint template grating 42 a , 42 b , and/or 42 c . The amount of radiation which is reflected by the substrate grating 44 a , 44 b and/or 44 c and respective imprint template grating 42 a , 42 b , and/or 42 c will depend upon the extent to which the substrate grating 44 a , 44 b and/or 44 c is aligned with the respective imprint template grating 42 a , 42 b , and/or 42 c . If the imprint template grating 42 a , 42 b , and/or 42 c and the respective substrate grating 44 a , 44 b and/or 44 c are positioned such that lines of the substrate grating 44 a , 44 b and/or 44 c are located directly beneath lines of the respective imprint template grating 42 a , 42 b , and/or 42 c , then little of the alignment radiation beam 35 a will be reflected from the substrate grating 44 a , 44 b and/or 44 c . This is because the alignment radiation which passes between reflective lines of the imprint template grating 42 a , 42 b , and/or 42 c will not be incident upon reflective lines of the respective substrate grating 44 a , 44 b and/or 44 c , but will instead pass between those lines without a significant proportion of the radiation being reflected. At the opposite extreme, if the substrate grating 44 a , 44 b and/or 44 c were to be positioned such that it was out of phase with the respective imprint template grating 42 a , 42 b , and/or 42 c (i.e. such that lines of the substrate grating 44 a , 44 b and/or 44 c lie beneath gaps of the respective imprint template grating 42 a , 42 b , and/or 42 c ), then alignment radiation which passed between lines of the imprint template grating 42 a , 42 b , and/or 42 c would be incident upon lines of the respective substrate grating 44 a , 44 b and/or 44 c . A substantial amount of alignment radiation would therefore be reflected by the substrate grating 44 a , 44 b and/or 44 c.
The physics which governs the reflection of alignment radiation by the composite grating formed by the imprint template grating 42 a , 42 b , and/or 42 c and the respective substrate grating 44 a , 44 b and/or 44 c is more complex than that described above. However, the effect is the same—namely that the amount of radiation which is incident upon the detector 40 depends upon the extent to which the substrate grating 44 a , 44 b and/or 44 c is aligned with the respective imprint template grating 42 a , 42 b , and/or 42 c.
FIG. 3 b shows a situation in which the substrate 20 has been positioned too far to the left (i.e. too far in the negative x-direction) relative to the imprint template 24 . In this instance, the intensity of reflected alignment radiation detected by the detector 40 (see FIG. 2 ) from the left-hand imprint template grating 42 c in combination with the left-hand substrate grating 44 c is greater than the intensity detected from the central imprint template grating 42 b in combination with the central substrate grating 44 b . The intensity of reflected alignment radiation detected by the detector 40 from the central imprint template grating 42 b in combination with the central substrate grating 44 b is greater than the intensity detected from the right-hand imprint template grating 42 a in combination with the right-hand substrate grating 44 a.
The tip-tilt mirror 36 is used to direct the alignment radiation beam 35 at each of the imprint template gratings 42 a - c in turn. This is represented in FIG. 3 b by three arrows 35 a - c . The intensity of radiation reflected by the gratings is detected each time by the detector 40 .
The intensity of radiation incident upon the detector 40 , which may be thought of as a zero-order reflected intensity (reflected from gratings), may vary quadratically as a function of displacement in the x-direction. This may be represented as:
I=I 0 +Kx 2 (Equation 1)
Applying this to each of the three grating pairs shown in FIG. 3 results in the following:
I a =I 0 +K ( x−d ) 2
I b =I 0 +Kx 2
I c =I 0 +K ( x−d ) 2 (Equation 2)
where I 0 and K are constants, d represents the offset of the substrate gratings relative to the imprint template gratings, and x is the misalignment between the substrate and the imprint template.
Equation 2 may be used to determine the misalignment x between the substrate and the imprint template. Taking the difference between I c and I a yields:
I c −I a =4 Kxd (Equation 3)
Taking the average of I c and I a and adding I b to this average yields:
I a +I c −2 I b =2 Kd 2 (Equation 4)
Finally, k may be eliminated from the equations in order to obtain:
x
=
(
d
2
)
I
c
-
I
a
I
c
+
I
a
-
2
I
b
(
Equation
5
)
By using an algorithm based on Equation 5, the processor 46 may process the intensity values output from the detector 40 in order to determine the misalignment x between the substrate 20 and the imprint template 24 . Once the misalignment x has been determined, the substrate table 22 may be moved to align the substrate 20 to the imprint template 24 (i.e. to remove or reduce the misalignment). Alternatively or additionally; the imprint template holder 26 may be moved to align the imprint template 24 to the substrate 20 .
Once the substrate 20 has been aligned to the imprint template 24 , the imprint template is pressed down towards the substrate 20 , causing the imprintable medium 50 to flow into recesses of a pattern provided on the imprint template. The actinic radiation source 28 is then switched on (or the actinic radiation beam 29 is unblocked), and the beam of actinic radiation is directed onto the imprintable medium 50 . The imprintable medium solidifies, thereby retaining the pattern imprinted by the imprint template 24 . The imprint template 24 and the substrate 20 are then separated, for example by moving the substrate table 22 downwards and away from the imprint template, or by moving the imprint template holder 26 upwards and away from the substrate. The substrate 22 is then removed from the substrate table 22 , and another substrate is placed on the substrate table. The alignment and imprint process is then repeated.
Equations 1 to 5 provide an indication of why the offsets +d, −d of the substrate gratings 44 a , 44 b and/or 44 c are useful. The offsets help to ensure that the intensity of alignment radiation reflected by each of the gratings provides useful information. If no offsets were to be present, then each combination of substrate and imprint template alignment grating would provide the same information, and there would not be sufficient information available to determine the misalignment of the substrate and imprint template.
Although the illustrated offsets are provided in the substrate gratings 44 a - c , they may additionally or alternatively be provided in the imprint template gratings 42 a - c . Indeed, since the offset are relative offsets between the substrate and imprint template gratings, a positive offset of the substrate gratings could be considered to be equivalent to a negative offset of the imprint template gratings.
Although the illustrated offsets comprise two equal and opposite offsets and a zero offset (−d, +d and 0), other offsets may be used. Three different offsets should be used, since there are three unknown parameters: the alignment error, the average value of the reflected alignment radiation (I 0 ), and the curvature of the parabola defined in Equation 1 (K). The offsets may have any suitable values. One of the offsets may be zero (zero is considered to be an offset in this context).
The alignment radiation beam 35 may, for example, be a laser beam (for example a mono-chromatic beam), or alternatively white light or some other broadband radiation generated by an extended source. The alignment radiation beam 35 may, for example, have a wavelength of 632 nm, and may, for example, be generated by a helium-neon laser.
The gratings may, for example, measure 40×40 □m. The gratings may be any other suitable size. However, as mentioned above, the gratings should be sufficiently large, relative to the cross-section of the alignment radiation beam, that the alignment radiation beam does not extend beyond edges of the gratings.
The substrate grating 44 a , 44 b and/or 44 c may be partially reflective. The imprint template grating 42 a , 42 b , and/or 42 c may be partially reflective.
The imprint template grating 42 a , 42 b , and/or 42 c and the substrate grating 44 a , 44 b and/or 44 c should have a pitch which is sufficiently large to allow non-zero diffraction orders to propagate between the gratings (the term ‘non-zero diffraction orders’ in this context refers to diffraction orders other than the zero order). If the pitch were to be too small then non-zero diffraction orders formed by the imprint template grating 42 a , 42 b , and/or 42 c would fall outside of the respective substrate grating 44 a , 44 b and/or 44 c . If the alignment radiation beam 35 were to have a wavelength of 632 nm, then the pitch of the gratings may, for example, be 300 nm or greater.
The pitch of the imprint template grating 42 a , 42 b , and/or 42 c and the substrate grating 44 a , 44 b and/or 44 c may be sufficiently small, relative to the cross-sectional size of the respective alignment radiation beam 35 a , 35 b , and/or 35 c (referred to hereafter as the measurement spot diameter), that at least 20 grating lines fall within the diameter of the measurement spot. The measurement spot may, for example, have a diameter of 20-30 microns. If this were to be the case, then the maximum pitch of the gratings would be around 1.5 microns.
A gap ‘Z’ is labeled in FIG. 3 between a lowermost surface of the imprint template 24 and an uppermost surface of the substrate 20 . The gap Z is filled with the imprintable medium 50 . The size of the gap Z may be such that alignment radiation transmitted by the imprint template grating 42 a , 42 b , and/or 42 c starts diverging, but the diverging alignment radiation falls completely on the respective substrate grating 44 a , 44 b and/or 44 c . In general, the gap may be dictated by aspects of imprint lithography such as the amount of imprintable medium 50 which is present. Typically the gap is rarely more than 1-2 microns, but it may be several microns.
The detector 40 may include a wavelength discriminating apparatus, which may, for example, have a spectral resolution of 10 or more. The wavelength discriminating apparatus may be used, for example, when the alignment radiation source 34 is a broadband radiation source. The wavelength discriminating apparatus, such as a filter, is useful because the variation of reflected alignment radiation as a function of the gap Z is wavelength dependent. If the alignment radiation source 34 is a narrow-band radiation source such as a helium-neon laser, then the detector 40 may, for example, be a photodiode without a wavelength discriminating apparatus.
The initial alignment (coarse alignment) between the substrate and the imprint template should be within the capture range provided by the targets 42 , 44 . The term ‘capture range’ is intended to mean the range of misalignments of the substrate and/or template from the aligned position over which alignment can be achieved using the gratings. The capture range of an embodiment of the invention is less than the pitch of the gratings. The capture range is approximately a quarter of the pitch of the gratings of targets 42 , 44 . This link between the capture range and the grating pitch may influence the grating pitch which is used. A smaller grating pitch will require a higher accuracy of coarse alignment, in order to ensure that the coarse alignment aligns the gratings within the capture range.
Although an embodiment of the invention has been described with the alignment radiation beam 35 being directed sequentially at each of the imprint template gratings 42 a - c in turn, an embodiment of the invention may direct the alignment radiation beam at each of the imprint template gratings at the same time. This may be done, for example, by splitting the alignment radiation beam into three separate beams that simultaneously illuminate the three imprint template gratings 42 a - c . Three detectors could be used to simultaneously measure the reflected alignment radiation. In an embodiment, any number of separate alignment beams and detectors may be used. Any number of tip-tilt mirrors or other beam-directing apparatuses may be used.
The imprint template may be an imprint template which is sufficiently large to imprint an entire substrate in one go (e.g. as shown in FIG. 2 ). Where this is the case, the imprint template may be provided with a multiplicity of patterns each of which may form a separate device.
Alternatively, the imprint template may imprint part of the substrate. Where this is the case, the imprint template is then removed from the imprinted part of the substrate and is used to imprint a different part of the substrate. This is repeated until all desired parts of the substrate have been imprinted. Alignment targets (comprising alignment gratings) may be provided at a multiplicity of locations on the substrate, in order to allow the imprint template to be aligned to each part of the substrate as required.
The alignment targets described herein may comprise gratings which extend in the x-direction, and therefore provide alignment between the substrate and the imprint template in the x-direction. Alignment targets which comprise alignment gratings extending in the y-direction may alternatively or additionally be provided to obtain alignment between the substrate and the imprint template in the y-direction.
Although only two imprint template alignment targets 42 , 43 are shown in the illustrated embodiment, any number of imprint template alignment targets may be provided. For example, two imprint template alignment targets which enable alignment in the x-direction and two which enable alignment in the y-direction may be provided (this may be a useful number of alignment targets to provide alignment of the imprint template and the substrate). Three, four or more imprint template alignment targets which enable alignment in the x-direction and three, four or more which enable alignment in the y-direction may be provided.
In the described embodiment, alignment is achieved by moving the substrate table 20 in the x and y directions. However, it is possible to move the imprint template 24 in the x and y directions to achieve alignment. This may be done instead of, or as well as, movement of the substrate table 20 in the x and y directions. In general terms, it may be that there is relative movement between the substrate and the imprint template.
An advantage of embodiment of the invention is that it does not require that the gratings are scanned relative to one another in order to obtain an alignment signal (as is the case with a phase-grating alignment based system).
A further advantage of an embodiment of the invention is that it does not require an imaging detector, but instead may rely upon intensity detection (an intensity detector is generally cheaper than an imaging detector).
The above described embodiment of the invention may be used for alignment between an imprint template 24 and a substrate 20 , as described above. In some instances, it may be desirable to monitor the alignment between the imprint template 24 and the substrate 20 over a period of time. For example, exposure of the imprintable medium 50 to the actinic radiation beam 29 may take place for several seconds, in order to ensure that the imprintable medium is cured and hence solidified. It may be desirable to monitor the alignment between the imprint template 24 and the substrate 20 during this period, and to minimize or reduce deviation from the aligned position during the period.
The embodiment of the invention described above may have a relatively slow speed of response (for example 0.1 seconds or slower), and may therefore not be capable of measuring and compensating for alignment deviations which occur more rapidly than this. An alignment apparatus which may have a faster response speed, and which may therefore be capable of measuring and compensating for such alignment deviations is shown in FIG. 4 .
FIG. 4 shows part of an imprint lithography apparatus. Many of the features shown in FIG. 4 correspond with features shown in FIG. 2 . Where this is the case, the features are provided with common reference numerals and are not described in detail here.
In FIG. 4 , a substrate 20 is held on a substrate table 22 , and an imprint template 24 is held by a template holder 26 . Alignment targets 42 , 43 are provided on the imprint template, and are positioned over corresponding alignment targets 44 , 45 provided on the substrate 20 . Imprintable medium 50 is provided between the imprint template 24 and the substrate 20 .
The apparatus of FIG. 4 further comprises an interferometer 60 which is arranged to direct a beam of coherent radiation towards a mirror 62 provided on a side of the substrate table 22 . This interferometer will hereafter be referred to as the substrate table interferometer 60 . The apparatus further comprises an interferometer 64 which is arranged to direct a radiation beam at a mirror 66 provided on a side of the imprint template holder 26 . This interferometer will hereafter be referred to as the imprint template holder interferometer 64 . Outputs from the interferometers 60 , 64 pass to the processor 46 (the same processor which receives signals output from the detector 40 shown in FIG. 2 ).
The interferometers 60 , 64 are capable of measuring the positions of the substrate table 22 and the imprint template holder 26 respectively with a high accuracy, which may, for example, be of the order of a few nanometers. The interferometers may have a faster speed of response than the alignment apparatus described above in relation to FIGS. 2 and 3 . The interferometers may, for example, have a bandwidth of the order of kilohertz.
The substrate 20 may be securely fixed to the substrate table 22 . This may for example be achieved by applying a vacuum to a lowermost surface of the substrate 20 through the substrate table 22 . Since the substrate 20 is securely fixed to the substrate table 22 , when the interferometer 60 detects movement of the substrate table 22 , the substrate 20 will also have undergone the same movement. Thus, movement of the substrate 20 may be monitored using the substrate table interferometer 60 .
The imprint template 24 is securely held by the template holder 26 . Thus, movement of the imprint template 24 may be monitored using the imprint template holder interferometer 64 .
The detector 40 (see FIG. 2 ) and the interferometers 60 , 64 may be rigidly held such that they do not move relative to one another (to within tolerances required to achieve a satisfactory alignment). For example, the detector 40 and interferometers 60 , 64 may be mounted on a frame of the lithographic apparatus (sometimes referred to as a metrology frame).
During alignment, an aligned position between the substrate 20 and the imprint template 24 may be determined using the alignment targets 42 - 45 and the detector 40 . The respective positions of the substrate table 22 and imprint template holder 26 for this aligned position may be measured using the interferometers 60 , 64 . Subsequent deviation of the substrate table 20 or imprint template holder 26 away from the aligned position may be measured by the interferometers 60 , 64 and corrected for by the processor. This may allow correction for deviations from the aligned position which may, for example, arise due to heating, mechanical disturbances, or other factors.
The interferometers 60 , 64 may be used to reduce or minimize deviation of the substrate 20 and/or imprint template 24 away from the aligned position during removal of the imprint template from the substrate (i.e. after the imprintable medium 50 has been cured).
Although the detector 40 and interferometers 60 , 64 have been described as being held on the same frame, they may be held on different frames. Where this is the case, an interferometer may be used to monitor relative movement between the frames.
A further imprint lithography apparatus to which an embodiment of the invention may be applied is shown schematically in FIG. 5 . A substrate 20 is held on a substrate table 22 , and is provided with a layer of imprintable medium 50 . The substrate 20 has been provided with a plurality of alignment targets 44 , 45 , 144 , 145 (other alignment targets are present but not labeled). A first imprint template holder 26 a holds a first imprint template 24 a , and a second imprint template holder 26 b holds a second imprint template 24 b . Each of the imprint template holders 26 a , 26 b is independently moveable both in the Z direction, and optionally independently moveable in a plane which is parallel to the surface of the substrate table 22 . Each imprint template 24 a , 24 b is provided with a plurality of alignment targets 42 , 43 , 142 , 143 .
The first and second imprint templates 24 a , 24 b are independently moved to or onto different locations on the substrate 20 , and are used to imprint a pattern onto the substrate in a manner described further above. The first and second imprint templates 24 a , 24 b are smaller than the substrate 20 , and thus multiple imprints by the imprint templates are needed in order to imprint patterns over the surface of the substrate.
In some instances it may be desirable to align the second imprint template 24 b with respect to the substrate 20 while the first imprint template 24 a is already aligned and is imprinting a pattern into the imprintable medium 50 (or vice versa). This is represented in FIG. 5 by an arrow showing actinic radiation 129 being directed through the first imprint template 24 a onto the substrate, and a double-headed arrow showing movement of the second imprint template 24 b in the x-direction. When this is the case, it may be desirable not to move the substrate table 22 during alignment of the second imprint template 24 b.
In a conventional phase grating based alignment system it may not be possible to imprint with a first imprint template 24 a while aligning a second imprint template 24 b . This is because movement of the substrate table 22 may be needed in order to generate a phase grating alignment signal. Instead of using a phase grating alignment system, the alignment system described further above in relation to FIGS. 2 and 3 may be used. This alignment system does not require movement of the substrate 22 in order to determine alignment, and therefore allows the second imprint template 24 b to be aligned to the substrate 20 without moving the substrate 20 .
The alignment system therefore allows alignment between the second imprint template 24 b and the substrate 20 while the first imprint template 24 a is imprinting a pattern into imprintable medium 50 provided on the substrate. This allows the imprint templates 24 a , 24 b to be moved independently of one another, thereby allowing flexibility in the routing of the imprint templates over the substrate 20 , and thus facilitating improved throughput of the imprint lithography apparatus.
The alignment system is not shown in FIGS. 4 and 5 in order to avoid making FIGS. 4 and 5 overly complex. However, the manner in which the alignment system could be provided for the imprint apparatus of FIGS. 4 and 5 are straightforward. For example, in the case of FIG. 5 , elements of the alignment system such as the tip-tilt mirror 36 (see FIG. 2 ) may be provided separately for each of the imprint templates 24 a , 24 b and the detector 40 may be provided separately for each of the imprint templates, or may be used in common for more than one imprint template.
As described further above, the alignment system described in relation to FIGS. 2 and 3 does not require an imaging detector, but may instead use an intensity detector (for example, a photodiode). In a multi-template imprint lithography system, where a separate alignment system is provided for each imprint template, it may be desirable to minimize the cost of the alignment system where possible. The use of an intensity detector rather than an imaging detector for the alignment system provides a reduction of the cost of the alignment system. This reduction of cost may be significant when two or more imprint templates are provided in the lithographic apparatus. Although two imprint templates are shown in FIG. 5 , any number of imprint templates (and corresponding alignment systems) may be used. The greater the number of imprint templates, the greater the cost saving provided by using an intensity detector rather than an imaging detector. Of course, an imaging detector based alignment system may used in combination with the alignment system described herein. For example, one template may have an imaging detector based alignment system and another template may have the alignment system described herein.
Although described embodiments of the invention, use UV radiation imprint lithography, an embodiment of the invention may use another form of imprint lithography such as hot imprint lithography.
|
A method of determining a position of a substrate relative to an imprint template is described, wherein the imprint template has at least three gratings and the substrate has at least three gratings positioned such that each imprint template grating forms a composite grating with an associated substrate grating, the at least three imprint template gratings and associated substrate gratings having offsets relative to one another. The method includes detecting an intensity of radiation which is reflected by the three composite gratings, and using the detected intensities to determine displacement of the substrate or imprint template from a position.
| 1
|
TECHNICAL FIELD
The technical field relates generally to program analysis. More particularly, it pertains to the enhancing of type reconstruction for bytecode programs so as to enhance program analysis.
Copyright Notice—Permission
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 files or records, but otherwise reserves all copyright rights whatsoever. The following notice applies to the software and data as described below and in the drawings attached hereto: Copyright© 1999, 2000, Microsoft Corporation, All Rights Reserved.
BACKGROUND
A program is a list of statements. These statements are written by a programmer in a language that is readable by humans. This list of statements may be translated, through processes that include front-end compilation, to produce an executable file that can cause a computer to perform a desired action. One front-end compilation process produces a bytecode program.
Bytecode programs are processor-independent programs that cannot be directly executed by most central processing units but are highly suitable for further processing, such as for generating binary instructions for various central processing units (CPUs). Because CPUs speedily interpret and execute binary instructions, it is advantageous to further compile the bytecode programs to produce binary instructions through a technique called back-end compilation.
A variable used in a program is expressed as a particular type. A type defines the nature of a variable. Types in programs are declared by the programmer and determine the range of values a variable can take as well as the operations that can be performed on it. Types enable a compiler to check that variables are used in a way that is consistent with their nature to avoid errors. Examples of type include integer, real number, text character, floating-point number, or classes.
The front-end compilation typically removes much of the type information in the process of producing a bytecode program. Such omission of type information constrains the ability of the back-end compilation to check for errors. Such a compilation process may produce inferior programs and lead to the eventual lack of acceptance of such programs in the marketplace.
Thus, what is needed are systems, methods, and structures to enhance reconstructing type information for bytecode programs.
SUMMARY
Systems, methods, and structures for enhancing type reconstruction are discussed. An illustrative aspect includes a system for enhancing program analysis. The system comprises a translator receptive to a first program to produce a second program and a type elaboration engine to produce an intermediate program. The type elaboration engine includes filters to produce reconstructed types of the intermediate program so as to enhance program analysis. The system further comprises an analyzer receptive to the intermediate program to produce a desired result.
Another illustrative aspect includes a method for enhancing type reconstruction. The method comprises collecting at least one constraint from an intermediate program, filtering the at least one constraint to obtain at least one solution, and constructing at least one type by selecting a minimal solution from the at least one solution.
Another illustrative aspect includes a method for collecting constraints for type reconstruction. The method comprises focusing on a portion of an intermediate program. The portion includes an unknown type and a remainder of the portion. The method further comprises determining at least one relationship between the unknown type and the remainder of the portion so as to solve the unknown type. The at least one relationship includes an equality relationship and an inequality relationship.
Another illustrative aspect includes a method for filtering to enhance type reconstruction. The method includes forming a first set of types. Each type in the first set of types has a less than or equal to relationship with respect to an unknown type. The method further comprises forming a filter for a type in the first set of types. The filter forms a second set of types. The type in the first set of types has a less than or equal to relationship with respect to each type in the second set of types. The act of forming a first set of types is iterated for each unknown type in a collection of constraints. The act of forming a filter is iterated for each type in the first set of types so as to form a plurality of the second set of types. The method further comprises intersecting each second set of types with other second sets of types to form a set of solutions to the collection of constraints.
Another illustrative aspect includes a method for constructing types. The method comprises selecting a minimal solution as a desired solution from a set of solutions that is obtained from filtering at least one constraint so as to determine an unknown type for an intermediate program of a bytecode program. The act of selecting includes mapping the desired solution to a type in a type hierarchy of a source program of the bytecode program if a one-to-one correspondence exists between the desired solution and the type in the type hierarchy. The act of selecting includes forming a desired type for the desired solution in a type hierarchy of a source program of the bytecode program if the type hierarchy lacks the desired type. The desired solution is the minimal solution when the desired solution has a greater than or equal to relationship with respect to other solutions in the set of solutions.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a system according to one aspect of the present invention.
FIGS. 2A–2B are block diagrams of a system according to one aspect of the present invention.
FIGS. 3A–3B illustrate a fragment of a type hierarchy according to one aspect of the present invention.
FIG. 4 is a process diagram of a method according to one aspect of the present invention.
FIG. 5 is a process diagram of a method according to one aspect of the present invention.
FIG. 6 is a process diagram of a method according to one aspect of the present invention.
FIGS. 7A , 7 B, 7 C, 7 D, 7 E and 7 F illustrate a fragment of a type hierarchy according to one aspect of the present invention.
FIG. 8 is a process diagram of a method according to one aspect of the present invention.
FIG. 9 is a process diagram of a method according to one aspect of the present invention.
FIG. 10 is a process diagram of a method according to one aspect of the present invention.
FIG. 11 is a process diagram of a method according to one aspect of the present invention.
FIG. 12 is a structure diagram of a data structure according to one aspect of the present invention.
DETAILED DESCRIPTION
In the following detailed description of exemplary embodiments of the invention, reference is made to the accompanying drawings which form a part hereof, and in which is shown, by way of illustration, specific exemplary embodiments in which the invention may be practiced. In the drawings, like numerals describe substantially similar components throughout the several views. These embodiments are described in sufficient detail to enable those skilled in the art to practice the invention. Other embodiments may be utilized and structural, logical, electrical, and other changes may be made without departing from the spirit or scope of the present invention. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the present invention is defined only by the appended claims.
FIG. 1 is a block diagram of a system according to one aspect of the present invention. FIG. 1 provides a brief, general description of a suitable computing environment in which the invention may be implemented. The invention will hereinafter be described in the general context of computer-executable program modules containing instructions executed by a personal computer (PC). Program modules include routines, programs, objects, components, data structures, etc., that perform particular tasks or implement particular abstract data types. Those skilled in the art will appreciate that the invention may be practiced with other computer-system configurations, including hand-held devices, multiprocessor systems, microprocessor-based programmable consumer electronics, network PCs, minicomputers, mainframe computers, and the like, which may have multimedia capabilities. The invention may also be practiced in distributed computing environments where tasks are performed by remote processing devices linked through a communications network. In a distributed computing environment, program modules may be located in both local and remote memory storage devices.
FIG. 1 shows a general-purpose computing device in the form of a conventional personal computer 120 , which includes processing unit 121 , system memory 122 , and system bus 123 that couples the system memory and other system components to processing unit 121 . System bus 123 may be any of several types, including a memory bus or memory controller, a peripheral bus, or a local bus, and may use any of a variety of bus structures. System memory 122 includes read-only memory (ROM) 124 and random-access memory (RAM) 125 . A basic input/output system (BIOS) 126 , stored in ROM 124 , contains the basic routines that transfer information between components of personal computer 120 . BIOS 126 also contains start-up routines for the system. Personal computer 120 further includes hard disk drive 127 for reading from and writing to a hard disk (not shown), magnetic disk drive 128 for reading from and writing to a removable magnetic disk 129 , and optical disk drive 130 for reading from and writing to a removable optical disk 131 such as a CD-ROM or other optical medium. Hard disk drive 127 , magnetic disk drive 128 , and optical disk drive 130 are connected to system bus 123 by a hard-disk drive interface 132 , a magnetic-disk drive interface 133 , and an optical-drive interface 134 , respectively. The drives and their associated computer-readable media provide nonvolatile storage of computer-readable instructions, data structures, program modules, and other data for personal computer 120 . Although the exemplary environment described herein employs a hard disk, a removable magnetic disk 129 and a removable optical disk 131 , those skilled in the art will appreciate that other types of computer-readable media which can store data accessible by a computer may also be used in the exemplary operating environment. Such media may include magnetic cassettes, flash-memory cards, digital versatile disks, Bernoulli cartridges, RAMs, ROMs, and the like.
Program modules may be stored on the hard disk, magnetic disk 129 , optical disk 131 , ROM 124 , and RAM 125 . Program modules may include operating system 135 , one or more application programs 136 , other program modules 137 , and program data 138 . A user may enter commands and information into personal computer 120 through input devices such as a keyboard 140 and a pointing device 142 . Other input devices (not shown) may include a microphone, joystick, game pad, satellite dish, scanner, or the like. These and other input devices are often connected to the processing unit 121 through a serial-port interface 146 coupled to system bus 123 ; but they may be connected through other interfaces not shown in FIG. 1 , such as a parallel port, a game port, or a universal serial bus (USB). A monitor 147 or other display device also connects to system bus 123 via an interface such as a video adapter 148 . In addition to the monitor, personal computers typically include other peripheral output devices such as a sound adapter 156 , speakers 157 , and further devices such as printers.
Personal computer 120 may operate in a networked environment using logical connections to one or more remote computers such as remote computer 149 . Remote computer 149 may be another personal computer, a server, a router, a network PC, a peer device, or other common network node. It typically includes many or all of the components described above in connection with personal computer 120 ; however, only a storage device 150 is illustrated in FIG. 1 . The logical connections depicted in FIG. 1 include local-area network (LAN) 151 and a wide-area network (WAN) 152 . Such networking environments are commonplace in offices, enterprise-wide computer networks, intranets, and the Internet.
When placed in a LAN networking environment, PC 120 connects to local network 151 through a network interface or adapter 153 . When used in a WAN networking environment such as the Internet, PC 120 typically includes modem 154 or other means for establishing communications over network 152 . Modem 154 may be internal or external to PC 120 , and connects to system bus 123 via serial-port interface 146 . In a networked environment, program modules, such as those comprising Microsoft® Word, which are depicted as residing within PC 120 or portions thereof, may be stored in remote storage device 150 . Of course, the network connections shown are illustrative, and other means of establishing a communications link between the computers may be substituted.
Software may be designed using many different methods, including object-oriented programming methods. C++ is one example of common object-oriented computer programming languages that provides the functionality associated with object-oriented programming. Object-oriented programming methods provide a means to encapsulate data members (variables) and member functions (methods) that operate on that data into a single entity called a class. Object-oriented programming methods also provide a means to create new classes based on existing classes.
An object is an instance of a class. The data members of an object are attributes that are stored inside the computer memory, and the methods are executable computer code that act upon this data, along with potentially providing other services. The notion of an object is exploited in the present invention in that certain aspects of the invention are implemented as objects in one embodiment.
An interface is a group of related functions that are organized into a named unit. Each interface may be uniquely identified by some identifier. Interfaces have no instantiation, that is, an interface is a definition only lacking the executable code needed to implement the methods which are specified by the interface. An object may support an interface by providing executable code for the methods specified by the interface. The executable code supplied by the object must comply with the definitions specified by the interface. The object may also provide additional methods. Those skilled in the art will recognize that interfaces are not limited to use in or by an object-oriented programming environment.
FIGS. 2A–2B are block diagrams of a system according to one aspect of the present invention. In FIG. 2A , a system includes a source program 202 0 . The source program 202 0 includes a program that is written in a computer programming language, such as Java. The source program 202 0 is input into a translator 204 . The translator 204 translates the source program 202 0 into a bytecode program 206 0 . In this embodiment, the translator 204 acts as a compiler.
The bytecode program 206 0 is an encoding of the source program 202 0 that the translator 204 produces when the source program 202 0 is processed. This encoding is in a processor-independent form that cannot be directly executed by most central processing units but is highly suitable for further analysis. One kind of analysis includes type checking. Type checking is a process performed by a compiler or interpreter to make sure that when a variable is used, the variable is treated as having the same data type as it was declared to have. A program that passes the rigors of the type checking analysis can be considered a program with strong typing. Strong typing is typically a characteristic of a programming language that does not allow the program to change the data type of a variable during program execution. Thus, strong typing has long been recognized as improving program correctness and enhancing efficient implementation. The various embodiments of the present invention extend the benefits of strong typing characteristics to intermediate forms of the bytecode program.
But to even begin the process of type checking a program, the program has to have types. The process of encoding the source program 202 0 by the translator 204 to produce the bytecode program 206 0 removes some of the types that were present in the source program 202 0 . In other words, the bytecode program 206 0 lacks some of the types that were present in the source program 202 0 . Some of the missing types include types for local variables, types for evaluation stack locations, types for small integers, such as booleans, bytes, shorts, chars, and integers. To reconstruct these types, the bytecode program 206 0 undergoes a type inference technique called type elaboration.
Returning to FIG. 2A , the bytecode program 206 0 is input into a type elaboration engine 208 . In one embodiment, the bytecode program 206 0 includes a verifiable bytecode program. The type elaboration engine 208 produces an intermediate program 210 0 . The type elaboration engine 208 includes filters to produce reconstructed types in the intermediate program 210 0 . Filters as discussed hereinbefore and hereinafter include using either upwardly closed sets or downwardly closed sets to filter solutions for reconstructed types. These reconstructed types help any further analysis of the intermediate program 210 0 .
The intermediate program 210 0 is input into an analyzer 212 . The analyzer 212 is receptive to the intermediate program 210 0 to produce a desired analytical result. In one embodiment, the analyzer 212 includes a compiler optimizer that enhances the execution of the intermediate program. In another embodiment, the analyzer 212 includes an interpreter that is adapted to use the reconstructed types to securely execute the intermediate program as an applet within a browser. In another embodiment, the analyzer 212 includes a generator that generates binary instructions from the intermediate program for a desired central processing unit. In a further embodiment, the analyzer 212 includes a debugger that is adapted to debug the intermediate program; the debugger is also adapted for type checking the intermediate program using the reconstructed types so as to enhance the identification of faults. In yet another embodiment, the analyzer 212 includes a garbage collector that is adapted to eliminate at least one undesired object of the reconstructed types.
FIG. 2B includes similar elements as discussed in FIG. 2A . For clarity purposes, the numerical subscripts of some of the reference numbers have been changed to depict particular aspects of the invention. The system includes the bytecode program 206 1 . The bytecode program 206 1 is input into the type elaboration 208 to produce the intermediate program 210 1 . In one embodiment, the bytecode program 206 1 is a verifiable bytecode program. The intermediate program 210 1 is then input into the translator 204 to produce a source program 202 1 . In this embodiment, the translator 204 acts as a decompiler.
FIGS. 3A–3B illustrate a fragment of a type hierarchy according to one aspect of the present invention. In FIG. 3A , program fragment 300 includes four interface definitions that define a fragment of a type hierarchy 302 . For illustrative purposes only, the program fragment 300 is a Java program fragment. Thus, the type hierarchy 302 includes an Object type 304 . Although the Object type 304 is not explicitly defined in the program fragment 300 , all classes automatically extend the Object type because the Object type is a supertype of all reference types in Java. The type hierarchy 302 also includes a Null type 316 . Although the Null type is not explicitly defined in the program fragment 300 , the Java programming language includes the Null type 316 that types a value, which is used to initialize instantiations of types.
The type hierarchy 302 includes a type SI 308 and a type SJ 306 as defined in the program fragment 300 . The type hierarchy 302 also includes a type I 312 and a type J 314 as defined in the program fragment 300 . Because the type I 312 and the type J 314 extend the type SI 308 , two lines emanate from the type SI 308 and terminate at the type I 312 and the type J 314 . Likewise, because the type I 312 and the type J 314 also extend the type SJ 306 , two lines emanate from the type SJ 306 and terminate at the type I 312 and the type J 314 . Therefore, the type I 312 has a multiple inheritance relationship with the type SI 308 . The type J 314 has a multiple inheritance relationship with the type SJ 306 .
In one embodiment, the type hierarchy 302 can be thought of as a mathematical hierarchy involving sets. For instance, the type SI 308 can be thought of as a set SI 308 . The set SI 308 includes three elements, which are the type SI 308 , the type I 312 , and the type J 314 . In the type hierarchy 302 , to indirectly reference the type I 312 and the type J 314 , it is possible to set the type of the indirect reference to the type SI 308 since the type SI 308 is a supertype of the type I 312 and the type J 314 . Thus, the type SI 308 can be thought of as the set SI 308 containing those types as discussed. In this embodiment, the inheritance relationship between any supertype and subtype (such as the type I 312 and the type SI 308 ) can be mathematically described as a less than or equal to relationship (such as I≦SI). The needs for describing the type hierarchy mathematically will be discussed hereinafter.
In FIG. 3B , a method of a program 320 is shown. This method is a method of a bytecode program but has been rendered in pseudo-code for clarity purposes. As can be seen, the type of the local variable x has been removed. Such removal may have occurred during the process of compiling a source program into a bytecode program. Notwithstanding the lack of typing information for the local variable x, the embodiments of the present invention provide a constraint collection technique to learn from the remaining portions of the method 320 to solve for the type of the local variable x.
For illustrative purposes only, from the method 320 , the type of x must be a type that can be assigned to the type I 312 or the type J 314 yet must be able to invoke the method siMeth( ) of the type SI 308 or the method sjMeth( ) of the type SJ 306 . Mathematically, there must be an element on the type hierarchy 302 that is greater than or equal to the types I 312 and J 314 (a supertype) but is less than or equal to the types SI 308 and SJ 306 (a subtype). However, the type hierarchy 302 lacks such a type. The embodiments of the present invention form a new type 310 to solve for x. However, if the type hierarchy 302 already includes the type 310 , the type 310 is selected as the desired type for x. These embodiments of the present invention are discussed in greater detail below.
Mathematically, the subtyping relationships between types in a programming language, such as Java, can be combined to form a partial ordering of the types. Thus, A is less than B if type A is a subtype of type B. The types A and B can be translated into elements of a set hierarchy with a “less than or equal to” relation. Thus, type hierarchies are partial orders (or posets) but not necessarily lattices. By definition, partial orders may lack all infimum and all supremum. However, in certain circumstances, a solution to a type reconstruction process requires that an infimum or a supremum be present in the type hierarchy. One suitable technique to add the needed infimum or supremum to partial orders includes the Dedekind-MacNeille completion. See H. M. MacNeille, Partial Ordered Sets , Transactions of the American Mathematical Society, 42:90–96 (1937); see also, G. Birkhoff, Lattice Theory , volume 25 of Colloquium Publications, American Mathematical Society (3 rd ed. 1995); see also, B. A. Davey and H. A. Priestley, Introduction to Lattices and Order , Cambridge Mathematical Textbooks (1990). The use of such a technique does not limit the embodiments of the present invention, and as such, will not be presented in full here. However, to enhance the computation of the type reconstruction, it is advantageous to use a technique that adds only a minimal number of elements into the type hierarchy.
FIG. 4 is a process diagram of a method according to one aspect of the present invention. A process 400 is a method for enhancing type reconstruction. In one embodiment, the process 400 is executed near the beginning of the compilation process. The process 400 includes an act 402 for processing preliminarily a bytecode program to produce an intermediate program. The act of processing 402 acts to condition the bytecode program by producing the intermediate program to ease the type reconstruction process. The act of processing 402 includes an act of assigning a type variable for each local variable of the bytecode program. The type variable is indicative of an unknown type. For illustrative purposes only, the unknown type may be assigned a temporary name, such as α n . “n” can be any integer used to uniquely identify each unknown type.
The process 400 includes an act 404 for collecting at least one constraint from the intermediate program. A constraint is a relationship between known types and unknown types. A collection of constraints may contain sufficient information regarding the relationships between types and unknown types such that a solution or a set of solutions for the unknown types emerges. These known types and unknown types are extracted from a portion of the intermediate program. The portion includes a statement, a declaration, or an expression of a bytecode program. The process 400 includes an act 406 for adding additional constraints for potential array types.
The process 400 includes an act 408 for eliminating cycles in the at least one constraint. A cycle exists when a type or an unknown type refers to itself in the collection of constraints. The act for eliminating cycles 408 improves performance of the process 400 by removing these cycles.
The process 400 includes an act 410 for filtering the at least one constraint to obtain at least one solution. The process 400 includes an act 412 for constructing at least one type by selecting a solution. The act for constructing 412 presents a type that is already known if that is the solution. Otherwise, the act for constructing 412 creates a new type.
The process 400 includes an act 414 for recording the solution for each unknown type. The act 414 for recording also resolves any the loss of type information with respect to small integer types, such as booleans, bytes, shorts, characters, and integers. Given the information provided by the collection of constraints, the type information for small integer types are made concrete in the act 414 by inserting type casting. In other words, if the bytecode convolves the integer types in a way that causes a larger integer value to be used in a context expecting a smaller integer, then appropriate type casting will be made by the act 414 for small integers.
FIG. 5 is a process diagram of a method according to one aspect of the present invention. A process 500 is a method for preliminary processing of a bytecode program to produce an intermediate program. The process 500 includes an act 502 for replacing at least one reference to a stack by at least one local variable to reduce complexity. The bytecode program is often stacked-based. Stacked-based programs are not a convenient form for further processing. Thus the act for replacing 502 replaces references in the bytecode program to the stack with explicit temporary variables. These temporary variables can be treated as local variables. However, in another embodiment, the bytecode program may be processed as is without executing the act for replacing 502 .
The process 500 includes an act 504 for assigning selectively a unique name to a variable so as to inhibit ambiguous uses of the variable. The bytecode program may permit a local variable to hold values of distinct types at different places in a method of the bytecode program. However, this sort of typing defeats the impetus toward strong typing. Thus, it is necessary to separate any ambiguous uses of locals. This is accomplished by the act for assigning 504 by having each static assignment to a local variable have a unique name.
The process 500 includes an act 506 for inlining at least one subroutine that is used by the bytecode program to preserve a context of a local variable. Such a subroutine may be used to allow multiple types for the same local variable so long as that local variable is not referenced within a particular programming block, such as the “finally” block of a “try/finally” set of handlers. But again, this defeats the very benefit of strong typing. However, in one embodiment, the act for inlining 506 is optionally executed since inlining the at least one subroutine is not a necessary condition for a successful type reconstruction.
FIG. 6 is a process diagram of a method according to one aspect of the present invention. A process 600 is a method for collecting constraints for type reconstruction. In one embodiment, the process 600 is executed to collect constraints for local variables for each method. The process 600 includes an act 602 for focusing on a portion of an intermediate program. The portion includes an unknown type and a remainder of the portion. The remainder of the portion includes additional information, such as other unknown types, known types, or relationships that can be further collected.
The process 600 includes an act 604 for determining at least one relationship between the unknown type and the remainder of the portion. The following table illustrates a portion of constraints that can be collected from an intermediate program.
The conventions of the symbols in the table can be as thus explained: The first column is simply a numerical indicator of each constraint for easy referencing in the following discussion. The second column is the nomenclature for a particular portion of a program for which constraints are being collected. The final column is the constraint information that is extracted from the said portion of the program. The constraint information includes an unknown type, a relationship, and the remainder of the portion of the program. The process 600 for collecting constraints will be iterated on the remainder of the said portion of the program to collect further constraint information.
I [ c ] = { α c = Σ ( c ) } ( 1 ) I [ x ] = { α x = Σ ( x ) } ( 2 ) I [ e , a ] = { α e ≤ Ω , α e , a = I } ⋃ I [ e ] where Σ ( a ) = Ω . I ( 3 ) I [ f ( e 1 , … , e n ) ] = { α f ( e 1 , … , e n ) = I ′ } ⋃ ( ⋃ i = 1 n I [ e i ] ) ⋃ ( ⋃ i = 1 n { α ei ≤ I i } ) ( 4 ) where Σ ( f ) = ( I i , … , I n ) -> I ′ I [ le = e ] = { α ≤ α le } ⋃ I [ le ] ⋃ I [ e ] ( 5 ) I [ return 1 e ] = α e ≤ I ′ } ⋃ I [ e ] where Σ ( f ) = I -> -> I ′ ( 6 ) I [ if ( e ) s 1 else s 2 ] = { α c ≤ Boolean } ⋃ I [ e ] ⋃ I [ s 2 ] ⋃ I [ s 2 ] ( 7 ) I [ let z = e in s ] = { α c ≤ α z } ⋃ I [ e ] ⋃ I [ s ] ( 8 ) I [ s 1 ; s 2 ] = I [ s 1 ] ⋃ I [ s 2 ] ( 9 ) I [ f ( x : Ω ′ , x 1 : I 1 , … , x n : I n ) { s } ] = { a x ≤ Ω ′ , α x = Ω } ⋃ ( ⋃ i - 1 n { α xi ≤ I i } ) ⋃ I [ s ] ( 10 ) where Σ ( f ) = ( Ω , I 1 , … , I n ) -> I ′ and Σ ( x ) = Ω ′ , Σ ( x i ) = I i , i = 1 … n
Every type of constraint is in a form of I[M], wherein I denotes a constraint collector, and where M is a portion of an intermediate program. Therefore, row (1) denotes constraint collection for a constant variable c. Row (2) denotes constraint collection for a parameter variable x. Row (3) denotes constraint collection for a field selection e.a. Row (4) denotes constraint collection for an invocation of a function f. Row (5) denotes constraint collection for an assignment statement. Row (6) denotes constraint collection for a return statement, where f is a function to which the return statement will return the execution of a program. Row (7) denotes constraint collection for a conditional statement. Row (8) denotes constraint collection for a local variable definition. Row (9) denotes a sequence of statements. Row (10) denotes a declaration of a function.
The right side of the equal sign in the table is the information that is extracted from the portion M of the intermediate program. Every α denotes an unknown type. Σ denotes a signature, which maps field names, method names, parameters, and constants to types. The signature is intended to model declared types and the types of the basic constants of the language, which include predefined functions, such as arithmetic functions. Ω is a set of reference types. I is a set of base types. Ω.I is a set of field types. (Ω, I 1 , . . . ,I n )→I′ is a set of method types, where Ω is the type of the this pointer, I 1 , . . . ,I n are the types for the parameters, and I′ is the type for the return of the method.
The information includes at least one relationship. The relationship can either be an equality relationship or an inequality relationship. The equality relationship is denoted by an equal sign “=”. The inequality relationship is denoted by a less than or equal to sign “≦”. The equality relationship defines two situations: it may define an unknown type to be a known type or it may define an unknown type to be another unknown type. In one embodiment, the equality relationship is transformed into two inequality relationships; thus, x=y may be represented as x≦y and y≦x. The inequality relationship may also define two situations: it may define that an unknown type has a less than or equal to relationship with a known type or it may define that an unknown type has a less than or equal to relationship with another unknown type.
The act for focusing 602 and the act for determining 604 may be iterated on the remainder of the portion to collect further constraints. The process for collecting constraints 600 may be iterated for each subroutine found in the intermediate program. In one embodiment, small integer constants are given the type of the smallest containing the small integer type.
FIGS. 7A–7F illustrate a fragment of a type hierarchy according to one aspect of the present invention. FIGS. 7A–7F contain elements similar to FIG. 3A . The hereinbefore discussion relating to those similar elements is incorporated here in full. FIGS. 7A–7E illustrate a method for filtering a collection of constraints to solve for unknown types. The method for filtering as discussed hereinbefore and hereinafter includes a method that is based on using upwardly closed sets as shown in FIGS. 7A–7E . However, an equivalent method may be based on using downwardly closed sets; such a method is the inverse of the method as discussed with FIGS. 7A–7E . FIG. 7F illustrates a method for selecting a minimal solution. The specific example used in FIGS. 7A–7F is for the purpose of illustration only.
In FIG. 7A , the fragment 702 of a type hierarchy includes types SI 708 and type SJ 706 . The fragment 702 also includes a type I 712 that has a subtype relationship with the type SI 708 and the type SJ 706 . The fragment 702 also includes a type J 714 that has a subtype relationship with the type SI 708 and the type SJ 706 . FIG. 7A also includes a collection of constraints 7000 collected from the fragment 702 . The collection of constraints 7000 indicates that the unknown type a is greater than or equal to the type I 712 and the type J 714 , and is less than or equal to the type SI 708 and the type SJ 706 .
Hereinafter, for clarity purposes, many of the reference numbers are eliminated from subsequent drawings so as to focus on the portion of interest of the graphs of the various figures.
FIG. 7B shows the fragment 702 following the next act of processing. The first act of the method for filtering includes an act for forming a first set of types. In one embodiment, each type in the first set of types has a less than or equal to relationship with respect to the unknown type α. The set of types in the set of constraints that are less than or equal to the unknown type α is the set 700 1 which is {I, J}. Thus, the set 700 1 is the first set of types.
FIG. 7C shows the fragment 702 following the next act of processing. The second act of the method for filtering includes an act for forming a filter for a selected type in the first set of types 700 1 . The filter forms a second set of types. In one embodiment, the selected type in the first set of types has a less than or equal to relationship with respect to each type in the second set of types. The filter is denoted by the symbol ⇑. Thus, ⇑I denotes a filter for the type I 712 . The ⇑I filters the type hierarchy 702 to obtain the set 700 2 that is {I, SI, SJ} because the type I 712 is less than or equal to the type SI 708 and the type SJ 706 . In one embodiment, suppose the set 700 2 were to be formed under an actual Java type hierarchy; the set 700 2 would also include Object type. Thus, the set 700 2 is the second set of types.
FIG. 7D shows the fragment 702 following the next act of processing. The act for forming a filter is iterated for each type in the first set of types 700 1 . Therefore a filter ⇑J is formed for the type J 714 . The ⋄J filters the type hierarchy 702 to obtain the set 700 3 that is {J, SI, SJ} because the type J 714 is less than or equal to the type SI 708 and the type SJ 706 . In one embodiment, suppose the set 700 3 were to be formed under an actual Java type hierarchy; the set 700 3 would also include Object type. Thus, the set 700 3 is another second set of types.
FIG. 7E shows the fragment 702 following the next act of processing. In the embodiment that uses upwardly closed sets, the third act of the method for filtering includes an act for intersecting each second set of types with other second sets of types to form a set of solutions. In the embodiment that uses the downwardly closed sets, the third act of the method for filtering includes an act for causing a union of each second set of types with other second sets of types to form a set of solutions. Since the collection of constraints 700 0 yields only two second sets of types 700 2 and 700 3 from the two filters ⇑I and ⇑J, these two sets of types are intersected to form a final set of solutions 700 4 , which is {SI, SJ}.
FIG. 7F shows the fragment 702 following the next act of processing. The method for filtering may be followed by the method for selecting a minimal solution from the final set of solutions. The act of selecting a minimal solution includes forming a type that has a less than or equal to relationship to the final set of solutions 700 4 . This act is illustrated in the Figure by (⇑I∩⇑J) l . This type is the set 700 5 , which is {I, J}. Since this type does not exist, the embodiments of the present invention create this type and insert it in the proper location 710 in the type hierarchy 702 .
FIG. 8 is a process diagram of a method according to one aspect of the present invention. A process 800 is a method for filtering to enhance type reconstruction. The process 800 uses upwardly closed sets. An equivalent process would use downwardly closed sets. The process 800 includes an act 802 for forming a first set of types. Each type in the first set of types has a less than or equal to relationship with respect to an unknown type. The act for forming 802 is iterated for each unknown type in a collection of constraints.
The process 800 includes an act 804 for forming a filter for a type in the first set of types. The filter forms a second set of types. The type in the first set of types has a less than or equal to relationship with respect to each type in the second set of types. The act of forming 804 is iterated for each type in the first set of types. Because the act of forming 804 is iterated for each type in the first set of types, a plurality of second sets of types may be generated.
The process 800 includes an act 806 for intersecting each set of type with other second sets of types to form a set of solutions to unknown types. The process 800 includes an act for caching the set of solutions so as to enhance incremental computation of subsequent sets of solutions. The act of caching is optionally executed.
In one embodiment, the process 800 can be described mathematically as (∩ τε D α ⇑τ). This term is from the solution formula which is μ(α)=(∩ τε D α ⇑τ) l . μ denotes a unique least solution to a collection of constraints C as collected by the operator I[M] as discussed above. α is the unknown type collected in the collection of constraints C. In order to solve for the unknown type α, the process first computes the set of types below α in the collection of constraints C. This computation produces the set D α . The process then computes the filters generated from each element in the set D α and intersects them. The unknown type α is then solved by mapping α to the set of types in a type hierarchy H, which are below every type in the intersection of filters.
The portion of the solution formula relies on types that are present in the set of constraints, avoiding a potential exponential blow up in the computation of the solutions. The duration of analysis for the solution formula is polynomial. Additionally, at least one embodiment of the present invention avoid forming ideals or sets of types by simply representing these sets with the generator type. Thus, this technique further enhances the computation of the solutions for the type reconstruction.
FIG. 9 is a process diagram of a method according to one aspect of the present invention. A process 900 is a method for constructing types. The method includes an act 902 for selecting a minimal solution as a desired solution from a set of solutions. The set of solutions is obtained from filtering at least one constraint so as to determine an unknown type for an intermediate program of a bytecode program. The desired solution is the minimal solution when the desired solution has a less than or equal to relationship with respect to any other solutions in the set of solutions. The unknown type includes an array type.
In one embodiment, the act 902 for selecting a minimal solution can be described mathematically as follows. If A is a subset of a type hierarchy H and x ε A, then x is called a minimal element of A if and only if y=x for any element y ε A with y≦x. Thus, for any given set of types, a minimal type of the given set of types is one that has a less than or equal to relationship with respect to any other solutions in the set of solutions. The operator Min can be applied to a subset of the type hierarchy H. Thus, Min A denotes a set of minimal elements of A. The result of the mathematics shows that if a type hierarchy has a known type and that known type is a minimal solution to the collection of constraints, the embodiments of the present invention will choose the known type instead of creating a new type to solve the collection of constraints.
The process 900 includes an act 904 for mapping the desired solution to a type in a known type in a type hierarchy of the bytecode program if the minimal solution is a set of one solution. The process 900 includes an act 906 for forming a desired type for the desired solution in a type hierarchy if the minimal solution is a set of more than one solution.
FIG. 10 is a process diagram of a method according to one aspect of the present invention. A process 1000 is a method for collecting constraints for array types. Certain programming languages, such as Java, allow subtyping for array types. This means that not only is there a subtyping relationship between types but the subtyping relationship is extended to the array of such types. Thus, additional constraints should be added.
The process 1000 includes an act 1002 for collecting a constraint between two unknown array types. Each unknown array type includes at least one element. The constraint between the two unknown array types includes a less than or equal to relationship. The process 1000 includes an act 1004 for adding another constraint for the unknown element types of the two unknown array types. This additional constraint among the unknown element types includes a less than or equal to relationship. The act of adding 1004 can be iterated if the unknown element type is a potential array type. A potential array type is defined to be at least one of an explicit array type and an unknown type that is related to a potential array type.
The process 1000 includes disregarding the unknown element types if the two unknown array types are not an array type.
FIG. 11 is a process diagram of a method according to one aspect of the present invention. A process 1100 is a method for eliminating cycles for type reconstruction. The process 1100 includes an act 1102 for computing a strongly connected component from a set of constraints so as to eliminate at least one cycle in the set of constraints. The strongly connected component includes a plurality of nodes. The strongly connected component includes a plurality of unknown types.
The process 1100 includes an act 1104 for examining an acyclic directed hypergraph by collapsing each node in the strongly connected component. Each unknown type in the strongly connected component is equal to the others. Each unknown type in the strongly connected component is adapted to receive the same solution in a set of solutions for the type reconstruction.
The process 1100 includes an act 1106 for forming a graph from the set of constraints for which the at least one cycle has been eliminated. This graph is called the SCC graph.
FIG. 12 is a structure diagram of a data structure according to one aspect of the present invention. A data structure 1200 is a structure for storing constraints and acting upon the constraints to form a solution to type reconstruction. The data structure 1200 includes a data member constraint 1202 to represent a constraint for a portion of a program. The data structure 1200 also includes a method member filtering 1208 for filtering at least one data member constraint 1202 to obtain a set of solutions so as to enhance type reconstruction.
The data member constraint 1202 includes a data member type 1204 to represent at least one of an unknown type and a known type. The data member constraint 1202 further includes a data member relationship 1206 to represent at least one of an equality relationship and an inequality relationship with another data member type 1204 of another data member constraint 1202 .
The data structure 1200 includes a method member selecting for selecting a minimal solution as a desired solution from the set of solutions to a set of data member constraints 1202 .
CONCLUSION
Methods have been described to enhance type reconstruction for programs. Such enhancement allows tools such as decompilers, interpreters, optimizers, debuggers, and garbage collectors to make superior assumptions about programs under analysis using the reconstructed types. One result from such enhancement includes software products that may run faster, contain fewer bugs, or both because the embodiments of the present invention extend the advantages of strong typing characteristics to the intermediate form of a source program. The reconstructed types are substantially similar to the original type system of the programming language of the source program, such as Java. Thus, the reconstructed types are easy for a user to read, verify, and comprehend.
The embodiments of the present invention focus on a class of bytecode programs called verifiable bytecode programs. Verifiable bytecode programs are programs of great interest since they are safe to run on computers. The type reconstruction techniques discussed hereinbefore provide substantially the extra types needed for enhancing the verification process of bytecode programs.
Although the specific embodiments have been illustrated and described herein, it will be appreciated by those of ordinary skill in the art that any arrangement which is calculated to achieve the same purpose may be substituted for the specific embodiments shown. This application is intended to cover any adaptations or variations of the present invention. It is to be understood that the above description is intended to be illustrative, and not restrictive. Combinations of the above embodiments and other embodiments will be apparent to those of skill in the art upon reviewing the above description. The scope of the invention includes any other applications in which the above structures and fabrication methods are used. Accordingly, the scope of the invention should only be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled.
|
Systems, methods, and structures are discussed that enhance type reconstruction for programs. Whereas previous methods insufficiently provide the set of types necessary for program analysis, the embodiments of the present invention can accept any verifiable bytecode programs and produce a set of types needed for program analysis. The embodiments of the present invention provide a technique called subtype completion that transforms a subtyping system by extending its type hierarchy to a lattice. However, such transformation inserts only a minimal amount of elements so as to enhance the computation of reconstructed types.
| 6
|
CROSS-REFERENCES TO RELATED APPLICATIONS
The present application is a U.S. National Phase of PCT Patent Application No. PCT/CN06/000216 filed Feb. 13, 2006 and claims priority to Chinese Patent Application 200510069576.4 filed on May 17, 2005, each of which is incorporated herein by reference in its entirety for all purposes.
TECHNICAL FIELD
The present invention provides a oligonucleotide with a sequence as shown in SEQ ID NO:1, or its functional homologue, a composition comprising the same and a method for treating B-cell neoplasm using the oligonucleotide by inducing apoptosis of B cell neoplastic cells, up-regulating CD40 on B cell neoplastic cells and by stimulating B cell neoplastic cells to produce IL-10. The oligonucleotide or its functional homologue can be used alone or in combination with chemotherapeutics, immunotherapeutics and radiation to treat B cell neoplasm.
BACKGROUND
Based WHO classification system (American Journal of Surgical Pathology, 1997, 21(1): 114-121), lymphoid malignancies are grouped into three major classes: B-cell neoplasm, T-cell/natural killer (NK)-cell neoplasm and Hodgkin's lymphomas.
The B-cell neoplasm is further divided into two groups: precursor B-cell neoplasm and peripheral B-cell neoplasm. Precursor B-cell neoplasm includes precursor B-acute lymphoblastic leukemia (B cell-acute lymphoblastic leukemia, B-ALL)/lymphoblastic lymphoma (LBL). Peripheral B-cell neoplasm includes B-cell chronic lymphocytic leukemia (B-CLL), small lymphocytic lymphoma, B-cell prolymphocytic leukemia, lympho plasmacytic lymphoma/immunocytoma, Mantle cell lymphoma, Follicular lymphoma, cutaneous follicular lymphoma, extranodal marginal zone B-cell lymphoma of MALT type, nodal marginal zone B-cell lymphoma (+/−monocytoid B-cells), splenic marginal zone lymphoma (+/−villous lymphocytes), hairy cell leukemia, plasmacytoma/plasma cell myeloma, diffuse large B-cell lymphoma, mediastinal (thymic) large B cell lymphoma, intravascular large B-cell lymphoma, primary effusion lymphoma and Burkift's lymphoma.
B-cell chronic lymphocytic leukemia (B-CLL) and B cell-acute lymphoblastic/lymphocytic leukemia (B-ALL) are two types of B cell leukemia. The B-CLL cells express CD19, CD5 and CD23 (Nicholas Chiorazzi, M.D., et al. N Engl. J Med 2005; 352:804-15). The B-ALL cells express CD19+CD10+ markers.
Small lymphocytic lymphoma is a B cell neoplasm. The monoclonal population of B cells in small lymphocytic lymphoma expresses CD19, CD5 and CD23 (Catherine Thieblemont, et al. Blood. 2004; 103:2727-2737).
Depending on the B-cell neoplasm diagnosed, current treatment options are chemotherapy, radiotherapy and immunotherapy.
CD40, expressed on the cell surface of normal B lymphocytes and dentritic cells, is a member of tumor necrosis factor receptor (TNFR) family. CD40L (CD154), expressed on T lymohocytes, is a member of tumor necrosis factor family (Castle B E, et al. J Immunol 1993; 151: 1777-1788). Interaction of CD40L and CD40 promotes the proliferation, differentiation and antigen presentation of B lymphocytes, dendritic cells and monocytes (Ranheim E A, et al. J Exp Med 1993; 177: 925-935; Yellin M J, et al. J Immunol 1994; 153: 666-674; Banchereau J, et al. Anhu Rev Immunol 1994; 12: 881-922; M. von Bergwelt-Baildon M S, et al. Blood 2002; 99: 3319-3325).
CD40 also expresses on the B cell neoplastic cells. It has been demonstrated that enhancing the CD40 expression promotes the apoptosis of B cell neoplastic cells (Peter Chu, et al. PNAS, March 19, 2002, vol. 99, no: 6 3854-3859; Frank Dicker, et al. BLOOD, 15 Apr. 2005 Volume 105, Number 8: 3193-3198).
Both in vitro and in vivo experiments indicated that stimulation and up-regulation of CD40 induced growth inhibition of B-cell neoplastic cells (Funakoshi et al., Blood 83: 2787-2794,1994; Murphy et al., Blood 86: 1946-1953,1995; Eliopoulos, A. G., et al. 1996. Oncogene 13:2243; Hirano, A., et al. 1999. Blood 93:2999; Tong, A. W., M et al. 2001.Clin. Cancer Res. 7:691).
Promoting CD40 expression on B cell neoplastic cells was reported to enhance the antigenicity of B cell neoplastic cells and consequently fostered the generation of cytotoxic T lymphocyte (CTL) specific to the cells. The CTL can efficiently kill B cell neoplastic cells (Dilloo D, et al. Blood. 1997; 90:1927-1933; Kato K, et al. J Clin Invest. 1998; 101:1133-1141; Wierda W G, et al. Blood. 2000; 96:2917-2924; Takahashi S, et al. Hum Gene Ther. 2001; 12:659-670; Takahashi S, et al. Cancer Gene Ther. 2001; 8:378-387). In the presence of CD40L, CD40 expressing B cell chronic lymphocytic leukemia cells can be killed by CD4 cytotoxic T lymphocytes (Frank Dicker, et al. Blood, 15 Apr. 2005 Vol 105, Num 8: 3193-3198). Interaction of D40L and CD40 on cells of Burkett's lymphoma could promote the cell to present tumor antigens to specific CTLs (Khanna, R. et al. 1997. J. Immunol. 159:5782). In vivo experiments and clinical trials also demonstrated that activation of CD40 could enhance the immunogenicity of B cell chronic lymphocytic leukemia (B-CLL) cell and consequently induce the generation of CTLs specific to the cells (Kato, K., et al. 1998. J. Clin. Invest. 101:1133; Wierda, W. G., et al. 2000. Blood 96: 2917).
Together, these data indicate that enhancing CD40 expression on B cell neoplastic cells can stimulate the anti-tumor immunity against B cell neoplasm. The anti-tumor immunity includes but not limits to the following:
1. promoting the apoptosis of B cell neoplastic cells; 2. inhibiting the growth of B cell neoplastic cells; 3. enhancing the immunogenicity of B cell neoplastic cells and therefore fostering the generation of CTLs specific to the cells.
Interleukin-10 (IL-10) is a homodimer cytokine produced by certain T cells, monocytes, macrophages and some of neoplastic cells developed from B cells, T cells or NK cells (Kitabayashi et al., 1995; Masood et al., 1995; Sjoberg et al., 1996; Beatty et al., 1997; Boulland et al., 1998; Jones et al., 1999). IL-10 activity is mediated by its specific cell surface receptor. The receptor expresses on antigen-presenting cells, lymphocytes and also B-cell chronic lymphocytic leukemia (B-CLL) cells. It was found that addition of exogenous IL-10 inhibited the proliferation of B-CLL cells freshly isolated from patients (Jesper Jurlander, Chun-Fai Lai, Jimmy Tan, et al. Characterization of interleukin-10 receptor expression on B-cell chronic lymphocytic leukemia cells. Blood, Vol 89, No 11 (June 1), 1997: pp 4146-4152). IL-10 was also reported to inhibit the proliferation of B-CLL cells and enhance the apoptosis of B-CLL cells (Anne-Catherine Fluckiger, Isabelle Durand, and Jacques Banchereau. Interleukin 10 Induces Apoptotic Cell Death of B-Chronic Lymphocytic Leukemia Cells. J. Exp. Med. Volume 179 January 1994 91-99). Immunostimulating anticancer properties of IL-10 have been discussed in a review from which it is speculated that IL-10 over-expression within the tumor microenvironment may catalyze cancer immune rejection (Simone Mocellin, Francesco M. Marincola and Howard A. Young. Interleukin-10 and the immune response against cancer: a counterpoint. Journal of Leukocyte Biology. 2005; 78:1043-1051).
In the present invention, we provide an oligonucleotide and a method for treating B cell neoplasm by using the oligonucleotide of the present invention. The oligonucleotide induces the apoptosis of B cell neoplastic cells, promotes CD40 expression on B cell neoplastic cells and stimulates the B cell neoplastic cells to produce IL-10, which all contributes to the treatment of a B cell neoplasm.
SUMMARY OF THE INVENTION
In the first embodiment, the present invention provides a oligonucleotide with a sequence of 5′-TCGTCGACGTCGTTCGTTCTC-3′ (designed as Oligo-2 or indicated SEQ ID NO:1), or its functional homologue. The Oligonucleotide or its functional homologue can have a phosphate backbone modification that is a phosphorothioate or phosphorodithioate modification partial or complete. The oligonucleotide or its functional homologue may have chemical modifications or have substitutions with rare bases. The oligonucleotide or its functional homologue can be a functional part of any other oligonucleotide or DNA fragment or be cloned into a plasmid, bacterial vector, viral vector or DNA vaccine respectively. The oligonucleotide with the sequence of SEQ ID NO:1 can be modified by adding one or more bases (preferable 1 to 10 based) to its each end or by changing bases in it. Those skilled in the art can determine to use the oligonucleotide with the sequence of SEQ ID NO:1 or its functional homologue, or the DNA fragment, single stranded or double stranded, comprising one or more copies of the oligonucleotide with the sequence (SEQ ID NO:1) to achieve the object of the present invention based on the well-knowledge in the art and the teaching of the present invention.
In the second embodiment, the present invention provides a method for treatment of B cell neoplasm using the oligonucleotide or its functional homologue of the present invention or the composition comprising the same in a subject. The subject is a human or animal. The B cell neoplasm includes but not limited to B cell leukemia, B cell lymphoma and myeloma.
In the third embodiment, the present invention provides a method for treating B cell neoplasm using the oligonucleotide or its functional homologue of the present invention or the composition comprising the same by inducing the apoptosis of B cell neoplastic cells.
In the fourth embodiment, the present invention provides a method for treating B cell neoplasm using the oligonucleotide or its functional homologue of the present invention or the composition comprising the same by up-regulating CD40 on B-cell neoplastic cells.
In the fifth embodiment, the present invention provides a method for treating B cell neoplasm using the oligonucleotide or its functional homologue of the present invention or the composition comprising the same by stimulating B-cell neoplastic cells to produce IL-10.
In another embodiment, the present invention provides a composition comprising therapeutically effective amount of the oligonucleotide or its functional homologue of present invention alone or in/with one more pharmaceutically acceptable carriers. The composition can be administered through enteral, parenteral and topical administration or by inhalation.
In yet another embodiment, the present invention provides a method for the treatment of B cell neoplasm, comprising administering a therapeutically effective amount of the oligonucleotide or its functional homologue of the present invention or the composition comprising the same and at least one of anti-B cell neoplasm agents including chemotherapeutics, immunotherapeutics and the agents used in radiotherapy.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 . Apoptosis of B-CLL Cells Induced by Oligo-2 (Dosage)
B-CLL cells were cultured in 10% human AB serum medium with or without various amount of Oligo-2. On day 7, the cells were stained with TMRE. The viable B-CLL cell number was calculated for TMRE-positiVe cell percentage.
FIG. 2 . The Effect of Oligo-2 on the Up-Regulation of CD40 on B-CLL Cells
The B-CLL cells were incubated with or without Oligo 2 for 7 days and then stained with FITC-CD40 antibody for analysis of CD40 expression using flow cytometry. The expression level was indicated with MFI number.
FIG. 3 . The Effect of Oligo-2 on the Up-Regulation of CD40 on Small Lymphocytic Lymphoma Cells
The small lymphocytic lymphoma cells were incubated with or without Oligo 2. On day 7, the cells were stained with FITC-CD40 antibody for analysis of CD40 expression using flow cytometry. The expression level was indicated with MFI number.
FIG. 4 . Apoptosis of B-ALL Cells Induced by Oligo-2
B-ALL cells were incubated with or without Oligo-2. On day 3, 5 and 7 of the incubation, the cells were stained with TMRE, followed by flow cytometry analysis. The viable B-ALL cell number was calculated for TMRE-positive cell percentage.
FIG. 5 . Up-Regulation of CD40 on B-ALL Cells by Oligo 2
B-ALL cells were cultured with or without 1 μg/ml Oligo-2. On day 3, 5 and 7 of the culture, the cells were stained with FITC-labeled anti-CD40 mAb for analysis of CD40 expression using flow cytometry. The expression level was indicated with MFI number.
FIG. 6 . Interleukin-10 Production from B-CLL Cells Induced by Oligo-2
The B-CLL cells were cultured with or without Oligo-2 in a serum-free medium. The supernatants were collected at the indicated time point and assessed for IL-10 using an ELISA kit.
FIG. 7 . The Effect of Oligo-2 on the Proliferation of Human Normal PBMC
The normal human PBMCs were cultured with Oligo-2, 2216 or 2006 for 36 h and then incorporated with [ 3 H] thymidine for determining the proliferation of the cells, respectively. The five blood samples were analyzed. The proliferation of cells was expressed as SI.
DETAILED DESCRIPTION OF THE INVENTION
Definitions
In this invention, the following terms shall have the meanings below:
An “oligonucleotide” means multiple nucleotides (i.e. molecules comprising a sugar (e.g. deoxyribose) linked to a phosphate group and to an exchangeable organic base). There are four organic bases cytosine (C), thymine (T), adenine (A) and guanine (G). The oligonucleotide can be synthesized by an automated oligonucleotide synthesizer available in the market or be prepared from existing nucleic acid sequences using known techniques.
A “back bone modification” of oligonucleotide shall mean that an oligonucleotide has a phosphorothioate modified phosphate backbone (i.e. at least one of the oxygens of the phosphate is replaced by sulfur) or other modified backbone. A “chemical modification” of oligonucleotide shall mean the modification by utilizing the active groups of the nucleotide or creating nucleotide analogues. The modifications can occur either during or after synthesis of the oligonucleotide. During the synthesis, modified bases (including but not limited to Thymidine analogues) can be incorporated internally or on the 5′ end. After the synthesis, the modification can be carried out using the active groups (via an amino modifier, via the 3′ or 5′ hydroxyl groups, or via the phosphate group).
A “B cell neoplasm” shall mean diseases developed from the abnormal proliferation of the cells of B lymphocyte lineage. The B cell neoplasm can be grouped into B cell leukemia, B cell lymphoma and myeloma (plasmacytoma/plasma cell myeloma). B cell leukemia includes B-cell chronic lymphocytic leukemia (B-CLL), precursor B-acute lymphoblastic leukemia (B cell acute lymphocytic leukemia, B-ALL), B-cell prolymphocytic leukemia and hairy cell leukemia. B cell lymphoma includes small lymphocytic lymphoma, lympho plasmacytic lymphoma/immunocytoma, Mantle cell lymphoma, Follicular lymphoma, cutaneous follicular lymphoma, extranodal marginal zone B-cell lymphoma of MALT type, nodal marginal zone B-cell lymphoma (+/−monocytoid B-cells), splenic marginal zone lymphoma (+/−villous lymphocytes), diffuse large B-cell lymphoma, mediastinal (thymic) large B cell lymphoma, intravascular large B-cell lymphoma, primary effusion lymphoma and Burkitt's lymphoma. A “subject” shall mean a mammal including but not limited to human, monkey, dog, cat, horse, cow, pig, goat, sheep, mouse and rat. The oligonucleotide of the invention can be administered to a subject with B cell neoplasm.
An “anti-B cell neoplasm agent” shall mean an agent used to treat B cell neoplasm in a subject. The agent includes the oligonucleotide of this invention, chemotherapeutics, immunotherapeutics and the agents used in radiotherapy. The oligonucleotide of the invention can be administered prior to, along with or after administration of one or more other anti-B cell neoplasm agents to achieve synergistic effect in treating a B cell neoplasm.
The “chemotherapeutics” shall mean the chemotherapeutics that treat B cell neoplasm in combination with the oligonucleotide of the invention. The oligonucleotide of this invention can be used with one or more chemotherapeutics in the treatment of B cell neoplasm. The chemotherapeutics include, but not limited to alkylating agents such as cyclophosphamide or chlorambucil, vinca alkaloids (e.g., vincristine and vinblastine), procarbazine, methotrexate, prednisone, anthracycline, L-asparaginase, purine analogs (e.g., fludarabine monophosphate, 2-chlorodeoxyadenosine and pentostatin), cytosine, arabinoside, cisplatin, etoposide and ifosfamide. The oligonucleotide of this invention can also be used with one or more chemotherapeutic combinations in the chemotherapy. The combinations include, but not limited to CVP (cyclophosphamide, vincristine and prednisone), CHOP (CVP and doxorubicin), C-MOPP (cyclophosphamide, vincristine, prednisone and procarbazine), CAP-BOP (CHOP plus procarbazine and bleomycin), m-BACOD (CHOP plus methotrexate, bleomycin and leucovorin), ProMACE-MOPP (prednisone, methotrexate, doxorubicin, cyclophosphamide, etoposide and leucovorin plus standard MOPP), ProMACE-CytaBOM (prednisone, doxorubicin, cyclophosphamide, etoposide, cytarabine, bleomycin, vincristine, methotrexate and leucovorin), MACOP-B (methotrexate, doxorubicin, cyclophosphamide, vincristine, fixed dose prednisone, bleomycin and leucovorin), IMVP-16 (ifosfamide, methotrexate and etoposide), MIME (methyl-gag, ifosfamide, methotrexate and etoposide), DHAP (dexamethasone, high dose cytarabine and cisplatin), ESHAP (etoposide, methylpredisolone, HD cytarabine, cisplatin), CEPP(B) (cyclophosphamide, etoposide, procarbazine, prednisone and bleomycin), CAMP (lomustine, mitoxantrone, cytarabine and prednisone), CHOP plus bleomycin, methotrexate, procarbazine, nitrogen mustard, cytosine arabinoside and etoposide. MOPP (mechlethamine (nitrogen mustard), vincristine (Oncovin), procarbazine and prednisone), ABVD (e.g., adriamycin, bleomycin, vinblastine and dacarbazine), ChIVPP (chlorambucil, vinblastine, procarbazine and prednisone), CABS (lomustine, doxorubicin, bleomycin and streptozotocin), MOPP plus ABVD, MOPP plus ABV (doxorubicin, bleomycin and vinblastine) or BCVPP (carmustine, cyclophosphamide, vinblastine, procarbazine and prednisone) and CAP (cyclophosphamide, doxorubicin and prednisone).
The “immunotherapeutics” shall mean the immunotherapeutics that treat B cell neoplasm in combination with the oligonucleotide of the invention. The oligonucleotide of this invention can be used with one or more immunotherapeutics in the treatment of B cell neoplasm. The immunotherapeutics include, but not limited to anti-CD20 antibodies. The CD20 antibody includes immunoglobulins and its fragments that are specifically reactive with a CD20 protein on cell surface of B cell neoplastic cells. CD20 antibodies can be polyclonal and monoclonal antibodies, chimeric antibodies, bi-specific antibodies and humanized antibodies. A “CD20” is a B-cell membrane protein (Tedder et al., Immunology Today 15: 450-454 (1994)) and is expressed on both normal and neoplastic B-cell (John C. Byrd, et al. J Clin Oncol 2001; 19: 2165-2170; Huhn D, et al. Blood 2001, 98: 1326-1331).
A “pharmaceutically acceptable carrier” denotes one or more solid or liquid filler, diluents or encapsulating substances that are suitable for administering the oligonucleotide of the invention to a subject. The carrier can be organic, inorganic, natural or synthetic. The carrier includes any and all solutions, diluents, solvents, dispersion media, liposome, emulsions, coatings, antibacterial and anti-fungal agents, isotonic and absorption delaying agents, and any other carrier suitable for administering the oligonucleotide of the invention and their use is well known in the art.
The “therapeutically effective amount” of the oligonucleotide of the invention shall refer to a dose used to achieve a desired result of treating B cell neoplasm in a subject. The dose can be determined by standard techniques well known to those skilled in the art and can vary depending the factors including, but not limited to the size or/and overall health of the subject or the severity of the disease. Introduction of the oligonucleotide of the invention can be carried out as a single treatment or over a series of treatments. Subject doses of the oligonucleotide of the invention for the administration range from about 1 μg to 100 mg per administration. However, doses for the treatment of B cell neoplasm may be used in a range of 10 to 1,000 times higher than the doses described above. The dosage regimen can be adjusted to provide the optimum therapeutic effect by those skilled in the art.
The “route” of administering the oligonucleotide of the invention shall mean the enteral, parenteral and topical administration or inhalation. The term “enteral” as used herein includes oral, gastric, intestinal and rectal administration. The term “parenteral” includes intravenous, intraperitoneal, intramuscular, subcutaneous, rectal or vaginal administration. The term “topical” denotes the application of the oligonucleotide externally to the epidermis, to the buccal cavity and into the ear, eye and nose.
A “pharmaceutical composition” shall mean the composition comprising an therapeutically effective amount of the oligonucleotide of the invention with or without a pharmaceutically acceptable carrier. The composition includes but not limited to aqueous or saline solutions, particles, aerosols, pellets, granules, powders, tablets, coated tablets, (micro)capsules, suppositories, syrups, emulsions, suspensions, creams, drops and other pharmaceutical compositions suitable for use in a variety of drug delivery systems. The compositions are suitable for injection, oral, buccal, rectal and vaginal use, inhalation and application in depot. In all cases, the composition must be sterile and stable under the conditions of manufacture and storage and preserved against the microbial contamination. For injection, the composition will include aqueous solutions or dispersions and powders for the extemporaneous preparation of injectable solutions or dispersion. “Powder” in this invention refers to a composition that contains finely dispersed solid particles containing the oligonucleotide of the invention. The powder may be formulated with other pharmaceutically accepted carriers (e.g., water, PBS, saline and other pharmaceutically accepted buffers) before use. The solutions can be prepared by incorporating the oligonucleotide in one or more appropriate solvents and other required ingredients. Dispersions can be prepared by incorporating the oligonucleotide into a vehicle, which contains a dispersion medium (e.g., glycerol, liquid polyethylene glycols and oils) and the other required ingredients. For oral administration, the composition will be formulated with edible carriers to form tablets, pills, dragees, capsules, liquids, gels, syrups, slurries, suspensions and the like. For buccal administration, the composition will be tablets or lozenges in conventional manner. For inhalation, the composition will be an aerosol spray from pressurized packs or a nebulizer or a dry powder and can be selected by one of skill in the art. The oligonucleotide may also be formulated as pharmaceutical acceptable compositions for rectal or vaginal applications and for depot application. The oligonucleotide of the invention in the composition can be used alone or in combination with one or more other agents including not limited to chemotherapeutics, immunotherapeutics and a ligand recognized by a specific receptor or molecule of target cell. The oligonucleotide of the invention in combination with another agent can be separate compositions and used as the following: (1) the oligonucleotide is mixed with a second agent before administration; (2) the oligonucleotide and a second agent are administered to a subject at different times; (3) the oligonucleotide and a second agent are administered to different sites of a subject. In addition, the composition may contain plasmid, bacterial vectors, viral vectors and nucleic acid vaccines carrying the sequence of the oligonucleotide of the invention.
EXAMPLES
The following examples are illustrative, and should not be viewed as limiting the scope of the present invention. Reasonable variations, such as those occur to reasonable artisan, can be made herein without departing from the scope of the present invention.
Example 1
Synthesis of the Oligonucleotide
A oligonucleotide with a sequence of 5′-TCGTCGACGTCGTTCGTTCTC-3′ (designed as Oligo-2, SEQ ID NO:1) has been designed and synthesized. To analyze the functions of the Oligo-2, two control oligonucleotides of 2006 with the sequence of 5′-tcgtcgttttgtcgttttgtcgtt-3′ (SEQ ID NO:2) and 2216 with the sequence of 5′-gggggacgatcgtcgggggg-3′ (SEQ ID NO:3) were also synthesized. Three of the oligonucleotide were synthesized in Sangon Biotech Company (Shanghai, China), tested for endotoxin by using the Limulus amebocyte lysate assay (Associates of Cape Cod, Inc) and manipulated in pyrogen-free reagents. 2006 ( J Immunol 2000: 164: 1617) is a well studied oligonucleotide that strongly activates normal B cells. 2216 (Eur J Immunol 2001; 31:2154) is another well studied oligonucleotide that induces high amounts of type I interferon in plasmacytoid dendritic cells.
The methods for synthesizing the oligonucleotide are well known for those skilled in the art and among others, solid-phase synthesis-is generally used. Specifically, in the process of the synthesis, the solid support used is controlled pore glass (CPG) bead. This bead has a surface with holes and channels and it is in these that the protected nucleotide is attached. The oligonucleotide synthesis begins with the 3′-most nucleotide and proceeds through a series of cycles composed of five steps that are repeated until the 5′-most nucleotide is attached. These steps are deprotection, activation, coupling, capping and stabilization.
Step 1. Deprotection
The protective group in the protected nucleoside attached to a CPG (controlled pore glass) bead is removed by trichloroacetic acid (TCA) leaving a reactive 5′-hydroxyl group.
Step2. Activation
In this step, tetrazole attacks the coupling phosphoramidite nucleoside forming a tetrazolyl phosphoramidite intermediate.
Step 3. Coupling
The tetrazolyl phosphoramidite intermediate reacts with the hydroxyl group of the recipient and the 5′ to 3′ linkage is formed. The tetrazole is reconstituted and the process continues.
Step 4. Capping
In this step, an acetylating reagent composed of acetic anhydride and N-methyl imidazole is used to block a reactive hydroxyl group on its 5′-most end of the oligonucleotides to avoid of coupling failure.
Step 5.Stabilization
Once the capping step is accomplished, the last step in the cycle is oxidation step, which stabilizes the phosphate linkage between the growing oligonucleotide chain and the most recently added base. This step is carried out in the presence of Iodine as a mild oxidant in tetrahydrofuran (THF) and water.
Following this final step the cycle is repeated for each nucleotide in the sequence. After the completion of the synthesis, the single stranded DNA molecule is purified by methods such as HAP, PAGE, HPLC, C18 and OPC.
Example 2
Apoptosis of Human B-CLL Cells Induced by Oligo-2
1. Preparation of Human B-CLL Cells
Blood samples from untreated B-CLL (pathologically identified) patients (The First Hospital, Jilin University, China) were drawn after obtaining written informed consent approved. Peripheral blood mononuclear cells (PBMCs) were isolated by Ficoll-Paque (Pharmacia) density gradient centrifugation. CD5+CD19+CD23+B-CLL cells in PBMCs were purified using B-cell isolation kit (Miltenyi Biotec, Bergisch Gladbach, Germany) to >95% of CD5+CD19+CD23+cells (B-CLL cells). The cell preparation was performed under the guidance of Miltenyi Biotec.
2. Apoptosis of Human B-CLL Cells Induced by Oligo-2
The B-CLL cells were incubated with Oligo 2 or 2006 or 2216 at a final concentration of 3 μg/ml in 10% human AB serum RPMI 1640 medium (HyClone) at 10 6 cells/well in a 48-well plate. The Oligo 2, 2006 or 2216 were diluted in serum free RPMI 1640 medium (HyClone). An equal volume of the dilute (serum free RPMI 1640 medium (HyClone)) was used as a control (Medium).
On day 3, 5 and 7 after incubation, the cells were counted and stained with tetramethyl-rhodamine ethylester (TMRE) (Molecular Probes Inc) (Lena Thyrell, et al. The Journal of Biological Chemistry Vol. 279, No. 23, Issue of June 4, pp. 24152-24162, 2004) for 10 minutes. The TMRE positive (viable) and TMRE-negative (apoptotic) B-CLL cells were determined by flow cytometry (B.D. FACS Aria). Viable B-CLL cell number was calculated by multiplying total cell count with the TMRE-positive cell percentage at each time point. The experiment was repeated with ten blood samples from B-CLL patients and the averaged result (n=10) showed that Oligo-2 significantly induced the apoptosis of B-CLL cells (Table-1) and the effect induced by Oligo-2 is approximately 2 fold stronger than that induced by 2006. In addition, the dose effect of Oligo-2 and 2006 on the apoptosis of the B-CLL cells was also observed. The result showed that that Oligo-2 at various dosages ranging from 0.1-10 μg/ml obviously induced the apoptosis of B-CLL cells ( FIG. 1 ). Comparatively, at the dosage of 1 μg/ml, the apoptosis inducing effect of Oligo-2 is approximately 3-fold stronger than that of 2006. Together, these results demonstrate that Oligo-2 can be used to treat B-CLL by inducing the apoptosis of B-CLL cells.
TABLE 1
Apoptosis of B-CLL cells induced by Oligo-2 (Kinetics)
Viable B-CLL cells (%) (n = 10)
Time of Incubation (day)
Group
3
5
7
Medium
82.2 ± 12.2
79.5 ± 9.25
81.3 ± 11.0
2216
67.7 ± 18.2
57.7 ± 16.7
50.7 ± 13.5
2006
66.5 ± 12.1
44.4 ± 15.0
40.2 ± 10.8
Oligo 2
45.5 ± 9.5
17.6 ± 5.6
14.2 ± 3.1
Example 3
Up-Regulation of CD40 on Human B-CLL Cells by Oligo-2
1. Preparation of Human B-CLL Cells
Human B-CLL cells were isolated from B-CLL patients with the procedures as described as in example 2.
2. Up-Regulation of CD40 on Human B-CLL Cells by Oligo-2
The B-CLL cells were incubated with Oligo 2 or 2006 or 2216 at a final concentration of 3 μg/ml in 10% human AB serum RPMI 1640 medium (HyClone) at 10 6 cells/well in a 48-well plate. The Oligo 2, 2006 or 2216 were diluted in serum free RPMI 1640 medium (HyClone). An equal volume of the dilute (serum free RPMI 1640 medium (HyClone)) was used as a control (Medium).
On 7 day after the incubation, the cells were counted and stained with FITC-CD40 antibody (Becton ickinson) (Molecular Probes Inc) (Lena Thyrell, et al. The Journal of Biological Chemistry Vol. 279, No. 23, Issue of June 4, pp. 24152-24162, 2004) for 10 minutes. The CD40 antibody stained B-CLL cells were determined by flow cytometry (B.D. FACS Aria). The result ( FIG. 2 ) showed that Oligo 2 significantly up-regulate the expression of CD40 on B-CLL cells, indicating that Oligo-2 can be used to treat B-CLL by up-regulating CD 40 on the cells. The up-regulation of CD 40 promotes the apoptosis of B-CLL cells, induces the growth inhibition of B-CLL cells and renders the B-CLL cells more immunogenic to stimulate the generation of CTLs specific to B-CLL cells. The experiment was repeated with at least ten blood samples from B-CLL patients with similar results.
Example 4
The Apoptosis of Human Small Lymphocytic Lymphoma Cells Induced by Oligo 2
1. Preparation of Human Small Lymphocytic Lymphoma Cells
The small lymphocytic lymphoma cells were isolated from the biopsy tissue of lymph node from patients (The First Hospital, Jilin University, China) with small lymphocytic lymphoma (pathologically identified) after obtaining written informed consent approved. The biopsy tissue was minced by rough surface glass slides to release the cells into 5 ml of 10% human AB serum RPMI 1640 media (HyClone) in a 6 cm culture plate. The released cells were filtered through stainless steel mesh and collected into a 50 ml conical tube containing 15 ml serum free RPMI 1640 medium (HyClone). The tube was centrifuged at 300×g for 10 minutes and then the supernatant was discarded. CD5+CD19+CD23+small lymphocytic lymphoma cells were purified using B-cell isolation kit (Miltenyi Biotec, Bergisch Gladbach, Germany) to >95% of CD5+CD19+CD23+cells (small lymphocytic lymphoma cells). The cell preparation was performed under the guidance of Miltenyi Biotec.
2. Apoptosis of Small Lymphocytic Lymphoma Cells Induced by Oligo-2
The small lymphocytic lymphoma cells were incubated with Oligo 2 or 2006 or 2216 at a final concentration of 3 μg/ml in 10% human AB serum RPMI 1640 medium (HyClone) at 10 6 cells/well in a 48-well plate. The Oligo 2, 2006 or 2216 were diluted in serum free RPMI 1640 medium (HyClone). An equal volume of the dilute (serum free RPMI 1640 medium (HyClone)) was used as a control (Medium).
On day 3, 5 and 7 after the incubation, the cells were counted and stained with tetramethyl-rhodamine ethylester (TMRE) (Molecular Probes Inc)(Lena Thyrell, et al. THE JOURNAL OF BIOLOGICAL CHEMISTRY Vol. 279, No. 23, Issue of June 4, pp. 24152-24162, 2004) for 10 minutes. The TMRE positive (viable) and TMRE-negative (apoptotic) small lymphocytic lymphoma cells were determined by flow cytometry (B.D. FACS Aria). Viable small lymphocytic lymphoma cell number was calculated by multiplying total cell count with the TMRE-positive cell percentage at each time point. The experiment was repeated with five samples from the patients with small lymphocytic lymphoma and the averaged result (n=5) showed that Oligo-2 significantly induces the apoptosis of the small lymphocytic lymphoma cells (Table-2), indicating that Oligo-2 can be used to treat small lymphocytic lymphoma by inducing the apoptosis of small lymphocytic lymphoma cells.
TABLE 2
Apoptosis of small lymphocytic lymphoma cells induced by Oligo-2.
Viable small lymphocytic lymphoma cells (%) n = 5
Time of Incubation (day)
Group
3
5
7
Medium
81.2 ± 7.7
78.4 ± 9.1
77.1 ± 13.2
2216
68.5 ± 15.0
58.7 ± 12.3
52.1 ± 10.2
2006
67.6 ± 10.3
45.3 ± 8.9
41.1 ± 8.2
Oligo 2
60.3 ± 12.2
23.2 ± 5.6
15.5 ± 6.2
Example 5
Up-Regulation of CD40 of Small Lymphocytic Lymphoma Cells Induced by Oligo 2
1. Preparation of Human Small Lymphocytic Lymphoma Cells
Human small lymphocytic lymphoma cells were isolated from patients with the procedures as described in example 4.
2. Up-Regulation of CD40 of Small Lymphocytic Lymphoma Cells Induced by Oligo-2
The small lymphocytic lymphoma cells were incubated with Oligo 2 or 2006 or 2216 at a final concentration of 3 μg/ml in 10% human AB serum RPMI 1640 medium (HyClone) at 10 6 cells/well in a 48-well plate. The Oligo 2, 2006 or 2216 were diluted in serum free RPMI 1640 medium (HyClone). An equal volume of the dilute (serum free RPMI 1640 medium (HyClone)) was used as a control (Medium).
On day 7 after the incubation, the cells were counted and stained with FITC-CD40 antibody (Becton ickinson) (Molecular Probes Inc) (Lena Thyrell, et al. The Journal of Biological Chemistry Vol. 279, No. 23, Issue of June 4, pp. 24152-24162, 2004) for 10 minutes. The CD40 antibody stained small lymphocytic lymphoma cells were determined by flow cytometry (B.D. FACS Aria). The result ( FIG. 3 ) showed that Oligo 2 significantly up-regulates the expression of CD40 on small lymphocytic lymphoma cells, indicating that Oligo-2 can be used to treat small lymphocytic lymphoma by up-regulating CD 40 on the cells. The up-regulation of the CD40 promotes the apoptosis of small lymphocytic lymphoma cells, induces the growth inhibition of small lymphocytic lymphoma cells and renders the small lymphocytic lymphoma cells more immunogenic to stimulate the generation of CTLs specific to the cells. The experiment was repeated with five samples with similar results.
Example 6
Apoptosis of Human B Cell-Acute Lymphoblastic/Lymphocytic Leukemia (B-ALL) Cells Induced by Oligo-2
1. Preparation of Human B-ALL Cells
Blood samples from untreated B-ALL (pathologically identified) patients (The First Hospital, Jlin University, China) were drawn after obtaining written informed consent approved. PBMCs were isolated by Ficoll-Paque (Pharmacia) density gradient centrifugation. CD19+CD10+B-ALL cells in PBMCs were purified using B-cell isolation kit (Miltenyi Biotec, Bergisch Gladbach, Germany) to >95% of CD19+CD10+cells (B-ALL cells). The cell preparation was performed under the guidance of Miltenyi Biotec.
2. Apoptosis of B-ALL Cells Induced by Oligo-2
The B-ALL cells were incubated with Oligo 2 or 2216 at a final concentration of 3 μg/ml in 10% human AB serum RPMI 1640 medium (HyClone) a at 10 6 cells/well in a 48-well plate. The Oligo 2 or 2216 was diluted in serum free RPMI 1640 medium (HyClone). An equal volume of the dilute (serum free RPMI 1640 medium (HyClone)) was used as a control (Medium).
On day 3, 5 and 7 after the incubation, the cells were counted and stained with tetramethyl-rhodamine ethylester (TMRE) (Molecular Probes Inc) (Lena Thyrell, et al. The Journal of Biological Chemistry Vol. 279, No. 23, Issue of June 4, pp. 24152-24162, 2004) for 10 minutes. The TMRE positive (viable) and TMRE-negative (apoptotic) B-ALL cells were determined by flow cytometry (B.D. FACS Aria). Viable B-ALL cell number was calculated by multiplying total cell count with the TMRE-positive cell percentage at each time point. The result showed that Oligo-2 significantly induced the apoptosis of B-ALL cells ( FIG. 4 ), demonstrating that Oligo-2 can be used to treat B-ALL by inducing the apoptosis of B-ALL cells. The experiment was performed with ten blood samples from B-ALL patients with similar results.
Example 7
The Up-Regulation of Cb40 on B-ALL Cells by Oligo-2
1. Preparation of Human B-ALL Cells
Human B-ALL cells were prepared from the blood samples of patients with the procedures as described in example 6.
The B-ALL cells were incubated with Oligo 2 or 2216 at a final concentration of 3 μg/ml in 10% human AB serum RPMI 1640 medium (HyClone) a at 10 6 cells/well in a 48-well plate. The Oligo 2 or 2216 was diluted in serum free RPMI 1640 medium (HyClone). An equal volume of the dilute (serum free RPMI 1640 medium (HyClone)) was used as a control (Medium).
On day 3, 5, 7 after the incubation, the cells were counted and stained with FITC-CD40 antibody (Becton ickinson) (Molecular Probes Inc)(Lena Thyrell, et al. The Journal of Biological Chemistry Vol. 279, No. 23, Issue of June 4, pp. 24152-24162, 2004) for 10 minutes. The CD40 antibody stained B-ALL cells were determined by flow cytometry (B.D. FACS Aria). The result ( FIG. 5 ) showed that Oligo 2 significantly up-regulate the expression of CD40 on B-ALL cells, indicating that Oligo-2 can be used to treat B-ALL by up-regulating CD 40 on the cells. The up-regulation of the CD40 promotes the apoptosis of B-ALL cells, induces the growth inhibition of B-ALL cells and renders the B-ALL cells more immunogenic to stimulate the generation of CTLs specific to B-ALL cells. The experiment was repeated with ten samples from the B-ALL patients with similar results.
Example 8
The Production of IL-10 from B-CLL Induced by Oligo 2
1. Preparation of Human B-CLL Cells
Human B-CLL cells were isolated from B-CLL patients with the procedures as described as in example 2.
2. The Production of IL-10 from B-CLL Induced by Oligo 2
The B-CLL cells were culture with Oligo 2 at a final concentration of 3 μg/ml in serum-free RPMI 1640 medium (HyClone) a at 10 6 cells/well in a 48-well plate in triplicates. The Oligo 2 was diluted in serum free RPMI 1640 medium (HyClone). An equal volume of the dilute (serum free RPMI 1640 medium (HyClone)) was used as a control (Medium). The culture supernatants were collected at 72 h or the indicated time points and assessed for IL-10 in Fluorokine MAP Immunoarray (R&D Systems) system. Our data showed that triggering with Oligo-2 led to the production of a high level of IL-10 from B-CLL cells ( FIG. 6 ). A profound increase of IL-10 production was detected at 6 h, peaked at 24 h, and remained high levels over the 72 h culture. In addition, our data further showed that adding exogenous rh-IL-10 (Schering Corp) into B-CLL cell cultures induced apoptotic B-CLL cells in an IL-10 dose-dependent manner, which could be specifically blocked by anti-IL-10 antibody (R & D Systems). These findings demonstrate that Oligo-2 can be used to treat B-CLL by inducing the production of IL-10 that which provokes the apoptosis of B-CLL cells in an autocrine manner. The experiment was repeated by using at least ten samples of B-CLL patient.
Example 9
The Effect of Oligo-2 on the Proliferation of Human Normal PBMC
Human PBMCs were isolated from buffy coats of normal blood donors (The Blood Center of Jilin Province, China) by Ficoll-Hypaque density gradient centrifugation (Pharmacia). The viability of the PBMCs was 95-99% as determined by trypan blue exclusion.
The PBMCs (6×10 5 /well) were plated in 96-well U-bottomed plates (Costar) and cultured with or without the Oligo-2 (6 μg/ml) in triplicates for 36 h, followed by pulsing With [ 3 H] thymidine (New England Nuclear, Boston, Mass.) for 16 h. The cells were harvested on glass fiber filters and detected in a scintillation counter. The cell proliferation was expressed as SI (stimulation index) (from triplet wells). Data from five normal blood samples are shown. 2006 and 2216 were used in controls. The results showed that Oligo-2 could stimulate the PBMCs to proliferate obviously ( FIG. 7 ), indicating that the Oligo-2, instead of inducing the apoptosis, is proliferation-stimulatory to normal human PBMCs and isn't toxic to the cultured cells.
Having described the invention in detail and by reference to the preferred embodiments it will be apparent to those skilled in the art that modifications and variations are possible without departing from the scope of the invention as defined in the following appended claims.
|
The invention provides an oligonucleotide with a sequence of SEQ ID NO: 1 or its functional homolgue, a composition comprising the same and a method for treating B cell neoplasm by using the oligonucleotide or its functional homologue or the composition comprising the oligonucleotide. The oligonulceotide induces the apoptosis of B cell neoplastic cells, up-regulates CD40 on B cell neoplastic cells and stimulates the production of IL-10 from B cell neoplastic cells.
| 2
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a rotating wheel assembly for slot machines, and more particularly to a rotating wheel assembly having a number of modules to allow easy maintenance and replacement of the elements thereof.
2. Description of the Related Art
A slot machine is popular in the modern world and includes a number of wheel rotating assemblies. FIGS. 10 and 11 of the drawings illustrate a typical rotating wheel assembly for a slot machine. The rotating wheel assembly includes a base 9, a step motor 91, a rotating wheel 93 is secured on an output shaft of the step motor 91 to rotate therewith, a figure card 94 is adhered to an outer periphery of the rotating wheel 93, a photoelectric element 92 attached to the base 9, and a shield bar 95 attached to a supporting rib (not labeled) of the rotating wheel 93. When the rotating wheel 93 stops, the figure on the figure card displayed to the player is discriminated according to the position of the shield bar 95 relative to the photoelectric element 92. The rotating wheel 93 is so frequently turned that it often malfunctions. Yet, the elements that constitute the rotating wheel 93 are fixed and thus result in inconvenience to maintenance and replacement. A further disadvantage resides in that the elements of the rotating wheel 93 cannot be applied to slot machines with base frames of different shapes and sizes. The present invention is intended to provide an improved rotating wheel assembly that mitigates and/or obviates the above problems.
SUMMARY OF THE INVENTION
It is a primary object of the present invention to provide an improved rotating wheel assembly that includes a number of modules to allow easy maintenance and replacement. The rotating wheel assembly includes a base that is releasably attached to a frame of a slot machine. The rotating wheel assembly further includes a rotating wheel consisting of an outer ring and an inner ring that are releasably engaged together to allow adjustment in the width. Each of the inner ring and the outer ring includes a groove for holding a figure card. A lamp device is mounted inside the rotating wheel and secured to a cylinder, which, in turn, is releasably engaged with a circular member on the base to allow a change in the angular position. In addition, a shielding plate is releasably attached to a rim of the inner ring to allow adjustment of position of the shielding plate in response to wrong discrimination as a result of long-term use of the rotating wheel assembly.
Other objects, advantages, and novel features of the invention will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a rotating wheel assembly in accordance with the present invention;
FIG. 2 is an exploded perspective view of the rotating wheel assembly in accordance with the present invention;
FIG. 3 is a front view of the rotating wheel assembly and a frame of a slot machine;
FIG. 4 is an enlarged fragmentary side view illustrating disengagement of a base from the frame in FIG. 3;
FIG. 5 is a front view of the rotating wheel assembly;
FIG. 6 is a view similar to FIG. 5, wherein the lamp device is mounted on the other side of the rotating wheel;
FIG. 7 is an enlarged sectional view illustrating engagement between a motor and an outer ring of the rotating wheel;
FIG. 8 is a partial exploded perspective view illustrating engagement between the outer ring, an inner ring, and a figure card;
FIG. 9 is a partial sectional view illustrating positioning of the figure card;
FIG. 10 is a perspective view of a conventional rotating wheel assembly; and
FIG. 11 is a side view of the conventional rotating wheel assembly.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1 to 9 and initially to FIG. 2, a rotating wheel assembly for slot machines in accordance with the present invention generally includes a base 2, a circuit board 3 attached to the base 2, a motor 4 mounted on top of the base 2, and a rotating wheel 5 mounted to an output shaft 41 of the motor 4 to rotate therewith. A lamp device 62 is mounted in the rotating wheel 5 for illumination, which will be described later.
The base 2 includes two horizontal beams 21 projected therefrom. One of the beams 21 includes a hole 211 defined therein, while the other beam 21 includes a lug 212 extended from a lateral side thereof. Referring to FIGS. 2 and 3, an engaging block 71 and a sleeve block 72 are detachably screwed to a frame 7 of a slot machine. The sleeve block 72 includes a receptacle 721 for receiving the lug 212 of the beam 21 on the base 2. The engaging block 71 includes a top plate 711 having an insert 712 on an underside thereof so as to be received in the hole 211 of the beam 21 on the base 2. An operative member 714 extends from the cover plate 711 and includes an engaging hook 713 on an underside thereof for engaging with a lateral side of the beam 21 with the hole 211. Thus, the base 2 is secured to the frame 7 of the slot machine, best shown in FIG. 3. The base 2 is removable by means of disengaging the beams 21 from the engaging block 71 and the sleeve block 72 to allow easy replacement and maintenance. It can be achieved by means of simple operation of moving the operative member 714 away from the beam 21, as shown in FIG. 4.
The circuit board 3 mounted in the base 2 controls rotations of the motor 4, illumination of the lamp device 6, and discrimination of angular position of the rotating wheel 5. As can be seen from FIG. 3, the circuit board 3 includes a U-shaped photoelectric element 31 and a number of pins 30 for connection with a cable connector 33 through which a main circuit board (not shown) of the slot machine is electrically connected to the circuit board 3 by a power line and signal control lines 34. Thus, the circuit board 3 is separate from the power line and the signal control lines 34.
Referring to FIGS. 1, 2, and 5, mounted on top of the base 2 is a circular member 22 that includes a central hole 221, two diametrically disposed semi-circular engaging grooves 222 arranged around the central hole 221, and two diametrically disposed positioning grooves 223 arranged around the central hole 221. A cylinder 6 includes a flange 64 formed on an end face thereof. The flange 64 is fittingly received in the central hole 221 of the circular member 221. A lamp holder 61 is attached to an outer periphery of the cylinder 6, and the lamp device 62 is mounted in the lamp holder 61. Two hooks 65 are diametrically disposed on the end face of the cylinder 6 and located outside the flange 64 for slidably engaging with the engaging grooves 222. Thus, the cylinder 6 is adjustably mounted to the circular member 2 to allow adjustment of angular position of the lamp device 62 (see FIGS. 5 and 6). A tab 66 extends outwardly from the cylinder 6 and includes a hole 661. A screw 662 is extended through the hole 661 to engage with a washer 663 positioned in one of the positioning groove 223 to thereby secure the cylinder 6 in place. The angular position of the lamp device 6 is thus fixed, as shown in FIGS. 5 and 6.
Referring to FIG. 2, the cylinder 6 further includes two diametrically disposed mounting members 63 on the outer periphery thereof. The motor 4 is detachably screwed to the slots 631 in the mounting members 63, thereby securely fixing the motor 4 in the cylinder 6.
The rotating wheel 5 includes an outer ring 52 and an inner ring 51. The outer ring 52 includes a rim 57 supported by a number of radial ribs 56. An axle section 53 is formed in a center of the outer ring 52 for engaging with the output shaft 41 of the motor 4. Referring to FIGS. 2 and 7, the axle section 53 includes an engaging groove 54, and a bottom wall that defines the engaging groove 54 includes a hole 541. A U-shaped member 55 is received in the engaging groove 54 and includes a hole 551. The output shaft 41 of the motor 4 includes an annular groove 411 and a transverse key hole 412. When the outer ring 52 engages with the output shaft 41, the output shaft 41 extends through the hole 551 of the U-shaped member 55 and the hole 541 of the engaging groove 54. A C-clip 413 is mounted in the annular groove 411 of the output shaft 41, and a key 414 is inserted into the key hole 412 and bears against a mediate section of the U-shaped member 55 to thereby securely engage the outer ring 52 and the output shaft 41.
Referring to FIGS. 2 and 8, a number of female extension 571 extend outwardly from the rim 57 toward the inner ring 51 in a direction normal to a plane on which the rim 57 locates. Each female extension 571 includes an engaging groove 572, and a bottom wall that defines the engaging groove 572 includes a hole 573. The inner ring 51 includes a rim 58 from which a number of male extensions 581 extend in a direction normal to a plane on which the rim 58 locates. Each male extension 581 is engaged with the engaging groove 572 of an associated female extension 571. Each male extension 581 includes a number of holes 582. A stem 584 of a male pin 583 is extended from an upper side of the female extension 571 through one of the holes 582 of the male extension 581 and the hole 573 of the female extension 571. A female pin 585 is provided on an underside of the female extension 571 and includes a holed stem 586 for fitting receiving the stem 584 of the male pin 583. Thus, the overall width of the rotating wheel 5 constituted by the inner ring 51 and the outer ring 52 is adjustable by means of placing the stem 584 of the male pin 583 in different holes 582 of the male extension 581.
Referring to FIGS. 2, 8, and 9, the rim 57 of the outer ring 52 includes a retaining groove 574, while the rim 58 of the inner ring 51 includes a retaining groove 587. The rims 57 and 58 have an identical diameter, and the retaining grooves 574 and 587 together define a retaining groove for holding the figure card 59 that has a number of figures on a side thereof (FIG. 1).
An engaging piece 575 is formed in the retaining groove 574, while a retaining block 588 is formed in the retaining groove 587. The figure card 59 includes a notch 591 (FIG. 8) that engages with the engaging piece 575, while two ends of the figure card 59 wound in the retaining grooves 574 and 587 are overlapped and retained in place by the retaining block 588, best shown in FIG. 9.
Referring to FIG. 8, the rim 58 of the inner ring 51 further includes a reference groove 589 that faces away from the outer ring 52. The location of the reference groove 589 corresponds to a specific figure on the figure card 59. A U-shaped shielding plate 8 is adjustably attached to the rim 58 by means of engaging a hook device 81 of the shielding plate 8 with the reference groove 589 and the retaining groove 588. In use, the shielding plate 8 passes through the photoelectric element 31 such that the circuit board 3 may discriminate which figure is displayed to the player, which is conventional and therefore not described in detail. If the figures of on all rotating wheels of the slot machine are not properly aligned, position of the shielding plate 8 relative to the reference groove 589 is adjusted to solve this misalignment problem.
According to the above description, it is appreciated that the rotating wheel assembly in accordance with the present invention includes the following advantages:
1. The elements of the rotating wheel assembly are separated into several modules to allow easy maintenance and replacement. More specifically, the base 2 is detachably connected to the frame 7, the circuit board 3 is separate from the power line and the signal control lines 34 from the main circuit board of the slot machine, and the figure card 5 is detachably retained in the inner ring 51 and the outer ring 52.
2. The angular position of the lamp device 62 is adjustable and thus can be used in all kinds of slot machines. The overall width of the rotating wheel 5 is adjustable so as to be used with figure cards of different width. The shielding plate 8 is adjustable relative to the reference groove 589 to thereby allow adjustment of the figures on the figure card 59 to align with the lamp device 62.
Although the invention has been explained in relation to its preferred embodiment, it is to be understood that many other possible modifications and variations can be made without departing from the spirit and scope of the invention as hereinafter claimed.
|
A rotating wheel assembly includes a base that is releasably attached to a frame of a slot machine. The rotating wheel assembly further includes a rotating wheel consisting of an outer ring and an inner ring that are releasably engaged together to allow adjustment in the width. Each of the inner ring and the outer ring includes a retaining groove for holding a figure card. A lamp device is mounted inside the rotating wheel and secured to a cylinder, which, in turn, is releasably engaged with a circular member on the base to allow a change in the angular position. A shielding plate is releasably attached to a rim of the inner ring to allow adjustment of position of the shielding plate in response to wrong discrimination as a result of long-term use of the rotating wheel assembly.
| 6
|
FIELD OF THE INVENTION
The present invention is directed toward a door panel comprising two multi-component doorskin subassemblies and a method of assembling same, and more specifically, toward a door panel comprising a plurality of folded metal elements permanently interconnected to form first and second doorskins, which doorskins are attached to stile and rail members, and a method of assembling same.
BACKGROUND OF THE INVENTION
Traditional wooden doors are formed from two vertical, parallel members called stiles connected at their top and bottom ends by two horizontal members called rails. One or more central panels are then connected between the stiles and rails to form a door. In a newer method of forming a door a frame of stiles and rails is provided, and first and second doorskins are attached to the outer faces of the frame. This method requires less labor and provides a hollow door interior that can be filled with insulation. In order to give the appearance of a traditional door, the doorskins are often formed with a contoured inner section and a smooth periphery that resemble interconnected rails and stiles.
Light weight metal door panels such as those used for storm doors or screen doors are often formed from first and second metal doorskins mounted on opposite sides of parallel stiles. The stiles are generally wooden, and hinges can be attached to one stile (the hinge stile) and a handle and/or latch to the other stile (the latch or strike stile) to form a door panel. For typical doors of this type, the upper halves of the center portions of the doorskins may be cut out to receive a lite such as a windowpane or a screen. In other door panels, substantially all the center portions of the doorskins are removed to accommodate a larger lite. Formed in this manner, the doorskins have a smooth outer finish and do not provide the appearance of a door formed with rails and stiles.
U.S. Pat. No. 4,546,585 shows one attempt to form a metal door that appears to be formed of rails and stiles. In this patent, a wooden frame is provided, and a metal covering or cladding is attached to the wooden frame. The cladding is formed from a number of separate elements that are interconnected in a temporary manner and attached to the wooden frame. Foam insulation is then injected into the temporary assembly to permanently secure all the elements. While this reference provides a door with a satisfactory appearance, it is unnecessarily difficult to assemble, and its individual elements must be carefully aligned while they are being joined. Moreover, because the elements that form the doorskins are not held together in a permanent manner until the finished assembly is filled with foam insulation, the doorskins may fall apart if handled roughly or stored and manipulated extensively before they are used in a door panel.
It would therefore be desirable to provide a metal door panel having interconnected stile and rail elements that is easy to manufacture and that does not need to be filled with foam insulation in order to permanently secure all its elements.
SUMMARY OF THE INVENTION
These and other problems are overcome by the present invention which comprises a door panel having first and second stiles to which are mounted first and second doorskins formed from interconnected, preferably metal, elements. The elements that overlay the stiles each include a longitudinally extending flange along a first edge while the rail elements that connect the stile elements include grooves for receiving the stile element flanges. Advantageously, the flange-in-groove connection helps keep the elements aligned while they are being assembled and, when the connection is pierced by a sharp tool, also provides a very secure joint.
In a preferred embodiment, the stile elements each include a longitudinally extending L-shaped projection along a second edge parallel to the flange, the short leg of the “L” engaging the longitudinal slot in a stile to secure the doorskin to the stile. The longitudinal grooves of the rail elements are formed inwardly from the end edges of the rail elements so that an end portion of the rail element overlies a portion of the stile element when the stile flange is received in the rail element groove. The groove includes an inner leg disposed toward the middle of the rail element and an outer leg that is shorter than the inner leg by an amount equal to the thickness of the stile element. In this manner, when the stile element flange is received in the rail element groove, the face of the stile element opposite the flange and the face of the rail element opposite the groove will be substantially coplanar.
After the stile element flanges are received in the rail element grooves, the grooves are pierced by a sharp tool to drive a portion of the groove inner leg against and preferably through the flange and into the outer leg of the groove. This forms a permanent connection between the rail elements and stile elements. Because the rail and stile elements of the doorskins are permanently connected in this manner, the doorskins can be preassembled and stored indefinitely until they are needed for a door assembly and are structurally sound at this stage of manufacture, before they are incorporated into a door panel filled with insulating material, as was necessary to permanently bond the doorskin elements together in the prior art.
Once two doors skin have been formed, the short legs of the L-shaped projections on the stile elements are inserted into longitudinal slots on parallel stiles and secured thereto to form a door. Rails may also be added to connect the stiles, and a lite frame may be provided at the center part of the door to hold a window or screen. The door can also, optionally, be filled with foam insulation.
It is therefore a principal object of the present invention to provide a door panel comprising a doorskin formed from a plurality of interconnected elements.
It is another object of the present invention to provide a method of assembling a doorskin by permanently interconnecting a plurality of metal elements.
It is a further object of the present invention to provide a door panel comprising a doorskin formed from permanently interconnected stile elements and rail elements.
It is still another object of the present invention to provide a doorskin formed from stile elements having flanges and rail elements having grooves wherein the stile element flanges are received and retained within the rail element grooves.
It is still a further object of the invention to provide a doorskin formed from stile elements and rail element configured to be easily alignable during an assembly process.
In furtherance of these objects, a door assembly is provided that includes a hinge stile and a latch stile each having a longitudinal groove, and first and second doorskin assemblies each having a central opening connected to opposite sides of the hinge stile and the latch stile, wherein each of the doorskin assemblies is formed from first and second stile elements and first and second rail elements connected between the first and second stile elements. The first and second stile elements each have a first side including an integrally formed L-shaped projection and a second side including a flange having first and second ends, and the first and second rail elements each comprise a planar body portion and a first end having a first edge and a second end having a second edge and a first U-shaped projection defining a groove and extending from the first end near the first edge and a second U-shaped projection defining a groove and extending from the second end near the second edge. The first end of the first stile element flange is received in the first rail element first end groove and permanently secured thereto by piercing and the first end of the second stile element flange is received in the first rail element second end groove and permanently secured thereto by piercing, and the first U-shaped projection includes an inner leg having a first length and an outer leg having a second length less than the first length.
A method of forming a door assembly is also disclosed that includes the steps of providing a first stile element having a first side including an L-shaped projection and a second side including a flange having a first end and a second end; providing a top rail element having a planar central portion and first and second ends each having a narrow groove; inserting the first end of the first stile element flange first end into the first rail element first end narrow groove; piercing the first rail element groove to drive a portion of the wall defining the groove into the,first stile element flange first end in the groove; providing a bottom rail element having a planar central portion and first and second ends each having a narrow groove; inserting the second end of the first stile element into the bottom rail element first end narrow groove; piercing the bottom rail element groove to drive a portion of the wall defining the groove into the first stile element flange second end in the groove; providing a second stile element having a first side including an L-shaped projection and a second side including a flange having a first end and a second end; placing the first end of the second stile element flange in the top rail element second groove; placing the second end of the second stile element flange in the bottom rail element second groove; piercing the second rail element groove to drive a portion of the wall defining the groove into the second stile element first end flange in the groove; piercing the second stile element groove to drive a portion of the wall defining the groove into the second stile element flange second end in the groove; attaching a latch stile to the first stile element L-shaped projection; attaching a hinge stile to the second stile element L-shaped projection; and attaching a doorskin to the latch stile and the hinge stile.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects and advantages of the invention will be better understood upon a reading and understanding of the detailed description of the invention provided below together with the following drawings.
FIG. 1 is a front elevational view of a door assembly according to the present invention.
FIG. 2 is a perspective view of one of the stile elements of the door assembly of FIG. 1 .
FIG. 3 is a perspective view of one of the rail- elements of the door assembly of FIG. 1 .
FIG. 4 is a sectional plan view taken along line 4 — 4 in FIG. 1 .
FIG. 5 is a sectional plan view taken along line 5 — 5 in FIG. 1 .
FIG. 6 is a detail view of the junction between the stile element of FIG. 2 and the rail element of FIG. 3 .
FIG. 7 is a perspective view of a portion of the junction shown in FIG. 6 .
FIG. 8 is a sectional side elevation taken along line 8 — 8 in FIG. 1 .
FIG. 9 is a sectional side elevation taken along line 9 — 9 in FIG. 1 .
FIG. 10 is a plan view of an alternate embodiment of one end of a rail element for connection to the stile elements of the door assembly of the present invention.
FIG. 11 is a detail view of an alternate embodiment of the junction between the stile element of FIG. 2 and the rail element of FIG. 3 .
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings, wherein the showings are for the purpose of illustrating a preferred embodiment of the invention only, and not for the purpose of limiting same, FIGS. 1 and 4 show a door assembly 10 comprising a hinge stile 12 having a longitudinal slot 13 , a strike or latch stile 14 having a longitudinal slot 15 , a top rail 16 , a bottom rail 18 and a first metal doorskin 20 having a lite 22 . The stiles and rails are preferably made from a lightweight wood, but could be formed from other materials known in the art without departing from the scope of this invention. A second doorskin 24 having a lite 26 is shown in FIG. 5 . Doorskins 20 and 24 are mirror images of one another, but are otherwise identical, and only doorskin 20 will be described hereafter, it being understood that doorskin 24 is composed of identical parts.
Doorskin 20 includes a plurality of interconnected elements, preferably formed from a sheet of metal such as steel or aluminum, that are attached to stiles and rails to form a door panel. Specifically, a first stile element 30 overlies hinge stile 12 , a second stile element 32 overlies strike stile 14 , a first or top rail element 34 overlies top rail 16 , and a second or bottom rail element 36 overlies bottom rail 18 .
Stile element 30 is shown by itself in FIG. 2 and comprises a planar central section 38 , a first side 40 and a second side 42 , an L-shaped projection 44 extending from the edge of first side 40 and including a long leg 46 and a short leg 48 , and a flange 50 extending from second side 42 at a right angle to central section 38 . Stile element 30 also includes a first end 52 having a flange 53 and a second end 54 having a flange 57 . Second stile element 32 includes one or more openings 55 shown in FIG. 1 for accommodating locking and latching hardware in a well-known manner, but is otherwise substantially identical to first stile element 30 .
Rail element 34 is shown by itself in FIG. 3 and includes a planar central section 56 , a top edge 58 having a flange 59 , a bottom edge 60 having a bottom flange 61 , a first side 62 having an edge 64 and a second side 66 having an edge 68 . First and second U-shaped projections 70 extend substantially between top edge 58 and bottom edge 60 and comprise inner legs 72 facing planar central section 56 , outer legs 74 and a narrow slot 76 defined in part by these inner and outer legs. For reasons to be described in more detail hereinafter, the outer legs 74 are shorter than the inner legs 72 by an amount equal to the thickness of the material from which the rail and stile elements are formed. First side 62 of rail element 34 and second side 66 of rail element 34 are generally coplanar, while central section 56 lies in a different plane parallel to the plane of the first and second sides. The width of narrow groove 76 is approximately equal to the thickness of the sheet metal material, and second rail element 36 is substantially identical to first rail element 34 .
Doorskin 20 is assembled by arranging first stile element 30 and second stile element 32 in parallel on a support surface (not shown) with flanges 50 facing upward, facing each other, and spaced apart by the distance between narrow grooves 76 of first rail element 34 . First rail element 34 is then placed on the first ends of the stile elements so that flanges 50 of stile elements 30 and 32 are received into narrow grooves 76 of the first rail element and so that top edge 58 of the first rail element is generally aligned with first end 52 of stile element 30 . Second rail element 36 is placed on the other ends of the stile elements in a similar manner. Because the distance between the U-shaped projections is known, the proper spacing between the stile element flanges can readily be maintained, and the stile and rail elements can be kept in proper alignment while they are permanently secured. To secure the elements of doorskin 20 to one another, a tool is used to pierce the U-shaped projections to form dimples 78 therein which can be seen in FIGS. 6 and 7. The dimples 78 preferably extend through inner legs 72 and into flanges 50 and may also extend partially into outer legs 74 to form a secure connection between the stile elements and the rail elements. Dimples formed along the length of the U-shaped projection at intervals of about 0.75 inch provide adequate strength for the panel. Second doorskin assembly 24 is formed in the same manner. The dimples may alternately extend inwardly through both the inner and outer legs as shown in FIG. 11 .
Because the outer legs of the U-shaped projections are shorter than the inner legs by an amount equal to the thickness of the material used for the stile elements, the surfaces of the stile elements and rail elements opposite the projections will be generally coplanar and provide a smooth finished appearance for the door assembly. Moreover, sides 62 and 66 of first rail element 34 overlie a portion of the planar central portions of the stile elements to provide increased rigidity to the doorskin in the area of the above-described joints.
To form a door assembly from the doorskins, hinge stile 12 is attached to first stile element 30 by inserting short leg 48 of L-shaped projection 44 into the longitudinal slot 13 of hinge stile 12 ; strike stile 14 is attached to second stile element 32 in a similar manner as shown in FIG. 4 . Top and bottom rails 16 and 18 are then connected between the stiles with flanges 59 on the first and second rail elements helping to position the top and bottom rails as shown in FIGS. 8 and 9. A second doorskin 24 , formed in the same manner as the first doorskin, is attached to the opposite side of this partial assembly. A lite frame 80 having clips 82 shown in FIGS. 1 and 5 is next attached to the portions of flanges 50 extending between the first and second rail elements, and optionally, the entire assembly may be filled with a foam insulation 84 in a conventional manner.
FIG. 10 shows a modified rail element 34 ′ which may provide a more rigid door assembly and help prevent leakage of foam insulation injected between the doorskins when used in the door panel described above. Elements in this figure that correspond to elements of the first embodiment are identified by the same reference numerals in this figure but include primes. In this embodiment, a portion 63 of side 62 ′ of first rail element 34 ′ is bent toward the plane of central portion 38 ′ at an angle α of about two to four degrees. When rail element 34 ′ is attached to the stile elements as described above, portions 63 press firmly against the central portion of the stile element which helps to reduce flexing in the assembly.
The subject invention has been described herein in terms of preferred embodiments; various obvious modifications and additions to these embodiments will become apparent to those skilled in the relevant arts upon a reading and understanding of this disclosure. All such modifications and additions are considered a part of this invention to the extent that they fall within the scope of the several claims appended hereto.
|
A door panel is disclosed that includes first and second doorskins each formed from two metal stile elements including a longitudinal flange and two rail elements including a pair of U-shaped projections defining narrow grooves, wherein the rail elements are connected to the stile elements by placing the stile element flanges into the rail element grooves and, piercing the U-shaped projections to form a permanent mechanical bond between the stile and rail elements. A method of forming such a door panel is also disclosed.
| 4
|
TECHNICAL FIELD
[0001] The present invention relates to the installation structure of a rail frame for guiding a sliding movement of a roller apparatus of a sliding insect window screen which is capable of supporting a sliding insect window screen and providing a sliding opening/closing action of the sliding insect screen. More particularly, the present invention relates to the sliding insect window screen comprising the rail frame which can more stably support the sliding insect window screen on the top surface and on the bottom surface, so even if a strong wind blows against the sliding insect screen, it is possible for the sliding insect window screen to maintain a stable state without shaking movement.
[0002] Moreover, the present invention relates to the sliding insect window screen which is appropriate for being installed in front of a sliding window for constituting a special sliding window system. The special sliding window system has a glass panel which is directly and removably seated on and supported by rollers without a quadrilateral door sash that supports the glass panel forming the sliding window so as to minimize a phenomenon of reducing an open view through the sliding window. Also, the glass panel includes vertical stiffeners with an enlarged cross-section (cross-section having a thickness thicker than the glass panel) attached to the both side surfaces of the glass panel so as to reinforce transverse bending rigidity of the glass panel and to exhibit high wind pressure resistance. In this special sliding window system with the above-described structure, upper and lower pocket guides are respectively formed in upper and lower door guide frames used as a window frame member that guides a sliding movement of the sliding window so as to guide the upper end and lower end of the sliding window in both inner and outer surfaces of the sliding window, thereby supporting a smooth movement of the sliding window. In order to allow the sliding window provided with the vertical stiffeners to be integrally installed within a door guide frame, and to allow the sliding window to be separated from the door guide frame in a state where the sliding window is provided with the vertical stiffeners, a pocket guide is formed as pocket guide segments removable from a door guide frame body, and the pocket guide segments are successively installed to be separable from each other on both the inner and outer surfaces of the sliding window along the travel direction of the roller guide rail.
BACKGROUND ART
[0003] The present invention relates to an insect window screen for installation on the outside of the windows in order to prevent indoor entry of various insects, and particularly the insect window screen of the mesh type with being coupled between a lower screen chassis and an upper screen chassis and sliding along the rail provided on the insect window screen installation frame equipped in front of the sliding window installation frame.
[0004] In general, there are two types of insect window screen. The one type is a fixed insect window screen which is fixed to the window installation frame by using hinge and screws. The other type is a moving insect window screen which is sliding along the rail on the insect window screen installation frame which is additionally constructed in front of window installation frame 10 of a window frame being provided for the window 20 as shown in FIGS. 1 and 2 .
[0005] The present invention relates to a moving insect window screen among the above two types of the insect window screen, i.e. a sliding insect window screen or insect window screen in short. According to conventional configurations of the moving insect window screen, as shown by the accompanying drawings in FIG. 1 , the roller of the lower screen chassis constituting the insect window screen 40 is firmly mounted on the lower rail provided on insect window installation frame 30 in the window frame, but a holder of the upper screen chassis constituting the window screen 40 is no longer in close contact with an upper rail provided on the insect window installation frame 30 of the window frame as shown in FIG. 2 . Therefore, in a part of the upper rail, there is a problem such as noise generated in case of that the insect wind screen 40 is shaken by the wind.
[0006] In addition, for example, when a sliding insect window screen is additionally installed to a window system that is provided between the indoor living room the balcony, a special constructing structure of the sliding insect window screen is necessary for that the sliding insect window can be easily installed to the insect window installation frame and separated from the insect window installation frame according to the change of season. However, according to the prior art, in order to adapt the sliding insect window screen for easy installation and removal, there is a problem in that the insect window screen is jerking when it is sliding along the rail and is shaken by wind pressure because of large installation clearance.
[0007] In order to solve this problem, Korea Patent No. 10-0376971 B1 provided an additional guiding wing member made of soft and elastic synthetic resin to the holder of the upper chassis constituting the insect window screen. According to the additional guiding wing member, when sliding insect window screen is installed into the insect window installation frame of the window frame, the additional guiding wing member of the holder of the upper chassis is pushed into the upper rail of the insect window installation frame and therefore the additional guiding wing member is resiliently bended against the upper rail into a reinforcing rib. To the next, the roller of the upper chassis is placed on the lower rail of the insect window installation frame, and then the additional guiding wing member is resiliently recovered into the original form to firmly contact to the upper rail of the insect window installation frame. As a result of these upper and lower contact structure, shaking by wind pressure could be prevented.
[0008] However, the above-described structure including the resilient guiding wing member added to the holder of the upper chassis by the Korea Patent No. 10-0376971 B1 has a structural limitation with regard to the wind load proof because of its resilient properties and its short durability based upon soft material.
[0009] In addition, as described in the prior art with reference to the attached FIGS. 1 and 2 and the drawings of Korea Patent No. 10-0376971 B1, because that the upper rail and lower rail of the insect window installation frame is exposed, the chassis of the insect window screen may interferes with the visibility of the window. Accordingly, the value of the effort and cost required to remove the door chassis of the glass window for the wide visibility may be compromised by the chassis of the insect window screen.
DETAILED DESCRIPTION OF THE INVENTION
Technical Problem
[0010] The present invention has been made in order to solve the problems in the prior art and a technical object of the present invention is to provide a new sliding insect window installation structure being capable of improving constructing convenience as well as durability so as to ensure wind pressure proof.
[0011] In addition, the present invention is to provide a technical means for the insect window screen capable of being integrally installed within the insect window installation frame and being simply separated from the insect window installation frame, wherein this means is also capable of allowing that holder and/or roller of the insect window screen is firmly installed on the upper and/or lower rail without relying on resilient force of the additional elastic material.
[0012] Furthermore, this technical means for the insect window installation frame comprising the upper rail and lower rail is capable of minimizing the extent of outside exposure of the chassis of the insect window screen which may decrease the wide and good visibility through the glass window designed by removing the door chassis.
Technical Solution
[0013] In order to solve the above-described problems, the present invention provides an insect window installation structure including an insect window installation frame for an insect window screen to be integrally installed within the insect window installation frame and to be simply separated from the insect window installation frame, comprising;
[0014] an insect window installation frame body pocket which is installed adjacent to a door installation frame; and
[0015] a rail bridge being detachably installed into an inside of said insect window installation frame body pocket with including rail extended along the sliding direction of the insect window screen at the position with a pre-determined distance from the bottom surface or ceiling surface of said insect window installation frame body pocket, and
[0016] wherein said rail bridge is formed as two or more rail bridge segments which are separately and detachably installed into the inside of said insect window installation frame body pocket, and
[0017] wherein said rail bridge segments are successively installed and detachably connected under or above the sliding insect window screen along the advancing direction of said rail.
Advantageous Effects
[0018] According to the present invention, an insect window screen can be integrally installed within the insect window installation frame and the installed insect window screen also can be simply separated from the insect window installation frame. Moreover not only the lower chassis constituting the insect window screen but also upper chassis constituting the insect window screen can have a roller member which is more tightly installed into a narrow space so that very smooth sliding movement by the rollers can be achieved both of the upper and the lower rail on the insect window installation frame, and even if a strong wind blows against the sliding insect screen, it is possible for the sliding insect window screen to maintain a stable state without shaking movement.
[0019] Furthermore, an insect window installation structure according to the present invention, an effect of maximizing durability against the wind pressure with good airtight performance can be achieved.
[0020] In addition, the upper rail and lower rail of the insect window installation frame is less exposed, therefore the chassis of the insect window screen may not interferes with the visibility of the window.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] FIGS. 1 and 2 are cross-sectional views illustrating a conventional sliding insect window installation structure.
[0022] FIG. 3 is a longitudinal cross-section view of illustrating a sliding insect window installation structure according to the present invention.
[0023] FIG. 4 is a plan view of illustrating a sliding window installation structure shown in FIG. 3 .
[0024] FIGS. 5 to 7 are illustrating usefulness and applicability of a sliding window installation structure with regard to the sliding insect window installation structure according to the present invention.
[0025] FIGS. 8 to 10 are cross-sectional views illustrating the operating states of installation and removal of the sliding insect window screen by using the lower structure of the insect window installation structure according to the present invention.
[0026] FIGS. 11 to 13 are cross-sectional views illustrating the operating states of installation and removal of the sliding insect window screen by using the upper structure of the insect window installation structure according to the present invention.
[0027] FIGS. 14 to 19 are plan views illustrating the operating states of removal of the rail bridge and separation of the insect window screen in an embodiment comprising three rail bridge segments in the upper/lower structure.
[0028] FIG. 20 is a cross-sectional view illustrating the operating state of removal of pocket guide segment and sliding door from the door installation frame in the sliding window installation structure with regard to the insect window installation structure according to the present invention.
MODE FOR CARRYING OUT THE INVENTION
[0029] Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings such that a person ordinarily skilled in the art to which the present invention belongs may easily embody the present invention. However, the present invention may be implemented in various forms and is not limited to the embodiments described hereinafter.
[0030] As described previously, the present invention is intended to solve a problem for the improvement of the sliding insect window installation structure for the insect window screen not to be an obstacle in case of being used together with the special window system having the increased openness of the windows, and also is intended to solve a structural problem produced in case of the installation or separation of the sliding insect screen. Herein, FIG. 3 is a longitudinal cross-section view of illustrating a sliding insect window installation structure according to the present invention, FIG. 4 is a plan view of illustrating a sliding window installation structure shown in FIG. 3 , and FIGS. 5 to 7 are illustrating usefulness and applicability of a sliding window installation structure with regard to the sliding insect window installation structure according to the present invention.
[0031] In addition, FIGS. 8 to 10 are cross-sectional views illustrating the operating states of installation and removal of the sliding insect window screen in case of using the lower structure of the insect window installation structure according to the present invention, and FIGS. 11 to 13 are cross-sectional views illustrating the operating states of installation and removal of the sliding insect window screen in case of using the upper structure of the insect window installation structure according to the present invention.
[0032] Moreover, FIGS. 14 to 19 are plan views illustrating the operating states of removal of the rail bridge and separation of the insect window screen in an embodiment comprising three rail bridge segments in the upper or lower structure.
[0033] An embodiment of the present invention exemplified in the drawings provides an insect window installation frame 200 , for an insect window screen 500 to be integrally installed within the insect window installation frame 200 and to be simply separated from the insect window installation frame 200 , comprising;
[0034] an insect window installation frame body pocket 210 which is installed adjacent to a door installation frame 100 ; and
[0035] a rail bridge 220 being detachably installed into an inside of said insect window installation frame body pocket 210 with including rail 222 extended along the sliding direction of the insect window screen 500 at the position with a pre-determined distance from the bottom surface or ceiling surface of said insect window installation frame body pocket 210 .
[0036] Whereas, a locking projection 201 may be protruded outside of one side of said insect window installation frame body pocket 210 , and said locking projection 201 can be inserted and coupled into a fastening groove 101 formed on the concave outer side of the door installation frame 100 .
[0037] In addition, said rail bridge 220 is formed as two or more rail bridge segments 220 - 1 , 220 - 2 , 220 - 3 which are separately and detachably installed into the inside of said insect window installation frame body pocket 210 , and said rail bridge segments 220 - 1 , 220 - 2 , 220 - 3 are successively installed and detachably connected under or above the sliding insect window screen 500 along the advancing direction of said rail 222 .
[0038] Preferably, so that said rail bridge 220 having a segmented structure which are separately and detachably installed, i.e. two or more rail bridge segments 220 - 1 , 220 - 2 , 220 - 3 can be installed into the inside of said insect window installation frame body pocket 210 , as shown in FIGS. 3 to 7 , a fastening tab 214 is provided along the advancing direction of said rail 222 in the inner side of said insect window installation frame body pocket 210 , and a inserting projection 224 is provided along the advancing direction of said rail 222 on the inner/outer end of said rail bridge 220 so that said inserting projection 224 can be inserted into said fastening tab 214 . Therefore, based upon the friction generated between said inserting projection 224 and said fastening tab 214 , said rail bridge 220 could not be separated from said insect window installation frame body pocket 210 without applying the external force. However, it is preferred that said inserting projection 224 and said fastening tab 214 are formed so that said rail bridge 220 could be easily detached from said insect window installation frame body pocket 210 when a user grips and pulls said rail 222 extruded from an upper surface of the bridge rail 220 .
[0039] Further, said rail bridge segment 220 : 220 - 1 , 220 - 2 , or 220 - 3 being provided as a bridge rail 220 , can be provided into any one or more structure among the upper structure and the lower structure of said insect window installation frame 200 , and as illustrated in the accompanying drawings, the sliding insect window screen 500 have a diversity in the working direction of installation and removal (the sliding insect window screen 500 may be installed/removed in various directions) in case of being provided all of the upper structure and the lower structure of said insect window installation frame 200 .
[0040] Herein, when said rail bridge 220 are removed from one of the upper structure and the lower structure of said insect window installation frame 200 as illustrated in FIG. 3 , in order that the sliding insect window screen 500 can be easily separated from the inner surface of said insect window installation frame body pocket 210 of said insect window installation frame 200 , for example, if a distance (refer to b″ of FIG. 3 ) from the lower end of the sliding insect window screen 500 to the bottom surface of the lower structure of said insect window installation frame body pocket 210 is greater than a distance (refer to a′ of FIG. 3 ) from the upper end of the sliding insect window screen 500 to the lower end of the upper structure of said insect window installation frame body pocket 210 , said rail bridge 220 is detached from said insect window installation frame body pocket 210 provided in the lower structure of said insect window installation frame 200 (see FIG. 8 ), and then the sliding insect window screen 500 can be downwardly moved into the free space (see FIG. 9 ), and then, as the upper end of said insect window screen 500 can be rotated in the forward outside the lower end of said insect window installation frame body pocket 210 of the upper structure (see FIG. 10 ). Finally, if said insect window screen 500 is slant upwardly lifted in this state, said insect window screen 500 can be removed from said insect window installation frame body pocket 210 of the lower structure (see FIGS. 8 to 10 ).
[0041] On the contrary case, said rail bridge 220 is firstly detached from said insect window installation frame body pocket 210 provided in the upper structure of said insect window installation frame 200 (see FIG. 11 ), and then the sliding insect window screen 500 can be upwardly moved into the free space (see FIG. 12 ), and then, as the lower end of said insect window screen 500 can be rotated in the forward outside the upper end of said insect window installation frame body pocket 210 of the lower structure (see FIG. 13 ), and finally if said insect window screen 500 is slant downwardly moved in this state, said insect window screen 500 can be removed from said insect window installation frame body pocket 210 of the upper structure (see FIGS. 11 to 13 ). Meanwhile, in order that such removal can be easily achieved, a distance (refer to b′ of FIG. 3 ) from the upper end of the sliding insect window screen 500 to the upper end of the upper structure of said insect window installation frame body pocket 210 should be greater than a distance (refer to a″ of FIG. 3 ) from the lower end of the sliding insect window screen 500 to the upper end of the lower structure of said insect window installation frame body pocket 210 .
[0042] Thus, according to the insect window installation structure including the insect window installation frame having a segmented structure which is separately and detachably installed, as shown by the FIGS. 8 to 10 and FIGS. 11 to 13 , if said rail bridge segment 220 : 220 - 1 , 220 - 2 , or 220 - 3 being provided as the rail bridge 220 at any one of the upper structure and the lower structure of said insect window installation frame 200 is removed from the said insect window installation frame 200 , said insect window screen 500 also can be removed from said insect window installation frame body pocket 210 , and the insect window screen 500 assembled through the production line can be integrally installed into said insect window installation frame body pocket 210 . Furthermore, an insect window installation structure capable of maximizing durability against the wind pressure with good airtight performance can be achieved because that a chassis portion of the insect window screen 500 is substantially accommodated in said insect window installation frame 200 as shown in the figures.
[0043] In addition, in order to improve dust resistance, water-tightness, and air-tightness of the sliding insect window screen system having the above-described structure, as illustrated in FIG. 3 , blocking members 540 such as mohair may be installed in a horizontal longitudinal direction on the opposite surfaces of said rail bridge segment 220 : 220 - 1 , 220 - 2 , or 220 - 3 provided as the rail bridge 220 and said sliding insect window screen 500 .
[0044] Meanwhile, in the case of the sliding insect window screen systems according to the embodiments described above, descriptions will be made on the configuration which allows the rail bridge segments 220 : 220 - 1 , 220 - 2 , 220 - 3 provided as the rail bridge 220 to be easily separated from said insect window installation frame body pocket 210 of the insect window installation frame 200 without interference with said sliding insect window screen 500 (refer to FIGS. 8 and 11 ) and the operating procedure thereof.
[0045] Hereinafter, embodiments of the apparatus for this removal process will be described with reference to the accompanying drawings such that a person ordinarily skilled in the art to which the present invention belongs may easily embody the present invention.
[0046] First, as illustrated in FIG. 4 , said rail bridge segments 220 : 220 - 1 , 220 - 2 , 220 - 3 provided as the rail bridge 220 in the upper or lower structure of the sliding window screen 500 are divisionally formed as two or more segments over the entire length of the rail 222 ( FIG. 4 being an illustrative three segments), and one or more segments may be formed to have a length removable from said insect window installation frame body pocket 210 in a state where the sliding insect window screen 500 is installed to be seated on the rollers 520 on the rail 222 of the other segment on the rail bridge 220 .
[0047] Hereinafter, the operation of the present invention will be described with reference to FIGS. 14 to 19 , assuming that three rail bridge segments 220 - 1 , 220 - 2 , 220 - 3 are divisionally installed as the rail bridge 220 in the upper structure or the lower structure of the sliding insect window screen 500 along the entire length of the rail 222 , as an example.
[0048] First, when the sliding insect window screen 500 is in the closed state as illustrated in FIG. 14 , sliding insect window screen 500 is in the state where it cannot be easily removed from the insect window installation frame boy pocket 210 of the insect window installation frame 200 due to the interference between the rail bridge segments 220 - 2 , 220 - 3 (segments noted by (b) and (c) in FIG. 14 ) provided as the rail bridge 220 and the sliding insect window screen 500 . However, the rail bridge segments 220 - 3 (segments noted by (a) in FIG. 14 ) located at a position where the sliding insect window screen 500 is not positioned as illustrated in FIG. 15 may be removed from the insect window installation frame body pocket 210 of the insect window installation frame 200 . Then, when the rail bridge segments 220 - 2 is slid into the position of the removed the rail bridge segments 220 - 1 as illustrated in FIG. 16 , so that the rail bridge segments 220 - 2 also can be removed from the insect window installation frame body pocket 210 of the insect window installation frame 200 , as illustrated in FIG. 17 .
[0049] In the state illustrated in FIG. 18 in which two rail bridge segments 220 - 1 and 220 - 2 are removed from the insect window installation frame body pocket 210 of the insect window installation frame 200 , the sliding insect window screen 500 may be removed from the insect window installation frame body pocket 210 of the insect window installation frame 200 as described above with reference to FIGS. 8 to 10 and 11 to 13 . The state in which the sliding insect window screen 500 is removed is illustrated in FIG. 19 .
[0050] Meanwhile, the order performed from FIGS. 14 to 19 may be referred to as the steps of removing the sliding insect window screen 500 from the insect window installation frame body pocket 210 of the insect window installation frame 200 and on the contrary, the order performed from FIG. 19 to FIG. 14 may be referred to as the steps of installing the sliding insect window screen 500 into the insect window installation frame body pocket 210 of the insect window installation frame 200 .
[0051] The embodiment described above exemplifies a case in which three rail bridge segments 220 - 1 , 220 - 2 , 220 - 3 are divisionally installed as the rail bridge 220 along the entire length of the rail 222 in the upper or lower structure of the sliding insect window screen 500 . Unlike this, it can be seen that the present invention may be implemented by divisionally installing the rail bridge segments 220 - 1 , 220 - 2 having different lengths as the rail bridge 220 . That is, in this case, the rail bridge segment larger than the entire width of the sliding insect window screen 500 may be removed from the insect window installation frame 200 so that the sliding insect window screen 500 may be removed from the insect window installation frame 200 or installed into the insect window installation frame 200 without any difficulty.
[0052] In addition, according to the concept similar to the present invention, the pocket guide segments 130 : 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )} provided as the pocket guide 130 supporting sliding window 400 may be provided in an upper structure and/or a lower structure of the door guide frame 100 , and therefore the sliding window 400 can be removed or installed in the door guide frame 100 (refer to FIG. 20 ). The more detailed descriptions with regard to the entire constitution and operation for this invention, are described in the Korea Patent Application No. 102012-0047789 and the PCT application No. PCT/KR2013/003912 previously filed by inventor and applicant of the present invention, therefore the specification and drawings filed incorporated by reference.
[0053] The scope of the present invention to be protected is not limited thereto and may cover various types of insect windows to which the present invention is applied, and various modifications and changes using the basic concept of the present invention defined in the accompanying claims also belong to the scope of the present invention.
|
The present invention relates to the installation structure of a rail frame for guiding a sliding movement of a roller apparatus of a sliding insect window screen which is capable of supporting a sliding insect window screen and providing a sliding opening/closing action of the sliding insect screen. more particularly relates to the sliding insect window screen comprising the rail frame which can more stably support the sliding insect window screen on the top surface and on the bottom surface, so even if a strong wind blows against the sliding insect screen, it is possible for the sliding insect window screen to maintain a stable state without shaking movement.
| 4
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to a receiver, and particularly to a receiver provided with a circuit in which the change-over between transmitting and receiving states of an opposite station can be easily recognized.
2. Description of the Prior Art
In the case of performing intercommunication by a transmitter and receiver combination, when the transmitting state is changed-over to the receiving state, it is necessary to say, for example, "Go-ahead, please" for maintenance of good timing in the transition of the transmitting and receiving states between a principal station and its opposite station. However, it is troublesome to say Go-ahead, please every time the transmitting state is changed-over to the receiving state. Likewise, when an opposite station is calling a principal station, it is inconvenient to say, for example, "We are on the air, do you hear us?"
Accordingly, it would be desirable when the transmitting state is switched to the receiving state, that a specific change-over sound would be automatically transmitted thereby to inform the principal station that the opposite station has been changed-over from the transmitting state to the receiving state. However, the transmission of such a specific oscillating sound may be legally prohibited in a field of simple radio service, so that any means for instructing the change-over has not been provided in the prior art transmitter and receiver. Hence, an arrangement which produces a change-over sound dependent upon the presence of a signal carrier without the transmission of a change-over signal at the beginning or end of transmission would be highly useful.
SUMMARY OF THE INVENTION
An object of this invention is to provide an improved transceiver.
More specifically, an object of this invention is to provide a receiver which is capable of recognizing the termination or initiation of transmission without any change-over sound signal being transmitted from the opposite station or appropriate notification such as Go ahead, please or We are on the air, do you hear us.
A further object of this invention is to provide a receiver in which a change-over sound signal is produced in the receiving station every time when the opposite station begins or ends a transmission so that the change-over between transmitting and receiving states can be smoothly performed.
Another object of this invention is to provide a receiver with a simple, low-cost circuit construction for detecting the presence of an opposite station signal in accordance with the automatic gain control level and to introduce an appropriate change-over signal from the output of an oscillator into the receiving system of the principal station.
According to one embodiment of the invention, a received signal creates a receiver reverse AGC voltage which sets the operating level of an IF amplifier. The change from a high to a low IF amplifier operating level corresponding to the termination of a received signal is differentiated to create a peaked waveform of negative direction which decreases the current flow in a normally "ON" transistor commonemitter amplifier. The resulting rise in collector voltage permits an interconnected RC oscillator which is normally biased "OFF" to begin oscillating. The oscillator signal is introduced into the receiver audio chain and a brief tone is produced corresponding to the termination of the received signal from the opposite station. An additional advantage associated with the above embodiment is a relationship between the duration of the change-over sound tone and the strength of the received signal, the shorter sound durations corresponding to weaker signals and smaller AGC level shifts.
Other embodiments of the invention with a similar operating principal include a system for use with a positive AGC, a system for creation of a change-over signal at the initiation of a received signal for calling purposes, and an arrangement for simple incorporation into a transceiver of a system with a change-over signal for termination of a received signal.
The other objects, features and advantages of the present invention will be apparent from the following description taken in conjunction with the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a circuit diagram showing a receiver according to a first embodiment of this invention;
FIGS. 2A to 2E are views of waveforms appearing at the respective parts of the circuit shown in FIG. 1;
FIG. 3 is a circuit diagram showing a receiver according to a second embodiment of this invention;
FIGS. 4A to 4D are views of waveforms appearing at the respective parts of the circuit shown in FIG. 3;
FIG. 5 is a circuit diagram showing a receiver according to a third embodiment of this invention;
FIGS. 6A to 6D are views of waveforms appearing at the respective parts of the circuit shown in FIG. 5; and
FIG. 7 is a circuit diagram showing a receiver according to a fourth embodiment of this invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the following embodiments presented, only the receiving portion of a transmitter-receiver combination is described. The transmitter portion of the principal station and the transmitter portion at the opposite station can be constructed in the same manner as the prior art. It should be further obvious to one skilled in the art that the transmitters and receivers described herein could each be replaced with a transceiver.
A first embodiment of the invention is shown in FIG. 1. Reference numeral 1 designates a radio frequency or RF amplifier, 2 a frequency converter, 3 an intermediate frequency or IF amplifier, 4 a detecting diode, 5 a volume adjusting variable resistor, 6 an audio frequency or AF amplifier, and 7 a speaker. In this example, a signal for reverse automatic gain control (AGC) is applied to the IF amplifier 3. That is, a collector of an IF amplifying transistor 31 in the IF amplifier 3 is connected through a primary winding of an IF transformer 32 and a resistor 33 to a voltage source terminal 34 to which a positive voltage +Vcc is applied, and the junction between the primary winding of the transformer 32 and the resistor 33 is grounded through a bypass capacitor 35. With the above arrangement, the diode 4 has derived therefrom a detected output which is applied through a low-pass filter 36 to the base of the transistor 31 as a DC voltage for reverse AGC.
In a detector circuit 80 for detecting an opposite station change-over from its transmitting state to its receiving state, there is provided a grounded-emitter transistor 81, the base of which is connected through a parallel connection of a differentiating capacitor 83 and a resistor 84 and further through a function switch 82 to the connection point between the primary winding of the transformer 32 and the resistor 33, and the collector of which is grounded through an integrating capacitor 85. In addition, an RC oscillator circuit 90 is formed by a transistor 91 as an oscillator for producing a brief changeover sound signal when the transmitting state is switched to the receiving state in the opposite station. The collector of the transistor 81 is connected through a resistor 92 to the base of the transistor 91 and the collector of the transistor 91 is connected through a resistor 93 to a movable contact of the variable resistor 5. In this case, when no signal is present, the transistor 81 is biased in conduction while the transistor 91 is cut off.
With the above circuit arrangement, let it be assumed that the function switch 82 is closed and an RF carrier signal such as shown in FIG. 2A is transmitted from the opposite station. In this case, since the IF amplifier 3 is fed with the voltage for reverse AGC, an AGC level shift signal Sb of rectangular-shape as shown in FIG. 2B, which has high levels corresponding to the presence of a signal from the opposite station, is obtained at the connection point between the primary winding of the transformer 32 and the resistor 33. The signal Sb is differentiated by the capacitor 83, the resistor 84, and the input impedance of the transistor 81 to form a differentiated signal Sc as shown in FIG. 2C which is applied to the base of the transistor 81 to make it nonconductive during the fall period of the signal Sc. Then, since the collector of the transistor 81 is connected to the capacitor 85, a audio oscillator control signal Sd as shown in FIG. 2D is derived from this collector every time the opposite station terminates its transmission. Thus, the transistor 91 is applied with a biasing voltage during a time period where the signal Sd is high, the oscillator circuit 90 begins to oscillate during the above time period, and the oscillator signal is supplied through a resistor 93 to the AF amplifier 6 and speaker 7. Hence, when the opposite station changes its transmitting state to the receiving state, an oscillating sound is produced from the speaker 7 for a certain period.
It is obvious to those skilled in the art that the oscillator signal injection point shown in this and the other invention embodiments is not exclusive; the signal injection may be accomplished at other points in the receiver audio chain as may be convenient.
As described above, according to the present invention, when the opposite station changes its transmitting state to the receiving state, a change-over sound is produced from the speaker to inform the principal station of the above transition, and hence the change-over from the transmitting state to the receiving state can be smoothly performed. In addition, it is not necessary to say Go-ahead, please every time the above change-over operation is performed.
In the case when a received signal from the opposite station is high in level and hence the signal Sb is high in level, the signal Sd is also high. In this case, a collector-emitter voltage of the transistor 91 changes in level from the cut-off region CO through the active region AC to the saturation region SA and finally returns back through the active region AC to the cut-off region CO as shown in FIG. 2E. The oscillator circuit 90 oscillates only when the transistor 91 has its collector-emitter voltage kept in the active region AC, so that when the level of the received signal is high, the change-over sound is reproduced twice in succession. Meanwhile, when the level of the received signal is lower than the former, the level of the signal Sd is also low. Accordingly, the collector-emitter voltage level of the transistor 91 remains longer in the active region AC without reaching the saturation region SA as shown in FIG. 2E by a dotted line, and hence a long change-over sound is produced. When the level of the received signal is even lower, the collector-emitter voltage of the transistor 91 keeps its level in the active region AC for a shorter period as shown in FIG. 2E by a chain line and hence a short pause sound is produced. Hence, when the received signal is high in level, the change-over sound is produced twice in succession, but as the received signal becomes lower, the change-over sound becomes continuous and shorter. As a result, the variation of the change-over sound indicates the approximate distance between the principal station and the opposite station.
The duration of the change-over sound can be changed by varying the value of the resistors 84, 92 and capacitors 83, 85. For example, in the case when the capacitor 85 is not used, since the transistor 81 is rendered conductive or nonconductive according to the signal Sc, the signal Sd becomes rectangular in waveform and hence during a period where the signal Sd is high, the transistor 91 is fed with a constant biasing voltage to make the oscillations of the oscillator circuit 90 constant. As a result, the change-over sound becomes constant during the presence of the received signal.
FIG. 3 shows a second embodiment of the transceiver according to this invention in which the IF amplifier 3 is applied with a voltage for forward AGC. In FIG. 3, elements corresponding to those of FIG. 1 are indicated by the same reference numerals with their repeated description being omitted. Additional components in this example are a resistor 94 which is connected between the resistor 93 and the variable resistor 5, and a diode 86 which is connected between the junction of the resistors 93 and 94 and the collector of the transistor 81. In addition, the transistor 81 is biased to cut off, while the transistor 91 is biased in conduction thereby causing the oscillator circuit 90 to be always oscillating.
With the above circuit arrangement, when an RF carrier signal as shown in FIG. 4A is transmitted from an opposite station, since the IF amplifier 3 is supplied with the voltage for forward AGC, a signal Sb' shown in FIG. 4B, which is low during a period when the signal is being transmitted, is obtained at the junction between the primary winding of the transformer 32 and the resistor 33. The signal Sb' is differentiated by the capacitor 83 and the input impedance of the transistor 81 to yield a differentiated signal Sc' as shown in FIG. 4C which is applied to the base of the transistor 81. Accordingly, the transistor 81 becomes conductive during a period where the signal Sc' is high, and, since the collector electrode of the transistor 81 is connected to the capacitor 85, an audio oscillator control signal Sd' as shown in FIG. 4D is obtained at the collector thereof every time the opposite station terminates its transmission. During a period when the signal Sd' is high, the diode 86 is forwardly biased in conduction so that the constant oscillating signal from the oscillator circuit 90 is by-passed through the diode 86 to ground, thus nullifying the signal. Meanwhile, during the period when the signal Sd' is low, the diode 86 is reverse biased in cut off. As a result, the oscillating signal from the oscillator circuit 90 is supplied through the resistors 93 and 94 and further through the amplifier 6 to the speaker 7 without being by-passed through the diode 86. Therefore, when the opposite station terminates its transmission, a change-over sound for instructing the transition is produced from the speaker 7.
FIG. 5 shows a third embodiment of the transceiver according to this invention where the IF amplifier 3 is fed with a voltage for reverse AGC, the collector of the IF amplifying transistor 31 is connected through the primary winding of the IF transformer 32 and the resistor 33 to the voltage source terminal 34, and the connection point between the primary winding of the transformer 32 and the resistor 33 is grounded through the by-pass capacitor 35 and also the detected output of the diode 4 is applied to the low pass filter 36 to derive therefrom the control voltage for reverse AGC which is applied to the base of the transistor 31. The other elements corresponding to those of FIG. 1 are attached with the same reference numerals and their description will be omitted for the sake of brevity.
In this embodiment, when an opposite station is transmitting, the receiving station detects the transmission starting time point and produces a change-over sound for instructing that the opposite station has started its transmission.
The circuitry for performing the above function consists of a detector circuit 170 to detect the transmission starting time of the opposite station, an oscillator circuit 180, and a switching circuit 190 for controlling an oscillating signal from circuit 180 by a detected signal of detector circuit 170. A grounded-emitter transistor 171 has its base connected through a contact a or b of function switch 172 and then through a capacitor 173 or a resistor 174 to the junction between the primary winding of the transformer 32 and the resistor 33. The collector of transistor 171 is grounded through a capacitor 175 and is also connected to the collector electrode of the transistor 181 through the diode 191 and further through a resistor 192. The diode 191 is fed with a biasing voltage by resistors 193 and 194. The connection point between the diode 191 and the resistor 192 is connected through a resistor 195 to the movable contact of the variable resistor 5. In addition, the transistor 171 is always kept nonconductive during a time period when any signal is not present.
With such an arrangement, since the transistor 171 is cut off, the diode 191 is forwardly biased in the ON state. Accordingly, the oscillating signal of the oscillator circuit 180 is by-passed through the diode 191 and the capacitor 175 to ground, nullifying the oscillator signal feed to the amplifier 6.
In this embodiment, it is assumed that the function switch 172 is connected to the contact a and an RF carrier signal as shown in FIG. 6A is transmitted from the opposite station. Then, since the IF amplifier 3 is fed with the voltage for reverse AGC, a rectangular signal Sb", which is high during the transmitting period of the opposite station as shown in FIG. 6B, is obtained at the connection point between the primary winding of the transformer 32 and the resistor 33. The signal Sb" is differentiated by the capacitor 173 and the input impedance of the transistor 171, so that the base of the transistor 171 has a differentiated pulse Sc" as shown in FIG. 6C applied to it. Accordingly, during a period where the upward pulse Sc" corresponding to signal initiation is present, the transistor 171 becomes conductive to produce an audio oscillator control pulse Sd" as shown in FIG. 6D at the collector thereof every time the opposite station starts its transmission.
Since the diode 191 is reverse biased OFF during a period when the pulse Sd" is low, the oscillating signal from the oscillator circuit 180 is applied through the resistors 192 and 195 and further through the amplifier 6 to the speaker 7 without being by-passed to ground. Accordingly, when the opposite station is changed-over from its receiving condition to its transmitting condition, a change-over sound is reproduced from the speaker 7 to instruct that the above transition has been carried out.
If the function switch 172 is connected to the contact b, during the period when the opposite station is being transmitted, the transistor 171 is kept conductive and the diode 191 remains OFF, so that the oscillating signal of the oscillator circuit 180 is continuously applied to the speaker 7 creating a continuous sound for the purpose of calling the receiving station.
According to the above embodiment of this invention, every start of transmission at the opposite station is instructed by a changeover sound at the receiving station, so that the receiving station is appropriately notified and no simultaneous transmission will occur. As described above, this embodiment is of the type where the voltage for reverse AGC is applied to the IF amplifier 3. However, in the case where the voltage for forward AGC is applied thereto, it may be sufficient to connect the emitter electrode of the transistor 31 to the connection point between the capacitor 173 and the resistor 174.
In all the embodiments described above, the transition between transmitting and receiving conditions at the opposite station is detected by utilizing the fact that the collector operating level of the transistor 31 is changed according to the AGC operation during both the periods when a signal is being received and not being received. With this invention, however, the transmitting and receiving transition at the opposite station is noted by the use of a change-over sound.
FIG. 7 shows an embodiment of a circuit used in a typical receiver with AGC information as described above. In this embodiment, an IF signal from the IF amplifier 3, which is constructed in the same manner as described above, is supplied through a function switch 282 to a full-wave rectifier circuit 289 and a rectified output therefrom is supplied through a capacitor 283 to a base of a transistor 281. In this case, the transistor 281 is always kept conductive while a transistor 291 of an oscillator circuit 290 is kept in cut-off. The rectifier circuit 289 has derived therefrom a signal Sb as shown in FIG. 2B in accordance with the signal of the opposite station and a differentiated signal from the signal Sb is applied to the base electrode of the transistor 281 to make it nonconductive only when the signal Sb is decreasing, so that the transistor 290 becomes conductive only during this period to start its oscillation. Accordingly, when the opposite station is varied from its transmitting state to its receiving state, a brief change-over sound is produced from the speaker 7 to instruct that the above transition operation has been carried out. There is no need to say Go-ahead, please at every change-over time.
It will be apparent that many modifications and variations may be effected without departing from the scope of the novel concepts of this invention.
|
Circuits for use with a receiver which notify the operator of a receiving station by means of an audio tone when an opposite station is calling or has ceased transmission. The transition of an opposite station from its transmitting to receiving state or vice versa is detected and a specific change-over sound based upon the detector output is introduced into the principal station's receiver audio amplifier circuits.
| 7
|
RELATED APPLICATIONS
This application claims priority to U.S. Provisional Application Ser. No. 61/159,602 filed Mar. 12, 2009 entitled Time Based High Intensity Discharge Lamp Control, and to U.S. Provisional Application Ser. No. 61/172,166 filed Apr. 23, 2009 entitled Time Based High Intensity Discharge Lamp Control, both of which are hereby incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to methods, systems and controllers for operating high intensity discharge (HID) lamps at a substantially constant luminous flux output.
BACKGROUND OF THE INVENTION
HID lamps include high pressure sodium lamps, metal halide lamps and mercury vapour lamps. They are typically used in areas such as sports stadiums, warehouses and large public areas, where high levels of light over large areas are required. HID lamps tend to have relatively high power ratings, for example above 150 Watts. They tend to operate under higher pressures and temperatures than fluorescent lamps.
Generally, a HID lamp system will use an inductive ballast that is designed to make the lamp operate at its approximate design power. When operated this way, the luminous flux output from the lamp is not constant and deteriorates over time. A lamp may lose up to one half of its light producing capacity by the end of its operating life.
In situations where a specified constant level of light is required, for example in sports stadiums, this means that either 1) the lamp needs to be replaced once its luminous flux output decreases below the specified level, or 2) additional lamps need to be installed to ensure that the particular level of light is achieved, despite deterioration in the luminous flux output from the lamp. Both options result in a higher cost of the lighting system. Also, in the first case, some of the operating life of the lamp may be wasted, and in the second case, higher energy use may be required.
It would be desirable to provide a method of operating HID lamps, and apparatus for performing the method, that ameliorates the effects of lamp deterioration.
OBJECTS AND SUMMARY OF THE INVENTION
According to one aspect, the present invention provides a method for operating one or more high intensity discharge (HID) lamps of a particular type and rating, and having a defined operating life, at a predetermined substantially constant luminous flux output, the method including the steps of:
(i) using a test lamp of a similar type and rating to the HID lamps to develop a power-time characteristic that defines the power required at different times in the operating life of the lamps to operate the lamps at the predetermined luminous flux output, and (ii) operating the HID lamps in accordance with the power-time characteristic.
Using the method, a HID lamp may be operated at a constant luminous flux output throughout its operating life, thereby ameliorating the light depreciation problem of lamp deterioration. The method results in a longer useful life of the lamp, and a more stable light output from the lamp. A lighting system using the present invention may therefore provide cost and energy savings.
The power-time characteristic developed using the test lamp is specific to HID lamps of similar type and rating to the test lamp. For example, the type of HID lamp may be metal halide (MH) or high pressure sodium (HPS) and the rating may be between 150 W and 2000 W. Separate power-time characteristics may be developed for HID lamps of different types and ratings.
The predetermined substantially constant luminous flux output may be tailored for the circumstances in which the lamps will be used. For example, a desired luminous flux output for a 1500 W metal halide lamp for use in sports lighting may be 145,000 lumens. The operating life of such a lamp is around 5000 hours.
Using a test lamp to develop a power-time characteristic may include the steps of:
(a) at a plurality of different times in the operating life of the test lamp: (i) measuring a luminous flux output from the test lamp, and (b) if the luminous flux output differs from the predetermined luminous flux, (ii) altering power to the test lamp until its luminous flux output equals the predetermined luminous flux, and (iii) recording the time of alteration and the amount of power required at that time, whereby to develop the power-time characteristic.
The power-time characteristic may be a graph of power vs time over the operating life of the test lamp, or it may be a table of values of power required at the plurality of different times in which data is recorded. It may alternatively be a list of codes associated with operating times, the codes representing the amount of power required at each time. In this case, recording the amount of power required involves recording a code representing the amount.
The power required may be an amount of power increase or decrease, a total power needed or an amount of power to be injected, for example, by a current injector or secondary ballast. The characteristic may be developed using one test lamp, or using multiple test lamps and taking an average or some other statistical measure of the lamp power.
Altering power to the test lamp may involve increasing or decreasing current to the test lamp. In this case, recording the amount of power required may involve recording the amount of current required. The record of current vs time may form the power-time characteristic, or the power required may be determined using the current and the voltage of the power supply.
The steps of altering power and recording time and amount of alteration may be done manually or automatically by hardware or software. For example, the power may be altered manually, and the data recorded automatically.
The plurality of different times at which measurements are made may be equally spaced over the operating life of the test lamp. For example, for a lamp with an operating life of 5000 hours, measurements may be made every 20 hours. Of course, it will be appreciated that measurements could be made more often than this and need not be equally spaced.
A lamp typically experiences its greatest luminous flux depreciation over the first part of its operating life (say for example over the first 1000 hours), then the flux steadily decreases after this time. It may be possible, therefore, to take measurements at intervals up to well into the steadily decreasing portion of the lamp's operating life (say for example up to 2000 hours) such that the recorded data will cover the first part (i.e. the relatively rapidly decreasing luminous flux part) of the lamp's operating life plus sufficient of its remaining operating life (i.e. the steadily decreasing luminous flux part) for the rest of the remaining part to be extrapolated so that the power-time characteristic covers the operating life of the HID lamps.
Operating the HID lamps in accordance with the power-time characteristic may include the steps of:
(a) at a plurality of different times in the operating life of the HID lamps: (i) altering power to the HID lamps so that they operate at a power corresponding to that time in the power-time characteristic.
The plurality of different times in the operating life of the HID lamps that the power to the lamps is altered may coincide with the plurality of different times in the operating life of the test lamp that measurements were taken. For example, if measurements were taken every 20 hours, the power to the HID lamps may be altered every 20 hours. It will be appreciated, however, that the times need not coincide.
Again, altering the power to the HID lamps may involve increasing or decreasing current to each lamp.
If the control of the lamps is centrally managed, operating the HID lamps may include the steps of:
(a) at a plurality of different times in the operating life of the HID lamps:
(i) communicating a power (for example, an increase or decrease in current) corresponding to that time in the power-time characteristic to controllers of the HID lamps.
If the power is recorded as a code, the method may involve communicating the code representing the amount of power, and then determining the amount of power from the code. This reduces the data that needs to be communicated.
According to a further aspect, the present invention provides a controller for operating a high intensity discharge (HID) lamp of a particular type and rating, and having a defined operating life, at a predetermined substantially constant luminous flux output, the controller including:
(i) a power control unit for electrical connection between a power supply and the lamp, for altering an amount of power supplied to the lamp, and (ii) a timer for recording an amount of time that the lamp has been operating,
wherein the power control unit alters the amount of power supplied to the lamp at a plurality of different times in the operating life of the lamp according to a power-time characteristic developed using a test lamp of a similar type and rating to the lamp, the power-time characteristic for operating HID lamps of that type and rating at the predetermined luminous flux output.
A power control unit suitable for use in the present invention may include a primary ballast to provide a primary current to the lamp, and a current injector for injecting a secondary current to the lamp in order to alter the amount of power supplied to the lamp. Such a power control unit is described in International Patent Application PCT/AU2004/000601 to the present applicant, the contents of which are incorporated by reference.
The power control unit may alternatively be a magnetic ballast, or an electronic ballast.
The controller may further include a memory storing the power-time characteristic, and a microprocessor for determining the power required at a given time from the power-time characteristic.
The timer may be an electronic clock with a non-volatile memory that accumulates and stores the total running time of the lamp.
According to another aspect, the present invention provides a system for operating one or more high intensity discharge (HID) lamps of a particular type and rating, and having a defined operating life, at a predetermined substantially constant luminous flux output, the system including:
(a) a slave controller for each HID lamp, each slave controller including:
(i) a power control unit for electrical connection between a power supply and the lamp, for varying the amount of power supplied to the lamp, and (ii) a receiver for receiving communications to the slave controller, and
(b) a master controller including:
(i) a timer for recording the amount of time that the HID lamps have been operating, and (ii) a transmitter for transmitting communications to the slave controller,
wherein the master controller communicates a power to the slave controllers at a plurality of different times in the operating life of the HID lamps, the power determined according to a power-time characteristic developed using a test lamp of a similar type and rating to the HID lamps, the power-time characteristic for operating HID lamps of that type and rating at the predetermined luminous flux output.
The master controller may include a memory storing the power-time characteristic, and a microprocessor for determining the power required at a given time from the power-time characteristic. If the power-time characteristic is stored as codes indicating the power required at specific operating times, the microprocessor determines the code corresponding to a given time, rather than the power required at the given time.
This information is then communicated to the slave controllers using the transmitter. The communication between the master and slave controllers may be wired, fibre optic, wireless or a combination of these types of communication links.
In the embodiment where codes are transmitted, the slave controller may include a memory storing the amount of power corresponding to codes in the power-time characteristic, and a microprocessor for determining the power required from a code. The slave controller can then run the lamp at the required power.
The master/slave controller system is suitable for situations where a series of lamps are illuminated simultaneously, for example, at a sports stadium. It reduces the cost of the lighting system, as the slave controllers do not need separate timers and memories to store the power-time characteristic.
For a better understanding of the invention and to show how it may be performed, embodiments of the present invention will now be described, by way of example only, with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic block diagram of a controller and other components to operate a lamp.
FIG. 2 is a flow chart of a method for developing a power-time characteristic for operating lamps of a particular type and rating at a substantially constant luminous flux output.
FIG. 3 is a graph of a typical power-time characteristic for a 1500 W metal halide lamp.
FIG. 4 is a schematic block diagram of a master controller and slave controllers.
FIG. 5 is a table storing a power-time characteristic as power codes corresponding to different time intervals in the operating life of a lamp.
FIG. 6 is a table relating the power codes of FIG. 5 with actual amounts of current to be injected into the lamp.
FIG. 7 shows in more detail the components of a master controller for establishing a power-time characteristic.
FIG. 8 is a flow chart of a method for operating lamps using a master controller and slave controllers.
FIG. 9 is a flow chart of a method for operating lamps having different starting times.
FIG. 10 is a graph showing power-time characteristics for operating lamps which have different starting times.
DESCRIPTION OF EMBODIMENTS
Specific embodiments of the invention will now be described with reference to the accompanying drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. The terminology used in the detailed description of the embodiments illustrated in the accompanying drawings is not intended to be limiting of the invention. In the drawings, like numbers refer to like elements.
FIG. 1 shows a schematic block diagram of a controller 10 and other components to operate a HID lamp 16 .
An AC power source 12 is placed in circuit with an ignitor 14 and the lamp 16 . The circuit also includes a power factor correction capacitor 18 connected across the terminals of the AC power source 12 .
The controller 10 shown in this embodiment includes a transformer 20 , being a step-up transformer that acts to inject voltage into the lamp circuit to facilitate lamp starting. The transformer 20 is connected in series with the lamp circuit and injects approximately 277 volts AC into the circuit and subsequently into the lamp 16 . This aids in starting of the lamp 16 , particularly as it ages.
The transformer 20 is electrically connected to a primary ballast 22 , which in this embodiment is an inductor. A control ballast 24 and an electronic switch (e.g. a triac) 26 are connected in parallel with the primary ballast 22 as a current injector. The primary ballast 22 , control ballast 24 and switch 26 together from a power control unit 27 .
When the switch 26 is closed, current flows through the control ballast 24 , and the control ballast 24 thereby injects current into the main circuit. The control ballast 24 is switched in a transient fashion, e.g. only for a portion of the duration of a cycle of the AC supply.
A microprocessor 28 controls the switch 26 to inject the additional current into the main circuit. A memory 29 is connected to the microprocessor 28 . The microprocessor 28 is operated by a power supply 30 , for example, a 5V DC regulated supply. A timer 32 records the amount of time that the lamp 16 has been operating.
Also shown in FIG. 1 is a flux meter 34 , for measuring a luminous flux output from the lamp 16 . The flux meter 34 may be used with the controller 10 and other components in a method for developing a power-time characteristic for operating lamps of a particular type and rating at a predetermined substantially constant luminous flux output. For this method, the lamp 16 is a test lamp with a similar type and rating. The method is depicted in FIG. 2 .
Referring to FIG. 2 , at step 40 a luminous flux output from the test lamp 16 is measured. The luminous flux output is then compared to the predetermined constant luminous flux output at step 42 . If it differs from this constant, the power to the test lamp 16 is altered at step 44 . For example, the power may be manually altered by pressing buttons connected to the microprocessor 28 , to direct it to close or open the switch 26 . This causes the secondary ballast 24 to inject more or less current into the main circuit, thereby increasing or decreasing the lamp power.
The comparing and altering steps 42 and 44 are repeated until the luminous flux output of the test lamp 16 equals the predetermined luminous flux. Then the time of alteration and the amount of power required (for example, the amount of increase or decrease in current) is recorded at step 46 , whereby to develop the power-time characteristic. The amount of power required may be recorded as a code representing the amount. The microprocessor 28 may automatically cause the data to be recorded in the memory 29 .
Steps 40 to 46 are repeated at a plurality of different times in the operating life of the test lamp 16 . These times may be equally spaced, or may be unequally spaced at convenient times to make the measurements.
FIG. 3 shows a graph of a typical power-time characteristic 50 for operating a 1500 W metal halide lamp at a luminous flux output of 145,000 lumens. To develop this characteristic 50 , measurements may be taken every 20 hours and, for example, 250 measurements may be made so that the power-time characteristic covers the operating life of the HID lamps.
It can be seen from the power-time characteristic 50 that the power required to operate the lamp 16 (and other lamps of a similar type and rating) at the predetermined luminous flux output at the start of the lamp's operating life is PMIN=1200 W. The required power increases rapidly for a first part of the operating life of the lamp 16 , and then increases steadily before reaching PMAX=1700 W. For some lamps, the rapid increase in required power over a first part of the lamp's operating life may be approximated by a constant gradient as indicated by the line 49 , and the steady increase in required power over the remaining operating life of the lamp may be similarly approximated by a constant gradient as indicated by the line 51 . If a lamp exhibits this type of power time characteristic for a constant luminous output, it may be possible to develop a power time characteristic for the whole operating life of the lamp by taking measurements that go past the “knee” region 53 of the curve 50 and then extrapolating the remainder of the curve from those measurements.
The power-time characteristic 50 can be used to operate other similar lamps at the predetermined luminous flux output.
In one embodiment, the lamps are each fitted with a controller 10 as shown in FIG. 1 , with the power-time characteristic 50 stored in the memory 29 . The timer 32 operates when the lamp is switched on to record the amount of time that the lamp has been operating. The primary ballast 22 is chosen to provide power of PMIN to the lamp.
At a plurality of different times in the operating life of the lamp, the microprocessor 28 determines the required power from the power-time characteristic stored in the memory 29 . The microprocessor 28 accordingly instructs the switch 26 to open or close, thereby increasing or decreasing the current injected into the main circuit by the secondary ballast 24 such that the required power is supplied to the lamp.
Referring to the graph of FIG. 3 , the line 52 shows the power provided by the primary ballast 22 , with the difference between the power-time characteristic 50 and the line 52 at a given time being the amount of power to be injected by the secondary ballast 24 .
In another embodiment, illustrated in FIG. 4 , a master controller 54 communicates a required power to slave controllers 56 , 58 and 60 . Each slave controller 56 , 58 and 60 is for operating a lamp 62 , 64 and 66 respectively. The lamps 62 , 64 and 66 are of a similar type and rating and are operated simultaneously.
The master controller 54 has a memory 68 storing a power-time characteristic developed using a test lamp for lamps of the type and rating of lamps 62 , 64 and 66 . As shown in FIG. 5 , the power-time characteristic in this embodiment is recorded in a look up table 55 as power codes 57 for each time interval 59 . In FIG. 5 , 255 time intervals 59 are shown, being spaced apart by 20 hours. Each time interval 59 represents a time 61 in the operating life of the lamps. As shown in look up table 55 , the same power code may be recorded against different time intervals 59 . The master controller 54 also has a microprocessor 70 , a timer 72 and a transmitter 74 . In this example, the transmitter 74 is an antenna for communicating with the slave controllers 56 , 58 and 60 .
Each slave controller 56 , 58 and 60 , has a power control unit 76 , 78 and 80 , which includes a primary ballast and current injector, as described in relation to FIG. 1 . The power control units 76 , 78 and 80 are electrically connected between a power supply 82 and the lamps 62 , 64 and 66 . In this example, a single power supply 82 is used for all of the lamps; however, it is possible to use a separate power supply for each lamp. A switch (not shown) may be included between the power supply 82 and before the slave controller/lamp combinations 56 - 62 , 58 - 64 and 60 - 66 for switching on the lamps. When this switch is switched ON, an appropriate signal (e.g. a logical high) may be supplied to the master controller 54 to activate it. When the switch is OFF, the signal to the master controller 54 (e.g. a logical low) renders the master controller 54 inactive. The timer 72 may operate only when the master controller 54 is active, thereby measuring the operating time of the lamps.
In this example, the slave controllers 56 , 58 and 60 are programmed with instructions that relate the power codes 57 of FIG. 5 with actual amounts of power 65 (in this case current—see FIG. 6 ) to be injected into the lamp. On receipt of a power code 57 , the microprocessors 83 , 85 and 87 operate the power control units 76 , 78 and 80 in accordance with these instructions to inject the correct amount of current into the lamps via the secondary ballasts.
In another example, the power codes 57 and corresponding amounts of power 65 could be stored in a look up table 63 (see FIG. 6 ) in the slave controller memories 77 , 79 and 81 . In this case, microprocessors 83 , 85 and 87 determine the power required 65 from the power code 57 using the information stored in the look up table 63 .
The slave controllers 56 , 68 and 60 also have receivers 84 , 86 and 88 in the form of antennas for receiving communications from the master controller 54 via its antenna 74 .
FIG. 7 shows in more detail the components of the master controller 54 . The master controller 54 includes, as previously described, a microprocessor 70 , with a memory 68 , a timer 72 and a transmitter 74 . FIG. 7 illustrates a master controller set up for developing the power time characteristic to be stored in its memory 68 and for operating, via the transmitter 74 , slave controllers (such as the slave controllers 56 , 58 , 60 of FIG. 4 ) or a test lamp. The transmitter 74 may be a serial communications port. The microprocessor 70 is powered by a suitable supply 67 , for example 5V dc, and operates a suitable display 71 via a display driver 69 for indicating time and power during development of the power time characteristic. Linked to the microprocessor 70 is a push button unit 73 .
To develop the power time characteristic, an operator, at each say 20 hour measurement point for a test lamp (which time may be displayed by appropriate initial manipulation of a push button—for example a single push of the up button), manipulates the up-down push buttons 73 until the luminous flux output of the test lamp matches the desired constant value (as indicated by a separate flux meter). When the test lamp output is at the desired constant value, appropriate manipulation of a button of the push button unit 73 (for example a rapid double push of the up button) causes the power (and/or code representing the power) and time at that measurement point to be stored in the memory 68 . Thus a power time characteristic in the form of a look up table is developed that defines the power required at different times in the operating life of HID lamps (of similar type and rating to the test lamp) for the lamps to give a substantially constant luminous flux output.
Where the master controller records only the power required, the power values may be subsequently converted into codes.
Where the master controller records only a code representing a power, then the appropriate power for that code may be simultaneously communicated to the slave controllers.
The use of codes to represent power means the master controller need only store a look up table 55 (see FIG. 5 ) showing a power code for each time interval. The slave controllers may then be programmed to convert the codes directly to the relevant power, or alternatively a look up table 63 relating the codes to the power required (see FIG. 6 ) may be stored in the slave controller memories.
The master controller 54 may then be used to drive slave controllers as illustrated by FIG. 4 .
FIG. 8 illustrates a method for operating the lamps 62 , 64 and 66 using the master controller 54 and slave controllers 56 , 58 and 60 .
At a plurality of times in the operating life of the lamps 62 , 64 and 66 , as recorded by the timer 72 , the microprocessor 70 looks up the power-time characteristic stored in the memory 68 to determine the power code 57 corresponding to that time interval 59 , which represents the power that the lamps should be operating at (step 92 ). At step 94 , using the transmitter 74 , the microprocessor 70 communicates this power code 57 to the slave controllers 56 , 58 and 60 . The communication link 90 is wireless in this case, but could be hardwired in other embodiments. The power code 57 may be transmitted from the master controller 54 to the slave controllers 56 , 58 and 60 , for example, every 30 seconds. For example, the same code may be transmitted for 20 hours, then the next code for the next 20 hours. This reduces the impact of corrupted transmissions.
The receivers 84 , 86 and 88 receive the communication, and at step 95 the microprocessors 83 , 85 and 87 look up the memories 77 , 79 and 81 to determine the power required 65 from the power code 57 . At step 96 the power control units 76 , 78 and 80 are operated to alter the power supplied to the lamps 62 , 64 and 66 such that the lamps operate at a substantially constant luminous flux output.
While power codes 57 have been transmitted in this embodiment, it will be appreciated that in another embodiment the power required could be directly transmitted from the master controller 54 to the slave controllers 56 , 58 and 60 .
In a further embodiment, a master controller 54 may control individual lamps separately via their slave controllers. Each slave controller is assigned an address (for example, a 2 digit number) that is used to communicate with that slave controller.
Again, in this embodiment the master controller 54 stores in memory 68 a power-time characteristic that can be used to operate the lamps. Where the lamps are the same, the power-time characteristic may be stored as a single look up table, for example table 55 shown in FIG. 5 . Where the lamps are different, separate look up tables storing each characteristic are required.
The master controller 54 may have a separate timer for each lamp, or the timer 72 could be used to measure the operating time of all of the lamps, by keeping a record of the starting time of each lamp.
This embodiment allows for lamps, which may fail prematurely before their end of life, to be replaced and their power-time characteristic reset so that they at all times produce a substantially constant luminous flux output.
With reference to FIG. 9 , for each lamp ( 100 , 102 , 104 and 106 ), its time of operation is determined and at step 110 , the microprocessor 70 looks up the power-time characteristic (for example table 55 ) and determines the power code 57 corresponding to that time. This power code 57 and the address code of the lamp are communicated to the slave controllers via the transmitter 74 at step 112 .
Only the slave controller whose address code is the same as the sent address code determines the power required 65 from the power code 57 at step 114 and alters the power supplied to its lamp at step 116 .
The master controller may communicate the two part codes (address code and power code) for each lamp every, for example, 30 seconds.
If a lamp is replaced before its normal end of life (typically 5000 hours) because of lamp failure (or any other reason) and a new lamp is connected to the slave controller, then the power-time characteristic for the lamp is reset in the master controller by resetting the timer for that slave controller to zero (or keeping a record of the new starting time of the lamp if a single timer 72 is used). All subsequent communication with the replacement lamp is done on this new time.
In practical terms, the resetting of the time for a replacement lamp may be achieved by:
a) placing the master controller in “reset-time mode” by pressing a push button on the master controller, b) displaying the slave controller address on the display (for example 00-99), and c) pressing a reset-time push button to effect the reset.
FIG. 10 shows graphically the operation of lamps 100 (lamp no. 1 ), 102 (lamp no. 2 ), 104 (lamp no. 3 ) and 106 (lamp no. 4 ) having different starting times (for example, because lamps 102 , 104 and 106 have replaced other lamps which have burnt out). In this example, lamp 100 is started at time=0, lamp 102 at time=1000 hours, lamp 104 at time=2000 hours and lamp 106 at time=1600 hours. As shown in the graph, the power-time characteristic 118 , 120 , 122 and 124 for lamps 100 , 102 , 104 and 106 effectively start at the respective lamp's starting time.
To operate the lamps at time=T (shown in the graph of FIG. 10 as 3000 hours), power codes 57 representing power P 1 , P 2 , P 3 and P 4 are transmitted from the master to the slave controllers with the respective address code of lamps 100 , 102 , 104 and 106 . This allows the lamps, despite their different operating times, to be operated at a substantially constant luminous flux output.
It is to be understood that various alterations, additions and/or modifications may be made to the parts previously described without departing from the ambit of the present invention, and that, in the light of the above teachings, the present invention may be implemented in software, firmware and/or hardware in a variety of manners as would be understood by the skilled person.
Although the invention has been described in terms of particular embodiments and applications, one of ordinary skill in the art, in light of this teaching, can generate additional embodiments and modifications without departing from the spirit of or exceeding the scope of the claimed invention. Accordingly, it is to be understood that the drawings and descriptions herein are proffered by way of example to facilitate comprehension of the invention and should not be construed to limit the scope thereof.
|
Apparatus and a method for operating high intensity discharge (HID) lamps at a predetermined substantially constant luminous flux output. A power-time characteristic is developed using a test lamp of similar type and rating to the HID lamps. This characteristic defines the power required at different times, which may be regularly spaced intervals of for example 20 hours, during the operating life of the HID lamps to operate the lamps at the predetermined luminous flux output. The power time characteristic is then “played back” in real time via a microprocessor based master controller for the HID lamps. The communications to the HID lamps may be wireless or hard wired. The result is that the HID lamps are operated at substantially constant lumens resulting in significant energy savings and improved lamp performance.
| 7
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a continuation of Ser. No. 10/906,109, filed on Feb. 3, 2005, and which is a continuation-in-part of Ser. No. 10/361,815, which is a continuation of Ser. No. 10/100,032, which is a continuation of Ser. No. 09/679,300, which is a continuation of PCT/SE99/00934. The entire contents of Ser. No. 10/361,815, Ser. No. 10/100,032, Ser. No. 09/679,300, and PCT/SE99/00934 are incorporated herein by reference.
[0002] The invention generally relates to a locking system for providing mechanical joining of floorboards. More specifically, the invention concerns an improvement of a locking system of the type described and shown in WO 94/26999. The invention also relates to a floorboard provided with such a locking system. According to one more aspect of the invention, a floorboard with different designs of the locking system on long side and short side is provided.
FIELD OF THE INVENTION
[0003] The invention is particularly suited for mechanical joining of thin floating floorboards, such as laminate and parquet flooring, and therefore the following description of prior art and the objects and features of the invention will be directed to this field of application, in particular rectangular floorboards that are joined on long sides as well as short sides. The features distinguishing the invention concern in the first place parts of the locking system which are related to horizontal locking transversely of the joint edges of the boards. In practice, floorboards will be manufactured according to the inventive principles of also having locking means for mutual vertical locking of the boards.
BACKGROUND ART
[0004] WO 94/26999 discloses a locking system for mechanical joining of building boards, especially floorboards. A mechanical locking system permits locking together of the boards both perpendicular to and in parallel with the principal plane of the boards on long sides as well as short sides. Methods for making such floorboards are described in SE 9604484-7 and SE 9604483-9. The principles of designing and laying the floorboards as well as the methods for making the same that are described in the above three documents are applicable also to the present invention, and therefore the contents of these documents are incorporated by reference in present description.
[0005] With a view to facilitating the understanding and description of the present invention as well as the understanding of the problems behind the invention, now follows with reference to FIGS. 1-3 a brief description of floorboards according to WO 94/26999. This description of prior art should in applicable parts be considered to apply also to the following description of embodiments of the present invention.
[0006] A floorboard 1 of known design is shown from below and from above in FIGS. 3 a and 3 b , respectively. The board is rectangular and has a top side 2 , an underside 3 , two opposite long sides 4 a , 4 b which form joint edges, and two opposite short sides 5 a , 5 b which form joint edges.
[0007] Both the long sides 4 a , 4 b and the short sides 5 a , 5 b can be joined mechanically without any glue in the direction D 2 in FIG. 1 c . To this end, the board 1 has a planar strip 6 which is mounted at the factory and which extends horizontally from one long side 4 a , the strip extending along the entire long side 4 a and being made of a flexible, resilient aluminum sheet. The strip 6 can be mechanically fixed according to the illustrated embodiment, or fixed by means of glue or in some other fashion. Other strip materials can be used, such as sheet of some other metal, and aluminum or plastic sections. Alternatively, the strip 6 can be integrally formed with the board 1 , for instance by some suitable working of the body of the board 1 . The strip, however, is always integrated with the board 1 , i.e. it is not mounted on the board 1 in connection with laying. The width of the strip 6 can be about 30 mm and its thickness about 0.5 mm. A similar, although shorter strip 6 ′ is arranged also along one short side 5 a of the board 1 . The edge side of the strip 4 facing away from the joint edge 4 a is formed with a locking element 8 extending along the entire strip 6 . The locking element 8 has an active locking surface 10 facing the joint edge 4 a and having a height of e.g. 0.5 mm. In connection with laying, the locking element 8 cooperates with a locking groove 14 , which is formed in the underside 3 of the opposite long side 4 b of an adjacent board 1 ′. The short side strip 6 ′ is provided with a corresponding locking element 8 ′, and the opposite short side 5 b has a corresponding locking groove 14 ′.
[0008] For mechanical joining of both long sides and short sides also in the vertical direction (direction D 1 in FIG. 1 c ), the board 1 is further along its one long side 4 a and its one short side 5 a formed with a laterally open recess 16 . The recess 16 is defined downwards by the associated strip 6 , 6 ′. At the opposite edges 4 b and 5 b there is an upper recess 18 defining a locking tongue 20 (see FIG. 2 a ) cooperating with the recess 16 to form a tongue-and-groove joint.
[0009] FIGS. 1 a - 1 c show how two such boards 1 , 1 ′ can be joined by downwards angling. FIGS. 2 a - 2 c show how the boards 1 , 1 ′ can instead be joined by snap action. The long sides 4 a , 4 b can be joined by both methods whereas the short sides 5 a , 5 b —after laying of the first row—are normally joined after joining of the long sides and merely by snap action. When a new board 1 ′ and a previously laid board 1 are to be joined along their long sides according to FIGS. 1 a - 1 c , the long side 4 b of the new board 1 ′ is pressed against the long side 4 a of the previously laid board 1 according to FIG. 1 a , so that the locking tongue 20 is inserted into the recess 16 . The board 1 ′ is then angled downwards to the subfloor 12 according to FIG. 1 b . Now the locking tongue 20 completely enters the recess 16 while at the same time the locking element 8 of the strip 6 enters the locking groove 14 . During this downwards angling, the upper part of the locking element 8 can be active and accomplish a guiding of the new board 1 ′ towards the previously laid board 1 . In the joined state according to FIG. 1 c , the boards 1 , 1 ′ are locked in both D 1 direction and D 2 direction, but may be displaced relative to each other in the longitudinal direction of the joint.
[0010] FIGS. 2 a - 2 c illustrate how also the short sides 5 a and 5 b of the boards 1 , 1 ′ can be mechanically joined in both D 1 and D 2 direction by the new board 1 ′ being moved essentially horizontally towards the previously laid board 1 . This can be carried out after the long side 4 b of the new board 1 ′ has been joined as described above. In the first step in FIG. 2 a , bevelled surfaces adjacent to the recess 16 and the locking tongue 20 cooperate so that the strip 6 ′ is forced downwards as a direct consequence of the joining of the short sides 5 a , 5 b . During the final joining, the strip 6 ′ snaps upwards as the locking element 8 ′ enters the locking groove 14 ′. By repeating the operations shown in FIGS. 1 and 2 , the entire floor can be laid without glue and along all joint edges. Thus, prior-art floorboards of the above-mentioned type are joined mechanically by, as a rule, first being angled downwards on the long side, and when the long side is locked, the short sides are snapped together by horizontal displacement along the long side. The boards 1 , 1 ′ can be taken up again in reverse order, without the joint being damaged, and be laid once more.
[0011] For optimal function, it should be possible for the boards, after being joined, along their long sides to take a position where there is a possibility of a small play between the locking surface 10 and the locking groove 14 . For a more detailed description of this play, reference is made to WO 94/26999.
[0012] In addition to the disclosure of the above-mentioned patent specifications, Norske Skog Flooring AS (licensee of Valinge Aluminum AB) introduced a laminate flooring with a mechanical joining system according to WO 94/29699 in January 1996 in connection with the Domotex fair in Hannover, Germany. This laminate flooring marketed under the trademark Alloc®, is 7.6 mm thick, has a 0.6 mm aluminum strip 6 which is mechanically fixed to the tongue side and the active locking surface 10 of the locking element 8 has an inclination of about 70°-80° to the plane of the board. The joint edges are impregnated with wax and the underside is provided with underlay board which is mounted at the factory. The vertical joint is designed as a modified tongue-and-groove joint. The strips 6 , 6 ′ on long side and short side are largely identical, but slightly bent upwards to different degrees on long side and short side. The inclination of the active locking surface varies between long side and short side. The distance of the locking groove 14 from the joint edge, however, is somewhat smaller on the short side than on the long side. The boards are made with a nominal play on the long side which is about 0.05-0.10 mm. This enables displacement of the long sides and bridges width tolerances of the boards. Boards of this brand have been manufactured and sold with zero play on the short sides, which is possible since the short sides need not be displaced in connection with the locking which is effected by snap action. Boards of this brand have also been made with more beveled portions on the short side to facilitate snapping in according to FIGS. 2 a - c above. It is thus known that the mechanical locking system can be designed in various ways and that long side and short side can be of different design.
[0013] WO 97/47834 (Unilin) discloses a mechanical joining system which is essentially based on the above known principles. In the corresponding product which this applicant began to market in the latter part of 1997, biasing between the boards is strived for. This leads to high friction and difficulties in angling together and displacing the boards. This document also shows that the mechanical locking on the short side can be designed in a manner different from the long side. In the described embodiments, the strip is integrated with the body of the board, i.e. made in one piece with and of the same material as the body of the board.
SUMMARY
[0014] Although the flooring according to WO 94/26999 and the flooring marketed under the trademark Alloc® have great advantages compared with traditional, glued floorings, further improvements are desirable.
[0015] Mechanical joints are very suitable for joining not only laminate floorings, but also wood floorings and composite floorings. Such floorboards may consist of a large number of different materials in the surface, the core and the rear side, and as described above these materials can also be included in the strip of the joining system, the locking element on the strip, fixing surfaces, vertical joints etc. This solution involving an integrated strip, however, leads to costs in the form of waste when the mechanical joint is being made. Alternatively, special materials, such as the aluminum strip 6 above, can be glued or mechanically fixed to the floorboard to be included as components in the joining system. Different joint designs affect the costs to a considerable extent.
[0016] A strip made of the same material as the body of the board and formed by working of the body of the board can in some applications be less expensive than an aluminum strip, especially for floorboards in lower price ranges. Aluminum, however, is more advantageous in respect of flexibility, resilience and displaceability as well as accuracy in the positioning of the locking element. Aluminum also affords the possibility of making a stronger locking element. If the same strength is to be achieved with a locking element of wood fiber, it must be wide with a large shearing surface, which results in a large amount of waste material in manufacture, or it must be reinforced with a binder. Depending on the size of the boards, working of, for instance, 10 mm of a joint edge may result in six times higher cost of waste per m 2 of floor surface along the long sides compared with the short sides.
[0017] In addition to the above problems relating to undesirable waste of material, the present invention is based on the insight that the long sides and short sides can be optimized with regard to the specific locking functions that should be present in these joint edges.
[0018] As described above, locking of the long side is, as a rule, carried out by downwards angling. Also a small degree of bending down of the strip during locking can take place, as will be described in more detail below. Thanks to this downwards bending together with an inclination of the locking element, the boards can be angled down and up again with very tight joint edges. The locking element along the long sides should also have a high guiding capability so that the long side of a new board in connection with downwards angling is pushed towards the joint edge of the previously laid board. The locking element should have a large guiding part. For optimal function, the boards should along their long sides, after being joined, be able to take a mutual position transversely of the joint edges where there is a small play between locking element and locking groove.
[0019] On the other hand, locking of the short side is carried out by the long side being displaced so that the strip of the short side can be bent down and snap into the locking groove. Thus the short side must have means which accomplish downwards bending of the strip in connection with lateral displacement. The strength requirement is also higher on the short side. Guiding and displaceability are less important.
[0020] Summing up, there is a great need for providing a mechanical joint of the above type at a low cost and with optimal locking functions at each joint edge. It is not possible to achieve a low cost with prior-art solutions without also lowering the requirements as to strength and/or laying function. An object of the invention is to provide solutions which aim at lowering the cost with maintained strength and function.
[0021] According to a first aspect of the invention, a locking system for mechanical joining of floorboards is thus provided, where immediately juxtaposed upper parts of two adjacent joint edges of two joined floorboards together define a joint plane perpendicular to the principal plane of the floor boards. To obtain a joining of the two joint edges perpendicular to the joint plane, the locking system comprises in a manner known per se a locking groove which is formed in the underside of and extends in parallel with the first joint edge at a distance from the joint plane, and a portion projecting from the lower part of the second joint edge and below the first joint edge and integrated with a body of the board, said projecting portion supporting at a distance from the joint plane a locking element cooperating with the locking groove and thus positioned entirely outside the joint plane seen from the side of the second joint edge, said projecting portion having a different composition of materials compared with the body of the board. The inventive locking system is characterized in that the projecting portion presents at least two horizontally juxtaposed parts, which differ from each other at least in respect of the parameters material composition and material properties.
[0022] In a first embodiment of the first aspect of the invention, said at least two parts of the projecting portion are located at different distances from the joint plane. In particular, they may comprise an inner part closest to the joint plane and an outer part at a distance from the joint plane. The inner part and the outer part are preferably, but not necessarily, of equal length in the joint direction. In this first aspect of the invention, a material other than that included in the body is thus included in the joining system, and in particular the outer part can be at least partially formed of a separate strip which is made of a material other than that of the body of the board and which is integrally connected with the board by being factory-mounted. The inner part can be formed at least partially of a worked part of the body of the board and partially of part of said separate strip. The separate strip can be attached to such a worked part of the board body. The strip can be located entirely outside said joint plane, but can also intersect the joint plane and extend under the joint edge to be attached to the body also inside the joint plane.
[0023] This embodiment of the invention thus provides a kind of combination strip in terms of material, for example a projecting portion comprising an inner part with the material combination wood fiber/rear laminate/aluminum, and an outer part of aluminum sheet.
[0024] It is also possible to make the projecting part from three parts which are different in terms of material: an inner part closest to the joint plane, a central part and an outer part furthest away from the joint plane. The inner part and the outer part can possibly be equal in terms of material.
[0025] The portion projecting outside the joint plane need not necessarily be continuous or unbroken along the joint edge. A conceivable variant is that the projecting portion has a plurality of separate sections distributed along the joint edge. As an example, this can be accomplished by means of a separate strip with a continuous inner part and a toothed outer part, said strip being attachable to a part of the board body, said part being worked outside the joint plane.
[0026] In an alternative embodiment of the first aspect of the invention, said at least two parts, which differ in respect of at least one of the parameters material composition and material properties, are instead juxtaposed seen in the direction parallel with the joint edges. For example, there may be a plurality of strip types on one and the same side, where each strip type is optimized for a special function, such as strength and guiding in connection with laying. As an example, the strips can be made of different aluminum alloys and/or of aluminum having different states (for instance, as a result of different types of heat treatment).
[0027] According to a second aspect of the invention, a locking system for mechanical joining of floorboards is provided. In this second aspect of the invention, the projecting portion is instead formed in one piece with the body of the board and thus has the same material composition as the body of the board. This second aspect of the invention is characterized in that the projecting portion, as a direct consequence of machining of its upper side, presents at least two horizontally juxtaposed parts, which differ from each other in respect of at least one of the parameters material composition and material properties.
[0028] The inventive principle of dividing the projecting portion into several parts which differ from each other in terms of material and/or material properties thus is applicable also to the prior-art “wood fiber strip”.
[0029] In the same manner as described above for the first aspect of the invention, these two parts can be located at different distances from the joint plane, and especially there may be three or more parts with different material composition and/or material properties. Optionally, two such parts can be equal in respect of said parameters, but they may differ from a third.
[0030] In one embodiment, said two parts may comprise an inner part closest to the joint plane and an outer part at a distance from the joint plane. There may be further parts outside the outer part. Specifically, an outer part can be formed of fewer materials than an inner part. For instance, the inner part may consist or wood fiber and rear laminate, whereas the outer part, by machining from above, consists of rear laminate only. In one embodiment, the projecting portion may comprise—seen from the joint plane outwards—an inner part, an outer part and, outside the outer part, a locking element supported by the outer part. The locking element may differ from both inner and outer part in respect of said material parameters.
[0031] The projecting portion may consist of three laminated layers, and therefore it is possible, by working from above, to provide a locking system which, counted from the top, has a relatively soft upper guiding part which need not have any particular strength, a harder central part which forms a strong active locking surface and absorbs shear forces in the locking element, and a lower part which is connected with the rest of the projecting portion and which can be thin, strong and resilient.
[0032] Laminated embodiments can be suitable in such floorboards where the body of the board consists of, for instance, plywood or particle board with several layers. Corresponding layers can be found in the walls of the locking groove. For plywood, the material properties can be varied by changing the direction of fibers in the layers. For particle board, the material properties can be varied by using different chip dimensions and/or a binder in the different layers. The board body can generally consist of layers of different plastic materials.
[0033] In the definition of the invention, the term “projecting portion” relates to the part or parts of the board projecting outside the joint plane and having a function in the locking system in respect of supporting of locking element, strength, flexibility etc.
[0034] An underlay of underlay board, foam, felt or the like can, for instance, be mounted even in the manufacture of the boards on the underside thereof. The underlay can cover the underside up to the locking element, so that the joint between the underlays will be offset relative to the joint plane F. Although such an underlay is positioned outside the joint plane, it should thus not be considered to be included in the definition of the projecting portion in the appended claims.
[0035] In the aspect of the invention which relates to embodiments with a projecting portion of the same material as the body of the board, any thin material layers which remain after working from above should in the same manner not be considered to be included in the “projecting portion” in the cases where such layers do not contribute to the locking function in respect of strength, flexibility, etc. The same discussion applies to thin glue layers, binders, chemicals, etc. which are applied, for instance, to improve moisture proofing and strength.
[0036] According to a third aspect of the invention, there is provided a floorboard presenting a locking system according to the first aspect or the second aspect of the invention as defined above. Several possibilities of combining prior-art separate strips, prior-art wood fiber strips and “combination strips” according to the invention are available. These possibilities can be used optionally on long side and short side.
[0037] For the above aspects, the projecting portion of a given joint edge, for instance a long side, has at least two parts with different material composition and/or material properties. For optimization of a floorboard, such a difference in materials and/or material properties, however, may be considered to exist between the long sides and short sides of the board instead of within one and the same joint edge.
[0038] According to a fourth aspect of the invention, a rectangular floorboard is thus provided, comprising a body and first and second locking means integrated with the body and adapted to provide a mechanical joining of adjacent joint edges of such floorboards along long sides and short sides, respectively, of the boards in a direction perpendicular to the respective joint edges and in parallel with the principal plane of the floorboards. According to this aspect of the invention, the floorboard is characterized in that said first and second locking means differ in respect of at least one of the parameters material composition and material properties. Preferably, said first and second locking means each comprise on the one hand a portion which projects from a joint edge and which at a distance from the joint edge supports a locking element and, on the other hand, a locking groove, which is formed in the underside of the body at an opposite joint edge for engaging such a locking element of an adjacent board. At least one of said locking means on the long side and the short side may comprise a separate element which is integrally fixed to the body of the board at the factory and is made of a material other than that included in the body of the board. The other locking means may comprise an element which is formed in one piece with the body of the board.
[0039] Within the scope of the fourth aspect of the invention, there are several possibilities of combination. For example, it is possible to select an aluminum strip for the long side and a machined wood fiber strip for the short side or vice versa. Another example is that for the short side or the long side a “combination strip” according to the first and the second aspect of the invention is selected, and for the other side a “pure” aluminum strip or a “pure” worked wood fiber strip is selected.
[0040] The above problem of undesirable costs of material is solved according to the invention by the projecting portion being made of different materials and/or material combinations and thus specially adaptable to the selected materials in the floorboard and the function and strength requirements that apply to the specific floorboard and that are specific for long side and short side. This advantage of the invention will be evident from the following description.
[0041] Since different requirements are placed on the long side and the short side and also the cost of waste differs, improvements can also be achieved by the long side and the short side being made of different materials or combinations of materials. In some applications, the long side can have, for instance, an aluminum strip with high guiding capability and low friction whereas the short side can have a wood fiber strip. In other applications, the opposite is advantageous.
[0042] In some applications, there may also be a need for different types of strip on the same side. The side may consist of, for instance, a plurality of different strips which are made of different aluminum alloys, have different thicknesses etc. and in which certain parts are intended to achieve high strength and others are intended to be used for guiding.
[0043] Different aspects of the invention will now be described in more detail by way of examples with reference to the accompanying drawings. The parts of the inventive board which are equivalent to those of the prior-art board in. FIGS. 1-3 are provided with the same reference numerals.
DESCRIPTION OF THE DRAWINGS
[0044] FIGS. 1 a - c illustrate in three steps a downwards angling method for mechanical joining of long sides of floorboards according to WO 94/26999.
[0045] FIGS. 2 a - c illustrate in three steps a snap-in method for mechanical joining of short sides of floorboards according to WO 4/26999.
[0046] FIGS. 3 and 3 b show a floorboard according to WO 94/26999 seen from above and from below, respectively.
[0047] FIG. 4 shows a floorboard with a locking system according to a first embodiment of the invention.
[0048] FIG. 5 is a top plan view of a floorboard according to FIG. 4 .
[0049] FIG. 6 a shows on a larger scale a broken-away corner portion C 1 of the board in FIG. 5 , and
[0050] FIGS. 6 b and 6 c are vertical sections of the joint edges along the long side 4 a and the short side 5 a of the board in FIG. 5 , from which it is particularly evident that the long side and the short side different.
[0051] FIGS. 7 a - c show a downwards angling method for mechanical joining of long sides of the floorboard according to FIGS. 4-6 .
[0052] FIG. 8 shows two joined floorboards provided with a locking system according to a second embodiment of the invention.
[0053] FIG. 9 shows two joined floorboards provided with a locking system according to a third embodiment of the invention.
[0054] FIGS. 10-12 illustrate three different embodiments of floorboards according to the invention where the projecting portion is formed in one piece with the body of the board.
DESCRIPTION OF PREFERRED EMBODIMENTS
[0055] A first preferred embodiment of a floorboard 1 provided with a locking system according to the invention will now be described with reference to FIGS. 4-7 . The shown example also illustrates the aspect of the invention which concerns differently designed locking systems for long side and short side.
[0056] FIG. 4 is a cross-sectional view of a long side 4 a of the board 1 . The body of the board 1 consists of a core 30 of, for instance, wood fiber which supports a surface laminate 32 on its front side and a balance layer 34 on its rear side. The board body 30 - 34 is rectangular with long sides 4 a , 4 b and short sides 5 a , 5 b . A separate strip 6 with a formed locking element 8 is mounted at the factory on the body 30 - 34 , so that the strip 6 constitutes an integrated part of the completed floorboard 1 . In the shown example, the strip 6 is made of resilient aluminum sheet. As an illustrative, non-limiting example, the aluminum sheet can have a thickness in the order of 0.6 mm and the floorboard a thickness in the order of 7 mm. For further description of dimensions, possible materials, etc. for the strip 6 , reference is made to the above description of the prior-art board.
[0057] The strip 6 is formed with a locking element 8 , whose active locking surface 10 cooperates with a locking groove 14 in an opposite joint edge 4 b of an adjacent board 1 ′ for horizontal locking together of the boards 1 , 1 ′ transversely of the joint edge (D 2 ). With a view to forming a vertical lock in the D 1 direction, the joint edge 4 a has a laterally open groove 36 and the opposite joint edge 4 b has a laterally projecting tongue 38 (corresponding to the locking tongue 20 ), which in the joined state is received in the groove 36 ( FIG. 7 c ). The free surface of the upper part 40 of the groove 36 has a vertical upper portion 41 , a bevelled portion 42 and an upper abutment surface 43 for the tongue 38 . The free surface of the lower part 44 of the groove 36 has a lower abutment surface 45 for the tongue 38 , a bevelled portion 46 and a lower vertical portion 47 . The opposite joint edge 4 b (see FIG. 7 a ) has an upper vertical portion 48 , and the tongue 38 has an upper abutment surface 49 , an upper bevelled portion 50 , a lower bevelled portion 51 and a lower abutment surface 52 .
[0058] In the joined state ( FIG. 7 c ), the two juxtaposed vertical upper portions 41 and 48 define a vertical joint plane F. As is best seen from FIG. 4 , the lower part 44 of the groove 36 is extended a distance outside the joint plane F. The joint edge 4 a is in its underside formed with a continuous mounting groove 54 having a vertical lower gripping edge 56 and an inclined gripping edge 58 . The gripping edges formed of the surfaces 46 , 47 , 56 , 58 together define a fixing shoulder 60 for mechanical fixing of the strip 6 . The fixing is carried out according to the same principle as in the prior-art board and can be carried out by means of the methods that are described in the above-mentioned documents. A continuous lip 62 of the strip 6 thus is bent round the gripping edges 56 , 58 of the groove 54 , while a plurality of punched tongues 64 are bent round the surfaces 46 , 47 of the projecting portion 44 . The tongues 64 and the associated punched holes 65 are shown in the broken-out view in FIG. 6 a.
[0059] There is a significant difference between the inventive floorboard shown in FIGS. 4-7 and the prior-art board according to FIGS. 1-3 . The area P in FIG. 4 designates the portion of the board 1 which is positioned outside the joint plane 1 . According to the invention, the portion P has two horizontally juxtaposed parts P 1 and P 2 , which differ in respect of at least one of the parameters material composition and material properties. More specifically, the inner part P 1 is, closest to the joint plane F, formed partially of the strip 6 and partially of the worked part 44 of the body. In this embodiment, the inner part P 1 thus comprises the material combination aluminum+wood fiber core+rear laminate whereas the outer part P 2 is a made of aluminum only. In the prior-art board 1 in FIGS. 1 a - c , the corresponding portion outside the joint plane is made of aluminum only.
[0060] As described above, this feature means that the cost of material can be reduced. Thanks to the fact that the fixing shoulder 60 is displaced towards the locking element 8 to such an extent that it is positioned at least partially outside the joint plane F, a considerable saving can be achieved in respect of the consumption of aluminum sheet. A saving in the order of 25% is possible. This embodiment is particularly advantageous in cheaper floorboards where waste of wood fiber as a result of machining of the body is preferred to a high consumption of aluminum sheet. The waste of material, however, is limited thanks to the fact that the projecting portion can also be used as abutment surface for the tongue, which can then be made correspondingly narrower perpendicular to the joint plane with the ensuing reduced waste of material on the tongue side.
[0061] This constructional change to achieve saving in material does not have a detrimental effect on the possibility of resilient vertical motion that must exist in the projecting portion P. The strength of the locking element 8 is not affected either. The outer part P 2 of aluminum is still fully resilient in the vertical direction, and the short sides 5 a , 5 b can be snapped together according to the same principle as in FIGS. 2 a - c . The locking element 8 is still made of aluminum and its strength is not reduced. However, it may be noted that the degree of resilience can be affected since it is essentially only the outer part P 2 that is resilient in the snap action. This can be an advantage in some cases if one wants to restrict the bending-down properties and increase the strength of the lock.
[0062] The angling together of the long sides 4 a , 4 b can also be carried out according to the same principle as in FIGS. 1 a - c . In general—not only in this embodiment—a small degree of downwards bending of the strip 6 may occur, as shown in the laying sequence in FIGS. 7 a - c . This downwards bending of the strip 6 together with an inclination of the locking element 8 makes it possible for the boards 1 , 1 ′ to be angled down and up again with very tight joint edges at the upper surfaces 41 and 48 . The locking element 8 should preferably have a high guiding capability so that the boards, in connection with downwards angling, are pushed towards the joint edge. The locking element 8 should have a large guiding part. For optimal function, the boards should, after being joined and along their long sides 4 a , 4 b , be able to take a position where there is a small play between locking element and locking groove, which need not be greater than about 0.02-0.05 mm. This play permits displacement and bridges width tolerances. The friction in the joint should be low.
[0063] In the joined state according to FIG. 7 c , the boards 1 , 1 ′ are locked relative to each other in The vertical direction D 1 . An upwards movement of the board 1 ′ is counteracted by engagement between the surfaces 43 and 49 , while a downwards movement of the board 1 ′ is counteracted on the one hand by engagement between the surfaces 45 and 52 and, on the other hand, by the board 1 resting on the upper side of the strip 6 .
[0064] FIG. 8 shows a second embodiment of the invention. The board 1 in FIG. 8 can be used for parquet flooring. The board 1 consists of an upper wear layer 32 a , a core 30 and a rear balance layer 34 a . In this embodiment, the projecting portion P outside the joint plane F is to a still greater extent made of different combinations of materials. The locking groove 14 is reinforced by the use of a separate component 70 of, for instance, wood fiber, which in a suitable manner is connected with the joint edge, for instance by gluing. This variant can be used, for instance, on the short side 5 b of the board 1 . Moreover, a large part of the fixing shoulder 60 is positioned outside the joint F.
[0065] FIG. 9 shows a third embodiment of the invention. The board 1 in FIG. 9 is usable to provide a strong attachment of the aluminum strip 6 . In this embodiment, a separate part 72 is arranged on the joint edge supporting the locking element 8 . The part 72 can be made of, for instance, wood fiber. The entire fixing shoulder 60 and the entire strip 6 are located outside the joint plane F. Only a small part of the separate strip 6 is used for resilience. From the viewpoint of material, the portion P located outside the joint plane F has three different areas containing the combinations of materials “wood fiber only” (P 1 ), “wood fiber/balance layer/aluminum” (P 2 ) and “aluminum only” (P 3 ). This embodiment with the fixing shoulder 6 positioned entirely outside the joint plane F can also be accomplished merely by working the body of the board, i.e. without the separate part 72 . The embodiment in FIG. 9 can be suitable for the long side. The locking element 8 has a large guiding part, and the projecting portion P outside the joint plane F has a reduced bending down capability.
[0066] When comparing the embodiments in FIGS. 8 and 9 , it may be noted that in FIG. 9 the tongues 64 are higher than the lip 62 . This results in a strong attachment of the strip 6 in the front edge of the fixing shoulder 60 , which is advantageous when bending down the strip 6 . This can be achieved without any extra cost of material since the tongues 64 are punched from the existing material. On the other hand, the lip 62 can be made lower, which is advantageous in respect of on the one hand consumption of material and, on the other hand, the weakening effect of the mounting groove 54 on the joint edge. It should further be noted that the locking element 8 in FIG. 8 is lower, which facilitates the snapping in on the short sides.
[0067] FIGS. 10-12 show three different embodiments of the invention, in which the projecting portion can be made in one piece with the board body or consists of separate materials which are glued to the edge of the board and are machined from above. Separate materials are particularly suitable on the short side where strength and resilience requirements are high. Such an embodiment means that the composition of materials on the long side and the short side can be different.
[0068] The above technique of providing the edge of the body, on the long side and/or short sides with separate materials that are fixed to the body to achieve special functions, such as strength, moisture proofing, flexibility etc, can be used also without utilizing the principles of the invention. In other words, it is possible also in other joining systems, especially mechanical joining systems, to provide the body with separate materials in this way. In particular, this material can be applied as an edge portion, which in some suitable fashion is attached to the edge of the body and which can extend over the height of the entire board or parts thereof.
[0069] In a preferred embodiment, the edge portion is applied to the body before the body is provided with all outer layers, such as top layer and rear balance layer. Especially, such layers can then be applied on top of the fixed, separate edge portion, whereupon the latter can be subjected to working in respect of form with a view to forming part of the joining system, such as the projecting portion with locking element and/or the tongue with locking groove.
[0070] In FIGS. 10 and 11 , the board body is composed of a top laminate 32 , a wood fiber core 30 and a rear laminate 34 . The locking element 8 is formed by the projecting portion P being worked from above in such manner that, seen from the joint plane F outwards, it has an inner part P 1 consisting of wood fiber 30 and laminate 34 , a central part P 2 consisting of laminate 34 only, and an outer part P 3 consisting of wood fiber and laminate 34 .
[0071] The embodiments in FIGS. 10 and 11 differ from each other owing to the fact that in FIG. 10 the boundary between the wood fiber core 30 and the rear laminate 34 is on a vertical level with the lower edge of the active locking surface 10 . Thus, in FIG. 10 no significant working of the rear laminate 34 has taken place in the central part P 2 . On the other hand, in FIG. 11 also the rear laminate 34 has been worked in the central part P 2 , which gives the advantage that the active locking surface 10 of the locking element 8 is wholly or partly made of a harder material.
[0072] The embodiment in FIG. 12 differs from the embodiments in FIGS. 10 and 11 by an additional intermediate layer 33 being arranged between the wood fiber core 30 and the rear laminate 34 . The intermediate layer 33 should be relatively hard and strong to reinforce the active locking surface 10 as shown in FIG. 12 . For example, the immediate layer 33 can be made of a separate material which is glued to the inner core. Alternatively, the immediate layer 33 may constitute a part of, for instance, a particle board core, where chip material and binder have been specially adapted to the mechanical joining system. In this alternative, the core and the intermediate layer 33 can thus both be made of chip material, but with different properties. The layers can be optimized for the different functions of the locking system.
[0073] Moreover, the aspects of the invention including a separate strip can preferably be implemented in combination with the use of an equalizing groove of the type described in WO 94/26999. Adjacent joint edges are equalized in the thickness direction by working of the underside, so that the upper sides of the floorboards are flush when the boards are joined. Reference letter E in FIG. 1 a indicates that the body of the boards after such working has the same thickness in adjacent joint edges. The strip 6 is received in the groove and will thus be partly flush-mounted in the underside of the floor. A corresponding arrangement can thus be accomplished also in combination with the invention as shown in the drawings.
[0074] 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 locking system for mechanical joining of floorboards, each of the floorboards comprising a body comprising plywood with several layers; a locking groove which is formed in an underside of and extends in parallel with a first joint edge at a distance from the joint plane, the locking groove having an opening, a bottom, and two side walls; a portion projecting from a lower part of the second joint edge and below the first joint edge and integrated with the body of the board; said projecting portion supporting, at a distance from the joint plane, a locking element for cooperating with the locking groove; said projecting portion being located entirely outside the joint plane as seen from the side of the second joint edge; and the walls of the locking groove comprise at least two layers of the body.
| 4
|
RELATED APPLICATION
This application claims the benefit of U.S. provisional application Serial No. 60/159,618 filed Oct. 14, 1999, entitled Optical High Speed Bus and High Speed Modular Computer Backplane.
TECHNICAL FIELD OF THE INVENTION
This invention is related in general to light beam routing in a computer system, and more particularly, the invention is related to a high speed bus and high speed modular light beam routing for a computer.
BACKGROUND OF THE INVENTION
Most people familiar with computer-based systems know that the primary mechanism to transfer data from one circuit card to another and for interconnecting the circuit cards is the backplane. Also known as a motherboard, the backplane is typically a printed circuit board with a limited number of sockets into which circuit boards may be inserted. Typically, an interrupt-based bus protocol is used to arbitrate between contending circuit cards requiring access to the bus.
Such backplane-based system bus architectures suffer from several disadvantages. The bandwidth or speed of the system is limited. For example, conventional small PCI (peripheral component interconnect) bus systems run at a maximum aggregate bandwidth of 133 megabytes per second. The number of circuit cards that may be part of the system is also restricted to the number of available sockets on the backplane. The backplane itself also adds weight and size to the system. Many backplanes are also custom designed, thereby adding cost and time to the development cycle.
In order to fully interconnect all circuit cards in the system, a large full access switch is required. Current networking topologies that guarantee data delivery in real time, such as asynchronous transfer mode (ATM) switches, require large switching hubs. Further, in order to achieve large bandwidths, conventional systems use single coax or fiber optic cables to carry the data traffic. Each link also requires a dedicated network adaptor card.
A unique system application is for those systems that require a separation of secured or encrypted and unsecured or decrypted data. Conventional systems use complex networks of discrete filters to isolate the secured or encrypted data from the unsecured data. These discrete filters take up extra space and require elaborate tests to verify the isolation of the secured data. Further, the speed of the backplane is adversely impacted.
SUMMARY OF THE INVENTION
In accordance with the present invention there is provided a bus module providing mechanical, electrical, optical, and power interface for individual circuit cards and for network adaptability. Each bus module provides low latency interconnectivity between modules for data packet transfer, such as 32-bit word read and write. Interconnectability of the bus module provides near unrestricted expansion of a computer backplane.
Each bus module includes an optical interface—left and optical interface—right. Each interface comprises a two-dimensional N by N, for example 16×16, bi-directional array of VCSEL (vertical cavity surface emitting laser)/photodetector elements. Each bi-directional VCSEL/photodetector element functions to provide high speed data communication through interconnected adjacent bus modules from one module in the interconnection to any other module by means of a pre-programmed transfer path through VCSEL/photodetector elements arranged in a row by column matrix. This provides the advantage of a high-speed data transfer without the need for a header for each data packet. The interconnection of one circuit card to other circuit cards through the interconnected bus modules is along a fixed path known to both the transmitting circuit card and the receiving circuit card.
In accordance with the present invention VCSEL/photodetector element arrays pass data to each other over free space. Bus alignment is an important aspect of this interconnect technology that allows programmed interconnect schemes by establishing dedicated channels from bus module “m” to bus module “n”, where “m” and “n” are within the range of 2 to N. By establishing such dedicated data links switching data transfer is simplified. The number of modules “C” that can be interconnected is valid for all positive values of “C” and “m” satisfying the equation C(C−1)<2 m.
In accordance with the present invention, there is provided an optical data transfer network comprising at least one network backplane bus module having a global electrical bus, a local electrical bus, and an optical bus. A plurality of bi-directional optical/electrical converters coupled to the optical bus converts optical signals to electrical signals and vice versa. An optical link interface coupled between the local electrical bus and the bi-directional optical electrical converters routes data between the local electrical bus and the optical bus. A controller coupled to an optical link interface provides signals for controlling data routing between the local electrical bus, the global electrical bus and the optical bus.
BRIEF DESCRIPTION OF THE DRAWINGS
For a better understanding of the present invention, reference may be made to the accompanying drawings, where:
FIG. 1 is a block diagram of an embodiment of an interface module coupled between a secured bus module and an unsecured bus module according to the teachings of the present invention;
FIG. 2 is a block diagram of an embodiment of a portion of the bus module according to the teachings of the present invention;
FIG. 3 is a more detailed block diagram of an embodiment a portion of the bus module according to the teachings of the present invention;
FIG. 4 is a block diagram showing a representative layout of VCSEL/photodetector pairs according to the teachings of the present invention;
FIG. 5 is a diagram illustrating an exemplary network channel interconnection scheme using the VCSEL/photodetector matrix;
FIG. 6 is a block diagram of an embodiment of switch fabric according to the teachings of the present invention;
FIG. 7 is a block diagram of an embodiment of a full access switch of the switch fabric according to the teachings of the present invention;
FIG. 8 is a block diagram of an embodiment of a bus interface according to the teachings of the present invention;
FIG. 9 is a block diagram of an embodiment of a receive/transmit circuit according to the teachings of the present invention;
FIG. 10 is a perspective view of an embodiment of a high speed electrical and optical bus module according to the teachings of the present invention; and
FIG. 11 is a perspective view of an embodiment of a series of interconnected high speed electrical and optical bus modules according to the teachings of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 is a block diagram of an embodiment of a high speed modular backplane system 10 having at least one secured bus module 12 (system X) coupled to an interface module 14 (X/Y Interface), in turn coupled to at least one unsecured bus module 16 (system Y). Each module 12 , 14 and 16 is constructed according to the teachings of the present invention. The secured bus module 12 and the unsecured bus module 16 have separate and independent global electrical buses 18 and 20 , respectively, to isolate the sensitive confidential (secured) data from unsecured data. The interface bus module 14 does not have a global electrical bus. Each bus module 12 , 14 and 16 has a local electrical bus 22 coupled to a circuit card (not shown) plugged into the bus modules by means of a conventional circuit card connector. An optical bus 24 links the bus modules together. Secure data is transmitted and received on the optical bus 24 utilizing a different optical wavelength from the optical wavelength utilized for unsecured data to maintain data isolation. An optical link interface 26 , an electrical/optical converter 28 and optical/electrical converter 30 , in each module 12 , 14 and 16 serve as the interface between the local electrical bus 22 and the optical bus 24 in each bus module under the control of a controller central processing unit (CPU) 32 . A bus bridge 34 in the modules 12 and 16 is an optional bus data buffer. A bus module with a bus bridge 34 is used when there is more than a predetermined number of bus modules interconnected.
FIG. 2 is a block diagram of an embodiment of an optical link interface 26 in a bus module according to the teachings of the present invention. The optical link interface 26 includes a switch fabric slice 36 that performs signal routing between the optical bus 24 and the local electrical bus 22 . A data bus interface 38 is coupled to the switch fabric slice 36 as an interface between the optical bus 24 and the local electrical bus 22 .
Referring to FIG. 3 there is shown a more detailed block diagram of the switch fabric slice 36 and optical bus buffers of a bus module according to the teachings of the present invention. The switch fabric slice 36 includes a receive/transmit circuit 40 coupled to a switch fabric 42 . The electrical/optical converter 28 and optical/electrical converter 30 each connects to buffer 46 having a predetermined wavelength VCSEL/photodetector diode 44 outputting a light signal and a predetermined wavelength photodetector 48 receiving light for conversion to an electrical signal. To insure optical isolation for security, the module 14 of FIG. 1 includes two different predetermined wavelength VCSEL/photodetector diodes 44 for secure and unsecure outputting of light signals and two different predetermined wavelength photodetectors 48 receiving light for conversion to an electrical signal.
FIG. 4 is a matrix illustration showing a representative layout of VCSEL/photodetector according to the teachings of the present invention. The exemplary layout is in a row and column configuration where each rectangle represents a VCSEL/photodetector and detector pair. Although the illustration shows an eight-by-eight array, the typical application utilizes an M by M array of laser/detector pairs, where “M” is a positive number.
FIG. 5 is a diagram illustrating an exemplary network channel interconnection for four circuit cards using the VCSEL/photodetector matrix as illustrated in FIG. 4 . In this example, the VCSEL/photodetector diode and photodetector pair in column 1 , row 4 of card 1 is used to transmit data from circuit card 1 to circuit card 4 . Therefore, the switch matrices for circuit cards 1 through 4 are configured to receive data from the local electrical bus in circuit card 1 , transmit the data onto the optical bus in bus module 1 , repeat the received data to pass through bus modules 2 and 3 , and route the received data to the local electrical bus in circuit card 4 and then to circuit card 4 plugged into bus module 4 .
FIG. 6 is a block diagram of an embodiment of switch fabric 36 according to the teachings of the present invention. By way of example, the switch fabric 36 comprises 256 (m) electrical signal switches 50 each having a left input output connection to one of the optical/electrical converters 30 . The general relationship between “C” and “m” is given by the expression C(C−1)<2m, as stated earlier. Each of the electrical signal switches 50 also includes a right input output connection to one of the electrical/optical converters 28 as illustrated in FIGS. 2 and 3. Each of the switches 50 is programmable to pass an electrical signal received at a left connection through the switch and applied to a right connection or in the alternative, depending on the program, the receive signal is directed to a multiplexer 52 . The multiplexer 52 is configured to receive a signal from any one of the 256 switches 50 for multiplexing to 1 of 24 possible serial links connected to a circuit card coupled to one of the bus modules containing a fabric switch 36 .
As illustrated in FIG. 6, the switch fabric 36 is configured to receive an electrical input signal on any one of 256 input lines and to transmit the received electrical signal to one of 256 output lines, where both the input lines and output lines are individually connected to one of the 256 switches 50 . Each of the 256 switches 50 are coupled to an address decoder 54 through one of 256 address registers 56 . The address decoder 54 receives a slot number code from the controller CPU 32 to either pass the input signals to an output terminal or to pass an input signal to the multiplexer 52 . This pass-through function is illustrated in FIG. 5 and previously discussed.
Although the description of FIG. 6 to this point only discussed transmission of signals from the multiplexer 52 , the multiplexer is bi-directional and also receives signals from a circuit card, thus making the switch fabric slice 36 also bi-directional. A signal received at one of the 24 inputs to the multiplexer 52 is applied to each of the 256 switches 50 that are individually programmed to transmit a received signal either to the left or to the right, that is, to an adjacent switch fabric slice 36 or to terminate the received signal within the switch 50 . This operation enables transmission of a received signal to an adjacent circuit card coupled to an adjacent bus module in a manner as described with reference to FIG. 5, cards 2 and 3 .
FIG. 7 is a block diagram of an embodiment of an access switch 50 of the switch fabric 36 according to the teachings of the present invention. The blocks labeled A through F are two-position switches which are opened or closed under the control of a signal from switch register 56 on one of the lines A-F. Data to be passed through the switch fabric slice 36 on an optical bus is transmitted via closed switches E and F. Data to be sent to or received from the local electrical bus 22 are transmitted via switches A through D.
Referring to FIG. 8, there is shown a block diagram of an embodiment of a global electrical bus interface 34 according to the teachings of the present invention. The bus interface 34 includes a bus arbiter 60 , a field programmable gate array core 62 , and an interface circuit 64 . The bus arbiter 60 responds to data on the global electrical bus 18 or 20 (FIG. 1) to control the transfer of electrical data signals to adjacent bus modules. Electrical data signals on the global electrical bus 18 or 20 are also input to the field programmable gate array core 62 that functions to selectively format electrical data signals for transmission from a bus module. The bus arbiter 60 in combination with the gate array core 62 identifies when electrical data transmitted on the global electrical bus 18 or 20 is intended for the circuit card coupled to the bus module.
An output from the gate array core 62 is applied to the 24 by 1 interface 64 in accordance with the identified circuit card coupled to a particular bus module. Typically, the interface 64 is a multiplexer. Data output from the interface 64 is applied to the local electrical bus 22 , and if identified with the circuit card coupled to a particular bus module, then the data is transferred to the circuit card. If the electrical data on the local electrical bus 22 is to be transmitted on the optical bus 24 then the output of the interface 64 is routed through the optical link interface 26 .
The above description of the bus interface 34 is based on the assumption that data is received by the bus interface on the global electrical bus 18 or 20 . The bus interface 34 is bi-directional and is configured to also receive electrical data from a circuit card or electrical data from the optical link interface 26 , in either case for further transmission on the global electrical bus.
FIG. 9 is a block diagram of an embodiment of a receive/transmit circuit 40 according to the teachings of the present invention. The receive/transmit circuit 40 includes memory circuits 66 T or 66 R such as a FIFO (first-in-first-out) registers, a controller 68 , and an array of multiplexers 70 (MUXs). Each of the multiplexers 70 is connected to the full access switch 52 (see FIG. 6) and multiplexes the received inputs to the respective memory 66 T or 66 R. Each of the memories 66 in response to control signals from the controller 68 selects the input from the multiplexers coupled thereto for transmission to a circuit card connected to the bus module. The selected electrical data signal may also be coupled through the global electrical bus interface 34 to the global electrical bus 18 or 20 . The electrical bus 20 is also configured to receive electrical data from a circuit card or the global electrical bus 18 or 20 through the memory 66 R.
When receiving data, the receive/transmit circuit 40 distributes a signal from a memory 66 R to the multiplexers connected thereto for further transmission and processing by full access switch 52 . The memory 66 T receives electrical data from the full access switch 52 for transmission to a circuit card or for transmission over the global electrical bus 18 or 20 while the memory 66 R functions to receive electrical data from a circuit card by means of the global electrical bus 18 or 20 . Operation of the memory 66 T and the memory 66 R is in accordance with signals from the controller 68 .
FIG. 10 is a perspective view of an embodiment of a high speed electrical and optical bus module 72 according to the teachings of the present invention. The bus module 72 configured to enable interconnection of a plurality of bus modules to form a computer backplane. The bus module 72 includes slot 74 containing an electrical connector to provide coupling to a circuit card (not shown). Optical ports or windows 76 are provided to receive and transmit optical signals when assembled together with adjacent bus modules. Electrical connectors 78 are provided to interconnect the bus modules 72 to form a global electrical bus 20 . The bus modules also include alignment buttons 80 or other mechanical connectors to provide secure physical connections with an adjacent bus module. Thus each module is also provided with mating elements to receive the alignment buttons.
Referring to FIG. 11 there is shown a perspective view of a plurality of interconnected high speed electrical and optical bus modules 12 , 14 , 16 according to the teachings of the present invention. Also shown are circuit cards 82 plugged into the card slots 74 of the bus modules. The interface bus module 14 is shown disposed between secured bus modules 12 and unsecured bus modules 16 to maintain separation and confidentiality of secured data.
The invention is a modular computer backplane and a full access switched network. In particular, secured data is separated and isolated from unsecured data to ensure confidentiality. The invention is fully scalable due to its modularity.
Although several embodiments of the present invention and its advantages have been described in detail, it should be understood that changes, substitutions, modifications, variations, and alterations can be made without departing from the teachings of the present invention as set forth by the appended claims.
|
A modular optical data communication network operational as a computer backplane includes interconnectable bus modules providing both optical data transmission and electrical data transmission. Each bus module comprises and optical link interface having one input receiving data from an optical/electrical converter and a second terminal connected to receive electrical data from an electrical/optical converter. The bus modules are interconnectable by coupling an electrical/optical converter of one module to an optical/electrical converter of an adjacent module through a free-space connection. Each optical link interface includes a row by column VCSEL/photodetector array for dedicated path transmission of data over an optical network from a circuit card coupled to one bus module transmitting data to a circuit card of an adjacent or remote bus module.
| 7
|
PRIORITY CLAIM
This application is a divisional of U.S. application Ser. No. 09/616,865, filed Jul. 14, 2000 now abandoned, which was a continuation of international application number PCT/US00/01867 filed Jan. 17, 2000 which claims priority to 60/117,718 filed Jan. 28, 1999.
BACKGROUND OF THE INVENTION
Allogeneic bone marrow transplantation (BMT) provides a potentially curative treatment for leukemias that are refractory to conventional therapy. In addition to providing hematopoietic rescue from myeloablative therapy, BMT offers an adoptive immunotherapy effect (graft-versus-leukemia-GvL) that can be beneficial in the elimination of residual leukemia. This was initially shown in cases where T cell depletion (TCD) has been used to prevent graft-versus-host disease (GvHD) but also experienced an increase in disease relapse (1). Indeed, relapse rates in high-risk patients (long-standing recurrent disease or relapse at the time of BMT) can be as high as 70% (2). Therefore, further improvement in disease-free survival is likely to depend on the antileukemic effectiveness of the transplant, i.e. maximizing the GvL effect.
Most experimental evidence suggests that GvL effectors are predominantly T cells that can either recognize allospecific molecules expressed on both normal and neoplastic hematopoietic cells or recognize cell surface molecules that are either unique to or preferentially expressed by the leukemia (3–7). Identification of specific cell populations that are important antileukemic effectors is an essential first step to successful GvL graft engineering and cellular immunotherapy.
Although several studies have suggested that γδ+ T cells may not be important primary effectors of GvHD (8–12), few have addressed the GvL potential of γδ+ T cells. Esslin (13) noted that in vitro activated γδ+ T cells can mediate broadly-based non-MHC restricted cytolytic activity to selected human tumor cell lines. Others have shown that γδ+ T cells can recognize unprocessed peptides, some of which are preferentially expressed on tumor cells (14–18). Finally, one report has shown cytotoxic anti-leukemic activity in a patient against B cell ALL by γδ+ T cells expressing the Vδ1 form of the T cell receptor (19). Taken together, these findings support a potential antileukemic role for γδ+ T cells.
Published data describing a series of 10 leukemia patients who developed an increased proportion of circulating CD3+CD4−CD8−Vδ1+γδ+ T cells between 60 and 270 days post-BMT from a partially mismatched related donor (PMRD) which continued for up to two years. Eight of these patients are surviving and remain free of disease, as compared to a DFS probability of 31% at 2.5 years among 100-day survivors with a normal number of γδ+ T cells (20). In addition, it has been recently shown that enrichment of the graft with γδ+ T cells may have contributed to the later development of increased γδ+ T cells (21). Regardless of the TCD protocol used, however, patients who developed increased γδ+ T cells showed the same cell phenotype and cytolytic function as well as a decreased incidence of relapse.
Allogeneic Bone Marrow Transplantation and Graft-Host Interactions: High-dose chemo/radiotherapy followed by bone marrow rescue provides a potentially curative treatment for a variety of leukemias and solid tumors that are refractory to conventional therapy. An alloreactive response, mediated by donor immunocompetent cells in the graft and directed against normal cells and tissues in the recipient can result in the development of graft-versus-host disease (GvHD). GvHD can occur in up to 50% of patients receiving unmodified, HLA-identical marrow, indicating that minor histocompatibility differences, not detected by conventional HLA matching techniques, can initiate this reaction (22, 23). For the majority of patients (approximately 70% ) who do not have matched sibling donor (MSD) alternative donors may be used but the risk of acute GvHD is increased due to differences in major as will minor histocompatibility antigens (1). The same alloreactive response, however, can be beneficial in the elimination of residual leukemia through an adoptive immunotherapy mechanism known as the graftversus-leukemia (GvL effect).
Allogeneic BMT and the use of Alternative Donors: In most instances, the ideal bone marrow donor is the HLA-identical sibling. Alternative donors include the HLA-phenotypically matched unrelated donor (MUD), a partially mismatched related donor (PMRD) or a cord blood donor (CBD), who can be a phenotypically matched or mismatched related or unrelated donor (1).
Graft engineering, T cell depletion, and graft-host interactions: Initial attempts to use non-manipulated marrow from MUDs and PMRDs have resulted in severe or fatal GvHD (24, 25). This stimulated the development of methods to remove the suspected mediators of GvHD (T lymphocytes) from the marrow ex vivo prior to infusion (26). Results from transplants in which patients received marrow that was highly depleted of T cells (pan-T cell depletion) were initially promising, in that GvHD was significantly reduced; however, this was accompanied by an increase in graft failure (27, 28), suggesting that donor T cells may eliminate the ability of residual recipient T cells to reject the graft.
Animal studies of PMRD transplants have indicated that both CD4 and CD8-positive cells are capable of mediating lethal GvHD (29). Initial human studies have therefore used ex vivo pan-T cell depletion to engineer these grafts. This has either been achieved by agglutination with soybean lectin and rosetting the residual T cells with sheep red blood cells, or by use of T cell-directed MAbs, e.g. anti-CD2, CD3, CD5, in combination with panning or complement to eliminate antibody-sensitized cells (26). In a study comparing 470 PMRD reduced the risk of acute GvHD, but increased the risk of graft failure, and there was no overall improvement in leukemia-free survival (30). Therefore, aggressive ex vivo pan-TCD was felt not to be optimal in facilitating PMRD BMT, and subsequent studies have explored the use of a modified pan-T cell depletion that leaves more T cells in the graft. Another option is the use of a more selective or targeted type of TCD often combined with post-transplant immune suppression (11–13).
When T cell depletion (TCD) has been used in matched sibling transplantation, a further concern has been an increase in disease relapse seen particularly in patients with CML (33). This apparent disruption in the graft-versus-leukemia (GvL) effect has discouraged investigators from using TCD other than when MHC-nonidentical grafts are used. We have, however, shown that the use of sequential immunomodulation of the patient and T cell depletion of up to 3 Ag PMRD grafts can result in stable and sustained engraftment in >95% of recipients with a low incidence of acute and chronic GvHD (32). Relapse rates in high-risk patients (long-standing recurrent disease or relapse at the time of BMT) can be as high as 70% (2). This indicates that even though it is possible to cross major histocompatibility barriers with successful engraftment and a low incidence of GvHD, further improvement in disease-free survival will depend on the antileukemic effectiveness of the transplant. While this might be accomplished by performing the transplant earlier in the disease course, many patients will not be referred for allogenic BMT until they have demonstrated resistance to conventional-dose therap. Thus, enhancement of the GvL effect may be an essential component of the curative potential of allogeneic BMT.
Biology of the GvL Effect: The GvL reaction is thought to be most effective in chronic phase CML (34, 35), although there is also evidence for a GvL effect in the acute leukemias (36). It is generally thought that T lymphocytes recognize and eliminate residual leukemia through both MHC restricted and non-MHC restricted pathways (37). Targets for GvL include minor and/or major mismatched histocompatibility antigens and/or leukemia specific antigens. (38, 39). Every allogenic BMT patient potentially could benefit from the alloreactive response, although the extent of this benefit varies depending on whether the leukemia expresses allogenic antigens to a degree that triggers recognition and killing.
T cell recognition of leukemia-associated antigens is also thought to be a potentially important means by which immunocompetent cells may recognize and eliminate residual leukemia. It is known that leukemia-reactive clones can be generated (15). Specific targets for leukemia-reactive clones remain the topic of intense investigation, and some potential leukemia-associated antigens have been identified (3, 16–19) and are discussed below. The ability to identify and stimulate a GvL effect via either or both of these mechanisms may be of therapeutic importance in reducing the risk of relapse in patients who have received TCD grafts.
γδ+ T lymphocytes: Five to ten percent of T cells in normal peripheral blood bear the γδ receptor (42), although this number may be slightly higher in Asians and Blacks. Recent observations suggest that γδ+ T cells play a substantially different role in the immune system than that of αβ+ T cells. One of the most obvious differences is that most γδ+ T cells usually do not co-express CD4 or CD8, and therefore may develop normally in the absence of MHC class II molecules (43) since positive selection may not be required. Similarly, it is difficult to elicit a response of γδ+ T cells against allogeneic MHC class I or II antigens, and when it has been possible to obtain γδ+ T cell clones against peptide antigens, recognition of these peptides is usually not restricted by classical MHC molecules (44). In addition, γδ+ T cells tend to recognize intact rather than processed polypeptide (44).
While the requirements for activation of human γδ+ T cells are still poorly understood, it is clear that they are different from those of αβ+ T cells. γδ T cells do not require presentation of antigens in the context of the MHC Class I or Class II molecules for activation (45), however, they probably require CD28-mediated co-stimulation, and, following activation, show autocrine IL-2 production (46). They can also be activated by anti-CD2 antibodies (47). γδ+ T cells which express CD25 have also been shown to adhere to fibronectin-coated plates via the VLA-4 receptor with subsequent expansion, and cross linking of VLA-4 and VLA-5 receptors result in co-stimulated expansion induced by an anti pan-δ monoclonal antibody (48). Recent evidence has also suggested that certain subtypes of γδ+ T cells, predominantly the γδ+CD8αα+ homodimer population, may be resistant to Cyclosporin A (49).
Potential role of TCR-γδ+ T lymphocytes in allogenic BMT: While activation mechanisms for γδ+ T cells are just being elucidated, even less is known about the role of these cells in graft-host interactions. Ellison (50) reported an increase in peripheral γδ+ T cells in murine studies of acute GvHD following allogeneic non-TCD BMT (50). In that study, depletion of γδ+ T cells resulted in a significant decrease in GvHD-related mortality. Blazar (51) also has shown that murine γδ+ T cells can play a role in rejection, alloengraftment, and GvHD through recognition of the “nonclassical” MHC class Ib antigens.
Studies in humans have to this point been in conflict with murine studies. Norton (8) did not find γδ+ T cells to be effectors of epidermal damage in cutaneous GvHD. Viale (9) did note an increase in the ratio of Vδ1:Vδ2 cells in patients with acute GvHD but the significance of this finding remained undetermined. Tsuji (11) showed that although γδ+ T cells cannot produce GvHD on their own, host γδ+ T cells were recruited into donor αβ+ lesions where they were activated and induced to proliferate. Transitory increases in the ratio of CD4 − CD8 − γδ+ T cells have been reported during the first four weeks post-BMT in patients treated by GM-CSF, but the cells return to normal levels within eight weeks post-BMT (10). In addition, increased γδ+ T cells have been found in one (study to be associated with viral and fungal infections during the first year following TCD BMT in patients receiving either PMRD or MUD grafts (12). In the same study, increases in γδ+ T cells were not found to be associated with GvHD.
The potential for a possible anti-tumor role for γδ+ T cells was established by Esslin (13), who noted that in vitro activated peripheral blood γδ+ T cells posses cytolytic activity to selected human tumor cell lines when compared to similarly activated αβ+ T cells. This reactivity was not MHC restricted, but was dependent on interaction with LFA-1b/ICAM1 rather than the γδ receptor. These cells predominantly expressed the Vγ9/Vδ2 form of the T cell receptor. Proliferate responses of both αβ+ and γδ+ T cells, however, were inhibited by MAbs to anti-HLA-A, -B, and -C. These findings suggest that γδ+ T cells activated through the TCR have an advantage in non-MHC restricted cytolysis which may correlate with a GvL response. It is known that γδ+ T cells respond to heat shock proteins (16–18), some of which may be expressed by lymphomas. Human alloreactive γδ+ T cells have also been generated which recognize TCT.1 (Blast-1/CD48), an antigen broadly distributed on hematopoietic cells (52). These γδ+ T cells preferentially expressed the Vγ3/Vδ1 form of the T cell receptor. Vδ1+ cell activation has also been reported in response to EBV-transformed B cells (14, 53), EBV-infected Burkitt lymphoma cells (53), and Daudi lymphoma cells (54). In addition, one recent report has shown cytotoxic anti-leukemic activity in a patient against B cell ALL by γδ+ T cells expressing the Vδ1 form of the T cell receptor (19).
We have been able to expand in vitro donor-derived γδ T cells which have a striking resemblance to those seen in the patients described above. Donor mononuclear cells were depleted of CD4+/CD8+ T cells, and expanded on a combination of immobilized pan-δ monoclonal antibody and irradiated recipient B cell leukemia. After initial culture and re-stimulation, the cultures expanded rapidly and contained almost exclusively Vδ1+γδ+ T cells which expressed CD3, CD25, and CD69, but were CD4− and CD8− which are cytolytic to recipient leukemia and K562 cells but are minimally cytolytic to self MNC and third party leukemia. These observations suggest that donor-derived γδ+ T cells can be generated in vitro, thus providing a potential mechanism for cellular immunotherapy of leukemia.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 shows the expansion of donor γδ+ T cells in culture.
FIG. 2 shows the phenotypic analysis of proliferating γδ+ T cells from cultures on pan-δ MAb with blasts.
FIG. 3 shows the phenotypic analysis of proliferating γδ+ T cells from cultures on pan-δ MAb without blasts.
FIG. 4 shows the phenotype of γδ+ T cells from Patient #1.
FIG. 5 shows the flow cytometric binding assay depicting the binding of activated donor γδ+ T cells to recipient leukemic CD19+ blasts.
FIG. 6 shows the cytotoxicity of donor γδ+ T cells.
FIG. 7 shows the cytotoxicity of expanded γδ+ T cells against various cell lines.
FIG. 8 shows the cytotoxic effects of expanded γδ+ T cells against other cell lines.
FIG. 9 shows the mRNA and surface expression of Vδ subtypes.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Experimental Protocols
Donor/recipient pairs: Three patients who presented for BMT with relapsed acute lymphoblastic leukemia or induction failure and their HLA-partially mismatched related donors were enrolled in this study.
Cell preparation: For recipients, sufficient blood was drawn to obtain a minimum of 2.5×10 7 leukemic cells, but less than 50 ml, prior to the start of pre-BMT conditioning therapy. Leukemic cells from the recipient were separated from normal mononuclear cells (MNC) using density gradient centrifugation on Percoll using 30–40% gradient. If necessary, further purification was accomplished by immunomagnetic depletion of normal T and NK cells. Purity of normal and blast monolayers were evaluated by flow cytometry using MAbs previously found to be diagnostic for the patient's leukemia. The cells were then cryopreserved at a concentration of 20×10 6 /ml in AIM-5 medium (Gibco) with 15% fetal bovine serum (Gibco) and 10% DMSO and stored in liquid nitrogen until donor selection was complete. Up to 50 ml of peripheral blood was then obtained from the corresponding partially mismatched related donor. These donor-derived γδ+ T cells were purified in the MNC layer by negative selection using CD4+ and CD8+ immunomagnetic microspheres (Dynal) at a ratio of 5 microspheres:cell. Removal of CD4+ and CD8+ cells from peripheral blood effectively depleted >95% of αβ+ T cells. The number of γδ+ T cells in the preparation and the effectiveness of the αβ+ T cell depletion was monitored by flow cytometry as described below using fluorochrome-conjugated antibodies to TCR-αβ, TCR-γδ, CD4, CD8, and CD3 (Becton-Dickinson Immunocytometry Systems-BDIS; San Jose, Calif.).
Culture and activation of γδ+ T cells: Cytotoxic γδ+ T cells were generated from donor-recipient pairs as follows: Tissue culture-treated 24 well plates were coated with 10 μg TCR-δ1 pan-δ monoclonal antibody (Endogen; Woburn, Mass.) in 300 μg PBS for 24 h at 4° C. to facilitate initial activation and expansion of γδ+ T cells as described by Esslin (13). Irradiated (50 Gy) primary leukemic blasts that were obtained and cryopreserved prior to BMT were thawed, washed ×3, and re-suspended in AIM-5 Media with 15% FBS and 25 IU of IL-2 at a concentration of 1.0×10 6 cells/ml. Aliquots of 1 ml of this suspension were plated on the coated wells. Following immunomagnetic depletion of CD4+ and CD8+ cells as described above, remaining donor-derived MNC were adjusted to a concentration of 1.0×10 6 cells/ml, and aliquots of 1 ml were added to the previously plated recipient blasts. Control wells consisted of CD4+CD8+ depleted MNC plated on TCR-δ1 monoclonal antibody in the absence of blasts or blasts in the absence of monoclonal antibody. The cultures were examined daily for characteristic morphology of proliferating clusters. Media was refreshed twice weekly or as necessary dependent on the robustness of proliferation as determined by microscopic examination and the phenol red pH indicator in the media. After two weeks in culture, cells were photographed, and subcultured 1:2 or 1:4 as necessary onto a freshly coated plate. The γδ+ T cell + blast wells were restimulated with freshly thawed blasts at the same concentration used previously and assayed at this time and weekly thereafter for phenotype, Vδ subtype, and absolute cell number. At week four, fold expansion was calculated and harvesting was begun for phenotypic, molecular, and functional assays described below and for cryopreservation and storage as described above for future study. These assays were performed at 4–6 weeks of culture. The concentration of γδ+ T cells measured on a biweekly basis determined the degree of γδ+ T cell stimulation for each culture condition. When necessary, proliferating cells were transferred onto pan-δ MAb-coated tissue cultured flasks (Becton Dickinson) and cultures were maintained for up to twelve weeks, at which time no further proliferation was observed.
Flow cytometry: Expanded/activated γδ+ T cells were analyzed by four color flow cytometry for expression of CD45, CD3, CD4, CD8, CD19, CD56, CD25, HLA-DR, CD69 (Becton Dickinson Immunocytometry Systems; San Jose, CA-BDIS), and Vδ1 (Endogen, Woburn, Mass.), TCR-γδ, CD57, CD94, and Vδ1-Vδ3 (Coulter Immunotech; Miami, Fla.) using monoclonal antibodies conjugated with fluorescein isothiocyanate (FITC), phycoerythrin (PE), peridinin chlorophyll protein (PerCP), or allophycocyanan (APC). Recipient primary B cell leukemias were analyzed for expression of CD19, CD10, CD45, CD7, CD20, CD23, sIgGκ, sIgGλ, HLA-ABC, and HLA-DR (all from BDIS). At least 50,000 ungated events were collected in a list mode file and cell subpopulations in the lymphocyte CD45/side scatter gate and CD3/side scatter gate are quantitated and expressed as a percentage of the total lymphocyte population. Analysis was performed on a FACS Calibur flow cytometer using CellQuest software (BDIS).
Flow cytometric binding assays. Binding of donor γδ+ T cells to specific targets was examined by flow cytometry. Donor γδ+ T cells were incubated in AIM-5 Media with 15% FBS for 30 minutes at 37° C., centrifuged, and resuspended in phosphate-buffered saline. The cell suspension was labeled with one MAb specific for the leukemia but not expressed on γδ+ T cells (CD19) and anti-TCR γδ, which is not expressed on the leukemia. The cell preparation was incubated at 4° C. for 30 min, washed ×3, and analyzed by flow cytometry as detailed above. Clusters which were positive for both CD19 and γδ were then examined for forward (FSC) and side scatter (SSC) to determine if the represented multi-cell clusters. Dual-positive cells with increased FSC and SSC were scored as bound blast/γδ+ T cell clusters. Controls consisted of cultures of resting and activated donor γδ+ T cells co-cultured K562 cells. K562 cells are autofluorescent, so labeling with a flurochrome was unnecessary. Resting γδ+ T cells do not bind K562 while activated γδ+ T cells do.
Cytotoxicity assays: Third-party mononuclear cells, K562 erythroleukemia cells, and recipient primary leukemia were used as targets. Aliquots of target cells were labeled overnight with 3,3′-dioctadecyloxacarbocyanine (DiOC 18 ) (Molecular Probes, Eugene, Oreg.). The cells were then washed in phosphate buffered saline (PBS) and resuspended in RPMI-1640 with 10% fetal bovine serum (FBS) at a concentration of 2×10 4 cells/mi. Control MNC and expanded γδ+ T cells were suspended in RPMI-1640 and diluted to yield E:T ratios of 40:1–2.5:1 and added to the target cells. Aliquots of 130 μl counterstaining solution consisting of propidium iodine (PI) and PBS (Molecular Probes) were then added to the cell mixtures. The tubes were pelleted by centrifugation at 1000×g for 30 sec and then incubated for 4 hours. Following incubation, the tubes were acquired in a FACS Calibur flow cytometer (BDIS) and analyzed for green fluorescence (DiOC 18 -560 nm) and red fluorescence (PI-630 nm). Analysis on a two parameter histogram allows separation of live target cells (DiOC 18 +PI−) and membrane-compromised targets are (DiOC 18 +PI+) from which % cytotoxicity was calculated.
γδ T cell Receptor Characterization: The clonal heterogeneity of γδ+ T cells determined by flow cytometry was further evaluated using molecular approaches to assess γδ TCR variable gene expression using peripheral blood mononuclear cells (PBMC) collected from the BMT donors and the expanded γδ+ T cells from derived from culture on the pan-δ MAb and co-culture with the recipient ALL. Total RNA was extracted from MNC or cultured cells by the acid-phenol guanidinium thiocyanate method (55) and reverse transcribed according to the GeneAmp RNA PCR protocol (Perkin-Elmer Cetus, Norwalk, Conn.). The cDNA product served as template for PCR amplifications utilizing γδ TCR gene family-specific primers according to established methods (56). PCR amplification products were analyzed by agarose gel electrophoresis in order to determine the number and identity of γδ TCR V gene families expressed in each sample. This analysis was facilitated by DNA blot hybridization with corresponding TCR Cγ- or Cδ-horseradish peroxidase (HRP) conjugated oligonucleotide probes followed by chemiluminescent detection (23). Amplified products were resolved on 4% sequencing gels and detected, due to the incorporation of fluorescent primers during amplification, using the Hitachi FMBIO-100 Fluorescent Imager or the ABI 377 (Perkin-Elmer) automated sequencer using Genescan™ software. This method (known as TCR spectratyping) provides a more refined assessment of γδ TCR clonal diversity in the specimens.
Results
Immobilized pan-δ MAb alone and with and leukemic blasts stimulate γδ+ T cells. As shown in FIG. 1 , γδ+ T cells strongly proliferated in response to immobilized pan-δ MAb alone and a combination of immobilized pan-δ MAb and blasts. Leukemic blasts alone did not support sustained proliferation of γδ+ T cells. It should be noted, however, that in one experiment γδ+ T cell proliferation occurred later in the culture than in the other two experiments. Immunophenotypic analysis of proliferating γδ+ T cell cultures. Phenotypic analysis revealed that proliferating γδ+ T cells from cultures on pan-δ MAb with blasts preferentially expressed Vδ1 ( FIG. 2 ) while γδ+ T cells proliferating on pan-δ MAb without blasts preferentially expressed Vδ2 ( FIG. 3 ). The γδ+ T cell cultures were predominantly CD3+CD4−CD8− and expressed activation-associated antigens CD69, CD25, and HLA-DR regardless of culture conditions ( FIG. 4 ). Functional analysis of γδ+ T cell cultures. Cultured donor-derived γδ+ T cells from both culture methods were tested for their ability to bind and to lyse primary leukemia from the corresponding BMT recipient. FIG. 5 shows that indeed donor γδ+ T cells will bind recipient leukemia. Donor γδ+ T cells were highly cytotoxic to recipient leukemia as well as the NK sensitive target cell line K562 ( FIG. 6 ). In one experiment, mild nonspecific cytotoxicity was seen against third party MNC. Different lytic profiles were seen which correlated with culture method and predominant Vδ gene usage ( FIGS. 7 & 8 ). Vδ1+ cells cultured on immobilized pan-δ MAb and recipient blasts lysed primary ALL from the recipient and K562 cells as well as lymphoid cell lines, but had essentially no activity against myeloid cell lines. In contrast, Vδ2 clones from cultures expanded on pan-δ MAb alone showed cytotoxic activity against all targets. TCR repertoire analysis of γδ+ T cells. Polyclonal γδ+ T cells from the healthy BMT donors expressed mRNA predominantly for Vδ2 followed by Vδ1 and the Vδ3 ( FIG. 9 ). Occasionally mRNA for Vδ4 and Vδ5 was seen. Examination of the Vδ repertoire of γδ cells cultured on pan-δ MAb alone was essentially unchanged from the peripheral blood Vδ repertoire. In contrast, γδ+ T cells cultured on pan-δ MAb and blasts showed preferential expression of Vδ1, followed by Vδ2 and Vδ3. High resolution analysis of these PCR products revealed.
It will be apparent to those of ordinary skill in the art that many modifications and substitutions can be made without departing from the spirit and the scope of the present invention.
REFERENCES
1. O'Reilly R J, Hansen J A, Kurtzberg J, Henslee-Downey P J, Martelli M, Aversa F., Allogeneic marrow transplantation: approaches for the patient lacking a donor. In Schecter, G. P., and McArthur, J. R. (eds), Hematology 1996: Education Program for the American Society of Hematology, 132–46.
2. Henslee-Downey P J, Abhyankar S H, Parrish R S, Pati A R, Godder K T, Neglia W J, Goon-Johnson K S, Geier S S, Lee C G, Gee A P. Use of partially mismatched related donors extends access to allogeneic marrow transplant. Blood 89 (10):3864, 1997.
3. Horowitz, M. M., Gale, R. P., Sondel, P. M., Goldman, J. M. et al. Graft versus leukemia reactions after bone marrow transplantation. Blood 75, 555, 1990.
4. Henslee, P. J., Thompson, J. S., Romond, E. H., Doukas, M. A. et al. T cell depletion of HLA and haploidentical marrow reduces graft-versus-host disease but it may impair a graft-versus-leukemia effect. Transpin. Proc. 19, 2701, 1987.
5. Sykes, M., Romick, M. L., Sachs, D. H. Interleukin 2 prevents graft-versus-host disease while preserving the graft-versus-leukemia effect of allogeneic T cells. Proc. Nat. Acad. Sci. 1990; 87: 5633.
6. Truitt, R. L., Atasoylu, A. A. Contribution of CD4+ and CD8+ T cells to graft-versus-host disease and the graft-versus-leukemia reactivity after transplantation of MHC compatible bone marrow Bone Marrow Transplantation 1991; 8:51.
7. Weiss, L., Lubin, I., Factorowich, I., Lapidot, Z., Reich, S., Reisner, Y., Slavin, S. Effective the graft-versus-leukemia effects independent of graft-versus-host disease after T cell depleted allogeneic bone marrow transplantation in a murine model of B cell leukemia/lymphoma. J. Immunol. 1994; 153: 2562.
8. Norton J, Al-Saffar N, Sloane J P. An immunohistological study of lymphocytes in human cutaneous graft-versus-host disease. Bone Marrow Transplantation 7:205, 1991.
9. Viale M, Ferrini S, Bacigalupo A. TCR positive lymphocytes after allogeneic bone marrow transplantation. Bone Marrow Transplantation 10:249, 1992.
10. Yabe M, Yabe H, Hattori K, Hinorhars T, Morimoto T, Kato S, Kusonoki A. Transition of T-cell receptor gamma/delta expressing double negative (CD4/CD8) lymphocytes after allogeneic bone marrow transplantation. Bone Marrow Transplantation 14:741,1994.
11. Tsuji S, Char D, Bucy R P, Simonsen M, Chen C, Cooper M D. +T-cells are secondary participants in acute graft-versus-host reactions initiated by CD4+ T-cells. European Journal of Immunology 26: 420, 1996.
12. Cela M E, Holliday M S, Rooney C M, Richardson S, Alexander B, Krance R A, Brenner M K, Heslop H E. +T-lymphocyte regeneration after T-lymphocyte-depleted bone marrow transplantation from mismatched family members or matched unrelated donors. Bone Marrow Transplantation 17:243, 1996.
13. Esslin A, Formby B. Comparison of cytolytic and proliferative activities of human and T-cells from peripheral blood against various human tumor cell lines. Journal of the National Cancer Institute 83:1564, 1994.
14. Orsini D L, VanGils M, Kooy Y M C, Struyk L, Klein G, van den Elsen P, Koning F. Functional and molecular characterization of B-cell-responsive V 1+ T-cells. European Journal of Immunology 24:3199, 1994.
15. Hoffman, T., Theobald, M., Bunjes, D., Weiss, M., Heimpel, H., Heidt, W. Frequency of bone marrow T cells responding to HLA-identical nonleukemic and leukemic stimulator cells. Bone Marrow Transplantation 1993; 12: 1.
16. Fisch, P., Malkovska, M., Braakman, E., Sturm, E., Bolhuis, R. L., Prieve, A., Sosman, J. A., Lam, V. A., Sondel, P. M. Gamma/delta T cell clones and natural killer cell clones mediate distinct patterns of non-major histocompatibility-restricted cytolysis. J. Exp. Med. 1990; 171: 1567.
17. Kaur, I., Voss, S. D., Gupta, R. S., Schell, K., Fisch, P., Sondel, P. M. Human peripheral gamma/delta T cells recognize hsp60 molecules on Daudi Burkitt's lymphoma cells. J. Immunol. 1993; 150: 2046.
18. Battistini, L., Salvetti, M., Falcone, B., Raine, C. S., Brosnan, C. F. Gamma delta T cell receptor analysis supports a role for HSP 70 selection of lymphocytes in multiple sclerosis lesions. Mol. Med. 1995; 1: 554.
19. Potential antileukemic effect of gamma delta T cells in acute lymphoblastic leukemia. Leukemia 1995: 9: 863.
20. Lamb L S, Henslee-Downey P J, Parrish R S, Godder K T, Thompson J, Lee C, Gee A P. Increased frequency of TCR- +T-cells in disease-free survivors following T-cell depleted partially mismatched bone marrow transplantation for leukemia. Journal of Hematotherapy 5:503, 1996.
21. Lamb, L. S., Gee, A., Hazlett, L, Musk, P., Parrish, R. S., O'Hanlon, T. P., Geier, S., Folk, R. S., Harris, W. G., McPherson, K., Lee, C., Henslee-Downey, P. J. Influence of T cell depletion method on circulating γδ+ T cell reconstitution and potential role in the graft-versus-leukemia effect Cytotherapy (in press).
22. Anasetti, C., Amos, D., Beatty, P G., Appelbaum, F. R. et al. Effect of HLA compatibility on engraftment of bone marrow transplants in patients with leukemia or lymphoma. New Engl. J. Med. 1989; 320: 197.
23. Anasetti, C., Beatty, P. G. Storb, R., Martin, P. J. et al. Effect of HLA incompatibility on graft-versus-host disease, relapse and survival after marrow transplantation for patients with leukemia or lymphoma. Human Immunol. 1990; 29: 79.
24. Beatty, P. G., Clift, R. A., Mickelson, E. M., Nisperos, B. B. Flournoy, N., Martin, P. J., Sanders, J. E., Stewart, P., Buckner, C. D., Storb, R., Thomas, E. D., Hansen, J. Marrow transplantation from related donors other than HLA-identical siblings. New. Engl. J. Med. 1985; 313: 765.
25. Gajewski, J., Ceka, M., Champlin, R. Bone marrow transplantation utilizing HLA-matched unrelated donors. Blood Reviews 1990; 4: 132.
26. Frame, J. N., Collins, N. H., Cartagena, T., Waldmann, H., O'Reilly, R., Dupont, B. & Kernan, N. A. T cell depletion of human bone marrow: comparison of Campath I plus complement, anti-T cell a-chain immunotoxin, and soybean agglutinin alone or in combination with sheep erythrocytes or immunomagnetic beads. Transplantation, 1989; 47: 984.
27. Kernan, N. A., Bordignon, C., Heller, G., Cunningham, I. et al. Graft failure after T cell depleted human leukocyte antigen identical marrow transplants for leukemia. Blood 1989; 74: 2227.
28. Martin, P. J., Hansen, J. A., Torok-Storb, B., Durnam, D. et al: Graft failure in patients receiving T cell depleted HLA-identical allogeneic marrow transplants. Bone Marrow Transplantation 1988; 3: 445.
29. Korngold, R. and Sprent, J. T cell subsets and graft-versus-host disease. Transpln Proc. 44, 335,1987.
30. Ash, R. C., Horowitz, M. M., Gale, R. P., van Bekkum, J. T. et al. Bone marrow transplantation from related donors other than HLA-identical siblings: effect of T cell depletion. Bone Marrow Transplantation 7, 441, 1991.
31. Henslee-Downey, P. J., Parrish, R., MacDonald, J. S., Romond, E. H., Marciniack, E., Coffey, C., Ciocci, G., Thompson, Jr. Combined in vitro and in vivo T lymphocyte depletion for the control of graft-versus-host disease following haploidentical marrow transplant. Transplantation 1886; 61; 738.
32. Lee, C., Henslee-Downey, P. J., Brouilette, M., Pati, A. R., Godder, K., Abhyankar, S. H., Gee, A. P. Comparison of OKT-3 and T10B9 for ex vivo T cell depletion of partially mismatched related donor bone marrow transplantation. Blood 1996; 86: 625a.
33. Goldman, J. M., Gale, R. P., Horowitz, M. M., Biggs, J. C., Champlin, R. E., Gluckman, E., Hoffman, R. G., Jacobsen, S. J., Marmot, A., M., McGlave, P. B., Messner, H. A., Rimm, A., A., Rozman, C., Speck, B., Tura, S., Weinger, R. S. & Bortin, M. M. Bone marrow transplantation for chronic myelogenous leukemia in chronic phase: Increased risk for relapse associated with T-cell depletion. Ann Int Med, 1988; 108; 806.
34. Hesner, M. J., Endean, D., Caspter, J. T., Horowitz, M. M., Keever-Taylor, C. A., Roth, M., Flomenberg, N., Drobyski, W. R. Use of unrelated marrow grafts compensates for reduced graft-versus-leukemia reactivity after T cell depleted allogeneic marrow transplantation for chronic myelogenous leukemia Blood 1995; 86: 3987.
35. Kolb, H. J., Schattenberg, A., Goldman, J. M., Hertenstein, B., Jacobsen, N., Arcese, W., Ljungman, P., Ferrant, A., Verdonck, L., Neiderweiser, D., van Rhee, F., Mittermueller, J., de Witte, T., Holler, E., Ansari, H. Graft-versus-leukemia effect of donor lymphocyte transfusions in marrow grafted patients. Blood 1995; 86: 2041.
36. Slavin, S., Naparstek, E., Nagler, A., Ackerstein, A., Kapelushnik, J., Or, R. Allogeneic cell therapy for relapsed leukemia after bone marrow transplantation with donor peripheral blood lymphocytes. Exp. Hematol. 1995; 23: 1553.
37. Antin, J. H. Graft-versus-leukemia: no longer an epiphenomenon. Blood 1993; 82: 2273.
38. Barrett, A. J. Strategies to enhance the graft-versus-malignancy effect in allogeneic transplants. Ann NY Acad Sci 1996; XX: 203.
39. Truitt, R. L., Johnson, B. D. Principles of graft-versus-leukemia reactivity. Biol of Blood and Marrow Transplantation 1995; 1: 61.
40. Datta, A. R., Barrett, A. J., Jiang, Y. Z., Guimaraes, A., Mavroudis, D. A., van Rhee, F., Gordon, A. A., Madrigal, A. Distinct T cell populations distinguish chronic myeloid leukemia cells from lymphocytes in the same individual: a model for separating GvHD from GVL reactions. Bone Marrow Transplantation 1994; 14: 517.
41. Champlin, R. Separation of graft-versus-host disease and graftversus-leukemia effect against chronic myelogenous leukemia. Exp. Hematol. 1995; 23: 1148.
42. Raulet, D. H. The structure, function, and molecular genetics of the γ/δ cell receptor. Ann. Rev. Immunol., 1989; 7: 175.
43. Bigby, M., Markowitz, J. M., Bleicher, P. A., Grusby, M. J., Simha, S., Siebrecht, M., Wagner, M., Nagler-Anderson, C., Glimcher, L. H. most γδ T cells develop normally in the absence of MHC class II antigens. J. Immunol. 1993; 151: 4465.
44. Lanier, L. Unusual lymphocytes-γδ T cells and NK cells. The Immunologist 1995; 3; 182.
45. Schild, H., Mavaddat, N., Litzenberger, C., Ehrlich, E. W., Davis, M. M., Bluestone, J. A., Matis, L., Draper, R. K. Chien, y. The nature of major histocompatibility complex recognition by γδ+ T cells. Cell 1994; 76: 29.
46. Sperling, A. I., Linsley, P. S., Barrett, T. A., Bluestone, J. A. CD-28 mediated costimulation is necessary for the activation of T cell receptor-γδ+ T lymphocytes. J. Immunol. 1993; 151: 6043.
47. Wesselborg, S., Janssen, O., Pechhold, K., Kabelitz, D. Selective activation of γδ+ T cells by single anti-CD2 antibodies. J. Exp. Med. 1991; 173: 297.
48. Avdalovic, M., Fong, D., Formby, B. Adhesion and costimulation of proliferative responses of human γδ T cells by interaction of VLA-4 and VLA-5 with fibronectin. Immunol Lett. 1993; 35: 101.
49. Lin, T., Matsuzaki, G., Umesue, M., Omoto, K., Yoshida, H., Harada, M., Singaram, C., Hiromatsu, K., Nomoto, K. Development of γδ CD4-CD8+αα but not TCR-αβ CD4−CD8+αα i-IEL is resistant to cyclosporin A. J. Immunol. 1995; 155: 4224.
50. Ellison, C. A., MacDonald, G. C., Rector, E. S., Gartner, J. G. γδ T cells in the pathobiology of murine acute graft-versus-host disease. J. Immunol. 1995; 155: 4189.
51. Blazar, B. R., Taylor, P. A. Bluestone, J. A., Vallera, D. A. Murine γδ-expressing T cells affect alloengraftment via the reconognition of nonclassical major histocompatibility complex class Ib antigens. Blood 1996; 87: 4463.
52. Chouaib, F., Porto, P., Delorme, D., Hercend, T. Further evidence for a g/d T cell receptor-mediated TCT.1/CD48 recognition. J. Immunol. 147: 2864; 1991.
53. Hacker, G., Kromer, S., Falk, M., Heeg, K., Wagner, H., Pfeffer, K. Vδ1+ subset of human γδ T cells responds to ligands expressed by EBV-infected Burkitt lymphoma cells and transformed B lymphocytes. J. Immunol. 149: 3984; 1992.
54. Marx. S., Wesch, D., Kabelitz, D. Activation of humn γδ T cells by Mycobacterium tuberculosis and Daudi lymphoma cells. J. Immunol. 158: 2842; 1997.
55. Chomczynski P, Sacchi N. Single-step method of RNA isolation by guanidinium thiocyanate-phenol-chloroform extraction. Anal. Biochem. 1987; 162:156.
56. O'Hanlon, T. P., Messersmith, W., Dalakas, M. C., Plotz, P. H., and Miller, F. W. T Cell Receptor Gene Expression by Muscle-Infiltrating Lymphocytes in Idiopathic Inflammatory Myopathies. Clin. Exp. Immunol. 1995; 100: 519.
|
Patients who develop increased numbers of γδ+ cytotoxic T lymphocytes 2–6 months after allogeneic bone marrow transplantation are less likely to relapse than those who do not. The γδ+ T cells isolated from blood of patients with increased γδ+ T cells are CD3+CD4−CD8−CD57+, cytolytic to K562 cells, and express the Vδ1 T cell receptor phenotype. Similar γδ+ T cells can be generated in vitro by culture of donor mononuclear cells which are enriched for γδ+ T cells by immunomagnetic depletion of depleted of CD4+ and CD8+ cells. This γδ-enriched cell preparation was cultured on a combination of immobilized pan-δ monoclonal antibody and irradiated recipient B cell leukemia. After four weeks, the cultures were almost exclusively Vδ1+CD3+CD4−CD8− cells that co-expressed activation-associated antigens CD69, CD25, and HLA-DR. Furthermore, they were cytolytic against the primary leukemia obtained from the recipient and lymphoblastic leukemia cell lines, yet had minimal cytotoxicity against normal donor-derived mononuclear cells or myeloid leulemia cell lines. These observations suggest that donor-derived cytotoxic γδ+ T cells can be generated in vitro, and may provide therapeutic potential for prevention of disease relapse.
| 0
|
RELATED APPLICATIONS
[0001] This application is a divisional patent application which claims the benefit of the filing date of U.S. patent application Ser. No. 11/228,594, filed Sep. 16, 2005, the disclosure of which is incorporated herein by reference in its entirety.
TECHNICAL FIELD
[0002] The subject matter disclosed herein relates generally to pin apparatuses and methods. More particularly, the subject matter disclosed herein relates to pin apparatuses and methods having particular suitability for use with a machine handle, such as a machine handle of a walk-behind machine such as a lawnmower.
BACKGROUND ART
[0003] Conventional technology used to adjust a handle of a walk-behind machine such as a lawnmower to adjust into different positions utilizes bolts, and sometimes knobs, typically tightened by hand. In light of the trend for walk-behind machines such as lawnmowers to be assembled and set up by customers rather than by dealers, it is desirable for the machines to be designed to provide for easy setup out of the box with virtually no required assembly. Since walk-behind machines such as lawnmowers are now many times being sold to customers that take them home in the box as shipped, an even greater need for easy handle setup and adjustability built into the same mechanism is desirable.
[0004] A variety of apparatuses and methods exist in the prior art for use with handles or handle components. U.S. Pat. No. 6,546,596 to Grote et al. disclose an extension pole for tools and teaches a locking pin housing which is tubular and which extends from a sleeve 36 . A locking pin 42 and a retainer spring 44 are contained within the locking pin housing 40 . Holes are defined in the floor of an extension tube keyway 20 , and the distal end 50 of the locking pin 42 is adapted for selectively engaging any of the holes. In this manner, the locking pin 42 can be biased or urged by spring 44 to extend into a latched position with at least a portion of the distal end engaging one of the holes.
[0005] U.S. Pat. No. 3,702,016 to Keesee discloses a handle unit for a lawnmower comprising locking pins 41 which are adapted to enter openings 39 and the aligned opening 38 to lock an upper handle member 34 in selected vertical positions relative to a lower handle member 22 . A compression spring 44 surrounds each locking pin 41 between a lateral flange 42 and a spring abutment 46 in order for the locking pin 41 to be urged inwardly toward the opening 38 .
[0006] U.S. Pat. No. 3,816,873 to Thorud et al. discloses a folding handle and latch assembly latch pins 25 which protrude through lower legs 15 and through aligned holes 26 in the upper lapping portion of upper legs 22 in order to maintain alignment of upper legs 22 with lower legs 15 . A spring-wire handle 27 is disclosed and passes through the inner end of the each of latch pins 25 . Each spring-wire handle 27 includes a transverse bend at a lower end which passes outwardly through the lower legs and is secured by retaining clips 28 .
[0007] U.S. Pat. No. 4,243,342 to Marto discloses a fastener assembly for connecting an attachment to a frame. The fastener includes a pin holder, a latched pin and a torsion spring.
[0008] U.S. Pat. No. 3,694,855 to Meyer et al. discloses an adjustable handle for lawnmowers. A locking cam 20 along with other, related structure is utilized with an elongated tie rod 15 passing though holes in handle components 9 and 10 such that locking can 20 can be used to quickly lock and unlock the folded and unfolded positions of handle components 9 and 10 .
[0009] U.S. Pat. No. 3,649,997 to Thorud discloses a folding handle latch utilizing an elongate latch pin 27 adapted for moving between openings defined through two spaced-apart, tubular handle components. A latch handle 28 can be formed of an integral length spring wire or rod and can attach at one end to one of the tubular components and at the other end to an end of latch pin 27 .
[0010] Despite the existence of the prior art such as that described above, much room for improvement exists for pin apparatuses and methods such as that having particular use with machine handles associated with walk-behind machines such as lawnmowers.
SUMMARY
[0011] In accordance with the subject matter disclosed herein, novel pin apparatuses and methods are disclosed. While the pin apparatuses and methods can be adapted for any suitable use, the pin apparatuses and methods have particular use with machine handles such as those associated with walk-behind machines such as lawnmowers. A pin apparatus according to the disclosure herein can comprise a housing defining an opening for receiving at least a portion of a pin. A pin can be provided having an elongated pin body with a proximal end section and a distal end section. The pin body can be adapted for positioning at least partially through the opening of the housing where the pin is movable with respect to the housing according to a method disclosed herein from an extended position where at least a portion of the distal end section extends to a predetermined extent outside of the opening, and a retracted position where the distal end section is in a retracted position from the predetermined extent. A handle can be provided external from the housing for moving the pin whereby movement of the handle moves the pin between the extended position and the retracted position.
[0012] It is therefore an object of the present disclosure to provide novel pin apparatuses and methods having particular suitability for use with a machine handle of a walk-behind machine, such as, for example, a lawnmower.
[0013] An objecting having been stated hereinabove, and which is achieved in whole or in part by the subject matter disclosed herein, other objects will become evident as the description proceeds when taken in connection with the accompanying drawings as best described hereinbelow.
[0014] It is an object of the presently disclosed subject matter to provide _.
[0015] An object of the presently disclosed subject matter having been stated hereinabove, and which is achieved in whole or in part by the presently disclosed subject matter, other objects will become evident as the description proceeds when taken in connection with the accompanying drawings as best described hereinbelow.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 of the drawings is an exploded view of a pin apparatus with a machine handle and a positioning plate according to the present disclosure;
[0017] FIG. 2 a of the drawings is an isolated, perspective view of the pin body from the pin apparatus of FIG. 1 , and FIGS. 2 b and 2 c are top and bottom end views, respectively, of the pin body;
[0018] FIG. 3 a of the drawings is an isolated, perspective view of the housing of the pin apparatus of FIG. 1 , and FIGS. 3 b and 3 c are top and bottom end views, respectively, of the housing;
[0019] FIG. 4 of the drawings is an isolated, perspective view of the bottom of the handle of the pin apparatus of FIG. 1 ;
[0020] FIG. 5 a of the drawings is a perspective view illustrating the position of the handle of the pin apparatus of FIG. 1 when the pin is in a retracted position;
[0021] FIG. 5 b of the drawings is a perspective view illustrating the position of the handle of the pin apparatus of FIG. 1 when the pin is in an extended position;
[0022] FIG. 6 a of the drawings is a side view in partial section of the pin apparatus with the pin in a retracted position;
[0023] FIG. 6 b of the drawings is a side sectional view of the pin apparatus with the pin in an extended position; and
[0024] FIGS. 7 a and 7 b of the drawings are side elevation views illustrating possible positions of the handle of the pin apparatus on a machine handle of a lawnmower when the pin is in a retracted position and when the pin is in an extended position.
DETAILED DESCRIPTION
[0025] In accordance with the subject matter disclosed herein, and with particular reference to the exploded view provided by FIG. 1 of the drawings, a pin apparatus generally designated 10 is provided and comprises a pin with a pin body generally designated 100 , a housing generally designated 200 , and a handle generally designated 300 . Pin body 100 , housing 200 and handle 300 are illustrated and discussed in greater detail herein below. While it is envisioned that pin apparatus 10 can be adapted for any suitable use, pin apparatus 10 in FIG. 1 is illustrated in an exploded view for assembly with a machine handle that can be associated with a walk-behind machine.
[0026] When assembled, pin apparatus 10 can extend at least partially through machine handle H and be used to maintain machine handle H in a desired alignment with respect to a positioning plate P. A retaining pin 150 can be used with pin body 100 to securely maintain the position of pin body 100 with respect to handle 300 when pin apparatus 10 is fully assembled as described in detail below. A biasing member, such as spring S, can be positioned around a portion of pin body 100 as further shown and described below. Positioning plate P can be attached to a walk-behind machine, such as a lawnmower, as further illustrated and described below. Machine handle H can be an elongated, pipe-type handle of any suitable cross-sectional configuration. As illustrated in FIG. 1 , a portion of machine handle H is illustrated as machine handle H is shown with a triangular cross section and wherein machine handle H defines an opening 400 that can be defined transversely through machine handle H and can be adapted for receiving at least a portion of housing 200 . When housing 200 is positioned through opening 400 of machine handle H, at least a portion of pin body 100 can extend through housing 200 such that handle 300 can attach to a portion of pin body 100 . As described in greater in detail below, handle 300 can be utilized to cause movement of pin body 100 within housing 200 such that pin body 100 can be in an extended position where a portion of pin body 100 extends at least partially into an opening defined in positioning plate P. As shown in FIG. 1 , positioning plate P can define at least one or more positioning holes or openings, such as openings 01 and 02 . It is envisioned that positioning plate P can define any number of suitable openings adapted for receiving at least a portion of pin body 100 in accordance with the present disclosure. Positioning plate P can be of any suitable shape or configuration adapted for attachment to a machine such as a walk-behind machine.
[0027] Referring specifically to FIGS. 2 a , 2 b and 2 c of the drawings, pin body 100 is illustrated in greater detail and comprises a proximal end section generally designated 102 and a distal end section generally designated 104 . Proximal end section 102 of pin body 100 can comprise an elongated, cylindrical outer configuration and define a transverse opening 106 therethrough for receiving retaining pin 150 . Handle 300 (shown in FIG. 1 ) can be positioned on proximal end section 102 of pin body 100 prior to placement of retaining pin 150 . After proper placement of handle 300 on proximal end section 102 , placement of retaining pin 150 through transverse opening 106 securely maintains handle 300 on proximal end section 102 of pin body 100 . Distal end section 104 of pin body 100 can comprise an outer wall section with a cylindrical shape of a greater diameter than the diameter of the outer wall section of proximal end section 102 . At one end of distal end section 104 , a tapered shelf 108 can be formed by distal end section 104 and extend peripherally around pin body 100 . At an opposite end of distal end section 104 , a flat shelf 110 can be formed by distal end section 104 and extend peripherally around pin body 100 . Flat shelf 100 can be adapted for engaging spring S as further described below.
[0028] Pin body 100 as shown can therefore extend and be disposed along a central longitudinal axis as both proximal end section 102 and distal end section 104 can be disposed along the same central axis. As illustrated, a majority of the length of pin body 100 comprises a cylindrical or tubular portion with an outer wall 112 of which at least a portion of which constitutes proximal end section 102 . Also as shown, distal end section 104 can comprise a cylindrical or tubular portion with an outer wall 114 of a diameter substantially less than the diameter of outer wall 112 . It is envisioned according to the present disclosure that any suitable diameters of outer walls 112 and 114 can be utilized for pin body 100 .
[0029] Referring now to FIGS. 3 a , 3 b , and 3 c of the drawings, housing 200 is illustrated and comprises an elongated housing body 202 that defines an opening generally designated 204 that can be disposed along a central, longitudinal axis of an elongated housing body 202 . Opening 204 can be in a top end 206 of elongated housing body 202 , and opening 204 can be suitably shaped and adapted for receiving proximal end section 102 of pin body 100 as shown and described further below. In top end 206 of elongated housing body 202 , opening 204 can have an inner wall 208 that can be cylindrical in shape and form an opening diameter suitable for receiving proximal end section 102 of pin body 100 as described further below. Further inside and toward an opposite end of elongated housing body 202 , opening 204 can have an expanded, inner wall 210 that can be cylindrical in shape and have an opening diameter greater than the opening diameter formed by inner wall 208 . Expanded inner wall 210 can extend entirely through elongated housing body 202 along a central axis thereof and be open at a bottom end 212 of elongated housing body 202 . The opening diameter formed by inner wall 210 can be suitably shaped and adapted for receiving distal end section 104 of pin body 100 . At the intersection of inner wall 208 and inner wall 210 of opening 204 , elongated housing body 202 can form a shelf 214 which can be suitably shaped and adapted for engaging an end of spring S as further illustrated and described below. A collar 216 can be attached to or formed as a part of bottom end 212 of elongated housing body 202 .
[0030] While it is envisioned in accordance with the present disclosure that the outer shape of elongated housing body 202 can be any shape suitable for use as described herein, elongated housing body 202 is illustrated for example only and without limitation as having an outer cylindrical shape that can be of a size and shape adapted for positioning through opening 400 of machine handle H as shown and described further below.
[0031] Referring now to FIG. 4 of the drawings, a bottom, perspective view of handle 300 is provided. As shown, handle 300 includes an upper grip portion 302 and a lower, cover portion generally designated 304 . Grip portion 302 can be of any suitable shape and configuration adapted for a user to grip and rotate, turn or twist handle 300 . Cover portion 304 can be formed as a part of handle 300 as a lower extension from grip portion 302 or cover portion 304 could be suitably attached to grip portion 302 . Cover portion 304 can be shaped and adapted for fitting onto a portion of machine handle H (shown in FIG. 1 ). As shown in FIG. 4 , cover portion 304 can be at least generally concave or V-shaped in cross-sectional shape and include a lower surface 306 that can have a shape and configuration at least substantially identical to the shape, configuration and profile of an upper surface of machine handle H as shown and described further below. On opposite ends of cover portion 304 , edges 308 a and 308 b can be formed by cover portion 304 and can be curved in a profile adapted to fit on an upper edge of machine handle H as shown and described further below. In order to allow handle 300 to fit and attach to proximal end section 102 of pin body 100 (shown previously), a central opening 310 can be defined from the bottom of handle 300 through cover portion 304 and extend into the inside of grip portion 302 where proximal end section 102 of pin body 100 can be positioned. As described with reference to FIG. 1 , a retaining pin 150 (shown in FIG. 1 ) can be used and positioned through an opening 312 defined through grip portion 302 of handle 300 .
[0032] FIGS. 5 a and 5 b of the drawings illustrate the positions of handle 300 with respect to machine handle H when pin body 100 (shown previously) is in a retracted position versus an extended position. When pin body 100 is a retracted position, handle 300 is positioned as illustrated in FIG. 5 a where grip portion 302 extends in a direction at least generally perpendicular to the direction of extension of machine handle H. In this position, cover portion 304 of handle 300 is aligned and positioned such that edge 308 a and edge 308 b (shown in FIG. 4 ) of cover portion of 304 engage and rest upon an upper surface 402 of machine handle H. In this position, a space or gap can exist between upper surface 402 of machine handle H and at least a portion of cover portion 304 of handle 300 .
[0033] When pin body 100 (shown previously) is in an extended position, handle 300 can be positioned as illustrated in FIG. 5 b where grip portion 302 extends in a direction at least generally parallel to the direction of extension of machine handle H. In this position, cover portion 304 of handle 300 can fit flush and entirely against upper surface 402 of machine handle H. Edge 308 a and edge 308 b (shown in FIG. 4 ) are positioned further down the sides and toward the bottom of upper surface 402 of machine handle H from their positions in FIG. 5 a . Additionally, no gap exists between upper surface 402 and cover portion 304 of handle 300 .
[0034] Referring now to FIG. 6 a of the drawings, pin apparatus 10 is illustrated in a fully assembled form and where pin body 100 is in a retracted position such that no portion of pin body 100 extends into or through opening 01 of positioning plate P. Movement of machine handle H is therefore permitted since no portion of pin body 100 extends into or through opening 01 of positioning plate P. To achieve this position, handle 300 is positioned as illustrated and described as in FIG. 5 a where grip 302 extends in a direction at generally perpendicular to the direction of extension of machine handle H and where cover portion 304 of handle 300 only contacts upper surface 402 of machine handle H by edges 308 a and 308 b (shown in FIG. 5 a ) of cover portion 304 engaging and resting upon the upper portion of upper surface 402 of machine handle H. In this position, proximal end section 102 of pin body 100 is maintained a distance away from machine handle H by retaining pin 150 securing and maintaining pin body 100 in its attachment with handle 300 . Spring S can be compressed in this position as spring S can be positioned peripherally around outer wall 112 of pin body 100 and extend between flat shelf 110 of distal end section 104 and shelf 214 of housing 200 . Collar 216 is positioned outside of the bottom of machine handle H and can limit and prevent upper movement of housing 200 while top end 206 of housing 200 . Top end 206 of housing 200 is illustrated as contained within machine handle H and can be of a size larger than the size of opening 400 in machine handle H in order to prevent movement of housing 200 through opening 400 in upper surface 402 of machine handle H. It is also envisioned according to the present disclosure that opening 400 in upper surface 402 of machine handle H could be larger than top end 206 and the overall outer diameter of elongated housing body 202 of housing 200 . In such a configuration, collar 216 can by itself retain housing 200 in a fixed position with respect to limited or prevented upward movement of housing 200 within machine handle H.
[0035] Outer wall 114 of distal end section 104 is positioned and adapted for vertical, sliding movement within the area within an elongated housing body 202 defined by expanded inner wall 210 . As shown in FIG. 6 a , tapered shelf 108 of distal end section 104 of pin body 100 is maintained at a predetermined position and does not extend into or through opening 01 of positioning plate P.
[0036] Referring now to FIG. 6 b of the drawings, pin apparatus 10 is shown in a fully assembled form and with pin body 100 in its extended position where at least a portion of pin body 100 extends into opening 01 of positioning plate P. In order to achieve this extended position from the retracted position shown in FIG. 6 a , handle 300 can simply be twisted to the position shown in FIG. 6 b where cover portion 304 of handle 300 fits against upper surface 402 of machine handle H. Lower surface 306 of cover portion 304 of handle 300 can fit directly on and against upper surface 402 of machine handle H as shown with no gap between any portion of cover portion 304 and machine handle H. Twisting or turning handle 300 from the position shown in FIG. 6 a to the position shown in FIG. 6 b moves pin body 100 downwardly within housing 200 such that proximal and section 102 of pin body 100 is closer to machine handle H than it was in the retracted position shown in FIG. 6 a . Such movement of handle 300 therefore forces pin body 100 downwardly through housing 200 . Bias provided by spring S within housing 200 facilitates movement of pin body 100 into its extended position as spring S urges distal end section 104 of pin body 100 downwardly. As shown in FIG. 6 b , distal end section 104 of pin body 100 has now progressed from the retracted position shown in FIG. 6 a to the extended position shown in FIG. 6 b where at least a portion of distal end section 104 extends into and/or through opening 01 of positioning plate P. As shown for example in FIG. 6 b , a portion of outer wall 114 of distal end section 104 has extended through and below opening 01 of positioning plate P. In this position, pin apparatus 10 therefore securely maintains machine handle H in a desired position with respect to positioning plate P.
[0037] While FIGS. 6 a and 6 b show pin body 100 first in a retracted position and then in an extended position, it can be appreciated that moving pin body 100 from its extended position shown in FIG. 6 b back to its retracted position shown in FIG. 6 a can easily be accomplished by simply twisting handle 300 to rotate and move handle 300 back to its position shown in FIG. 6 a.
[0038] FIGS. 7 a and 7 b of the drawings illustrate, for example only and without limitation, use of pin apparatus 10 with association with a walk-behind machine shown as a lawnmower 500 . A positioning plate 502 can be attached to or formed as part of lawnmower 500 , and machine handle H can be attached to positioning plate 502 at a pivot 504 . Positioning plate 502 can define a plurality of positioning holes, such as for example positioning holes 504 A, 504 B and 504 C shown in FIG. 7 a and also positioning hole 504 D shown in FIG. 7 b . Positioning holes 504 A-D are adapted for receiving at least a portion of pin body 100 (shown previously). Pin apparatus 10 can be used to selectively and securely position machine handle H in a desired alignment with respect to positioning plate 502 . Proper alignment and adjustment of machine handle H is important since an upper end or attachment to machine handle H is typically engaged to push lawnmower 500 . The pivotal attachment of machine handle H to positioning plate 502 permits pivotal movement of machine handle H such that machine handle H can be positioned adjacent either of positioning holes 504 A-D. Handle 300 of pin apparatus 10 is shown in FIG. 7 a in its position as illustrated also in FIGS. 5 a and 6 a where pin body 100 (shown previously) is in its retracted position thereby allowing movement of machine handle H to selectively position machine handle H adjacent to a desired one of positioning holes 504 A-D. Once machine handle H is positioned adjacent a desired one of positioning hole 504 A-D, handle 300 can be twisted from the position shown in FIG. 7 a to the position shown in FIG. 7 b to secure and lock in place machine handle H in a desired alignment with respect to positioning plate 502 . When pin apparatus 10 is in the position as shown in FIG. 7 b , at least a portion of pin body 100 (shown previously) extends into the adjacent positioning hole of positioning plate 502 to secure and prevent pivotal movement of machine handle H. As shown for exemplary purposes only in FIG. 7 b , handle 300 of pin apparatus 10 is positioned to secure and lock machine handle H into a position or alignment where pin body 100 (shown previously) extends into positioning hole 504 a of position of plate 502 .
[0039] It can therefore be readily understood that pin apparatus 10 can be used in association with lawnmower 500 to secure machine handle H in a desired position and alignment with respect to positioning plate 502 of lawnmower 500 . Once pin apparatus 10 has been utilized to secure machine handle H in a desired position with respect to positioning plate 502 it can be readily be understood that subsequent alignment adjustments of machine handle H can be easily accomplished by simply again twisting handle 300 of pin apparatus 10 to move handle 300 from the position shown in FIG. 7 b back to the position shown in FIG. 7 a allowing pivotal movement of machine handle H with respect to positioning plate 502 .
[0040] It will be understood that various details of the presently disclosed subject matter may be changed without departing from the scope of the present subject matter. Furthermore, the foregoing description is for the purpose of illustration only, and not for the purpose of limitation.
|
Pin apparatuses and methods are disclosed having particular suitability for use with machine handles such as those associated with walk-behind machines such as lawnmowers. A pin apparatus can include a housing defining an opening for receiving at least a portion of a pin. A pin can be provided having an elongated pin body with a proximal end section and a distal end section. The pin body can be adapted for positioning at least partially through the opening of the housing where the pin is movable with respect to the housing according to a method disclosed herein from an extended position where at least a portion of the distal end section extends to a predetermined extent outside of the opening, and a retracted position where the distal end section is in a retracted position from the predetermined extent. A handle can be provided external from the housing for moving the pin whereby movement of the handle moves the pin between the extended position and the retracted position.
| 8
|
This application claims benefit of European Patent Application Serial No. EP 12193653.8, filed on Nov. 21, 2012. The teachings of European Patent Application EP 12193653.8 are incorporated herein by reference in their entirety.
FIELD OF THE INVENTION
The invention relates to distance measurement and in particular to a distance sensor, an air spring height sensor and an air spring for a vehicle having an air spring height sensor or a distance sensor.
BACKGROUND OF THE INVENTION
Height or distance measurement has a wide variety of possible applications. However, the environment where the height measurement is being made can present a wide variety of challenges. This is particularly the case in situations where height or distance measurements are being made in automotive applications. For example, in measuring the height of a vehicle frame above the surface of a road, challenges are typically presented by road noise, dirt, dust, and vibrations which are normally present in the environment surrounding the vehicle where the measurement is being taken.
DE 10 2006 017 275 A1 and EP 1845278 A1 describe an air spring having an integrated positioning device, wherein the distance between two parts of the air spring can be measured by an analogue proximity sensor. Commonly used proximity sensors are, for example, based on an ultrasonic measurement principle which is very sensitive in noisy and vibrating environments, as the acoustic noise and the ultrasonic measurement principle are based on the same physical principle, i.e. sound propagation. These pneumatic air springs have an integrated height measuring device, a pressure chamber or an inner chamber. The exterior of the inner chamber is aligned in the analog proximity sensor and a metal plate is arranged opposite to the interior of the proximity sensor. The proximity sensor and the metal plate are formed pre-adjustable to each other.
Further, DE 10 2008 064 647 A1 describes an air spring for a vehicle having a measuring device, which measuring device may transmit data and energy via predetermined and fixed distance contactless. This pneumatic cushioning equipment has a base unit which has a pressure source and a valve unit which has an air supply made of non-metallic material, particularly plastic. A switching valve of the base unit is provided between the pressure source and appropriate valve unit of the arranged air supply.
EP 2 366 972 and United States Patent Publication No. 2012/0056616 A1 describe a sensor device for height measurement in an air spring and a corresponding method allowing determining changes in a working stroke of the air spring. These publications more specifically disclose a sensor device for a height measurement, comprising: a transceiving coil arrangement including at least one transceiving coil; a transmitting drive unit; a receiver unit; a reference coil arrangement; and a reference control unit, wherein the transceiving coil arrangement is coupled to both the transmitting drive circuit and the receiver unit, wherein the reference control unit is coupled to the reference coil arrangement, wherein the reference coil arrangement is movably positioned with respect to the transceiving coil arrangement, wherein the drive unit is adapted to drive the transceiving coil arrangement with an AC power signal of a predetermined duration for generating a magnetic field, wherein the reference control unit is adapted for accumulating energy out of the generated magnetic field and for generating a reference signal based on an amount of the accumulated energy, and wherein the receiver unit is adapted for receiving the reference signal and for outputting a signal for determining a distance between the transceiving coil arrangement and the reference coil arrangement based on at least one out of a group, the group consisting of the reference signal and the duration of the AC power signal.
SUMMARY OF THE INVENTION
It may be seen as an objective technical problem to provide a distance sensor for an air spring which allows an improved accuracy when determining the working stroke of an air spring.
The object of the present invention is solved by the subject matter of the independent claims, wherein further embodiments are incorporated in the dependent claims and the following specification.
According to an aspect of the invention, an air spring height sensor is provided which comprises a receiver for receiving a height signal and an evaluation unit, wherein the receiver is adapted for being mounted to an air spring so as to sense a height signal with respect to said air spring. The evaluation unit comprises an input terminal, a multiplexer, a first signal branch starting from the input terminal and terminating at a first multiplexer input, and a second signal branch starting from the input terminal and terminating at a second multiplexer input. The first signal branch includes a first amplitude limiter being adapted to cut off the amplitude above a predetermined first threshold value. The multiplexer is adapted to select a measurement signal from one of the inputs of the multiplexer.
The height signal as described above and hereinafter may in particular be inversely proportional to the height of the air spring, i.e. to the working stroke of the air spring. In other words, the greater the distance to be measured is, i.e. the current working stroke of an air spring, the smaller or lesser will the height signal value be.
The height signal may in particular be determined by a receiving coil of the receiver, wherein the receiving coil is adapted to receive a magnetic field generated by a transmitting coil. The height signal may then be determined by an electric current which is induced in the receiving coil by the magnetic field. The closer the transmitting coil and the receiving coil are arranged with respect to each other, the higher will the electric current induced in the receiving coil be. Thus, the induced electric current in the receiving coil is a parameter or a criterion for the distance between the transmitting coil and the receiving coil.
In case the value of the height signal has no linear course or linear plot when changing the distance or height to be measured, the distance determination may be of fluctuating accuracy. In other words, when the height signal changes to a great degree in dependence of the changed distance between transmitting coil and receiving coil, small changes in the distance may be detected as the height signal may change to a large degree, whereas when the height signal changes to a small degree in dependence of the changed working stroke of the air spring, small changes in the working stroke lead to small changes in the height signal and may thus be subject to uncertainty. In other words, in a distance range or working stroke in which the first derivative of the height signal over the distance is high, the distance and in particular distance changes may be detected with higher accuracy compared to a distance range in which the first derivative of the height signal over the distance is low.
The air spring height sensor as described above and hereinafter enables providing of height signals in a first distance range or value range of the height signal to a first multiplexer input and height signals in a second distance range or value range of the height signal to a second multiplexer input such that the signals may be processed in a different manner, for example by applying an amplification to one of the height signals, provided to the first multiplexer input or the second multiplexer input.
Thus, for an improved height measurement accuracy of an air spring, those height signal of the two signals may be selected for determining the height of the air spring which provides a signal form with a higher value of the first derivative of the signal form. The air spring height sensor as described above and hereinafter may in particular be used for wireless distance sensing and in more particular for distance measurement using a transmitting coil and a receiving coil, wherein a magnetic field generated by the transmitting coil and received by the receiving coil is the criterion for determining the distance between the transmitting coil and the receiving coil which may both be mounted to moving elements of an air spring which moves towards and away from each other in an operating state of the air spring.
According to an embodiment of the invention, the first branch between the first amplitude limiter and the first multiplexer input includes a digital programmable filter.
The digital programmable filter may be adapted to perform digital signal processing to the signal transmitted via the first branch. The signal of the first branch may be smoothed by the digital programmable filter by filtering out frequencies above a given frequency, i.e. the filter acts as a low pass filter. The digital programmable filter may also be adapted as a band pass.
According to a further embodiment of the invention, the first branch between the digital programmable filter and the first multiplexer input includes a logarithmic amplifier.
The logarithmic amplifier may in particular be adapted to linearize the output signal of the digital programmable filter. In one embodiment the logarithmic amplifier is adapted to amplify the height signal such that the first derivative of the height signal is constant in a given distance range of the height signal. Thus, the accuracy of the height measurement may be increased as the sensitivity of the height signal to distance changes is constant in a given range of height values.
According to a further embodiment of the invention, the second signal branch includes a second amplitude limiter being adapted to cut off the amplitude above a predetermined second threshold value being higher than the first threshold value.
Both the second amplitude limiter and the first amplitude limiter are adapted to cut off a height signal exceeding the first threshold value in order to avoid to large signal amplitude which may cause signal distortion at the subsequent modules.
According to a further embodiment of the invention, the evaluation unit comprises a third signal branch starting between the first amplitude limiter and the digital programmable filter and terminating at a third multiplexer input.
The third signal branch enables to branch off the amplified height signal of the first branch at the output of the first amplitude limiter such that the branched off signal may be provided to the third multiplexer input with an amplification but without a logarithmic amplification.
This enables to choose one of the multiplexer inputs and the according height signal depending on the value range of the output signal of the receiver, i.e. depending on the output value of the height signal provided by the receiver, or the measured distance or working stroke of the air spring.
According to a further embodiment of the invention, the first signal branch between the first amplitude limiter and the digital programmable filter includes a signal amplifier.
Thus, the first multiplexer input is being provided with a height signal which is being amplified in a first stage, filtered by a digital programmable filter in a second stage and amplified by a logarithmic amplifier in a third stage. The second multiplexer input is being provided with the original height signal from the output of the receiver, wherein the height signal's value is subjected to an amplitude limitation only. The third multiplexer input is being provided with a limited height signal which is being amplified by the signal amplifier.
The first multiplexer input, second multiplexer input, and third multiplexer input are part of a multiplexer which is adapted to provide one of the height signals of the first multiplexer input, the second multiplexer input, and the third multiplexer input to a multiplexer output for further processing of the height signal.
The multiplexer may be adapted to lead through one of the three input values dependent on the value of the original height signal at the output of the receiver. In case the original height signal is in a first value range, the multiplexer leads through the height signal of the second multiplexer input. In case the original height signal is in a second value range, the multiplexer leads through the height signal of the third multiplexer input. In case the original height signal is in a third value range, the multiplexer leads through the height signal of the first multiplexer input.
In this scenario, the first value range of the original height signal indicates a small distance which means that the provided height signal has a relatively high value such that amplification or other further processing of the height signal may not be necessary in the first value range. The second value range indicates a medium distance which means that the provided height signal is decreased compared to the first value range as the height signal is inversely proportional to the distance. In particular, the height signal may decrease exponentially in one embodiment of the invention. The second value range may require an amplification of the height signal to facilitate the detection and determination of small distance changes even though the sensitivity of the receiver is decreased with an increased measuring distance. The third value range indicates a large measuring distance whereas the original height signal provided by the receiver may indicate almost no changes with small distance changes. In the third value range a logarithmic amplification may be necessary in order to prepare and treat the original height signal as to detect small distance changes even though the measuring distance is relatively high.
In one embodiment, the value ranges may be set up as follows: the first value range may correspond to a measuring distance between 1 mm and up to 50 mm; the second value range may correspond to a measuring distance between 50 mm and up to 150 mm; the third value range may correspond to a measuring distance between 150 mm and up to 400 mm.
According to a further embodiment of the invention, the air spring height sensor further comprises a height measuring signal transmitter and a controlling device. The height measuring signal transmitter is adapted to transmit a height measuring signal such that the receiver upon transmitting receives a signal representing a distance between the height measuring signal transmitter and the receiver. The controlling device is adapted for controlling a carrier frequency of the height measuring signal.
The transmitter is adapted for generating a magnetic field wherein the receiver is adapted to receive the magnetic field such that an electric current is induced in the receiver and in particular in a receiver coil. In one embodiment, the transmitter may also comprise a coil which may be a wounded coil with or without a core and wherein the core may comprise iron or a ferromagnetic material. Depending on the distance between the transmitter and the receiver the electric current induced in the receiver coil may vary as described above in more detail.
The controlling device may be adapted to drive or trigger the height measuring signal transmitter and in particular the generation of the magnetic field by the transmitting coil. The controlling device may further be adapted to detect noise signals in the received height signal, wherein the carrier frequency may be changed in case the noise on the used carrier frequency overlays or superimposes the height signal. In other words, in case the signal to noise ratio of the measured height signal is to large, the carrier frequency of the height measuring signal may be changed.
According to a further embodiment of the invention, the controlling device is adapted to switch the carrier frequency of the height measuring signal, to compare output signals of the multiplexer upon different frequencies of the height measuring signal, and to evaluate the compared output signals of the multiplexer so as to eliminate disturbed signals.
The air spring height sensor may thus be used in an environment in which other radio signals may be present as the controlling device may be able to identify and eliminate disturbed height signals.
According to a further embodiment of the invention, the controlling device is adapted to control the digital programmable filter upon reception of an output signal of the multiplexer. Thus, the controlling device may be able to adapt the filter properties of the digital programmable filter as to adapt the filtered height signal.
According to a further aspect of the invention, an air spring is provided which comprises a first mounting element being adapted for being mounted to a first vehicle portion, a second mounting element being adapted for being mounted to a second vehicle portion, an air volume limited by a resilient belly having a first edge and a second edge, which belly with the first edge is sealed to the first mounting element and with the second edge is sealed to the second mounting edge, and an air spring height sensor as described above and hereinafter. The receiver of the air spring height sensor is mounted to the air spring so as to sense a height signal with respect to at least one of the first mounting element and the second mounting element.
The air spring may be used as a spring in a wheel suspension of a vehicle. The air spring height sensor in the air spring facilitates an accurate measurement of the working stroke of the air spring with a high sensitivity of the output signal of the air spring height sensor about a large measurement range or working stroke of the air spring.
According to one embodiment of this invention, the receiver is mounted to one of the first mounting element and the second mounting element so as to sense a height signal with respect to the other one of the first mounting element and the second mounting element. Thus, the air spring height sensor enables a distance measurement between the first mounting element and the second mounting element of the air spring.
According to a further aspect of the invention, a distance sensor is provided which comprises a receiver for receiving a distance signal and an evaluation unit. The evaluation unit comprises an input terminal, a multiplexer, a first signal branch starting from the input terminal and terminating at a first multiplexer input, and a second signal branch starting from the input terminal and terminating at a second multiplexer input, wherein the first signal branch includes a first amplitude limiter being adapted to cut off the amplitude above a predetermined first threshold value.
The distance sensor allows providing a distance signal via the first signal branch and via the second signal branch to the multiplexer, wherein the multiplexer leads through one of the provided signals in dependency of the signal value. In case the signal value exceeds the threshold value, the cut off signal is lead through by the multiplexer. In case the signal value does not exceed the threshold value, the original signal value is lead through by the multiplexer.
These and other aspects of the present invention will become apparent from and elucidated with reference to the embodiments described hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates an air spring according to an exemplary embodiment of the invention.
FIG. 2 illustrates an air spring according to a further exemplary embodiment of the invention.
FIG. 3 illustrates a wheel suspension with an air spring according to a further exemplary embodiment of the invention.
FIG. 4 illustrates a wheel suspension with an air spring according to a further exemplary embodiment of the invention.
FIG. 5A illustrates a height signal form of an air spring height sensor according to a further exemplary embodiment of the invention.
FIG. 5B illustrates a height signal form of an air spring height sensor according to a further exemplary embodiment of the invention.
FIG. 6 illustrates an air spring height sensor according to a further exemplary embodiment of the invention.
FIG. 7A illustrates a height signal form of an air spring height sensor according to a further exemplary embodiment of the invention.
FIG. 7B illustrates a height signal form of the third multiplexer input of an air spring height sensor according to a further exemplary embodiment of the invention.
FIG. 7C illustrates a height signal form of the first multiplexer input of an air spring height sensor according to a further exemplary embodiment of the invention.
The reference numerals used herein are as follows:
1 air spring 2 first vehicle portion 3 second vehicle portion 10 first mounting element 20 second mounting element 30 belly 31 first edge 32 second edge 40 working stroke 50 height measurement signal 50 A first amplification stage 50 B second amplification stage 50 C third amplification stage 100 air spring height sensor 101 receiver 102 height measuring signal transmitter 200 evaluation unit 201 input terminal 210 first signal branch 211 first amplitude limiter 212 signal amplifier 213 digital programmable filter 214 logarithmic amplifier 220 second signal branch 221 second amplitude limiter 230 third signal branch 240 multiplexer 241 first multiplexer input 242 second multiplexer input 243 third multiplexer input 250 analog-digital converter 260 controlling device 261 signal output 263 feedback line
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 illustrates an air spring 1 with a first mounting element 10 and a second mounting element 20 . The air spring further comprises a belly 30 with a first edge 31 and a second edge 32 . The first edge 31 of the belly 30 is mechanically interconnected with the first mounting element 10 and the second edge 32 is mechanically interconnected with the second mounting element 20 . The belly encloses an air volume such that the working stroke 40 of the air spring represents a movement of one of the first mounting element 10 and the second mounting element 20 towards the other one of the first mounting element 10 and the second mounting element 20 .
A receiver 101 in form of a coil and a height measuring signal transmitter 102 are located within the air volume of the air spring as indicated by the air spring illustrated in dotted lines. The receiver 101 is located close to the first mounting element 10 of the air spring and the height measuring signal transmitter 102 is located close to the second mounting element 20 of the air spring. Both, the receiver and the height measuring signal transmitter may be designed as coreless coils such that a working stroke 40 of the air spring is not reduced by these devices which are located within the air volume of the air spring.
FIG. 1 shows the air spring and the air spring height sensor in both the mounted and the unmounted state, wherein on the left side of the drawing the unmounted state and on the right side of the drawing the mounted state is depicted.
The air spring as described above and hereinafter may in particular be a smart air spring with an air spring height sensor as described above and hereinafter as air spring level unit or height measurement system. The air spring may in particular be an air spring with intelligent sensor and actuator functions. One of the important features is the integrated air spring height sensor. The function of the air spring height sensor is it to measure with reasonable accuracy the current absolute axial position of the air spring, i.e. the distance between the first mounting element and the second mounting element. With other words: what is the current length of the air spring. Such a sensor solution may require its own, application specific electronics which will be described in more detail below.
The air spring height sensor as described above and hereinafter may offer the following features: reduced or no sensitivity to electromagnetic interferences (EMI), insensitive or fully compensated for the potential effects caused by temperature and temperature fluctuations or variations, reasonably high signal resolution for the targeted measurement range, no shortening of the original operating or working stroke of the air spring, low electric current consumption, fast signal response with a wide signal bandwidth range, low or no emissions of electromagnetic interferences, insensitive to metallic objects of different kinds that may be placed near the air spring or placed inside the air spring, wherein in the latter limits of maximum size and maximum mass of the metallic object apply, insensitive to changes of humidity, dirt and dust to a certain extent.
The air spring height sensor as described above and hereinafter is not limited to air spring applications. Wherever a large measurement stroke of a linear-position-sensor is required, this described electronics solution may be applicable. Large measurement stroke means that the signal amplitude ratio may change in exponential ratio, for example in a range greater than 1:100. Examples include, but are not limited to, height and position changes in vehicle suspension system including all types of vehicles, like trucks, passenger cars, rains, planes, motor bikes, etc., control of industrial processing equipment like tooling, milling, drilling, mixing, filling, shifting, sorting, like luggage sorting and handling at airports, parcel sorting at the mail service, etc., test equipment like flight simulator, engine test bed, furniture reliability tests, sports equipment testing, etc., large scale, indirect load measurement systems like weight-on-beam design, large scale mining equipment like oil drilling, tunneling, steering and position control systems in ships (rudder position), planes (flaps, rudder,). Other applications for this application may be measuring accurately the distance to a metallic object, like when the engine (locomotive) of a train is coupling to a rail-road wagon, or when a pushing-truck at the airport is automatic or semi-automatic coupling to the front-wheel of a plain. When implementing an air spring height sensor as described above and hereinafter into a smart air spring system, it may be important not to shorten the actual mechanical stroke of the air spring.
There may exist several different ways to integrate an air spring height sensor as described above and hereinafter into an air spring. FIG. 1 shows one of these possibilities, where the height measuring signal transmitter 102 is placed at one end of the air spring body, i.e. at the second mounting element 20 (like the bottom) and the receiver 101 is placed at to other end of the air spring body, i.e. at the first mounting element 10 . Other design solutions are that the height measuring signal transmitter and the receiver are placed at one and the same side (not shown in FIG. 1 ), for example.
FIG. 2 illustrates an air spring 1 in a first state or in an uncompressed state on the left side of the drawing and the air spring 1 in a second state or in a compressed state on the right side of the drawing. The difference between the length of the air spring in the first state and in the second state corresponds to the maximum working stroke of the air spring. As the height measuring signal transmitter and the receiver are designed as coils with a minimum extension in direction of the working stroke, the working stroke of the air spring is almost not or not reduced when arranging the air spring height sensor as described above and hereinafter within the air volume of the air spring.
A manufacturer's specification of an air spring may define the usable working stroke range 40 which is shown in connection with the first state and the second state of the air spring in FIG. 2 . In particular, the user of the air spring should not alter the air spring as to inflate it any higher or deflate it any lower than described in the manufacturer's specification. Going beyond the specified “Min/Max” positions may result in damages to the rubber belly of the air spring. In any case, to avoid damaging the air spring height sensor components when the air spring may get fully deflated, the individual sensing components height measuring signal transmitter and receiver have to be spaced sufficiently so that they never crash into each other at the minimum distance or when the air spring takes the second state. In a preferred embodiment, the air spring height sensor as described above and hereinafter may be built in such way that the height measuring signal transmitter and the receiver may come very close to each other when the air spring is fully deflated or collapsed.
The second state is the state in which the sensor signal transfer is most efficient and therefor the largest height signal can be expected at the output of the passive or active working signal receiver. This signal may also be called the original or untreated height signal.
When moving from the second state to the first state, the distance between the height measuring signal transmitter and the receiver steadily increases such that the original height signal is decreasing, wherein the decreasing may occur exponentially.
FIG. 3 illustrates a wheel suspension of a vehicle with two air springs 1 as described above and hereinafter. The second vehicle portion 3 , i.e. the movable part of the wheel suspension which is mounted to the wheel, is adapted to move along the arrows 40 , which correspond to the measuring distance and the working stroke of the air springs, wherein one mounting element of the air spring is attached to the second vehicle portion. The other one of the mounting elements of the air spring is mounted to the first vehicle portion 2 .
FIG. 4 illustrates an alternative wheel suspension of a vehicle with one air spring 1 , wherein one of the mounting elements of the air spring is attached to the movable second vehicle portion 3 and the other one of the mounting elements is attached to the first vehicle portion 2 . The second vehicle portion is rotatably movable around a hinge which mechanically interconnects the first vehicle portion and the second vehicle portion.
FIG. 5A illustrates the height signal 50 as a voltage Vin over the distance L between the height measuring signal transmitter and the receiver, wherein the voltage Vin decreases exponentially with increasing distance L. FIG. 5A illustrates the original height signal as provided at the output of the receiver of the air spring height sensor as described above and hereinafter.
The height signal form shown in FIG. 5A illustrates a very steep curve of the original or untreated sensor signal. The signal amplitude may be dropping by a factor of 1000 for the desired measurement range or working stroke. Within the very first few cm of distance reduction or movement of the air spring (starting at the “near deflated” position or in the second state where the air spring working stroke is at the minimum point), the signal amplitude Vin is dropping rapidly by near 50%. At the near “Max” point of the air spring working stroke or in the first state, the signal amplitude changes are the very smallest as the signal gain curve is here near flat.
For standard signal processing electronics designs it may be challenging to guarantee a reasonable high measurement signal quality over the entire measurement range. Under normal circumstances the signal to noise ratio and the temperature drift of the sensor signal will be at its worst when the air spring is inflated to near the “Max” position or in the first state.
FIG. 5B illustrates the height signal 50 shown in FIG. 5A wherein the signal is partitioned into a first amplification stage 50 A, a second amplification stage 50 B, and a third amplification stage 50 C.
In the first amplification stage 50 A the first derivative of the height signal may be high enough such that a distance change or a change of the L-value leads to a sufficient change of Vin which means that a movement of the receiver may be detected with reasonable accuracy.
In the second amplification stage 50 B the first derivative of the height signal is lower than in the first amplification stage 50 A. The height signal may require to be amplified in this distance range or value range of Vin, respectively such that changes of L lead to higher changes in Vin when the height signal has been amplified.
In the third amplification stage 50 C the height signal is nearly flat such that the signal may require a logarithmic amplification in order to detect sufficient signal changes in Vin when L changes.
The air spring height sensor as described above and hereinafter enables the different treatment of the amplification stages such that a height measurement over the complete working stroke or distance range may be carried out with high and constant accuracy even though the height signal Vin is inversely proportional to the measured distance and decreases exponentially with increasing distance.
The curve shown in FIG. 5B suggests three signal amplification stages 50 A, 50 B, and 50 C. The height signal that is in the segment 50 C will be amplified with the highest amplification factor, while the sensor signal in the segment A may need not to be amplified at all.
It should be noted that also more than three amplification stages are possible. With an increasing number of amplification stages the height signal value range may be treated more accurate. Any number from one additional stage to more than ten stages is possible here, whereby minimum two stages (resulting into a 2-signal-channel electronics design) to maximum four stages (resulting into a 4-signal-channel electronics design) may be the optimum for most typical applications. When choosing one amplification stage only (without any additional amplification stage), then there is no other stage to choose from or to switch between them.
FIG. 6 illustrates an air spring height sensor 100 for providing three amplification stages of the original height signal as indicated in FIG. 5B .
The receiver 101 provides the original height signal via the first signal branch 210 to the first amplitude limiter 211 and via the second signal branch 220 to the second amplitude limiter 221 . The second amplitude limiter 221 is connected to the second multiplexer input 242 of the multiplexer 240 and provides the amplitude limited original height signal to the second multiplexer input 242 .
The first amplitude limiter 211 provides the height signal to the signal amplifier 212 for applying an amplification factor of up to 10 to the height signal. Other amplification factors are applicable as well. Subsequently, the amplified height signal is provided first via the third signal branch to the third multiplexer input 243 and second to the digital programmable filter 213 . The digital programmable filter 213 provides the height signal to the logarithmic amplifier 214 which further provides the logarithmic amplified height signal to the first multiplexer input 241 .
Thus, the height signal in the first amplification stage 50 A is provided to the multiplexer via the second branch 220 , the second amplification stage 50 B is provided to the multiplexer via the third branch 230 , and the third amplification stage 50 C is provided to the multiplexer via the first branch 210 .
Depending on the value of Vin, the multiplexer leads through the value of the according multiplexer input to the analog-digital converter 250 and further to the controlling device 260 . It should be noted that for further processing of the height value lead through by the multiplexer the information of the applied amplification to the height signal is required in order to determine the correct distance or height.
The controlling device 260 is adapted to control the digital programmable filter 213 via the feedback line 263 , whereas the band pass frequencies for the filter process may be transmitted to the digital programmable filter in case such amendments to the filter are necessary in order to reduce the signal to noise ratio, for example.
FIG. 6 shows the signal pass of an exemplary embodiment of the air spring height sensor, beginning with the signal receiver stage and ending with a micro-controller device at the right side. The use of a micro-controller is optional and there are other solutions available when digital signal processing or digital control algorithms are required (as they are required to operate the digital filter).
The first signal branch 210 may be considered the main signal path and shows the following functions (starting from left to right): a signal amplitude limiter 221 , a signal amplifier 212 , a digital programmable filter 213 , a logarithmic (or exponential gain curve) amplifier 214 , a multiplexer 240 , and an analogue-to-digital signal converter 250 .
The signal amplitude limiter 211 is for preventing running the following circuit into saturation as too large of a signal amplitude would do, and with this may cause signal distortion.
A signal amplifier 212 may be required only when a multi-channel signal path design is used (a multi-channel means more than one channel, such as two or five), wherein the signal amplification factor may be within the range 3 to 10 (this may apply to a three signal-channel design).
A digital programmable filter 213 is in form of a band pass, such as a switch-mode capacitor filter, for example, can be tuned to any desired frequency and may eliminate the needs for a relative large number of passive and active electronics components (as required when building an analogue signal filter). In addition the actual and effective filter frequency may not vary when the operational temperature is changing. Nor may such filter design be dependent from the absolute tolerance of the individual passive electronic components (in comparison to a traditional analogue circuit filter design).
The air spring height sensor as described above and hereinafter may require electronic signal filter circuitry, which traditionally may be designed and produced using discreet analogue components (capacitors, inductors, resistors, transistors, OpAmps, etc.). To ensure functional stability it may be important that the critical components are manufactured with small tolerances only (1% resistors or better, for example) and that circuit compensation is included to deal with the changes in the operational temperature. A much more advanced solution may be the use of a digital programmable filter (in particular like those that use switch-capacitor-circuits). Those circuits are self-compensated, and can be freely programmed to any desired filter frequency and filter type. With very few exceptions a modern switch-mode-capacitor-filter may work almost like a “perfect filter”. The filter center frequency (either: band pass, low-pass, or high pass) may be set by a clock frequency. Any clock frequency can be used within a manufacturer specified range. Such clock frequency can be provided by a Micro-controller 260 and is stabilized (kept accurate) by the controllers timing circuit (like a crystal or temperature compensated resonator). So, there may be no temperature drift, or component tolerance offset. Another benefit when using digital filter techniques may be that the entire system can switch in an instant between different operational frequencies. This may be important when trying to implement a frequency hopping solution, i.e. the function of using different carrier frequencies. The frequency hopping solution may be one possible approach when trying to improve the air spring height sensor stability in case of potentially presents EMI (Electro Magnetic Interferences) signals.
The benefits when using switched-mode-capacitor filters may be: drastically reduction in numbers of required individual components to build the filter (cost and space issue); eliminating the need for small tolerance components (cost and stability issue); insensitiveness or insensitivity to changes of the operating temperature range (stability issue).
The ability to change the signal filter frequency may be important when trying to implement the function of different carrier frequencies. This means that the actual operational frequency of the entire air spring height sensor can be altered when interfering signals may block entirely the usage of, or interfere partially with a certain frequency.
A logarithmic (or exponential gain curve) amplifier 214 for the purpose of this active device is to linearize the sensors signal output and preferably cover an amplitude changing range of 1:1000.
The air spring height sensor as described above and hereinafter may have a very large measurement voltage range of Vin from several volts to fractions of mV. Because of the very large measurement voltage range of the air spring height sensor, a standard, linear operating amplifier may limit the distance measurement range. Alternatively a very costly, high performance amplifier may need to be used that has an excellent signal-to-noise ratio specification. For this application as described above and hereinafter a logarithmic gain amplifier stage 214 may be very beneficial as the signal gain is, by definition, much higher when the input signal is very small, and the signal gain is reduced when the input signal is getting larger and larger. Another benefit when using a logarithmic amplifier may be that the sensor output signal is already linearized. Meaning that the “linearized” amplifier output signal is proportional to the measurement distance between the height measuring signal transmitter and the receiver. Potentially this means no further signal linearization is required.
The Multiplexer 240 (MUX) is a device which will switch between the three different signal channels (in this example), obtained at the first multiplexer input 241 , the second multiplexer input 242 , and the third multiplexer input 243 .
The analogue-to-digital signal converter 250 is for a signal ratio of 1:1000 a ten-bit ADC may be required. To improve the signal quality a 12 or 14 bit ADC may be better, but may also increase the costs for the system.
In many instances, a micro-controller unit (MCU) may include the functions of the MUX and ADC already such that these components may be integrated on an MCU.
FIGS. 7A, 7B, and 7C illustrate the height signal at the second multiplexer input 242 via the second signal branch 220 ( FIG. 7A ), at the third multiplexer input 243 via the third branch 230 ( FIG. 7B ), and at the first multiplexer input 241 via the first branch 210 ( FIG. 7C ), respectively.
Furthermore, each of the FIGS. 7A, 7B, and 7C illustrates the according amplification stage 50 A, 50 B, and 50 C, respectively. The multiplexer 240 is adapted to lead through the Vin value of the multiplexer input which is assigned to the amplification stage corresponding to the current distance value.
Thus, the height signal Vin lead through by the multiplexer ensures a high first derivative and according an accurate distance measurement.
This application claims benefit of European Patent Application Serial No. EP 12193653, filed on Nov. 21, 2012. While certain representative embodiments and details have been shown for the purpose of illustrating the subject invention, it will be apparent to those skilled in this art that various changes and modifications can be made therein without departing from the scope of the subject invention.
|
An air spring height sensor ( 100 ) is provided which comprises a receiver ( 101 ) for receiving a height signal and an evaluation unit ( 200 ). The receiver is adapted for being mounted to an air spring so as to sense a height signal with respect to said air spring. The evaluation unit comprises an input terminal ( 201 ), a multiplexer ( 240 ), a first signal branch ( 210 ) starting from the input terminal and terminating at a first multiplexer input ( 241 ), and a second signal branch ( 220 ) starting from the input terminal and terminating at a second multiplexer input ( 242 ). The first signal branch includes a first amplitude limiter ( 211 ) being adapted to cut off the amplitude above a predetermined first threshold value. The multiplexer is adapted to select a measurement signal from one of the inputs of the multiplexer.
| 6
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention pertains generally to ink fountains utilized in offset printing apparatus, and more specifically to a control apparatus for adjusting the position of ink keys utilized in ink fountains.
2. Description of the Background Art
In the area of offset printing apparatus, ink fountains are generally used. Contained within the typical ink fountain is an inking roller (commonly called a fountain roller) and an ink metering blade (commonly called a fountain blade) which is positioned adjacent to the fountain roller. The position of the fountain blade in relation to the fountain roller is such that a gap is formed. The spacing of the gap determines the amount of ink that is applied to the fountain roller, and which in turn is transferred via other rollers to a print medium such as paper. Because it is quite common for the amount of ink transferred to vary across the print medium, it is often necessary to adjust the spacing of the gap across the length of the fountain roller. This adjustment is generally performed by operating manually or electrically controlled adjusting keys (commonly called ink keys) which are located at fixed locations along the length of the ink fountain. By moving the position of the fountain blade with respect to the position of the fountain roller, each ink key controls the spacing of the gap with respect to a particular segment, or zone, of the print medium.
Heretofore, ink keys have been of a screw-type which have required adjustment by application of rotational force or of a pusher-type which require application of a reciprocating force. Examples of devices which have been previously developed for application of rotational force are disclosed in U.S. Pat. No. 4,864,930 issued to Runyan et al. on Sep. 12, 1989; U.S. Pat. No. 4,669,382 issued to Jentzsch et al. on Jun. 2, 1987; U.S. Pat. No. 4,709,635 issued to Kubert et al. on Dec. 1, 1987; and U.S. Pat. No. 4,803,923 issued to Kenichi on Feb. 14, 1989. Examples of devices which have been previously developed for application of reciprocating force are disclosed in U.S. Pat. No. 4,711,176 issued to Michel on Dec. 8, 1987; and U.S. Pat. No. 4,829,898 issued to Wieland on May 16, 1989. Examples of devices which have been previously developed using eccentric discs which are used to adjust the position of the blade are disclosed in British Pat. No. 2,132,139 issued to Albert on Jul. 4, 1984; and U.S. Pat. No. 4,729,312 issued to Rodi et al. on Mar. 8, 1988. While the foregoing patents disclose devices which are capable of controlling the spacing of the gap between the fountain roller and the fountain blade, they do not provide for the fine incremental adjustments and repeatability of settings provided by the present invention.
The foregoing patents reflect the state of the art of which the applicants are aware and are tendered with the view toward discharging the applicants' acknowledged duty of candor in disclosing information which may be pertinent in the examination of this application. It is respectfully stipulated, however, that none of these patents teach or render obvious, singly or when considered in combination, the applicants' claimed invention.
SUMMARY OF THE INVENTION
The present invention provides for "push-pull" operation of ink keys utilized in connection with the ink fountain of an offset printing apparatus, as opposed to rotational operation of ink keys more commonly employed. The ink key is removed from the ink fountain and replaced with the mechanism of the present invention.
By way of example and not of limitation, the present invention generally comprises a linear actuator, a lever arm, an intermediate cam, a driver cam, and an ink key, all of which are contained within a housing. One end of the lever arm is connected to the shaft of the linear actuator. Rigidly attached to the other end of the lever arm is an intermediate cam, cylindrical in shape, in which an off-center hole is located. A pin extending through the hole in the intermediate cam and into the housing pivotally connects the intermediate cam to the housing. The driver cam contains a hole sufficiently large to permit it to be placed over the intermediate cam with a circular bearing located between their circumferences. Located at one edge of the driver cam is a threaded receptacle for acceptance of an ink key. When the ink key is installed, the longitudinal axis of the ink key will be substantially parallel to the longitudinal axis of the shaft of the linear actuator. When the linear actuator is operated, the ink key follows the direction of the shaft of the linear actuator with a push-pull, or reciprocating, movement. Utilization of a lever arm, intermediate cam, and driver cam in this manner provides for an approximately 12.5 to 1 reduction in distance of travel between the ink key and the shaft of the linear actuator; that is, when the shaft of the linear actuator moves 0.001 inches, the ink key moves in the same direction a distance of approximately 0.00008 inches. By using a linear actuator capable of movement in steps of 0.001 inches, extremely fine adjustment of the spacing of the gap between the fountain roller and the fountain blade is made possible. Additionally, the apparatus can produce pressure on the ink key in an amount equal to approximately 12.5 times that produced by the linear actuator.
An object of the invention is to provide for reciprocating movement of ink keys.
Another object of the invention is to provide for adjustment of the spacing of the gap between the fountain roller and fountain blade in increments of approximately 0.00008 inches.
Another object of the invention is to provide for linear adjustment of ink keys.
Another object of the invention is to prevent the fountain blade from damaging the fountain roller.
Another object of the invention is to permit the ink key to break through dried ink and continue operation.
Another object of the invention is to provide for remote control of ink keys.
Another object of the invention is to provide an ink key control apparatus which can be installed without alteration of the existing printing apparatus.
Another object of the invention is to eliminate the use of gears for positional control of a fountain blade.
Another object of the invention is to eliminate imprecise control resulting from gear backlash.
Another object of the invention to provide for efficient transfer of linear to linear motion.
Another object of the invention is to permit high speed control of an ink key.
Another object of the invention is to provide an ink key servo mechanism with minimum parts and high reliability.
Further objects and advantages of the invention will be brought out in the following portions of the specification, wherein the detailed description is for the purpose of fully disclosing preferred embodiments of the invention without placing limitations thereon.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be more fully understood by reference to the following drawings which are for illustrative purposes only:
FIG. 1 is an exploded view of the preferred embodiment of the present invention.
FIG. 2 is a cross-sectional view of the apparatus shown in FIG. 1.
FIG. 3 is an orthogonal schematic view of the lever arm and cam components of the present invention showing the transformation of rotational and axial motion.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring more specifically to the drawings, for illustrative purposes the present invention is embodied in the apparatus generally shown in FIG. 1 and FIG. 2. It will be appreciated that the apparatus may vary as to configuration and as to details of the parts without departing from the basic concepts as disclosed herein.
In the preferred embodiment, the actuating means comprises linear actuator 10. Linear actuator 10 is securely mounted to housing 12 which encloses the components of the apparatus using a plurality of screws 11 and washers 13. Linear actuator 10 includes an internal threaded rotor to which shaft 14 is attached.
Linear actuator 10 is typically electrically controlled to operate in linear increments of 0.001 inches, thereby producing reciprocating axial motion of shaft 14. A second mode of operation will produce movement of shaft 14 in increments of 0.0005 inches. The linear output force of linear actuator 10 applied to shaft 14 is inversely proportional to the linear step rate; that is, a faster step rate yields a lower linear force.
To minimize cost, instead of including control circuitry within housing 12, connection wires 16 are brought out of linear actuator 10 and terminated in connector 18. Connector 18 then mates with receptacle 20 on connection board 22, which is wired to connector 24 for external control of the apparatus.
Shaft 14 is coupled to ball joint 26 using threads 28 which mate with threads internal to ball joint 26. Ball joint 26 is straddled by bushing 30 and cup 32 which together are pressed into lever arm 34 at one end and held in place by spring washer 36 and retention clip 38 to form a split radial bushing. Nylon is the preferred choice of materials for bushing 30 and cup 32. This permits shaft 14 to move lever arm 34 without placing lateral stress on shaft 14 and consequently linear actuator 10, which would otherwise occur if shaft 14 were rigidly attached to lever arm 34. Additionally, there is enough holding force applied to ball joint 26 to prevent shaft 14 from spinning when linear actuator 10 is operated.
Attached to the opposite end of lever arm 34 is cam 36 which forms a lobe securely attached to, or machined from, lever arm 34. Cam 36 is cylindrical in shape and has a first face and a second face, one of the two faces mating with lever arm 34. Extending through cam 36 and between the two faces therein is opening 38, which is eccentrically located within cam 36. The off-center placement of opening 38 is critical to the operation of the apparatus. Bearing 40, which comprises a needle bearing, is pressed into opening 38. Use of a needle bearing minimizes backlash and improves accuracy. Pin 42 extends through opening 44 in the center of bearing 40 and into opening 46 in housing 12, thereby pivotally coupling lever arm 34 to housing 12.
Thus far the portion of the apparatus which causes movement of lever arm 34 and cam 36 has been described. Referring also to FIG. 3, when shaft 14 is extended or retracted by linear actuator 10, the axial motion of shaft 14 is transferred to lever arm 34. Cam 36 attached to lever arm 34 pivots about pin 42, thus transforming the axial motion of shaft 14 into rotational motion of cam 36. Because opening 38 in cam 36 is located off-center, the rotational motion of cam 36 and its surface 46 is eccentric.
Cam head 48 serves as a driver cam for the apparatus. Cam head 48 includes an opening 50 into which bearing 52 is inserted. Bearing 52 is a needle bearing of the same type as bearing 40. The opening in bearing 52 then fits over cam 36. Cam head 48 is oblong in shape and includes driver lobe 54. Driver lobe 54 has internal threads which mate with threads 56 on ink key 58. Cam head 48 is operated by cam 36 and transforms the eccentric rotational motion of cam 36 into axial motion imparted to ink key 58. Referring also to FIG. 3, when cam 36 rotates its eccentric motion causes cam head 48 to move along an axis substantially parallel to the longitudinal axis through shaft 14. This results in axial motion being imparted to ink key 58. The relationship of the sizes between cam 36 and cam head 48 results in a transformation which is linear with an approximate 12.5 to 1 reduction in distance of travel between ink key 58 and shaft 14; that is, when linear actuator 10 causes shaft 14 to move 0.5 inches, ink key 58 moves in the same direction a distance of approximately 0.04 inches.
FIG. 3 schematically shows the transformation of motion as described above. To retract ink key 58, linear actuator 10 is actuated to impart axial motion to shaft 14. When shaft 14 is retracted by linear actuator 10, lever 34 moves toward linear actuator 10. As a result, cam 36 rotates counterclockwise around pin 42. The eccentric rotation of cam 36 is transferred to cam head 48 where is it transformed into axial motion imparted to ink key 58. Ink key 58 then retracts, following the same direction of travel as shaft 14. This transformation of the rotational motion of cam 36 into substantially axial motion of cam head 48 occurs because cam 36 rotates only slightly. Otherwise, cam head 48 would rotate with cam 36. Extension of ink key 58 follows the same pattern of motion, except that linear actuator 10 is actuated to extend shaft 14 causing cam 36 to rotate clockwise.
Ink key 58 slides within bushing 60 which acts as a guide. Bushing 60 is securely mounted to housing 12 using a plurality of screws 62 extending through threaded openings 64. Bushing 60 has an external threads 66 for attaching the apparatus to an ink fountain and smooth bore openings 68 for tightening with a spanner wrench. It should be noted that the length of ink key 58 and the size of bushing 60 are configured to mate with each particular ink fountain and are the only components unique to each printing press. The remainder of the apparatus contains completely interchangeable components.
In order to prevent damage to the fountain blades and fountain roller in the ink fountain from excessive travel of ink key 58, the apparatus contains an adjustable stop 70. Stop 70 includes threads which mate with threaded opening 72 in lever arm 34. With proper adjustment, stop 70 extends through threaded opening 72 and engages anvil 74 in housing 12, thus limiting the amount of travel of lever arm 34. On initial installation and setup, the maximum travel of ink key 58 is set by using a feeler gauge to set a gap between the fountain roller and the fountain blade. Manual adjust knob 76 is then rotated until the proper gap is set. Stop 70 is then rotated until its bottoms out against anvil 74. Manual adjust knob 76 is also available for adjustment of the position of ink key 58 in the event of failure of linear actuator 10.
In operation, the present invention is used to vary the amount of ink on a fountain roller used in an offset printing process. The amount of ink required is determined by the pattern on the printing plates. Ink is deposited on the rollers from an ink reservoir using the flexible edge of a fountain blade. The distance the blade is away from the fountain roller determines the amount of ink deposited. The present invention is used to vary that distance, thereby varying the amount of ink used. Typically, the total gap between the fountain roller and the fountain blade is between 0.001 inches (no ink) and 0.03 inches (full ink).
Ink key 58 is retracted or extended to move the fountain blade and thereby vary the gap between the fountain blade and the fountain roller. Ink key 58 does not attach to the fountain blade to pull it back; rather, the fountain blade springs back toward its rest position (which is at a distance greater than the full ink position) when ink key 58 is retracted. Linear actuator 10 can be actuated in steps of 0.001 inches at a step rate of one hundred steps per second, thereby producing a force of approximately eighty ounces. The ratio of transformation from lever arm 34 to cam 36 to cam head 48 is 12.5 to 1, thereby imparting a force of approximately sixty-two and one-half pounds to ink key 58. This level of force, which is in turn imparted to the fountain blade, is sufficient to overcome binding of ink key 58 which may result from dried ink. Additionally, the transformation ratio is such that each 0.001 inch step of shaft 14 results in ink key 58 moving only 0.00008 inches. For example, in order to move ink key 58 and the fountain blade a distance of 0.029 inches, which is essentially the full range of adjustment of the gap between the fountain roller and the fountain blade, the system operator will actuate linear actuator 10 to produce 362.5 steps. This results in very precise movement of the fountain blade over a wide range of incremental settings.
In normal operation, linear actuator 10 requires a step pulse width of one millisecond to achieve factory specifications. It should be noted, however, that linear actuator 10 is capable of enhanced performance in that it can also operate in half-steps of 0.0005 inches. It should also be noted that linear actuator 10 has a holding force sufficient to maintain the position of ink key 58 and the fountain blade without continued actuation. This serves as a power saving feature. Power is applied only during adjustment of the position of ink key 58. In addition, an ink fountain requires multiple ink keys for adjustment of the fountain blade, thereby requiring multiple units of the present invention. The number of units required is determined by the length of the fountain roller and the spacing between ink keys. However, ink keys need only be adjusted one at a time. Therefore, by operating only one unit of the present invention at a time, total power consumption can be reduced. Additionally, multiplexing over a control cable to operate multiple linear actuators can be used to address and operate individual units.
External control of the apparatus is performed by a microprocessor based motion controller which includes a high current driver for linear actuator 10. The microprocessor records and processes the position of shaft 14 and moves shaft 14 on demand. Position feedback is not used, since the microprocessor provides positive control of linear actuator 14. The microprocessor also communicates with a host computer system where the operator of the printing apparatus will determine the desired position of each ink key. Communication with the host is facilitated with high speed serial data transfer.
The invention described herein eliminates the use of gears and, therefore, prevents imprecise control resulting from gear backlash. By using linear to linear motion, efficient transfer of motion can be thus be effected. Accordingly, it will be seen that this invention provides for complete and accurate positional control of an ink key and fountain blade in a printing apparatus. Although the description above contains many specificities, these should not be construed as limiting the scope of the invention but as merely providing illustrations of some of the presently preferred embodiments of this invention. Thus the scope of this invention should be determined by the appended claims and their legal equivalents.
|
A computer operated device for controlling an ink key (58) used to adjust the position of a fountain blade used in an ink fountain of a printing apparatus. A linear actuator (10) imparts reciprocating axial motion to a shaft (14) which in turn actuates a lever arm (34). The lever arm (34) operates an eccentrically pivoting cam (36) which transforms the axial motion from the linear actuator (10) into eccentric rotational motion. A second cam (48) reconverts the eccentric rotational motion of the first cam (36) into reciprocating axial motion and imparts that motion to the ink key (58) with a substantial reduction in distance of travel relative to that of the shaft (14) of the linear actuator (10), thereby permitting precise incremental adjustment of the position of the ink key (58).
| 1
|
BACKGROUND OF THE INVENTION
1. Field
The invention relates to an assembly for controlling fluid delivery via a syringe. In particular, the invention relates to a drive system coupled to the plunger of a syringe which is monitored and contorlled by an optical/electronic feedback system for precisely determining and controlling the position and motion (velocity and acceleration) of the plunger.
2. State of the Art
Present commercial clinical laboratory applications of syringe delivery systems typically include a stepper motor attached to a drive mechanism which is coupled to the plunger of a syringe. A typical example of such systems are digitial pumps such as the Cavro Modular Digital Pump, Model SB, manufactured and sold by Cavro Scientific Instruments, Inc., Sunnyvale California.
In conventional systems, the stepper motor usually has increments of resolution of not less than 1.8° per step (approximately 200 steps per revolution). Furthermore, no positional feedback loop is used to ensure accuracy and detect errors of motion. In practice it is not unusual, for example, that the control to the stepper motor will indicate that a determined number of programmed steps has been taken, but that the stepper motor in fact does not rotate the number of steps programmed. An error in the position of the plunger thus occurs and concomitantly an error in the amount and rate of delivery of fluid from the syringe will occur also. Accordingly, there is a need for an assembly which accurately and precisely controls and monitors the position and motion of the syringe plunger so that accurate amounts of fluid can be delivered. The present invention is considered to provide such assembly.
SUMMARY OF THE INVENTION
The present invention comprehends a syringe drive assembly comprising a syringe, including a syringe body and a plunger moveable within the body, drive means operably coupled to the plunger, primary control means directly coupled to the drive means, and sensing means associated with the drive means and the primary control means, the sensing means being operable to sense the temporal position of the drive means. The sensing means may sense the temporal position of the drive means indirectly from the temporal position of the primary control means. The sensing means includes feedback control means responsive to the sensed position of the primary control means of the drive means. In one aspect, the primary control means includes a motor having a rotatable shaft on which the sensing means is supported or fixed to generate a signal responsive to the temporal position of the shaft. The signal is utilized by the primary control means to further control the position and motion of the plunger. In a preferred embodiment, the sensing means includes an optical/electronic encoder coupled to a secondary controller for controlling input to the primary control means.
In another aspect, the syringe drive assembly comprises a base, a syringe having a body supported on the base and a plunger moveable within the body, drive means supported on the base and coupled to the plunger, motor means having a shaft coupled to the drive means, and sensing means associated with the shaft of the motor means for sensing the position of the shaft. The syringe drive assembly can include stabilizing means associated with the base and the drive means to facilitate linear movement of the plunger. The syringe drive assembly may include a support surface on the base which is parallel to the plunger, a slot in the parallel support surface and a bearing that rides within the slot as the plunger and the linear drive means moves in unison. Other aspects of the invention will be apparent from the figures and the detailed description of the invention which follows.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front elevational view of the syringe drive assembly of the present invention;
FIG. 2 is a side view of the invention illustrated in FIG. 1;
FIG. 3 is a view from the other side partially cut away, particularly illustrating the linear drive means and the linear guide means of the present invention; and
FIG. 4 is a block diagram illustrating the control functions useful in the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The invention deals with a syringe assembly for accurately and precisely controlling the position and motion of a plunger in a syringe body to deliver precise fluid volumes in a predetermined manner over time. The assembly includes drive means operably coupled to the plunger and a primary control means coupled to the drive means. The primary control means includes a motor, preferably a D-C motor, and a microprocessor control that controls both the position of the motor (i.e. the angular position of the motor shaft in its revolutionary movement) and the motion of the motor (i.e the angular acceleration and velocity of the motor shaft).
Since in a conventional syringe/plunger assembly the plunger is adapted to move linearly within the syringe body, the drive means utilzes elements that provide a linear drive system for the plunger. The plunger usually is required to move in one direction to draw fluid into the syringe body and in a second, opposite direction to deliver fluid from the syringe body. The drive means conveniently includes means for coupling the primary control means, in which the motor provides rotational movement, to the plunger while translating the rotational movement into linear movement. This is accomplished by directly coupling the output shaft of the motor to a lead screw. Means are provided on the lead screw to linearly traverse the lead screw when the lead screw rotates. Typically, a threaded nut is provided that is threaded on the lead screw and is attached by a suitable coupling means to the plunger. When the motor and lead screw rotate, the threaded nut traverses the lead screw and moves the plunger through the coupling mechanism.
Linear movement of the plunger if facilitated by the bearing block and support bearings that ride on a linear guide rod to promote movement parallel to that of the plunger. The threaded nut is allowed to "float" relative to the bearing block which functions as a portion of the coupling means and such a function dramatically reduces wear between the syringe plunger and the syringe body. Such a "float" typically is accomplished by attaching the nut to the bearing block by means of shoulder bolts or the like that permit relative movement between the bearing block and the threaded nut.
Additional stabilizing means can be provided between the aforementioned guide means and the plunger to further assure linear movement of the plunger. Such stabilizing means are conveniently provided by bearing means, which may include a slotted bearing track to retain a bearing means on a support coupled to the plunger between the guide means and the plunger.
The assembly also includes sensing means for detecting the temporal position of the plunger. Such means can detect both position and motion (i.e. velocity and acceleration) of the plunger. Most conveniently, sensing of the plunger parameters is accomplished indirectly by monitoring the position and motion of the primary control means while directly coupling the primary control means to the drive means. This is done by directly coupling the motor output shaft to the lead screw by a cogged belt, e.g. timing belt, or the like. By "directly coupling" is meant that there is substantially no lost motion between movement of the motor output shaft and the lead screw other than what might be experienced from usual belt or gear lash. The sensing means conveniently includes a signal generating means affixed to the motor output shaft that monitors the angular movement of the motor output shaft. Typically, one can use an optical/electronic encoder coupled to a microprocessor to sense the shaft position and instruct the primary control means to control the output shaft position. Feedback control means are provided within the primary control means for accurately and precisely controlling output shaft position and motion.
With particular reference to FIGS. 1, 2 and 3, the present invention includes a base 10 on which is supported a syringe 12. The base 10 includes a support plate 14, a face plate 16 and leg extensions 18 and 20. The leg extension 20 of face plate 16 can of course be intergally formed therewith. Extensions 18 and 20 provide space beneath support plate 14 for various hardware included in the present invention.
Syringe 12 includes a syringe body 24 in which is moveably located a syringe plunger 26. Syringe plunger 26 is connected to a support shaft 28 which has mounted thereon a stabilizing bearing 30, e.g. ball bearings or sliding bearings, which is adapted to ride in a bearing groove 22 in face plate 16. The end of shaft 28 remote from the syringe plunger 26 is attached to a bearing block 32, conventionally by simply being inserted into a hole near the bottom of the bearing block but other attachment means could be used as well. The bearing block 32 includes a first linear bearing 34 and a second linear bearing 36, e.g. each may be linear ball bearings, which are adapted to move along guide rod 38. An extension of bearing block 32 is provided by a sleeve 42 of which is attached a nut 46 having a flange 48. Nut 46 is threaded to mate with lead screw 44 and has a flange 48 formed thereon through which screws 50 attach nut 46 to sleeve 42. Screws 50 are shoulder screws which permit nut 46 to float relative to sleeve 42. In that manner, skewing of bearing block 32 by the turning motion of lead screw 44 and nut 46 is prevented. Accordingly, bearing block 32 rides easily along guide rod 38, preferably cylindrical, and facilitates linear movement of the plunger 26 in syringe body 24 greatly reducing the wear between the two. Extensive wear between plunger 26 and syringe body 24 will result in leakage that ultimately becomes unacceptable to the user. The present structure greatly minimizes wear, substantially increasing the cycle life of the syringe assembly.
Attached to one end of lead screw 44 is a pulley 58 which itself is operatively coupled via a belt 60 to another pulley 56 mounted on the end of the motor output shaft 54 of motor 52. Motor 52 is mounted on support plate 14. Belt 60 typically is a positive drive belt like a cogged or toothed belt, e.g. a timing belt or timing chain, which is adapted to mate with complimentary grooves in pulleys 56 and 58 to provide a direct coupling between the output shaft 54 of motor 52 and lead screw 44. Such direct coupling substantially prevents any slipping of belt 60 and reduces lost motion between pulley 56 and pulley 58. A thumb wheel 62 is provided at the end of lead screw 44 to provide for manual operation of the lead scew when necessary. The thumb wheel function allows the operator to manipulate the syringe while the power is off, for example to change seals between the plunger and the syringe body.
Directly coupled to the output shaft 54 is an encoder 64 which is adapted to interface with a control system, typically a microprocessor, to monitor the exact position of motor output shaft 54. A variety of encoder/control systems are available, for example the HCTL-1000 from Hewlett Packard, Palo Alto, California and the Model 4327 Servo Motor Controller of Technology 80 Inc., Minneapolis, Minnesota are useful.
The fluid delivery system additionally includes a valve 66, that may be two-way, having an inlet 72 and outlet 74, and a valve motor 68, typically a DC motor operated at less than 48 volts, on which is mounted a valve motor control 69. A support block 70 attached to face plate 16 is utilized to support the valve motor 68 and valve motor control 69. Valve motor control 69 interfaces with a microprocessor control system such that the position of valve 66 is appropriately controlled when fluid is being added to the syringe or dispensed therefrom.
The control mechanism is illustrated schematically in FIG. 4. As described and illustrated there, the syringe drive 100 is controlled by a motor means 102 which is coupled to an encoder 104. Encoder 104 transmits signals to motor control 106 which utilizes such signals for the primary control of motor means 102. In addition, a command control 108 inputs information to motor control 106 to provide the desired position and motion control of syringe 100. In actual practice, the command control 108 controls voltage to a DC motor 52 and tracks the position of encoder 64. Encoder 64 typically and illustratively is an optical system that may commercially obtained, including a wheel having a grating disposed thereon which is interposed between a light source, for example a light emitting diode and a sensor, typically a phototransistor. Since the wheel is connected directly to the motor shaft, and the motor shaft rotates, pulses are created between the source and the sensor which monitors acceleration, deceleration and total movement. Those signals are fed into motor control 106 which monitors the position and the motion (velocity and acceleration) of motor shaft 54. Since motor shaft 54 is directly coupled to lead screw 44, movement and position of motor shaft 54 directly relates to movement and position of lead screw 44. Additionally, since bearing block 32 is directly coupled to syringe plunger 26, accurate monitoring of the position and motion of syringe plunger 26 is effected. The difference between the desired position of the motor and the actual position of the motor as determined by the encoder is the position error. By utilizing an encoder wheel with 500 slots and a sensor source combination with two light emitting diodes 90° out of phase, up to 2,000 positions of the motor shaft can be monitored. Typically, the lead screw will have 16/18 threads per inch. although coarser threading may be used but then generally with a finer grating system on the encoder wheel. Syringe volumes may range from 10 microliters to hundreds of milliliters (although larger volumes will generally require the ganging of syringes of lesser volume to maintain delivery accuracy), but most typically not more than 5 to 10 milliliters for clinical laboratory applications. The number of pulses available in a syringe stroke of approximately 6 centimeters can approximate over 100,000. Such fine tuning provides for very accurate control of syringe plunger 26.
In operation, to add fluid to the syringe, command control 108 is set by an operator to drive ouput shaft 54 of motor 52 to a determined position. At the same time, command control 108 will instruct valve motor control 69 to open inlet 72 to allow liquid to be drawn into syringe body 24 from a source (not shown). Upon actuation by the operator, motor output shaft 54 will be actuated to move a predetermined position in accordance with a programmed motion. As output shaft 54 rotates, motion is transferred to lead screw 44 via pulleys 56 and 58 and belt 60. As lead screw 44 rotates, it will drive nut 46, which, because of its attachment to sleeve 42, drives bearing block 32 along guide rod 38. As the bearing block 32 moves downwardly, it pulls plunger 26 through the direct coupling with support shaft 28. Bearing 30 rides in bearing slot 22 as plunger 26 descends.
As output shaft 54 rotates, encoder 64 sends signals, i.e. a pulse train, back to motor control 106. The controller compares the decoded motor position with the commanded position and determines the position error. The controller utilizes the position error (and usually a derivative signal) to form a motor command which adjusts the motion of motor 52 based on that feedback signal. When the plunger 26 has reached the end of its travel, motor control 106 stops motor 52 since there is no longer any difference between the actual position of the motor and the commanded position of the motor. The dispensing of the liquid is controlled by the command control 108 in substantially the manner described previously. Valve 66 switches to outlet 74 and output shaft 54 is rotated in the opposite direction to move plunger 26 upwardly. Motion and control of the upward movement of the plunger 26 is effected and monitored as described above.
For illustration purposes encoder 64 has been placed on the end of motor shaft 54. The encoder 64 could also be placed on the end of lead screw 44. Various other mechanisms of direct coupling of the motor 52 to lead screw 54, for example direct gearing and the like, can be provided .
While the foregoing invention has been described with reference to the drawings, and the presently preferred embodiments, there are intended to be illustrative and not intended to limit the scope of the invention claimed. Various modifications or changes to the methods and apparatus described herein will be apparent to those skilled in the art and are intended to be included and encompassed by the claims appended hereto.
|
An assembly is described for accurately and precisely controlling the position of a plunger in a syringe to deliver precise fluid volumes. The assembly includes a motor coupled to a lead screw that drives a bearing block along a linear guide rod to move the plunger of the syringe in a linear fashion. The position of the plunger is accurately controlled by attaching a digital encoder to the rotating motor shaft. The encoder and associated electronics output to a controlling processor that generates a series of regular pulses, typically 300 to 500 responsive to each motor revolution. Utilizing appropriate gear ratios of the motor and the lead screw, the number of pulses per full syringe stroke in typical applications can be on the order of one hundred thousand. The final position and the motion of the plunger (velocity and acceleration) can be controlled to within a few encoder pulses, thus precisely controlling the rate of delivery of the fluid and the volume of the fluid actually delivered by the syringe. A closed positive feedback system is utilized to detect positional errors and obtain improved precision and accuracy.
| 8
|
FIELD OF THE INVENTION
The invention relates to a luminaire. More specifically, the invention relates to a luminaire combining ambient light with task light.
BACKGROUND OF THE INVENTION
Luminaires that combine ambient light with task light are known in the art. Known are for example devices that combine a reading light (e.g. based on a halogen light source) that directs and focuses light substantially downwards to illuminate a book and a background light (e.g. an incandescent or halogen light source) that directs light substantially upwards to a ceiling for providing diffuse background light. Typically each light source is provided with its own light fitting wherein both light fittings may be combined into a single luminaire. In general, both light sources—i.e. the reading light and the background light—are individually controllable. For example the reading light may have an individual on/off switch and the background light may be provided with an integrated on/off dimmer switch.
In the above type of luminaires the different light sources are point sources meaning that illumination originated from a singular point. Additional reflectors and/or diffusers may be used to reshape the light beam. Nonetheless, the light distribution profile across each light beam—the reading light beam and the background light beam—is generally constant. This therefore limits the application of both light sources to “uniform illumination”.
SUMMARY OF THE INVENTION
For the purpose of describing the invention, the term “task light” means light suitable for performing a task, such as studying, office work, playing cards, etc. For the purpose of describing the invention, the term “ambient light” means light suitable for creating a background illumination (e.g. indirect light though illumination of surrounding elements such as ceilings or walls) or a decorative illumination (e.g. direct light having an added value through its specific color and/or shape combination as for example known from wall mounted decorative luminaires). In general, task light and ambient light are experienced as a different quality of light.
According to one aspect of the invention, a luminaire is provided that comprises a task light module for providing task light and an ambient light module for providing ambient or decorative light, wherein the task light module comprises at least one point light source and the ambient light module comprises at least one surface light source. In a preferred embodiment the task light module comprises an LED (Light Emitting Diode light source) and the ambient light module comprises an OLED (Organic Light Emitting Diode light source).
In a further aspect of the invention, the luminaire comprises a lighting fixture comprising the task light module and the ambient light module and a base for positioning the luminaire in an environment and for supporting a lighting fixture. The base may be specifically adapted for table top mounting, floor mounting, wall mounting or ceiling mounting. The lighting fixture is preferably moveable with respect to the base. This movement may be used for redirecting the task and/or ambient light into the environment. The movement may also be used to dynamically control the ratio of amount of task light versus amount of ambient light produced by each of the light modules. For example, the luminaire's light output may be 100% ambient light versus 0% task light when the lighting fixture is in a first position (e.g. a vertical position for table top or floor mounted luminaires), and 100% task light versus 0% ambient light when the lighting fixture is in an second position (e.g. a horizontal position for table top or floor mounted luminaires). For that purpose, position and/or movement detection means may be provided to detect the position and/or displacement of the lighting fixture relative to the base and set the light output for each of the at least one task light source or at least one ambient light source based on the lighting fixture's position or displacement. Position and/or movement detection means, such as rotation sensors or MEMS based accelerometers, are well known in the art and may be integrated in the lighting fixture. A microprocessor may be integrated in the lighting fixture to control the light output of the different light sources based on the lighting fixture's position and/or displacement. An advantage of this type of light control is that it creates an intuitive direct link between a physical interaction of a user with the luminaire (e.g. putting the lighting fixture in a reading position) and the desired light output (e.g. producing task light for reading), without requiring an additional user interface such as dimmers, etc. In other words, as the user moves the lighting fixture from a vertical position to a horizontal position the light output automatically changes from ambient/decorative light to task light. The correspondence between the lighting fixture's position and type of light output (i.e. ambient light, task light or a combination thereof) and the transition curves may be preset for each type of luminaire of may be configurable or selectable by the user. The transition curves may include one or more hysteresis areas around specific lighting fixture positions, wherein the light output characteristics don't change. These hysteresis areas in fact correspond to tolerance for setting a desired lighting fixture positions or selecting a desired light output by the user. For example a hysteresis of about ±10 degrees rotation angle around the lighting fixture position for 100% task light makes it easier for the user to set this light condition and possibly to direct the light output within the limits of ±10 degrees rotation angle without effecting the amount or type of light output.
Switching the luminaire on/off may be done independent from the position or movement of the lighting fixture, e.g. by using an independent proximity sensor located in the base or on the lighting fixture for on/off tapping control of the luminaire, or may be integrated in the position or movement control of the lighting fixture in that for example a specific position, referred to as a home position, may be associated with an off state of the luminaire. In the latter case, the luminaire may switch on automatically when the lighting fixture is moved out of its home position. Also the home position may be provided with a hysteresis to create some tolerance in operating the luminaire.
The lighting fixture may have a blade shaped appearance, i.e. a structure of which the average thickness is significantly smaller than the average length and width. This blade will be further referred to as a “light blade”. In a preferred embodiment the light blade is significantly longer than it is wide, i.e. the aspect ratio of the average length versus average width of the light blade is significantly higher than 1:1, preferably higher than 5:1 and more preferably higher than 10:1.
The light blade may be directly connected to the base of the luminaire by means of a hinge, allowing the light blade to rotate around a pivoting point, or may be linked indirectly to the base of the luminaire by means of an intermediate member such as a supporting arm. In the latter case, the light blade may be pivotally connected to one end of the supporting arm whereas the other end of the supporting arm may itself be pivotally or rigidly connected to the base.
The advantage of a blade shaped lighting fixture is that the lighting fixture includes at least one substantially flat surface and at least one surrounding edge into which one or more light sources may be integrated. Different design options are possible, each providing a different combination of light output. For example, a blade allows the integration of a plurality of task light sources along an edge of the blade and/or a plurality of ambient light sources integrated in a flat surface of the blade. More specifically, the ambient light may for example be created from a linear array of individual controllable square-size OLED light sources integrated in the blade surface, each OLED having substantially the size of the light blade width. The task light may for example be generated from a linear array of individually controllable LED's integrated in an edge of the blade or into the opposite blade surface of the ambient light. Also a plurality of arrays of OLED or LED light sources may be used. The array of light sources enables a whole range of different static/dynamic light effects added to task light and/or ambient light. An example of a static light effect may be a light beam producing a linear light output gradient dark-to-bright across the light blade from left to right. An example of a dynamic light effect may be a light beam producing a running light across the light blade from left to right or the simulation of a cloudy sky moving over the light blade. Dynamic lighting configurations may preferably be incorporated for the ambient light module only. A microprocessor may be use to control all of the individual light sources to produce the appropriate light effect. The microprocessor preferably is integrated in the blade shaped light fixture. There may be different ways of implementing a user interaction for selecting or activating a particular light effect. In one example, a user interface that is integral with the light blade may be used. This user interface may be based on a touch pad that is integrated with the light blade, a proximity sensor which is integrated in an edge of the blade or at an end of one of the arrays of lighting sources. Operating the touch pad or tapping the area adjacent the proximity sensor may instruct the microprocessor to switch to a different light effect or cycle through a set of preconfigured light effects. In another example, a user interaction may be set up using a wireless communication with the microprocessor for controlling the light effects produced by the light sources.
A further aspect of the invention includes the use of colored light in the ambient and/or task light. For example, the ambient light may include some additional red (to ease the mind), whereas the task light may include some additional blue (to enhance focus). OLED technology is very well suitable for producing colored light, for example be using stacked RGB OLED structures that are, next to intensity, also color controllable. In LED technology, RGB LED assemblies may be used—possibly in addition to white LEDs—to create an array of light sources. The color of the ambient light and/or the task light may be fixed or user controllable. Different way of controlling color and an associated user interface are known in the art. One example is the color ring used with the Philips LivingColors for intuitive remote control of the generated light color.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a table top or floor mounted luminaire according to the invention.
FIG. 2 shows wall mounted luminaire according to the invention.
DETAILED DESCRIPTION
FIG. 1 discloses a table top or floor mounted luminaire 1 according to the invention. It comprises a base 2 for positioning the luminaire on the table or on the floor and a lighting fixture 4 in the form of a blade. The lighting fixture 4 is pivotally connected to supporting arm 3 , which itself is pivotally connected to the base 2 . As illustrated in the FIGS. 1A through 1C , the lighting fixture 4 can be rotated relative to supporting arm 3 . The lighting fixture 4 comprises an array of OLED light sources 5 integrated in a surface of the blade shaped lighting fixture 4 . Illustrated in FIG. 1C , the lighting fixture 4 also comprises an array of LED light sources 6 integrated in the opposite surface of the blade shaped lighting fixture 4 . When the lighting fixture 4 is in a substantially vertical position (illustrated FIG. 1A ), the luminaire produces an ‘ambient light only’ effect from its array of OLED light sources. When the lighting fixture is in a substantially horizontal position (illustrated in FIG. 1C ), the luminaire produces a ‘task light only’ effect from its array of LED light sources. The transition from ‘ambient light only’ to ‘task light only’ may be linear with the rotation angle of the lighting fixture 4 but may also be non-linear. In one example, and only considering a rotation of the lighting fixture 4 between 0 degrees and 90 degrees, the light effect ‘ambient light only’ is maintained until the lighting fixture is rotated 45 degrees, after which the ambient light gradually turns into task light. The light effect ‘task light only’ may be reached when the rotation angle is 80 degrees and above. In some embodiments of the invention, at least one of a rotation, a translation or a position of the lighting fixture relative to the base is detected by a sensor 7 and a light output from the task light module and a light output from the ambient light module, is dynamically controlled by a processor 8 based on an output from the sensor 7 .
Similarly, FIG. 2 illustrates a wall mounted luminaire 11 according to the invention. It comprises a base 12 for mounting the luminaire on the wall and a lighting fixture 14 in the form of a blade. The lighting fixture 14 is pivotally connected to supporting arm 13 , which itself is pivotally connected to the base 12 . As illustrated in the FIGS. 2A through 2C , the lighting fixture 14 can be rotated relative to supporting arm 13 and/or relative to the base 12 . The lighting fixture 14 comprises an array of OLED light sources 15 integrated in a surface of the blade shaped lighting fixture 14 . Illustrated in FIG. 2C , the lighting fixture 14 also comprises an array of LED light sources 16 integrated in an edge, preferably the downward facing edge, of the blade shaped lighting fixture 14 . When the lighting fixture 14 is in a substantially aligned position with the base 12 and the supporting arm 13 , i.e. substantially positioned against the wall (illustrated in FIG. 1A ), the luminaire produces an ‘ambient light only’ effect from its array of OLED light sources. When the lighting fixture is moved away from the wall (illustrated in FIG. 1C ), the luminaire produces a ‘task light only’ effect from its array of LED light sources. The transition from ‘ambient light only’ to ‘task light only’ may be linear with the rotation angle of the lighting fixture 14 relative to the base 12 —de facto relative to the wall—but may also be non-linear. In one example, a ‘task light’ effect may be produces when the lighting fixture 14 is moved into a position window 75 degrees to 115 degrees relative to the base 12 , i.e. perpendicular to the base 12 including a tolerance window of ±15 degrees.
As illustrated in FIG. 2C , the lighting fixture 14 may have multiple arrays of light sources for producing an ambient light effect. In the embodiment depicted, the lighting fixture 14 includes an array of OLED light sources 15 (a total of 18 OLEDs is shown) integrated in a first surface of the blade shaped lighting fixture 14 and an array of side emitting light guides 17 (a total of 3 light guides is shown) integrated in the opposite surface of the blade shaped lighting fixture 14 . Each light guides may for example be optically coupled with a LED light source at one of its ends. The embodiment of FIG. 2 illustrates a possible combination of decorative light, produced by the array of OLEDs facing away from the wall, and background light, produced by the array of light guides facing towards the wall. The combined decorative and background lighting effect may be active when the lighting fixture 14 is moved substantially parallel (including for example a tolerance window of ±15 degrees of rotation) to the base 12 .
|
A luminaire is disclosed that allows a transfer from ambient light to task light through physical manipulation by the user. The luminaire comprises OLED light sources for generating an ambient light effect and LED light sources for generating a task light effect.
| 5
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a button feeding device, and more particularly to a button feeding device in the form of an independent attachment for a button attaching machine for providing proper alignment of buttons transferred from a magazine.
2. Description of Related Art
A button feeding device is disclosed in Federal Republic of Germany Pat. No. 10 55 335, equivalent to U.S. Pat. No. 2,921,544 in which a button is taken from a conventional magazine, is slid into the filling jaws of an alignment station and is turned momentarily by a lowerable driver disk, which carries out turning movements of about 180°, until the holes in the button are received by the pins of a pin holder. The pin holder is fastened on the end of a connecting rod which is part of a flat, four-pivot crank mechanism. In this way, the pin holder passes over a path of movement having the shape of approximately a quarter circle which terminates in an approximately linear section only at the end of said movement.
This known button feeding device has the following disadvantages:
1. Since the pin holder is movable only in the horizontal plane, the button clamp must be lifted briefly after the pin holder has transferred the button into the button clamp. Without this lifting movement, which delays the course of the operation, it is not possible to withdraw the button from the pin holder.
2. The driver disk, which carries out rotary oscillations, cannot be shifted towards the center of rotation of its drive.
3. The pivot points of the crank mechanism which moves the pin holder are subject to wear, particularly upon continuous use, and tend to become noisy.
In another button feeding device, disclosed in German Democratic Republic Pat. No. 34 682, a button, after being removed from a magazine, drops into an alignment station formed by a momentarily lowerable pot and is turned by a plate which carries out a rotary movement until the pins of the pin holder which is arranged above the button engage in the holes in the button. The pin holder is guided on a parabolic path by a four-pivot slider-crank mechanism. This device has the same disadvantages with respect to susceptibility to wear and noise that were noted above. Furthermore, it is not possible with the device of German Democratic Republic Pat. No. 34 682 to displace the plate from the center of rotation of its drive.
SUMMARY OF THE INVENTION
Accordingly, a principal object of the invention is to avoid the above-mentioned disadvantages of the known prior art devices.
In accordance with a preferred embodiment of the invention, a button feeding device includes a button alignment shaft which is displaceable with respect to the center of rotation of its drive. The device has a pin holder which aligns the button and transfers it into the button clamp, the pin holder carrying out a linear quadrangular movement which takes place over a non-curved path.
With the button feeding device of the invention, it is possible to briefly lift the button slightly upward by the pins of the pin holder, turn the button by the button alignment shaft around its axis of symmetry only until the pins enter the holes in the button, and then transfer the button, by a carriage assembly which has only one rotary point and two slide points, on a non-curved path into the button clamp. No additional lifting of the button clamp is necessary upon the removal of the button from the pin holder, in view of the quadrangular movement of the pin holder.
According to one aspect of the invention, there is provided a button feeding device for aligning a button and placing it in sewing position. There are receiving means for receiving a button from a magazine and locating it in an alignment station. Driver disk means at the alignment station rotate the button to align it so that holes in the button are in a desired position. Button clamp means at a sewing station receive the button after alignment and place the button at a sewing position. Pin holder means hold the button in operative engagement with the driver disk means for being aligned thereby and for transferring the button to the button clamp means after alignment. Alignment shaft means, on which said driver disk means is mounted for rotation, have a first longitudinal axis. There are drive means having a second longitudinal axis for rotating the alignment shaft means. The alignment shaft means is displaceable such that the second longitudinal axis is displaceable with respect to the first longitudinal axis, while still being rotatable by the drive means.
According to a further aspect of the invention, the button feeding device comprises carriage means on which the pin holder means is mounted for being moved substantially horizontally between the alignment station and the sewing station. The pin holder means is further moved substantially vertically upward at the alignment station to bring the button into operative engagement with the driver disk means and it is moved substantially vertically downward at the sewing station for transferring the button to the button clamp means. The pin holder means is thereby moved by the carriage means in a substantially linear quadrangular path.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects, features and advantages of the invention will be seen from the following detailed description of a preferred embodiment thereof, with reference to the drawings, in which:
FIG. 1 is a perspective view of a complete button feeding device according to an embodiment of the invention, the button clamp mechanism being partially indicated;
FIG. 2 is a left side view of the carriage, shown in its forward position with the cover plate removed, the drive for the button alignment shaft and the button clamp not being shown;
FIG. 3 is a right side view of the carriage, the drive for the button alignment shaft and the button clamp not being shown; and
FIG. 4 is a perspective view of a forward portion of the button feeding device, including the button alignment shaft.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a button feed device, which in this embodiment is an attachment to be arranged alongside a known button sewing machine (not shown). A frame 31 comprising a plate 39 and two side parts 40, 41 serves as basic structure for the button feeding device and is to be firmly connected to the protruding cylindrical sewing-material support arm (now shown) of the button attaching machine.
On the top of the plate 39 there is provided, as shown in FIG. 1, a guide channel 36 which conducts buttons coming from a fixed magazine (not shown) to an alignment station just in front of the sewing point. The alignment station includes a vertically arranged button alignment shaft 2 and two guide jaws 38, mounted below the plate 39, which receive and guide a button 37 which has been brought into the alignment station, without holding it fast. The guide jaws 38 can be adjusted to center them on the center of rotation of the button alignment shaft 2 by adjustment screws 44. By suitable slight adjustments of the guide jaws 38, the alignment station can easily be set for different outside diameters of buttons. Further description of this adjustment of the guide jaws 38 is unnecessary since it is effected in a manner similar to the known adjustment of the button clamps 35.
Above the plate 39 there is provided an angle member 13 in which the button alignment shaft 2 is rotatably mounted (see FIGS. 1 and 4). Furthermore, a column 42 is firmly connected to the plate 39 and receives an extension 43. On the extension 43 is mounted a drive 1 which consists of a separate small motor 4, operating independently of the sewing drive, with a reduction gearing behind it. At the output of the reduction gearing there is arranged a stub shaft 5 which is rotatably mounted in the extension 43 and has a slot 10 on its free end.
The button alignment shaft includes a bolt 12 which is mounted for rotation, but nonremovably, in the angle member 13. Mounted on an upper end of the bolt 12 is a pin 6, which has a slot 11 near the bolt 12 (see FIG. 4). A driver disk 34 consisting of resilient material is firmly connected to the bottom of the bolt 12, as shown in FIG. 4.
After the loosening of its fastening screws the angle member 13 can be displaced horizontally on the plate 39, whereby the longitudinal axis of the button alignment shaft 2 can be adjusted within well-defined limits with respect to the center of rotation of the stub shaft 5. In this way, functionally correct alignment of the button alignment shaft 2 with the center of the two guide jaws 38 is possible.
Rotary movement is transmitted from the drive 1 to the button alignment shaft 2 by a coil spring 7, which at its upper and lower ends has linearly bent arms 8 and 9, respectively, extending through its center axis. The arm 8 is received in form-locked manner by the slot 10 and the arm 9 is received in form-locked manner by the slot 11. Said coil spring 7 permits, on the one hand, the adjustment of the button alignment shaft 2 towards the center of rotation of the drive 1, i.e., towards the center of rotation of the stub shaft 5; while, on the other hand, by the removal of the coil spring 7, the rapid installation and removal of the button clamp 35 is assured.
The linear transfer of the aligned button 37 from the alignment station to its correct position for sewing in the button clamp 35, which can be noted in FIG. 4, is effected by a carriage 15 which is displaceable on a slide rod 14 mounted between the side parts 40, 41. To prevent the carriage 15 from rotating about the slide rod 14, the carriage 15 includes a block 45 which is mounted on a second slide rod 46. The slide rod 46 extends parallel to the slide rod 14 and is also mounted between the side parts 40, 41. For moving the carriage 15 there is provided a double-acting cylinder 18, actuatable by a pressure fluid, which acts on an extension 47 which is rigidly attached to the carriage 15, which cylinder can be acted on in a known manner by compressed air or a hydraulic fluid. The control of the action of the pressure fluid on the cylinder 18, for example by means of solenoid valves, is well known and will not be described in detail here.
Within the carriage 15 there is force-fitted a horizontally arranged pin 19 on which a rocker 20 is swingably mounted. The rocker has two arms 48, 49 of equal length, in each of which there is an adjustable stop 28 which limits the swinging motion of the rocker 20. On an extension 27 which extends above the front of the rocker 20 there is fastened a support angle member 21. After loosening its attachment screws the support angle member 21 can be set in different positions within a well-defined region. It is advisable to provide a leaf spring 51 below the support angle member 21, at its front end, to which spring a pin holder 3 is fastened, the pins of which thus press relatively gently against the bottom of the button 37 which is to be aligned.
Rigidly connected to the rocker 20 is an angle member 52, visible in FIG. 3, having lower arms 53 which form a U-shape and thereby grip around the slide rod 46. Four washers 54 are provided on said slide rod. Compression springs 16, 17 are also placed on the slide rod 46 between the washers 54 and the side parts 40, 41.
A cover plate 33 is removably fastened to the carriage 15. Behind this cover plate is a continuous groove of rectangular cross-section extending parallel to the slide rod 14, said groove receiving two slides 22. Between these slides there is arranged a compression spring 23 which presses one slide 22 to the front and the other to the rear. Furthermore, the forward slide 22 (see FIG. 2) has a projecting cylindrical pin 24 and the rear slide has a projecting pin 24'. The two pins 24, 24' pass through the outer walls of the carriage 15.
Furthermore, as shown in FIGS. 1 and 2, two push rods 25 which are movable vertically at right angles to the slides 22 are mounted in suitably shaped grooves in the carriage 15, the lower ends of each of the push rods 25 resting on one of the slides 22. Each of these push rods 25 has a slot 26 into which one of the end pieces of the arm 48 or 49 of the rocker 20 engages in form-locked fashion.
In the side part 40 there is provided an adjustable stop 29 which limits the forward position of the carriage 15. There is also arranged in the side part 40 another adjustable stop 30 against which the pin 24 strikes before reaching the forward position of the carriage 15. In the side part 41 an adjustable stop 32 is also provided against which the pin 24' strikes before reaching the rear position of the carriage 15. Each of the stops 28, 29, 30 and 32 includes an adjustment screw, the adjusted position of which is secured by a lock nut.
The manner of operation of the button feeding device will now be described. In the operation of the button attaching machine, buttons are continuously removed automatically in a known manner from a stationary magazine, and then pass by their own weight, through a known flexible guide hose 50 made of spring steel, into a guide channel 36. In order to assist in the passing of the buttons, a compressed air nozzle (not shown in the drawing) is arranged on a side of the guide channel 36. The jet of air which escapes from the nozzle causes the button 37 to pass freely through the guide channel 36, as a result of which the button 37 passes reliably into the guide jaws of the alignment station.
At the same time as the introduction of a button 37 into the alignment station, the carriage 15 passes, by corresponding actuation of the cylinder 18, into its rearward position, the compression spring 17 being increasingly compressed. Shortly before reaching the rearward position, the pin 24' comes against the stop 32, as a result of which the slide 22 pushes, against the action of the compression spring 23, in the direction opposite the instantaneous direction of motion of the carriage 15 until the lower surface of the rear push rod 25 no longer rests against the top of the rear slide 22. The rear push rod 25 is immediately pushed downwards in the direction towards the pin 24' by the compression spring 17 acting through the angle member 52, which thereby relaxes the spring 17 to some extent. As a result of the downward movement of the rear push rod 25, the front push rod 25 is brought by the rocker 20 into its upper position.
By such swinging of the rocker 20 in the clockwise direction (as seen from the left), the pin holder 3 is moved upward, and the tips of its pins press the button 37 in the guide jaws 38 upward to such an extent that the top thereof comes to rest against the bottom of the driver disk 34. The driver disk 34 then turns the button 37 around its axis of symmetry until the holes in the button are received on the pins of the pin holder 3. The button 37 then drops a small amount until it rests fully on the pin holder 3, as a result of which its top side no longer rests against the bottom of the driver disk 34.
The other cylinder chamber of the cylinder 18 is then actuated, as a result of which the carriage 15 is now pushed from the rear to the front against the action of the compression spring 16 and in this way the button 37 on the pin holder 3 is brought into the raised button clamp 35. Shortly before the front end position of the carriage 15 is reached, the pin 24 comes against the stop 30, as a result of which the rocker 20 is now swung in counterclockwise direction by the downward movement of the left-hand push rod 25. At this point the pin holder 3 is lowered so that its pins leave the holes in the button 37.
In this way, the pin holder 3 follows a rectangular path (see the chain line adjacent pin holder 3 in FIG. 3). At this point, the button 37, which has been aligned in proper position for sewing, is dependably transferred to the button clamp 35 which--while the pin holder 3 travels in the lower part of its linear quadrangular path into the rear position--moves downward and in this way places the button 37 on the sewing material which has been made ready. Thereupon, the sewing of the button 37 is commenced by the button attaching machine. At the same time the next button 37 passes into the guide jaws 38 and is aligned in the manner described above, and then transferred into the button clamp 35 which has been raised again after the button attaching processes.
Although an illustrative embodiment of the invention has been described in detail herein, it is understood that the invention is not limited to such embodiment, but rather that modifications and variations on the invention may occur to one of ordinary skill in the art within the scope of the invention, as defined only by the claims.
|
A button feeding device includes a button alignment shaft having a longitudinal axis which is displaceable with respect to the longitudinal axis of the main drive shaft. The button alignment shaft and the main drive shaft are advantageously linked for rotation by a coil spring. The device has a pin holder which aligns the button and transfers it into a button clamp, a carriage being provided to move the pin holder over a substantially linear quadrangular path.
| 3
|
TECHNICAL FIELD
[0001] The present disclosure relates to the field of automated manual transmissions. More specifically but not exclusively the present invention relates to an automated manual transmission and a method of controlling at least part of the gearshifts of an automated manual transmission.
BACKGROUND
[0002] Conventional manual transmissions use gearshift systems whereby the driver manually selects the desired gear by shifting a gear stick into a certain position in the gearbox. The gear stick is in direct connection with an internal shift mechanism usually comprising some form of shift rails, shift forks and shift collars. One disadvantage of such a system is that the gearbox and the gear stick have to be arranged in such a configuration that all components can easily be interconnected by a mechanical linkage. To allow for a more flexible installation, systems have been developed wherein the mechanical linkage has been replaced by a system wherein electro-hydraulic solenoids direct oil to and from pistons mounted at the end of the shift rails to control the position of the shift rail. A well known problem associated with such a system is the locating and securing of this shift mechanism in a neutral position. The positive neutralisation of a mechanism is essential to prevent erroneous gear engagement and multiple gear sets being engaged simultaneously. A failure to do so could result in uncontrolled machine behaviour and severe mechanical damage. Previous arrangements, such as for example the 5-speed Power Synchro gearbox of Turner Powertrain, Wolverhampton, UK, utilise a multiple piston set-up whereby a set of compound pistons operate on hydraulic principles to neutralise the shift rail. This arrangement has certain disadvantages such as the complexity of the components and machining procedures and hence cost.
[0003] It is an aim of the present invention to solve one or more of the problems set forth above.
SUMMARY OF THE INVENTION
[0004] It is an object of the present disclosure to provide a gearshift arrangement with a first and a second shift member as part of respectively a first and second mechanism. The arrangement further has a sensing arrangement adapted to monitor the position of the first shift member relative to a neutral position and an actuating arrangement operable to position the first shift member into the neutral position based on at least one signal from the sensing arrangement. A mechanical arrangement is included and is adapted to prevent movement of the second shift member if the first shift member is not in a neutral position.
[0005] A second object of the disclosure is to provide a method of operating a gearshift arrangement having a first and a second shift member as part of respectively a first and second shift mechanism. The method includes the steps of electronically determining the position to a neutral position of the first shift member, positioning the first shift member into a neutral position based on at least one determination from the previous step and mechanically preventing movement of the second shift member if the first shift member is not in the neutral position.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 is a schematic vertical section through a gearbox according to the present invention;
[0007] FIG. 2 is a schematic cross sectional view of a detent mechanism which may be used in the gearbox of FIG. 1 ; and
[0008] FIG. 3 a, 3 b and 3 c are schematic views of a shift fork as used in the gearbox of FIG. 1 .
DETAILED DESCRIPTION
[0009] Referring to FIGS. 1 and 2 , gearbox 10 has a first shift mechanism 11 for the engagement of first and second gear and a second shift mechanism 111 for the engagement of third and fourth gear. More gears and/or gear mechanisms may be added. For simplicity, as both first shift mechanism 11 and second shift mechanism 111 are substantially similar, only shift mechanism 11 will be described in detail. Like numbers in first shift mechanism 11 and second shift mechanism 111 indicate like structures.
[0010] The first shift mechanism includes three shift members, namely a shift rail 12 , a shift collar 16 and a shift fork 14 . Shift fork 14 is rigidly connected to shift rail 12 , but is in a floating engagement with shift collar 16 . FIGS. 3 a - 3 c shows shift fork 14 with two prongs 17 that engage with a counterpart such as circumferential groove 19 on shift collar 16 . Although in this example shift fork 14 is of the two prong type and engages shift collar 16 via groove 19 in a floating fashion, the principle is applicable to other types of shift fork and collar arrangements. Shift collar 16 is for this disclosure considered to include the actual gear engagement clutch, for example a synchroniser clutch.
[0011] Connected to opposite ends of shift rail 12 are single acting pistons 18 and 20 ( 20 is not shown, 120 is shown instead) as part of an actuating arrangement 21 . However one dual acting piston (not shown) may be used instead of two single acting pistons 18 and 20 if preferred. Pistons 18 and 20 may be pressurised by a fluid such as air or like in this case oil, the oil flow being generated by a pump (not shown) and directed to and from pistons 18 and 20 by solenoid valves 22 and 24 respectively. Alternatively, shift rail 12 may be actuated by an electronic solenoid (not shown) rather than an electro-hydraulic system. Other electro-hydraulic solenoid arrangements may also be possible, whereby one or multiple electro-hydraulic solenoids may operate together with directional valves or mechanical linkages to simplify the system or reduce the number of components or cost.
[0012] Specifically now referring to FIG. 2 , interlocking device 30 is in this example a kind of detent arrangement with a series of balls 32 a, 32 b, 32 c and 32 d, preferably made of metal, of which balls 32 a and 32 d at both extremes of the series each may engage with a recesses 33 and 133 in shift rails 12 and 112 . Recesses 33 and 133 in shift rails 12 and 112 are located on the rails in a position corresponding to neutral positions when the recess is lined up with the corresponding balls 32 a or 32 d. A neutral position for shift rails 12 and 122 is defined as the position in which shift collars 16 and 116 are in a position where no gears are engaged or being engaged. The overall length of the series of balls 32 a - d is greater than the distance between the two nearmost outer surfaces of shift rails 12 and 112 . This prevents in normal operation the engagement of a multiple of any of 1 st , 2 nd , 3 rd and 4 th gears. A different number of balls such as 32 a - d or different arrangements having cylindrical or other shapes or non-metal components may be used.
[0013] Shift rail 12 further has a series of adjacent recesses 34 a, 34 b and 34 c, substantially similar to shift rail 112 with recesses 134 a, 134 b and 134 c. This is the same principle for both shift rails, so for simplicity only shift rails 12 with recesses 34 a - c will be discussed in the following paragraph. Recesses 34 a - c may engage with a detent mechanism such as ball 37 and spring 38 to define three discrete positions as part of a mechanical arrangement 36 . The first position may correspond to shift mechanism 11 engaging first gear. The second position may correspond to shift mechanism 11 being in a neutral position, whilst the third position may correspond to shift mechanism 11 engaging second gear. The biased detent aids in locating shift rails 12 into any of the three positions and keeping it in that position. Ball 37 is preferably made of metal, but other materials as well as other shapes may be used. FIG. 1 shows a variation 35 of this detent mechanism, whereby the principle is the same, but the position of the mechanism is different.
[0014] Furthermore there are sensing arrangements 39 and 139 . Again for simplicity only one such arrangement is discussed here, because the principles and components are substantially similar for both shift mechanisms 11 and 111 . Sensor 40 may be fitted to a location in gearbox 10 , or for ease of servicing external whilst at least partially protruding through a wall of gearbox 10 . The sensing part is preferably located in a position adjacent to shift fork 14 , because sensor 40 is responsive to activator 42 which is either fitted to or an integral part of shift fork 14 . One possible type of sensor and activator arrangement is a non-contact linear position sensor together with a ferrous activator. The sensor may for example be a blade sensor as manufactured by Gill Technology, Lymington, Hampshire, UK. Sensor 40 is preferably a proportional and adjustable sensor to give a wider range of detection and to enable a calibration procedure. However, other suitable sensing arrangements may be used, for example contact sensors. If some type of activator is required it may also be fitted in a different position, for example on the shift rail or the shift collar. As shift rail 12 , shift fork 14 and shift collar 16 all have fixed relative positions to one another, it is not significant which component is used for activation of the sensor, because in normal operation the positions of all other components may be determined once one has been sensed.
[0015] The signal generated by sensor 40 is sent preferably to an electronic control unit (ECU) 44 . ECU 44 may be programmed to monitor and control a wide variety of transmission and other functions, but is able to process the signal sent from sensor 40 . ECU 44 further may receive an input from for example a vehicle driver and may process the signals to than send a signal to control solenoid valves 22 and 24 . An alternative may be to have a system without ECU 44 , wherein solenoid valves 22 and 24 are activated directly or indirectly by signals from sensor 40 or a multiplicity of similar sensors. ECU 44 may be able to control both shift mechanisms 11 and 111 .
INDUSTRIAL APPLICABILITY
[0016] During normal operation gearbox 10 and hence shift mechanisms 11 and 111 may be in a neutral position. The vehicle driver selects a desired gear, which is signaled to ECU 44 . ECU 44 further receives signals from sensors 40 and 140 . If all parameters are acceptable ECU 44 may activate one of solenoid valves 22 , 24 , 122 and 124 to direct a flow of oil from a pump (not shown) onto one of pistons 18 , 20 , 118 and 120 to shift one of shift mechanisms 11 and 111 . The oil pressure acting on the piston may during a shift be varied by for example the solenoid valve to give smooth gear engagement and disengagement.
[0017] For example, the vehicle driver wishes to engage first gear from neutral. Via an input device his selection is signalled to ECU 44 . ECU 44 has also detected the neutral positions of shift mechanisms 11 and 111 via sensors 40 and 140 . If all conditions are met, ECU 44 sends a signal to solenoid valve 24 to direct oil from a pump (not shown) to piston 20 and a signal to solenoid valve 22 to create a return connection for the oil displaced by piston 18 . The oil acting on piston 20 moves shift rail 12 and hence shift collar 16 to a position wherein shift collar 16 engages first gear. Once the gearshift is completed both solenoid valves 22 and 24 open up the oil connection from pistons 18 and 20 to a return line, so all pistons are depressurised. During this shift the oil pressure acting on piston 18 has to be high enough to overcome the resistance of the actual gear engagement and to lift ball 37 out of recess 34 b. Once first gear engagement is completed or near completion, ball 37 engages with recess 34 c. Because shift rail 12 is in an out of neutral position, interlocking device 30 prevents shift rail 112 from movement as ball 32 d is now firmly engaged with recess 133 .
[0018] If the driver decides to shift to a gear that can only be engaged by shift mechanism 112 , for example 3 rd gear, the following actions will take place. Before shift mechanism 112 can be activated, shift mechanism 12 has to be put into the neutral position. Under normal operating conditions, ECU 44 will not activate shift mechanism 112 before it receives a signal from sensor 40 that shift mechanism 12 is in the neutral position. However, in case that an electronic failure or error happens and ECU 44 attempts to engage shift mechanisms 12 and 112 simultaneously, interlocking mechanism 30 prevents this from happening. This mechanical interlocking feature is extremely important to avoid serious damage to gearbox 10 . To neutralise shift mechanism 12 , ECU 44 signals solenoid valve 22 to direct oil onto piston 18 and solenoid valve 24 to create a return connection for the oil displaced by piston 20 . Shift rail 12 will then move towards the neutral position. Activator 42 is continuously sensed by sensor 40 which signals to ECU 44 a signal corresponding to the position of 42 and hence shift mechanism 11 . Once shift rail 12 is close to reaching the neutral position, ECU 44 may signal solenoid valve 22 to reduce the flow of oil to piston 18 to reduce the speed of shift rail 12 and so prevent an overshoot condition wherein shift rail 12 passes the neutral position. When shift rail 12 is substantially in the neutral condition, ECU 44 may signal on or both solenoid valve 22 and 24 to stop all flow to and from pistons 18 and 20 . In approximately the same period detent mechanism 36 engages with recess 34 b to aid shift rail 12 to settle in the neutral position and to give positive retention of shift rail 12 in that neutral position.
[0019] Because of both shift rails 12 and 112 now being in the neutral position, neither of shift rails 12 and 112 are prevented from movement by interlocking device 30 .
[0020] The following step is where shift mechanism 112 has to engage 3 rd gear. ECU 44 receives or has received a signal from sensor 40 about the neutral position of shift rail 12 . ECU 44 signals solenoid valve 124 to direct oil onto piston 120 and solenoid valve 122 to open a return connection for the oil displaced by piston 118 . The remainder of the shift is substantially similar as the engagement of first gear as described in paragraph 14 onwards. Although some of the steps as described have to be performed in a certain order, this is not essential for all steps. Also some of the steps may at least partially overlap. 1
|
Transmissions in which the mechanical gear shift arrangements are replaced by electro-hydraulic operated shift mechanisms that have to be able to be neutralised positively to ensure a proper operation. An arrangement and method are provided to determine the position of the shift rail so a shift can be made only if the conditions are right. To prevent engagement of two shift members at the same time and consequent damage in case of electronic failure, mechanical safety features such as detents are included.
| 8
|
FIELD OF THE INVENTION
The present invention relates to metal surfaces coated with fluoropolymers and more particularly to tubes whose outer surface is coated with fluoropolymers. These tubes are useful for the development of offshore hot oil wells, since it is necessary for the tubes which transport hot oil to withstand corrosion by seawater.
THE TECHNICAL PROBLEM
No steel tube coating which can be readily produced industrially and which can withstand high temperature under offshore conditions is known at the present time. For the development of offshore hot wells, one solution consists in cooling the oil with a heat exchanger before raising it to the surface. This technique is very expensive. Furthermore, the cooling may result in the formation of a cold plug. It is also possible to make use of special steels, but they are prohibitively expensive. A coating made of fluoropolymer, for example PVDF (common abbreviation for polyvinylidene fluoride), as disclosed in the invention makes it possible to convey hot fluids (150° C.) under offshore conditions, using ordinary steel tubes.
PRIOR ART
Patent DE 3 422 920 discloses outer coatings for steel tubes, comprising, successively, a layer of epoxy resin, a layer of grafted polypropylene and, finally, an outer layer of a mixture of polypropylene and of a polypropylene/polyethylene block copolymer. The glass transition temperature Tg of the epoxy resin is between 80° C. and 94° C. These coatings are suitable for hot water at 90° C.
U.S. Pat. No. Re 30 006 discloses outer coatings for steel tubes, comprising, successively, an epoxy resin and a polyethylene modifed by grafting or copolymerization with maleic anhydride. Nothing is stated regarding the Tg of the epoxy resin; however, the polyethylene does not make it possible to work above 80° C.
Patent EP-A-0 770 429 discloses a coated metal surface such as the outer surface of a tube, comprising, successively, a layer of epoxy resin placed next to the metal and having a glass transition temperature of greater than 120° C., a layer of binder based on polypropylene modified by grafting and a layer of thermoplastic polymer. The thermoplastic polymer is chosen from polyamides, polyamide alloys and polypropylene. These coatings do not offer any protection against corrosion by seawater to tubes transporting oil at 150° C.
Patent EP-A-404 752 discloses structures consisting, successively, of a substrate, a primer and a layer of PVDF. The primer is a mixture of an epoxy resin with either PMMA (common abbreviation for polymethyl methacrylate) or a copolymer of methyl methacrylate and of ethyl acrylate. Patent EP-A-0 354 822 discloses similar structures. This coating does not withstand corrosion by seawater when the tubes transport oil at 150° C.
Patent WO 97/27260 discloses structures consisting, successively, of a substrate, a primer and a layer of PVDF. The primer is a mixture of at least two of the following three polymers, namely (i) a PVDF homopolymer, (ii) a PVDF copolymer comprising at least 50 mol % of VF2 and (iii) an acrylic polymer containing carboxylic acid functions, such as, for example, copolymers of methyl methacrylate and of acrylic acid. The substrate may be the outer surface of a tube. Patent WO 97/49777 discloses similar structures. This coating does not withstand corrosion by seawater when the tubes transport oil at 150° C.
It has now been found that a coating comprising, respectively, a layer of epoxy resin, a layer of binder based on PVDF and on at least one polymer chosen from acrylic polymers and oxidized fluoropolymers and a layer of PVDF, the epoxy resin being on the side of the metal, protects the metal against corrosion by seawater even if the metal is at 150° C. Variants of this coating, which are detailed later, may also be used.
BRIEF DESCRIPTION OF THE INVENTION
The present invention relates to a coated metal surface comprising, successively:
a layer (1) of epoxy primer placed next to the metal,
a layer (2) of binder comprising 98 to 50 parts by weight of at least one fluoropolymer L3 per 2 to 50 parts, respectively, of at least one polymer chosen from acrylic polymers L1 and polymers L2 which are fluoropolymers chemically modified by a partial dehydrofluorination followed by an oxidation,
a layer (3) of fluoropolymer.
The present invention also relates to a process for manufacturing these coated surfaces. The metal surface is first degreased, sanded and then heated. The epoxy primer of the layer (1) is deposited in liquid form or by spraying or electrostatic spraying if it is a powder onto the metal surface heated to 200-240° C. After about 20 to 30 seconds, i.e. slightly before the end of the gel time and before the resin has crosslinked, in order for there to remain epoxide functions to react with the binder, the binder of the layer (2) is deposited either by spraying if it is in powder form, or by coating or rolling. Next, the fluoropolymer of the layer (3) is deposited in the same way. As regards the outer surface of metal tubes, the process is performed in the same way for the epoxy primer, and the binder is then either deposited by spraying if it is available in powder form, or extruded through a circular die (also known as a crosshead) arranged concentrically around the tube. The binder may also be extruded through a flat die producing a continuous strip which is wound around the tube, for example by means of rotating the tube on itself. The fluoropolymer is deposited in the same way.
The coating of the invention can readily be produced on a conventional coating line, due to the excellent processability of PVDF. The coating can be applied continuously, at a speed of at least 50 cm/minute, at a temperature of less than 250° C., this temperature making it possible to conserve all the initial properties of the steel. The ease of use is an advantage over other known solutions thermostable polymers such as polysulfone, polyphenylene ether or polyether imide which require either high temperatures or a long and intricate implementation with reactive solvents (post-curing).
According to a first variant, the coating does not comprise the layer (3). However, it is recommended that the layer (2) which becomes the outer layer should be thicker than in the structure of the main invention.
According to a second variant, the coating does not comprise the layer of primer (1), the layer of binder necessarily contains the polymer L2 and the surface is necessarily the outer surface of tubes.
That is to say that in this second variant, the invention relates to a coated metal surface which is the outer surface of tubes, comprising, successively:
a layer (2) of binder placed next to the metal and comprising 98 to 50 parts by weight of at least one fluoropolymer L3 per 2 to 50 parts, respectively, of a mixture comprising at least one polymer chosen from polymers L2 which are fluoropolymers chemically modified by a partial dehydrofluorination followed by an oxidation, and optionally at least one polymer chosen from acrylic polymers L1,
a layer (3) of fluoropolymer.
According to a third variant, the coating does not comprise the layer (2) and the layer (1) comprises a mixture of epoxy primer and of polymer L2.
That is to say that in this third variant, the invention relates to a coated metal surface comprising, successively:
a layer (1) of primer placed next to the metal and comprising 1 to 70 parts of a polymer chosen from polymers L2 which are fluoropolymers chemically modified by a partial dehydrofluorination followed by an oxidation, per 30 to 99 parts, respectively, of an epoxy primer,
a layer (3) of fluoropolymer.
The coating obtained has good impact strength, flexibility allowing slight bending of the tube and excellent adhesion to the metal, even at high temperature (up to 150° C.). These good properties are maintained on contact with seawater.
DETAILED DESCRIPTION OF THE INVENTION
The term “epoxy primer” used for the layer (1) advantageously denotes the product of the reaction of a thermosetting epoxy resin and of a hardener. Their principle is disclosed, for example, in Kirk-Othmer Encyclopaedia of Chemical Technology Vol. 9—pages 267-289, 3 rd edition. This layer (1) may also be defined as any product of the reaction of an oligomer bearing oxirane functions and of a hardener. As a result of the reactions carried out during the reaction of these epoxy resins, a crosslinked material is obtained corresponding to a three-dimensional network which is more or less dense depending on the base characteristics of the resins and hardeners used.
The term “epoxy resin” means any organic compound containing at least two functions of oxirane type, which can be polymerized by ring-opening. The term “epoxy resin” denotes any common epoxy resin which is liquid at room temperature (23° C.) or at higher temperature. These epoxy resins may be monomeric or polymeric, on the one hand, and aliphatic, cycloaliphatic, heterocylic or aromatic, on the other hand. Examples of such epoxy resins which may be mentioned include resorcinyl diglycidyl ether, bisphenol A diglycidyl ether, triglycidyl p-aminophenol, bromobisphenol F diglycidyl ether, m-aminophenyl triglycidyl ether, tetraglycidylmethylenedianiline, (trihydroxyphenyl)methane triglycidyl ether, polyglycidyl ethers of novolac phenol-formaldenhyde, polyglycidyl ethers of novolac ortho-cresol and tetraglycidyl ethers of tetraphenylethane. Mixtures of at least two of these resins may also be used.
The preferred resins are epoxy resins containing at least 1.5 oxirane functions per molecule and more particularly epoxy resins containing between 2 and 4 oxirane functions per molecule. Epoxy resins containing at least one aromatic ring, such as bisphenol A diglycidyl ethers, are also preferred.
As regards the hardener, the hardeners generally used are epoxy-resin hardeners which react at room temperature or at temperatures above room temperature. Non-limiting examples which may be mentioned include:
Acid anhydrides, including succinic anhydride,
Aromatic or aliphatic polyamines, including diaminodiphenyl sulphone (DDS) or methylenedianiline or 4,4′-methylenebis(3-chloro-2,6-diethylaniline) (MCDEA),
Dicyandiamide and its derivatives,
Imidazoles,
Polycarboxylic acids,
Polyphenols.
The resins used in the present invention are crosslinkable between 180° C. and 250° C.
The gel time is defined by AFNOR standard NFA 49-706. This is the time required to bring about a rapid increase in viscosity at a given temperature. The gel time is advantageously between 20 and 60 seconds.
The Tg is advantageously greater than 120° C. These resins may be in the form of powder or liquid which is sprayed onto the metal surface, which has been degreased, sanded and heated beforehand.
These are advantageously one-component powder resins which are conventionally obtained as follows:
The epoxy resin (solid at room temperature, e.g.: high mass DGEBA), the hardener, optionally the accelerators, the fillers, etc. are mixed together in the molten state; during this step, pre-crosslinking takes place but without going as far as the gel point,
The mixture is cooled at the mixer outlet, so as to stop the crosslinking,
The homogeneous solid obtained is made into powder.
A one-component powder is thus obtained which can be applied by the usual processes and which completes its crosslinking on contact with hot metal. Generally, for these applications, the preferred systems are those which crosslink only at high temperature, (180-240° C.) such that there is no problem of storage at room temperature (shelf life or pot life of 6 months-1 year).
These resins may comprise additives such as silicones, pigments such as titanium dioxide, iron oxides, carbon black, fillers such as calcium carbonate, talc or mica.
As regards the acrylic polymer (L1) of the layer (2), it consists essentially of alkyl (meth)acrylate units. The other monomers constituting (L1) may be acrylic or non-acrylic monomers, which may be reactive or unreactive. The term “reactive monomer” means: a chemical group capable of reacting with the oxirane functions of epoxy molecules or with the chemical groups of the hardener. Non-limiting examples of reactive functions which may be mentioned include: oxirane functions, amine functions, carboxyl functions, acid chloride functions and alcohol functions. The reactive monomer may be (meth)acrylic acid or any other hydrolyzable monomer leading to these acids. Among the other monomers which may constitute (L1), non-limiting examples which may be mentioned include glycidyl methacrylate and tert-butyl methacrylate. Examples of polymer (L1) which may be mentioned include homopolymers of an alkyl (meth)acrylate. Alkyl (meth)acrylates are described in Kirk-Othmer, Encyclopaedia of chemical technology, 4 th edition, in Vol. 1, pages 292-293 and in Vol. 16, pages 475-478. Mention may also be made of copolymers of at least two of these (meth)acrylates and copolymers of at least one (meth)acrylate with at least one monomer chosen from acrylonitrile, butadiene, styrene and isoprene, provided that the proportion of (meth)acrylate is at least 50 mol %. (L1) is advantageously PMMA with a few percent by weight of acid function. These polymers (L1) either consist of the monomers and optionally of the comonomers mentioned above and do not contain any impact modifier, or they also contain an acrylic impact modifier. The acrylic impact modifiers are, for example, random or block copolymers of at least one monomer chosen from styrene, butadiene and isoprene and of at least one monomer chosen from acrylonitrile and alkyl (meth)acrylates, and they may be of core-shell type. The impact modifiers may also be triblock copolymers consisting of a polystyrene block, a polybutadiene block and a PMMA block. These triblock copolymers are disclosed in patent application WO 99/29772. These acrylic impact modifiers may be mixed with the polymer (L1) once prepared or may be introduced during the polymerization of (L1) or prepared simultaneously during the polymerization of (L1). The amount of acrylic impact modifier may be, for example, from 0 to 30 parts per 100 to 70 parts of (L1) and advantageously from 5 to 20 parts per 95 to 20 parts of (L1). It would not constitute a departure from the context of the invention if (L1) was a blend of two or more of the above polymers.
The Tg of (L1) is advantageously greater than or equal to 120° C. and preferably greater than or equal to 130° C.
The MFI (melt flow index) of (L1) may be between 2 and 15 g/10 min measured at 230° C. under a 3.8 kg load.
The MVFR (melt volume flow rate) of (L1) may be between 1.5 and 12 cm 3 /10 min measured at 230° C. under a 3.8 kg load. Polymers that are suitable for (L1) are Sumipex TR® from Sumitomo® and Oroglas HT121® from Atoglas. These are copolymers of methyl methacrylate and of (meth)acrylic acid.
As regards the fluoropolymer L2 of the layer (2), it is obtained from a fluoropolymer which is chemically modified by a partial dehydrofluorination followed by an oxidation. The fluoropolymer which is modified may be a fluoroplastic or a fluoroelastomer, provided that they contain units of general formula (I):
in which X and X′ may be, independently of each other, a hydrogen atom, a halogen, in particular fluorine or chlorine, or a perhaloalkyl, in particular perfluoroalkyl.
The fluoropolymers which may be used may be prepared by polymerization or copolymerization of olefinic unsaturated monomers. To obtain a fluoropolymer having the unit of formula (I), the monomer and/or the comonomers must comprise both fluorine atoms linked to carbon atoms and hydrogen atoms linked to carbon atoms. For example, the fluoropolymers which may be used may be homopolymers prepared from hydrofluorocarbon monomers, or may be copolymers derived from perfluoro unsaturated monomers copolymerized with one or more unsaturated monomers containing hydrogen —H, namely a hydrofluorocarbon monomer and/or a non-fluoro monomer.
As examples of olefinic unsaturated monomers which may be used, mention may be made of hexafluoropropylene (HFP), tetrafluoroethylene (TFE), vinylidene fluoride (VF 2 ), chlorotrifluoroethylene (CTFE), 2-chloropenta-fluoropropene, perfluoroalkyl vinyl ethers such as CF 3 —O—CF═CF 2 or CF 3 —CF 2 —O—CF═CF 2 , 1-hydropentafluoropropene, 2-hydropentafluoropropene, dichloro-difluoroethylene, trifluoroethylene, 1,1-dichlorofluoroethylene and perfluoro-1,3-dioxoles such as those disclosed in U.S. Pat. No. 4,558,142, and olefinic unsaturated monomers comprising no fluorine, such as ethylene, propylene, butylene and higher homologues.
Diolefins containing fluorine may be used, for example diolefins such as perfluorodiallyl ether and perfluoro-1,3-butadiene.
The olefinic unsaturated monomers or comonomers may be polymerized to obtain a fluoropolymer by the processes known in the prior art of fluoropolymers.
In particular, as regards the processes for synthesizing poly(vinylidene fluoride) (PVDF), patents U.S. Pat. No. 3,553,185 and EP-A-0 120 524 disclose processes for synthesizing PVDF by placing vinylidene fluoride (VF 2 ) in aqueous suspension and polymerizing it. Patents U.S. Pat. No. 4,025,709, U.S. Pat. No. 4,569,978, U.S. Pat. No. 4,360,652, and EP-A-0 655 468 disclose processes for synthesizing PVDF by placing VF 2 in aqueous emulsion and polymerizing it.
In general, the olefinic unsaturated fluoro monomers may be polymerized and optionally copolymerized with non-fluoro olefinic monomers in aqueous emulsions. The emulsions contain, for example, a water-soluble initiator such as an ammonium or alkali metal persulfate or alternatively an alkali metal permanganate, which produce free radicals, and also contain one or more emulsifiers such as ammonium or alkali metal salts of a perfluorooctanoic acid.
Other aqueous colloidal suspension processes use initiators that are essentially soluble in the organic phase, such as dialkyl peroxides, alkyl hydroperoxides, dialkyl peroxydicarbonates or azoperoxides, the initiator being associated with colloids such as methylcelluloses, methylhydroxy-propylcelluloses, methylpropylcelluloses and methylhydroxyethylcelluloses.
Many fluoropolymers and copolymers are commercially available, in particular those from the company Elf Atochem S.A. under the brand name Kynar®.
The fluoropolymer which is modified to convert it into L2 is preferably in the form of an aqueous dispersion, such as an emulsion or a suspension. This dispersion may be the product resulting from one of the synthetic methods recalled above.
The polymer which is modified to convert it into L2 is preferably PVDF homopolymer or a VF2-HFP copolymer.
This fluoropolymer is subjected to a partial dehydrofluorination with a base and the fluoropolymer thus partially dehydrofluorinated is then reacted with an oxidizing agent to give a new fluoropolymer L2.
This dehydrofluorination of the fluoropolymer is obtained by a base in aqueous medium or in an organic solvent. Bases which may be used are cited in WO 98/08880. They may be, for example, a hydroxide such as potassium hydroxide (KOH), ammonium hydroxide (NH 4 OH), sodium hydroxide (NaOH), lithium hydroxide (LiOH), a carbonate such as potassium carbonate (K 2 CO 3 ) or sodium carbonate (Na 2 CO 3 ), a tertiary amine, a tetraalkylammonium hydroxide or a metal alkoxide. A process for the dehydrofluorination in aqueous medium of a fluoropolymer emulsion is also disclosed in patent application WO 98/08879. The base may be used with or without catalyst. The base may also be an amine derivative of hydrocarbon-based structure which is soluble or partially soluble in water or organic solvents, in particular 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) or 1,4-diazabicyclo[2.2.2]octane (DABCO).
The catalyst may be, for example, tetrabutylammonium bromide (TBAB) and tetraalkylphosphonium, alkylarylphosphonium, alkylammonium and alkylphosphonium halides. The basic compound and the optional catalyst may be dissolved or diluted in a solvent such as naphthalene, tetrahydrofuran (THF) and water.
The oxidation is preferably obtained in heterogeneous aqueous medium with hydrogen peroxide (H 2 O 2 ) or with the hypochlorite anion (ClO − ) following the introduction of a hypochlorous acid salt (ClOM1) in which the cation (M1) corresponds, for example, to an alkali metal such as sodium or potassium. Specifically, hydrogen peroxide in aqueous phase makes it possible to have an advantageous process by minimizing the waste compared with a process using an organic solvent. Hydrogen peroxide in aqueous phase also allows a simplified treatment of the effluents compared with other oxidizing agents. Hypochlorous acid salts show the same advantages as hydrogen peroxide on account of their possibility of use in aqueous phase, and have a particular advantage in process terms since they can be introduced, partially or totally, from the first dehydrofluorination step.
The treatment with hydrogen peroxide may be activated in the presence of a metal catalyst, such as iron (II), which is introduced, for example, in the form of halides. According to the same principle, the treatment with the hypochlorous acid salt may be performed in the presence of a metal catalyst, such as manganese (III) or nickel (II) combined with various ligands such as alkylated polyamines, phthalocyanins or porphyrins. The reaction with the hypochlorite anion can also be promoted by adding an aprotic solvent, such as acetonitrile or glymes.
However, other oxidizing agents that are active in aqueous medium may be used, for example palladium or chromium halides, in particular PdCl 2 and CrCl 2 , alkali metal permanganates, for example KMnO 4 , peracid compounds, alkyl peroxides or persulfates, optionally combined with H 2 O 2 or with activating co-reagents, such as sodium metabisulphite or potassium metabisulphite.
The reaction or the contact with aqueous H 2 O 2 is advantageously performed at a pH ranging from 6.5 to 8 and preferably from 6.7 to 7.6. The reason for this is that for a pH of less than 6.5, the reaction is very slow, and for a pH of greater than 8, there is a risk of the H 2 O 2 decomposition reaction running out of control.
The reaction or the contact with H 2 O 2 is advantageously performed at a temperature ranging from 20° C. to 100° C. and better still from 50° C. to 90° C.
The total amount of H 2 O 2 added, calculated on the basis of the pure peroxide, is advantageously from 1% to 50% by weight relative to the total weight of the reaction medium. This amount preferably ranges from 2% to 12%.
The reaction or the contact with the hypochlorite anion is advantageously performed at a pH ranging from 6 to 14.
The reaction or the contact with the hypochlorite anion is advantageously performed at a temperature ranging from 20 to 100° C. or better still from 50 to 90° C.
The total amount of hypochlorite anion added, calculated on the basis of sodium hypochlorite (NaClO), is advantageously from 0.1% to 50% by weight relative to the total weight of the reaction medium. This amount preferably ranges from 0.5% to 10%.
According to the process of the present invention, the modified polymers L2 have adhesion properties that are greatly increased compared with fluoropolymers that are not chemically modified.
The MFI (melt flow index) of L2 is advantageously between 0.2 and 5 g/10 min (at 230° C. under a 10 kg load) for L2 derived from the PVDF homopolymer and between 2 and 10 g/10 min (at 230° C. under a 5 kg load) for L2 derived from the copolymer of VF2 and of HFP.
As regards the fluoropolymer L3 of the layer (2), it may be chosen from polymers and copolymers containing units of general formula (I) cited above for the polymers treated to produce L2.
Examples of fluoropolymers L3 which will be cited most particularly are
PVDFs, vinylidene fluoride (VF2) homopolymers and copolymers of vinylidene fluoride (VF2) preferably containing at least 50% by weight of VF2 and at least one other fluoromonomer such as chlorotrifluoroethylene (CTFE), hexafluoropropylene (HFP), trifluoroethylene (VF3) or tetrafluoroethylene (TFE),
trifluoroethylene (VF3) homopolymers and copolymers,
copolymers, and in particular terpolymers, combining the residues of chlorotrifluoroethylene (CTFE), tetrafluoroethylene (TFE), hexafluoropropylene (HFP) and/or ethylene units and optionally VF2 and/or VF3 units.
Among these fluoropolymers L3 that are advantageously used are PVDF homopolymer and VF2-HFP copolymers.
The melting point of L3 is advantageously greater than 150° C. A melting point which is as high as possible is preferred.
The MVFR (melt volume flow ratio) of L3 is advantageously between 2 and 25 cm 3 /10 min and preferably between 4 and 10 cm 3 /10 min (at 230° C. under a 5 kg load).
The proportion of L3 is advantageously from 95 to 70 parts by weight per 5 to 30 parts, respectively, of at least one polymer chosen from acrylic polymers L1 and the polymers L2.
The binder of this layer (2) can contain additives and fillers usually used in fluoropolymers.
A catalyst capable of increasing the reactivity of the reactive functions of L1 or L2 with the epoxy may be added. This catalyst may be 1,4-diazabicyclo[2.2.2]octane (DABCO) or methyl-2-imidazole (M2ID). These catalysts are disclosed in French patent FR-A-2 745 733.
A blend of L1 and L2 may also be used, i.e. the binder comprises 98 to 50 parts of L3 per 2 to 50 parts, respectively, of a blend of L1 and L2.
The proportion of L3 is advantageously from 95 to 70 parts by weight per 5 to 30 parts, respectively, of a blend of L1 and L2.
The binder may be manufactured by mixing together, in molten form, the various constituents in the usual devices for blending thermoplastic materials, and then used immediately or recovered after cooling in the form of powder or granules. It may also be manufactured by dry-blending of the various constituents in the form of powder or granules.
As regards the fluoropolymer of the layer (3), it may be chosen from the family of fluoropolymers described for L3. It is advantageously a PVDF homopolymer or a VF2-HFP copolymer having a melting point of at least 165° C. The MVFR is advantageously between 0.5 and 5 cm 3 /10 min (at 230° C. under a 5 kg load).
The fluoropolymer of this layer (3) may contain additives and fillers usually used in fluoropolymers.
A common PVDF plasticizer, a dye or an acrylic impact modifier or triblock copolymer which may be chosen from the impact modifiers of L1 described above may also be added. The proportion of impact modifier in this layer (3) may be from 5 to 15 parts by weight per 95 to 85 parts, respectively, of fluoropolymer.
The thicknesses of the various layers may be from 50 to 150 μm for the layer (1), from 100 to 500 μm for the layer (2) and from 1000 to 5000 μm for the layer (3). The thicknesses are preferably, in μm, starting with the layer (1): 80/250/1500.
The metal surface may be of any type; however, the invention is particularly useful for the outer surface of tubes, these tubes possibly having an outside diameter, for example, of up to 0.8 or 1.5 m and a thickness of from 2 to 25 mm.
As regards the coating of tubes, the preferred process breaks down as follows:
preparation of the steel tube: degreasing, shot-blasting and optionally surface treatment (chromatation, etc.);
treatment of the tube in an infrared oven so as to reach a temperature of between 180 and 220° C.;
application of the epoxy primer powder by electrostatic spraying (or other process in the case of a liquid epoxy resin);
application of the binder by lateral extrusion, with bearing from a roll press. The time separating the application of the epoxy resin and the application of the binder must be less than the gel time of the epoxy;
application of the outer layer made of fluoropolymer by lateral extrusion, bearing from a roll press;
cooling with water.
The binder and the outer layer may also be extruded using a “crosshead” surrounding the tube. The binder and optionally the outer layer may also be applied by a powder process.
Besides the degreasing and shot-blasting, the steel may be chromated or silanized to improve the attachment of the primer.
As regards the first variant, the thicknesses of the various layers may be from 50 to 150 μm for the layer (1) and from 1 000 to 5 000 μm for the layer (2). The thicknesses are preferably, in μm, starting from the layer (1): 80/1 500. All the other elements described for the main invention apply.
As regards the second variant, the thicknesses of the various layers may be between 100 and 500 μm for the layer (2) and from 1 000 to 5 000 μm for the layer (3). The thicknesses are preferably, in μm, starting from the layer (2): 250/1500. All the other elements described for the main invention apply.
As regards the third variant, the thicknesses of the various layers may be from 100 to 500 μm for the layer (1) and from 1 000 to 5 000 μm for the layer (3). The thicknesses are preferably, in μm, starting with the layer (1): 250/1 500. The primer is advantageously prepared by dry-blending the one-component epoxy resin powder and the L2 powder. All the other elements described for the main invention apply.
EXAMPLES
Materials Used
Steel Tube:
Welded steel tube (shade E36-4) of length 3 meters, outside diameter 114.3 mm and thickness 6.3 mm, sold by Van Leeuwen Tubes (45120 Chalette sur Loing, France).
Chromatation:
Accomet PC chromatation system, sold by Brent Europe Ltd. (address: Ridgeway, Iver, Buckinghamshire, SLO 9JJ, UK).
Epoxy Primers of the Layer (1):
Eurokote® 798: Epoxy primer powder produced by BS Coating. Gel time 45±5 s at 180° C. Tg=120-140° C. (DSC on crosslinked film).
Scotchkote® 6258: Novolac epoxy primer powder produced by 3M®. Gel time 26 s at 182° C. Tg=166° C. (DMA on crosslinked film).
Materials Used for the Binders of the Layer (2):
Polymers L3:
Kynar® 3120-15: HFP/VF2 copolymer produced by Atofina, with a melt volume flow rate MVFR=4 cm 3 /10 min at 230° C. under 5 kg, and a melting point of 165° C.
Kynar® 2850-04: HFP/VF2 copolymer produced by Atofina, with a melt volume flow rate MVFR=10 cm 3 /10 min at 230° C. under 5 kg, and a melting point of 158° C.
Acrylic Polymer L1:
Oroglas® HT121: copolymer of methyl methacrylate and of acrylic acid, produced by Atofina, of Tg=130° C. and MVFR=1.8 cm 3 /10 min at 230° C. under 3.8 kg.
Fluoropolymer L2:
MKB212: Product obtained according to the procedure described later, starting with a PVDF latex which is a precursor of Kynar® 1000HD, PVDF homopolymer of MVFR=1.1 cm 3 /10 min at 230° C. under 5 kg and with a melting point of 169° C. The melting point of MKB212 is 168° C.
Fluoropolymer of the Layer (3):
Kynar® 740: vinylidene fluoride homopolymer produced by Atofina, with a melt volume flow rate MVFR=1.1 cm 3 /10 min at 230° C. under 5 kg and a melting point of 168° C.
Preparation of MKB212:
A polyvinylidene fluoride latex Kynar 1000 HD, prepared according to the emulsion process as disclosed in patent U.S. Pat. No. 4,025,709, is used as fluoropolymer starting material. After drying at 105° C. for 24 hours, this latex gives a dry powder. This latex, referred to as Latex 1 hereinbelow, contains 40% by weight of PVDF. However, the process according to the present invention may be applied in particular to any PVDF latex or VF2 copolymer obtained by an emulsion process or to any suspension of PVDF or VF2 copolymer obtained by a suspension process.
Dehydrofluorination step: The preparation of 7.2 kg of an aqueous sodium chloride solution containing 15% by weight of NaOH in water is commenced in a stirred 20-liter reactor. This solution is brought to 70° C., followed by addition thereto of 7.2 kg of Latex 1 optionally diluted in deionized water so as to have a given solids content, at a rate of 0.72 kg/min with stirring at 180 rpm. A brown coagulated emulsion is thus obtained which becomes progressively darker the more the degradation proceeds. Depending on the dehydrofluorination reaction time, a fine black powder is obtained which becomes progressively insoluble in the usual organic solvents, in particular dimethylformamide (DMF) or N-methylpyrrolidone (NMP).
Step of reaction with an oxidizing agent: The reaction medium is acidified to pH=5, with continuous stirring and while maintained at a temperature of 70° C., by adding about 2.5 kg of 36% by weight hydrochloric acid. 1.68 kg of 35% by weight hydrogen peroxide are then added at a rate of 0.4 kg/min, after which the pH is increased to a value of between 6.6 and 7.6 by adding a sodium hydroxide solution containing 15% by weight of NaOH. The mixture is left to react while maintaining the pH between 6.6 and 7.6 by adding the same sodium hydroxide solution. A gradual decoloration of the coagulated emulsion is observed, which becomes pale yellow to ochre.
Finishing: The solid coagulate in suspension is filtered to give a pale yellow powder which is washed with three dispersions in 20 liters of water with stirring and successive filtrations. A powder is thus obtained which is dried in an oven at 105° C. to constant weight.
Characterization: The characterization of this powder is carried out by measuring the absorbance at 300 nm which is obtained by analysis with a Perkin-Elmer LC-75 spectrophotometer using a concentration of 0.1% by weight of product in NMP. The dissolution time is 24 hours before carrying out the measurement.
Structures with Binder Comprising the Acrylic Polymer L1
Example 1
Kynar 3120-15 and Oroglas HT121 are mixed together in a Fairex Super 2/50 single-screw extruder in a proportion of 85/15 by mass. The mixture is granulated at the extruder outlet.
The steel tube to be coated (114 mm outside diameter) is degreased and then shot-blasted. Immediately after this operation, the tube mounted on a gantry support rotating at 10 rpm and advancing at 50 cm/min is heated to 200° C. with an induction oven and coated with the primer powder Eurokote 798 sprayed via a spray gun. The laterally extruded binder is wound around the tube on the primer 10-20 s after depositing this primer. The Kynar 740 also extruded laterally, coats the first two layers immediately after. A roll press ensures good contact between the various layers. The coated tube is cooled with water for 3 minutes.
The flow rates of the spray gun and of the two extruders are adjusted so as to have 70-100 μm of primer, 250-350 μm of binder and 1 250-1 500 μm of Kynar 740.
In summary, the structure of the coating obtained is as follows:
Eurokote 798/binder {85% Kynar 3120-15, 15% Oroglas HT121}/Kynar 740 80 μm/300 μm/1 400 μm
For the assessment, the tube is cut into rings which are then assessed by peeling according to standard prEN 10 285:1 998. For each temperature test (110, 130 and 150° C.), three rings are peeled. The mean force and the standard deviation are calculated on the three values obtained. The peeling results and the breaking modes are given in Table I.
Example 2
The structure below is prepared in the same way as in Example 1:
Eurokote 798/binder {70% Kynar 3120-15, 30% Oroglas HT121}/Kynar 740 80 μm/300 μm/1 400 μm
Example 3
The structure below is prepared in the same way as in Example 1, but on a chromated tube:
Accomet PC/Eurokote 798/binder {85% Kynar 3120-15, 15% Oroglas HT121}/Kynar 740
80 μm/300 μm/1 400 μm
The Accomet PC chromating solution is applied by brush to the tube after shot-blasting. The treatment in the induction oven at 200° C. suffices to ensure good drying before applying the primer.
Example 4
The structure below is prepared in the same way as in Example 3, but with a thicker outer layer:
Accomet PC/Eurokote 798/binder {85% Kynar 3120-15, 15% Oroglas HT121}/Kynar 740
80 μm/300 μm/2 000 μm
Example 5
The structure below is prepared in the same way as in Example 3:
Accomet PC/Scotchkote 6258/binder {85% Kynar 2850-04, 15% Oroglas HT121}/Kynar 740
80 μm/300 μm/1 400 μm
Example 6
The structure below is prepared in the same way as in Example 1:
Eurokote 798/binder {85% Kynar 2850-04, 15% Oroglas HT121}/Kynar 740
80 μm/300 μm/1 400 μm
TABLE I
Results of peeling in N/cm and breaking mode at 110, 130 and 150° C.
Structure
Example 1
Example 2
Example 3
Example 4
Example 5
Example 6
110° C. Mean
147
134
141
158
167
164
Standard
±9
±8
±5
±10
±4
±10
deviation
Mode
CP
CP
C
C
CP + F
CP + F
130° C. Mean
108
114
117
106
125
—
Standard
±9
±10
±10
±14
±1
—
deviation
Mode
CP
CE
C
C
CP + F
—
150° C. Mean
40
7
56
42
40
10
Standard
±10
±16
±21
±1
±3
deviation
Mode
CP/AO
AO
C
C
C
AO
Breaking modes: C = cohesive break in the binder, CE = cohesive break in the binder in the outer layer interface region, CP = cohesive break in the binder in the epoxy primer layer interface region, AO = primer adhesive-metal break, +F = with creep of the peeling arm
Structures with Binder Comprising the Fluoropolymer L2:
Example 8
The structure below is prepared in the same way as in Example 1:
Eurokote 798/binder {85% Kynar 3120-15, 15% MKB212}/Kynar 740
80 μm/300 μm/1 400 μm
The results are given in Table II.
Example 9
The structure below is prepared in the same way as in Example 1:
Eurokote 798/binder {70% Kynar 3120-15, 30% MKB212}/Kynar 740
80 μm/300 μm/1 400 μm
Example 10
The structure below is prepared in the same way as in Example 1:
Scotchkote 6258/binder {85% Kynar 3120-15, 15% MKB212}/Kynar 740
80 μm/300 μm/1 400 μm
TABLE II
Results of peeling in N/cm and breaking mode at 110, 130 and
150° C.
Structure
Example 8
Example 9
Example 10
110° C. Mean
169
187
162
Standard deviation
±4
±2
±1
Mode
CE + F
CE + F
C
130° C. Mean
134
142
128
Standard deviation
±4
±5
±2
Mode
CE + F
CE + F
CE + F
150° C. Mean
10
11
90
Standard deviation
±1
±5
Mode
AO
AO
CE + F
Breaking modes: C = cohesive break in the binder, CE = cohesive break in the binder in the outer layer interface region, CP = cohesive break in the binder in the epoxy primer layer interface region, AO = primer adhesive-metal break, +F = with creep of the peeling arm
|
The present invention relates to a coated metal surface comprising, successively:
a layer (1) of epoxy primer placed next to the metal,
a layer (2) of binder comprising 98 to 50 parts by weight of at least one fluoropolymer L3 per 2 to 50 parts, respectively, of at least one polymer chosen from acrylic polymers L1 and polymers L2 which are fluoropolymers chemically modified by a partial dehydrofluorination followed by an oxidation,
a layer (3) of fluoropolymer.
According to a first variant, the coating does not comprise the layer (3). However, it is recommended that the layer (2) which becomes the outer layer should be thicker than in the structure of the main invention.
According to a second variant, the coating does not comprise the layer of primer (1), the layer of binder necessarily contains the polymer L2 and the surface is necessarily the outer surface of tubes.
According to a third variant, the coating does not comprise the layer (2) and the layer (1) comprises a mixture of epoxy primer and polymer L2.
The invention relates more particularly to the coating of the outer surface of tubes. These tubes are useful for the development of offshore hot oil wells, since it is necessary for the tubes which transport the hot oil to withstand corrosion by seawater.
| 8
|
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of co-pending provisional application Ser. No. 61/925,078, filed on Jan. 8, 2014, entitled “LYRE CAPABLE OF SECURING A READABLE ELECTRONIC TABLET OR MOBILE DEVICE TO A MUSICAL INSTRUMENT.”
FIELD
[0002] The present invention relates to music lyres, and more particularly to a music lyre which holds an electronically powered tablet, smart phone, or other mobile media device, and stores and displays data of musical notation and other music-related media.
BACKGROUND
[0003] Traditionally, a marching band musician carries a music book (plastic folio folder), which contains dozens of paper-printed pages of sheet music, on a lyre attached to their musical instrument (trumpet, saxophone, drum, etc.). The lyre is typically a spring biased clip that grips the bottom of the folio. When the folios become packed with paper and gains excessive weight the entire device becomes cumbersome and unwieldy. The user becomes limited in the movement they have due to the possibility of the music and the device falling off or spilling its contents.
[0004] Paper folios containing dozens of printed pages of sheet music quickly acquire mass and bulk becoming difficult to manage and read during inclement weather when attached to the lyre. These conditions constrain the musician's mobility and musical performance while searching for specific music. Additionally, in windy conditions, the sheet music may blow or flip making it difficult for the musician to play the desired music.
SUMMARY
[0005] The invention replaces the traditional lyre with a “smart lyre” designed to hold an electronically powered tablet, smart phone, or other mobile media device, which stores and displays data of musical notation and other music-related media.
[0006] The use of mobile device secured to the smart lyre negates the limited capacity of paper music or information the musician has available during a performance. The smart lyre, holding a tablet or smart phone enables the musician to access and view virtually unlimited amounts of electronic music and information, which can be updated repeatedly thus eliminating excess use of print and paper.
DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1 is a prior art lyre for supporting a music folio;
[0008] FIG. 2 is a front elevation view of the music lyre of the present invention;
[0009] FIG. 3 is a back elevation view of the music lyre of the present invention;
[0010] FIG. 4 is a perspective view of the music lyre of the present invention;
[0011] FIG. 5 is a side view of the case of the music lyre of the present invention;
[0012] FIG. 6 is a back elevation view of the music lyre showing the case separated from the mounting plate;
[0013] FIG. 7 is an exploded perspective view of the music lyre of the present invention;
[0014] FIG. 8 is a side exploded perspective view of the music lyre of the present invention; and
[0015] FIG. 9 is a back exploded perspective view of the music lyre of the present invention.
DETAILED DESCRIPTION
[0016] Referring initially to FIG. 1 , a prior art musical instrument lyre 10 includes a support rod 12 secured to a clamp 14 for support paper sheet music or paper folio 16 . The support rod 12 may be secured to a receiver (not show) attached to a musical instrument (not shown). The prior art musical instrument lyre 10 is not mechanically designed to securely hold a mobile or tablet device to an instrument. The use of paper sheet music for a musical ensemble creates storage issues; can be costly to print, heavy and contributes to the excessive use/waste of paper, unlike digitally stored media/music saved and stored in a mobile or tablet device attached to a smart lyre. A marching band musician carries a music book (plastic folio folder), which contains dozens of paper-printed pages of sheet music, on a lyre attached to their musical instrument (trumpet, saxophone, drum, etc.). When the folios become packed with paper and gains excessive weight the entire device becomes cumbersome and unwieldy. The user becomes limited in the movement they have due to the possibility of the music and the device falling off or spilling its contents. The present invention replaces the traditional lyre with a “smart lyre” designed to hold an electronically powered tablet, smart phone, or other mobile media device, which stores and displays data of musical notation and other music-related media. The invention claimed here solves this problem.
[0017] Referring to FIGS. 2-5 , a music lyre of the present invention generally indicated by reference numeral 20 . The music lyre 20 includes a case 22 adapted to support and secure a mobile electronic device 24 . The musician places a mobile device 24 or tablet into the smart lyre 20 , which is affixed to the musician's instrument (not shown) that permits the user to read musical notation 26 on the device/tablet's display screen 28 while simultaneously permitting the musician, while standing or marching, to observe the musical conductor. The smart lyre 20 also permits the user to view printed instructions; review or record performance video and audio for evaluation. Viewing material on the mobile device 24 or tablet eliminates weight and paper storage concerns for the user.
[0018] Also, it can allow a tablet or mobile device affixed to the invention to be able to produce an audio or visual record, as well as annotation on a mobile or tablet device while holding the musical instrument in a playing position.
[0019] The case includes a hard rubber or plastic housing which may be coated with silicone or other soft rubber and is adapted and sized to receive a tablet and or mobile device 24 . The case 22 provides a secure fit for the mobile device 24 ensuring the device 24 will not fall out of the case 22 during use. The back of the case 22 has raised parallel plastic rails 30 to allow the mobile enclosure to couple to a mounting plate 32 secured to the end of a mounting bracket 34 . The back of the case 22 may also include a stop 36 to limit the mounting plate 32 from sliding through the rails 30 .
[0020] The mounting plate 32 may be made of a hard plastic that provides a rigid mounting for the case 22 and mobile device 24 or electronic tablet. The mounting bracket 34 may be plastic or metal, and may be coated in silicone rubber. The mounting bracket 34 is secured to the mounting plate 32 . A free end 38 of mounting bracket 34 is configured to be inserted into an open slot that is found universally mounted on almost all marching band instruments. The length of the mounting bracket 34 is determined according to each instrument's size and appropriate viewing distance.
[0021] The music lyre 20 provides a secure shell/mold for the mobile device 24 and holds and protects the mobile device 24 while it is being used. The tablet or mobile device's 24 screen 28 is visible and accessible to user control inputs. The sides of the case 22 surrounding the device allow physical inputs for headphones or other mobile or tablet components the user may attach while still having the mobile device 24 or tablet device secured and used.
[0022] The case 22 . includes rails 30 on the back to allow easy joining and removal of the bracket 34 from the case. A user aligns the mounting plate 32 with the rails 30 of the case 22 to mate the case 22 to the mounting bracket that will be connected into the musical instrument opening.
[0023] The mounting bracket 34 may be angled, depending on the form and function of the musical instrument, as to allow o be connected to an open slot/receiver that is found universally on almost all marching band instruments (not shown).
[0024] A mold of the case 22 may be designed to accept a tablet, smart phone, or other mobile device 24 . The mounting bracket 34 may be permanently joined to the mounting plate 32 or may be releasably coupled to the mounting plate 32 . Alternatively, the mounting plate 32 may be an integral part of the case 22 with a receiver for receiving an end of the mounting bracket 34 opposite the free end 38 .
[0025] A secure fit of a tablet or mobile device 24 as well as a secure fit of the case 22 to the mounting bracket 34 that will support the weight of the device is desired. The video/data screen 28 of the device 24 should be viewable without obstruction while secured in the smart lyre 20 . The mounting plate 32 that slides and connects to the back of the case 22 should fit firmly without allowing vibration between the bracket and the enclosure. The mounting bracket 34 should be of an appropriate thickness, strength, and angled correctly to equally fit in the open slot/receiver found universally on marching band instruments for readability (not shown).
[0026] Mold may be created to fit different tablet or mobile device sizes depending on the needs of the user. By making the tablet or mobile device case 22 and the mounting bracket 34 two different pieces, a user could may the case 22 from one mounting bracket 34 and quickly attach the tablet or mobile device in the shell to another mounting bracket 34 that can fit a different instrument. The appropriate use of one enclosure for a saxophone would not facilitate its use for a clarinet. The clarinet would need a ring mount to the body of the instrument. A marching drum would not need the bent right angles but rather a straight metal wire extending from its unique lyre input. The interchangeability provides variable uses to the musical instrument spectrum.
[0027] Musicians, college and secondary school musical ensembles may have their traditional paper sheet music electronically stored and available to view on a mobile device 24 they already own. The musician would place the mobile device 24 securely into the case 22 and attach the case to their instrument thus allowing the musician to read the musical notes 26 or information on device's display screen 28 . A student musician using the musical lyre 20 in combination with a tablet or mobile device 24 may record the audio of their performance, annotate instructions, video graph their movement on a marching band field or any number of the musical abilities mobile devices 24 may provide. This invention allows modern electronic devices to be used in more depth than previous instrumental sheet music holding devices currently available, The present invention, in combination with the tablet or mobile device 24 eliminates the need for paper folios and facilitates a faster method of distributing music-related materials and related content to the musician and ensemble.
[0028] The music lyre 20 may include ports 40 and 42 in the case 22 , which also allows a tablet or mobile device 24 to record the performance, as well as allow annotation on a mobile or tablet device while holding the musical instrument in a playing position.
[0029] It is to be understood that while certain forms of this invention have been illustrated and described, it is not limited thereto, except in so far as such limitations are included in the following claims and allowable equivalents thereof.
|
Lyre capable of securing a readable electronic tablet or mobile device to a musical instrument is disclosed. The use of mobile device secured to the smart lyre negates the limited capacity of paper music or information the musician has available during a performance. The smart lyre, holding a tablet or smart phone enables the musician to access and view virtually unlimited amounts of electronic music and information, which can be updated repeatedly thus eliminating excess use of print and paper.
| 5
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of Ser. No. 507,440, filed June 24, 1983, which is a continuation-in-part of Ser. No. 358,637, filed Mar. 16, 1982, now abandoned for YARNS AND TOWS COMPRISING HIGH STRENGTH METAL-COATED FIBERS, PROCESS FOR THEIR PRODUCTION, AND ARTICLES MADE THEREFROM by Louis George Morin. This application is also related to applications for IMPROVED TENSIONING MECHANISM AND CATHODE ROLLERS FOR FIBER PLATING by Louis George Morin and Robert E. Hoebel (110-024) and CONTACT ROLLER MOUNTING ASSEMBLY AND TENSIONING MECHANISM FOR ELECTROPLATING FIBER by Robert E. Hoebel (110-029), both filed June 24, 1983.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to metal coated filaments and to a process and an apparatus for their continuous production.
2. Description of the Prior Art
Filaments comprising non-metals and semi-metals, such as carbon, boron, silicon carbide, polyester, nylon, aramid, cotton, rayon, and the like, in the form of monofilaments, yarns, tows, mats, cloths and chopped strands are known to be useful in reinforcing metals and organic polymeric materials. Articles comprising metals or plastics reinforced with such fibers find wide-spread use in replacing heavier components made up of lower strength conventional materials such as aluminum, steel, titanium, vinyl polymers, nylons, polyester, etc., in aircraft, automobiles, office equipment, sporting goods, and in many other fields.
A common problem in the use of such filaments, and also glass, asbestos and others, is a seeming lack of ability to translate the properties of the high strength filaments to the material to which ultimate and intimate contact is to be made. In essence, even though a high strength filament is employed, the filaments are merely mechanically entrapped, and the resulting composite pulls apart or breaks at disappointingly low applied forces
The problems have been overcome in part by depositing a layer or layers of metals on the individual filaments prior to incorporating them into the bonding material, e.g., metal or plastic Metal deposition has been accomplished by vacuum deposition, e.g., the nickel on fibers as described in U.S. Pat. No. 4,132,828; and by electroless deposition from chemical baths, e.g., nickel on graphite filaments as described in U.S. Pat. No. 3,894,677; and by electrodeposition, e.g., the nickel electroplating on carbon fibers as described in Sara, U.S. Pat. No. 3,622,283 and in Sara, U.S. Pat. No. 3,807.996. When the metal coated filaments of such procedures are twisted or sharply bent, a very substantial quantity of the metal flakes off or falls off as a powder. When such metal coated filaments are used to reinforce either metals or polymers, the ability to resist compressive stress and tensile stress is much less than what would be expected from the rule of mixtures, and this is strongly suggestive that failure to efficiently reinforce is due to poor bonding between the filament and the metal coating.
It has now been discovered that if electroplating is selected and if an amount of voltage is selected and used in excess of that which is required to merely dissociate (reduce) the electrodepositable metal ion on the filament surface, a superior bond between filament and metal layer is produced. The strength is such that when the metal coated filament is sharply bent, the coating may fracture, but it will not peel away. Moreover, continuous lengths of such metal coated filaments can be knotted and twisted without substantial loss of the metal to flakes or powder. High voltage is believed important to provide or facilitate uniform nucleation of the electrodepositable metal on the filament, and to overcome any screening or inhibiting effect of materials absorbed on the filament surface.
Although a quantity of electricity is required to electrodeposit metal on the filament surface, an increase in voltage to increase the amperes may cause the filaments to burn, which would interrupt a continuous process. The aforesaid Sara U.S. Pat. No. 3,807,966, uses a continuous process to nickel plate graphite yarn, but employs a plating current of only 2.5 amperes, and long residence times, e.g. 14 minutes, and therefore low, and conventional, voltages. In another continuous process, described in U.K. Pat. No. 1,272,777, the individual fibers in a bundle of fibers are electroplated without burning them up by passing the bundle through a jet of electrolyte carrying the plating material, the bundle being maintained at a negative potential relative to the electrolyte, in the case of silver on graphite, the potential between the anode and the fibers being a conventional 3 volts.
The present invention provides an efficient apparatus to facilitate increasing the potential between anode and the continuous filament cathode, since it is a key aspect of the present process to increase the voltage to obtain superior metal coated fibers. In addition, since it permits extra electrical energy to be introduced into the system without burning up the filaments, residence time is shortened, and production rates are vastly increased over those provided by the prior art. As will be clear from the detailed description which follows, novel means are used to provide high voltage plating, strategic cooling, efficient electrolyte-filament contact and high speed filament transport in various combinations, all of which result in enhancing the production rate and quality of metal coated filaments. Such filaments find substantial utility, for example, when incorporated into thermoplastic and thermoset molding compounds for aircraft lightning protection, EMI/RFI shielding and other applications requiring electrical/thermal conductivity. They are also useful in high surface electrodes for electrolytic cells. Composites in which such filaments are aligned in a substantially parallel manner dispersed in a matrix of metal, e.g., nickel coated graphite in a lead or zinc matrix are characterized by light weight and superior resistance to compressive and tensile stress. The apparatus of this invention can also be employed to enhance the production rate and product quality when electroplating normally non-conductive continuous filaments, e.g., polyaramids or cotton, etc., if first an adherent electrically conductive inner layer is deposited, e.g., by chemical means on the non-conductive filament
SUMMARY OF THE INVENTION
It is a basic object of the present invention to provide fibers formed of a conductive semimetallic core with metallic coatings.
It is another object of the present invention to provide a process in which the electroplating of the fibers is effected under high voltage electroplating conditions.
Further, it is an object of the present invention to provide a process and apparatus which will efficiently and rapidly coat fibers with metallic coatings and facilitate the rinsing and collecting of the finished product.
A still further object of the present invention is to provide fibers that are evenly plated around their diameter to the extent that any deviation in thickness of the plating is less than ten percent.
It is also an object of the present invention to plate all the fibers in a tow with the same width of material, within ten percent, regardless of whether the tow width is small or large, i.e., 3K to 12×12K.
It has been found that these and other objects are obtained by the use of high voltages in the apparatus and process of the subject invention.
In accordance with the present invention, apparatus has been provided in which a plurality of fibers can be simultaneously plated efficiently with a metal surface and thereafter cleaned and reeled for use in a variety of end products.
The apparatus is provided generally with a pay-out assembly adapted to deliver a multiplicity of fibers to an electrolytic plating bath. The pre-treatment process includes tri-sodium phosphate cleaning, rinsing and acid wash. Thereafter, metal-plating is performed in a continuous process by the passage of the clean fibers through an electrolyte in which the plating of the fibers is carried out at high voltage conditions. Means are provided to cool the fibers during the passage from the contact roll associated with the electrolytic tank and the electrolyte bath. Preferred means, in essence, are constituted by a recycle of electrolyte at strategic positions over the contact rollers and the fiber. The process also contemplates a series of discrete electrolytic tanks associated with separate rectifiers to facilitate variable current plating. The current is varied as a function of the resistance developed by the plating on the fibers.
After the plating has been completed, the plated fibers are rinsed by water and steam treated and thereafter dried.
As a result of the high voltage electroplating process, the continuous line is provided with means for synchronization of each of the process steps with the other. The high voltage environment also includes a specially designed commutation system for the contact rollers in which fingers of unequal length are provided and by the specially designed anode arrangement comprising an anode basket, a portion of which is coated with insulation for protection from the electrolyte bath.
The rinse tanks and electrolytic tanks are specially designed for maintenance of electrolyte level and minimal accumulation of waste rinse fluid.
The special rollers developed to use in the pay-out further facilitate the effectiveness of the process.
DESCRIPTION OF THE DRAWINGS
The invention will be more readily understood when viewed in association with the following drawings wherein:
FIG. 1 is a schematic view of the overall process of the subject continuous electrolytic plating process except for the pay-out assembly.
FIG. 2 is an elevational view of the pay-out section arranged specifically to simultaneously deliver a multiplicity of fibers to the electrolytic plating operation.
FIG. 3 is a plan view of the pay-out assembly of FIG. 2.
FIG. 4 is a sectional elevational view of the pay-out roller assembly.
FIG. 5 is a sectional view through line 5--5 of FIG. 4.
FIG. 6 is an isometric view of the wetting and tensioning rollers between the pay-out and electrolytic bath.
FIG. 7 is a sectional elevational view of the pre-treatment tank and associated apparatus.
FIG. 8 is an elevational view of one electrolytic tank.
FIG. 9 is a plan view of the tank of FIG. 8.
FIG. 10 is a sectional elevational view through line 10--10 of FIG. 8.
FIG. 11 is an isometric view of the commutation fingers.
FIG. 12 is an isometric view of one contact roller in association with the means for providing coolant to the fibers and a current carrying medium from the contact roller to the bath.
FIG. 13 is an elevational view of a section of the electrolytic tank depicting an anode basket.
FIG. 14 is a plan view of the means for delivering electrolyte to the fibers extending from the contact roller to the electrolytic bath.
FIG. 15 is a detail plan view of the nozzles of the spray assembly of FIG. 12.
FIG. 16 is a schematic of the electrolytic coolant conductor and a contact roller.
FIG. 17 is a sectional elevational view of a contact roller of the process assembly.
FIG. 18 is a detail of the end cap of the roller of FIG. 17.
FIG. 19 is a partial detail of the opposite end of the roller of FIG. 17.
FIG. 20 is a partially exploded sectional elevational view of the contact mount for the anode basket.
FIG. 21 is an isometric view of the anode basket of the subject invention.
FIG. 22 is a view of the electrical system of the present invention.
FIG. 23 is a sectional elevational view of the rinse tanks and associated apparatus.
FIG. 24 is a sectional elevational view of the washing-tee of the subject invention.
FIG. 25 is a view through line 25--25 of the washing-tee of FIG. 24.
FIG. 26 is a view through line 26--26 of the washing-tee of FIG. 24.
FIG. 27 is a drawing of the mechanism for synchronously driving the apparatus of the subject invention.
FIG. 28 is a plan view through line 28--28 of the section of FIG. 27.
FIG. 29 is a side elevational view of the roller assembly in the drying section of the system.
FIG. 30 is a sectional view of a guide roller shown through line 30--30 of FIG. 29.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The process and apparatus of the present invention are directed to providing an efficient and complete means for metal-plating non-metallic and semi-metallic fibers.
The process of the invention relies on the use of very high voltage and current to effect satisfactory plating. As a result of the high voltage and current, an apparatus has been developed that can produce high volumes of plated material under high voltage conditions.
The process of the present invention and the apparatus particularly suitable for practicing the process of the invention are described in the preferred embodiment in which the specified fiber to be plated is a carbon or graphite fiber and the plating metal is nickel. However, the process and apparatus of the present invention are suitable for virtually the entire spectrum of metal-plating of non-metallic and semi-metallic fibers.
The overall process and schematic of the apparatus except for the pay-out assembly are generally shown in FIG. 1. The operative process includes in essence, a pay-out assembly for dispensing multiple fibers in parallel, tensioning rollers 6, a pre-treatment section 8, a plating facility 10, a rinsing station 12, a drying section 14 and take-up reels 16.
More particularly, the pre-treatment section 8 shown generally in FIG. 1 includes a tri-sodium phosphate cleaning section 26 and an associated washing-tee 28, rinse section 30 and associated washing-tees 32 and 32A, a hydrochloric acid section 34 and associated tee 36, and rinse section 38 with associated washing-tees 40 and 40A all of which are described in FIG. 7. The plating facility 10 is comprised of a plurality of series arranged electrolyte tanks shown illustratively in FIG. 1 as tanks 18, 20, 22 and 24, each of which is charged with current by a separate rectifier, better seen in FIGS. 8 and 22. The rinsing section 12, shown generally in FIG. 1 is comprised of tank and tee assemblies similar to the pre-treatment apparatus. An arrangement of cascading tanks 42 and tees 44, 44A and 44B cycle rinse solution of water and electrolyte over the fibers 2. Thereafter, clean water is passed over the fibers 2 in the rinse section 46 provided with tanks and washing-tees 48 and 48A seen more specifically in FIG. 26. The rinsed fiber 2 is passed through section 50 wherein it is air blasted in subsection 53 and then steam-treated in section 55 to produce an oxide surface on the metal plate. The process is completed by passage of the metal plated fiber 2 through the drying unit 14 and reeling of the finished fibers on take-up reels 17 in the reeling section 16.
As seen generally in FIG. 1, the apparatus is provided with means to convey the fibers 2 through the system rapidly without abrading the fibers 2. The combination of strategically located guide rollers 51, tension rollers 6, force imposing rollers in the drying section 14 and a synchronous drive assembly shown in FIG. 27 rapidly conveys the fibers 2 through the apparatus without abrasion of the fibers 2.
The operation begins with the pay-out assembly 4 shown in FIGS. 2 and 3. Functionally, the fibers 2 from the pay-out assembly 4 are delivered over a guide roller 5 through the tensioning rollers 6 to the pre-treatment section 8.
As best seen in FIGS. 2 and 3, the pay-out assembly 4 is comprised of a frame 52 on which the pay-out rollers 54 are mounted. The structure of the rollers 54 is better seen in FIGS. 4 and 5 and will be described more particularly in association with FIGS. 4 and 5. The pay-out rollers 54 are mounted on the frame 52 on a rail 56 and a rail 58. The rollers 54 on rail 56 are arranged to pay-out the fibers 2 to the electroplating system while the rail 58 is an auxiliary rail adapted to mount the spare rollers 54 available to provide alternate duty. A rail 60 mounts guide rollers 62 over which the fibers 2 from the pay-out rollers 54 travel to reach the tensioning rollers 6. As best seen in FIG. 2, the fibers 2 extend from the respective rollers 54 over individual guide roller 62 associated with a particular roller 54 to the common guide roller 5 and into the tensioning roller assembly 6. Guide bars 59 are provided to guide fibers 2 from the pay-out rollers 54 to the associated guide rollers 62.
As seen in FIG. 3, the guide rollers 62 are aligned adjacent to each other to avoid interference between the fibers 2 as a plurality of fibers 2 are simultaneously delivered to the system to be treated and plated.
The structure of the pay-out rollers 54 is best seen in FIGS. 4 and 5. The pay-out rollers 54 are comprised essentially of a centrally disposed rod 66 having end bearings 68 and 70, and are arranged to accommodate a compressive frame 64 formed of wires 72. Practice has taught that four resilient wires 72 arranged ninety degrees from each other will form a frame 64 suitable for mounting most commercial spools of fiber. Bearing 68 is arranged to bear against either the rail 56 or the rail 58 of the pay-out assembly 4.
The rod 66 is provided with a threaded end 76 that passes through an opening in the rails 56 or 58. A conventional nut (not shown) is used to attach the pay-out roller 54 which is thus cantilever mounted with the free end bearing 70 having a sliding fit on the bar 66. Thus, if the pay-out roller frame wires 72 are compressed, the bearing 70 can move transversely on the rod 66. Further, the frame wires 72 of the roller mount 64 are provided with tapered ends 74. As a result of the taper in the frame wires 72 and the transversely movable bearing 70, the compressive frame 64 can adjust to accept fiber spools of various diameter.
The pay-out assembly 4 delivers the fibers 2 over a guide roller 5 to a wetting roller 80 and then to the tensioning rollers 6. A wetting tub 84 is provided with water which wets the fibers 2 and enables suitable and more efficient cleaning and rinsing of the fibers 2 during pre-treatment. The tensioning rollers 6 seen in FIG. 1 are shown in more detail in FIG. 6.
The tensioning rollers 6 comprise an assembly of five rollers 90, all of which are driven through a single continuous chain 87 by a common source such as a variable speed motor 92. Each roller 90 is mounted on a shaft 89 which also mounts a fixed gear 91 around which the chain 87 is arranged. Idler rollers 97 are also arranged to engage the chain 87. A gear 93 extending from the shaft 95 of the variable speed motor 92 drives the continuous chain 87 through a chain 101 and a gear 103 fixed to the shaft 89 of a roller 90. It is necessary that tension be provided to the fibers 2 at a location in the line upstream of the first plating contact roller. The plating contact roller and the fibers 2 must be in tight contact to facilitate the operation at the high voltage and high current levels necessary for the process. With tight contact, low resistance is provided between the fibers 2 and the contact rollers, thus the high current passing through the system circuit will not overload the fibers 2 causing destruction of the fibers. As a result, the tension roller assembly 6 is located upstream of the electroplating tanks 18, 20, 22, 24 (FIG. 1) to provide that tension. On the other hand, the fibers should be subjected to as little drag as possible. Inherent in the fibers 2 is the tendency to separate at the surface and accumulate fuzz. The variable drive motor 92 is coupled to all five of the rollers 90 to provide variable speed for the rollers at some speed equal to or less than the speed of the fibers 2. At carefully controlled speeds the necessary tension is provided without causing fuzz to accumulate on the fibers. The apparatus and process are designed to afford a tension roller assembly 6 in which the tension rollers 90 travel at a slower speed than the fibers 2. The tension on the fibers 2 is maintained by varying the speed of the tension roller 90 in response to visual determination of the tension.
In the pre-treatment section 8, best seen in FIGS. 1 and 7, the apparatus is comprised of a tri-sodium phosphate cleaning section 26 followed by a rinse section 30, and an acid cleaning section 34 followed by another rinse section 38. Each of the pre-treatment sections 26, 30, 34 and 38 are provided respectively with washing-tees 28, 32-32A, 36 and 40-40A shown in detail in FIGS. 22-24. Each pre-treatment section 26, 30, 34 and 38 is also provided with a tank into which the discharge from the washing-tees 28, 32A, 32, 63, 40A and 40 flow. The tri-sodium phosphate cleaning section 26 and the acid cleaning station 34 have single tanks 27 and 31 respectively. The rinse sections 30 and 38 have two tanks each, 33, 41 and 39, 49 respectively. In operation the fibers 2 pass through the tees 28, 32A, 32, 36, 40A and 40 in one direction while fluid passes through in the opposite direction.
A tri-sodium phosphate cleaning solution of generally any suitable concentration can be used in the cleaning section 26. However, practice has taught that eight ounces of tri-sodium phosphate per gallon of water at 180° F. will provide the cleaning necessary for carbon fibers. Water is used in the rinse section 30 to remove residual tri-sodium phosphate from the fibers 2 exiting from the tri-sodium phosphate section 26.
The fibers then pass through the tee 36 in the acid cleaning section 34 as the acid solution passes counter-currently with the fibers 2. The acid suitable for pre-treatment in association with the tri-sodium phosphate cleaning is a 10% hydrochloric acid solution. Thereafter, the fibers 2 are rinsed with water in the rinse section 38 wherein water again enters through the top of the tees 40 and 40A and exists through the upstream section of the tee opening thereby passing counter-currently with the fibers 2.
As seen in FIG. 7, the pre-treatment section 8 is interconnected to facilitate the pre-treatment of the fibers 2 and to avoid or minimize the accumulation of contaminated pre-treatment solution. Each pre-treatment tank is provided with a stand pipe 308 that has a basket filter 310 arranged over the opening. Discharge from the tank is pumped from each tank through the stand pipe 308 by a pump 306. A line 316 from the stand pipe 308 in the rinse tank 49 communicates with the fluid inlet of the tee 40A associated with the rinse tank 39. A line 326 is connected to the inlet of the tee 40 associated with the tank 49 and a discharge line 320 is provided for the discharge of fluid from the tank 39.
A recirculating line 314 extends from the stand pipe 308 in the tank 31 to the fluid inlet of tee 36 to recirculate the hydrochloric acid wash. An inlet line 324 is provided to deliver initial and make-up hydrochloric acid wash to the fluid side of the tee 36.
The rinse tanks 41 and 33 are provided with a line 325 to the fluid inlet of the tee 32 associated with the tank 41 and a line 316 from the stand pipe 308 in tank 41 to the inlet of the tee 32A associated with the tank 33. A discharge line 322 is provided for discharge from the tank 33.
The tri-sodium phosphate tank 27 is provided with both a recirculating line 312 from the stand pipe 308 to the inlet of the tee 28 and a line 300 to deliver initial and make-up tri-sodium phosphate to the fluid inlet of the tee 28.
A neutralizing tank 318 charged with a neutralizing agent 330, such as Dolomite, is provided in the system to receive hydrochloric acid discharge from rinse tank 39 and tri-sodium phosphate discharge from rinse tank 33.
In operation the fibers 2 pass through the tees 28, 32A, 32, 36, 40A and 40 as fluid passes from the fluid inlets of the tees out the upstream fiber entry openings of the tees. The tri-sodium phosphate wash is recycled through stand pipe 308 and recycle line 312. Residue on the fibers 2 after passage from the tee 28 is rinsed from the fibers 2 by clear water that passes through the tee 32 associated with the rinse tank 41 and discharge from the rinse tank 41 that passes through the tee 32A associated with the rinse tank 33. The fluid in the rinse tank 33 which becomes contaminated with tri-sodium phosphate is discharged to the neutralizing tank 318.
After the fibers 2 leave the rinse section 30, hydrochloric acid wash is passed over the fibers 2 in tee 36. The discharge from the tee 36 is recycled to the fluid inlet of the tee 36 through stand pipe 308 in the tank 31 and recirculation line 314. The fibers 2 leaving the tee 36 are rinsed in rinse section 38. Clear water enters the rinse section 38 through the tee 40 associated with the rinse tank 49 and flows to the rinse tank 49. The fluid from rinse tank 49 is pumped through line 316 to the fluid inlet of the tee 40A associated with the rinse tank 39 and passed over the fibers 2 into the rinse tank 39. The fluid in the rinse tank 39 becomes contaminated with hydrochloric acid and is discharged through line 320 to the neutralizing tank.
The nature of the tri-sodium phosphate and the hydrochloric acid in combination with a calcium based material such as Dolomite neutralize the waste and minimize the additional treatment required for the waste before discharge through line 328 to waste.
The pre-treated fibers 2 are next electroplated. As seen in FIG. 1, a plurality of electroplating tanks 18, 20, 22 and 24 are provided in series. Under the high voltage-high current conditions of the process, the series arrangement of electroplating tank 18, 20, 22 and 24 afford means for providing discrete voltage and current to the fibers 2 as a function of the accumulation of metal-plating on the fibers 2. Thus, depending on the amount of metal-plating on the fibers 2, the plating voltage and current can be set to levels most suitable for the particular resistance developed by the fiber and metal.
The electrolytic plating tank 18 is shown in FIGS. 8, 9 and 10 and is identical in structure to the plating tanks 20, 22 and 24 shown in FIG. 1. The tank 18 is arranged to hold a bath of electrolyte. The tank 18 has mounted therewith contact rollers 100 and anode support bars 102 which are arranged in the circuit. The contact rollers 100 receive current from the bus bar 104 and the anode support bars 102 are connected directly to a bus bar 106. Each of the plating tanks 18, 20, 22 and 24 are provided with similar but separate independent circuitry as seen in FIG. 22. The anode support bars 102 have mounted thereon anode baskets 110 arranged to hold and transfer current to nickel or other metal-plating chips.
Each tank 18, 20, 22 and 24 is also provided with heat exchangers 114 to heat the electrolyte bath to reach the desirable initial temperature at start-up and to cool the electrolyte during the high intensity current operation.
The tank 18 is provided with a well 103 defined by a solid wall 105 in which a level control 107 is mounted and with a recirculation line 109. The recirculation line 109 includes a pump 111 and a filter 113 and functions to continuously recirculate electrolyte from the well 103 to the tank 18. Under normal operating conditions recirculated electrolyte will enter the tank 18 and cause the electrolyte in the tank to rise to a level above the wall 105 and flow into the well 103. When electrolyte has evaporated from the tank the level in the well will drop and call for make-up from the downstream rinse section 12 shown in FIG. 26.
The tank 18 is also provided with a line 132 and pump 134 through which electrolyte is pumped to a manifold 128 that delivers the electrolyte to the spray nozzle 130 above the contact rollers 100.
As shown in more detail in FIG. 13, the fibers 2 pass over the contact rollers 100 and around idler rollers 112 located in proximity to the bottom of the tank. The idler rollers 112 are provided in pairs around which the fibers 2 pass to move into contact with the succeeding contact roller 100.
The rollers 100 in the tank 18 communicate with the bus bar 104 through contact member 118. The detail of the contact member 118 seen in FIG. 11 shows that the contact members 118 are formed of a copper bar 120 and a plural array of phosphor bronze fingers 122 and 124 that together provide the positive contact over a sufficiently large area on the contact roller 100 to avoid creating a high resistance condition at the point of contact. The fingers 122 and 124 are resiliently mounted on the bar 120 and by the nature of the material, are urged into contact with the contact roller 100 at all times.
Thus, a high strength positive electrical contact assembly is provided for an environment wherein conventional brush contacts cannot serve well.
The high voltage-high current process of the present invention is further facilitated by means for protecting the fibers 2 during the passage between the electrolyte bath and the various contact rollers. The system includes the recirculating spray system 126 shown generally in FIGS. 8 and 9 through which electrolyte is recycled from the plating tanks and sprayed through the spray nozzles 130 on the fibers 2 at contact points on the contact rollers 100.
The spray nozzles 130 are arranged with two parallel tubular arms 136 and 138 having nozzle openings 139 located on the lower surfaces thereof. As best seen in FIG. 15, one tubular arm 136 of the spray nozzle 130, is arranged to direct electrolyte tangentially on the fibers 2 at the point at which the fibers 2 leave the contact roller 100. The other tubular arm 138 of the spray nozzle 130 is arranged to deliver electrolyte directly on the top of the contact roller 100 at the point at which the fiber 2 engages the contact roller 100. As previously indicated, it is vital that sufficient tension be applied on the fibers 2 to insure that the fibers 2 are maintained in a tight direct line between the contact rollers 100 and the idler rollers 112. The need for a tight line is to assure that the low contact resistance suitable for current travel is available with high conductivity through the fibers 2 from the contact rollers 100 to the electrolyte bath. The electrolyte which is recirculated over the contact rollers 100 and the fibers 2 provide a parallel resistor in the circuit and serve to cool the fibers 2.
It is known that the fibers 2 being plated have a low fusing current, such as 10 amps for a 12K tow of about 7 microns in diameter. However, the process of the present invention requires about 25 amps between contacts or about 125 amps per strand in each tank.
Furthermore, both contact resistance and anisotropic resistance must be overcome. The contract resistance of 12K tow of about 7 microns on pure clean copper is about 2 ohms, thus at 45 volts twenty-two and one-half amps are required before any plating can occur. The anisotrophic resistance is 1,000 times the long axis. Thus, the total contact area must be 1,000 times the tow diameter, which for 7 microns is 0.34 inches. Practice has taught that one-half inch of contact will properly serve the electrical requirement of the system when plating 7 micron tow, hence two and three inch contact rollers 100 are used. It is also vital that the contact rollers 100 be located at a specified distance above the electrolyte bath to enable the system to operate at the high voltages necessary to achieve the plating of the process. In practice, it has been found that the contact rollers 100 should be located one-half to one inch from the electrolyte bath when voltages of 16 to 25 volts are applied. Further, it has been found that recirculation of about 2 galons per minute per contact roller traveling at about 11/2 to 25 ft./min. will properly cool the fiber and provide a suitable parallel resistor when above 5,000 amps are passed through the system on three cells.
The electrolyte in the process is a solution constituted of eight to ten ounces of metal, preferably in the form of NiCl 2 and NiSO 4 per gallon of solution. The pH of the solution is set at 4 to 4.5 and the temperature maintained between 145° and 150° F. Recirculation of the electrolyte through the spray nozzles 130 at the desired rate requires that the nozzle openings be 3/32 inches in diameter on 1/8" centers over the length of each tubular arm 136 and 138. The presence of electrolyte on the fibers is vital, but care is taken to avoid excessive electrolyte otherwise the contact rollers will become subjected to the plating occurring in the electrolyte.
The anode support bar 102 for the anode basket 110 is shown in detail in FIG. 20 and is comprised of essentially three layers. A steel inner bar 150 is provided to afford structural support for the anode basket 110. A copper coating 152, such as a copper pipe, over the steel bar 150 is provided to afford the electrical properties desirable for the passage of current, and an insulator of some material, such as vinyl 154, is provided to insulate the entire anode support bar 102. At strategic locations on the bar 102, the vinyl is removed and notches 156 expose the copper coating 152 to afford electrical contact.
As best seen in FIG. 21, the anode basket 110 is provided with the conventional openings 158 found in anode baskets but also has a vinyl insulated covering 162 that extends from the top of the anode basket 110 to a location below the surface of the electrolytic bath. Practice has taught that insulating the anode basket 110 four to twelve inches from the top will protect the anode basket 110 from destruction of the protective oxide under the high intensity current and voltage conditions experienced in the process. The conventional hooks 160 found on the anode baskets 110 are arranged to fit within the notches 156 provided on the anode support bar 102. Further, the anode basket is preferably made of titanium due to the nature of the high voltage environment and the electrolyte. The high voltage has been found to remove the surface of the titanium which is normally a TiO 2 layer that protects the anode basket 110 from the electrolyte.
The contact rollers 100 are shown in detail in FIGS. 17-19. Each contact roller 100 is located in close proximity to the electrolyte in the plating tanks and each is adapted to transmit high current through the system in a high intensity voltage environment. The contact roller 100 thus is designed for continual replacement. The contact roller 100 is provided with fixed end mounting sections 170 and 172 which hold a cylindrical copper tube 174. The cylindrical copper tube 174 is arranged to contact the commutator fingers 122-124 and deliver current through both the fibers 2 and recycled electrolyte to the electrolyte bath. The copper tube 174 is formed of conventional type L copper which must be able to carry 350 amperes. The diameter of the tubing is critical in that the diameter dictates the contact surface for the fibers 2 and the distance that the contact roller 100 will be from the electrolyte surface. As a result, the mounts 170 and 172 are fixedly arranged in alignment with each other to releasably support the tube 174 of the contact roller 100. The mount 170 is provided with a bearing support 176 through which a screw mount 178 passes. The screw mount 178 rotatably supports the copper tube 174 on a bushing support 180 and has the capacity to release the copper tube 174 upon retraction of the bushing support 180 by withdrawing the screw 178. The mount 172 includes a bushing support 182 on which a detent 184 is formed. Each copper tube 174 is provided with a notched mating slot 186 to fit around the detent 184 and effect positive attachment of the copper tube 174 to the bushing support 182 thereby obviating any uncertainty in alignment and facilitating dispatch in replacing each copper tube section 174.
The overall electrical system 188 of the process and apparatus is shown schematically in FIG. 22 wherein the capacity for discrete application of voltage and current to each electrolytic tank 18, 20, 22, 24 can be seen. Conventional rectifiers 189, 191, 193 and 195 are arranged as a D.C. power source to deliver current to the respective contact rollers 100 on each electrolytic tank. Bus bars 104, 194, 196, 198 are shown for illustration extending respectively from the rectifiers 189, 191, 193 and 195 to one of the six contact rollers 100 on the electrolytic tanks 18, 20, 22 and 24. However, all six contact rollers 100 on each electrolytic tank are directly connected to the same bus bar. Bus bars 106, 202, 204 and 206 are shown extending respectively from the same rectifiers 189, 191, 193 and 195 through cables 208 to one anode support bar 102 mounted on the electrolytic tanks 18, 20, 22 and 24. Again the respective anode bus bars contact each anode support bar 102 mounted on each electrolytic tank connected to the bus bar.
As a result of the arrangement, discrete high voltage can be delivered to each electrolytic tank 18, 20, 22, 24 as a function of the metal plating on the fibers 2 in each electrolytic tank.
Practice has taught that in volume production the voltage in the first electrolyte tank 18 should not be below 16 volts and seldom be below 24 volts. The voltage in the second tank 20 should not be below 14 volts and the voltage in the third electrolyte tank 22 should not be below 12 volts.
Illustratively, fibers 2 have been coated in a system of three rectifier-electrolyte tank assemblies, rather than the four shown in FIGS. 1 and 22, under the following conditions wherein excellent coating has resulted:
______________________________________RECTIFIER 189 191 193AMPS 1,400 1,400 1,400VOLTS 45 26 17______________________________________
The nickel metal coated fibers 2 produced under these conditions have the following properties and characteristics:
______________________________________Filament Shape Round (but dependent on graphite fiber)Diameter 8 micronsMetal Coating Approximately 0.5 microns thick, about 50% of the total fiber weight.Density 2.50-3.00 grams/cm..sup.3Tensile Strength Up to 450,000 psiTensile Modulus 34 M psiElectrical 0.008 ohms/cm. (12K tow)Conductivity 0.10 ohms/1000 strands/cm.______________________________________
After the nickel plating has occurred, the fully plated fibers 2 are delivered to the rinsing section 12 seen in FIG. 1.
The drag-out section 42 and rinse section 46 are arranged with tanks to accumulate the discharge from the tees 44, 44A, 44B, 48 and 48A and both neutralize the discharge for waste disposal and provide a repository for accumulation of make-up for the electrolyte tanks 18, 20, 22 and 24.
As best seen in FIG. 23, the tanks in the drag-out section 42 consist of a cascading tank with separate compartments 252, 254 and 256. The cascading tank is a conventional three station cascade counter-current rinse tank manufactured by National Plastics, Thermal Electron Division. The cascading tank automatically provides for passage of the discharge fluid from the downstream tanks to the upstream tank by passage around the overflow dams 258. The fluid accumulated in tank 256 will reach a level above the separation wall 255 between tank 256 and tank 254 and pass to tank 254. Similarly, when the level in tank 254 is greater than the level of the separation wall 251, the fluid will pass further upstream to tank 252.
The rinse section includes tanks 250 and 260. Both tanks 250 and 260 are provided with stand pipes 268 having basket filters 270 arranged at the top opening. A conveying line 261 is connected to the stand pipe 268 in tank 260 and is provided with the pump 264. The discharge from tank 260 is pumped to the tee 48A associated with tank 250 to rinse the fibers 2. The discharge from the tank 250 is delivered through line 276 to the cascading tank assembly, or alternatively through line 278 to waste disposal.
A line 271 is provided to connect the discharge in the tank 252 to the tanks 18, 20, 22 and 24 which are equipped with level control devices 107 that open solenoid valve 273 when the level in a tank 18, 20 , 22 or 24 drops to a level that requires electrolyte.
In the operation, the fibers 2 pass through the tees 44B, 44A, 44, 48A and 48 and are rinsed with water. The clear water is delivered to the system through line 267 to the tee 48 and flows counter to the direction of the fibers 2 to discharge through the upstream end of the tee 48 into the tank 260. The discharge from the tank 260 is pumped to the fluid inlet of tee 48A and is discharged through the upstream end of the tee 48A into the tank 250. The fluid in the tank 250 is relatively dilute due to the previous rinse treatment of the fibers 2, thus it can be discharged through line 278 as waste or delivered to the tank 256 as needed. The tanks 256, 254 and 252 operate continuously in the recirculation mode, thereby producing a fluid that becomes increasingly rich in electrolyte. As a result, a minimum of contaminated water is generated in the system while an electrolyte rich solution is produced for electrolyte make-up.
A tee, designated 28, used in the system pre-treatment section 8 and rinse section 12 is shown in FIGS. 24-26. As previously indicated, the tees are designed to afford countercurrent travel of solution with the fibers 2. In practice, the tees 28 are designed with an upstream opening 210 and a downstream opening 212 for the passage of fibers 2 therethrough. The tees 28 are also provided with a dome housing 214 through which the solution such as rinse water can enter and bathe the fibers 2 as the fibers 2 pass through the tee 28. The tees 28 are also provided with a sleeve 216 that creates a pressure head which directs water in the upstream direction. In addition, the tees are designed with the opening 210 for the passage of fibers 2, at an elevation slightly below the opening 212. Thus, the path by which water escapes from the tee is from the delivery pipe 218 through the opening 210. The combination of the differential elevation in the openings 210 and 212 and the presence of the sleeve 216 located in the downstream section of the tee 28 promotes travel of the solution in a direction upstream as the fibers are moving downstream.
The apparatus of the present invention is arranged for synchronous operation as shown in FIGS. 27-29. A motor 222 is provided to insure that the contact rollers 100 and the guide rollers 51 rotate at the same speed to avoid abrading the fibers 2.
The motor 222 directly drives an assembly of rollers 223 arranged to effect a capstan. The rollers 223 are located in the dryer 14 and as best seen in FIG. 29 cause the fiber to reverse direction six times. The reversal in direction is sufficient to impose a force on the fibers 2 that will pull the fibers through the apparatus without allowing slack.
In addition, the motor 222 is connected by a gear and chain assembly to drive each contact roller 100 and each guide roller 51 at the same speed.
In essence, the gear and chain assembly is comprised of guide drive assemblies 225, best seen in FIG. 28 and contact roller drive assemblies 227. Each guide drive assembly 225 includes drive transmission gear 230 mounted on shafts 231, a gear 224 fixedly secured to the guide roller 51 and a chain 233 that engages the gears 230 and 224.
The contact roller drive assembly includes drive transmission gear 239 mounted on the shafts 231 common to the gears 230, a gear 241 fixedly secured to each contact roller 100 and a chain 243 that engages both gears 239 and each of the gears 241 on the six contact rollers 100 associated with each electrolyte tank.
As seen in FIG. 30 each guide roller 51 is formed with grooves 280 having tapered sides 282 and flat surfaces 284. The diameter of the guide roller at the surface 284 is the same as the diameter of the contact rollers 100 and the capstan rollers 223, thus constant speed is experienced by the fibers 2 along the path through the apparatus.
The flat surfaces 284 afford a means by which the fibers or tows 2 spread to either facilitate drying or wetting depending on the operative effect desired.
The location of the capstan rollers 223 in the dryer 14 enhances drying. The flat surface and force applied to the fibers 2 spreads the fibers and thereby accelerates drying.
The system also includes a variable speed clutch override drive motor 219 for the take-up reels 17. The force generated by the variable torque motor 219 provides the force to draw the fiber 2 through the system. However, the capstan rollers 223 provide a means to isolate the direct force imposed on the fibers 2 at the take-up reels 17 from the fibers 2 upstream of the capstan rollers.
|
A graphite fiber is electroplated by passing the fiber continuously through an electrolyte solution in a tank. Current is delivered to the fiber at a contact immediately prior to the surface of the electrolyte in the tank. The voltage is maintained above 16 volts. The fiber is kept cool enough outside the bath to prevent degradation by recycling the electrolyte to bathe the fiber from the point of contact to the point of immersion into the electrolyte.
| 3
|
BACKGROUND OF THE INVENTION
This invention relates to fluid control valves, and more particularly to such valves that automatically open in response to elevated temperatures.
SUMMARY OF THE INVENTION
The present invention comprises a fluid control valve especially, but not exclusively, useful for protecting cryogenic fluid circuit installations from dangerous temperature increases, the valve comprising a plug-type flow control element that is spring-biased towards its open position yet is held in its closed position during normal operating temperatures by a temperature responsive retention system. The retention system comprises a support plate movably secured to the exterior of the valve's seat body by a plurality of cap screws or the like, a screw-like compression element adjustably threaded through the plate and extending freely through a wall of the valve's seat body into engagement with the flow control element, and a plurality of annular washer-like spacers of fusible material, such as a metal alloy, between the plate and the heads of the cap screws. When the spacers melt, thereby freeing the plate to move toward the cap screw heads, the flow control element moves in response to its bias spring from its closed position to its open position, whereby fluid can then flow through the valve.
The valve is designed so as to be connectible between two pipes or conduits so that when the valve opens communication between the pipes is established. The interior of the valve is sealed from the outer atmosphere at all times, regardless of the position of the flow control element or of the temperature to which the valve is subjected, so that there is never any loss of pressure to the outside.
The choice of a specific metal alloy or other fusible material employed for the spacers depends on the temperature at which the valve is desired to open, and such material may be modified to provide different melting points and thus permit different utilizations (for example, successive openings of a plurality of valves as the temperature increases).
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a vertical central section through a valve embodying the features of the present invention, showing the flow control element in its closed position and the valve interconnecting two pipes.
FIG. 2 is a view like FIG. 1, showing an alternate form of the valve.
FIG. 3 is an enlarged fragmentary view of the flow control element, compression element, valve body and compression element seal of the valve of FIG. 2.
FIG. 4 is a schematic illustration of a fluid circuit installation including three valves according to the present invention.
FIG. 5 is an enlarged fragmentary view of a portion of the schematic of FIG. 4.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In reference first to FIG. 1, a valve 10 in accordance with the present invention broadly comprises an inlet-outlet body 12 with inlet and outlet ports 14, 16 respectively, a seat body 18 threaded at 20 to the body 12, a plug-type flow control element 22 within a chamber 24 between the body 12 and the body 18, a helical or coil spring 26 in a chamber 28 in the body 12 that biases the flow control element 22 towards its open position (not shown), and a temperature responsive flow control element retention system comprising a support plate 30 movably secured to the exterior of the seat body 18 by a plurality (preferrably three or more) of circumferentially spaced cap screws 32 (only one shown), a plurality of annular washer-like spacers 34 (only one shown) between the heads 32a of the cap screws and the support plate 30, a screw-like compression element 36 threaded through the support plate 30 and freely extending through a bore 37 in the seat body 18 into the chamber 24 and into engagement with the flow control element 22, and a lock nut 38 for securing the compression element 36 in proper position. Between the body 12 and the body 18 is an annular fluid gasket or seal 40, and another annular gasket or seal 42 functions as a fluid barrier between the body 18 and the support plate 30 when the spacers 34 are intact as shown.
At the opening of the chamber 28 into the chamber 24 is an annular lip 44 against which the flow control element 22 rests when in its illustrated "closed" position, and the compression element 36 functions to establish and maintain fluid-tight contact between the element 22 and the lip 44, thereby preventing flow of fluid through the valve between an inlet pipe A and an outlet pipe B. A similar annular lip 46 at the opening of the bore 37 into the chamber 24 provides a stop against which the flow control element 22 rests in its "open" position (not shown), and in that position the spring 26 presses against the element 22 with sufficient force to assure fluid-tight contact between that element and the lip 46.
The valve 10 preferably is disposed vertically as illustrated, with the support plate 30 below the seat body 18, whereby gravity assists the spring 26 in urging the flow control element 22 toward the lip 46.
Since the valve 10 is intended to remain in its illustrated closed condition, thereby preventing flow from the pipe A to the pipe B, until the ambient temperature rises to a dangerous level, the choice of the composition of the fusible spacers 34 depends upon what that temperature level is for the particular installation and upon the melting point of the composition. Accordingly, the valve 10 can be tailored to suit a wide variety of uses by merely selecting the appropriate fusible composition for the spacers 34.
As should be apparent from the foregoing, so long as the fusible spacers 34 are intact the compression element 36 exerts a force upon the flow control element 22 greater than that of the spring 26, thereby holding the element 22 against the annular lip 44, i.e. in the element's "closed" position. When the spacers 34 melt in response to sufficient temperature elevation their holding function with respect to the support plate 30 is destroyed, and the spring 26 urges the flow control element 22 into its "open" position (not shown) against the annular lip 46. During this movement the compression element 36 and the support plate 30 are forced to move in the same direction until the plate comes to rest against the cap screw heads 32a.
In the alternate embodiment of the valve 10 shown in FIG. 2, an annular seal 48 is positioned in an annular groove 50 in the bore 37 to establish a fluid barrier between the bore and a smooth cylindrical surface 36a on the adjacent portion of the compression element 36.
FIG. 4 illustrates an example of a safety circuit installation using one or more valves V1, V2, V3, each being of the type described above and shown in FIGS. 1-3, that open the circuit automatically and controllably by melting of their spacers in accordance with the present invention. In this example the valves V1, V2, V3 provide protection to a container 50 provided with a diaphragm valve 52, the valve 52 having a diaphragm 54 and a main pilot 56 that operates in response to an internal pressure force in the direction of the arrow F1. An external pressure force, represented by the arrow F2, also may be provided if desired. The pilot 56 is set to a pressure P0.
Communicating with the upper chamber 52a of the valve 52 is the outlet 58a of a safety pilot valve 58. As seen in FIG. 4, the outlet pipe B of the valve V1 is connected to the inlet of the pilot valve 58. This permits the valve 52 to vent for a setting P1 lower than P0, as when the temperature increases abnormally. A major portion of the container 50 therefore can be evacuated through the diaphragm valve 52 since that valve 52 opens before an elevated temperature has had enough time to render the installation dangerous.
As shown in FIG. 4, the inlets A of the valves V1, V2, and V3 can be connected to the container 52, in which case the setting P1 must be lower than the pressure in the container 52. It is also possible to supply the inlets A from a subsidiary air or nitrogen network if the network has an available pressure higher than P1, either constant so that the container 52 is completely evacuated or becoming less than P1 when the protection system has opened, the valve 52 thereafter closing and the pressure in the container 52 stabilizing at P1 as in the case when the supply to the inlets A is provided from the container.
The valves V1, V2 and V3 can be connected in parallel as shown in FIG. 4, thereby to protect several zones surrounding the container 52. In such an installation, the sensing of a dangerously elevated temperature in any one of the zones causes the related valve V1, V2 or V3 to open. The valves V1, V2 and V3 also can be connected in series (not shown) if desired in which case as the temperature increases the valves open sequentially until the safety pilot valve 58 is actuated.
If desired, a vent setting means 60 may be provided at the outlet of the safety valve 58 to facilitate adjustment of the main vent of the diaphragm valve 52. Such a setting means can comprise a needle valve as shown in FIG. 5, having a needle 62 axially adjustable with respect to a seat 64 in a valve body 66. Also, depending upon the type of safety valve 58, a closure plug 68 (FIG. 5) can be provided at a point in the fluid circuit of the valve 58 to prevent the supply fluid from flowing under the pilot diaphragm.
Although the best mode contemplated for carrying out the present invention has been herein shown and described, it will be apparent that modification and variation may be made without departing from what is regarded to be the subject matter of the invention.
|
A fluid control valve for protecting a cryogenic fluid circuit comprising a spring biased plug-type control element that is held closed by a spacer meltalile in the presence of fire.
| 8
|
CROSS REFERENCES TO CO-PENDING APPLICATIONS
None.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is for a leak-proof lead barrier system for use with metal stud framed walls typically installed in X-ray rooms and other areas where radiation protection is needed. The leak-proof lead barrier system utilizes a lead barrier plate secured to the interior of a metal stud before lead-backed gypsum board is installed. The leak-proof lead barrier system can also be adapted for use with header and footer plates.
2. Description of the Prior Art
The current method for creating a leak-proof lead barrier to be used with metal studs and lead laminated gypsum board requires the installer to countersink all the drywall screws into the lead laminated gypsum board when securing the lead laminated gypsum board to metal studs. Once the screws are countersunk, lead screw caps slightly larger than the screw heads are positioned over each and every drywall screw and also countersunk before the seams are taped and finished. In addition to the lead screw caps, a thin strip of sheet lead needs to be installed between the lead portion of the gypsum board and the metal stud where two or more sheets of the lead laminated gypsum board are butted together to prevent leakage at the seam.
The current method requires extensive, time-consuming labor to install, especially at the joints where two or more sheets of lead laminated gypsum board meet. In addition to the time and labor drawbacks, the integrity of the gypsum in the lead laminated gypsum board is compromised due to countersinking the screws and the use of lead screw caps, which causes the gypsum to crack and crumble.
The present invention addresses and corrects all of the previously mentioned shortcomings and will be described in detail in the preferred embodiment.
SUMMARY OF THE INVENTION
The general purpose of the present invention is to provide a leak-proof lead barrier system to be used in conjunction with lead laminated gypsum board.
According to one embodiment of the present invention, there is provided a lead barrier plate, including a mounting portion and a barrier portion, which is appropriately secured to the interior of a metal stud prior to installing lead laminated gypsum board. This lead barrier plate provides a lead barrier where holes are created in the lead backing of the lead laminated gypsum board when it is screwed onto the metal studs and where two or more sheets of the lead laminated gypsum board meet, eliminating the need for lead screw caps and strips of sheet lead at seams.
One significant aspect and feature of the present invention is an angled lead barrier plate which mounts to the interior of a metal stud.
Another significant aspect and feature of the present invention is one-step installation of the leak-proof lead barrier plate.
Still another significant aspect and feature of the present invention is elimination of lead screw caps which compromise the integrity of the gypsum board.
Yet another significant aspect and feature of the present invention is elimination of lead sheet metal applied to the interior seam of two or more lead laminated gypsum boards.
A further significant aspect and feature of the present invention is that thickness of the lead barrier plate may be changed to accommodate the needs of the user without affecting form or function.
Having thus enumerated significant aspects and features of the present invention, it is the principal object of the present invention to provide a leak-proof lead barrier system to be used with lead laminated gypsum board and metal studs.
One object of the present invention is to provide a leak-proof lead barrier system which can be installed in one step.
Another object of the present invention is to provide a leak-proof lead barrier system which does not require lead screw caps.
Yet another object of the present invention is to provide a leak-proof lead barrier system which does not require additional lead sheeting where two or more lead laminated gypsum boards meet.
Still another object of the present invention is to provide a means of creating a leak-proof lead barrier system which will not compromise the integrity of the lead laminated gypsum board.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects of the present invention 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 when considered in connection with the accompanying drawings, in which like reference numerals designate like parts throughout the figures thereof and wherein:
FIG. 1 illustrates an isometric view of a leak-proof lead barrier system, the present invention;
FIG. 2 illustrates a top cross-sectional view of the leak-proof lead barrier system; and,
FIG. 3 illustrates a top cross-sectional view of the prior art method of creating a leak-proof lead barrier system.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 illustrates an isometric view of a leak-proof lead barrier system 10 , the present invention. The leak-proof lead barrier system 10 is created by vertically aligning and securing an angled lead barrier plate 12 , having a mounting portion 16 and a barrier portion 14 , to the interior of the central planar portion 18 of a metal stud 20 . The lead barrier plate 12 is secured to the metal stud 20 by a plurality of sheet metal screws 30 a - 30 n which pass through the mounting portion 16 of the lead barrier plate 12 and into the central planar portion 18 of the metal stud 20 . It is to be understood that other appropriate means of securement may be used such as, but not limited to, welding, extrusion or metal adhesive. In the illustrated case, the number of sheet metal screws 30 a - 30 n is dependent on the height of the metal stud 20 . Each metal stud 20 has a front planar portion 22 and a rear planar portion 24 which extend outwardly from central planar portion 18 , and flanges 26 and 28 extend inwardly from the front planar portion 22 and rear planar portion 24 , as illustrated.
The purpose and use of the leak-proof lead barrier system 10 will become visibly apparent when lead laminated gypsum boards are secured to either the front planar portion 22 (FIG. 2 ), the rear planar portion 24 (not illustrated) or both planar portions 22 and 24 (not illustrated) of the metal stud 20 .
FIG. 2 illustrates a top cross-sectional view of the leak-proof lead barrier system 10 . The lead barrier plate 12 is mounted to the metal stud 20 as described in FIG. 1 . Illustrated in particular are two lead laminated gypsum boards 32 a and 32 b , each having a lead portion 34 a and 34 b , respectively, and oriented in abutting fashion. The juncture where the lead laminated gypsum boards 32 a and 32 b meet is centrally aligned along the front planar portion 22 of the metal stud 20 where a plurality of drywall screws 36 a - 36 n secure the lead laminated gypsum boards 32 a and 32 b to the metal stud 20 . Once again, the number of drywall screws 36 a - 36 n needed is dependent on the height of the lead laminated gypsum boards 32 a and 32 b and metal stud 20 .
Once the lead laminated gypsum boards 32 a and 32 b are appropriately secured to the front planar portion 22 of metal stud 20 , it becomes apparent that holes 38 a - 38 n are created in the lead portions 34 a and 34 b of the lead laminated gypsum boards 32 a and 32 b , creating leaks. Due to the fact that gamma rays, including X-rays, only travel in a straight line, the barrier portion 14 of the lead barrier plate 12 extends beyond flanges 26 and 28 , the holes 38 a - 38 n , and the juncture where lead laminated gypsum boards 32 a and 32 b abut. Thus, a leak-proof lead barrier system 10 is created without lead screw caps being installed over each screw or a narrow strip of sheet lead being installed at the seams, as shown in the prior art illustration of FIG. 3 .
FIG. 3 illustrates a top cross-sectional view of the prior art method of creating a leak-proof lead barrier system 100 , having lead laminated gypsum boards 104 a and 104 b , each having a lead portion 105 a and 105 b , a metal stud 106 , and drywall screws 118 a - 118 n identical to those previously described. The metal stud 106 is comprised of a central planar portion 108 , a front planar portion 110 , a rear planar portion 112 and two flanges 114 and 116 . Illustrated in particular is a sheet lead strip 102 which is positioned between lead portions 105 a and 105 b of the lead laminated gypsum boards 104 a and 104 b and metal stud 106 and secured in place by drywall screws 118 a - 118 n which are countersunk into lead laminated gypsum boards 104 a and 104 b . The sheet lead strip 102 provides leak protection where lead laminated gypsum boards 104 a and 104 b abut, and lead screw caps 120 a - 120 n are installed over each drywall screw 118 a - 118 n and countersunk to provide leak protection for the holes created by the drywall screws 118 a - 118 n . By countersinking both the drywall screws 118 a - 118 n and the lead screw caps 120 a - 120 n , the gypsum layers of the lead laminated gypsum boards 104 a and 104 b typically crack and crumble, compromising the integrity of the entire sheets.
The present invention provides an easy one-step application which is less labor intensive, less time consuming and does not compromise the integrity of the gypsum in the lead laminated gypsum boards.
Various modifications can be made to the present invention without departing from the apparent scope hereof.
LEAK-PROOF LEAD BARRIER SYSTEM
PARTS LIST
10
leak-proof lead
barrier system
12
lead barrier
plate
14
barrier portion
16
mounting portion
18
central planar
portion
20
metal stud
22
front planar
portion
24
rear planar
portion
26
flange
28
flange
30a-n
sheet metal
screws
32a-b
lead laminated
gypsum boards
34a-b
lead portions
36a-n
drywall screws
38a-n
holes
100
leak-proof lead
barrier system
102
sheet lead strip
104a-b
lead laminated
gypsum boards
105a-b
lead portions
106
metal stud
108
central planar
portion
110
front planar
portion
112
rear planar
portion
114
flange
116
flange
118a-n
drywall screws
120a-n
lead screw caps
|
A leak-proof lead barrier system to be installed on the interior of metal studs, to be used in conjunction with lead laminated gypsum board. The leak-proof lead barrier system provides an easier and less time-consuming method of sealing a radiation protective room in one step.
| 4
|
This is a divisional of application Ser. No. 172,038 filed Mar. 23, 1988, issued as a U.S. Pat. No. 4,934,425 June 19, 1990.
BACKGROUND OF THE INVENTION
This invention relates to non-pneumatic tires having angularly oriented ribbed members and webs between ribs composed of resilient polyether urethane elastomeric materials. In particular, a urethane made of polyether polyols having two distinctly different molecular weights are used to make the urethane elastomer.
Urethanes have been used in the manufacture of solid tires useful for such applications as industrial tires, off-the-road tires, bicycles tires and the like. They have not been entirely satisfactory in such applications because such urethane solid tires do not have the proper cushioning and handling characteristics for a soft vehicle ride on such applications as passenger vehicles. Also, such solid tires suffer from internal heat build-up and subsequent degradation of the elastomer material in prolonged high speed service conditions or under rough terrain situations where the tire is being deformed.
Various polyurethane elastomers have been proposed for use on such solid tires, including those described in U.S. Pat. No. 3,798,200 and U.S. Pat. No. 3,963,681 both to Kaneko et al. In these two pieces of prior art it is proposed that polyether urethane elastomers can be utilized which are prepared from two prepolymers having differing molecular weights. In U.S. Pat. No. 3,963,681 it is disclosed that by using a flex life test such De Mattia it is determined that the preferred urethane elastomer is one prepared using a polyfunctional isocyanate and a polyether prepared using prepolymers having different average molecular weights. It is further disclosed that for polytetramethylene ether glycol the critical molecular weight is 4,500. One of the two polyethers used to make the invention must have a molecular weight above the 4,500 critical molecular weight and the other must be below this critical molecular weight in order to achieve the improved De Mattia flex life. U.S. Pat. No. 3,798,200 discloses a 4,000 critical molecular weight for polytetramethylene glycol ethers utilized in the urethane teaches that the average weight of the two polyethers must lie between 4,500 and 20,000 weight average molecular weight. It further teaches that one of the polyethers must lie below the critical molecular weight of 4,500 and the other be above such a critical molecular weight. In comparative Example 9, a composition outside of the invention of the reference is described in which a 1,900 molecular weight polyether and an 850 molecular weight is blended 50:50, reacted with 2 mols of 2,4 tolylene diisocyanate and subsequently cured with methylene bis ortho-chloroaniline. Such a composition was found to have poor cut growth and flex crack resistance as measured by De Mattia flex testing.
Contrary to the teachings of U.S. Pat. No. 3,798,200, it has been quite unexpectedly found that a non-pneumatic tire utilizing a rib-and-web structure of this invention yields a non-pneumatic tire which can favorably compare with pneumatic tires for service life under both high speed, long duration test conditions and under very rough road conditions while still giving good ride and handling characteristics similar to a pneumatic tire. Such a device of the invention is superior to a pneumatic tire in that it cannot be punctured or damaged in the way a pneumatic can.
The non-pneumatic tire concept set forward in European patent publication number 159,888 which claimed convention priority from U.S. application Ser. No. 600,932 filed Apr. 16, 1984, introduced a configuration of tire which utilized an entirely new design approach to a high speed non-pneumatic tire having suitable ride characteristics for passenger tires. This design features the ability of the ribs and webs to provide a variable spring rate in the tires and enables it to deform locally when an obstacle is encountered on a rough road driving condition. These requirements are in addition to the common requirements which were encountered in previous generations of solid tires that the internal heat build-up be kept to a minimum and the flex life of the tire be long.
In view of the unique requirements of structure as a object of the invention to provide a urethane material which can endure both long duration, high speed conditions as well as the ability to locally deflect in rough terrain service. It is a further object to provide a non-pneumatic tire having good vehicle ride characteristics under a variety of road conditions. In order to achieve such results, it is necessary to recognize that dynamic modulus of the material is critically important as well as flex fatigue life and dynamic heat build-up properties (hysteresis). The recognition of the criticality of utilizing a urethane with two distinct molecular weight glycols with an organic diamine curative provided the balance in properties required for good vehicle ride characteristics as well as long life.
BRIEF DESCRIPTION OF THE INVENTION
In accordance with one embodiment of the invention there is provided: a non-pneumatic tire rotatable about an axis, having improved hysteresis and flex fatigue resistance comprising: an annular body of resilient polyether urethane elastomeric material formed of a first isocyanate end capped low molecular weight polyether polyol having a molecular weight of between 200 and 1,500 and a second high molecular weight isocyanate end capped polyether polyol having a molecular weight between 1,500 and 4,000 cured with an aromatic diamine curative, said annular body having a generally cylindrical outer member at the outer periphery thereof, a generally cylindrical inner member spaced radially inward from and coaxial with said outer member, a plurality of axially extending, circumferentially spaced-apart rib members connected at their corresponding inner and outer ends to said inner and outer cylindrical members, said rib members being generally inclined at an angle of about 0° to 75° to radial planes which intersect them at their inner ends, and at least one web member having opposite side faces, said web member having its inner and outer peripheries connected respectively to said inner and outer cylindrical members, said web member being connected on at least one of its side faces to at least one of said rib members to thereby form with said rib member a load-carrying structure for said outer cylindrical member, said load carrying structure being constructed to permit locally loaded members to buckle.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a side elevation view of a non-pneumatic tire and rim assembly embodying the invention;
FIG. 2 is an enlarged fragmentary view of a portion of the tire and rim assembly shown in FIG. 1, showing the intermediate load-carrying and cushioning structure thereof in greater detail: and
FIG. 3 is a sectional elevation view, taken along the line 3--3 of FIG. 2, showing one single-web member version of this invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIGS. 1, 2 and 3 wherein a preferred embodiment of this invention is illustrated, a tire 10 is shown mounted on a wheel 12 for rotation about an axis 15. The tire 10 comprises an annular body 16 of resilient elastomeric material having an outer cylindrical member 18 at the outer periphery thereof on which a tread 20 may be mounted. The annular body 16 is also provided with an inner cylindrical member 22 at its inner periphery which is adhered to or otherwise fastened to an outer cylindrical surface 24 of wheel rim member 12. Inner cylindrical member 22 is of the same length as, coaxial to, and coextensive with outer cylindrical member 18.
The outer cylindrical member 18 is supported and cushioned by a plurality of circumferentially spaced-apart rib members 26, each of which includes a first axial portion 28 (FIG. 3) and a second axial portion 30, and by a web member 32, which in this embodiment of the invention is planar and is connected on one of its side faces 32a to the first portion 28 of rib members 26 and is connected on its other side face 32b to the second portion 30 of rib members 26.
The planar web member 32 is positioned midway between the axial ends of the inner and outer cylindrical members 18 and 22. It is connected at its inner periphery 32c to the inner cylindrical member 22 and is connected at its outer periphery 32d to the outer cylindrical member 18. Similarly, the various rib members 26 (FIG. 2) are connected at their radially inner ends to the inner cylindrical member 22 and at their radially outer ends to the outer cylindrical member 18. The ribs 26 are preferably undercut where their ends connect to the inner and outer cylindrical members, as shown at 34, to enhance flexibility of the connection.
The rib members 26 extend generally axially along the inner and outer cylindrical members 22 and 18 (Fig. 3) and, in the preferred embodiment as shown in FIG. 1 are inclined at an angle A (FIG. 1) of 15° to 75° to radial planes R which intersect them at their functions with the inner cylindrical member 22. In an alternate embodiment (not shown), the rib members 26 can be extended radially with no angle A or with a lesser angle of between 0° and 15° . The web member 32 (FIG. 3) in this embodiment lies in a plane that is perpendicular to the rotational axis 14 of the tire 10.
In the preferred embodiment shown in FIGS. 1 to 3, the first axial rib member portions 28 and the second axial rib member portions 30 are each inclined at the same angle to the radial planes R which intersect them at their radially inner ends but the angles of the first portions 28 are preferably oppositely directed with respect to the radial planes R from the angles of the second portions 30. Thus, as viewed in FIG. 3, the first rib portion proceeds upwardly from the section lines to connect with the outer cylindrical member 18, while the second rib portion 30 proceeds downwardly from the section lines to connect with the inner cylindrical member 22.
In FIGS. 1-3, "r o " is the outer radius of the annular body 16, "A" is the inclination angle that the rib members 26 make with the radial planes R, "d i " is the radial thickness of the inner cylindrical member 22, "d o " is the radial thickness of the outer cylindrical member 18, "L" is the angularly directed length of the rib members 26, "D" is the radial distance from the outer surface of the inner cylindrical member 22 to the inner surface of the outer cylindrical member 18, "d w " is the axial thickness of the web member 32, "d s " is the thickness of the rib member 26 measured perpendicularly to its length L, "t i " is the axial length of the inner cylindrical member 22, "t o " is the axial length of the outer cylindrical member 28, and "t i " is the radial dimension of the inner surface of the inner cylindrical member 22.
In a tire of the type shown in FIGS. 1-3, the rib members 26 are constrained to deform primarily in compression by the influence of the web member 32, which may be cast as an integral part of the structure. The web member 32 tends to prevent the rib members 26 from deforming in bending, and the effect is to greatly increase structural stiffness. In addition, the rib members 26 tend to prevent the web member 32 from buckling in the axial direction so the rib members and web member work together synergistically to carry tire loads.
Another desirable characteristic of a non-pneumatic tire or any tire is an overall spring rate that changes depending on the type of surface against which the tire is loaded. Specifically, it is desirable that the spring rate be lower over a bump or cleat than over a flat surface.
The annular body 16 may be adhered to the surface 24 of wheel rim 12 by being molded directly thereto in a liquid injection molding process, with the outer cylindrical surface 24 of the rim having been prepared in accordance with known processes to adheringly receive the elastomeric material of the body 16. Preferably, the wheel rim 12 is provided with radial flanges 36 and 38 which cooperate with the mold in forming the annular body 16 on the wheel rim surface 24.
Method of Manufacture
The tire can be conveniently made in a mold having an inner cavity of complementary shape to the tire 10 shown in FIGS. 1-3. The mold may have an inner mold ring substituted in place of the wheel rim 12. The mold is filled with a reaction mixture of the preferred components of the invention.
The reaction mixture is added to the mold under sufficient pressure to insure that all air in the mold is displaced by liquid reaction mixture. It has been found that pressure in the area of 450 kPa is a suitable pressure. Once the mold is filled it is heated for about one hour for the purpose of curing the liquid reactants. Subsequently, the mold is opened and the annular body 16 is demolded and post-cured for a suitable number of hours.
A simple tire tread composed of tough abrasion-resistant elastomer such as conventional tire treads are manufactured from is applied to the outer cylindrical member 18. The tread has a minimal thickness to assure little heat build-up during flexing. A thickness of about 0.6 cm has been found suitable. The tread may be adhered by conventional and well-known adhesives which vary depending on the composition of the tread. If an inner mold ring has been substituted for the wheel rim 12, the rim 12 must be adhered by suitable adhesives to the inner surface of the annular body 16. The resulting assembly can be used to replace a conventional passenger car tire and wheel assembly. A car with the tire and wheel assembly can be driven without deleteriously affecting control of the car without damage to the non-pneumatic tire of the invention.
Urethane Elastomer of the Invention
The invention resides in the specific selection of a polyether polyol prepolymer for the urethane elastomer which has at least two distinct molecular weight polyols included in the prepolymer system.
The polyether used in this invention is the polyether having a terminal functional group containing active hydrogen capable of reacting with an isocyanate group. The functional group is selected from the group consisting of hydroxyl group, mercapto group, amino group and carboxyl group.
Moreover, a pre-extended polymer obtained by reaction between a low molecular weight polymer and a diisocyanate or a product obtained by reaction between prepolymer and diol compound may be used in this invention.
Polyethers used in this invention are alkylene glycol such as polyethylene glycol, polypropylene glycol, polytetramethylene ether glycol and the like, polyalkylene triol such as polypropylene triol and the like, polyalkylene dicarboxylic acid, polyalkylene dithiol, polyalkylene diamine and their pre-extended polymer, and preferably polyalkylene glycol, and more preferably polytetramethylene ether glycol and its pre-extended polymer.
In this invention, a mixture of two or more different kinds of polyethers having molecular weights which are different from each other must be used. In this case, it is essential that at least one peak is located at the lower molecular weight region (200-1,500) and at least one peak is located at the higher molecular weight region (1,500-4,000).
Polytetramethylene ether glycol (PTMEG) is the most preferred polyol of the invention. A first low molecular weight polyether glycol is utilized having a molecular weight of between 200 and 1,500. The essential second higher molecular weight polyether glycol has a molecular weight between 1,500 and 4,000. A more preferred range for the low molecular weight material is between 250 and slightly above 1,000. For the higher molecular weight second glycol, it is just below 2,000 to about 3,000. The most preferred range is is a low molecular weight glycol of about 1,000 molecular weight and a higher molecular weight glycol of about 2,000. The first and second polyether polyols may be blended in molar ratios of between 95:5 to 50:50 where the first number in the ratio is always the low molecular weight polyol. More preferred range is 90:10 to 60:40. The most preferred range is 85:15 to 80:20.
The prepolymer for use in the tire of the invention is formed by reacting the first and second polyether polyols set forth above with a multifunctional isocyanate. The more preferred are the toluene diisocyanates. The two most preferred materials are 100% 2,4 toluene diisocyanate and the 80/20 blend of the 2,4 and 2,6 toluene diisocyanate isomers. The ratio of TDI to polyol is commonly expressed in the art as NCO:OH ratio. The isocyanate to polyol ratio may be in the range of 1.7:1.0 to 2.3:1.0. A more preferred range of ratios is 1.85:1.0 to 2.2:1.0. The most preferred range of ratios is 1.95:1.0 to 2.15:1.0. The percentage of free NCO in the resulting prepolymer is also in common use for characterizing prepolymers.
Polyfunctional isocyanates used in this invention are not particularly limited, but are preferably aromatic and aliphatic diisocyanates and triisocyanates. Aromatic diisocyanates are, for example:
tolylene-2,4-diisocyanate;
tolylene-2,6-diisocyanate;
naphthalene-1,5-diisocyanate;
diphenyl-4,4'-diisocyanate:
diphenylmethane-4,4'-diisocyanate;
dibenzyl-4,4'-diisocyanate:
stilbene-4,4'-diisocyanate:
benzophenone-4,4'-diisocyanate;
and their derivatives substituted with alkyl alkoxy, halogen or nitro groups, e.g., 3,3'-dimethylphenyl-4,4'diisocyanate or 3,3'-dichlorodiphenylmethane diisocyanate, their mixtures and the like, aliphatic diisocyanates, and tricyanates. Among them, there may be preferably used:
tolylene-2,4-diisocyanate;
tolylene-2,6-diisocyanate;
naphthalene-1,5-diisocyanate;
diphenyl-4,4'-diisocyanate;
diphenylmethane-4,4'-diisocyanate;
1,6-hexamethylene diisocyanate;
1,3 and 1,4-cyclohexyl diisocyanate;
methylene bis(4-cyclohexyl diisocyanate);
1,3- and 1,4-xylene diisocyanate and their mixtures.
The curing agents in this invention may be aromatic or aliphatic polyamines or polyols. Aromatic diamines are, for example, 4,4'methylene bis(2-chloroaniline), 2,2',5-trichloro-4,4'-methylenediamines, napthalene-1,5-diamine, ortho, meta, paraphenylenediamine, tolylene-2,4-diamine, dichlorobenzidine, diphenylether-4,4'-diamine, their derivatives and mixtures.
Among them there are preferably employed 4,4'methylene bis 2-chloroaniline, methylene dianiline, trimethyl bis(p-amino benzoate), bis amino phenylthioethane, napthalene-1,5-diamine, dichlorobenzidine, diphenylether, 4,4'-diamine, hydrazine, ethylenediamine, hexamethylene-1,6-diamine, piperazine, ethylene glycol, 1,3-propylene glycol, 1,3 and 1,4-butane diol, trimethylpropane and their mixtures.
The final urethane elastomer is cured using aromatic organic diamines which are well-known and commercially available. The more preferred material is 4,4'-methylene bis(2-chloroaniline) which will periodically be referred to as MBOCA. Also preferred is the diethyl toluene diamine (DETDA) which is available commercially from Ethyl Corporation under the trade name Ethacure 100. A suitable material which has a different cure rate is methylenedianiline-NaCl complex, commercially available from Uniroyal Chemical Company, Inc. as Caytur. The most preferred curative is 4,4'-methylene bis(2-chloroaniline).
The stoichiometry of the prepolymer to curative is expressed on a molar equivalence basis, hereinafter called equivalence ratio, rather than on a weight basis. The broadest equivalence ratio of prepolymer to curative is about 80 to about 115. More preferred is 90 to 110 and most preferred is 100 to 105. The equivalence ratio is also commonly called--percent of theory--or simply stoichiometry.
It has been found through a long process of experimentation that several dynamic properties of elastomers must be carefully evaluated together in order to produce an elastomer suitable for the annular elastomeric body of the tire of this invention. A measure of dynamic modulus must reveal that the chosen elastomeric material has a relatively constant dynamic modulus over a wide temperature range. The tendency of the elastomer to build up internal heat due to elastic inefficiency is commonly called hysteresis in the industry. The hysteresis is commonly expressed in terms of a value obtained from a hysteresis-type test which is commonly described as tangent delta or, more commonly, tan δ. The tan δ should show a decrease with a rise in temperature, indicating little internal heat build-up is occurring in the elastomeric body of article being tested.
The flex fatigue test helps measure the ability of the elastomer to withstand the millions of cycles to which a non-pneumatic tire may be subjected. The test which has been found to correlate favorably with actual test tires is the cut growth resistance as run in accordance with ASTM D-3629-78. Test conditions are: temperature 70° C., atmosphere is air, rate of rotation is 500 rpm and elongation is 23% . The device utilized is the TEXUS® Flex tester available from Testing Machines, Inc., New York, Model No. 31-11.
Dynamic measurements to determine a tan δ value are useful to assure that a suitably low hysteresis value is obtained for the material. Several hysteresis devices are useful including the Rheovibran Tester, Hysterometer, and the Rheometrics Viscoelastic Tester for Solids, Model RVE-S, made by Rheometrics, Inc., New Jersey. These instruments impose a sinusoidal shear strain to the specimen, and analyze the torque responses and phase relation to the strain.
The ultimate test of the suitability of an elastomer for use in a high speed tire is its ability to resist heat build-up and degradation at prolonged high speed service. United States Department of Transportation has developed a test designated MVSS 109 high speed test procedure S5.5 in which the test wheel and tire is run on a dynamometer at carefully prescribed strain loads, dynamometer speeds and time periods. This test is designed for a pneumatic tire. The following is a simplified indication of the test regimen, specific details can be obtained by review of MVSS 109. Load (NPS) 92% of maximum rated load in a 40° C. elevated temperature environment. Table I shows the speed intervals at which the tires described in the examples were run. The MVSS 109 test reviewed call for test termination after 31/2 hours (top speed 85 mph). However, in order to induce failure in the test tires, the test was continued as noted in Table I with incremental speed increases until the tires failed.
TABLE I______________________________________MVSS 109 Test Method MVSS 109 Test Conditions Speed Internal Cummulative (MPH) (Hours) (Hours)______________________________________Load (NPS) 50 2 20.92 max load 75 1/2 21/2 80 1/2 3 85 1/2 31/2* 90 1/2 4 95 1/2 41/2 100 1/2 5 105 1/2 51/2 110 1/2 6 115 1/2 61/2 120 1/2 7 125** 1/2 71/2______________________________________ *MVSS 109 is stopped after 31/2hours @ 85 mph. **125 mph maintained for any additional time periods.
In order to determine the ultimate capability of a tire to withstand highway conditions, this test was run beyond its normal termination time of 31/2 hours to distinguish between materials used in the manufacture of the tire. Therefore, the life of the tire in hours may exceed the 31/2 hour test specified in the Test Method.
SAMPLE AND TIRE PREPARATION PROCEDURE
Comparative A-C and Examples 1,2
The polyether urethane compositions of Comparative A, B, and C., were prepared by reacting a polytetramethylene ether glycol (nominal number average molecular weight of 1,000) with toluene diisocyanate in ratios sufficient to produce a prepolymer having the NCO/OH ratio shown in Table II.
The prepolymers were then reacted with the designated diamine curative in the indicated ratios. It is conventional and well-known that the curative and prepolymer may have to be preheated to facilitate handling of the materials. If a small sample is being prepared for physical testing, the mixing is done batchwise in appropriate quantities. If the tire of FIGS. 1-3 is being produced, the curative and prepolymer are pumped continuously into a mixing head which injects the reaction mixture into a mold as earlier described under the subsection Methods of Manufacture.
Example 1 of the invention was prepared by sequentially reacting each polytetramethylene ether glycol with sufficient quantities of 80/20 2,4/2,6 TDI to form two distinct prepolymers which were then mixed in the indicated molar ratio with the MBOCA curative as previously described.
Example 2 illustrates the most preferred method of manufacturing the tire of the invention. The 1,000 and 2,000 molecular weight PTMEG polyols are preblended prior to forming the prepolymer with TDI. The prepolymer is then reacted with the MBOCA curative to form the tire. This preblending of the polyols produces optimal properties in the tire as measured by TEXUS®Flex as shown in Table II under Test Results.
TABLE II__________________________________________________________________________ Examples 1 2 Comparatives Blended Preblended A B C Prepolymers PTMEG__________________________________________________________________________Prepolymer CompositionPTMEG 100 100 100 85 85(1000 molecular wt.)PTMEG 15 15(2000 molecular wt.)2,4 toluene diisocyanate X X2,4-2,6 toluene diiso- X X Xcyanate (80/20 blend)NCO/OH Ratio 2:1 2:1 2:1 2.15:1 2.15:1% NCO 5.0 6.3 6.3 6.3 6.3Curative4,4-methylene bis(2- X X X X Xchloroaniline)Equivalence Ratio 100 100 100 100 100Physical PropertiesHardness (Shore A 92 96 95 95 95durometer)Tensile, psi 5800 4700 6500 4730 4600Elongation, % 420 410 380 390 410Modulus, psi100% 1400 1640 1800 1810 1730200% -- 2070 -- 2260 2120300% 2600 -- 4300 3130 2750*Dynamic PropertiesFlex fatigue, cycles 3200 5000 2750 11250 13500(TEXUS ® Flex 70° C. @23% elongation)Tire Life, Hours 2.0 4.25 3.28 5.50 --(MVSS 109 - mph (50 mph) (90 mph) (80 mph) (105 mph) --at failure)__________________________________________________________________________ *Dynamic properties values are average of following number of samples: A--average of 3; B--average of 2; C average of 5; Example 1--average of 2 Example 2--single value.
The dynamic properties of Examples 1 and 2 illustrate the dramatic advancement achieved by using blended PTMEG prepolymers of different molecular weight to produce the non-pneumatic tire of FIGS. 1-3. The flex fatigue life of Example 1 is 135% better than the best of the Comparative Examples-(B). The life of the tire of Example 1 is dramatically better, both in duration and the ultimate speed capabilities. Example 1 lasted for 5.5 hours with the tire achieving a speed of 105 mph in the final 30 minutes, as shown in Table I. By contrast, the best of the Comparative (B) failed at 4.25 hours at 90 mph. U.S. Pat. Nos. 3,798,200 and 3,963,681 to Kaneko utilized similar polyether urethane chemistry to yield the conclusion that the average molecular weight of a mixture of polyethers must fall in the range of 4,500 to 20,000 average molecular weight or 1,000 to 4,500 with the requirement that the molecular weight of one polyether be less than 4,500 and another must be above 4,500. The specific molecular weight ranges were selected based on cut growth and flex crack resistance as measured according to De Mattia fatigue tester. Surprisingly, our invention relates to an appreciation that excellent tensile strength and, more importantly, superior high speed tire performance in actual road condition results from utilizing two distinct molecular weight polyethers in the ranges of 200 to 1,500 and 1,500 to 4,000. Comparative Examples 9 and 10 in U.S. Pat. No. 3,798,200 indicates that cut growth and flex crack resistance is poor using the De Mattia flex results. Therefore, this prior art reference teaches specifically away from the applicant's invention in which it has been appreciated that a combination of physical properties relate most favorably and are positively correlated with superior tire performance on both the dynamometer-type test as set out in MVSS 109 and in actual road courses. The average molecular weight should lie between 1,000 and 2,000 which is contrary to the teachings and conclusions of U.S. Pat. No. 3,798,200 and 3,963,681.
This invention resides in the recognition of the superior performance provided by a tire of the physical characteristics previously described (ribs and web structure) in conjunction with this specific polyether urethane chemistry. This combination yields a tire which is non-pneumatic in character but which can perform on the highway with durability and vehicle handling characteristics similar to a pneumatic tire.
It will be readily apparent to the skilled practitioner in the art that many modifications and changes can be made to the embodiments specifically documented herein. Such modification and changes are a part of the invention if they fall within the scope of the invention defined in the appended claims hereto.
|
A non-pneumatic tire is disclosed having a polyether polyol urethane elastomeric body with a plurality of angular radial ribs interconnected by webbing. The urethane is formed of at least two isocyanate-end capped polyether polyols of differing molecular weights to yield a tire with improved highway life and good vehicle ride characteristics.
| 2
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a so-called short-distance photographing lens which can photograph objects from infinity to a very short distance.
2. Description of the Prior Art
Various types of short-distance photographing lenses called the microlenses or the macrolenses have heretofore been put into practice, but there have been no sufficient ones. These lenses are designed to provide the best performance for objects at a relatively short distance, but their image forming performance has unavoidably been deteriorated as the photographing magnification has become greater. It has, therefore, been necessary to mount an attachment lens exclusively for use for the correction of aberrations on a lens body in order to maintain an excellent image forming performance for short-distance objects for which the photographing magnification is one-to-one magnification. Also, the F-number of the conventional lenses has been on the order of 3.5 at best and they have been unsatisfactory as commonly used lenses in terms of the brightness.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a short-distance photographing lens having a great aperture and having an excellent image forming performance in a photographing range from infinity to objects at a very short distance.
The short-distance photographing lens of the present invention comprising a forward group having a positive refractive power, a rearward group also having a positive refractive power, and a diaphragm provided between the two groups, and is designed such that during the focusing of the lens for infinity object to a short-distance object, both groups are moved toward the object side while the air space between the two groups is increased.
By adopting the so-called spacing correction, the present invention has established a new technique of aberration correction in the short-distance photographing condition of a lens system comprising two positive groups. In the present invention, the air space between the two groups, namely, the so-called diaphragm space, becomes great during the short-distance photography and therefore, where the diaphragm is provided integrally with the rearward group, the entrance pupil is displaced far away from the object and the angle formed between it and the optic axis of the light flux entering the lens system becomes small, thus facilitating the aberration correction. Where the diaphragm is provided integrally with the forward group, the exit pupil goes away from the image and the angle of the light flux leaving the lens system becomes small, thus facilitating the aberration correction again in this case. Therefore, by suitably balancing the distribution of refractive power, namely, the distribution of apparent brightness, of each of the forward and rearward groups, it is possible to reduce the aggravation of the aberrations during short-distance photography without making the lens system complicated. As a lens system comprising two lens groups of positive refractive power with a diaphragm interposed therebetween, the Gaussian type lens is typical and where it is desired to make such type of lens system have a great aperture ratio and a sufficiently long back focus, the refractive power of the forward group tends to become remarkably weaker than the refractive power of the rearward group. Where the lens system is made to have a great aperture ratio, each lens becomes thick and the back focus becomes short. Therefore, in order to provide a sufficient back focus in the condition of photographing an infinity object, the refractive power of the forward group must be weakened. This means that the light flux leaving the object is not so much converged by the forward group, and as the object is at a shorter distance, the emergent light from the forward group becomes more divergent. This light flux is taken over by the rearward group and thus, increase of the refractive power and brightness of the rearward group is required, but it is very difficult to design the rearward group so that it can well correct the various aberrations. It is, therefore, necessary to enhance the refractive power of the forward group more than in a conventional lens of this type having a great aperture ratio, and to increase the duty of the forward group as much as possible. By doing so, the duty of the rearward group for aberration correction is alleviated in the shortest distance range, and even in the case of the short distance the light flux from the object can be used in its condition of becoming a converged light flux after leaving the forward group. However, too great a refractive power of the forward group makes the aberration correction in the forward group difficult and it is therefore desirable to limit the refractive power of the forward group to such an extent that the light flux from the object at the shortest distance becomes a slightly divergent light flux after leaving the forward group.
The invention will become fully apparent from the following detailed description thereof taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A and 1B are cross-sectional views of a first embodiment of the present invention, FIG. 1A showing the condition during infinity object photographing and FIG. 1B showing the condition during shortest distance object photographing.
FIGS. 2A, 2B and 2C illustrate the various aberrations in the lens system of FIG. 1, FIG. 2A showing the aberrations when the object distance d0=∞, FIG. 2B showing the aberrations when the object distance d0=164.194 and the photographing magnification β=-1.0, and FIG. 2C showing the aberrations when d0=∞ and β=-1.0.
FIGS. 3A and 3B are cross-sectional views of the optical system according to a second embodiment of the present invention, FIG. 3A showing the condition when d0=∞ and FIG. 3B showing the condition when d0=209.438 and β=-0.7143.
FIGS. 4A and 4B illustrate the various aberrations in the optical system of FIG. 3, FIG. 4A showing the aberrations when d0=∞ and FIG. 4B showing the aberrations when d0=209.438 and β=-0.7143.
FIGS. 5A and 5B are cross-sectional views of a third embodiment of the present invention, FIG. 5A showing the condition when d0=∞ and FIG. 5B showing the condition when d0=205.696 and β=-0.7143.
FIGS. 6A and 6B illustrate the various aberrations in the system of FIG. 5, FIG. 6A showing the aberrations when d0=∞ and FIG. 6B showing the aberrations when d0=205.696 and β=-0.7143.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
From the above-described characteristic of the lens system according to the present invention, it is desirable to satisfy the following conditions.
1.6<f1/f<2.4 (1)
1.5<f1/f2<2.5 (2)
where f represents the total focal length of the entire system, and f1 and f2 represents the focal lengths of the forward and the rearward group, respectively.
The condition of formula (1) prescribes appropriate distribution of the refractive power for the forward group. If the lower limit of this condition is exceeded, the refractive power of the forward group will become too strong and it will be difficult to make the back focus sufficiently long in the infinity photographing condition and the variation in spherical aberration will become remarkable in the infinity object photographing condition and in the shortest distance object photographing condition. To correct this, the forward group must unavoidably be of a complicated construction. On the other hand, if the upper limit is exceeded, the duty of the refractive power for the rearward group will become relatively too strong and therefore, the spherical aberration in the shortest distance will occur so remarkably that it will be difficult to correct it. Enhancing the refractive power of the rearward group is effective to provide a great aperture ratio, as already noted, but it is disadvantageous for objects at the shortest distance and it is desirable to prescribe the refractive power of the rearward group in the above-indicated range as a lens system providing a high photographing magnification like that provided by the present invention.
The condition of formula (2) prescribes the ratio of the focal lengths, namely, the distribution of the refractive powers, of the forward and the rearward groups and with the condition of formula (1), this condition is for making the lens system bright and reducing the shortest distance and providing a high photographing magnification. Also, this condition, with the condition of formula (1), prescribes the spacing between the forward and the rearward groups. If the lower limit of the condition of formula (2) is exceeded, the refractive power of the forward group will become too strong and the amounts of various aberrations in the forward group will be increased. To correct this, the number of lenses forming the forward group may be increased to thicken the lens system, but since the principal point of the forward group which is adjacent to the image side comes into the interior of the lens, the lenses of the two groups interfere with each other during the photographing of an infinity object when the forward and the rearward groups come closest together and it becomes difficult to provide a sufficient diaphragm space. If the upper limit of formula (2) is exceeded, good aberration correction will be possible in the infinity photographing condition even if considerably high brightness is provided, but in the shortest distance photographing condition, various aberrations will occur so remarkably that no good correction can be maintained.
In the construction comprising a forward group and a rearward group as described above, the so-called modified Gaussian type lens system is specifically adopted as the basic construction. That is, as shown in FIG. 1 which shows a cross-sectional view of the optical system according to a first embodiment, the forward group G1 comprises, in order from the object side, a first positive lens L1 having its surface of sharper curvature facing the object side, a positive meniscus lens L2 having its convex surface facing the object side, and a negative meniscus lens L3 having its convex surface also facing the object side, and the rearward group G2 comprises a meniscus lens L4 consisting of a negative lens and a positive lens cemented together and having its concave surface facing the object side, and a second positive lens L5. In the conventional system wherein photographing of the shortest distance object is effected without changing the diaphragm spacing in such a lens construction, the spherical aberration is over-corrected and the astigmatism was great and the curvature of field was remarkable while, at the same time, excessive coma occurred, but by varying the diaphragm spacing according to the present invention, these aggravating aberrations can be corrected very well. Also, such a construction satisfies the condition of achromatism in the forward group G1 and the rearward group G2, and therefore, suffers little deterioration of the image resulting from the chromatic aberration even if each group is greatly moved with the diaphragm spacing varied. Thus, by a relatively simple construction, it is possible to correct the various aberrations sufficiently well even for objects at a very short distance. Here, if the average refractive index N1 of each lens forming the forward group is
1.68<N1<1.78 (3)
and if r1 and r2 represent the curvature radii of the object side surface and the image side surface of the first positive lens L1 located nearest to the object, it is desirable that the following relation be established:
0.7<(r2+r1)/(r2-r1)<0.97 (4)
If the refractive index of the forward group becomes smaller than the lower limit of the condition of formula (3), the curvature of each lens surface will become sharper to bear the refractive power as the forward group determined by formulas (1) and (2) and various aberrations, especially, a high order of spherical aberration, will occur remarkably to make the correction at the shortest distance difficult. On the other hand, if the upper limit of this condition is exceeded, the refractive index of the negative lens will tend to become high to effect achromatization in the forward group and the Petzval sum will become excessive in the positive direction to thereby bring about an increased curvature of field. Also, the condition of formula (4) is for well correcting the high order of spherical aberration in the shortest distance, as well as for correcting the negative distortion which occurs remarkably in the shortest distance if the aperture ratio of the lens system is increased. In the present lens system of the above-described construction, it is possible to minimize the astigmatism and to maintain the planarity of the image plane by increasing the diaphragm spacing with respect to the object at a shorter distance, whereas the negative distortion tends to be remarkable. It is, therefore, desirable to permit the positive distortion to a certain extent for an infinity object and the shape of the first positive lens L1 having the greatest function in correction of distortion has been determined by the so-called shape factor as shown by formula (4). If the lower limit of this condition is exceeded, a great deal of coma will occur and, if the upper limit of the condition is exceeded, the negative distortion will be increased so that it will become difficult to well correct the negative distortion by other components.
Embodiments of the lens system for short distance photography according to the present invention will hereinafter be described.
The first embodiment shown in FIG. 1 adopts the so-called modified Gaussian type and is constructed so as to satisfy all of the above-described four conditions. FIG. 1A shows the condition of the present embodiment during infinity object photography, and FIG. 1B shows the condition of the present embodiment during shortest distance object photography. This embodiment is constructed such that the diaphragm is movable with the rearward group. The numerical data of this embodiment are shown in Table 1 and the various aberrations are illustrated in FIG. 2. FIG. 2A shows the various aberrations when the object distance (the distance from the foremost lens surface of the lens system to the object) d0=∞, and FIG. 2B shows the various aberrations when the object distance d0=164.194 and the photographing magnification β=-1.0. The ordinate of spherical aberration at shortest distance object photography (β=-1.0) is shown hereinafter by numerical aperture (N.A.) instead of F-number. FIG. 2C shows spherochromatism and the lateral chromatic aberration when d0=∞ i.e. β=-1.0. It is seen that although the present embodiment is a bright lens system having F-number of 2.8, the chromatic aberration and the other aberrations are maintained in very well corrected conditions even in one-to-one magnification.
TABLE 1______________________________________(1st Embodiment)______________________________________Focal length f = 100.0 F-number 2.8Angle of view 2ω = 42.92°r1 = 93.082 d1 = 6.818 n1 = 1.77279ν1 = 49.4r2 = -1091.818 d2 = 0.182r3 = 34.545 d3 = 6.818 n2 = 1.71300ν2 = 53.9G1 r4 = 57.109 d4 = 1.909r5 = 163.636 d5 = 1.909 n3 = 1.61293ν3 = 36.9r6 = 29.252 d6 = variabler7 = -40.555 d7 = 1.909 n4 = 1.69895ν4 = 30.0r8 = 545.455 d8 = 14.636 n5 = 1.74443ν5 = 49.4G2 r9 = -45.455 d9 = 0.182r10 = 345.538 d10 = 6.818 n6 = 1.79668ν6 = 45.4r11 = -225.162d6 = 13.301 when the object distance d0 = ∞.d6 = 29.773 when the object distance d0 = 164.194,i.e. the photographing magnification β = -1.0.The diaphragm lies 5.818 ahead of the foremostlens surface of the rearward group G2. f1 = 208.824 f2 = 115.797______________________________________
In a second embodiment, as shown in FIGS. 3A and 3B, a positive meniscus lens L23 having a relatively weak refractive power and having its convex surface facing the object side is provided between the positive meniscus lens L2 and the negative meniscus lens L3 of the forward group in the construction of the first embodiment to provide a better correction of aberration in the forward group. FIG. 3A shows the condition when d0=∞ and FIG. 3B shows the condition when d0=209.438 i.e. β=-0.7143. The numerical data of this embodiment are shown in Table 2, and the various aberrations when d0=∞ and d0=209.438 i.e. β=-0.7143 are shown in FIGS. 4A and 4B, respectively. It is seen that although this embodiment has as great an aperture ratio as F-number 2.0, the various aberrations are well corrected even in the shortest distance.
TABLE 2______________________________________(2nd Embodiment)______________________________________Focal length f = 100.0 F-number 2.0Angle of view 2ω = 32.13° r1 = 84.959 d1 = 4.667 n1 = 1.64006 ν1 = 60.0 r2 = -1325.784 d2 = 0.133 r3 = 36.591 d3 = 6.000 n2 = 1.73200 ν2 = 53.7 r4 = 75.228 d4 = 1.333G1 r5 = 99.468 d5 = 4.667 n3 = 1.77279 ν3 = 49.4 r6 = 130.339 d6 = 1.733 r7 = 186.171 d7 = 2.000 n4 = 1.74950 ν4 = 34.96 r8 = 28.492 d8 = variable r9 = -38.353 d9 = 2.000 n5 = 1.66096 ν5 = 32.8 r10 = 213.825 d10 = 12.133 n6 = 1.77511 ν6 = 43.4G2 r11 = -46.259 d11 = 2.000 r12 = 309.113 d12 = 5.733 n7 = 1.71300 ν7 = 53.9 r13 = -182.440d8 = 13.710 when the object distance d0 = ∞.d8 = 32.377 when the object distance d0 = 209.438,i.e. the photographing magnification β = -0.7143.The diaphragm lies 5.333 ahead of the foremost lenssurface of the rearward group G1. f1 = 204.000 f2 = 107.692______________________________________
In a third embodiment, as shown in FIGS. 5A and 5B, a negative lens L23' comprising a negative lens and a positive lens cemented together is provided instead of the positive meniscus lens L23 in the construction of the above-described second embodiment to provide better achromatization in the forward group and enhance the correction capability for the other aberrations. As in the second embodiment, it has become possible to provide a lens system of F-number 2.0. FIG. 5A shows the condition when d0=∞ and FIG. 5B shows the condition when d0=205.696 i.e. β=-0.7143.
The numerical data of this embodiment is shown in Table 3, and the various aberrations when d0=∞ and β=-0.7143 are shown in FIGS. 6A and 6B, respectively.
TABLE 3______________________________________(3rd Embodiment)______________________________________Focal length f = 100.0 F-number 2.0Angle of view 2ω = 32.130 r1 = 108.589 d1 = 6.000 n1 = 1.77279 ν1 = 49.4 r2 = -1622.547 d2 = 0.133 r3 = 49.292 d3 = 6.000 n2 = 1.77279 ν2 = 49.4 r4 = 75.600 d4 = 5.333G1 r5 = 998.957 d5 = 2.667 n3 = 1.69895 ν3 = 30.0 r6 = 51.669 d6 = 6.667 n4 = 1.79631 ν4 = 40.92 r7 = 163.969 d7 = 0.133 r8 = 79.592 d8 = 2.667 n5 = 1.59507 ν5 = 35.6 r9 = 33.079 d9 = variable r10 = -37.087 d10 = 2.000 n6 = 1.64831 ν6 = 33.8 r11 = 247.596 d11 = 12.133 n7 = 1.80411 ν7 = 46.6G2 r12 = -50.893 d12 = 0.133 r13 =-1276.096 d13 = 5.733 n8 = 1.80411 ν8 = 46.6 r14 = -102.211d9 = 11.086 when the object distance d0 = ∞.d9 = 29.753 when the object distance d0 = 205.696,i.e. the photographing magnification β = -0.7143.The diaphragm lies 5.333 ahead of the foremostlens surface of the forward group G1. f1 = 204.000 f2 = 107.692______________________________________
According to the present invention, as has been described above, there is achieved a lens system which has no auxiliary lens added thereto and which is simple in construction and yet has a great aperture ratio and maintains good correcting conditions of aberrations even during the photographing of objects at a very short distance.
|
A lens system for photographing objects from infinity to a very short distance has a forward group having a positive refractive power, a rearward group disposed rearwardly of the forward group and having a positive refractive power, and a diaphragm member provided between the two groups. The forward group is movable by a predetermined distance along the optic axis of the lens system in accordance with the object distance for focusing. The rearward group is movable by an amount smaller than the amount of movement of the forward group in the direction of the optic axis in accordance with the object distance for focusing.
| 6
|
BACKGROUND OF THE INVENTION
The invention relates to a method and a device for measuring the flow vectors in gas flows.
From German Patent 37 12 153 C1, a method is known from which the precharacterizing part of claim 1 starts. In this method, the light of two laser beams is focussed by a focussing device in the flow channel at two focussing points arranged in close succession. When passing the focussing points, particles contained in the gas flow are illuminated. The scattered radiation reflected by the particles generates a start pulse when passing the first focussing point and a stop pulse when passing the second focussing point. By the time interval between these two pulses, that component of the vector of the particle velocity can be determined which extends in the plane of the two beams and passes through both focussing points. For determining that component of the flow vector which extends in beam direction, two measurements must be effected, wherein the measuring volume is respectively rotated by 180°, with the point of focus axially offset. By calculating the difference between the two measuring rates, the flow angle is detected with respect to the normal plane to the optical axis. This method requires a long measuring time due to the focal length variation.
The U.S. Pat. No. 4,919,536 describes a system for measuring the velocity field of a gas flow containing particles by using a laser Doppler spectral image converter. Particles transversely flow through a light plane generated by a laser. Two video cameras receive the scattered light generated by the particles. One camera receives the scattered light directly, and the other receives the scattered light via an optical frequency/amplitude converter. The velocity distribution over the light plane is detected from the video signals of the two cameras. Only a single velocity component is detected, namely the component in the direction of the angle bisector between the laser beam plane and the camera direction.
SUMMARY OF THE INVENTION
It is the object of the present invention to provide a method and device for measuring the flow vectors in gas flows to be able to completely determine the flow vectors by amount and spatial direction by means of a simple measuring equipment requiring not much space and being employable at sites difficult to access.
The method of the invention determines the flow vectors along that axis which passes through the two focussing spots according to the start-stop principle, i.e. like a light barrier by measuring the transit time. Measuring of that component that extends in the direction of the optical axis, i.e., transversely to the straight line passing through the focussing spots and in the longitudinal direction of the two beams, is made according to the Doppler principle, wherein use is made of the circumstance that a particle moving in the direction of the optical axis of a beam does not emit light with the radiation frequency of scattered light but with a frequency different therefrom, the frequency deviation being proportional to the velocity component in beam direction. In any case, in the method and with the device according to the invention, those photoelectric converters which are also used for the start-stop measurement are partly co-used for the Doppler measurement of the velocity vector extending in the direction of the optical axis. The measuring path formed between the focussing spots of the laser beams is rotated in the course of the measurement so as to detect the vector angle in the focal plane extending vertically to the beam direction. By using the same beams, the velocity component vertical thereto is detected according to the Doppler principle and allocated, particle by particle, to the other velocity component, i.e., the one in the focal plane.
The device according to the invention offers the advantage of a simple construction. It can be used in narrow sites and such sites difficult to access, e.g. in a flow channel for measuring the flow conditions at turbine blades, the beams being sent through a window of the flow channel and generating the measuring volume in the interior of the flow channel. Only a relatively small aperture angle is required for the optical access to the flow channel. The measurement of the velocity component in the direction of the optical axis is independent of the measurement of the two other velocity components (amount and direction within the focal plane). Detecting the flow component at right angles to the focal plane does not require any additional measuring time.
BRIEF DESCRIPTION OF THE DRAWINGS
Hereinafter, embodiments of the invention are explained in more detail with reference to the drawings, in which:
FIG. 1 shows a block diagram of a first embodiment of the invention in a simplified form,
FIG. 2 shows an enlarged representation of the detail II of FIG. 1,
FIG. 3 is a perspective view of the measuring volume,
FIG. 4 shows an enlarged representation of the detail III of FIG. 1,
FIG. 5 shows the transmission characteristics of the optical frequency/amplitude converter,
FIG. 6 shows a representation of the pulses generated at the photoelectric converters upon the passage of a particle through the measuring volume,
FIG. 7 shows another embodiment of a measuring device with an additional processing of the signals generated by the photoelectric converters for suppressing interferences, and
FIG. 8 is a schematic representation of a further embodiment of the measuring device.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows the basic construction of a first embodiment of the measuring device.
A laser 10 produces a laser beam 11. The laser is, e.g., an Ar + laser having a wavelength of 514 nm, or a frequency-doubled YAG laser having a wavelength of 532 nm. The laser beam 11 is divided into two diverging component beams 11a, 11b by means of a λ/4 plate 61 and a beam splitter 12, e.g., a Rochon prism (FIG. 2). Both component beams are substantially aligned in parallel by an optic 12a and deflected at right angles onto a prism 14 by a mirror 13. The prism 14 deflects the component beams again at right angles. Behind the prism 14, there is a focussing optic 15 focussing each of the component beams 11a, 11b in the measuring volume MV, a focussing spot of its own being formed for each beam. The focussing spot of the beam 11a is located in the measuring volume MV accurately on the optical axis OA of the focussing optic 15, while the focussing spot of the beam 11b is laterally offset from the optical axis OA.
The focussing spots included in the measuring volume MV are imaged in an imaging plane 17 by the focussing optic 15. Behind the imaging plane 17, there is a microscope 17 imaging the imaging plane 17 onto the receiving surfaces of two photoelectric converters PEC1 and PEC2. The beam 19 of the one focussing spot F1 is guided to a beam splitter 20 transmitting the one component beam S1 to the converter PEC2 and sending the other component beam S2, via a mirror 21, through a frequency/amplitude converter 22 to the other photoelectric converter PEC1.
The beam 23 issuing from the other focussing spot F2 is received only by the converter PEC2.
FIG. 3 shows the measuring volume MV. The focussing spot F1 of the component beam 11a lies on the optical axis OA of the focussing optic 15, and the focussing spot F2 of the other component beam 11b is spaced laterally therefrom and lies parallel thereto. As can be seen from FIG. 2, the focussing spots F1 and F2 are no fixedly defined points but elongated. When rotating the beam splitter 12, the one component beam 11a remains on the optical axis OA, whereas the other component beam 11b is pivoted about the optical axis OA. This pivot angle is designated by α in FIG. 2. The angle β denotes the deviation of the velocity vector v from the normal plane to the optical axis OA.
A particle P passing the two focussing spots F1 and F2 is successively illuminated by both component beams 11a, 11b. Then, the particle emits scattered light received by the converters PEC1 and PEC2. The light pulses of the component beam 11a are supplied to the converter PEC1 and thereupon, this converter generates start pulses. The light pulses caused by the component beam 11b are supplied to the converter PEC2, and thereupon, this converter generates stop pulses. Besides, the converter PEC2 additionally generates a pulse whenever the converter PEC1 generates a pulse.
In FIG. 6, the start pulse generated by the converter PEC1 is designated by 25 and the stop pulse generated by the converter PEC2 by 26. The time t between the start pulse 25 and the stop pulse 26 is a measure for the velocity component v T of the particle P between the two component beams 11a, 11b. In order to determine the entire velocity vector v, it is important to know the velocity component v z , (FIG. 3) in the direction of the optical axis OA. To determine the velocity component v z , the frequency/amplitude converter 22 is used in combination with the two photoelectric converters PEC1 and PEC2.
The optical frequency/amplitude converter has the effect that it transmits incident light with a transmission factor dependent on the wavelength.
The light frequency of the beam 19 issuing from the focussing spot F1 depends on the frequency of the irradiation light and on the velocity component v z of the particle in beam direction. This velocity component generates a Doppler shift of the scattered light. The Doppler shift Δυ amounts to ##EQU1## wherein υ 0 is the frequency of the laser light, Δυ is the Doppler shift of the scattered light in backscattering, and c is the light speed. As a consequence, the Doppler shift Δυ is a measure for the velocity component v z in beam direction.
As optical frequency/amplitude converter, a iodine cell having the transmission behavior shown in FIG. 5 and depending on the frequency υ is used. In FIG. 5, the transmission of the iodine cell T(υ) is illustrated in dependence on the frequency υ. When the frequency υ 0 changes due to a velocity component v z , the laser light reflected by the particle has a frequency υ(v z ), whereby the transmission T of the converter 22 changes by the value ΔT.
Hence, the converter 22 provides the photoelectric converter PEC1 with light of an intensity varying as a function of the velocity component v z in the direction of the optical axis. Thereupon, the photoelectric converter PEC1 generates an electric pulse whose amplitude depends on the intensity of the incident light, i.e. varies corresponding to the transmission of the converter 22.
The output signals of the converters PEC1 and PEC2 are supplied as start and stop pulses to a multichannel analyzer 30 via the lines 28 and 29. Further, the output pulses of the converters PEC1 and PEC2 are supplied to a divider 31. Meanwhile, the amplitude of the output signal of the converter PEC2 serves as reference value for the amplitude of the output signal of the converter PEC1.
As can be seen from FIG. 6, the start light pulses are not only supplied to the converter PEC1 via the converter 22, but also via the partially transmitting mirror 20 to the converter PEC2, which generates a reference pulse 27 simultaneously with the start pulse 25 (FIG. 6). Thus, the ratio between the pulses 25 and 27 is formed in the divider 31 and supplied to the multichannel analyzer 30 via a line 33.
From the Doppler shift, the velocity component v z is determined according to the above equation (1). Therefrom, the multichannel analyzer 30 calculates the angle β for each particle passage in accordance with ##EQU2##
The velocity component v z is determined based on the Doppler principle and the velocity component v T within the normal plane to the optical axis is determined by transit time measurement between the beams 11a and 11b.
FIG. 7 shows an embodiment wherein the measuring equipment is identical to that of FIG. 1 down to the photoelectric converters PEC1 and PEC2. The processing of the electrical signals of the photoelectric converters, however, is different, which is explained hereinafter.
The pulses generated by the photoelectric converters PEC1 and PEC2 are very noisy. The output signals of the photoelectric converter PEC1 are supplied to a frequency filter 41 via an amplifier 40 and transferred to an exponentiator 43. From the input signal I, the exponentiator 43 forms the output signal I n with the exponent n. The output signal of the exponentiator 43 is supplied to the one input of a dividing circuit 45 via an integrator 44.
The output signals of the photoelectric converter PEC2 are likewise amplified in an amplifier 46 and supplied, via a filter 47 and an electronic switch 48, to an exponentiator 49 which also forms the nth power of its input signal. The output of the exponentiator 49 is connected to the other input of the dividing circuit 45 via an integrator 50.
The dividing circuit 45 divides the dividend A by the divisor B, and the output signal A/B is supplied to a root calculator 51 extracting the nth root from this output signal (as radicand). The output signal of the root calculator 51 is supplied to an input of the multichannel analyzer 30.
The switches 42 and 48 are controlled by a trigger circuit 52 receiving the signal of the filter 41 as input signal and also controlling the multichannel analyzer 30. The integration intervals of the integrators 43 and 49 are determined through the trigger circuit.
By the described signal processing, the output signals of the photoelectric converters are exponentiated with an exponent n and integrated over a time interval t 2 -t 1 , before the division is effected. Thereafter, the integral values are divided and the nth root of the quotient is extracted. Thereby, it is achieved that the intensive central portion of a pulse, which has a good signal-to-noise ratio, is given more weight than the signal edges in which the signal-to-noise ratio is worse. Experimentally, n=2 has proven to be useful. The integration interval t 2 -t 1 is arranged such that it begins before a start pulse and ends after the start pulse.
While the two photoelectric converters PEC1 and PEC2 supplying the start signals and the stop signals are also used for the Doppler principle in the previous embodiments as well, the embodiment of FIG. 8 provides for an additional photoelectric converter PEC3 to which the start light pulses are supplied via a partially transmitting mirror 16 arranged between the two mirrors 60 and 21. The photoelectric converter PEC2 generates the reference pulses for the pulses generated by the photoelectric converter PEC1, whose amplitudes are influenced by the transmission of the frequency/amplitude converter 22. The signals of the converters PEC1 and PEC2 are supplied to the dividing circuit 45, which supplies the quotient to the multichannel analyzer 30 thereupon. The signals of the converter PEC3, which are more intensive than those of the converter PEC1, are used as start signals for the transit time measurement. The signals of the converter PEC2 are used as stop signals.
|
In the optical measurement of the flow vectors in gas flows, two substantially parallel light beams (11a, 11b) are focussed at separate focussing spots. The particles passing the focussing spots light up and thereby generate a start pulse and a stop pulse, respectively. Therewith, the component of the flow vector extending in the normal plane to the optical axis (OA) is detected by transit time measurement. The flow component pointing in the direction of the optical axis (OA) is detected independent thereof according to the Doppler principle by supplying the scattered light generated by the particles to an optical frequency/amplitude converter (22).
| 6
|
RELATED APPLICATIONS
This present application claims priority to co-pending U.S. Provisional patent application Ser. No. 60/055,014, filed on Aug. 6, 1997; U.S. Provisional Patent Application Ser. No. 60/054,960, filed on Aug. 7, 1997; and U.S. Provisional Patent Application Ser. No. 60/075,208, filed on Feb. 19, 1998. The entire teachings of each application are incorporated herein by reference.
BACKGROUND OF THE INVENTION
Flexible, temporary road signs for advance warning to a motorist of an approaching unsafe driving area or construction site are known in the art. A flexible road sign, capable of being disassembled and rolled up for convenience and portability, is exemplified by the teachings in U.S. Pat. No. 4,980,984. However, such signs are inconvenient to store when not in use.
SUMMARY OF THE INVENTION
The invention includes a portable and compact retroreflective sign system. The system includes a base, a winding mechanism roller attached to the base, and a retroreflective roll-up sheeting having a first end and a second end, wherein the first end is attached to the roller and the sign is wound about the roller. A sign support is attached to the base for supporting the roll-up sign in an unrolled position, wherein the sign support is extendible from the base. An attachment means is present at the second end of the retroreflective roll-up sheeting for attaching the sheeting to the sign support.
The present invention has many advantages including being compact and portable storage system. Also, the storage system provides substantial stability to the sign system in windy conditions.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a first embodiment of a compact retroreflective sign system in a closed position.
FIG. 2 is a perspective view of the first embodiment in an open position.
FIG. 3 is a perspective view of a second embodiment of the compact retroreflective sign system in a closed position.
FIG. 4 is a perspective view of the second embodiment of the compact retroreflective sign system in a partially opened position.
FIG. 5 is a perspective view of the second embodiment of the compact retroreflective sign system in an open position.
DETAILED DESCRIPTION OF THE INVENTION
The features and details of the method and apparatus of the invention will now be more particularly described with reference to the accompanying drawings and pointed out in the claims. It will be understood that the particular embodiments of the invention are shown by way of illustration and not as limitations of the invention. The principal features of this invention can be employed in various embodiments without departing from the scope of the invention.
A portable and compact retroreflective sign system 10 includes a retroreflective sign, which when in its rolled position, is housed in a box 14 with a hinged cover 16, as shown in FIG. 1. In one embodiment, the box has a height of about 30 cm, a width of about 30 cm, and the length of about 90 cm. The cover 16 can include a handle 18 to allow easy carrying of the box and latches 20 for securing the cover closed. In addition, the box 14 has legs 22 which can swivel about points 24 outwardly to provide greater stability and support of the opened sign to prevent it from tipping over in windy conditions.
Shown in FIG. 2, box 14 is in an opened position. The rolled retroreflective sign is pulled straight up together or separately with a collapsible sign support 26. In one embodiment, the collapsible sign support 26 can be a telescoping pole and can have a height of about 175 cm.
The winding mechanism roller 28, such as in a window shade or self-winding projector screen, allows easy setup of the sign as well as easy roll-up of the sign after use. Alternatively, the roller may be manually wound. Further, the box 14 provides good protection of the sign once rolled up. The portable and compact system provides portability, while minimizing the manual and complicated steps of setting up and rolling up a traditional flexible roll-up sign which is supported with a cross-rib system.
In another embodiment, as shown in FIG. 3, system 50 can include handle 52 and latches 54 for securing the system closed. System 50 includes a series of base panels 56 which surround inner box body 58. Base panels 56 have hinges 60 to allow the panels to unfold. As shown in FIG. 4, the base panels 56 of the system 50 can be fully opened and laid flat on the ground. A winding mechanism roller 62 includes retroreflective sheeting 64, which includes cube-corner prisms 65, wound around roller 62. The winding mechanism roller 62 is attached to the interior of inner box body 58. A collapsible support 66 which is attachable by attachment means 68, such as a hook or latch, to one end of the retroreflective sheeting 64 is sufficiently extendable.
As shown in FIG. 5, retroreflective sheeting 12 is in an unwound position and the collapsible support 66 is in an extended position. The inner box body 58, which is pivotly mounted to the panels 56 by an attached pivot means, such as a carousel (not shown), and can then be rotated about ninety degrees to set on the flatten base panels. In this embodiment, the base panels serve as a base to support the opened retroreflective sheeting to help prevent it from tipping over in windy conditions. As shown, the inner box body 58 is rotated at an angle, preferably perpendicularly, to the folds of base panels to help provide stability to the system.
The retroreflective sheeting can include a traffic sign 70, such as a MEN WORKING, YIELD or STOP sign. After use, the sign is retracted by winding together with the collapsible support 66 into inner box body 58 and the base panels 56 of the system can then be folded and closed.
An example of a material suitable as a roll-up sign is disclosed in International Publication No. 97/37252, published on Oct. 7, 1997 and corresponding U.S. patent application Ser. No. 08/625,199, filed on Apr. 1, 1996, the teachings of which are incorporated herein in its entirety by reference. The system can be used at various sites where a temporary sign is needed such as with road work.
Retroreflective materials are typically formed of a sheet of thermoplastic, which has a colorant mixed therein with the polymers. Attached to the sheet of thermoplastic is an array of cube-corner or prismatic retroreflectors as described in U.S. Pat. No. 3,712,706, issued to Stamm on Jan. 23, 1973, the teachings of which are incorporated herein in its entirety by reference. Generally, the prisms are made by forming a master die on a flat surface of a metal plate or other suitable material. To form the cube-corner, three series of parallel equidistant intersecting V-shaped grooves 60 degrees apart are inscribed in the plate. The die is then used to process the desired cube-corner array into a flat plastic surface. When the groove angle is 70 degrees, 31 minutes, 43.6 seconds, the angle formed by the intersection of two cube faces (dihedral angle) is 90 degrees and the incident light is retroreflected back to the source.
The efficiency of a retroreflective structure is the measure of the amount of incident light returned within a cone diverging from the axis of retroreflection. A distortion of the prismatic structure adversely affects the efficiency. Furthermore, cube-corner retroreflective elements have low angularity at some orientation angles, for instance, the elements will only brightly reflect light that impinges on it within a narrow angular range centering approximately on its optical axis. Low angularity arises from the inherent nature of these elements which are trihedral structures having three mutually perpendicular lateral faces. The elements are arranged so that the light to be retroreflected impinges into the internal space defined by the faces, and the retroreflection of the impinging light occurs by internal retroreflection of the light from face to face of the element. Impinging light that is inclined substantially away from the optical axis of the element (which is a trisection of the internal space defined by the faces of the element) strikes the face at an angle less than its critical angle, thereby passing through the face rather than being reflected. Further details concerning the structures and the operation of cube-corner microprisms can be found in U.S. Pat. No. 3,684,348, issued to Rowland on Aug. 15, 1972, the teachings of which are incorporated by reference herein in its entirety. A method for making retroreflective sheeting is also disclosed in U.S. Pat. No. 3,689,346, issued to Rowland on Sep. 5, 1972, the teachings of which are incorporated by reference herein in its entirety. The disclosed method is for forming cube-corner microprisms in a cooperatively configured mold. The prisms are bonded to sheeting which is applied thereover to provide a composite structure in which cube-corner microprisms project from one surface of the sheeting.
Equivalents
Those skilled in the art will recognize or be able to ascertain using no more than routine experimentation, many equivalents to the specific embodiments of the invention described specifically herein. Such equivalents are intended to be encompassed in the scope of the claims.
|
A portable and compact retroreflective sign system includes a base, a winding mechanism roller attached to the base, and a retroreflective roll-up sheeting having a first end and a second end, wherein the first end is attached to the roller and the sign is wound about the roller. A sign support is attached to the base for supporting the roll-up sign in an unrolled position, wherein the sign support is extendible from the base. An attachment means is present at the second end of the retroreflective roll-up sheeting for attaching the sheeting to the sign support.
| 4
|
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of priority under 35 U.S.C. §119 of German Patent Application DE 10 2011 111 002.3 filed Aug. 18, 2011, the entire contents of which are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The invention relates to an actuator, in particular for opening a lock or locking arrangement of an emergency oxygen container or a mask door in an aircraft.
BACKGROUND OF THE INVENTION
[0003] In passenger aircraft, a passenger support unit or passenger service unit PSU, is typically arranged above the seat rows, in which unit, apart from the illumination and ventilation, in particular passenger oxygen masks are also arranged, which in the case of a pressure drop within the cabin, fall downwards, in order to be within reach of the passengers. For this, a compartment or container which is closable by mask door arranged on the lower side and in which typically two four or also more passenger oxygen masks are arranged, depending on the number of seats located therebelow, is provided in the passenger support unit. The masks usually have an emergency oxygen supply tube, via which they are connected to a suitable stationary oxygen connection in the passenger service unit. The stationary oxygen connection is typically connected to an emergency oxygen container.
[0004] In the case of requirement, the mask door as well as the emergency oxygen container must be opened, in order to be able to supply the passengers with oxygen. It is known in the state of the art, for these to be able to be opened in an aircraft from a central location, or however to be able to be opened by the passenger himself in a simple manner.
[0005] It is also known in the state of the art, to apply components of shape memory alloys as actuators. Thereby, one differentiates between three types of activation. With the first type of activation, the current is led directly through the shape memory alloy. The current heats the shape memory alloy on account of the resistance. Heat can alternatively be fed indirectly. Thereby, an electrical current heats a medium which then heats the shape memory alloy. Moreover, heat can be fed directly from a medium changing the temperature, such as for example with a thermostat in a cooling circuit.
[0006] In passenger aircraft, the input variable for opening a locking of the emergency oxygen container or mask door consists of a high alternating voltage. It is counted as belonging to the state of the art, to open such flaps by way of electromagnets. The disadvantage with this however is that the electromagnet is comparatively heavy, which is basically problematic with aircraft applications, and that on account of the actuation, one can only ascertain in the emergency case or in sporadic intervals for test purposes, the moving component can jam to the extent that the magnet force is possibly no longer sufficient to move this. This represents a significant safety risk.
SUMMARY OF THE INVENTION
[0007] Against this background, it is an object of the invention to provide an actuator which on the one hand is suitable for larger alternating voltages, consumes less current, is lightweight and operates reliably also after a longer period of not being actuated, i.e. produces a high actuation force.
[0008] According to the invention, this object is achieved by an actuator which in particular is suitable for opening a locking arrangement of an emergency oxygen container or a mask door in an aircraft, but also for other applications, comprising an opener of a shape memory alloy and of a resistance wire which is arranged thereon, is connected thereto in a heat-conducing manner and is connectable to a supply voltage. The actuator according to the invention is particularly advantageous for opening a locking arrangement of an emergency oxygen container or a mask door in an aircraft, but can however also be used for other applications in an advantageous manner, which are neither restricted to an aircraft nor to the opening procedure per se. Thus basically any and every actuation can be effected, e.g. the opening of an emergency door in a building, the opening of a flap of a car and much more.
[0009] The solution according to the invention is in particular particularly suitable for the application in an aircraft which is discussed here, since the resistance wire, given a suitable dimensioning, can be subjected directly to the alternating voltage which is available, without too high a current arising. Moreover, such an actuator can be manufactured inexpensively, simply and with only a little weight. The actuation forces of the actuator according to the invention are comparatively high, so that they also ensure a reliable actuation, in particular the opening, even after a longer period of not being actuated. The heating by way of the thermally conductive connection between the resistance wire and the opener is effected almost immediately, thus with a time delay which in practice is not noticeable.
[0010] Basically, the voltage can also be applied directly to the shape memory alloy. Since shape memory alloys have a low resistance, very high currents result with high voltages and these high currents could destroy the shape memory alloy. For this reason, the voltage would have to be transformed to a lower voltage, if it is to be applied directly to the shape memory alloy.
[0011] Advantageously, the resistance wire at least partly is wound around the opener, in order in this manner to achieve a rapid and intensive heating of the opener when subjecting the wire to current.
[0012] An opener is a component which is suitable for actuating a locking arrangement such that it is brought from a closed position into an opened position. Preferably, an opener is a component which is shaped in an elongate manner, so that a temperature change can effect a main extension of the opener in a single direction, which is to say in the longitudinal direction. Preferably, the cross section of the opener is circular, so that the risk of damage to the resistance wire is particularly low.
[0013] A locking arrangement is preferably configured to securely hold an emergency oxygen container and/or a mask door in a closed condition. A locking arrangement can then for example comprises a mechanical bar or an electromagnet for this. The opener is then preferably configured to be able to displace the mechanical bar into a position, in which it can no longer hold the emergency oxygen container or the mask door in a closed condition. If the locking arrangement comprises an electromagnet, the opener can be configured to disconnect this from an electric current.
[0014] Shape memory alloys are often called memory metals. This is due to the fact that they can assume an earlier shaping again despite a subsequent large deformation. The shape change is based on the temperature-dependent lattice transformation of two different crystal structures of a material. The shape memory alloy can have a one-way effect. The one-way effect is characterised by a one-off shape change on heating a sample which was previously pseudo-plastically deformed, for example in the martensitic condition. The shape memory alloy can also have an external two-way effect. The shape return on cooling a component and which is forced by way of a for example mechanical force acting externally, is indicated as an external two-way effect. This can be realized by a spring for example, which was tensioned during the heating. Preferably, the shape memory alloy has an intrinsic two-way effect, so that the opener is set up to be able to assume two different shapes at two different temperatures. The component has preferably gone through several thermo-mechanical treatment cycles, so that it can assume its defined shape again on cooling. Preferably, stress fields in the material were formed by way of this, which encourage the formation of certain martensite variants on cooling. Thus the trained shape for the cold condition preferably only represents a preferred shape of the martensite structure.
[0015] The shape memory alloy preferably comprises NiTi (nickel-titanium; nitinol) and/or CuZn (copper-zinc) and/or CuZnAl (copper-zinc-aluminium) and/or CuAlNi (copper-aluminium-nickel) and/or FeNiAl (iron-nickel-aluminium).
[0016] A resistance wire is a wire which has an electrical resistance. If current is led through the resistance, electrical power is converted into thermal power. The resistance wire can therefore also be indicated as a heating wire. It is possible to keep the mass to be heated small by way of the use of a resistance wire. The activation time can also be kept small by way of this.
[0017] Usefully, the opener is configured to change its length with changes of its temperature. By way of this, the opener can be applied in a particularly simple manner to open an emergency oxygen container and/or a mask door.
[0018] In one advantages design, a thermistor is connected in series before the resistance wire as a protection for this. The resistance wire is particularly protected by way of this and cannot heat to an unallowable extent on application of an electrical current.
[0019] Thermistors, PTC-resistors or PTC-thermistors are electrically conductive materials which are capable of conducting the current better at lower temperatures than at higher ones. Their electrical resistance increases with an increasing temperature. This type of resistors thus has a positive temperature coefficient. The thermistors can have a pure metal. Preferably, thermistor is manufactured of semi-conductive, polycrystalline ceramics, for example BaTiO 3 which in a certain temperature range build up a blocking layer at the grain boundaries.
[0020] A particularly advantageous design envisages the resistance wire comprising copper, nickel and manganese. The thermal power of the resistance wire can remain comparatively independent of the temperature of the resistance wire by way of this. A heating and thus desired defined length change of the opener can thus be set in a particularly accurate manner.
[0021] Particularly preferably, the resistance wire comprises 53 to 57% copper, 43 to 45% nickel and 0.5 to 1.2% manganese. A specific electrical resistance increasing particularly slowly with temperature and over a very large temperature range results by way of this. The released thermal power on application of an electric current remains particularly independent on the surrounding temperature by way of this.
[0022] In each case, one can envisage a distance between the windings of the resistance wire, in order to securely prevent a length change of the opener leading to a damage of the resistance wire. By way of this, the resistance wire can compensate length changes of the opener in a simple manner. Preferably, the width of the distance between two windings corresponds to at least the diameter of the resistance wire. Particularly preferably, the width of the distance is as large as double the diameter of the resistance wire.
[0023] In one advantageous embodiment, the opener and the resistance wire are at least partly received in a tube. By way of this, the opener can be led such that it is located in each case in a defined position at different temperatures. With a temperature increase and a lengthening of the opener resulting from this, the opener on account of this can extend in only two directions which are opposite to one another. An undesired sagging of the opener can be prevented. Moreover, it is this possible to ensure the functioning of the actuator even with unfavourable surrounding conditions, such as the installation in an environment, in which particles which can reach the resistance wire and which for example can tap current therefrom, are located. The opener can extend in only one direction if the tube is closed at one end.
[0024] Preferably, the wall of the tube is designed as thinly as possible. By way of this, one can prevent heat from being unnecessarily led away from the resistance wire. Moreover, such a design has a favourless effect on the weight of the actuator. Preferably, the thickness of the wall of the tube is smaller than the diameter of the resistance wire. Particularly preferably, the thickness of the wall corresponds to half the diameter of the resistance wire.
[0025] If the opener as well as the resistance wire are received in the tube, the wall of the tube advantageously consists of a material which has a low electrical conductivity and a low thermal conductivity. Preferably, the specific electric resistance of the tube lies above 10 16 Ω·mm 2 /m, particularly preferably above 10 18 Ω·mm 2 /m at 20 degrees Celsius. Preferably, the thermal conductivity of the tube lies below 1 W/(m*K), particularly preferably below 0.5 W(m*K) at 0 degrees Celsius.
[0026] In order to prevent the resistance wire becoming damaged with length changes of the opener, the opener at least partly can be received in a tube, and the resistance wire at least partly be wound around the tube. By way of this, the opener can also be led such that it is located in each case in a defined position at different temperatures. Moreover, a precise leading of the opener is possible by way of this. If the tube is provided between the opener and the resistance wire, the wall of the tube advantageously consists of a material which has a small electrical conductivity and a high thermal conductivity. Preferably, the specific electric resistance of the tube lies above 10 16 Ω·mm 2 /m, particularly preferably above 10 18 Ω·mm 2 /m at 20 degrees Celsius. Preferably, the thermal conductivity of the tube with this embodiment lies above 15 W/(m*K), particularly preferably above 200 W(m*K) at 0 degrees Celsius.
[0027] In one advantageous embodiment, the tube is a capillary. By way of this, it is possible to keep the mass of the tube very low, so that a rapid activation is possible with low energy consumption. A capillary is preferably a very fine, longitudinally extended cavity with a very small inner diameter.
[0028] In one advantageous embodiment, the actuator is arranged in a passenger service unit in an aircraft. By way of this, the actuator can be applied in a particularly effective manner for opening a mask door in an aircraft.
[0029] A passenger service unit is installed into large passenger aircraft in the pressure cabin above each passenger seat row. It contains for example reading lamps, loudspeakers, oxygen masks which fall out of an opening with a pressure drop, as well as suitably illuminating notice signals such as the fasten seatbelt signs. Often, a loudspeaker is located there for the audio instructions of the cabin crew.
[0030] Preferred embodiments of the invention are hereinafter explained in more detail by way of the attached drawings. The various features of novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and specific objects attained by its uses, reference is made to the accompanying drawings and descriptive matter in which preferred embodiments of the invention are illustrated.
BRIEF DESCRIPTION OF THE DRAWINGS
[0031] FIG. 1 is a greatly simplified view showing a longitudinal section of an actuator and a bar of a mask door;
[0032] FIG. 2 is a view showing a longitudinal section of an actuator in a representation according to FIG. 1 , with which the opener is received in a tube.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0033] Referring to the drawings in particular, FIG. 1 shows a longitudinal section of an actuator 1 and a bar 6 of a mask door 7 . The actuator 1 comprises an opener 2 . The opener 2 is a rod with a circular cross section which consists of a memory shape alloy.
[0034] A resistance wire 3 is wound around a middle part of the opener 2 and is electrically insulated from the opener 2 via an insulating layer. Here, 280 windings of the resistance wire 3 are located on the opener 2 . The resistance wire 3 is thereby wound around the opener 2 such that a distance is present between the individual windings. This distance corresponds roughly to the diameter of the resistance wire 3 . The resistance wire 3 has about 55% copper, 44% nickel and 1% manganese.
[0035] At its ends, the resistance wire 3 is connected to connection leads 4 . These connection leads 4 connect the resistance wire 3 to a supply voltage 5 .
[0036] Apart from the actuator 1 , a bar 6 and a part region of a mask door 7 is shown in FIG. 1 . The bar 6 has an L-shape with a first limb 8 and with a second limb 9 and is rotatably mounted in a bearing 10 . The bar 6 is arranged such that the first limb 8 lies in front of the mask door 7 , and the second limb 9 is located in the direct vicinity of a first end 11 of the opener 2 .
[0037] If current is led from the supply voltage 5 through the connection leads 4 and through the resistance wire 3 , this is heated, since a part of the electric energy is converted into thermal energy by way of the electric resistance of the resistance wire 3 . A part of the thermal energy is released to the opener 2 by way of thermal conduction, heat radiation and convection, since the resistance wire 3 bears directly on the opener 2 . The opener 2 is heated by way of this.
[0038] Since the opener 2 is fixed on one side (bearing A) and changes its shape at high temperatures such that it increases its length, the end 11 of the opener 2 moves to the second limb 9 of the bar 6 . If the end 11 presses against the second limb 9 , a force on the bar 6 arises, whose line of action goes past the bearing 10 , in which the bar 6 is rotatably received. A torque on the bar 6 arises by way of this, and the effect of this torque is that the bar 6 rotates in the clockwise direction about the bearing 10 . By way of this, the first limb 8 of the bar 6 moves out of a region, in which it lies in front of the mask door 7 , into a region in which it releases the mask door 7 . By way of this, an opening of the mask door 7 is made possible by way of leading a current through the connection leads 4 . In order to ensure that the mask door 7 opens when the bar 6 releases this, a compression spring which is not shown and which exerts a pressure onto the mask door 7 , is provided on the side of the mask door 7 which is away from the bar.
[0039] Due to the fact that distances between the individual windings of the resistance wire 3 are provided, one prevents the resistance wire 3 from becoming damaged when the opener 2 extends.
[0040] A simpler, quicker, inexpensive and more robust actuator 1 for alternating voltages and one which consumes less energy and fulfils electric demands amongst other things with regard to the emission of interference and current distortions, is provided due to the fact that the opener 2 is heated indirectly by way of the resistance wire 3 .
[0041] It would not be possible to heat the opener 2 in a direct manner without voltage transformation, since the supply voltage 5 supplies a high alternating voltage. This alternating voltage would have to be transformed to a lower voltage, which entails quite some effort, if this voltage were to be applied directly to the opener 2 . The opener 2 has a very low resistance which with high voltages would lead to very high currents which would destroy the opener 2 . Moreover, with a voltage transformation of an alternating input variable, an undesired current distortion can occur.
[0042] FIG. 2 shows a longitudinal section of an actuator 1 , with which the opener 2 is received in a tube 12 . The tube 12 consists of steel. It has a wall thickness of 0.1 mm. The resistance wire 3 has an electrical insulation layer formed by paint and is wound around the tube 12 .
[0043] The opener 2 with a longitudinal change is additionally guided through the tube 12 . Thus it is ensured that the opener 2 extends in a certain direction when it heats up. Moreover, one prevents the resistance wire 3 from being able to be damaged when the length of the opener 2 changes.
[0044] The wall thickness of the tube 12 is relatively thin, since the resistance wire 3 can be provided at a small distance to the opener 2 by way of this. Since the tube is of metal, a good thermal conduction between the resistance wire and the opener is effected. With the embodiment represented by way of FIG. 2 , the opener by way of the bearing A is also prevented on one side from moving away from the bar 6 with an extension due to heating, and rather a length change in the direction of the second limb 9 of the bar 6 is effected.
[0045] With the embodiment represented by way of FIG. 2 , a restoring spring 13 is yet provided, which ensures that the opener 2 returns back into its initial position with a subsequent cooling. The bar represented in FIG. 2 functionally corresponds to that represented by way of FIG. 1 , even if the bar in FIG. 2 has a different shape and mounting.
[0046] While specific embodiments of the invention have been shown and described in detail to illustrate the application of the principles of the invention, it will be understood that the invention may be embodied otherwise without departing from such principles.
APPENDIX
List of Reference Numerals
[0000]
1 actuator
2 opener
3 resistance wire
4 connection lead
5 supply voltage
6 bar
7 mask door
8 first limb
9 second limb
10 bearing
11 first end
12 tube
13 restoring spring
A bearing
|
An actuator for opening a locking of an emergency oxygen container or a mask door in an aircraft. The actuator includes an opener of a shape memory alloy and a resistance wire. The resistance wire is at least partly wound around the opener and can be connected to a supply voltage.
| 8
|
BACKGROUND OF THE INVENTION
The field of the present invention is that of priming systems for an explosive charge.
Ordinarily, a priming system comprises a pyrotechnic priming component (or primer) that initiates a secondary explosive booster charge, the secondary explosive booster charge providing initiation of the principal explosive charge.
The primer is a pyrotechnic component that contains a small quantity of very sensitive primary explosive. The secondary explosive booster charge is less sensitive than the primer, but can be initiated by it.
The principal drawback of known priming systems has to do with the extremely sensitive nature of the primer and the primer boosters.
Moreover, in order to initiate insensitive explosives, priming components that can deliver high energies have to be employed.
To prevent untimely detonation of explosive charges, safety and arming devices have been designed with which the primer or primer booster can be isolated from the remainder of the pyrotechnic system.
These devices are complex and costly mechanical assemblies.
Priming systems are all the more difficult to implement (and bulky) if the explosive being initiated is of the insensitive type, and thus requires substantial levels of priming energy.
SUMMARY OF THE INVENTION
One purpose of the invention is to propose a safety priming system that does not possess such disadvantages. Specifically, the priming system according to the invention allows initiation of an explosive charge without using pyrotechnic components with a primary composition, and without even using priming explosives.
Another purpose of the invention is to provide a priming system particularly well suited for safely priming of insensitive explosives.
A first aspect of the invention provides a safety priming system for an explosive charge having a block made of pyrotechnically inert material, the block having on one of its surfaces a cavity placed facing the explosive charge, and structure for allowing percussion of the block at a receiving surface substantially parallel to that on which the cavity is present.
Advantageously, the percussion structure includes a pressurizable chamber that can be filled with a compressible fluid using a supply line, one end of which chamber, arranged facing the receiving surface of the block, is closed by a sliding piston that is made integral with the chamber by connecting structure that can be unlocked by the action of a control device.
According to one particular embodiment, the connecting structure may include explosive pins.
According to another particular embodiment, the connecting structure may include pegs that are retractable by the action of an actuator.
The fluid may, for example, selected from among the following gases: air, helium, carbon dioxide, nitrogen.
According to a first embodiment, the cavity may be covered with a lining of ductile material, and the block may be made of a material whose impact impedance is greater than or equal to that of the lining.
The material of the block can be selected, for example, from the following: titanium, iron, beryllium, cobalt, aluminum.
The lining of the block can then advantageously be made of aluminum or an aluminum alloy.
According to another embodiment, the cavity may not be covered with a lining, and the block is made of a material that is ductile under impact.
In this case the material of the block can be selected from the following: aluminum, uranium, copper.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood upon reading the description below of preferred embodiments thereof, made with reference to the attached Figures that schematically depict priming system according to the inventions wherein:,
FIG. 1 shows a priming system according to a first embodiment of the invention in which a lining serves as the jetted material;
FIG. 2 shows a priming system according to a second embodiment of the present invention in which the block itself serves as the jetted material; and
FIG. 3 shows a retractable pin that is useable with either of the first and second embodiments of the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIG. 1, a priming system 1 according to the invention is intended to initiate an explosive charge 2 that includes, for example, of a mixture of octogene (hamocyclonite) and TATB (triaminotrinitrobenzene) arranged inside a casing 3.
The priming system and the explosive are arranged inside a munition (not depicted), for example, a bomb or a missile launched by a firing platform such as an aircraft.
Priming system 1 comprises a substantially cylindrical block 4 made of a pyrotechnically inert material. The block can be made, for example, of titanium.
The block 4 possesses a substantially conical cavity 5, onto which a lining 6 is affixed, for example, by adhesive bonding.
The cavity can possess another type of concave profile (for example spherical).
In order for a jet to be able to develop, the profile of the cavity must have at every point a radius of curvature that is less than the maximum radius of the cavity.
Lining 6 will be made of a ductile material, whose impact impedance will therefore be selected to be less than or equal to that of the constituent material of block 4. For example, a lining made of aluminum or aluminum alloy can be selected.
It is also possible that no lining is arranged in the cavity (FIG. 2). The block would then preferably be made of a material that is ductile under impact, i.e. possessing a plastic yield stress less than 500 MPa. Materials meeting this criterion are, for example, aluminum, uranium (unalloyed), and copper.
Provision of a lining makes it possible to produce a jet by applying to the block an energy level lower than that necessary to produce a jet in the absence of a lining.
As an example, it might thus be possible to combine an aluminum lining with a block whose material would be selected from the following: titanium, iron, beryllium, cobalt, aluminum.
Cavity 5 is arranged facing explosive charge 2, at a distance on the order of 20 to 50 mm. Block 4 can be fastened onto casing 3 using flanges 20, for example.
Priming system 1 also comprises percussion structure 7. The percussion structure 7 includes a piston 8 that closes one end 9 of a pressurizable chamber 10.
The piston is made integral with chamber 10 by connection structure that can be unlocked by the action of a control device 11.
The control device comprises a programmable electronic system that provides for release of the connecting structure at the moment selected for initiation of explosive charge 2. The electronic system is activated by firing or release of the munition. It performs safety functions, in particular by preventing release of the connecting structure for a sufficient time to ensure a safe distance between the munition and the firing platform.
The electronic system causes release of the connecting structure in response to a control datum, for example a signal provided by a proximity fuse or a timer. Such a control device is well known to those skilled in the art, and therefore will not be described in further detail.
In this case the connecting structure includes three explosive pins 12 that are regularly distributed angularly and are initiated by the control device.
The connecting structure may comprise pins that are retractable by the action of an actuator having a spring element 30. (FIG. 3)
The actuator can be electrically controlled, and comprise in particular a motor or an electromagnet.
As a variant, the actuator can have a pneumatic control.
The chamber can be filled with a compressible fluid, for example helium, which also has the advantage of not being explosive.
The fluid is brought into the chamber through a supply line 13 that can be closed by a valve 14, a pressure gauge 15 making it possible to monitor the pressure inside chamber 10.
The percussion structure 7 is arranged in the vicinity of block 4 and piston 8 possesses one external surface 16 that is substantially parallel to a receiving surface 17 of block 4.
The priming system according to the invention operates as follows:
When the munition must be made operational, for example, when the munition is mounted on an aircraft, chamber 10 is filled with compressible fluid that is brought to the desired operating pressure.
The fluid may be put into place in chamber 10 by the aircraft pilot shortly before the munition is fired.
The control device is programmed by placing into the memories of the control device the various desired parameters: arming safety distance, operating mode (percussion, proximity, chronometric), and self-destruct timing.
When the control device intakes the explosive pins, piston 8 is no longer integral with chamber 10. The piston 8 is pushed by the pressure of the fluid and strikes receiving surface 17 of block 4.
The shock wave received by block 4 is transmitted to lining 6, that deforms and produces a jet of material that projects onto explosive charge 2 and initiates explosive charge 2.
In the event the lining is absent, it is the constituent material of the block itself that deforms at the cavity and produces the jet.
The physical phenomenon involved is analogous to that observed when a shaped-charge jet forms. In this case the inert block 4 plays the part of an explosive charge on which a lining is placed.
The energy developed by the jet is less than that utilized in shaped charges comprising a block of explosive, but it is still sufficient to allow initiation of an explosive charge.
As an example, a charge of the Octogene (homocyclonite)/TATB type can be initiated by an aluminum jet having a velocity of 6000 m/s. A jet of this kind can be produced with a 0.5 kg cylindrical block (diameter 60 mm, height 50 mm) of titanium that is struck by a piston having an energy of 60 kJ. It is easy to obtain such an energy by using a chamber filled with a fluid at a pressure of 100 MPa.
The individual skilled in the art will be able to dimension the various elements of the priming system according to the invention depending on the energy necessary to initiate the explosive charge.
It should thus be noted that the priming system according to the invention does not utilize any priming explosive. The only pyrotechnic elements include the explosive pins, but the energy that they develop is insufficient in itself to allow initiation of explosive charge 2. In addition, block 4 then acts as a protective screen, isolating the explosive charge from any spatter that might come from the pins.
The energy allowing initiation is provided by the pressurized fluid, but the pressurized fluid is not placed into the chamber 10 until the moment the munition is used.
Note, therefore, that while the munition is stored, chamber 10 is empty. In this case initiation of the explosive pins cannot lead to that of the explosive charge.
Specifically, the pins would then release the piston, which would not be pushed by the fluid and therefore cannot impact against block 4 to cause formation of a jet.
If an attempt is then made to fill chamber 10 with fluid, because piston 8 is no longer integral with the chamber it is not possible to produce the pressure necessary for proper operation of the priming system.
Failure of the piston will then be evidenced by the leakage of fluid that will flow toward the outside of the munition through one or more openings 18 provided for this purpose.
The priming system according to the invention thus makes it possible to achieve a very high level of safety.
The invention also makes it possible, in a simple and reliable manner, to ensure priming of low-sensitivity explosives such as composite explosives, for example octogene(homocyclobite)/polyurethane or hexogene(cyclonite)/polybutadiene mixes.
The invention also makes it possible to define a modular priming system that is easily adaptable to various types of charge. All that is necessary, for example, is to modify the working pressure of the fluid to produce a different impact energy and an initiation power that is also different, but without modifying the various elements constituting the system.
As a variant, it is possible to use as percussion structure for the block various pyrotechnic modules integral with the receiving surface of the block.
Such modules would be selected so that the energy delivered by only one was insufficient to produce formation of a jet capable of initiating the explosive charge.
They would also be selected so that it was necessary to initiate all the pyrotechnic modules simultaneously to ensure formation of a jet and detonation of the charge.
An appropriate electronic control device would ensure simultaneous initiation at the desired moment.
This therefore ensures an excellent level of safety, because a single pyrotechnic module is insufficient to initiate the charge. The module is moreover isolated from the charge by the screen including the block material.
|
A priming system includes a block made of pyrotechnically inert material having on one of its surfaces a cavity placed facing an explosive charge. Structure for allowing percussion of the block is mounted at a receiving surface substantially parallel to a surface where the cavity is located. The priming system can thus be completely devoid of pyrotechnic components.
| 5
|
PRIOR APPLICATION
This application is a U.S. national phase application that is based on and claims priority from International Application No. PCT/SE2011/051317, filed 4 Nov. 2011.
FIELD OF THE INVENTION
The present invention relates to a method for preparation of white liquor in a chemical recovery process of the kraft process. It affects the total system lay out of the causticizing process between input of raw green liquor and final production of a clear white liquor.
BACKGROUND OF THE INVENTION
The causticizing process has conventionally used a lot of different process steps for;
reception of the green liquor; separation of dregs from green liquor; washing and drying dregs obtained from the previous separation step; mixing of clear green liquor and burnt lime in order to slake lime and start the causticizing reaction; tanks for completion of the causticizing reaction; separation of lime mud from white liquor; lime mud washing and drying.
A typical conventional causticizing process is shown in FIG. 1 . The raw green liquor RGL is first received in an equalizing tank EQT and from there pumped to a first green liquor separation process, here shown as a green liquor pressurized disc filter GLF. The green liquor filter separates dregs from the raw green liquor and produces clear green liquor which is sent to a green liquor storage tank GLT. The clear green liquor is then sent, most often via a green liquor cooler GLC, to the slaker SL where burnt lime is mixed into the green liquor. The cooler is needed to reduce temperature ahead of the slaker to keep the slurry in the slaker under boiling point as the reactions occurring in and after the slaker are exothermic. Grits, i.e. unreacted fractions of the burnt lime, are also separated out from the slaker. After mixing in the slaker, the slurry is sent to a series of causticizing vessels CT 1 -CT 2 -CT 3 , often named the causticizing train, wherein the chemical causticizing reactions are completed. Once these causticizing reactions are completed, the slurry is pumped to a white liquor separation process, here shown as white liquor pressurized disc filter WLF. The white liquor filter separates lime mud from the caustiziced liquor and produces clear white liquor, which is sent to a white liquor storage tank WLT. The clear white liquor is then sent directly to be used in the kraft cooking or bleaching line, or alternatively via a polysulfide modification process to said kraft cooking. The lime mud, which still may have a residual content of alkali, is sent to a lime mud washing and drying stage, here shown as a lime mud pressurized disc filter LMF.
Once the lime mud is washed and dried it may be passed to the lime kiln in order to convert it to burnt lime to be used in the slaker again.
In these conventional causticizing processes as shown in FIG. 1 , a specific start up procedure for the green liquor separation process has been used. During start up, the green liquor filter has initially been filled with causticizised liquor from the causticizing train CT 1 -CT 2 -CT 3 in order to build up a precoat of lime mud on the surface of the filter cloth. The reason for this formation of lime mud precoat is that this precoat exhibit a far better separation efficiency than the cloth itself and has a better filterability than would a precoat formed by dregs from green liquor. The filterability improves by a factor of 6 if a precoat is formed by lime mud instead of green liquor mud (dregs). However, this short establishment of the precoat using causticizised liquor from the causticizing train CT 1 -CT 2 -CT 3 has never been used for longer periods than about 5% of the total cycle time of the green liquor filter, and as soon as this precoat has been formed, the major part of the operating time for the green liquor filter has been used for green liquor filtering, and the main part of the white liquor produced, typically more than 90% of the total amount, is obtained from the dedicated white liquor filter.
However, usage of pressurized disc filters, one for white liquor filtration and one for green liquor filtration, are expensive as the costs for these filters are high. Filtering techniques are often better as cleaner product liquors could be obtained with small amounts of suspended solids in the product liquors, typically with content less than 20 ppm, as compared with typical green liquor having more than 1500 ppm. Another advantage is that dregs or lime mud separated from these filters could be obtained at very high dryness in the range 40-60% and 60-75% respectively. Alternative techniques has therefore been considered, and usage of conventional settling tanks for green liquor has once again been considered simply due to less investment costs, even though the amount of suspended solids often are much higher, typically four times more.
Another problem with these conventional processes is that so many different and dedicated separation apparatuses are needed, requiring a lot of free building area. This will be problematic when trying to increase capacity of the causticizing plant, as most often no available room is at hand for additional apparatuses increasing the capacity.
SUMMARY OF THE INVENTION
The invention is based upon the surprising finding that using a common separation process apparatus for white and green liquor separation will maintain a very efficient green liquor separation process as of reduced content of suspended solids, low residual alkali in dregs separated as well as high dryness in dregs. There is thus no need for a multitude of dedicated separation processes for white and green liquor.
The present invention also shows a method for simplification of the recausticizing process using far less separation apparatuses and thus may provide a solution for increasing capacity in any given available area not having the possibility of increasing the building area of the causticizing plant.
Another objective is to reduce the risk for down time. Normally the MTBF (mean time between failures) for the causticizing process will increase as the numbers of apparatuses needed in sequence in the process flow are decreased.
The invention will enable replacement of two separate and dedicated separation processes for white- and green liquor separation with only one separation process used for both the entire white- and green liquor separation. The new separation apparatus will have a slightly larger footprint area than one of the previously used separation apparatuses, but require far less foot print area than the two previous separation apparatuses put together. Even though buffer tanks preceding the common separation apparatus will increase in size, would the net foot print area be reduced in the system.
The method according to the invention is intended for preparation of white liquor in a chemical recovery process of the kraft process. Here the raw green liquor is first fed to a green liquor separation process wherein dregs are separated out and clear green liquor is obtained. Thereafter burnt lime is added to the clear green liquor in a slaker, followed by a causticizing train with a number of causticizing vessels wherein the causticizing process is finished producing causticized liquor. Thereafter the causticized liquor is sent to a white liquor separation process wherein lime mud is separated out and a clear white liquor is obtained to be used as cooking liquor in the kraft process either in form of the clear white liquor or as modified by polysulfide modification in a polysulfide process. The separated lime mud is sent to a lime mud washing and drying process before feeding the washed lime mud to a lime kiln. In this type of process the method is characterized in that the green liquor separation process and the white liquor separation process takes place in the same common filter apparatus with no dedicated green liquor separation apparatus nor any dedicated white liquor separation apparatus, and where the white liquor separation process and the green liquor separation process are conducted in sequence in the same filter apparatus and where the white liquor separation process has a part of the cycle time in the range 20-50% of the total cycle time in the same filter apparatus.
In order to maintain the flexibility of the process the method is further characterized in that an equalizing buffer tank is preceding the green liquor separation process and where the equalizing buffer tank has a storage capacity holding raw green liquor for at least 5 hours in said equalizing buffer tank, and where a last buffer tank in the causticizing train has a storage capacity holding a causticized liquor for at least 2 hours in said last buffer tank in the causticizing train. With this embodiment could the causticizing process be maintained even in case of any interruption in the dissolving tank (where green liquor is formed) or any interruption in the causticizing reaction process following the slaker operation.
In order to further improve the flexibility of the process, the method is further characterized in that the equalizing buffer tank is filled with raw green liquor while emptying the buffer tank in the causticizing train when performing the white liquor separation in the common filter apparatus, and thereafter emptying the equalizing buffer tank of raw green liquor while filling the buffer tank in the causticizing train when performing the green liquor separation in the common filter apparatus. By this alternating filling and emptying the buffer tanks the separation process can be in continuous operation producing the necessary volumes of both separated green and white liquors.
In order to use the buffer tanks as much as possible the method is further characterized in that the level of liquors in the buffer tanks are controlled within 20-95% of the total retention capacity during white and green liquor separation. A certain minimum content of liquor is needed to maintain a stabilizing volume in the equalizing tank as well as a minimum level for agitation in the buffer tank, and filling of buffer tanks should not reach a full 100% filling degree which may risk overflow of liquors and special handling actions for such overflow.
In order to improve formation of an optimal lime mud precoat with a minimum of residual dregs content, which content of dregs may reduce filterability, is the method further characterized in that the green liquor separation process in said common filter apparatus is ended by a complete emptying of raw green liquor and addition of an intensified wash out process using a volume of washing liquid of at least 5% of the liquor volume held in the common filter apparatus, said washing liquid not containing any dregs or lime mud particles, said intensified wash out process also entailing intense agitation in the liquid volume held in the common filter apparatus. In this context it would be beneficial for the volume of washing liquid used during the intensified wash out process to exceed 3 m 3 in most typical processes having a capacity of over 5300 m 3 green liquor per day and over 5000 m 3 white liquor per day. The wash liquid should be clean in such aspects that any content of dregs are less than 1/100 of the content in the green liquor to be filtered.
According to one further aspect of the inventive method is also a cake of precoat maintained on the filter surface during the intensified wash out process. The wash out process ending each cycle after green liquor separation is intended to flush out the vat of the separating apparatus with the objective to flush out any dregs accumulated in the vat, while maintaining the precoat so that the following white liquor separation process could start immediately after termination of the wash out process.
According to yet a further embodiment of the inventive method is also a total removal of the precoat on the common filter apparatus including a filter cloth wash activated after two or more green liquor separation cycles and wherein a total new precoat is established in subsequent white liquor separation process in said common filter apparatus. In some cases could as many as up to 3-4 green liquor separation cycles be performed in sequence, interrupted by white liquor separation cycles in between, before a total removal of the precoat is activated. The number of green liquor cycles possible is dependent on the current status of the green liquor or the causticized white liquor as of impurities and is very much specific for each mill and current type of kraft pulping operation.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic representation of a conventional causticizing process;
FIG. 2 is a schematic representation of the causticizing process according to the invention;
FIG. 3 is showing the liquor flows during the white liquor cycle according to the invention;
FIG. 4 ; is showing the liquor flows during the green liquor cycle according to the invention;
FIG. 5 ; is showing a typical sequence with white- and green liquor cycles according to the invention;
FIG. 6 ; is showing the usage in buffer tanks during green and white liquor cycles according to the invention;
FIG. 7 ; is showing precoat removal on filter surfaces of the common filter apparatus;
FIG. 8 ; is showing a typical disc filter apparatus preferably used for the common filter apparatus.
DETAILED DESCRIPTION OF THE INVENTION
The inventive method is described in connection with a system set up as shown in FIG. 2 . In here is one single common filter apparatus GLF/WLF used for the green and white liquor cycles.
The raw green liquor RGL is first received in an equalizing tank EQT and from there pumped to the green liquor separation process when the feed valve for green liquor FV GL is open and the feed valve for white liquor FV WL is closed (black valves indicate closed status). The separation process is here shown implemented in a pressurized disc filter GLF/WLF. The common filter apparatus GLF/WLF now operating as a green liquor filter separates out dregs from the raw green liquor and produces clear green liquor sent to a green liquor storage tank GLT when the output valve for green liquor OV GL is open and the output valve for white liquor OV WL is closed. The clear green liquor is then sent, most often via a green liquor cooler GLC, to the slaker SL where burnt lime is mixed into the green liquor. The cooler is needed to reduce temperature to well below boiling point as the reactions occurring in and after the slaker are exothermic. Grits, i.e. unreacted components from the burnt lime, are also separated out from the slaker. After mixing in the slaker the mixture is sent to a series of causticizing vessels CT 1 -CT 2 -CT 3 , often named the causticizing train, wherein the chemical causticizing reactions are completed. As the feed valve for white liquor FV WL is closed the vessels CT 1 -CT 2 -CT 3 , preferably only the last vessel CT 3 , are used as storage vessels for the causticizised liquor when the common filter apparatus GLF/WLF is used as a green liquor filter during the green liquor cycle.
When the storage vessel CT 3 is reaching the upper storage capacity limit, the common filter is switching to white liquor filtration. During the white liquor filtration the feed valve for green liquor FV GL is closed and the feed valve for white liquor FV WL is opened, while the output valve for green liquor OV GL is closed and the output valve for white liquor OV WL is opened. During the white liquor cycle the liquid is pumped from storage vessel CT 3 to a white liquor separation process in the common filter apparatus GLF/WLF, here shown as a white liquor pressurized disc filter. During the white liquor cycle the filter separates out lime mud from the caustiziced liquor and produces clear white liquor sent to a white liquor storage tank WLT. The clear white liquor is then sent directly to be used in the kraft cooking or bleaching line, or alternatively via a polysulfide modification process to said kraft cooking. The lime mud, which still may have a residual content of alkali, is sent to a lime mud washing and drying stage, here shown as a lime mud pressurized disc filter LMF. Once the lime mud is washed and dried it may be passed to the lime kiln in order to convert it to burnt lime to be used in the slaker again.
In FIG. 3 only the flows during the white liquor cycle are shown when operating the common filter apparatus GLF/WLF. This cycle is preferably initiated during 1.5-2 hours, during which the equalizing tank EQT for receiving raw green liquor RGL is only used as buffering tank, i.e. with no outflow of any raw green liquor. As no filtered green liquor is produced, the green liquor tank GLT is in an emptying process, feeding clear green liquor to the slaker and onwards via the causticizing train CT 1 -CT 2 -CT 3 to the common filter apparatus GLF/WLF. The resulting filtered white liquor is fed from the common filter apparatus GLF/WLF to the white liquor tank WLT.
In FIG. 4 only the flows during the green liquor cycle are shown when operating the common filter apparatus GLF/WLF. This cycle is preferably initiated during 2.5-3 hours, during which the causticizing train CT 1 -CT 2 -CT 3 for receiving causticizised liquor is only used as buffering tank, i.e. with no outflow of any causticizised liquor. As no filtered white liquor is produced, the white liquor tank WLT is in an emptying process, feeding clear white to the cooking or bleaching process in the kraft pulping process. Raw green liquor RGL is fed from the equalizing tank EQT to the common filter apparatus GLF/WLF. The resulting filtered green liquor is fed from the common filter apparatus GLF/WLF to the green liquor tank GLT.
In FIG. 5 are shown a number of white and green liquor cycles in sequence operated according to the inventive method. Typically within a 10 hour total cycle there are preferably a first white liquor cycle during 1.8 hours followed by a first green liquor cycle during 2.8 hours, and repeated with a subsequent second white liquor cycle during 1.8 hours followed by a second green liquor cycle during 2.8 hours. After the white liquor cycles there are preferably only an emptying of the common filter apparatus GLF/WLF from causticizised white liquor during the time interval A. But after the green liquor cycles there are preferably not only an emptying of the common filter apparatus GLF/WLF from raw green liquor during the time interval B, but also an improved addition of an intensified wash out process using a volume of washing liquid of at least 5% of the liquor volume held in the vat of the common filter apparatus during filtering. As indicated before, the washing liquid should not contain any larger amounts of dregs, as the objective is to flush out any dregs that may have settled into the vat of the filter apparatus, whose presence may have a negative impact during the start of the white liquor cycle and formation of a precoat with only lime mud on the filter cloth of the filtering apparatus. If any dregs are still kept in the common filtering apparatus when filling it up with causticized liquor, these dregs residuals may be suspended in the causticized liquor and then remain in the precoat formed, thus reducing the filtering capacity. In order to flush out any dregs should preferably also said intensified wash out process be complemented by intense agitation in the liquid volume held in the common filter apparatus. This could be implemented by any intense recirculation inside the vat of the common filtering apparatus or adding the washing liquid trough so called mammoth pumps located in the bottom area of the vat. The mammoth pumps are during filtering operations fed with pressurized air in order to prevent settling in the vat, and looks like an educator nozzle that is driven by the air flow and which induce a suction effect around the nozzles at the bottom wall of the vat.
As indicated in FIG. 5 is also a total renewal of the precoat including a thorough cloth wash implemented after a last green liquor cycle, here indicated as a 30 minutes cloth wash.
In FIG. 6 are shown how the equalizing tank EQT and the last tank CT 3 in the causticizing train CT 1 -CT 2 -CT 3 are used as buffer tanks during the white liquor cycle (left hand part of figure) and the green liquor cycle/right hand side of figure). During the white liquor cycle the liquid level in the equalizing tank EQT is rising from a level of 20% and up to about 95%, while the liquid level in CT 3 is dropping from a level of 95% and down to about 20%. In the subsequent green liquor cycle the opposite effect occurs, i.e. the liquid level in the equalizing tank EQT is dropping from a level of 95% and down to about 20%, while the liquid level in CT 3 is rising from a level of 20% and up to about 95%.
In FIG. 7 is shown a filter disc section used in a disc filter apparatus as shown in FIG. 8 . Knives located on each side of the rotating disc, are scraping off an outer layer of the precoat. In FIG. 7 is shown the principle constitution of the precoat after a green liquor cycle, where an outermost layer of dregs has been caught on top of the lime mud base precoat. The knives advance a little bit into the lime mud base precoat and create a clean lime mud surface for the following white liquor cycle. During the white liquor cycle the knives are retracted allowing the lime mud base precoat to build up again in thickness.
In a preferred mode of operation, the knives are located about 12 mm from the filter cloth during start of WL filtration and is retracted to position about 22 mm when a precoat of lime mud is built up on the filter cloth. At the end of the WL filtration period a lime mud precoat with a thickness of 22 mm is thus established. When GL filtration is started, the knives are successively moved towards the filter cloth and when reaching a distance of 12 mm the GL filtration stops. WL filtration starts by moving the knives to a distance of 10 mm in order to expose a fresh lime mud precoating and rebuilding a new lime mud precoat with 22 mm thickness.
In a test of the inventive method using a cycle sequence as shown in FIG. 5 , the total cycle time was about 619 minutes (the “10 h” in figure). In this total cycle the WL filtration was about 230 minutes, i.e. 37% of the total cycle, and the GL filtration about 330 minutes, i.e. 53% of the total cycle. The rest of the total cycle, about 10%, is non productive time (A, B and 30 min cloth wash in FIG. 5 ). In the test a common filter apparatus was used with a pressurized disc filter, see FIG. 8 , having a total filter area of 280 m 2 and a vat holding some 55 m 3 liquor to be filtered, producing 5 100 m 3 WL/day and 5 350 m 3 GL/day.
While the present invention has been described in accordance with preferred compositions and embodiments, it is to be understood that certain substitutions and alterations may be made thereto without departing from the spirit and scope of the following claims.
|
The method is for preparation of white liquor in a chemical recovery process of the kraft process. The green liquor separation process and the white liquor separation process are taking place in the same common filter apparatus with no dedicated green liquor separation apparatus or any dedicated white liquor separation apparatus. The white liquor separation process and the green liquor separation process are conducted in sequence in the same filter apparatus. The white liquor separation process has a part of the cycle time in the range 20-50% of the total cycle time in the same filter apparatus.
| 3
|
CROSS REFERENCE TO RELATED APPLICATIONS
This is a U.S. national stage application of International Application No. PCT/JP2009/051088, filed on 23 Jan. 2009. Priority under 35 U.S.C. §119(a) and 35 U.S.C. §365(b) is claimed from Japanese Application No. JP2008-084551, filed 27 Mar. 2008, the disclosure of which is also incorporated herein by reference.
TECHNICAL FIELD
The present invention generally relates to a manufacturing of a semiconductor device, specifically, to a method for a film formation by the decomposition of a gas-state base material and a film forming apparatus.
BACKGROUND
In today's semiconductor integrated circuits, the diameter of the via plug formed with copper (Cu) inside of an insulating film between layers is reduced from 65 nm to 45 nm along with the miniaturization. It is expected that the diameter of the via plug will be further reduced to 32 nm or 22 nm in recent future.
As the semiconductor integrated circuits are miniaturized, it is difficult to form a barrier metal film or a Cu seed layer by the conventional PVD method in a miniaturized via hale or a wiring groove in view of the step coverage. Accordingly, a film forming technology by the MOCVD method or the ALD method is studied in which an improved step coverage can be realized at a low temperature that does not damage the insulating film between layers formed with a low dielectric material (low-K material).
However, the MOCVD method and the ALD method generally use an organic metal as a base material where metal atoms are combined with an organic group. As a result, impurities tend to reside in the formed film, and thus, the quality of the film is not stable even if the step coverage looks satisfactory. For example, when a Cu seed layer is formed on a metal film of Ta barrier by the MOCVD method, the formed Cu seed layer tends to generate a condensation thereby making it difficult to form a Cu seed layer that stably covers the Ta barrier film with a uniform film thickness. When an electrolysis plating is performed using the seed layer that generated the condensation as an electrode, potential defects may be included in the Cu layer charged at the wiring groove or the via hole. As a result, problem occurs such as the increase of the electric resistance as well as the electro-migration tolerance or a deterioration of the stress-migration tolerance.
Thus, a method has been recently suggested where a barrier metal film or a Cu seed layer is formed directly on the insulating film between layers by the MOCVD technology of a metal film using a metal carbonyl base material. Metal carbonyl base material is readily dissociated at a relatively low temperature to form a metal layer, and the CO, which is the ligand of metal carbonyl base material, does not reside in the formed film and immediately discharged to outside of the film forming reaction system. As a result, the barrier metal film or the Cu seed layer can be formed with a good quality having extremely low impurities. Using this method, a W film can be formed using, for example, W(C) 6 , as a barrier metal layer, or a ruthenium (Ru) film can be formed using, for example, Ru 3 (CO) 12 , as the Cu seed layer.
SUMMARY
Problems to be Solved by the Invention
In the mean time, since the metal carbonyl base material has a characteristic that can be easily dissociated at a relatively low temperature, a technology has been proposed where the carbon monoxide gas is supplied as a carrier gas to suppress the dissociation of the base material during the transport of the base material (base material supply system). It is known that the carbon monoxide has an effect to suppress the dissociation.
For example, in the technology that forms an Ru film as a Cu seed film, Ru carbonyl base material such as Ru 3 (CO) 12 is supplied to the base material supply system using CO gas as a carrier gas to suppress the dissociation of the Ru carbonyl base material during the transport procedure.
FIG. 1 illustrates the constitution of a film forming apparatus 10 , according to the above-described relevant technology.
Referring to FIG. 1 , film forming apparatus 10 is exhausted by an exhaust system 11 , and includes a processing chamber 12 equipped with a substrate holding plate 13 that holds a substrate to be processed W. A gate valve 12 G is formed at process chamber 12 allowing the substrate to be processed W passes through.
A heater is embedded in substrate holding plate 13 , and the substrate to be processed W is maintained at a desired process temperature by driving the heater through a driving line 13 A.
Exhaust system 11 is formed with a turbo molecular pump 11 A and a dry pump 11 B connected serially, and nitrogen gas is supplied to turbo molecular pump 11 A via a valve 11 b . A variable conductance valve 11 a is provided between process chamber 12 and turbo molecular pump 11 A to maintain the entire pressure of process chamber 12 being constant. Also, in film forming apparatus 10 of FIG. 1 , an exhaustion path 11 C is provided configured to bypass turbo molecular pump 11 A for a rough vacuum of process chamber 12 by dry pump 11 B, a valve 11 c is provided in exhaustion path 11 C and another valve 11 d is provided at the downstream side of turbo molecular pump 11 A.
In process chamber 12 , a film forming base material is supplied with a gas state via a gas introducing line 14 B from a base material supply system 14 that includes a base material container 14 A.
In the illustrated embodiment, Ru 3 (CO) 12 which is the carbonyl compound of Ru is maintained in base material container 14 A, and the CO gas is provided as a carrier gas via bubble ring gas line 14 a that includes MFC (a mass flow controller). As a result, evaporated Ru 3 (CO) 12 raw gas is supplied to process chamber 12 as a carrier gas that contains the raw gas and CO carrier gas via gas introduce line 14 B and shower head 14 S, along with the CO carrier gas from line 14 d that includes line MFC 14 c.
Also, in the constitution of FIG. 1 , along with valves 14 g , 14 h and MFC 14 e , a line 14 f is provided that supplies inert gas such as Ar, and the inert gas is added to Ru 3 (CO) 12 raw gas supplied to process chamber 12 via line 14 B.
Also, in film forming apparatus 10 , a controller 10 A is provided to control process chamber 12 , exhaust system 11 and base material supply system 14 .
Also, the formation of Ru film on the substrate to be processed W is performed by Ru 3 (CO) 12 →3Ru+12CO which is the dissociation reaction of the Ru 3 (CO) 12 base material.
The reaction proceeds toward the right side when the partial pressure of the CO gas existing in the film forming reaction system is low. As a result, the reaction proceeds instantly as soon as the CO gas is exhausted outside of process chamber 12 thereby deteriorating the step coverage of the formed film. Due to this, the inside of process chamber 12 is maintained with a high concentration CO gas atmosphere to prevent an excessive reaction of the dissociation (Patent Literature 2).
However, the inventor of the present invention discovered that when film forming apparatus 10 having a conventional shower head 14 S is used as shown in FIG. 1 , the deposition rate of the Ru film becomes non-uniform on the substrate W to be processed as shown in FIG. 2 . More specifically, the deposition rate is higher at the center of the substrate than the periphery portion so that a distribution profile is generated regarding the deposition rate in the surface. Accordingly, as shown in FIG. 3 , it has been discovered that the Ru film formed on the substrate to be processed W has a film thickness profile in which the thickness is thicker at the center of the substrate to be processed W and thinner at the periphery portion, and the variation of the film thickness in the surface reaches up to 15%.
It is noted that the results of FIG. 2 and FIG. 3 are based on a case where an approximately cylindrical processing chamber having an inner diameter of 505 mm is used as process chamber 12 , a silicon wafer W having a diameter of 300 mm is held on substrate holding plate 13 as the substrate to be processed W, the distance between shower head 14 S and the substrate to be processed W is set to be 18 mm, Ru 3 (CO) 12 gas is supplied with a flow rate of 1 sccm˜2 sccm as a source gas along with CO carrier gas with a flow rate of 100 sccm, and the Ru film is formed at 190° C. of substrate temperature.
Therefore, a technology is required to suppress the deposition rate distribution profile in the surface or film thickness distribution profile in the surface.
Patent Literature 1: Japanese Laid-Open 2002-60944 Patent Literature 2: Japanese Laid-Open 2004-30401
Means to Solve the Problems
According to an aspect, the present invention provides a film forming method characterized by forming a metal film on the surface of the substrate to be processed. In the method, a process gas including a raw gas containing metal carbonyl and a carrier gas containing carbon-monoxide flows to the region of an upper-outer side of the diameter direction than the outer periphery of the substrate to be processed while avoiding the surface of the substrate to be processed, and the metal carbonyl is diffused into the surface of the substrate to be processed by the flow of the process gas to form the metal film.
According to another aspect, the present invention provides a film forming apparatus characterized by including a substrate holding plate that supports a substrate to be processed, a process chamber that defines a process space along with the substrate holding plate, and an exhaust system that exhaust the process space at the upper-outer side of the diameter direction of the substrate holding plate. The film forming apparatus further includes a process gas supply unit provided at the process chamber to face the substrate holding plate to supply the process gas formed with the raw gas and carrier gas to the process space. In particular, a process gas introduce unit is provided at the process gas supply unit in such a way that the process gas flows at the upper-outer side of the diameter direction than the substrate to be processed on the substrate holding plate when the substrate holding plate is viewed from a vertical direction, to the exhaust system in the process space while avoiding the substrate to be processed.
According to yet another aspect, the present invention provides a computer-readable medium characterized by storing the software that, when executed by a general purpose computer, controls a film forming apparatus. The film forming apparatus includes a substrate holding plate that supports a substrate to be processed, a process chamber that defines a process space along with the substrate holding plate, and an exhaust system that exhaust the process space at the upper-outer side of the diameter direction of the substrate holding plate. The film forming apparatus further includes a process gas supply unit provided at the process chamber to face the substrate holding plate to supply the process gas formed with the raw gas and the carrier gas to the process space. In particular, a process gas introduce unit is provided at the process gas supply unit in such a way that the process gas flows at the upper-outer side of diameter direction than the substrate to be processed on the substrate holding plate when the substrate holding plate is viewed from a vertical direction, to the exhaust system in the process space while avoiding the substrate to be processed. Moreover, the process gas supply unit is provided with metal carbonyl base material as the process gas and carbon-monoxide as a carrier gas, and the general purpose computer controls the temperature of the substrate holding plate to be lower than the temperature at which the carbon-monoxide suppresses the dissociation of the metal carbonyl.
Effects of the Invention
According to the present invention, it is possible to suppress the thickness variation of the formed film in the surface by flowing the process gas which includes a process gas and a carrier gas to the space of an upper-outer side of the diameter direction than the outer periphery of the substrate to be processed while avoiding the substrate to be processed, and performing the film formation on the surface of the substrate to be processed by diffusing the chemical species of the process gas into the surface of the substrate to be processed from the flow of the process gas.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of a CVD apparatus having a shower head used for a conventional film forming of an Ru film.
FIG. 2 is a graph that explains the project of the present invention.
FIG. 3 is a graph that explains the project of the present invention.
FIG. 4 illustrates a conventional film formation of the Ru film using the shower head.
FIG. 5 is a graph illustrating the pressure distribution and the moving fluid speed distribution of the process gas in the surface that occurs during the film formation of FIG. 4 .
FIG. 6 illustrates base material distribution and film thickness distribution in the surface generated during the film formation of FIG. 4 .
FIG. 7 illustrates the outline of the film formation of the Ru film according to the present invention.
FIG. 8 illustrates the outline of the film formation of the Ru film according to the present invention.
FIG. 9 illustrates the outline of the film formation of the Ru film according to the present invention.
FIG. 10 illustrates the outline of the film formation of the Ru film according to the present invention.
FIG. 11 a is a schematic diagram of a film forming apparatus according to a first embodiment of the present invention.
FIG. 11 b is a schematic diagram of a film forming apparatus according to a first embodiment of the present invention.
FIG. 11 c is a schematic diagram of a film forming apparatus according to a first embodiment of the present invention.
FIG. 12 a is a graph illustrating the uniformity of the deposition rate in the surface during the film forming of the Ru film according to the first embodiment.
FIG. 12 b is a graph explaining the measurement of FIG. 12 a.
FIG. 13 is a graph illustrating the size effect of a baffle plate in the film forming apparatus of FIG. 11 a through FIG. 11 c.
FIG. 14 is a graph illustrating the temperature dependence of the dissociation suppression effect of the Ru carbonyl base material in the carbon monoxide atmosphere.
FIG. 15 is a graph illustrating the relationship between the uniformity of the Ru film thickness deposited on the substrate to be processed at various temperatures and the substrate temperature.
FIG. 16 is a graph illustrating the variation of the Ru film forming speed according to the temperature changes of the base material chamber.
FIG. 17 is a graph illustrating the variation of the Ru film forming speed according to the gas flow rate changes of the CO carrier gas.
FIG. 18 illustrates a modified example of the first embodiment.
FIG. 19 illustrates another modified example of the first embodiment.
FIG. 20 is a schematic diagram of a film forming apparatus according to a second embodiment.
FIG. 21 is a first diagram illustrating a film forming procedure using the film forming apparatus of FIG. 20 .
FIG. 22 is a second diagram illustrating a film forming procedure using the film forming apparatus of FIG. 20 .
FIG. 23 is a third diagram illustrating a film forming procedure using the film forming apparatus of FIG. 20 .
FIG. 24 is a fourth diagram illustrating a film forming procedure using the film forming apparatus of FIG. 20 .
FIG. 25 is a fifth diagram illustrating a film forming procedure using the film forming apparatus of FIG. 20 .
FIG. 26 a sixth diagram illustrating a film forming procedure using the film forming apparatus of FIG. 20 .
FIG. 27 is a seventh diagram illustrating a film forming procedure using the film forming apparatus of FIG. 20 .
FIG. 28 is an eighth diagram illustrating a film forming procedure using the film forming apparatus of FIG. 20 .
DETAILED DESCRIPTION OF EMBODIMENTS
Inventors of the present invention investigated, as a research on which the present invention is based, the cause of the non-uniformity of the deposition rate and film thickness in the surface as shown in FIG. 2 or FIG. 3 in film forming apparatus 10 using the shower head illustrated in FIG. 1 by examining the moving fluid speed simulation, and obtained the following information.
FIG. 4 illustrates the simulation results of the moving fluid speed distribution of the process gas flow that occurs in the process space between shower head 14 S and the substrate to be processed W when the Ru film is deposited by film forming apparatus 10 of FIG. 1 by supplying the process gas mentioned above from the shower head to the surface of the substrate to be processed using the conventional shower head having the same discharge holes formed at a surface that faces the substrate to be processed while exhausting from the exhausting system formed at the outer periphery of substrate holding plate 13 . Also, in the simulation results of FIG. 4 , the lighter portion represents the gas concentration, and, accordingly represents the portion where the pressure is high. In FIG. 4 , while the gas flow rate at each point is represented as a tiny arrow, the process gas pressure and the distribution of the moving fluid speed in the surface of the substrate to be processed W are represented as a graph in FIG. 5 since it is difficult to represent in FIG. 4 due to the resolution.
Referring to FIG. 4 , when the gas is discharged from shower head 14 S to stage 13 , that is, when the gas is discharged from gas discharge holes 14 s equally formed at the side of shower head 14 S that faces the substrate to be processed W disposed on substrate holding plate 13 , the discharged gas flows along the surface of the substrate to be processed to the exhaustion system of the outer periphery with a high speed. At that time, as indicated with the dotted line in the figure, the gas pressure is slightly higher near the center of the shower head to which the gas is provided from line 14 B as shown in FIG. 5 . Also, the moving fluid speed of the process gas toward the outer periphery direction is slow at the center of the substrate to be processed. As a result, as shown in FIG. 6 , the concentration of the base material becomes higher near the center portion of the substrate to be processed W, and corresponding to this, the film thickness is increased at the center portion of the substrate to be processed W thereby generating the film thickness distribution as shown in FIG. 2 .
Meanwhile, a gas flow is formed on the surface of the substrate to be processed W along the diameter direction to the outer periphery and the moving fluid speed is increased toward the outer periphery of the substrate to be processed W, which can be known from FIG. 4 and FIG. 5 . In the simulation of FIG. 4 or FIG. 6 , a wafer having a diameter of 300 mm is used as a substrate to be processed, and shower head 14 S with a diameter of 370 mm has discharge holes 14 s with a diameter of 6.5 mm spaced equally with 13.8 mm intervals. Also, the distance between shower head 14 S and the substrate to be processed W is set to be 18 mm, and the gas is supplied to the shower head with the flow rate of 100 sccm.
Based on the above knowledge, the inventors of the present invention conceived the formation of the Ru film on the substrate to be processed W as shown in FIG. 7 , in which process gas supply member 24 S, instead of shower head 14 S, having a gas discharge opening 24 s as a gas introduction unit at the outer side than the outer periphery of the substrate to be processed W, is used to supply the gas to the outer side than the outer periphery of the substrate to be processed W. Also, a constitution is used that exhausts from an exhaust system (not shown) formed at the outer side than the outer periphery of the substrate to be processed W to form the Ru film on the substrate to be processed W by the chemical species of the process gas diffused from the outer periphery portion to the surface of the substrate to be processed W.
In the constitution of FIG. 7 , the direct supply of the gas to the surface of the substrate to be processed W is blocked by baffle portion 24 B formed at the inner side than opening 24 s of process gas supply member 24 S, and the chemical species diffused from the gas flowing the outer periphery of the substrate to be processed W reaches the surface of the substrate W.
As a result, as roughly illustrated in FIG. 8 , it appears that a uniform base material concentration is formed on the surface of the substrate to be processed W and the Ru film is formed on the substrate to be processed W with the same thickness.
Each of FIG. 9 and FIG. 10 shows the thickness distribution and deposition rate distribution, respectively, of the Ru film in the surface of the substrate when the Ru film is formed with the same film forming apparatus as used in the experiment of FIG. 2 and FIG. 3 but with the discharge holes of shower head 14 S are blocked except for the holes at the most outer 3 rows. It is noted that the results from FIG. 2 and FIG. 3 are overlapped with the results of FIG. 9 and FIG. 10 .
Referring to FIG. 9 , by supplying the process gas to the outer side than the outer periphery of the substrate to be processed W to perform the film formation, it is confirmed that the standard deviation (σ) of the film thickness variation of the Ru film formed on the substrate to be processed W decreased to about 15% to 3% as compared to the case where shower head 14 S having equally formed discharge holes is used, and the maximum thickness difference (Δ) of the surface is decreased from 12.8 Å to 2.8 Å. Likewise, as is clear from FIG. 10 , the deposition rate in the surface is greatly improved as compared to the case where shower head 14 S is used.
First Embodiment
FIG. 11 a illustrates the constitution of film forming apparatus 40 according to the first embodiment of the present invention. Referring to FIG. 11 a , film forming apparatus 40 includes an outside chamber 41 exhausted by an exhaust system (not shown), and an inside process chamber 42 formed at the inside of outside chamber 41 and is provided with an exhaust path 42 A at the outer periphery. Inside process chamber 42 is exhausted via outside chamber 41 . Substrate holding plate 43 is provided at the bottom portion of inner process chamber 42 to support the substrate to be processed W and carries a cover ring 43 A coupled at the periphery portion. Cover ring 43 A is coupled with the lower end portion of the outside wall of inner process chamber 42 , and inner process chamber 42 defines a closed process space 42 S.
Although, process space 42 S is provided with the process gas from process gas supply line 42 D, a baffle plate 42 B is provided in process space 42 S between opening 42 d at inner process chamber 42 of process gas supply line 42 D and the substrate to be processed W on substrate holding plate 43 , as illustrated in FIG. 11 b and FIG. 11 c . The supplied process gas flows to exhaust path 42 A through opening 42 C formed at the periphery of baffle plate 42 B. Here, FIG. 11 b illustrates the plan view of baffle plate 42 B, and FIG. 11 c is a cross-sectional view along the line B-B′ of FIG. 11 b.
Referring to FIG. 11 b and FIG. 11 c , baffle plate 42 B is formed with a flange portion 42 Ba which forms a portion of inner process chamber 42 and a baffle portion 42 Bb supported by a rib 42 Bc. And for baffle portion 42 Bb, flange portion 42 Ba is supported at inner process chamber 42 . Flange portion 42 Ba is provided with screw holes 42 Bd to fix into inner process chamber 42 .
Substrate holding plate 43 includes a baffle plate 43 B which is different from baffle plate 42 B. The process gas exhausted from opening 42 C through exhaust path 42 A flows into the exhaustion system identical to exhaust system 11 of FIG. 1 through opening 43 b inside baffle plate 43 B.
As a result, the desired Ru film is formed by the dissociation from the reaction of the Ru 3 (CO) 12 molecules described above and diffused from the flow of the process gas that passes opening 42 C.
Meanwhile, when process gas supply member 24 S of FIG. 7 is used instead of shower head 14 S in film forming apparatus 10 of FIG. 1 , while the distribution of the thickness and the deposition rate of the formed Ru film in the surface are improved as explained in FIG. 9 and FIG. 10 , the deposition rate is decreased drastically as shown in FIG. 10 .
Therefore, in order to improve the deposition rate without degrading the distribution of the Ru film thickness and the deposition rate in the surface, an experiment has been performed in which the diameter D of baffle plate 42 , the distance between baffle plate 42 B and the substrate to be processed W, the width C of exhaust path 42 A and the width A of opening 43 b formed at baffle plate 43 B are varied to form the Ru film. Exhaust path 42 A and opening 43 b are working as an iris or an aperture inserted into the exhaust system of film forming apparatus 40 . In the experiment, the Ru 3 (CO) 12 raw gas is supplied from process gas supply line 42 D with a flow rate of 1 sccm˜2 sccm along with 100 sccm of CO carrier gas, and the Ru film is formed at 190° C. of substrate temperature.
FIG. 12 a illustrates the experimental results where the horizontal line represents the deposition rate and the vertical line represents the position in the surface of the substrate to be processed W. In FIG. 12 a , the position in the surface of the substrate indicates a position along the A-A′ line of a silicon wafer having a diameter of 300 mm used as a substrate to be processed W.
Referring to FIG. 12 a , “Ref” indicates the experiment of FIG. 10 , and “I” represents a case where a disk type member having a diameter of 200 mm is used as baffle plate 42 B, the distance G is set to be 67 mm, the width C of exhaust path 42 A is set to be 19.5 mm, and the width A of opening 43 b is set to be 77 mm. “II” represents a case where a disk type member having a diameter of 300 mm is used as baffle plate 42 B, the distance G is set to be 67 mm, the width C of exhaust path 42 A is set to be 19.5 mm, and the width A of opening 43 b is set to be 77 mm. “III” represents a case where a disk type member having a diameter of 300 mm is used as baffle plate 42 B, the distance G is set to be 25 mm, the width C of exhaust path 42 A is set to be 19.5 mm, and the width A of opening 43 b is set to be 77 mm. “IV” represents a case where a disk type member having a diameter of 300 mm is used as baffle plate 42 B, the distance G is set to be 67 mm, the width C of exhaust path 42 A is set to be 2 mm, and the width A of opening 43 b is set to be 77 mm. “VI” represents a case where a disk type member having a diameter of 300 mm is used as baffle plate 42 B, the distance G is set to be 67 mm, the width C of exhaust path 42 A is set to be 19.5 mm, and the width A of opening 43 b is set to be 2 mm.
While the average deposition rate is 3.6 Å/min and the standard deviation (σ) of the variation in the surface is 2.8% in the “Ref” experiment, the average deposition rate is 11.1 Å/min and the standard deviation (σ) of the variation in the surface is 11.6% in the experiment “I”. In the experiment “II”, the average deposition rate is 12.4 Å/min and the standard deviation (σ) of the variation in the surface is 5.0%. In the experiment “III”, the average deposition rate is 8.9 Å/min and the standard deviation (σ) of the variation in the surface is 17.7%. In the experiment “IV”, the average deposition rate is 15.0 Å/min and the standard deviation (σ) of the variation in the surface is 5.5%. In the experiment “V”, the average deposition rate is 14.9 Å/min and the standard deviation (σ) of the variation in the surface is 5.7%. In the experiment “VI”, the average deposition rate is 15.5 Å/min and the standard deviation (σ) of the variation in the surface is 5.4%.
Referring to FIG. 12 a , as illustrated in FIG. 11 a , it can be known that the deposition rate is improved by making the conductance of the exhaustion path from processing chamber 42 at exhaust path 42 A and opening 43 b small. Moreover, it can be also known that the distribution of the deposition rate in the surface is improved when the diameter D of baffle plate 42 B is 300 mm which is the same as the diameter of the substrate, rather than 200 mm.
As described above, it is confirmed that the uniformity of the film formation on the substrate to be processed strongly depends on the diameter D of baffle plate 42 B, and the inventors of the present invention investigated the uniformity of the Ru film thickness in the surface obtained when the diameter D of baffle plate 42 B is further increased to 340 mm in film forming apparatus 40 of FIG. 11 a or FIG. 11 c . The results are shown in FIG. 13 where the horizontal line represents the position in the surface along the line A-A′ of FIG. 12 b , and the vertical line represents the standardized thickness of the Ru film at the center portion (substrate inside position=0 mm) of the substrate to be processed W, as in FIG. 12 a.
Referring to FIG. 13 , the uniformity inside the surface is superior when the diameter D of baffle plate 42 B is 300 mm (the standard deviation of the variation of the film thickness is 5.9%) as compared to when the diameter D of baffle plate 42 B is 200 mm (the standard deviation of the variation of the film thickness is 11.6%). Specifically, when the diameter D is changed from 200 mm to 300 mm, the degree of the improvement of the uniformity in the surface is extremely large such that the standard deviation of the film thickness variation in the surface ranges from 11.6% to 5.9%. Accordingly, it can be decided that the improvement of the uniformity of the formation of the Ru film on the substrate to be processed W is more effective when the diameter of the baffle plate 42 B is larger than that of the substrate to be processed W.
However, as described above, in the present invention, the dissociation is suppressed during the transport of the base material by using the CO as a carrier gas during the formation of the metal film by the CVD method using the metal carbonyl base material such as Ru. Also, as in the present embodiment, in a substrate processing apparatus having an apparatus where the metal carbonyl is diffused into the center portion of the substrate to be processed W and the dissociation during the diffusion is suppressed and transported by using the carbon monoxide atmosphere, it is important to maintain the suppression effect of the dissociation of the metal carbonyl during the diffusion by the CO to perform a film formation that has an excellent characteristic of, for example, the step coverage.
FIG. 14 is a graph that illustrates the effect of the substrate temperature with respect to the dissociation suppression effect by the addition of the CO gas to the base material of Ru 3 (CO) 12 . In FIG. 14 , the vertical line represents the deposition rate of the Ru film, and the horizontal line represents the substrate temperature. Also, the line I indicates the formation of the Ru film where the CO is not added to the Ru 3 (CO) 12 , and the line II indicates the formation of the Ru film from the base material of Ru 3 (CO) 12 under the CO atmosphere.
Referring to FIG. 14 , it is confirmed that when the substrate temperature is below 200° C., the deposition rate of Ru 3 (CO) 12 film under the CO atmosphere is very low and the dissociation is practically suppressed. However, it is also confirmed that when the substrate temperature exceeds 200° C., the suppression effect is gradually decreased, and the effectiveness is almost lost when exceeding 230° C. Accordingly, when the temperature of the substrate to be processed W is set to be 235° C. or higher in film forming apparatus 40 of FIG. 11 a or FIG. 11 c , the film is preferentially formed at the periphery of the substrate and the uniformity of the desired film formation in the surface is damaged.
In view of this, when a metal film is formed in film forming apparatus 40 of FIG. 11 using the metal carbonyl base material, for example, when the Ru film is formed using Ru 3 (CO) 12 base material, it is preferable that the substrate temperature is set to be 230° C. or lower where the dissociation suppression effect of the metal carbonyl by the CO is effectively act. Also, it is more preferable to set the substrate temperature to be 200° C. or lower because the dissociation suppression effect acts sufficiently at the temperature range. Moreover, since the dissociation of Ru 3 (CO) 12 base material begins at 100° C. or higher when the CO exists, it is preferable to set the substrate temperature to be 100° C. or higher.
Also, the deposition rate of the Ru film on the substrate to be processed W can be improved as well by increasing the temperature of the base material container that constitute a portion of base material supply system 14 as shown in FIG. 1 .
FIG. 16 is a graph that illustrates the variation of the uniformity of the deposition rate in the surface when the temperature of a base material container 14 A is changed in the film forming apparatus having the constitution of FIG. 7 that uses process gas supply member 24 S instead of shower head 14 S in film forming apparatus of FIG. 1 .
In FIG. 16 , data “I” indicates a case where the temperature of the base material container is set to be 75° C. and corresponds to the result of prior FIG. 10 . In contrast, data “II” is a case where a baffle plate identical to baffle plate 43 B of FIG. 11 a is provided around substrate holding plate 13 in the constitution of FIG. 7 . It is confirmed that while other conditions are the same as in data “I”, the average deposition rate is increased up to 6 Å/min because the conductance of the exhaust path is reduced. In data “II”, the variation of the deposition rate of the formed Ru film in the surface is suppressed as 2% of standard deviation, and an improved uniformity in the substrate surface is achieved.
Also, in FIG. 16 , data “III” indicates the distribution of the deposition rate in the surface when the maintaining temperature of base material container 14 A is set to be 85° C. in the film forming apparatus where the baffle plate is added to the constitution of FIG. 7 based on the constitution of FIG. 1 . As can be known from FIG. 16 , the average deposition rate is improved 60% from 6 Å/min to 10 Å/min by increasing the maintaining temperature of base material container 14 A from 75° C. to 85° C. and maintaining other conditions to be the same. In data “III” as well, the variation of the deposition rate in the surface is suppressed by 2.6% of standard deviation to obtain an improved uniformity in the substrate surface.
Also, in the constitution of FIG. 7 through FIG. 11 , the deposition rate of the Ru film can be improved by maintaining the partial pressure of the CO gas in the process chamber and by increasing the flow rate of the CO carrier gas.
FIG. 17 is a graph that illustrates the uniformity of the deposition rate of the Ru film in the surface when only the flow rate of the CO carrier gas is increased from 100 sccm to 200 sccm and other conditions are maintained to be the same, in film forming apparatus 40 of FIG. 11 a through FIG. 11 c
Referring to FIG. 17 , it is indicated that the average deposition rate is 14.9 Å/min when the flow rate of CO carrier gas is 100 sccm. However, when the CO carrier gas flow rate increases to 200 sccm, the deposition rate increases about 30% to 19.4 Å/min. Also, the variation of the deposition rate in the surface is maintained in the range of 5.5%˜5.7% of standard deviation under any circumstances and an excellent uniformity in the substrate surface is achieved.
FIG. 18 and FIG. 19 each illustrates the constitution of a baffle plate 52 B as a modified embodiment of baffle plate 42 B of FIG. 11 b.
Referring to FIG. 18 and FIG. 19 , when viewed from a vertical direction with respect to substrate holding plate 43 , baffle plate 52 B is provided with 3 rows of opening 52 b or 2 rows of opening 52 c positioned along the outer periphery of the substrate to be processed W corresponding to opening 42 C of FIG. 11 a through FIG. 11 c . For example, it is possible to supply the process gas to the outside of outer periphery of the substrate to be processed W as in film forming apparatus 40 of FIG. 11 a by setting the diameter of opening 52 b or 52 c to be 6.5 mm and the distance to be 13.8 mm.
Second Embodiment
FIG. 20 illustrates the constitution of film forming apparatus 60 in an idling state, according to the second embodiment. Referring to FIG. 20 , film forming apparatus 60 has a structure in which an outer chamber 62 is fixed on a base unit 61 and an inner process chamber 63 formed with a process gas introduce opening 63 A is installed to a flange portion 63 F. Outer chamber 62 corresponds to outer chamber 41 of FIG. 11 a , and a carry in/out space 62 A for the substrate is provided at the side wall.
Meanwhile, inner process chamber 63 corresponds to inner process chamber 42 of FIG. 11 a and has a cylindrical shape. Also, process gas introduce opening 63 A is provided on the upper portion of inner process chamber 63 roughly coinciding with the central shaft. Also, a cool/heat medium path 63 B is provided in inner process chamber 63 to control the temperature.
The bottom portion of inner process chamber 63 is opened, and a substrate holding plate 64 corresponding to substrate holding plate 43 of FIG. 11 a is provided at the front end of a support unit 64 A covering the bottom portion. As a result, inner process chamber 63 along with substrate holding plate 64 defines a process space 63 S.
Support unit 64 A of substrate holding plate 64 is maintained by an actuator 61 A and an arm 61 a with respect to base unit 61 , and the actuator may be either an electronic type or an oil pressure type. An up/down movement indicated as arrows is performed by driving actuator 61 A. Also, the combined portion of support unit 64 A and outer chamber 62 is sealed by a seal member 62 C that includes bellows 62 c.
The bottom portion of outer chamber 62 is provided with an exhaust pipe (not shown), and by connecting exhaust system 11 of FIG. 1 , process space 63 S is exhausted through the exhaust path formed in between substrate holding plate 64 along with support unit 64 A and outer chamber 62 .
As shown in FIG. 20 , a flange-type baffle portion 64 F is provided near substrate holding plate 64 , and a continuous exhaust pipe 63 C is provided in between baffle portion 64 F and the bottom portion of inner process chamber 63 . Exhaust path 63 C is provided continuously at an outer side than the outer periphery of the substrate to be processed W held on inner process chamber 63 . The conductance of exhaust path 63 C varies by moving substrate holding plate 64 into up/down direction.
A heater 64 H is embedded in substrate holding plate 64 and driven by the driving current from an electrode 64 h . Also, a lifter pin 64 L is formed on substrate holding plate 64 with the lower end portion 64 l including a pin driving unit is fixed to a portion of outer chamber 62 . Therefore, when substrate holding plate 64 is descended by actuator 61 A, lifter pin 64 L is protruded to an upper direction than substrate holding plate 64 thereby lifting the substrate to be processed on substrate holding plate 64 . Also, a cool/heat medium path 64 B is provided at the lower part of heater 64 H inside substrate holding plate 64 to pass the cool/heat medium.
Also, substrate holding plate 64 includes a cover ring 64 R which is coupled to the outer periphery of the substrate to be processed held thereon. Cover ring 64 R passes through substrate holding plate 64 and extends to the lower direction. Also, cover ring 64 R includes a drive unit 64 r which is coupled to a portion of outer chamber 62 and clears the combination with the substrate to be processed when substrate holding plate 64 descends.
Also, in film forming apparatus 60 of FIG. 20 , a baffle plate 65 corresponding to baffle plate 42 B of FIG. 11 a is provided inside inner process chamber 63 facing the substrate to be processed on substrate holding plate 64 and with a diameter bigger than that of the substrate to be processed. Also, opening 65 A corresponding to opening 42 C of FIG. 11 a is provided at the outer side than the outer periphery of the substrate to be processed on substrate holding plate 64 . Baffle plate 65 includes flange portion 65 F at the outside of opening 65 A, and flange portion 65 F is fixed to the upper half body 63 U of inner process chamber 63 by screw 65 d . The lower portion of flange portion 65 F is fixed to the lower half body 63 L of inner process chamber 63 by screw 65 e . Upper half body 63 U and lower half body 63 L along with flange portion 65 F form inner process chamber 63 .
Also, film forming apparatus 60 of FIG. 20 is equipped with a controller 66 formed with a general purpose computer loaded with a program to control the entire operation including the operation of actuator 61 A.
Next, referring to FIG. 21 through FIG. 28 , an exemplary process of forming the Ru film on a silicon substrate is described using film forming apparatus 60 of FIG. 20 .
Referring to FIG. 21 , actuator 61 A is driven toward the lower direction by controller 66 , and substrate holding plate 64 A is separated from inner process chamber 63 and descends. As a result, exhaust path 63 C is widely opened corresponding to substrate carry in/out space 62 A of outer chamber 62 . In the state of FIG. 21 , exhaust path 63 C the width of 32.3 mm in an up/down direction. In the state of FIG. 21 , as substrate holding plate 64 descends, lifter pin 64 L protrudes from the surface of substrate holding plate 64 , and cover ring 64 R also changes its positional relationship which is separated toward the upper direction than the surface of substrate holding plate 64 .
Next, as illustrated in FIG. 22 , an arm 71 of the substrate transport mechanism supporting the substrate to be processed W from substrate carry in/out space 62 A is inserted into a position between lifter pin 64 L and cover ring 64 R through the widely opened exhaust path 63 C, and as illustrated in FIG. 23 , the substrate to be processed W is separated from arm 71 by driving drive unit 641 to ascend lifter pin 64 L.
Also, as illustrated in FIG. 24 , arm 70 is retreated from carry in/out space 62 A and the gate valve (not shown) is closed.
Next, as illustrated in FIG. 25 , actuator 61 A is driven and substrate holding plate 64 is elevated putting support unit 64 A in between, and the substrate to be processed W supported on lifter pin 64 L is supported by substrate holding plate 64 . At this state, exhaust path 63 C has a 10 mm width along the up/down direction.
Next, as illustrated in FIG. 26 , actuator 61 A is driven by a tiny amount, and substrate holding plate 64 is elevated by a tiny amount thereby setting the width of exhaust path 63 C to be 8 mm. Also, at this state, cover ring 64 R is combined to the side surface of the substrate to be processed W and maintained.
Also, in the process of FIG. 27 , substrate holding plate 64 is elevated a little further by the driving of actuator 61 A and the distance between baffle plate 65 and the substrate to be processed W is set to be 67 mm. Also, the up/down direction width of exhaust path 63 C is set to be 2 mm, and the process gas containing Ru 3 (CO) 12 gas and CO carrier gas is introduced from process gas introduce opening 63 A. The introduced process gas is exhausted from opening 65 A of the outer periphery of baffle plate 65 to exhaust path 63 C. As a result, the Ru film is deposited with an identical rate in the surface of the substrate to be processed W out of the Ru 3 (CO) 12 molecules diffused from the process gas flow, and the Ru film having an improved uniformity is deposited on the surface of the substrate to be processed W. Also, the process gas discharged from exhaust path 63 C is exhausted from the exhaust pipe (not shown) through exhaust path 62 B formed between outer chamber 62 and substrate holding plate 64 , or between support unit 64 A.
In the process of FIG. 27 , by controlling the temperature of the substrate to be processed W with 200° C. or higher and 230° C. or lower, the preemptive Ru film deposition at the periphery of the substrate to be processed W is effectively suppressed by the CO gas and the problem of a selective deposition of the Ru film at the periphery of the substrate to be processed W, as described in FIG. 15 , can be avoided
After the process of FIG. 27 , although the description is omitted, the substrate to be processed W is taken out by arm 71 of the substrate transport mechanism, the condition of film forming apparatus 60 is returned to the condition of FIG. 20 as illustrated in FIG. 28 , and the inside of inner process chamber 63 is purged.
In the present embodiment, as for baffle plate 65 , not only the baffle plate described in FIG. 11 b and FIG. 11 c but also the baffle plate described in FIG. 18 and FIG. 19 may be used.
Also, in the present embodiment, by flowing the cool/heat medium to cool/heat medium path 63 B or 64 B, the temperature of outer chamber 62 and inner process chamber 63 can be maintained at 80° C. and the deposition of the Ru film other than the substrate to be processed W can be suppressed.
As can be known from the above description, the present invention is not limited to the method of the Ru film formation in which Ru 3 (CO) 12 gas is used as a base material and the CO gas is supplied along with, but may be effective to form other metal film such as W, Co, Os, Ir, Mn, Re, Mo by supplying the carbonyl base material along with the CO gas.
While preferred embodiments are described above, the present invention is not limited to the specific embodiments, but various modifications may be possible within the scope of the claims.
The present invention is based on and claims priority from Japanese Patent Application No. 2008-084551 filed on Mar. 27, 2008, the disclosure of which is incorporated herein in its entirety by reference.
|
Disclosed is a method for film formation, comprising allowing a treatment gas stream containing a metal carbonyl-containing treatment gas and a carbon monoxide-containing carrier gas to flow into a region on the upper outside of the outer periphery of a substrate to be treated in a diameter direction of the substrate while avoiding the surface of the substrate and diffusing the metal carbonyl from the treatment gas stream into the surface of the substrate to form a metal film on the surface of the substrate.
| 7
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional application of commonly assigned, co-pending U.S. patent application Ser. No. 09/655,122, filed Sep. 5, 2000 and entitled “Control Method of Searching Neighboring Cells, Mobile Station, and Mobile Communication System”, which application is incorporated herein by reference in its entirety. That patent application is based on Japanese Patent Application Nos. 11-252294 (1999) filed Sep. 6, 1999 and 11-260409 filed Sep. 14, 1999, the contents of which are also incorporated hereinto by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] 1. The Field of the Invention
[0003] The present invention relates to a mobile communication system for carrying out multiple access using spread spectra, and particularly to a neighboring cell search method applied to handover control during communication or to zone re-selection control during the idle mode in the system and a mobile station constituting the system.
[0004] 2. The Relevant Technology
[0005] A mobile communication system like a widespread mobile phone system offers its services by dividing the entire service area into rather small radio zones called cells. As shown in FIG. 1, such a system comprises a plurality of base stations 111 for covering divided radio zones (cells), and mobile stations 112 for communicating with the base stations by establishing radio channels.
[0006] Direct Sequence CDMA (DS-CDMA) is a scheme for a plurality of users to carry out communications using the same radio frequency band by transmitting information through second modulation that spreads a conventional information data modulation signal with a high rate spreading code. The radio signal of each user is identified by a spreading code assigned to the user.
[0007] In the mobile communication system, the spreading code used for the spreading usually consists of a combination of two types of spreading codes: a “first spreading code group” with the same period as an information symbol period and commonly assigned to all the base stations; and a “second spreading code” with a considerably longer period than the information symbol period and uniquely assigned to each of the base stations.
[0008] [0008]FIG. 2 is a schematic diagram illustrating a method of using the spreading codes in the mobile communication system to which the present invention is applied. In FIG. 2, the upper layer represents a scrambling code layer 202 with a long period uniquely assigned to individual base stations, and the lower layer represents a channelization code layer 204 with a short period commonly assigned to all the base stations. The signals transmitted from the base stations are identified using long period scrambling codes uniquely assigned to the individual base stations. A plurality of codes re defined as the scrambling codes for the entire system, and system designers select the codes to be assigned to the base stations among them.
[0009] For the mobile stations to demodulate information transmitted from the base stations, they must receive the information in synchronization with the timing of the spreading code repeated periodically at the transmitting side. In particular, as for the scrambling codes, detection of the timing requires a long time because of the long period. Accordingly, it is important for the mobile station to detect the repetition timing of the scrambling codes to demodulate perch channels of the base stations. In the present specification, the repetition timing of the scrambling codes is referred to as “phase”. It is not necessary to detect the absolute phase in practice, but to find the relative difference in the timing between the scrambling codes of the base stations, that is, the phase difference. Thus, the term “phase” refers to the relative phase between the scrambling codes in the present specification.
[0010] [0010]FIG. 3 is a schematic diagram illustrating timing relationships between the scrambling codes associated with signals sent from the base stations to a mobile station.
[0011] [0011]FIG. 3 illustrates a case of an inter-cell asynchronous mobile communication system, in which synchronization between the base stations are not necessarily required, and the timing of the scrambling codes received by the mobile station differs for each base station. On the contrary, in an inter-cell synchronous system establishing synchronization between the base stations, the timing of the scrambling codes is exactly adjusted to the timing assigned in advance to the base stations. Accordingly, the relative timing of the scrambling codes between the base stations is fixed and unchangeable. Comparing the inter-cell asynchronous system with the inter-cell synchronous system, the former has an advantage over the latter that it does not require any timing source such as the GPS (Global Positioning System) which is necessary for the synchronous system, and hence is more flexible in extending the system or the like.
[0012] The radio signal transmitted from a base station at certain transmission power travels through space with a certain attenuation, and arrives at a receiving site. Since the attenuation the radio signal undergoes increases with the distance from the transmitting site to the receiving site, it is common that a perch channel transmitted from a distant base station is received at a lower received level, and a perch channel transmitted from a near base station is received at a higher received level. In practice, however, the propagation loss is not determined only by the distant, but varies because of such conditions as the geography and buildings. As a result, the received power of the perch channels from the base stations fluctuate sharply with the move of the mobile station. In the condition in which the received levels of the perch channels from the base stations fluctuate sharply, perch channels received above a certain required received level alter incessantly. This is because the received level of the current perch drops suddenly, or the received level of a perch un-receivable increases abruptly above the receivable level. Thus, to receive the signals from the base stations with better quality, it is important for the mobile station to continuously monitor the perches from the base stations, and to select the best base station.
[0013] In the asynchronous mobile communication system, a mobile station must search for a perch quickly whose spreading code and phase are unknown. As a method of searching for a phase, there is one called “3-step cell search” disclosed in a document by K. Higuchi, M. Sawahashi and F. Adachi, “Fast Cell Search Algorithm In Inter-Cell Asynchronous DS-CDMA Mobile Radio”, IEICE Trans. Commun., Vol. E81-B, No.7, July 1998. The method provides a “masked symbol” part of the perch channel which undergoes double spreading by a channelization code and a scrambling code. Here, the “masked symbol” is spread only by the channelization code without using the scrambling code.
[0014] [0014]FIG. 4 is a schematic diagram illustrating a structure of a perch channel.
[0015] First, the mobile station despreads the received signal using a channelization code 404 commonly used by all the base stations. This enables the mobile station to detect a peak at the timing of a masked symbol 408 of received signal independently of the types of the scrambling codes (first step).
[0016] Subsequently, in response to the timing extracted at the first step, the mobile station detects a scrambling code group code 406 superimposed at the same position as the masked symbol 408 , and identifies the group to which the scrambling code belongs which is used by the base station in connection with the reception (second step).
[0017] Finally, using the scrambling codes belonging to the group determined at the second step, the mobile station identifies the scrambling code 402 used by the base station (third step).
[0018] In the system to which this method is applied, a lot of scrambling codes are divided into groups in advance. In contrast, in the inter-cell synchronous system, since the phase differences of the scrambling codes between the base stations are known in advance, and hence the searching timing can be limited to a fixed timing width (search window), the power consumption or time taken for the cell search can be saved.
[0019] The conventional search method in the inter-cell asynchronous system, however, requires more power consumption and time for the cell search than the inter-cell synchronous system, presenting a problem of exhausting the battery power of the mobile terminal quickly. On the other hand, employing the inter-cell synchronous system to simplify the cell search of the mobile station presets problems of hindering making full use of the above mentioned advantages of the inter-cell asynchronous system, and of increasing the cost of the total system.
[0020] As described above, the mobile communication system such as a currently wide spread mobile phone system comprises the plurality of base stations 111 for covering divided radio zones, and the mobile stations 112 for communicating with the base stations by establishing radio channels as shown in FIG. 1.
[0021] The radio signal transmitted from a base station at certain transmission power travels through space with a certain attenuation, and arrives at a receiving site. Since the attenuation the radio signal undergoes increases with the distance from the transmitting site to the receiving site, a perch channel transmitted from a distant base station is usually received at a lower received level, and a perch channel transmitted from a near base station at a higher received level. In practice, however, the propagation loss is not determined only by the distant, but varies because of such conditions as the geography and buildings. As a result, the received power of the perch channels from the base stations fluctuates sharply with the move of the mobile station. Thus, to receive the signals from the base stations at better quality, it is important for the mobile station to continuously monitor the perch channels from the base stations, and to select the best base station. To select the best base station, the mobile station must continuously confirm the propagation condition of a captured perch channel, or search for uncaptured new perch. Such confirmation of the propagation state of the captured perch channel and the search for the uncaptured new perch channel are generically called “quality measurement of the perch channel” the present specification.
[0022] On the other hand, a technique called intermittent reception is applied to the mobile station to prolong the life of the battery by reducing the power consumption. Although the mobile station in an idle mode must continuously monitor the paging, the intermittent reception halts the receiver as much as possible when unnecessary to receive, thereby saving the power consumption.
[0023] [0023]FIG. 5 is a schematic diagram illustrating a structure of a paging channel defined by ARIB IMT-2000 Study Committee, “Japan's Revised Proposal for Candidate Radio Transmission Technology on IMT-2000: W-CDMA Revised Proposal Version 1.1” (September, 1998, ARIB). According to this paper, to increase the effect of the intermittent reception, the paging channel is structured such that multiple mobile stations are divided into a plurality of groups, and paging signals for respective groups are mapped onto a single physical channel. FIG. 5 illustrates a paging signal assigned to one of the groups. In FIG. 5, reference symbols PIs each designate a very short signal informing whether paging is present or not. Reference symbols MUIs each designate a portion including paging information (ID number of mobile station). In FIG. 5, such a configuration is assumed in which the PIs are transmitted twice (PI 1 and PI 2 ) to improve the receiving accuracy of the PI, and four pieces of paging information (MUI 1 -MUI 4 ) can be transmitted for four mobile stations per group. In other words, the paging signal consists of two PIs and four MUIs, and receiving time period per paging signal is about 15 milliseconds. The paging channel consists of multiplexed paging signals with the same structure, the number of which equals the number of the groups. FIG. 5 illustrates that the mobile station receives the paging signal of its own group at every 720 millisecond interval.
[0024] The mobile station receives the PI portion, first, and then the MUI portion only when a decision is made that the paging is present as a result of receiving the PI portion. This offers two advantages: First, it is enough for the mobile station to receive only the paging of its own group; and second, to receive only the PI portion when there is not paging information. This in turn can limit the actually required receiving time rate to a small value, making it possible to reduce the power consumption to a very small amount.
[0025] [0025]FIG. 5 illustrates the paging information which is already transmitted from the base station and selected through the decision by the mobile station. In an actual situation, however, the mobile station must search for the perch channels of the neighboring base stations as it moves. Since the mobile station must receive a lot of receivable perch channels to search for the neighboring base stations, it is important to minimize the frequency of the search operation to increase the effect of the intermittent reception.
[0026] Thus, to select the best base station with the movement of the mobile station, there is a tradeoff between the continuous monitoring of the perch channels of the neighboring base stations by searching and receiving them, and the reduction in the operation time rate of the receiver to prolong the battery of the mobile station as long as possible. On the one hand, the reduction in the operation time rate of the receiver will results in a decrease in the selection accuracy of the base station, bringing about undesirable results such as degradation in the service quality. On the other hand, an increase in the operation time rate of the receiver to improve the selection accuracy of the base station will consume the battery of the mobile station quickly, presenting a problem of markedly impairing the usefulness of the mobile station. In the conventional cell search control method, however, the quality measurement of the perch channel is implemented periodically as described in the following paper with considering the tradeoff between the selection accuracy of the base station and the service quality: K. Yunoki, A. Higashi and N. Tsutsumi, “Cell Search Strategy on W-CDMA Mobile Station”, B-5-186 of the 1999 IEICE General Conference. Specifically, since the quality measurement of the perch channel is carried out independently of the reception of the paging signal, the mobile station must operate its receiver at both timings of quality measurement of the perch channel and the reception of the paging signal, which presents a problem of increasing the consumption of the battery, one of the essential resources of the mobile station.
BRIEF SUMMARY OF THE INVENTION
[0027] It is therefore an object of the present invention to provide a control method of searching for a neighboring cell, and a mobile station in an inter-cell asynchronous system with taking full advantage of the system, and saving the power consumption and time required for the cell search by the mobile station without increasing the total cost of the system.
[0028] Another object of the present invention is to save the power consumption with maintaining the accuracy of selecting the best base station in the mobile communication system that comprises a plurality of base stations and mobile stations communicating with the base stations by means of the code division multiple access. This is implemented by the mobile station by receiving perch channels transmitted from the base stations, by deciding the base station the mobile station should wait for or communicate with, and by monitoring the paging signal to the mobile station itself by the intermittent reception in the idle mode.
[0029] In the first aspect of the present invention, there is provided a control method of searching for a neighboring cell of a mobile station communicating with base stations in a direct sequence CDMA mobile communication system which transmits information by carrying out double modulation using a first spreading code group and one of second spreading codes, the first spreading code group including spreading codes that have a same repetition period as an information symbol period and are used in common by the base stations, the second spreading codes having a repetition period longer than the information symbol period, and being different for each of the base stations, the control method of searching for a neighboring cell comprising:
[0030] a step of storing into a first table the second spreading code and its phase of at least one perch channel, which second spreading code and phase are known;
[0031] a step of storing a second spreading code used by a neighboring base station into a second table;
[0032] a first search step of searching for a perch channel whose second spreading code and phase are unknown; and
[0033] a second search step of searching for a perch channel whose second spreading code and phase are known, wherein
[0034] the control method of searching for a neighboring cell carries out the first search step and the second search step using the first table and the second table.
[0035] Here, the control method of searching for a neighboring cell may further comprise the step of transferring, when capturing a perch channel in the first search step of searching for a perch channel whose second spreading code and phase are unknown, the second spreading code corresponding to the perch channel from the second table to the first table.
[0036] The control method of searching for a neighboring cell may further comprise the steps of:
[0037] carrying out the second search step using the first table;
[0038] carrying out the first search step using the second table; and
[0039] detecting a new perch channel by comparing a search result at the second search step with a search result at the first search step.
[0040] The first search step may comprise:
[0041] a step of detecting a peak of a received signal at a timing of a masked symbol of the received signal by despreading the received signal using the first spreading code group;
[0042] a step of identifying a group to which the second spreading code belongs; and
[0043] a step of identifying the second spreading code.
[0044] The control method of searching for a neighboring cell may comprise the steps of:
[0045] carrying out the second search step using the first table;
[0046] carrying out a third search step using the second table, the third search step consisting of part of sub-steps constituting the first search step;
[0047] deciding detection of a new perch channel by comparing a search result of the second search step with a search result of the third search step; and
[0048] carrying out a fourth search step in response to a decision result, the fourth search step consisting of sub-steps of the first search step, which are not carried out in the third search step.
[0049] The direct sequence CDMA mobile communication system may spread information into a signal with a bandwidth broader than a frequency bandwidth of the information using a spreading code sequence with a rate higher than an information transmission rate.
[0050] In the second aspect of the present invention, there is provided a mobile station communicating with base stations in a direct sequence CDMA mobile communication system which transmits information by carrying out double modulation using a first spreading code group and one of second spreading codes, the first spreading code group including spreading codes that have a same repetition period as an information symbol period and are used in common by the base stations, the second spreading codes having a repetition period longer than the information symbol period, and being different for each of the base stations, the mobile station comprising:
[0051] a first table for storing the second spreading code and its phase of at least one perch channel, which second spreading code and phase are known;
[0052] a second table for storing a second spreading code used by a neighboring base station;
[0053] first search means for searching for a perch channel whose second spreading code and phase are unknown; and
[0054] a second search means for searching for a perch channel whose second spreading code and phase are known, wherein
[0055] the first search means and the second search means carry out their search using the first table and the second table.
[0056] Here, the mobile station may further comprise means for transferring, when the first search means captures a perch channel whose second spreading code and phase are unknown as a result of the search, the second spreading code corresponding to the perch channel from the second table to the first table.
[0057] The second search means may carry out its search using the first table;
[0058] the first search means may carry out its search using the second table, and the mobile station may further comprise:
[0059] means for making decision of detecting a new perch channel by comparing a search result by the second search means with a search result by the first search means.
[0060] The first search means may comprise:
[0061] means for detecting a peak of a received signal at a timing of a masked symbol of the received signal by despreading the received signal using the first spreading code group;
[0062] means for identifying a group to which the second spreading code belongs; and
[0063] means for identifying the second spreading code.
[0064] The second search means may carry out its search using the first table, and the mobile station may further comprise:
[0065] third search means for carrying out its search using the second table, the third search means consisting of part of the first search means;
[0066] means for deciding detection of a new perch channel by comparing a search result of the second search means with a search result of the third search means; and
[0067] fourth search means for carrying out its search in response to a decision result, the fourth search means consisting of a remaining part of the first search means.
[0068] The direct sequence CDMA mobile communication system may spread information into a signal with a bandwidth broader than a frequency bandwidth of the information using a spreading code sequence with a rate higher than an information transmission rate.
[0069] A direct sequence CDMA mobile communication system may comprise the mobile station.
[0070] According to the configuration, the power and time required for the cell search can be reduced because the first table, which is prepared for storing captured perch channels, that is, perch channels whose second spreading code and phase are acquired by the mobile station, enables the mobile station to carry out the search for the perch channel only in a predetermined time range (search window) with regard to the phase of the perch channel.
[0071] The mobile station usually receives from its visiting base station, information on the scrambling codes used by the neighboring base stations, and carries out the cell search in accordance with the information. The present invention is configured such that it transfers the captured perch channels from the second table to the table of already captured perches. This makes it possible to further narrow down candidates in searching for the perch with the unknown phase, thereby simplifying the search for the perch not only with the known phase but also with the unknown phase.
[0072] Moreover, according to one aspect of the present invention, it applies the second search process to the first table; applies to the second table a third search process consisting of steps up to a midpoint of the steps of the first search process; makes a decision of the new perch channel by comparing the search result of the second search process with that of the third search process; and obtains the difference between the first search process and the third search process on the basis of the decision result. This enables the mobile station to make full use of the second spreading code and phase of each captured perch channel, and hence to make a decision as to whether a new perch channel other than the captured perch channel appears or not by carrying out the search of the perch channels with the known phases up to the intermediate step 1 or 2, without carrying out the entire three steps of the 3-step cell search, thereby simplifying the 3 step cell search which is not always essential.
[0073] In the third aspect of the present invention, there is provided a cell search control method in a CDMA mobile communication system including a mobile station which decides a base station the mobile station waits for or communicates with by receiving a perch channel transmitted from the base station, and which monitors a paging signal to the mobile station by means of intermittent reception in the idle mode, the cell search control method comprising the step of:
[0074] carrying out, in the mobile station, measurement of receiving quality of the perch channel in synchronization with timing of receiving the paging signal sent to the mobile station.
[0075] Here, the measurement of the receiving quality of the perch channel may be carried out in the mobile station when a time period counted from a latest measurement of the receiving quality of the perch channel exceeds a predetermined value.
[0076] In the fourth aspect of the present invention, there is provided a CDMA mobile communication system including a mobile station communicating with a plurality of base stations, each of the base stations comprising:
[0077] perch channel transmitting means for transmitting a perch channel to the mobile station; and
[0078] paging signal transmitting means for transmitting a paging signal to the mobile station, and the mobile station comprising:
[0079] base station decision means for deciding a base station the mobile station waits for or communicates with through the perch channel by receiving the perch channel transmitted by the perch channel transmitting means;
[0080] paging signal reception decision means for deciding in an idle mode as to whether the paging signal transmitted to the mobile station by the paging signal transmitting means is received or not by intermittent reception; and
[0081] receiving quality measurement means for measuring the receiving quality of the perch channel, wherein
[0082] the receiving quality measurement means carries out the measurement of the receiving quality of the perch channel in synchronization with timing of receiving the paging signal when the paging signal reception decision means decides that the paging signal is received.
[0083] Here, the mobile station may further comprise counting means for counting a time period from a latest measurement of the receiving quality of the perch channel, and the receiving quality measurement means may carry out the measurement of the receiving quality of the perch channel when the time period counted by the counting means exceeds a predetermined value.
[0084] In the fifth aspect of the present invention, there is provided a mobile station in a CDMA mobile communication system communicating with a plurality of base stations, the mobile station comprising:
[0085] base station decision means for deciding a base station the mobile station waits for or communicates with through a perch channel by receiving the perch channel transmitted from the base station;
[0086] paging signal reception decision means for deciding in an idle mode as to whether the paging signal transmitted to the mobile station from the base station is received or not by intermittent reception; and
[0087] receiving quality measurement means for measuring the receiving quality of the perch channel, wherein
[0088] the receiving quality measurement means carries out the measurement of the receiving quality of the perch channel in synchronization with timing of receiving the paging signal when the paging signal reception decision means decides that the paging signal is received.
[0089] Here, the mobile station may further comprise counting means for counting a time period from a latest measurement of the receiving quality of the perch channel, and the receiving quality measurement means may carry out the measurement of the receiving quality of the perch channel when the time period counted by the counting means exceeds a predetermined value.
[0090] Thus, in the mobile communication system utilizing the code division multiple access, the base stations employ the same radio frequency. Accordingly, the perch channels and paging channels of the base stations are all transmitted on the same radio frequency, and are identified by the spreading codes. This makes it possible to use the radio stage, which receives the radio frequency and extracts the spread modulation signal, in common to receive the perch channels and paging channels, thereby reducing the uptime of the radio stage by matching the timing of receiving these channels.
[0091] As described above, because the base stations employ the same radio frequency, user radio waves of voices or data are also transferred at the same frequency. This can bring about the degradation in the receiving quality of the perch channel or paging channel because the user radio waves become interference in receiving the perch channel or paging channel.
[0092] Furthermore, in the time periods of much interference because of a great number of such user radio waves, the number of paging signals transmitted from the base stations over the paging channels are also increased. In contrast, in time periods suffering only small interference from the user radio waves, the number of paging signals transmitted from the base stations over the paging channels is also reduced. Thus, the receiving quality of the perch channels or paging channels depends on the transmission frequency of the paging signals in such a manner that it is improved with a decrease in the number of the paging signals, and impaired with an increase in the number thereof. This teaches that to maintain the selection accuracy of the base station at a high level when the receiving quality of the perch channel is low, it is necessary to increase the frequency of measuring the receiving quality of the perch channel, thereby increasing the quality measurement frequency.
[0093] According to one aspect of the present invention, it is configured such that it carries out the quality measurement of the perch channel in synchronization with the received timing of the paging signal. This will automatically increase the measurement frequency of the receiving quality of the perch channel in the case where the receiving quality is low, thereby improving the selection accuracy of the base station, but decrease the measurement frequency in the case where the receiving quality of the perch channel is high, thereby saving the power consumption. In addition, the present invention is configured such that it counts the elapsed time from the latest measuring of the receiving quality of the perch channel, and carries out the measurement of the receiving quality of the perch channel when the elapsed time exceeds a predetermined value. This makes it possible to carry out the measurement of the receiving quality of the perch channel at a minimum frequency even when the paging signals are very few such as in midnight.
[0094] The above and other objects, effects, features, and advantages of the present invention will become more apparent from the following description of embodiments thereof taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0095] To further clarify the above and other advantages and features of the present invention, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. It is appreciated that these drawings depict only typical embodiments of the invention and are before not to be considered limiting of its scope. The invention will be described and explained with additional specificity and detail through the use of the accompanying drawings in which:
[0096] [0096]FIG. 1 is a diagram illustrating an example of a mobile communication system;
[0097] [0097]FIG. 2 is a schematic diagram illustrating a method of using spreading codes of the mobile communication system;
[0098] [0098]FIG. 3 is a schematic diagram illustrating relationships of the timing between scrambling codes for the signals transmitted from base stations to a mobile station;
[0099] [0099]FIG. 4 is a schematic diagram illustrating a structure of a perch channel;
[0100] [0100]FIG. 5 is a schematic diagram illustrating a structure of a paging channel;
[0101] [0101]FIG. 6 is a block diagram showing a configuration of a mobile station to which the present invention is applied;
[0102] [0102]FIG. 7 is a schematic diagram illustrating an operation in accordance with the present invention;
[0103] [0103]FIG. 8 is a schematic diagram illustrating an operation of deciding a new perch;
[0104] [0104]FIG. 9 is a schematic diagram illustrating an operation of deciding a new perch when using the first and second steps to search for the new perch;
[0105] [0105]FIG. 10 is a flowchart illustrating an operation of the mobile station 602 in FIG. 7;
[0106] [0106]FIG. 11 is a flowchart illustrating an operation of the mobile station in FIG. 8;
[0107] [0107]FIG. 12 is a block diagram showing a configuration of a mobile station to which the present invention is applied;
[0108] [0108]FIG. 13 is a flowchart illustrating an operation of a mobile station in accordance with the present invention;
[0109] [0109]FIG. 14 is a flowchart illustrating an operation of a mobile station in accordance with the present invention; and
[0110] [0110]FIG. 15 is a schematic diagram illustrating an operation state observed on a time axis when the cell search control method in accordance with the present invention is operating.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0111] The invention will now be described with reference to the accompanying drawings.
[0112] EMBODIMENT 1
[0113] [0113]FIG. 6 is a block diagram showing a configuration of a mobile station to which the present invention is applied.
[0114] A mobile station 500 comprises a mobile station transceiver 502 , a user interface 504 , a neighboring base station information acquisition and processing unit 506 , a common controller 508 , a cell search controller 510 , a memory 512 , an antenna 514 and a bus 516 . In the mobile station as shown in FIG. 6, only portions associated with the present invention are illustrated.
[0115] The mobile station transceiver 502 demodulates user information and control signals transmitted from the base stations after their radio frequency modulation, and transmitting user signals and control signals after their coding and modulation. The mobile station transceiver 502 is connected to the antenna 514 and user interface 504 .
[0116] The common controller 508 carries out the overall control of the mobile station.
[0117] The cell search controller 510 controls the cell search operation with regulating the timing in accordance with neighboring base station information, and stores search results into the memory 512 .
[0118] The neighboring base station information acquisition and processing unit 506 receives and processes scrambling code information about the neighboring base stations sent from the visiting base station, and stores it into the memory 512 .
[0119] The bus 516 interconnects the common controller 508 , cell search controller 510 , neighboring base station information acquisition and processing unit 506 and memory 512 .
[0120] [0120]FIG. 7 is a schematic diagram illustrating an operation of the present invention. The operation of the mobile station 602 in FIG. 7 will now be described with reference to the flowchart of FIG. 10.
[0121] As illustrated in the right-hand side of FIG. 7, the mobile station 602 captures information about scrambling codes used by its neighboring base stations from the visiting base station, from which the mobile station receives the paging information, and stores the information into a code table 608 of the neighboring base stations in a code table 604 on the memory as illustrated in the left-hand side of FIG. 7 (step S 902 ).
[0122] Using the table 608 , the mobile station 602 carries out the cell search for perch channels with unknown scrambling codes and phases (step S 904 ), creates a table 606 for holding the scrambling codes and phases of the captured perch channels (thin solid-line arrows on the right-hand side of FIG. 7) (step S 906 ); and eliminates the scrambling codes from the code table 608 of the neighboring base stations (step S 908 ).
[0123] As for the perch channels which cannot be captured until then (broken line arrows on the right-hand side of FIG. 7), both their scrambling codes and phases are unknown. As described above, the phases correspond to the phase differences between the scrambling codes. In FIG. 7, numerical examples are illustrated of the phase differences between the scrambling codes with regard to the timing the mobile station has as a reference, which numerical examples are represented in terms of chips (one chip corresponds to one bit of a spreading code consisting of a bit stream of “0” and “1”).
[0124] Moving along the arrow, the mobile station carries out the cell search, and when it can capture a cell, it transfers it to the captured table 606 (step S 910 ).
[0125] [0125]FIG. 8 is a schematic diagram illustrating an operation of making a decision of a new perch. The operation of the mobile station of FIG. 8 be described with reference to a flowchart of FIG. 11.
[0126] [0126]FIG. 8 illustrates a case which carries out only the first step as the new perch search, and decides a new perch from its result.
[0127] To search for the new perch, the mobile station carries out the first step of searching for some phase position (step S 1002 ). Apart from this, it performs a window search for reassuring the phases of the captured perch channels (step S 1004 ). Subsequently, it compares both the results (step S 1006 ); makes a decision that any perch other than the currently captured perches is a new perch channel (step S 1008 ); and identifies the scrambling code by executing the second and third steps for the perch channel (step S 1010 ).
[0128] [0128]FIG. 9 illustrates an example of a decision operation of the new perch using the first and second steps as the new perch search.
[0129] It differs from FIG. 8 in that it can make use of the scrambling code group information when deciding as to whether the result of the new perch search is a captured perch or a new perch.
[0130] In FIG. 9, G 1 , G 7 , G 15 and G 3 each designate a scrambling code group. More specifically, the G 1 , G 7 , G 15 and G 3 denote that the groups, to which the scrambling codes used for the perches detected at these phases, are the first, seventh, 15 th and third group, respectively.
[0131] Comparing their phases with those of the scrambling code groups of the captured perches, the mobile station identifies a perch if the phases differ, and then carries out the third step.
[0132] In FIG. 9, the perch received at the phase G 3 is decided as the new perch because its phase and scrambling code differ from those of the captured perches.
[0133] In addition, although not illustrated in the drawings, execution of all the steps from the first to third steps as the new perch search can be implemented in the same manner as illustrated in FIGS. 8 and 9, except that it can use, for deciding the new perch, both the scrambling code and phase as the result of the new perch search.
[0134] Although the present embodiment is described for the convenience sake as though the mobile station always carried out the new perch search and captured perch confirmation simultaneously, the embodiments in accordance with the present invention are not limited to this. For example, when carrying out both searches for the new and captured perches regularly, such a configuration can be implemented in which their intervals are set differently so that one of them is carried out at a higher (or lower) frequency than the other. Alternatively, a configuration can be implemented in which they can be controlled adaptively to the conditions as needed.
[0135] As long as the new perch decision is made by comparing the captured perches with the results of the new perch search, a similar effect can be achieved.
[0136] As described above, the present invention can provide the control method of neighboring cell search, and the mobile station, with making use of the advantages of the inter-cell asynchronous system, and with minimizing the power consumption and time required for the cell search by the mobile station without increasing the total cost of the system.
[0137] SECOND EMBODIMENT
[0138] Next, the second embodiment of the present invention will be described with reference to FIGS. 12 - 15 .
[0139] [0139]FIG. 12 is a block diagram showing a configuration of a mobile station to which the present invention is applied.
[0140] [0140]FIG. 12 shows only portions of the mobile station associated with the present invention.
[0141] A mobile station 300 comprises a radio signal transceiver 302 , a traffic channel transceiver 304 , a user interface 306 , a perch channel receiver 308 , a perch channel receiving quality measurement controller 310 , a paging signal receiver 312 , a common controller 314 , a memory 316 , an antenna 3
[0142] common bus 320 .
[0143] The radio signal transceiver 302 connected to the antenna 318 is a device for receiving user information and a control signal transmitted from a base station after radio frequency modulation, and for transmitting user information or control information about voices or data to be transmitted from the mobile station to the base station. Although it is integrally illustrated in Fig. 12 , the transmitter and receiver can be provided separately. The traffic channel transceiver 304 connected to both the radio signal transceiver 302 and user interface 306 is a device for carrying out codec of the user information such as voice or data. The perch channel receiver 308 measures the receiving quality of the perch channel, and extracts broadcast information from the base station by decoding the perch channel. The perch channel receiving quality measurement controller 310 , issuing a command to the perch channel receiver 308 , controls the measurement operation of the receiving quality of the perch channel. The paging signal receiver 312 receives and decodes a paging signal sent from the base station. The common controller 314 carries out the overall control of the mobile station, and the memory 316 is used for storing various items of information. The common bus 320 interconnects the perch channel receiver 308 , perch channel receiving quality measurement controller 310 , paging signal receiver 312 , common controller 314 and memory 316 .
[0144] Next, the operation of the mobile station with such a configuration will be described with reference to FIGS. 13 and 14.
[0145] As described above, the intermittent receiving technique is applied to the mobile station. Besides, as disclosed in the foregoing paper “Japan's Revised Proposal for Candidate Radio Transmission Technology on IMT-2000:W-CDMA Revised Proposal Version 1.1”, a great number of mobile stations are divided into a plurality of groups, and each paging signal assigned to one of the groups is mapped onto a single physical channel to configure the paging channels. FIG. 5 illustrates a paging signal assigned to one of the groups. In FIG. 5, reference symbols PIs each designate a very short signal informing whether paging is present or not; and MUIs each designate a portion including paging information (ID number of mobile station). The mobile station receives the PI portion, first, and then the MUI portion only when a decision is made that the paging is present from the receiving result of the PI portion.
[0146] [0146]FIG. 13 is a flowchart illustrating the operation of the mobile station in accordance with the present invention.
[0147] The mobile station decides as to whether a timing for receiving the PI comes, first (step S 1402 ), and when the timing comes, it activates the radio signal transceiver 302 to receive the PI portion in the paging signal (step S 1404 ). When it decides that the paging is not present from the receiving result, it stops the operation of the radio signal transceiver 302 (step S 1414 ). In contrast, when it decides that the paging is present, it continues to operate the radio signal transceiver 302 (step S 1406 ). At the same time, it commands the paging signal receiver 312 to receive the paging signal (step S 1408 ), and causes the perch channel receiving quality measurement controller 310 to issue the command to the perch channel receiver 308 to measure the receiving quality of the perch channel (step S 1410 ). Subsequently, it decides whether the individual operations have been completed (step S 1412 ), stops the operation of the radio signal transceiver 302 when completed (step S 1414 ), and waits until the next timing of receiving the PI comes (step S 1402 ).
[0148] [0148]FIG. 14 is a flowchart illustrating the operation of the mobile station with a configuration of carrying out the next quality measurement at the time when a predetermined time period has elapsed after the previous quality measurement.
[0149] The mobile station decides as to whether a timing for receiving the PI comes, first (step S 1502 ), and when the timing comes, it activates the radio signal transceiver 302 to receive the PI portion in the paging signal (step S 1504 ). When it decides that the paging is not present from the receiving result, it proceeds to the decision step of the elapsed time from the latest quality measurement (step S 1508 ). When the elapsed time has exceeded the predetermined value, it carries out the same operation as when the decision is made that the paging is present (step S 1506 ). When the elapsed time is below the predetermined value, it halts the operation of the radio signal transceiver 302 (step S 1516 ), and waits for the next timing (step S 1502 ). In contrast, when it decides that the paging is present at step S 1504 , it continues to operate the radio signal transceiver 302 (step S 1506 ). At the same time, it commands the paging signal receiver 312 to receive the paging signal (step S 1510 ), and causes the perch channel receiving quality measurement controller 310 to issue the command to the perch channel receiver 308 to measure the receiving quality of the perch channel (step S 1512 ). Subsequently, it decides as to whether the individual operations have been completed (step S 1514 ), stops the operation of the radio signal transceiver 302 when completed (step S 1516 ), and waits until the next timing of receiving the PI comes (step S 1502 ).
[0150] [0150]FIG. 15 is a schematic diagram illustrating an operation state observed on a time axis when the cell search control method in accordance with the present invention is operating.
[0151] In FIG. 15, the top view illustrates the quality measurement of the perch channel, and the bottom view illustrates the paging reception. Shadowed portions in the top view denote portions of executing the quality measurement of the perch channel. The bottom view illustrates the paging reception taking an example of a paging channel in which a paging signal consists of the PIs (narrow portions) and MUIs (wide portions). When the PIs indicate the presence of the paging information, the corresponding MUIs are denoted as a shadowed portion, whereas when they indicate the absence of the paging information, the MUIs are denoted as a blank. Thus, the mobile station does not receive the blank MUIs because they have no paging information.
[0152] As illustrated in FIG. 15, according to the present invention, the receiving quality measurement of the perch channel is controlled in accordance with the presence or absence of the paging information. Specifically, when the paging information is present, the measurement of the perch channel receiving quality is executed at the same time as the paging reception, whereas when the paging information is absent, the measurement of the perch channel receiving quality is skipped.
[0153] As described above, the embodiment according to the present invention is configured such that the mobile station controls the timing of measuring the receiving quality of the perch channel in synchronization with the paging signal to the mobile station so that the measurement of the receiving quality of the perch channel is carried out simultaneously with the reception of the paging signal. This makes it possible to save the power consumption with maintaining the high accuracy of selecting the best base station.
[0154] Furthermore, the embodiment is configured such that it counts the elapsed time from the measurement of the receiving quality of the perch channel, and when the elapsed time exceeds the predetermined value, it carries out the measurement of the receiving quality of the perch channel. This makes it possible to maintain the accuracy of selecting the best base station at a higher accuracy, making is possible to further reduce the power consumption.
[0155] OTHER EMBODIMENTS
[0156] As to the standards of the third generation mobile communication system, IMT-2000 (International Mobile Telecommunications-2000), the 3GPP (Third Generation Partnership Project) is making a plan. Details of paging information transmission method is described in the standard “3GTS 25.211 V3.3.0”. To increase the versatility of the standard, it is modified slightly from the “Japan's Revised Proposal for Candidate Radio Transmission Technology on IMT-2000: W-CDMA”. Specifically, it is configured such that the information about the presence and absence of the paging is transmitted over a PICH (Paging Indicator CHannel), and the paging information itself is transmitted over an SCCPCH (Secondary Common Control Physical CHannel). Although the physical configuration is thus modified, the standard is the same as the present specification in the procedure for the mobile station to receive the PI portion before receiving the paging information, and to receive the paging information itself only when a decision is made that the paging is present as a result of receiving the PI, and in the effect of the intermittent reception obtained from the procedure. Accordingly, it will be obvious for those skilled in the art that the present invention is applicable to the “3GTS 25.211 V3.3.0”. In addition, it is obvious for those skilled in the art that the present invention is not limited to the radio schemes described above, but can be implemented in any radio schemes utilizing the present invention.
[0157] Moreover, although the foregoing embodiments handle the case in which the embodiments are implemented independently, the present invention is not limited to this. For example, any proper combination of the foregoing embodiments can be implemented, which will be obvious to those skilled in the art.
[0158] The present invention may be embodied in other specific forms without departing from its spirit or essential characteristics. The described embodiments are to be considered in all respects only as illustrative and not restrictive. The scope of the invention is, therefore, indicated by the appended claims rather than by the foregoing description. All changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
|
A control method of searching for a neighboring cell of a mobile station communicating with a base-station is provided in a direct sequence CDMA mobile communication system which transmits information by carrying out double modulation using a first spreading code group and a second spreading code. The first spreading code group includes spreading codes that have a same repetition period as an information symbol period and are used in common by the base stations, and the second spreading code has a repetition period longer than the information symbol period. The base stations are assigned different second spreading codes. The control method stores at least one second spreading code and its phase into a first table, which second spreading code corresponds to a perch channel whose second spreading code and phase are known; stores a second spreading code used by a neighboring base station into a second table; searches for a perch channel whose second spreading code and phase are unknown; and searches for a perch channel whose second spreading code and phase are known. The neighboring cell search method can save the power consumption and time required for the mobile station to carry out the cell search with preventing an increase in the total cost of the system.
| 8
|
BACKGROUND OF THE INVENTION
[0001] The present invention is directed to peptide analogues of glucagon-like peptide-1, the pharmaceutically-acceptable salts thereof, to methods of using such analogues to treat mammals and to pharmaceutical compositions useful therefor comprising said analogues.
[0002] Glucagon-like peptide-1(7-36) amide (GLP-1) is synthesized in the intestinal L-cells by tissue-specific post-translational processing of the glucagon precursor preproglucagon (Varndell, J. M., et al., J. Histochem Cytochem, 1985:33:1080-6) and is released into the circulation in response to a meal. The plasma concentration of GLP-1 rises from a fasting level of approximately 15 pmol/L to a peak postprandial level of 40 pmol/L. It has been demonstrated that, for a given rise in plasma glucose concentration, the increase in plasma insulin is approximately threefold greater when glucose is administered orally compared with intravenously (Kreymann, B., et al., Lancet 1987:2, 1300-4). This alimentary enhancement of insulin release, known as the incretin effect, is primarily humoral and GLP-1 is thought to be the most potent physiological incretin in humans. In addition to the insulinotropic effect, GLP-1 suppresses glucagon secretion, delays gastric emptying (Wettergren A., et al., Dig Dis Sci 1993:38:665-73) and may enhance peripheral glucose disposal (D'Alessio, D. A. et al., J. Clin Invest 1994:93:2293-6).
[0003] In 1994, the therapeutic potential of GLP-1 was suggested following the observation that a single subcutaneous (s/c) dose of GLP-1 could completely normalize postprandial glucose levels in patients with non-insulin-dependent diabetes mellitus (NIDDM) (Gutniak, M. K., et al., Diabetes Care 1994:17:1039-44). This effect was thought to be mediated both by increased insulin release and by a reduction in glucagon secretion. Furthermore, an intravenous infusion of GLP-1 has been shown to delay postprandial gastric emptying in patients with NIDDM (Williams, B., et al., J. Clin Endo Metab 1996:81:327-32). Unlike sulphonylureas, the insulinotropic action of GLP-1 is dependent on plasma glucose concentration (Holz, G. G. 4 th , et al., Nature 1993:361:362-5). Thus, the loss of GLP-1-mediated insulin release at low plasma glucose concentration protects against severe hypoglycemia. This combination of actions gives GLP-1 unique potential therapeutic advantages over other agents currently used to treat NIDDM.
[0004] Numerous studies have shown that when given to healthy subjects, GLP-1 potently influences glycemic levels as well as insulin and glucagon concentrations (Orskov, C, Diabetologia 35:701-711,1992; Holst, J. J., et al., Potential of GLP -1 in diabetes management in Glucagon III, Handbook of Experimental Pharmacology, Lefevbre P J, Ed. Berlin, Springer Verlag, 1996, p. 311-326), effects which are glucose dependent (Kreymann, B., et al., Lancet ii: 1300-1304, 1987; Weir, G. C., et al., Diabetes 38:338-342, 1989). Moreover, it is also effective in patients with diabetes (Gutniak, M., N. Engl J Med 226:1316-1322, 1992; Nathan, D. M., et al., Diabetes Care 15:270-276, 1992), normalizing blood glucose levels in type 2 diabetic subjects (Nauck, M. A., et al., Diagbetologia 36:741-744, 1993), and improving glycemic control in type 1 patients (Creutzfeldt, W. O., et al., Diabetes Care 19:580-586,1996), demonstrating its ability to, inter alia, increase insulin sensitivity/reduce insulin resistance. GLP-1 and agonists thereof have been proposed for use in subjects at risk for developing non-insulin dependent diabetes (see WO 00/07617) as well as for the treatment of gestational diabetes mellitus (U.S. Patent Pub. No. 20040266670).
[0005] In addition to the foregoing, there are a number of therapeutic uses in mammals, e.g., humans, for which GLP-1 and agonists thereof have been suggested, including, without limitation: improving learning, enhancing neuro-protection, and/or alleviating a symptom of a disease or disorder of the central nervous system, e.g., through modulation of neurogenesis, and e.g., Parkinson's Disease, Alzheimer's Disease, Huntington's Disease, ALS, stroke, ADD, and neuropsychiatric syndromes (U.S. Patent Pub. No.'s 20050009742 and 20020115605); converting liver stem/progenitor cells into functional cells pancreatic (WO03/033697); preventing beta-cell deterioration (U.S. Patent Pub. No.'s 20040053819 and 20030220251) and stimulation of beta-cell proliferation (U.S. Patent Pub. No. 20030224983); treating obesity (U.S. Patent Pub. No. 20040018975; WO98/19698); suppressing appetite and inducing satiety (U.S. Patent Pub. No. 20030232754); treating irritable bowel syndrome (WO 99/64060); reducing the morbidity and/or mortality associated with myocardial infarction (US Patent Pub No. 20040162241, WO98/08531) and stroke (see WO 00/16797); treating acute coronary syndrome characterized by an absence of Q-wave myocardial infarction (U.S. Patent Pub. No. 20040002454); attenuating post-surgical catabolic changes (U.S. Pat. No. 6,006,753); treating hibernating myocardium or diabetic cardiomyopathy (U.S. Patent Pub. No. 20050096276); suppressing plasma blood levels of norepinepherine (U.S. Patent Pub. No.20050096276); increasing urinary sodium excretion, decreasing urinary potassium concentration (U.S. Patent Pub. No. 20050037958); treating conditions or disorders associated with toxic hypervolemia, e.g., renal failure, congestive heart failure, nephrotic syndrome, cirrhosis, pulmonary edema, and hypertension (U.S. Patent Pub. No. 20050037958); inducing an inotropic response and increasing cardiac contractility (U.S. Patent Pub. No. 20050037958); treating polycystic ovary syndrome (U.S. Patent Pub. No.'s 20040266678 & 20040029784); treating respiratory distress (U.S. Patent Pub. No. 20040235726); improving nutrition via a non-alimentary route, i.e., via intravenous, subcutaneous, intramuscular, peritoneal, or other injection or infusion (U.S. Patent Pub. No.20040209814); treating nephropathy (U.S. Patent Pub. No. 20040209803); treating left ventricular systolic dysfunction, e.g., with abnormal left ventricular ejection fraction (U.S. Patent Pub. No. 20040097411); inhibiting antro-duodenal motility, e.g., for the treatment or prevention of gastrointestinal disorders such as diarrhea, postoperative dumping syndrome and irritable bowel syndrome, and as premedication in endoscopic procedures (U.S. Patent Pub. No. 20030216292); treating critical illness polyneuropathy (CIPN) and systemic inflammatory response syndrome (SIRS) (U.S. Patent Pub. No. 20030199445); modulating triglyceride levels and treating dyslipidemia (U.S. Patent Pub. No.'s 20030036504 and 20030143183); treating organ tissue injury caused by reperfusion of blood flow following ischemia (U.S. Patent Pub. No. 20020147131); treating coronary heart disease risk factor (CHDRF) syndrome (U.S. Patent Pub. No. 20020045636); and others. GLP-1 is, however, metabolically unstable, having a plasma half-life (t 1/2 ) of only 1-2 min in vivo. Exogenously administered GLP-1 is also rapidly degraded (Deacon, C. F., et al., Diabetes 44:1126-1131, 1995). This metabolic instability limits the therapeutic potential of native GLP-1.
[0006] A number of attempts have been taken to improve the therapeutic potential of GLP-1 and its analogs through improvements in formulation. For example, International patent publication no. WO 01/57084 describes a process for producing crystals of GLP-1 analogues which are said to be useful in the preparation of pharmaceutical compositions, such as injectable drugs, comprising the crystals and a pharmaceutical acceptable carrier. Heterogeneous micro crystalline clusters of GLP-1(7-37)OH have been grown from saline solutions and examined after crystal soaking treatment with zinc and/or m-cresol (Kim and Haren, Pharma. Res. Vol. 12 No. 11 (1995)). Crude crystalline suspensions of GLP(7-36)NH 2 containing needle-like crystals and amorphous precipitation have been prepared from phosphate solutions containing zinc or protamine (Pridal, et. al., International Journal of Pharmaceutics Vol. 136, pp. 53-59 (1996)). European patent publication no. EP 0619322A2 describes the preparation of micro-crystalline forms of GLP-1(7-37)OH by mixing solutions of the protein in pH 7-8.5 buffer with certain combinations of salts and low molecular weight polyethylene glycols (PEG). U.S. Pat. No. 6,566,490 describes seeding microcrystals of, inter alia, GLP-1 which are said to aid in the production of purified peptide products. U.S. Pat. No. 6,555,521 (U.S. '521) discloses GLP-1 crystals having a tetragonal flat rod or a plate-like shape which are said to have improved purity and to exhibit extended in vivo activity. U.S. '521 teaches that such crystals are relatively uniform and remain in suspension for a longer period of time than prior crystalline clusters and amorphous crystalline suspensions which were said to settle rapidly, aggregate or clump together, clog syringe needles and generally exacerbate unpredictable dosing.
[0007] A biodegradable triblock copolymer of poly [(dl-lactide-co-glycolide)-β-ethylene glycol-β-(-lactide-co-glycolide)] has been suggested for use in a controlled release formulation of GLP-1. However like other polymeric systems, the manufacture of triblock copolymer involves complex protocols and inconsistent particulate formation.
[0008] Similarly, biodegradable polymers, e.g., poly(lactic-co-glycolic acid) (PLGA), have also been suggested for use in sustained delivery formulations of peptides. However the use of such biodegradable polymers has been disfavored in the art since these polymers generally have poor solubility in water and require water-immiscible organic solvents, e.g., methylene chloride, and/or harsh preparation conditions during manufacture. Such organic solvents and/or harsh preparation conditions are considered to increase the risk of inducing conformational change of the peptide or protein of interest, resulting in decreased structural integrity and compromised biological activity. (Choi et al., Pharm. Research, Vol. 21, No. 5, (2004).) Poloxamers have been likewise faulted. (Id.)
[0009] The GLP-1 compositions described in the foregoing references are less than ideal for preparing pharmaceutical formulations of GLP's since they tend to trap impurities and/or are otherwise difficult to reproducibly manufacture and administer. Also, GLP analogs are known to induce nausea at elevated concentrations, thus there is a need to provide a sustained drug effect with reduced initial plasma concentrations. Hence, there is a need for GLP-1 formulations which are more easily and reliably manufactured, that are more easily and reproducibly administered to a patient, and that provide for reduced initial plasma concentrations in order to reduce or eliminate unwanted side-effects.
SUMMARY OF THE INVENTION
[0010] The invention may be summarized in the following paragraphs as well as the claims. Accordingly, it is a first object of the invention to provide a pharmaceutical composition comprising a GLP-1 analog according to formula (I):
(Aib 8,35 )hGLP-1(7-36)NH 2 (I)
or a pharmaceutically acceptable salt thereof, wherein the formulation of said composition provides for superior manufacturing, administration, pharmacokinetic and pharmacodynamic properties, as well as attenuated negative side-effects.
[0011] In a first aspect of said first object the invention provides for a pharmaceutical composition having an improved drug release profile, preferably with a reduced initial burst.
[0012] In a second aspect of said first object the invention provides for pharmaceutical composition comprising a compound of formula (I) having an extended duration of action.
[0013] In a third aspect of said first object the invention provides for a pharmaceutical composition comprising a compound of formula (I) or a pharmaceutically acceptable salt thereof and a pharmaceutically acceptable carrier or diluent. Preferably said carrier or diluent comprises water.
[0014] In a first preferred embodiment of said third aspect of said first object said pharmaceutical composition further comprises zinc. More preferably, said pharmaceutical composition comprises an aqueous mixture, suspension or solution, wherein said compound of formula (I) is present at a concentration of approximately 0.5%-30% (w/w). More preferably the concentration of said compound of formula (I) in said aqueous mixture, suspension or solution is approximately 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%,10%, 11%, 12%, 13%,14%, 15%,16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, or 30% (w/w). More preferably, the concentration of said compound of formula (I) in said aqueous solution is approximately 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%,10%, 11%, 14%, 15%, 16%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 29%, or 30% (w/w). More preferably still, the concentration of said compound of formula (I) in said aqueous solution is approximately 1%, 2%, 3%, 4%, 5%, 6%, 9%, 10%, 11%, 22%, 23%, 24%, 25%, or 26% (w/w). Even more preferably still, the concentration of said compound of formula (I) in said aqueous solution is approximately 1%, 2%, 3%, 4%, 5%, 6%, 10%, 22%, 23%, 24%, 25%, or 26% (w/w). Still more preferably, the concentration of said compound of formula (I) in said aqueous solution is approximately 1%, 2%, 5%, 10%, 23% or 25% (w/w).
[0015] In a second preferred embodiment of said third aspect of said first object, said pharmaceutical composition further comprises zinc, wherein the molar ratio of said compound of formula (I) to zinc in said pharmaceutical composition ranges from approximately 6:1 to approximately 1:1. More preferably, said ratio ranges from approximately 5.5:1 to approximately 1:1. More preferably still, said ratio ranges from approximately 5.4:1 to approximately 1.5:1. Even more preferably still, said ratio is approximately 5.4:1, 4.0:1, or 1.5:1. Most preferably, said ratio is approximately 1.5:1.
[0016] Preferably, in said second preferred embodiment of said third aspect of said first object, said zinc is provided as zinc chloride or zinc acetate. More preferably, said zinc acetate is provided as ZnAc 2 .2 H 2 O.
[0017] Preferably, in both of said first and second preferred embodiments of said third aspect of said first object, the pH of said pharmaceutical composition is adjusted upward using a base. More preferably, said pH adjustment is made using NaOH. More preferably still, the pH of said pharmaceutical composition is adjusted with NaOH such that, when diluted to approximately ½ initial concentration using 0.9% NaCl, a pH value of approximately 5.0-5.5 is obtained using direct potentiometric determination.
[0018] In a first preferred embodiment of said second aspect of said first object, the invention features a pharmaceutical composition according to said third aspect, including, independently for each occurrence, each of said preferred embodiments of said third aspect, wherein the composition is formulated such that the compound according to formula (I) is released within a subject in need thereof, e.g., a mammal, preferably a human, for an extended period of time. Preferably said release of said compound extends for at least one hour, more preferably at least 4, 6, 12, or 24 hours. More preferably still, said composition is formulated such that the compound according to formula (I) is released within a subject for at least 36, 48, 60, 72, 84, or 96 hours. More preferably still, said composition is formulated such that the compound according to formula (I) is released within a subject for at least approximately 5, 6, 7, 8, 9, 10, 11, 12, 13, or 14 days. More preferably still, said composition is formulated such that the compound according to formula (I) is released within a subject for at least approximately 2, 3 or 4 weeks.
[0019] It is a second object of the present invention to provide for a method of eliciting a GLP-1 agonist effect, said method comprising contacting a receptor of the GLP-1 (7-36)NH 2 ligand with the compound according to formula (I), said compound according to formula (I) being provided to said receptor, directly or indirectly, via a composition according to said third aspect, including, independently for each occurrence, each of said preferred embodiments of said third aspect.
[0020] In a first preferred embodiment of said second object of the invention, said receptor of the GLP-1(7-36)NH 2 ligand is present in an animal subject, preferably a primate, more preferably a human being. Thus, in this embodiment the present invention provides a method of eliciting an agonist effect from a GLP-1 receptor in a subject in need thereof which comprises administering to said subject a composition of the instant invention, wherein said composition comprises an effective amount of a compound of formula (I) or a pharmaceutically acceptable salt thereof.
[0021] In a more preferred embodiment of said second object of the invention, said subject is a human afflicted with, or at risk of developing, a disease or condition selected from the group consisting of Type I diabetes, Type II diabetes, gestational diabetes, obesity, excessive appetite, insufficient satiety, and metabolic disorder. Preferably said disease is Type I diabetes or Type II diabetes.
[0022] In another more preferred embodiment of said second object of the invention, said subject is a human afflicted with, or at risk of developing, a disease selected from the group consisting of Type I diabetes, Type II diabetes, obesity, glucagonomas, secretory disorders of the airway, arthritis, osteoporosis, central nervous system disease, restenosis, neurodegenerative disease, renal failure, congestive heart failure, nephrotic syndrome, cirrhosis, pulmonary edema, hypertension, and disorders wherein the reduction of food intake is desired, a disease or disorder of the central nervous system, (e.g., through modulation of neurogenesis, and e.g., Parkinson's Disease, Alzheimer's Disease, Huntington's Disease, ALS, stroke, ADD, and neuropsychiatric syndromes), irritable bowel syndrome, myocardial infarction (e.g., reducing the morbidity and/or mortality associated therewith), stroke, acute coronary syndrome (e.g., characterized by an absence of Q-wave myocardial infarction, post-surgical catabolic changes, hibernating myocardium or diabetic cardiomyopathy, insufficient urinary sodium excretion, excessive urinary potassium concentration, conditions or disorders associated with toxic hypervolemia, (e.g., renal failure, congestive heart failure, nephrotic syndrome, cirrhosis, pulmonary edema, and hypertension), polycystic ovary syndrome, respiratory distress, nephropathy, left ventricular systolic dysfunction, (e.g., with abnormal left ventricular ejection fraction), gastrointestinal disorders such as diarrhea, postoperative dumping syndrome and irritable bowel syndrome, (i.e., via inhibition of antro-duodenal motility), critical illness polyneuropathy (CIPN), systemic inflammatory response syndrome (SIRS), dyslipidemia, organ tissue injury caused by reperfusion of blood flow following ischemia, and coronary heart disease risk factor (CHDRF) syndrome.
[0023] In another aspect of said second object, the invention features a method of converting liver stem/progenitor cells into functional pancreatic cells, of preventing beta-cell deterioration and of stimulating beta-cell proliferation, of suppressing plasma blood levels of norepinepherine, of inducing an inotropic response and of increasing cardiac contractility, of improving nutrition via a non-alimentary route, (e.g., via intravenous, subcutaneous, intramuscular, peritoneal, or other injection or infusion rout), of pre-treating a subject to undergo an endoscopic procedures, and of modulating triglyceride levels, in a subject in need thereof, said method comprising administering to said subject a formulation of the present invention comprising an effective amount of a compound of formula (I) or a pharmaceutically acceptable salt thereof. Preferably said subject is a mammalian animal, more preferably a primate, more preferably still a human being.
[0024] With the exception of the N-terminal amino acid, all abbreviations (e.g. Ala) of amino acids in this disclosure stand for the structure of —NH—CH(R)—CO—, wherein R is the side chain of an amino acid (e.g., CH 3 for Ala). For the N-terminal amino acid, the abbreviation stands for the structure of (R 2 R 3 )—N—CH(R)—CO—, wherein R is a side chain of an amino acid and R 2 and R 3 are as defined above, except when A 7 is Ura, Paa or Pta, in which case R 2 and R 3 are not present since Ura, Paa and Pta are considered here as des-amino amino acids. Amp, 1Nal, 2Nal, Nle, Cha, 3-Pal, 4-Pal and Aib are the abbreviations of the following a-amino acids: 4-amino-phenylalanine, β-(1-naphthyl)alanine, β-(2-naphthyl)alanine, norleucine, cyclohexylalanine, β-(3-pyridinyl)alanine, β-(4-pyridinyl)alanine and α-aminoisobutyric acid, respectively. Other amino acid definitions are: Ura is urocanic acid; Pta is (4-pyridylthio) acetic acid; Paa is trans-3-(3-pyridyl) acrylic acid; Tma-His is N,N-tetramethylamidino-histidine; N-Me-Ala is N-methyl-alanine; N-Me-Gly is N-methyl-glycine; N-Me-Glu is N-methyl-glutamic acid; Tle is tert-butylglycine; Abu is α-aminobutyric acid; Tba is tert-butylalanine; Orn is ornithine; Aib is α-aminoisobutyric acid; β-Ala is β-alanine; Gaba is γ-aminobutyric acid; Ava is 5-aminovaleric acid; Ado is 12-aminododecanoic acid, Aic is 2-aminoindane-2-carboxylic acid; Aun is 11-aminoundecanoic acid; and Aec is 4-(2-aminoethyl)-1-carboxymethyl-piperazine, represented by the structure:
[0025] What is meant by Acc is an amino acid selected from the group of 1-amino-1-cyclopropanecarboxylic acid (A3c); 1-amino-1-cyclobutanecarboxylic acid (A4c); 1-amino-1-cyclopentanecarboxylic acid (A5c); 1-amino-1-cyclohexanecarboxylic acid (A6c); 1-amino-1-cycloheptanecarboxylic acid (A7c); 1-amino-1-cyclooctanecarboxylic acid (A8c); and 1-amino-1-cyclononanecarboxylic acid (A9c). In the above formula, hydroxyalkyl, hydroxyphenylalkyl, and hydroxynaphthylalkyl may contain 1-4 hydroxy substituents. COX 5 stands for —C═OX 5 . Examples of —C═OX 5 include, but are not limited to, acetyl and phenylpropionyl.
[0026] The full names for other abbreviations used herein are as follows: Boc for t-butyloxycarbonyl, HF for hydrogen fluoride, Fm for formyl, Xan for xanthyl, Bzl for benzyl, Tos for tosyl, DNP for 2,4-dinitrophenyl, DMF for dimethylformamide, DCM for dichloromethane, HBTU for 2-(1H-Benzotriazol-1-yl)-1,1,3,3-tetramethyl uronium hexafluorophosphate, DIEA for diisopropylethylamine, HOAc for acetic acid, TFA for trifluoroacetic acid, 2CIZ for 2-chlorobenzyloxycarbonyl, 2BrZ for 2-bromobenzyloxycarbonyl, OcHex for O-cyclohexyl, Fmoc for 9-fluorenylmethoxycarbonyl, HOBt for N-hydroxybenzotriazole; PAM resin for 4-hydroxymethylphenylacetamidomethyl resin; Tris for Tris(hydroxymethyl)aminomethane; and Bis-Tris for Bis(2-hydroxyethyl)amino-tris(hydroxymethyl)methane (i.e., 2-Bis(2-hydroxyethyl)amino-2-(hydroxymethyl)-1,3-propanediol).
[0027] The term “halo” or “halogen” encompasses fluoro, chloro, bromo and iodo.
[0028] The terms “(C 1 -C 12 )hydrocarbon moiety”, “(C 1 -C 30 )hydrocarbon moiety” and the like encompass branched and straight chain alkyl, alkenyl and alkynyl groups having the indicated number of carbons, provided that in the case of alkenyl and alkynyl there is a minimum of two carbons.
[0029] A peptide of this invention is also denoted herein by another format, e.g., (Aib 8,35 )hGLP-1(7-36)NH 2 , with the substituted amino acids from the natural sequence placed between the first set of parentheses (e.g., Aib 8,35 denotes that Aib is substituted for Ala 8 and Gly 35 in hGLP-1). The abbreviation GLP-1 means glucagon-like peptide-1; hGLP-1 means human glucagon-like peptide-1. The numbers between the second set of parentheses refer to the number of amino acids present in the peptide (e.g., hGLP-1(7-36) refers to amino acids 7 through 36 of the peptide sequence for human GLP-1). The sequence for hGLP-1(7-37) is listed in Mojsov, S., Int. J. Peptide Protein Res,. 40, 1992, pp. 333-342. The designation “NH 2 ” in hGLP-1(7-36)NH 2 indicates that the C-terminus of the peptide is amidated. hGLP-1(7-36) means that the C-terminus is the free acid. In hGLP-1(7-38), residues in positions 37 and 38 are Gly and Arg, respectively, unless otherwise indicated.
BRIEF DESCRIPTION OF THE DRAWING
[0030] FIG. 1 is a schematic illustration which depicts a syringe-based device useful for assuring homogeneity of semi-solid compositions of the invention.
DETAILED DESCRIPTION
[0000] Synthesis of Peptides
[0031] Peptides useful for practicing the present invention can be and were prepared by standard solid phase peptide synthesis. See, e.g., Stewart, J. M., et al., Solid Phase Synthesis (Pierce Chemical Co., 2d ed. 1984). The substituents R 2 and R 3 of the above generic formula may be attached to the free amine of the N-terminal amino acid by standard methods known in the art. For example, alkyl groups, e.g., (C 1 -C 30 )alkyl, may be attached using reductive alkylation. Hydroxyalkyl groups, e.g., (C 1 -C 30 )hydroxyalkyl, may also be attached using reductive alkylation wherein the free hydroxy group is protected with a t-butyl ester. Acyl groups, e.g., COE 1 , may be attached by coupling the free acid, e.g., E 1 COOH, to the free amine of the N-terminal amino acid by mixing the completed resin with 3 molar equivalents of both the free acid and diisopropylcarbodiimide in methylene chloride for one hour. If the free acid contains a free hydroxy group, e.g., p-hydroxyphenylpropionic acid, then the coupling should be performed with an additional 3 molar equivalents of HOBT.
[0032] When R 1 is NH—X 2 —CH 2 —CONH 2 , (i.e., Z 0 =CONH 2 ), the synthesis of the peptide starts with BocHN—X 2 —CH 2 —COOH which is coupled to the MBHA resin. If R 1 is NH—X 2 —CH 2 —COOH, (i.e., Z 0 =COOH) the synthesis of the peptide starts with Boc-HN—X 2 —CH 2 —COOH which is coupled to PAM resin. For this particular step, 4 molar equivalents of Boc-HN—X 2 —COOH, HBTU and HOBt and 10 molar equivalents of DIEA are used. The coupling time is about 8 hours.
[0033] The protected amino acid 1-(N-tert-butoxycarbonyl-amino)-1-cyclohexane-carboxylic acid (Boc-A6c-OH) was synthesized as follows. 19.1 g (0.133 mol) of 1-amino-1-cyclohexanecarboxylic acid (Acros Organics, Fisher Scientific, Pittsburgh, Pa.) was dissolved in 200 ml of dioxane and 100 ml of water. To it was added 67 ml of 2N NaOH. The solution was cooled in an ice-water bath. 32.0 g (0.147 mol) of di-tert-butyl-dicarbonate was added to this solution. The reaction mixture was stirred overnight at room temperature. Dioxane was then removed under reduced pressure. 200 ml of ethyl acetate was added to the remaining aqueous solution. The mixture was cooled in an ice-water bath. The pH of the aqueous layer was adjusted to about 3 by adding 4N HCl. The organic layer was separated. The aqueous layer was extracted with ethyl acetate (1×100 ml). The two organic layers were combined and washed with water (2×150 ml), dried over anhydrous MgSO 4 , filtered, and concentrated to dryness under reduced pressure. The residue was recrystallized in ethyl acetate/hexanes. 9.2 g of the pure product was obtained. 29% yield.
[0034] Boc-A5c-OH was synthesized in an analogous manner to that of Boc-A6c-OH. Other protected Acc amino acids can be prepared in an analogous manner by a person of ordinary skill in the art as enabled by the teachings herein.
[0035] In the synthesis of a peptide containing A5c, A6c and/or Aib, the coupling time is 2 hrs. for these residues and the residue immediately following them.
[0036] The substituents R 2 and R 3 of the above generic formula can be attached to the free amine of the N-terminal amino acid by standard methods known in the art. For example, alkyl groups, e.g., (C 1 -C 30 )alkyl, can be attached using reductive alkylation. Hydroxyalkyl groups, e.g., (C 1 -C 30 )hydroxyalkyl, can also be attached using reductive alkylation wherein the free hydroxy group is protected with a t-butyl ester. Acyl groups, e.g., COX 1 , can be attached by coupling the free acid, e.g., X 1 COOH, to the free amine of the N-terminal amino acid by mixing the completed resin with 3 molar equivalents of both the free acid and diisopropylcarbodiimide in methylene chloride for about one hour. If the free acid contains a free hydroxy group, e.g., p-hydroxyphenylpropionic acid, then the coupling should be performed with an additional 3 molar equivalents of HOBT.
[0037] The following examples describe synthetic methods that can be and were used for making peptides with which the instant invention may advantageously be practiced, which synthetic methods are well-known to those skilled in the art. Other methods are also known to those skilled in the art. The examples are provided for the purpose of illustration and are not meant to limit the scope of the present invention in any manner.
[0038] Boc-βAla-OH, Boc-D-Arg(Tos)-OH and Boc-D-Asp(OcHex) were purchased from Nova Biochem, San Diego, Calif. Boc-Aun-OH was purchased from Bachem, King of Prussia, PA. Boc-Ava-OH and Boc-Ado-OH were purchased from Chem-Impex International, Wood Dale, Ill. Boc-2Nal-OH was purchased from Synthetech, Inc. Albany, Oreg.
EXAMPLE 1
[0039] (Aib 8,35 )hGLP-1(7-36)NH 2
[0040] A detailed synthesis procedure for (Aib 8,35 )hGLP-1(7-36)NH 2 has been provided in International Patent Publication No. WO 00/34331 (PCT/EP99/09660), the contents of which are incorporated herein in their entirety. Briefly, the compound was synthesized on an Applied Biosystems (Foster City, Calif.) model 430A peptide synthesizer which was modified to do accelerated Boc-chemistry solid phase peptide synthesis. See Schnolzer, et al., Int. J. Peptide Protein Res., 90:180 (1992). 4-methylbenzhydrylamine (MBHA) resin (Peninsula, Belmont, Calif.) with the substitution of 0.91 mmol/g was used. The Boc amino acids (Bachem, Calif., Torrance, Calif.; Nova Biochem., LaJolla, Calif.) were used with the following side chain protection: Boc-Ala-OH, Boc-Arg(Tos)-OH, Boc-Asp(OcHex)-OH, Boc-Tyr(2BrZ)-OH, Boc-His(DNP)-OH, Boc-Val-OH, Boc-Leu-OH, Boc-Gly-OH, Boc-Gln-OH, Boc-Ile-OH, Boc-Lys(2CIZ)-OH, Boc-Thr(Bzl)-OH, Boc-Ser(Bzl)-OH, Boc-Phe-OH, Boc-Aib-OH, Boc-Glu(OcHex)-OH and Boc-Trp(Fm)-OH. The Boc groups were removed by treatment with 100% TFA for 2×1 min. Boc amino acids (2.5 mmol) were pre-activated with HBTU (2.0 mmol) and DIEA (1.0 mL) in 4 mL of DMF and were coupled without prior neutralization of the peptide-resin TFA salt. Coupling times were 5 min. except for the Boc-Aib-OH residues and the following residues, Boc-Lys(2CIZ)-OH and Boc-His(DNP)-OH wherein the coupling times were 2 hours.
[0041] At the end of the assembly of the peptide chain, the resin was treated with a solution of 20% mercaptoethanol/10% DIEA in DMF for 2×30 min. to remove the DNP group on the His side chain. The N-terminal Boc group was then removed by treatment with 100% TFA for 2×2 min. After neutralization of the peptide-resin with 10% DIEA in DMF (1×1 min), the formyl group on the side chain of Trp was removed by treatment with a solution of 15% ethanolamine/15% water/70% DMF for 2×30 min. The peptide-resin was washed with DMF and DCM and dried under reduced pressure. The final cleavage was done by stirring the peptide-resin in 10 mL of HF containing 1 mL of anisole and dithiothreitol (24 mg) at 0° C. for 75 min. HF was removed by a flow of nitrogen. The residue was washed with ether (6×10 mL) and extracted with 4N HOAc (6×10 mL).
[0042] The peptide mixture in the aqueous extract was purified on reverse-phase preparative high pressure liquid chromatography (HPLC) using a reverse phase VYDAC® C 18 column (Nest Group, Southborough, Mass.). The column was eluted with a linear gradient (20% to 50% of solution B over 105 min.) at a flow rate of 10 mL/min (Solution A=water containing 0.1% TFA; Solution B=acetonitrile containing 0.1% of TFA). Fractions were collected and checked on analytical HPLC. Those containing pure product were combined and lyophilized to dryness. In one example of synthesis of this compound, 135 mg of a white solid was obtained. Purity was 98.6% based on analytical HPLC analysis. Electro-spray mass spectrometer (MS(ES))S analysis gave the molecular weight at 3339.7 (in agreement with the calculated molecular weight of 3339.7).
[0000] Formulation Procedures—Part I
[0000] 1. Materials
[0043] ZnCl 2 , NaOH pellets, and hydrochloric acid, 35%, were obtained from Panreac Quimica, Barcelona, Spain. WFI (sterile water for injection/irrigation) was obtained from B. Braun Medical, Barcelona, Spain.
[0000] 2. Preparation of Stock Solutions
[0000] A. Preparation of a ZnCl 2 Stock Solution with Concentration Between 1-4 mg/mL, Dissolving with HCl pH=3.
[0044] 1. Add HCl 35% to WFI while stirring, to achieve pH=3. Measure pH to confirm.
[0045] 2. In a volumetric flask, transfer a weighed amount of ZnCl2. Add enough HCl pH=3 (from step A.1) to volume and stir. Final concentration to be approximately 1-4 mg ZnCl2/mL. B. Preparation of a NaOH stock solution with concentration between 0.1-10 mg/mL, dissolving with water for injection.
[0046] 1. In a volumetric flask, transfer a weighed amount of NaOH. Add enough WFI to volume and stir. Final concentration to be 0.1-10 mg NaOH/mL.
[0000] Preparation of compositions with 1-2-10% peptide and ZnCl2, without adjusting pH upward with base (e.g., from a freeze-dried vial)—Preparation of a freeze-dried composition with (Aib 8,35 )HGLP-1 (7-36)NH 2
[0000] C. 20 mg (Aib 8,35 )HGLP-1(7-36)NH 2 /vial:
[0000]
1. In a volumetric flask, transfer an exact volume of acetic acid. Add enough WFI to volume and stir. Final concentration to be 0.04% (VN).
2. In a volumetric flask, transfer a weighed amount of (Aib 8,35 )HGLP-1(7-36)NH 2 (acetate salt). Add sufficient 0.04% acetic acid (from step C.1), with stirring, to bring final concentration to 20 mg (Aib 8,35 )HGLP-1(7-36)NH 2 /mL. After sterile filtration, 1 ml aliquots of the solution are transferred to lyophilization vials and freeze dried.
D. 50 mg (Aib 8,35 )HGLP-1(7-36)NH 2 /vial:
1. In a volumetric flask, transfer an exact volume of acetic acid. Add enough WFI to volume and stir. Final concentration to be 0.1% (VN)
2. In a volumetric flask, transfer a weighed amount of (Aib 8,35 )HGLP-1(7-36)NH 2 . Add enough acetic acid 0.1% (from step D.1) to achieve a final concentration of 50 mg (Aib 8,35 )HGLP-1(7-36)NH 2 /mL. After sterile filtration, 1 ml aliquots of the solution are transferred to lyophilization vials and freeze dried.
Preparation of a ZnCl2 solution with a desired concentration:
1. In a volumetric flask, transfer an aliquot ZnCl2 stock solution. Sufficient HCl (pH=3, from step
A.1) is added to achieve target composition in view of peptide raw material. (See F.1., below.)
2. A known weight of peptide is stirred with the necessary volume (100% of total volume of excipient) of solution of ZnCl2 from 1., to achieve the target concentration (e.g., 1%, 2% or 10% (w/w)).
1% compositions: Take a vial with 20 mg (Aib 8,35 )HGLP-1 (7-36)NH 2 (step C) and add 2 mL of ZnCl2 solution of proper concentration (See F.1., below) 2% compositions: Take a vial with 20 mg (Aib 8,35 )HGLP-1(7-36)NH 2 (step C) and add 1 mL of ZnCl2 solution of proper concentration (See F.1., below) 10% compositions: Take a vial with 50 mg (Aib 8,35 )HGLP-1(7-36)NH 2 (step D) and add 0.45 mL of ZnCl2 solution of proper concentration (See F.1., below)
Shake Until Dissolution.
Compositions with 1-2-10% peptide and ZnCl2, without upward adjustment of pH (standard liquid composition method. See F.2., below)
Preparation of a ZnCl2 solution with the appropriate concentration: Take an aliquot of the stock solution (from Formulation Procedures—Part I, subpart A, above), and adding HCl (pH=3 to volume.
1. In a volumetric flask, transfer an aliquot ZnCl2 stock solution. Add enough HCl pH=3 (from step A.1) to volume and stir. Final concentration must be adjusted to every composition and peptide raw material (See F.1., below)
Take a known weight of peptide and add the necessary weight (100% of total weight of excipient) of the immediately foregoing ZnCl2 solution to achieve the target concentration (1%, 2% or 10% (w/w)).
1. In a flask, transfer a weighed amount of (Aib 8,35 )HGLP-1(7-36)NH 2 (acetate salt). Add enough ZnCl2 solution of proper concentration (See F.1., below) to achieve the target composition (i.e.: 1%, 2% or 10% w/w) and stir to homogenize. The composition is then sterile filtered and sealed in a final container.
Compositions with 1-2-10% peptide, ZnCl2 and upward adjusted pH (from a freeze-dried vial). Preparation of a ZnCl2 solution with the appropriate concentration:
1. In a volumetric flask, transfer an aliquot ZnCl2 stock solution. Add enough HCl pH=3 (from step A.1) to volume and stir. Final concentration must be adjusted to every composition and peptide raw material (See F. 1., below)
Take a known weight of peptide and add the necessary volume (90% of total volume of excipient) of the immediately foregoing ZnCl2 solution related to achieve an intermediate product.
1% compositions: Take a vial with 20 mg (Aib 8,35 )HGLP-1(7-36)NH 2 (step C) and add 1.8 mL of ZnCl2 solution of proper concentration (See F.1., below) 2% compositions: Take a vial with 20 mg (Aib 8,35 )HGLP-1(7-36)NH 2 (step C) and add 0.9 mL of ZnCl2 solution of proper concentration (See F.1., below) 10% compositions: Take a vial with 50 mg (Aib 8,35 )HGLP-1(7-36)NH 2 (step D) and add 0.40 mL of ZnCl2 solution of proper concentration (See F.1., below) Shake until dissolution.
Add the necessary volume (10% of total volume of excipient) of diluted NaOH solution (depending on Peptide & Acetate content in peptide raw material, and target peptide concentration in composition) to achieve the target concentration & pH.
1% compositions: Add 0.2 mL of NaOH solution of proper concentration 2% compositions: Add 0.1 mL of NaOH solution of proper concentration 10% compositions: Add 0.05 mL of NaOH solution of proper concentration Shake until dissolution.
Compositions with 1-2-10-25% peptide, ZnCl2 and increasing pH (for 1, 2 & 10% compositions use liquid formulation process (see F.2., below); for 25% formulation use semi-solid/gel formulation process (see F.3., below.)).
Preparation of a ZnCl2 solution with the appropriate concentration: taking an aliquot of the stock solution from 2.A., above, and adding HCl pH 3 to volume.
1. In a volumetric flask, transfer an aliquot ZnCl2 stock solution. Add enough HCl pH=3 (from step A.1) to volume and stir. Final concentration must be adjusted to every composition and peptide raw material (See F.1., below)
Take a known weight of peptide and to add the necessary weight (75% of weight of total excipient) of solution of ZnCl2 related in last point, to achieve an intermediate product.
1. In a flask (or a syringe like container for 25% formulation by semi-solid/gel process, below), transfer a weighed amount of (Aib 8,35 )HGLP-1 (7-36)NH 2 C. Add enough ZnCl2 solution of proper concentration (See F.1., below). Stir to homogenize (if liquid formulation process) or push-pull to homogenize (if semi-solid/gel process).
Add the necessary weight (25% of total weight of excipient) of diluted NaOH solution (depending on Peptide & Acetate content in API, and target peptide concentration in composition) to achieve the target concentration & pH.
Stir to homogenize (if liquid formulation process) or push-pull to homogenize (if semi-solid/gel process).
Necessary weight/volume of excipient.
[0067] The total weight of excipient (E) to be added in each composition is be calculated as follows:
E =Weight of excipient (mg)=( A× 100 /T )−(A/P)
wherein:
[0068] A=content of pure peptide (mg);
[0069] T=target concentration of the composition; e.g., 1, 2, 10 or 25 if target is 1%, 2%, 10% or 25%, respectively; and
[0070] P=content of pure peptide (mg peptide/100 mg formulation) of raw material.
[0071] With respect to the total volume of excipient, the assumption that 1 mL=1 g is applied (e.g., re: freeze-dried compositions).
[0072] Volumes/Weights (W) of solution of ZnCl2 that must be added to each composition (mg solution or mL solution),
[0073] Compositions in which pH is not adjusted with base, e.g., NaOH: W=100% E;
[0074] Compositions in which pH is not adjusted with base, e.g., NaOH, and liquid formulation process (below) or semi-solid/gel process (also below): W=75% E;
[0075] Compositions with increased pH and freeze-dried reconstitution: W=90% E.
[0076] Volumes/Weights (W) of solution of NaOH that must be added to each composition (mg solution or mL solution),
[0077] Compositions with base-adjusted pH and liquid formulation process or semi-solid/gel process. W=25% E; and
[0078] Compositions with increased pH & increased pH and freeze-dried reconstitution: W=10% E.
[0000] F.1. Appropriate concentrations of ZnCl2
[0079] The appropriate concentration of ZnCl2 to be used in each composition is be calculated as follows:
Concentration ZnCl2 (mg/mL) or (mg/g)=(136.29 ×A )/( W× 3339.76×R)
wherein:
A; Content of pure peptide (mg).
[0080] T: Target concentration of the composition, being 1, 2, 10 or 25 if target is 1%, 2%, 10% or 25%.
[0081] R: Molar Ratio Peptide/Zn, being R=1.5, for 1, 2 & 10% compositions or R=4.0 for 25% compositions.
[0082] W: Weight (g) or Volume (mL) of solution of ZnCl2 that must be added to each composition (g solution or mL solution).
[0000] F.2. Liquid Formulation Process
[0083] As noted herein, certain formulations of the current invention can be and were produced using the following liquid formulation process. By was of illustration, examples C5, C6, C7, C8, C9, C10, C11, C12 and C13 all were prepared essentially according to the following procedure. In each of the foregoing examples NaOH was used to adjust the pH of the composition.
[0084] 1) The raw Peptide is accurately weighed into a glass vial.
[0085] 2) The total composition amount and liquid volume are calculated according to Peptide content in peptide raw material and in view of the desired final composition.
[0086] 3) The total liquid volume to be used in compositions is split up between the zinc and the NaOH solutions.
[0087] 4) Zinc salt concentration is adjusted so that the total zinc amount needed is incorporated with 80% total liquid volume in the composition.
[0088] 5) The zinc solution (either ZnCl2 or ZnAc 2 .2H 2 O) is accurately weighed and transferred to peptide vial.
[0089] 6) The composition is stirred until homogenization and peptide content is determined in the intermediate product as an “in process” control.
[0090] 7) Once the target peptide content in the intermediate product is concluded, the remaining intermediate bulk product is accurately weighed and the amount of NaOH solution calculated (the remaining 20% volume is added as NaOH solution).
[0091] 8) The NaOH solution is accurately weighed and transferred to the vial.
[0092] 9) The composition is stirred until homogenization.
[0000] F.3. Semi-solid/Gel Formulation Process
[0093] Reference is made to FIG. 1 herein, which depicts the steps followed in order to obtain homogeneous compositions for examples C1-C4.
[0094] a. Examples C1, and C2 were prepared essentially according to the following procedures.
[0095] 1) The peptide is accurately weighed into the barrels of a disposable syringe S 1 . The syringe is previously fitted with a special two-way hand valve HV (I.D.=0.5 mm), the tubing placed inside the syringe Luer hole.
[0096] 2) The syringe plunger is secured with a stainless steel rod SR.
[0097] 3) HV in S 1 is connected to a vacuum source and HV is opened. After 10 min HV is closed.
[0098] 4) The solvent (Zinc solution) is accurately weighed into a second disposable syringe S 2 .
[0099] 5) S 2 is then connected to the free part of HV.
[0100] 6) HV is opened and the solvent is pulled by the vacuum inside the powder container S 1 . 7) HV is closed and the solvent syringe S2 is removed, while the solvent hydrates the powder in S 1 .
[0101] 8) SR is removed and the syringe plunger is slowly released (a fast movement would compress the mixture).
[0102] 9) The syringe plunger is moved (push and pull), without opening HV, so that the powder mass is fully soaked by solvent.
[0103] 10) A special two-way stainless connector SC (I.D.=1.0 mm) is placed in syringe S2 (the tubing placed inside the syringe Luer hole) and its plunger is pushed to the end.
[0104] 11) HV in S 1 is opened to vent vacuum and then HV is removed. The syringe plunger is moved so that air chamber in the syringe barrel is minimized.
[0105] 12) S 1 and S 2 are connected by SC and the composition is kneaded from S 1 to S 2 through SC.
[0000] b) Compositions Including Peptide and Zinc Salt and NaOH Solutions
[0106] Examples C3 and C4 included NaOH in their compositions. The total liquid volume to be used in those batches is split up between the zinc and the NaOH solutions. Therefore, zinc salt concentration is adjusted so that the total zinc amount needed is incorporated with 50% total liquid volume in composition (step 4 ). The remaining 50% volume is added as NaOH solution and additional steps are required, as follows:
[0107] 13) After homogenization, peptide content is determined in the intermediate product (from step 12 ) as an “in process” control.
[0108] 14) Once the target peptide content in the intermediate product is concluded, the remaining intermediate bulk product is accurately weighed and the amount of NaOH solution calculated.
[0109] 15) The NaOH solution is accurately weighed into a third disposable syringe S 3 .
[0110] 16) The syringe plungers are pushed so that air chambers in the syringes are minimized. Both syringes are connected by SC and the composition is kneaded through SC.
[0111] Formulation Procedures—Part II
Ex. **Peptide:Zn Peptide No. *Peptide % Solution Ratio Dose C1 10 ZnCl 2 0.846 mg/ml 5.4:1 1 mg C2 5 0.40 mg ZnCl 2 /mL 5.4:1 1 C3 10 50% ZnCl 2 1.69 mg/mL, 50% NaOH 1 mg/mL 5.4:1 1 C4 10 50% ZnCl 2 2.28 mg/mL, 50% NaOH 1 mg/mL 4:1 1 C5 5 80% ZnCl 2 0.674 mg/mL, 20% NaOH 3.81 mg/mL 4:1 1 C6 2 80% ZnCl 2 0.26 mg/mL, 20% NaOH 2.15 mg/mL 5.4:1 1 C7 10 80% ZnCl 2 3.81 mg/mL, 20% NaOH 4.47 mg/mL 1.5:1 1 C8 10 80% ZnAc 2 .2H 2 O 2.3 mg/mL, 20% NaOH 6.1 mg/mL 4:1 1 C9 2 80% ZnCl 2 0.695 mg/mL, 20% NaOH 1.75 mg/mL 1.5:1 1 C10 2 80% ZnAc 2 .2H 2 O 1.12 mg/mL, 20% NaOH 1.44 mg/mL 1.5:1 1 C11 2 80% ZnCl 2 0.695 mg/mL, 20% NaOH 1.75 mg/mL 1.5:1 1 C12 1 80% ZnCl 2 0.384 mg/mL, 20% NaOH 0.875 mg/mL 1.5:1 1 C13 10 80% ZnCl 2 3.85 mg/mL, 20% NaOH 4.47 mg/mL 1.5:1 15 *Target value shown. Actual value within 5% of target in all cases. **Target value shown. Actual values within 10% of target in all cases
Determination of GLP-1 Receptor Affinity
[0112] A compound useful to practice the present invention can be tested for its ability to bind to the GLP-1 receptor using the following procedure.
[0000] Cell Culture:
[0113] RIN 5F rat insulinoma cells (ATCC-# CRL-2058, American Type Culture Collection, Manassas, Va.), expressing the GLP-1 receptor, were cultured in Dulbecco's modified Eagle's medium (DMEM) containing 10% fetal calf serum, and maintained at about 37° C. in a humidifed atmosphere of 5% CO 2 /95% air.
[0000] Radioligand Binding:
[0114] Membranes were prepared for radioligand binding studies by homogenization of the RIN cells in 20 ml of ice-cold 50 mM Tris-HCl with a Brinkman Polytron (Westbury, N.Y.) (setting 6,15 sec). The homogenates were washed twice by centrifugation (39,000 g/10 min), and the final pellets were resuspended in 50 mM Tris-HCl, containing 2.5 mM MgCl 2 , 0.1 mg/ml bacitracin (Sigma Chemical, St. Louis, Mo.), and 0.1% BSA. For assay, aliquots (0.4 ml) were incubated with 0.05 nM ( 125 I)GLP-1(7-36) (˜2200 Ci/mmol, New England Nuclear, Boston, Mass.), with and without 0.05 ml of unlabeled competing test peptides. After a 100 min incubation (25° C.), the bound ( 125 I)GLP-1(7-36) was separated from the free by rapid filtration through GF/C filters (Brandel, Gaithersburg, Md.), which had been previously soaked in 0.5% polyethyleneimine. The filters were then washed three times with 5 ml aliquots of ice-cold 50 mM Tris-HCl, and the bound radioactivity trapped on the filters was counted by gamma spectrometry (Wallac LKB, Gaithersburg, Md.). Specific binding was defined as the total ( 125 I)GLP-1(7-36) bound minus that bound in the presence of 1000 nM GLP1(7-36) (Bachem, Torrence, Calif.).
[0000] B. Determination of Solubility vs pH
[0115] B.1. Determination of Compound Solubility vs pH in Buffered Saline
[0116] A compound that may advantageously be used to practice the invention can be tested to determine its solubility in PBS at different pHs and temperatures using the following procedure.
[0117] A stock PBS buffered solution is made by dissolving one packet of pre-mixed powder (SIGMA, Product No.: P-3813) in one liter of de-ionized water to yield 10 mM phosphate-buffered saline with 138 mM NaCl, 2.7 mM KCl, and a pH of 7.4. PBS buffers with different pH values may be made by adjusting the pH of this stock solution with phosphoric acid and/or sodium hydroxide.
[0118] 2 mg samples of a compound to be tested, e.g., a compound of Example 1, may be weighed into glass vials. Into each vial is added a 50 μl aliquot of PBS buffer at a certain pH. The solution is vortexed, and if necessary sonicated, until clear. For each pH tested the total volume of buffer needed to dissolve 2 mg of the compound is recorded and the solubility was calculated.
[0119] Peptide solutions that are clear at room temperature (20-25° C.) are placed in a refrigerator (4° C.) overnight and the solubility of the peptide at 4° C. is then examined.
[0120] B.2. Determination of Compound Solubility vs pH in Saline
[0121] A compound that may advantageously be used to practice the invention can be tested to determine its solubility in saline at different pH values and temperatures using the following procedure.
[0122] A stock saline solution is prepared by dissolving 9 grams of NaCl in one liter of de-ionized water. Saline solutions with different pH values are made by adjusting the pH of this stock solution with HCl and/or NaOH. 2 mg samples of a compound to be tested, e.g., a compound of example 1, are weighed into glass vials. Into each vial is added a 50 μl aliquot of saline solution at a certain pH. The vial is vortexed and, if necessary, sonicated until clear. For each tested pH the total volume of saline needed to dissolve 2 mg of the compound is recorded and the solubility is calculated.
[0123] Solutions that are clear at room temperature (20-25° C.) are placed in a refrigerator (4° C.) overnight and the solubility at 4° C. then examined.
[0124] B.3. Determination of Compound Solubility in Saline at pH 7.0
[0125] Compounds that may advantageously be used to practice the invention can be tested to determine their solubility at room temperature in saline having pH=7 using the following procedure.
[0126] Saline solution is prepared by dissolving 9 grams of NaCl in one liter of de-ionized water. A 2 mg sample of a compound to be tested, e.g., a compound of example 1, is weighed into a glass vial and 1 mL aliquots of saline are added, with vortexing and sonication, until clear. The total volume of saline used to dissolve 2 mg of peptide is recorded and the solubility at room temperature is calculated.
[0127] B.4. Determination of Compound Solubility in Saline at various pH
[0128] Compounds that may advantageously be used to practice the invention can be tested to determine their solubility at room temperature in saline solutions having various pH values using the following procedure.
[0129] A stock saline solution is prepared by dissolving 9 grams of NaCl in one liter of de-ionized water. Saline solutions having various pH values are obtained by treating aliquots of this stock saline solution with HCl and NaOH.
[0130] A 2 mg sample of a compound to be tested, e.g., the compound of example 1, is are weighed into glass vials. Aliquots of 50 μl of a saline buffer at a certain pH are added. The solution is vortexed and sonicated until clear. The total volume of buffer used to dissolve 2 mg of peptide is recorded and the solubility is calculated.
[0000] C. Determination of Aqueous Solubility of Compound vs Zinc Concentration
[0131] A compound that may advantageously be used to practice the invention can be tested to determine its solubility in pH 7 water at different zinc concentrations using the following procedure.
[0132] A stock zinc solution is prepared by dissolving ZnCl 2 in de-ionized water to a concentration of 100 mg/ml and adjusting the pH to 2.7 using HCl. Solutions having various ZnCl 2 concentrations (“Zn Test Solutions”) are prepared by making appropriate dilutions of the stock solution.
[0133] 1 mg of a compound to be tested, e.g., the compound of example 1, is dissolved in 250 μl of each Zh Test Solution to yield a solution having 4 mg/ml of the compound. The pH of this solution is then adjusted using 0.2 N NaOH until white precipitates are observed to form. The precipitation solution was centrifuged and the mother liquor analyzed using HPLC. The UV absorption area of test compound peak is measured and the concentration of the test compound in the mother liquor is determined via comparison to a calibration curve.
[0134] As a representative example of a compound that may be used to practice the invention, the compound of Example 1 was tested in the immediately foregoing assay and the following results were obtained (aqueous saline, pH 7.0, room temperature):
TABLE 2 ZnCl 2 concentration Solubility (μg/mL) (mg/mL) 0 5.788 80 0.0770 500 0.0579 1000 0.0487 1500 0.0668 2500 0.1131
F. Determination of pl Using IEF Gels
[0135] Invitrogen's Novex IEF pH3-10 gels may be used to measure the pl of GLP-1 peptides. Peptidyl compounds to be tested are dissolved in water to a concentration of 0.5 mg/ml. For each such compound, 5 μl of the resulting solution is mixed with 5 μl of Novex® Sample Buffer 2× (comprised of 20 mM Arginine free base, 20 mM Lysine free base and 15% Glycerol) and the resulting 10 μl sample solution is loaded onto the gel along with a protein standard sample.
[0136] Running buffers are also obtained from Invitrogen and the gel is run according to manufacture's instructions, generally as follows: 100 V constant for 1 hour, followed by 200 V constant for 1 hour, followed by 500 V constant for 30 minutes.
[0137] The gel is then fixed in 12% TCA containing 3.5% sulfosalicylic acid for 30 minutes, and then stained for 2 hours with Colloidal Coomassie Blue according to the instructions found on the Novexe Colloidal Blue Kit thereafter, then de-stained in water overnight.
[0138] The gel is scanned and analyzed by the program Fragment Analysis 1.2. pl's of unknown peptides are calculated relative to the pl's of standard compounds having pl values of: 10.7, 9.5, 8.3, 8.0, 7.8, 7.4, 6.9, 6.0, 5.3, 5.2, 4.5, 4.2, and 3.5.
[0000] G. In Vivo Assays
[0139] Compositions of the present invention can be tested to determine their ability to promote and enhanced effect in vivo using the following assays.
[0140] G.1. Experimental Procedure:
[0141] The day prior to the experiment, adult male Sprague-Dawley rats (Taconic, Germantown, N.Y.) that weighed approximately 300-350 g were implanted with a right atrial jugular cannula under chlorohydrate anesthetic. The rats were then fasted for 18 hours prior to the injection of the appropriate test composition or vehicle control at time 0. The rats continued to be fasted throughout the entire experiment.
[0142] A 0.5 mg/ml ZnCl 2 solution was prepared by dilution of a solution of 100 mg/ml ZnCl 2 in an HCl solution having pH 2.7 water. 1 mg of the compound of formula (I) ((Aib 8,35 )hGLP1(7-36)NH 2 ) was dissolved in 250 μl of this solution to yield a clear solution having 4 mg/ml of the compound and 0.5 mg/ml Zn at pH 4.
[0143] At time zero the rats were injected subcutaneously (sc) either with (a) the immediately forgoing solution of (Aib 8 , 35 )hGLP-1(7-36)NH 2 ), or with vehicle control. In both cases the injection volume was very small (4-6 μL) and the dose of GLP-1 compound administered to the subject was 75 μg/kg. At the appropriate time after the sc injections a 500 μl blood sample was withdrawn via the intravenous (iv) cannula and the rats were given an iv glucose challenge to test for the presence of enhanced insulin secretion. The times of the glucose challenge were 0.25, 1, 6, 12 and 24 hours post-compound injection. After the initial blood sample was withdrawn glucose (1 g/kg) was injected iv and flushed in with 500 μl heparinized saline (10U/mL). Thereafter, 500 μl blood samples were withdrawn at 2.5, 5, 10 and 20 minutes post-glucose injection. Each of these was immediately followed by an iv injection of 500 μl heparinized saline (10U/mL) through the cannula. The blood samples were centrifuged, plasma was collected from each sample and the samples were stored at −20° C. until they were assayed for insulin content. The amount of insulin in each sample was determined using a rat insulin enzyme-linked immunosorbant assay (ELISA) kit (American Laboratory Products Co., Windham, N.H.).
[0144] Results:
[0145] A sustained insulin-enhancing activity was observed that was inducible by glucose injection over the full 24 hours of the experiment.
[0000] H. In Vivo Assays
[0146] There are a number of in vivo assays known in the art which enable the skilled artisan to determine a composition's ability to promote extended release of active compound in vivo.
[0147] H.1. By way of example, an aqueous test formulation was prepared comprising 1% (w/w) of the compound of formula (I) (acetate salt) in a buffered solution of ZnCL2 (peptide:Zn ratio=1.5:1.0).
[0148] A total of 6 male Beagle dogs, ages 42- 78 months and 14-21 kg bodyweight were maintained with free access to water and once daily food (approx. 400 g of dry standard diet (SAFE 125). The dogs were fasted 18 hours before administration of test composition.
[0149] The test composition was administered by subcutaneous route in the interscapular area by. The volume of administration (approx. 20 microliters per animal) was made by 0.3 mL Terumo syringes with 0.33-12 mm (BS=30M2913). A theoretical dose of approximately 0.2 mg peptide was thus achieved.
[0150] Blood samples were taken periodically, at approx. time=0, 8, 15, 30, 45 min, and 1, 2, 4, 8, and 12 hours, and 1, 2, 3, 4, 5, and 6 days after administration. The blood was rapidly chilled after sampling until centrifugation, and the plasma decanted and rapidly frozen pending assay. Determination of peptide plasma concentration was made after off line solid pase extraction, followed by on-line phase extraction coupled to LC-MS/MS, and the data obtained managed by Analyst v1.2 software.
[0151] Results:
[0152] The composition demonstrated an extended release of the active peptide for at least 2 days.
[0153] H.2. Similarly, a semi-solid composition was prepared comprising the compound according to formula (I) (acetate salt) (10% w/w), in a solution comprising 50% ZnCL 2 (2.28 mg/ml and 50% NaOH (1 mg/ml), resulting in a molar ratio, peptide:Zn, of approximately 4.0:1. The composition continued to release the active compound for approximately seven days.
[0154] Further assays with various permutations of the disclosed formulation have likewise been subject to in vivo assay and have confirmed that compositions of the present invention provide a useful drug delivery platform for the compound of formula (I).
[0155] The peptides used in this invention advantageously may be provided in the form of pharmaceutically acceptable salts. Examples of such salts include, but are not limited to, those formed with organic acids (e.g., acetic, lactic, maleic, citric, malic, ascorbic, succinic, benzoic, methanesulfonic, toluenesulfonic, or pamoic acid), inorganic acids (e.g., hydrochloric acid, sulfuric acid, or phosphoric acid), and polymeric acids (e.g., tannic acid, carboxymethyl cellulose, polylactic, polyglycolic, or copolymers of polylactic-glycolic acids). A typical method of making a salt of a peptide of the present invention is well known in the art and can be accomplished by standard methods of salt exchange. Accordingly, the TFA salt of a peptide of the present invention (the TFA salt results from the purification of the peptide by using preparative HPLC, eluting with TFA containing buffer solutions) can be converted into another salt, such as an acetate salt by dissolving the peptide in a small amount of 0.25 N acetic acid aqueous solution. The resulting solution is applied to a semi-prep HPLC column (Zorbax, 300 SB, C-8). The column is eluted with (1) 0.1N ammonium acetate aqueous solution for 0.5 hrs., (2) 0.25N acetic acid aqueous solution for 0.5 hrs. and (3) a linear gradient (20% to 100% of solution B over 30 min.) at a flow rate of 4 ml/min (solution A is 0.25N acetic acid aqueous solution; solution B is 0.25N acetic acid in acetonitrile/water, 80:20). The fractions containing the peptide are collected and lyophilized to dryness.
[0156] As is well known to those skilled in the art, the known and potential uses of GLP-1 are varied and multitudinous (See, Todd, J. F., et al., Clinical Science, 1998, 95, pp. 325-329; and Todd, J. F. et al., European Journal of Clinical Investigation, 1997, 27, pp. 533-536). Thus, the administration of the compounds of this invention for purposes of eliciting an agonist effect can have the same effects and uses as GLP-1 itself. These varied uses of GLP-1 may be summarized as follows, treatment of: Type I diabetes, Type II diabetes, obesity, glucagonomas, secretory disorders of the airway, metabolic disorder, arthritis, osteoporosis, central nervous system diseases, restenosis, neurodegenerative diseases, renal failure, congestive heart failure, nephrotic syndrome, cirrhosis, pulmonary edema, hypertension, disorders wherein the reduction of food intake is desired, as well as the various other conditions and disorders discussed herein. Accordingly, the present invention includes within its scope pharmaceutical compositions as defined herein comprising, as an active ingredient, a compound of formula (I).
[0157] The dosage of active ingredient in the formulations of this invention may be varied; however, it is necessary that the amount of the active ingredient be such that a suitable dosage is obtained. The selected dosage depends upon the desired therapeutic effect, on the route of administration, and on the duration of the treatment, and normally will be determined by the attending physician. In general, an effective dosage for the activities of this invention is in the range of 1×10 −7 to 200 mg/kg/day, preferably 1×10 −4 to 100 mg/kg/day, which can be administered as a single dose or divided into multiple doses.
[0158] The formulations of this invention are preferably administered parenterally, e.g., intramuscularly, intraperitoneally, intravenously, subcutaneously, and the like.
[0159] Preparations according to this invention for parenteral administration include sterile aqueous or non-aqueous solutions, suspensions, gels, or emulsions, provided that the desired in vivo release profile is achieved. Examples of non-aqueous solvents or vehicles are propylene glycol, polyethylene glycol, vegetable oils, such as olive oil and corn oil, gelatin, and injectable organic esters such as ethyl oleate. Such dosage forms may also contain adjuvants such as preserving, wetting, emulsifying, and dispersing agents. They may be sterilized by, for example, filtration through a bacteria-retaining filter, by incorporating sterilizing agents into the compositions, by irradiating the compositions, or by heating the compositions. They can also be manufactured in the form of sterile solid compositions which can be dissolved in sterile water, or some other sterile injectable medium immediately before use.
[0160] Unless defined otherwise, 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. Also, all publications, patent applications, patents and other references mentioned herein are incorporated by reference.
|
The present invention is directed to peptide analogues of glucagon-like peptide-1, the pharmaceutically-acceptable salts thereof, to methods of using such analogues to treat mammals and to pharmaceutical compositions useful therefor comprising said analogues.
| 0
|
This application is a continuation of application Ser. No. 08/028,400, filed Mar. 9, 1992, and now abandoned, which is a continuation in part of application Ser. No. 07/818,851, filed Jan. 10, 1992, now U.S. Pat. No. 5,240,614.
FIELD OF THE INVENTION
This invention relates to fluid filtration devices, such as blood dialysis devices and bioreactors and membranes for such devices. More specifically, the invention relates to an improved dialysis device having rectifying filtration properties, dual-skinned membranes for performance of such dialysis and other filtration procedures.
BACKGROUND OF THE INVENTION
Dialysis membranes and devices perform important life sustaining functions when used in artificial kidneys and other types of filtration devices. A well recognized problem of high flux dialyzers is the back filtration from dialysate to the blood of undesirable molecules. Due to the high cost of using sterile, pyrogen-free dialysates, it would be highly desirable to have available a dialysis membrane which could remove relatively large solutes such as β-2microglobulin while preventing passage of similarly sized molecules from dialysate to blood. Membranes, however, which offer a high rate of diffusion of solutes from the blood to dialysate also suffer from high rates of back diffusion of solutes from dialysate back to the blood. Similarly, existing membranes which offer a high rate of convection also suffer from high rates of back filtration. A need has therefore existed for dialysis membranes which provide for adequate removal of uremic toxins from the blood while preventing back transport of undesirable substances to the blood. Similarly, other fluid filtration processes benefit from the availability of membranes having such rectifying properties.
A need has also existed for devices such as bioreactors in which rectifying membranes provide a means for simultaneously supplying nutrients to and carrying products and waste byproducts from live cells that are used to make products which cannot be economically produced by traditional synthetic chemistry techniques.
SUMMARY OF THE INVENTION
An important object of the invention is to provide new and improved membranes for filtration devices such as dialysis devices. A further aspect of the invention is to provide improved filtration devices containing membranes with rectifying properties, i.e., have a greater sieving coefficient in one direction than the other, and improved filtration methods using such devices.
A further important aspect of the present invention involves providing dual-skinned membranes such as hollow fibers in which the pore size and structure, and the resulting sieving coefficient, differs between the two opposed surfaces of the membrane. In the preferred embodiment, the membranes are in the shape of hollow fibers in which the sieving coefficient, or permeability to molecules of a particular size, of the inner wall or skin of the fiber is greater than that of the outer wall. Such fibers can be assembled into dialysis devices in accordance with known procedures to provide such dialysis devices in which large solutes can be removed from a fluid, such as blood, flowing within the interior of the fibers to a filtrate or dialysate liquid which surrounds the fibers. Since a tighter or less permeable skin is provided on the outside of the fibers, it has been found that back transport from the outside of the fibers to the inside is substantially reduced.
Another important object of the invention is to provide dual-skinned membranes useful in dialysis as one way or rectifying membranes which reduce back filtration. The preferred membranes are dual-skinned polymeric materials preferably in the form of hollow fibers. The membranes have skins of polymer on their opposite sides with differing solute permeability or sieving coefficient characteristics. Such membranes can be formed by extruding a polymer dissolved in a solvent while contacting at least one surface with a non-solvent for the polymer that is miscible with the solvent. The other surface is also contacted with a non-solvent, but one which is either different from the first non-solvent or which contains a soluble additive that changes the pore size and structure of the skin formed on the dissolved extruded polymer.
In another aspect of the invention improved dialysis devices having rectifying properties are formed by using the membranes provided by the invention. The preferred dialysis devices of the invention are formed from hollow polymeric fiber membranes having a microporous structure within the walls thereof, with the microporous structure having a skin of polymer containing invisible pores formed integrally with the interior and exterior surfaces thereof. The exterior skin has a sieving coefficient different from that of the internal skin. The rectifying dialysis devices of the invention provide a means for removing unwanted material from bodily fluids such as blood in which a high rate of filtration of solutes from blood to dialysate is offered, while a substantially lower rate of back filtration of undesired solutes from dialysate to blood is maintained.
DRAWINGS
The invention will be further explained in the following detailed description and with reference to the accompanying drawings, wherein:
FIG. 1 is a diagrammatic view illustrating the process for forming membranes of the invention in hollow fiber form;
FIG. 2 is a cross-sectional view of an annular extrusion die used in the practice of the invention;
FIG. 3 is a side elevational view with portions in cross-section of a filtration device of the present invention;
FIG. 4 is a sketch in greatly enlarged scale illustrating, hypothetically, the mechanism of filtration that occurs in use of the filtration devices of the invention;
FIGS. 5 and 6 are cross-sectional views of a hollow fiber membrane of the invention of different magnifications taken with an electron microscope; and,
FIG. 7 is a side elevational view of a bioreactor device in accordance with the invention.
FIGS. 8-14 are graphical representations of the results obtained from testing of specific examples described herein.
DETAILED DESCRIPTION
Referring more specifically to the drawings, FIG. 1 diagrammatically illustrates a hollow fiber spinning system 60. A solution 62 of a polymer in an organic solvent is contained in vessel 64 from where it is pumped to an annular extrusion die 68 by means of a metering pump 66. Similarly, a coagulant solution 72 which is a non-solvent for the polymer is contained in a second vessel 70 and is transferred to die 68 by means of another pump 74.
The interaction of non-solvent 72 and the polymer solution 62 at the interface 63 formed as the solutions exit the die in contact with each other determined the ultimate structure and properties of the inner membrane.
The formed extrudate then falls through an air gap 76 and enters a bath 78 containing a second non-solvent coagulant solution 80. The interaction of the extrudate with the second solution 80 determines the structure and properties of the outer membrane. The fiber is pulled through bath 78 by means of driver roller 82 and through one or more additional baths 84, as required, to completely extract the solvent from hollow fibers. The extracted fiber is finally taken up onto a multi-segment winder 86 and allowed to dry. Dried fibers 88 are cut to length and placed in a housing 90. The fibers 88 are sealed in the housing by means of a thermosetting resin 92. The assembly is fitted with end caps 94 and 96. An inlet 97 and outlet 98 for filtrate liquid are also provided on the housing.
FIGS. 5 and 6 illustrate in magnified cross-section a typical fiber 88 of the invention showing internal microporous structure 83, an inner skin 85 and an outer skin 87 having different porosity than inner skin 85. Membranes of this invention preferably have an inner diameter of about 200 microns and generally range in inner diameter from about 100 to 1000 microns.
The overall sieving coefficient is the fraction of the incoming solute that passes through the membrane along with the fluid that is being filtered. It is calculated by dividing the concentration of solute on the downstream side of the membrane by its concentration on the upstream side of the membrane.
For a single-skinned membrane, the overall sieving coefficient is equal to the sieving coefficient of the skin, which is the fraction of solute that passes through that skin. The sieving coefficient of the skin itself depends only on the relative sizes of the pore and the solute molecule. The tighter the skin (i.e. smaller the pores), the smaller the fraction of a given molecule which will pass through it.
However, for a dual-skinned membrane, the concentration of solute which reaches the second skin depends on the characteristics of the first skin as well as the flow conditions, so the overall sieving coefficient is a property of both flow and membrane properties. The key to the rectifying membrane, in which the sieving coefficient in one direction is different from the sieving coefficient in the other direction, is that flow in one direction results in buildup of solute within the two skins of the membrane.
FIG. 4 is a schematic of a dual-skinned rectifying membrane 88 in which the outer skin 12 is tighter than the inside skin 14 and fluid is passing from the inside to the outside as a result of an imposed pressure gradient. In this case, some of the molecules which enter the central area 16 of membrane 88 become trapped when they reach the tighter outer skin 12. The concentration inside the membrane goes up until it reaches a steady state value, and the resulting concentration in the fluid 20 outside the fiber goes up along with it. The concentration in the fiber lumen 18 has not changed, so the overall sieving coefficient increases with time until it reaches a steady-state value that is higher than would be obtained with the tight skin 12 alone.
If that same membrane is exposed to a pressure gradient from the opposite direction, with flow from the outside to the inside, the solute has a hard time getting into the membrane at all, so there is no buildup in the membrane. In this case both the concentration within the membrane and the concentration on the downstream side of the membrane are low, and the overall sieving coefficient is smaller than that which was obtained in the other direction.
Various polymers can be employed in the process of the invention to form hollow fibers. The polymers must be soluble in at least one organic solvent and insoluble in another liquid that is miscible with the solvent. Examples of suitable polymers are polysulfone, polyetherimide, polyacrylonitrile, polyamide, polyvinylidene diflouride, polypropylene, and polyethersulfone. Illustrative examples of solvents for such polymers include N-methyl-2-pyrrolidone, N,N'-dimethylformamide, N,N'-dimethylacetamide and γbutyrolactone. The preferred non-solvent which can be used as a coagulation or gelation agent for formation of the skins is water. Other suitable liquids include methanol, ethanol-water mixtures such as 95 or 99.5 vol % ethanol in water, or isopropyl alcohol. Various materials can be added to the non-solvents to form skins of differing porosities. Examples include polyvinyl alcohol, Tetra-ethylene-glycol, poly-ethylene-glycol, perchlorate salts, and polyvinyl pyrrolidone.
An important advantage of the present invention is the ability to provide fibers having different sieving coefficients depending on the direction of filtrate flow, for molecules to be filtered out of a liquid. A further advantage is the ability to provide fibers having different sieving coefficients for filtration out of a liquid of molecules having narrowly defined molecular weight ranges. For example, fibers can be provided that have the ability to filter molecules in the range of 5000 to 10,000 differently from one side of the membrane than the other. By appropriate modification of the porosity, the sieving coefficient differential can also be optimized for molecules having a molecular weight range of 10,000 to 100,000 or even 200,000. Optimization is achieved by adjusting the composition of the coagulant solution and the amount and type of dopants added, as well as by varying the spinning conditions such as flow rate, line speed and gap distance.
EXAMPLES
The following examples illustrate preferred processes for producing and using membranes in accordance with the invention. All parts are given by weight unless otherwise indicated.
EXAMPLE 1
Hollow fibers were prepared using the spinning system and processes described in FIGS. 1 and 2 under the formulation and process conditions shown in Table I.
Test Procedure
Test modules were assembled by potting 100 fibers in mini-dialyzer cases with a length of about 22 cm and an internal diameter of about 0.6 cm. Polyurethane potting extended approximately 1 cm from each header, leaving an active length of about 20 cm. Dialysate ports were located approximately 1 cm from the potting material at each end.
Standard dialysate of the following composition was prepared from concentrate using a hemodialysis machine proportioning system:
sodium 134 mEq/l
potassium 2.6 mEq/l
calcium 2.5 mEq/l
magnesium 1.5 mEq/l
chloride 104 mEq/l
acetate 36.6 mEq/l
dextrose 2500 mEq/l
Myoglobin solution was prepared by adding the 330 mg of myoglobin per liter of dialysate. Myoglobin (molecular weight=17,000) is used as a marker for middle molecules such as B-2 microglobulin (molecular weight=12,000) because it can be measured spectrophotometrically.
The lumen and filtrate compartments were primed with alcohol (isopropanol or ethanol) using a syringe. The test module was then rinsed with excess dialysate, pumping 250 ml through lumen with filtrate port closed and then 200 ml more with one filtrate port open. To measure inlet flow rate, the dialysate ports were closed, the infusion pump was set to the desired speed (10.5 ml/min), outflow was determined by timed collection.
For the sieving coefficient measurement, the test module was clamped in a vertical position, with fibers perpendicular to the table top. An infusion pump was connected to an inlet reservoir, and tubing from the infusion pump was connected to the bottom header. Tubing to waste was connected to the top header. The dialysate ports were closed, the pump was started, and the time at which the test solution reached the device was denoted as time zero.
At time zero, the dialysate side was drained of priming solution by opening both dialysate stopcocks. The lower dialysate port was then closed, and the time zero filtrate sample was taken from the upper port as soon as the filtrate compartment was filled. At the same time, the outlet lumen sample was collected into another beaker. Inlet lumen samples were taken directly from the inlet reservoir. Subsequent filtrate samples were collected at 3 minute intervals, with no loss of filtrate between samples. All samples were measured for myoglobin content using a Gilford spectrophotometer. The sieving coefficient, S, was calculated using the following equation: ##EQU1## Sampling was continued until the calculated sieving coefficient was constant for 3 consecutive samples.
The fibers were assembled into test modules and the sieving coefficients determined in accordance with the foregoing procedure. The sieving coefficients of the fibers of this example for myoglobin were found to be 0.35 when filtrate flow was directed radially outwardly and 0.80 when filtrate flow was inward.
TABLE I______________________________________Polymer PolysulfoneSolvent N-methylpyrrolidoneSpinning Solution Concentration 15 g/100 gCore Fluid Composition 15/85 2-propanol/waterPrecipitation Bath Composition 2/98 2-propanol/waterWash Baths Composition WaterGap Distance 1 cmLine Speed 18 meters/minSpinning Solution Flow Rate 1.8 cc/minCore Fluid Pin Diameter 0.009 inchesDie Annular Gap 0.0035 inches______________________________________
EXAMPLE 2
Hollow fibers were prepared as in Example 1 except that the core fluid composition was 10/90 2-propanol/water and that of the precipitation bath was 5/95 2-propanol/water. FIGS. 5 and 6 are scanning electron micrographs of the resulting fiber in cross- section taken at 2000 times magnification and 400 times magnification, respectively, showing the finger-like structures extending from each boundary and meeting in the middle wall. Sieving coefficients for myoglobin were found to be 0.45 for outward filtrate and 0.90 for inward flow.
EXAMPLE 3
Hollow fibers were prepared as in Example 1 except that the core fluid composition was 70% isopropyl alcohol and 30% water. The spinning solution concentration was 20 weight percent of polysulfone in N-methylpyrrolidone with 10% acetone. The precipitation bath was water. Sieving coefficients were determined for dextran using the following procedure:
1) Dextran Sieving Coefficient. A dextran solution of the following composition was prepared in phosphate buffered saline (0.9%):
Dextran FP1 (Serva) 0.2 g/l
Dextran 4 (Serva) 1.0 g/l
Dextran T40 (Pharmacia) 1.0 g/l
Dextran T10 (Pharmacia) 0.3 g/l
Dextran solution was perfused through the lumen, with filtrate collected from the shell side. Dextran solution was also perfused through the shell side, with filtrate collected from the lumen. The order of the tests varied. Solution flow rate was 5 ml/min, and the transmembrane pressure was between 150 and 200 mm Hg. Inlet samples were taken directly from the dextran solution reservoir. Filtrate samples were taken at 5 minutes intervals. The filtrate concentration values stabilized after 15 minutes. The filtrate concentration value at 40 or 60 minutes were used to calculate sieving coefficient. The bulk solution concentration was assumed to be equal to its inlet value and constant throughout the length of the dialyzer. Samples were analyzed by high performance liquid chromatography (HPLC) using a refractive index detector. ##EQU2## Results are shown in FIG. 8.
Sieving coefficients for alcohol dehydrogenase (MW approximately 150,000) and β-amylase (MW approximately 200,000) were determined by the procedure outlined above, by with the samples analyzed by a commercially available assay kit (Sigma Chemical Co.). The sieving coefficients for alcohol dehydrogenase were 0.05 for outward flow and 0.76 for inward flow. The sieving coefficients for β-amylase were 0.01 for outward flow and 0.17 for inward flow.
EXAMPLE 4
Hollow fibers were prepared as in Example 1 except that the core fluid composition was 50% isopropyl alcohol and 50% water. The spinning solution contained 20% by weight of polysulfone and N-methylpyrrolidone with 10% acetone. The precipitation bath was water. The sieving coefficient for dextran was determined for lumen to shell and shell to lumen. The results are shown in FIG. 9.
EXAMPLE 5
Hollow fibers were prepared as in Example 1 except that the core fluid composition was isopropyl alcohol. The spinning solution was polysulfone in a concentration of 15% by weight and in addition 15% by weight of polyvinylpyrrolidone in N-methylpyrrolidone. The core fluid composition was isopropyl alcohol and the precipitation bath was water. The sieving coefficient for dextran was determined as in Example 3 with the results being shown in FIG. 10.
EXAMPLE 6
Polysulfone hollow fiber membranes were prepared with an outer skin having a 5,000 kilodalton (kD) nominal molecular weight (MW) cutoff and a skin with a larger, but unknown MW cutoff on the inner fiber surface. For these fibers, the sieving coefficients of dextrans of various molecular weight were found to be greater when filtrate flow was directed radially inward than when filtrate flow was directed outward.
Protein Sieving Coefficient. The following proteins were dissolved in phosphate buffered saline (0.9%):
______________________________________Solution 1 2.0 g/lBovine serum albuminSolution 2 1.0 g/lOvalbumin (chicken egg albumin)Solution 3 0.08 g/lMyoglobinSolution 4 0.12 g/lCytochrome c______________________________________
Protein solution was perfused through the lumen, with filtrate collected from the shell side. Protein solution was also perfused through the shell side, with filtrate collected from the lumen. The order of the tests varied. Inlet samples were taken directly from the protein solution reservoir. Filtrate samples were taken at 5 minutes intervals. The filtrate concentration values stabilized after 15 minutes. The filtrate concentration value at 40 or 60 minutes were used to calculate sieving coefficient. The bulk solution concentration was assumed to be equal to its inlet value and constant throughout the length of the dialyzer. Samples were analyzed for absorbance at a characteristic wavelength using a spectrophotometer. Bovine serum albumin and ovalbumin were analyzed at 280 nm. Myoglobin and cytochrome c were analyzed at 410 nm. The results for sieving coefficients of both dextran and proteins tested according to the foregoing procedure are shown in FIG. 11.
EXAMPLE 7
Hollow fibers were prepared according to the procedure of Example 1 using the following materials:
Polymer: Polyetherimide
Solvent: N-methylpyrrolidone
Spinning solution concentration: 20 wt %
Core fluid composition: Water
Precipitation bath: Water
The sieving coefficient data for dextran when tested as shown in FIG. 12.
EXAMPLE 8
Hollow fibers were prepared according to the procedure of Example 1 using the following materials:
Polymer: Polyetherimide
Solvent: N-methylpyrrolidone
Spinning solution concentration: 25 wt %
Core fluid composition: 50/50 Water/N-methylpyrrolidone
Precipitation bath: Water
The sieving coefficient data for dextran is shown in the following FIG. 13.
EXAMPLE 9
According to current theory on the behavior of rectifying membranes, internal concentration polarization of solute is responsible for the asymmetric sieving characteristics of the above examples. The accumulation of solute between the two skins of the membrane should require a finite amount of time to occur. Consequently, the sieving coefficient in one direction should increase with time until equilibrium is reached. For most common membranes, the sieving coefficient is generally greatest in early time measurements and may decrease with time as pores clog with retained solute.
In FIG. 14, the sieving coefficient in the shell to lumen direction is shown as a function of time for the membrane of Example 3. For this experiment, filtrate was collected at one minute intervals for the first ten minutes of filtration. The sieving coefficient, particularly in the 50,000 to 100,000 range, did increase significantly with time.
A bioreactor is shown in FIG. 7 and consists of a device somewhat similar to the dialysis device shown in FIG. 3. In this case, however, the space 89 surrounding the fibers and enclosed by the interior of housing 90 and thermosetting resin 92 forms a reaction vessel for growth of living cells. Ports 97 and 98 are either omitted or can be closed by means of valves 99 and 100 as indicated. Depending on its size, the product may pass back through the membranes 88 and be purified from the waste stream or it may collect in the shell space which constitutes the reaction vessel from which it may be removed on either a semi-continuous or batch basis.
Transport of nutrients, waste products and desired biological products across the membrane may be by diffusion and/or convection. The axial pressure drop which occurs within the hollow fibers leads to Starling's flow, with convection from the tube side to the shell side at the device inlet and convection from the shell side to the tube side at the device outlet.
Some types of cells require expensive growth media which may contain 10% bovine fetal calf serum. Use of a rectifying membrane allows serum components to pass through the membranes to the cells and then be concentrated in the shell space, thereby reducing the volume of media required. This also reduces the cost of purifying products which pass through the membrane because the volume of the purification stream is smaller.
Rectifying membranes can also be used to concentrate products directly. If the desired product is formed of molecules that are larger than the metabolic waste products as well as the nutrients, the rectifying membrane device can be used to concentrate the products in the shell space while allowing nutrients to reach the cells and waste products to be washed away by the fluid stream passing through the interiors of the hollow fiber membranes.
Membranes in accordance with the present invention can thus be formed with the tighter skin either on the interior or exterior of a hollow membrane. In either event it is important that the skins on each side of the membrane contain pores that are invisible at 10,000 times magnification. This will insure the presence of sufficiently tight skins on each side of the membrane to cause a build-up of solutes in the microporous interior of the membrane between the skins. Such build-up of solutes is believed to be important to the construction of membranes in which different sieving coefficients are obtained for flow through the membrane in different directions.
|
The invention provides dual-skinned membranes useful as one way or rectifying membranes which reduce back filtration of solute molecules in dialysis and which improve nutrient supply and product recovery in membrane bioreactors. The membranes are dual-skinned polymeric materials preferably in the form of hollow fibers. The membranes have skins of polymer on the opposite sides with differing permeability to solutes and sieving coefficient characteristics. The skin on each side have pores that are invisible at 10,000 times magnification, the microporous structure between said skins contains pores capable of retaining solutes in a molecular weight range of about 5000 to 200000 in an increased concentration between the interior and the exterior skins. Improved dialysis devices are formed by using bundles of the hollow fiber membranes as a dialysis means having rectifying properties.
| 1
|
CROSS-REFERENCE TO RELATED DOCUMENTS
This disclosure is related to and incorporates by reference in its entirety, co-pending U.S. patent application Ser. No. 13/506,651 entitled “Well Pump Puller,” filed by Joseph Dennis Miller on May 7, 2012.
BACKGROUND OF THE INVENTION
Wells are constructed to access subsurface water for various purposes, such as for drinking and irrigation. Electric well pumps (“well pumps”) are utilized to pump subsurface water up to the surface. Typical well configurations include a well casing that extends from the ground surface (which include points above the ground surface) to a point below the subsurface water, with a well pump being disposed within the casing. Typical structure connected to such pumps and extending to the ground surface include a water pipe, which often includes multiple connected segments, for carrying the subsurface water, and electrical wiring for providing electrical current to such pumps.
A well pump can fail for various reasons. Therefore, well pumps can require replacement, which requires a failed well pump to be extracted from within a well.
A prior solution is provided in U.S. Pat. No. 3,741,525 by Smedley (“Smedley”), which discloses a well puller that pulls a well pump via a permanent high-tensile strength cable. As disclosed, this solution includes a well application that necessarily requires the addition of a permanent high-tensile strength lifting cable, and expressly teaches away from pulling a plastic water pipe, as “it lacks the strength to sustain the tensile forces resulting when the pump and seal are pulled from the well.” A significant drawback with the Smedley solution is that prior provisioning of such a permanent high-tensile strength lifting cable is required for this solution to be effectuated.
Another prior solution is the “Pull-a-Pump”, which is a well pump puller having motorized means that can extract a well pump by pulling a water pipe connected to a pump. Specifically, this solution includes a pair of motorized, opposing traction belts between which a well pipe is gripped and moved upwardly. As the belts move, the pipe and pump are lifted from within a well casing.
SUMMARY OF THE INVENTION
It is, therefore, an object of the present invention to provide a well pump puller.
It is another object of the present invention to provide a well pump puller that can allow a well pump to be extracted from within a well by pulling pre-existing electrical wiring connected to the pump while concurrently reducing the risk of the well pump falling into the well.
The present invention reduces this risk by reducing yank forces on the wiring and/or by providing a pipe catch adapted to catch and hold a water pipe connected to a well pump if the electrical wiring mechanically fails during an extraction of the well pump.
An exemplary environment of the present invention can include a well pump disposed within a well casing that extends from a ground surface point (which includes points just above the ground surface) to a below-ground point. Electrical wiring can have a first wiring end connected to the well pump and a second wiring end extending up to the ground surface point; and a water pipe can have a first pipe end connected to the well pump and a second pipe end extending up to the ground surface point.
In an exemplary embodiment of the present invention, a well pump puller for extracting a well pump from within a well casing can include a rigid base, a rigid support element, and an elastic element.
In an exemplary aspect, a rigid base can include an engagement element and a base extension. An engagement element can be adapted to engage the well casing and/or the ground surface. A base extension can extend upwardly from the ground surface point.
In another exemplary aspect, a rigid support element can be moveably engaged with the base extension; and can rotatably support a spindle. A spindle can have a rotation element for rotating the spindle, and can be adapted to fixably receive a second wiring end of the electrical wiring.
In a further exemplary aspect, an elastic element can be disposed between, and abut, the base and the support element during a well pump extraction.
In yet another exemplary aspect, when the second wiring end is fixably received by the spindle and the rotation element is rotated, the electrical wiring can be wound around the spindle resulting in a pulling force applied to the electrical wiring, which pulls the well pump and the water pipe from within the well casing towards the ground surface. During such an extraction, the elastic element can deform to absorb at least a portion of any yank forces arising at least in part from the pulling force.
The following are optional exemplary aspects, of which one or more can be combined with the basic invention as embodied above:
the spindle can include a spindle lock and a safety latch to prevent the spindle from rotating in one of a clockwise direction and a counter-clockwise direction, and to allow the spindle to rotate in the other of the clockwise direction and the counter-clockwise direction; the base or the support element can include a wire guide disposed between the spindle and the well casing, where the wire guide includes a rounded edge against which the electrical wiring slides before the electrical wiring is wound around the spindle; the base or the support element can include a rigid pipe guide having at least one frame element that defines an opening, disposed over the well casing, and having a size greater than the water pipe, and as the well pump and water pipe are pulled out from within the well casing, the water pipe travels through the opening; in addition to a pipe guide, the base or support element can include a pipe catch having at least one rigid flap, adjacent to the opening, and having a first flap end hingedly connected to the pipe guide and a second flap end having a concave shape, the at least one flap being, biased in a locking position, and moveable between an unlocking position, in which the second flap end is angled upwardly, and the locking position, in which the at least one flap covers a portion of the opening; the base or support element can include a drill abutment adapted to abut at least one of the right and left side of a drill; and the drill abutment can be rotatably moveable between a stored position and an active position.
In another exemplary embodiment of the present invention, a well pump puller for extracting a well pump from within a well casing can include a rigid base, a rigid pipe guide, and a pipe catch.
The following are exemplary aspects of this embodiment: a rigid base can include an engagement element and a base extension; an engagement element can be adapted to engage the well casing and/or the ground surface; a base extension can extend upwardly from the ground surface point and can rotatably support a spindle; and a spindle can have a rotation element for rotating the spindle, and can be adapted to fixably receive a second wiring end of the electrical wiring.
Further exemplary aspects of the embodiment are as follows: a rigid pipe guide can be connected to the base and can have at least one frame element that defines an opening, disposed above the well casing, and having a size greater than the water pipe; a pipe catch can include at least one rigid flap, adjacent to the opening, and having a first flap end hingedly connected to the pipe guide and a second flap end having a concave shape; and the at least one flap can be, biased in a locking position, and moveable between an unlocking position, in which a respective second flap end is angled upwardly, and the locking position, in which the at least one flap covers a portion of the opening.
Additional exemplary aspects of this embodiment are as follows: when the second wiring end is fixably received by the spindle and the rotation element is rotated, the electrical wiring can be wound around the spindle resulting in a pulling force applied to the electrical wiring, which pulls the well pump and the water pipe from within the well casing towards the spindle, with the water pipe being guided through the opening with the at least one flap being in the unlocked position; and if the water pipe is subsequently moved downwardly after being guided upwardly through the opening, the second flap end locks the water pipe in a static position by abutting the water pipe and creating static friction in conjunction with at least one of the at least one frame element and a second rigid flap.
Further, this exemplary embodiment can include any one or more of the basic and optional exemplary aspects described above and/or herein.
These and other exemplary aspects of the present invention are described herein.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is illustrated by way of example, and not in limitation, in the figures of the accompanying drawings, in which:
FIG. 1 illustrates an exemplary embodiment of the present invention having a base, a support element rotatably supporting a spindle, and an elastic element.
FIG. 2 illustrates a detailed view of an exemplary engagement element that can engage a ground surface and/or a well casing.
FIG. 3 illustrates an exemplary embodiment of the present invention additionally having optional components of a pipe guide, a pipe catch, a wire guide, a spindle lock, and a safety latch.
FIG. 4 illustrates an exemplary embodiment of the present invention additionally having optional components of a spindle lock, safety latch, and a pipe abutment.
FIG. 5 illustrates another exemplary embodiment of the present invention having a base, a base extension rotatable supporting a spindle, a pipe guide, and a pipe catch.
DETAILED DESCRIPTION OF THE INVENTION
The invention will now be described in more detail by way of example with reference to the embodiments shown in the accompanying figures. It should be kept in mind that the following described embodiments are only presented by way of example and should not be construed as limiting the inventive concept to any particular physical configuration, material, or order.
As noted above, installed well pumps can require replacement due to their failure, and accordingly, can require extraction from within wells. When extracting a well pump from within a well, there is a risk that the well pump can fall to the bottom of the well due to human or mechanical error. Manually extracting a well pump can be exceedingly tedious, especially when well depths are great, as such extracting can involve pulling the water pipe up by hand or motor until the well pump reaches the surface. While some wells may only require depths of 50 feet or less, some can require depths exceeding 450 feet to reach subsurface water (e.g., an aquifer). However, extracting a well pump that has fallen to the bottom of a well due to a failed extraction can be significantly more tedious, expensive, and time-consuming. Thus, recovering a fallen well pump can be extremely difficult and costly.
The pulling force required to pull a well pump from within a well to the ground surface must be sufficient to overcome weight considerations and resistive forces arising during an extraction of the well pump.
Exemplary weight considerations can include the following: a typical residential well pump can weigh about 30 pounds; water pipe (typically, 1.25″ PVC Schedule 40) can weigh about 0.43 pounds/foot; water within a water pipe weighs 8 pounds/gallon; and electrical wiring can weigh about 0.075 pounds/foot. Given these weight considerations, it is feasible for the total weight of such combinations to exceed 230 pounds for a 200 foot well and 430 pounds for a 400 foot well.
Exemplary physical forces existing during an extraction of a well pump can arise due to the following: drag forces that can arise from moving the water pump through subsurface water existing within the well casing above the well pump; and kinetic friction that can arise from mineral build-up on the well pump and/or inner walls of a well casing sliding against each other or against the well pump and/or inner walls.
When extracting a well pump by pulling it via electrical wiring connected thereto, there exists a risk that well pump can fall into the well due to the electrical wiring mechanically failing (or breaking). Such mechanical failure can arise if the pulling force, by itself or in combination with other conditions, creates an amount of strain on the electrical wiring that exceeds the effective tensile strength of the electrical wiring:
Mechanical Failure= Fp>TSe,
where F p is the pulling force, and TS e is the effective tensile strength of the wiring.
Two significant problems exacerbate this risk: yank forces, and mechanical defects of the electrical wiring.
Yank forces can arise, for example, from variability of the pulling force and/or variability of resistive forces. A yank force can be expressed as the derivative of force with respect to time, and can be represented as follows:
Y=dF/dT , where
Y is the yank force, F is the pulling force on the wiring, and d/dT is the derivative with respect to time t.
Notably, a drag force can be expressed as follows:
F D =½ρν 2 C D A, where
F p is the drag force, which is by definition the force component in the direction of the flow velocity, ρ is the mass density of the subsurface water, ν is the velocity of the object relative to the subsurface water, A is the reference area, and C D is the drag coefficient.
Motorized and manual generation of a pulling force can provide a variable pulling force that may exceed the tensile strength of the wiring. For example, the generated pulling force applied to the electrical wiring to move the well pump from a static position can exceed the tensile strength of the electrical wiring, especially when the pulling force is increased or applied too quickly. Moreover, variability in the generation of the pulling force can arise due to human interaction or error, such as, for example and not in limitation, manual generation of the pulling force, manual operation of a motor (e.g., the triggering a variable speed drill), or between manual “pulls” generated by hand. Notably, a pulling force, by itself or in combination with drag forces and/or friction, applied too quickly can generate a problematic yank force.
Further, variability of resistive forces can arise as a pulling force is applied to electrical wiring. For example, where mineral build-up on the well pump housing and/or inner walls of the well casing exist, the sudden generation of static, even if temporary, resistive forces, while a pulling force is being applied, can arise, which can significantly increase the strain on the electrical wiring due to the addition of a yank force. Moreover, drag forces can increase relative to the speed at which the well pump is pulled.
Mechanical defects of the electrical wiring can significantly reduce the effective tensile strength of the wiring. Typical electrical wiring utilized in subsurface well pump applications can include various gauges, such as, for example and not in limitation, 14 American Wire Gauge (AWG) Stranded Wiring. For example, a 14 AWG Stranded Wiring can have a production-defined breaking strength between 128 lbs and 349 lbs. However, in practice, the effective breaking strength of electrical wiring can be less than production-defined strengths due to production defects, in-field wiring damage, and/or environmental conditions, such as wiring deterioration, environmental temperature, sulfur exposure, and long-term temperature fluctuations, for example and not in limitation, all of which may not be readily apparent when a well pump is initially installed, or when a well pump is subsequently extracted. Where the effective breaking strength of electrical wiring is significantly reduced, the risk of electrical wiring failing mechanically during the extraction of a well pump can be undesirably high.
Therefore, the present invention can be embodied in a well pump puller that can reduce the risk of a well pump falling into a well when extracting the well pump via its electrical wiring by reducing the mechanical strain on the electrical wiring from yank forces and/or by securably fixing the pipe in a static position if the electrical wiring fails during such an extraction.
Initially, it should be noted the present invention can be designed or otherwise built from any one or more materials, including but not limited to any type of metal, plastic, ceramic, naturally occurring, synthetic, or man-made material or materials, as long as the final product can functionally operate as described. Thus, use of the word “rigid” is intended to mean overall rigidness, such that effective functionality as described and claimed is achieved.
FIG. 1 illustrates a basic exemplary embodiment of the present invention, in which a well pump puller can include a base 110 ; a support element 120 rotatably supporting a spindle 130 ; and an elastic element 140 disposed between the base and the support element. As further illustrated in FIG. 1 , base 110 can include an engagement element 111 , and a base extension 112 that extends upwardly.
Referring now to FIG. 2 , an engagement element can include a ground engager 212 and/or a casing engager (see infra) A ground engager 212 can be provided with a flat shape for abutment with the ground 160 and to support base 210 . As further illustrated in FIG. 2 , casing engager can include a vertically-oriented channel 214 , a pair of bolt sleeves 215 , and a u-bolt 216 having a pair of wing nuts 217 . As illustrated, channel 214 can be disposed against a well casing 150 , with u-bolt 216 being disposed around the casing and through bolt sleeves 215 . Wing nuts 217 can then be engaged with u-bolt 216 and tightened to engage base 110 to well casing 150 , which provides support for the base.
Notably, an engagement element according to the present invention is not necessarily limited to the specific exemplary aspects and structures illustrated above. For example and not in limitation, engagement element can include any compatible structure to engage well casing 150 and/or the ground 160 adjacent thereto, such as one or more clamps, hose clamps, ratchet clamps, straps, cables, brackets, bolts, nuts, feet, bases, or any other known or apparent structure(s) able to engage well casing 150 . Further, an engagement element can be provided as a hollowed cylindrical flange having an outside diameter less than an inner diameter of well casing 150 , such that the flange can fit within the well casing with base 110 abutting the top of the casing. Such configuration can provide both vertical and horizontal support for base 110 .
FIG. 1 also illustrates an exemplary well pump puller during an exemplary extraction of a well pump (not shown). Initially, an exemplary well pump puller can be positioned adjacent to an exemplary well casing 150 . When an exemplary puller is so positioned, and engagement element can be engaged with the ground surface 160 and/or well casing 150 ; a first end of pre-existing electrical wiring 170 can be connected to a well pump (not shown) disposed within the well casing; and a second end of wiring 170 can be fixably received by spindle 130 . As illustrated, in one exemplary manner, a second end can be fixed to spindle 130 via optional notch 132 in which the second end can be fixably wedged. Notably, however, fixation can alternatively or conjunctively be effectuated in any other desired manner, such as wrapping wiring 170 around spindle 130 and over itself to create static friction; tying wiring 170 around spindle 130 in a knot or friction-conducive configuration; or wrapping and/or tying wiring 170 around a pin or other protrusion or depression (not shown) provided with spindle 130 .
After wiring 170 is fixably received by spindle 130 , rotation element 134 can be rotated, which rotates spindle 130 . In an exemplary aspect, rotation element 134 can be rotated by hand or motor, and illustratively, can be provided as one or more of a crank, a crank handle, a gear, a sprocket, a shank, or any other structural element that allows direct or indirect application of a rotational force to rotation element 134 , which transfers such force to spindle 130 . As illustrated in FIG. 1 , rotation element can be provided as a shank 134 for connection to a chuck 135 of an electric drill 136 , for example and not in limitation. In this example, rotation of rotation element 134 can be effectuated by activating drill 136 , which rotates spindle 130 .
As electrical wiring 170 is wound around spindle 130 due to its rotation, a pulling force is generated on the wiring, which pulls the wiring up from within the well casing 150 and towards spindle 130 . As wiring 170 is pulled up, a target well pump, as well as a water pipe 180 connected to the pump, can also be pulled upwardly from within well casing 150 . When the pump reaches the ground surface 160 , the well pump can then be accessed manually and subsequently discarded or repaired.
As illustrated in FIG. 1 , to reduce the force-effect of yank forces on electrical wiring 170 during extraction of a well pump, elastic element 140 can be disposed between base 110 and support element 120 . As further illustrated in FIG. 1 , base extension 112 can have a hollowed portion, and a portion of support element 120 can be adapted to slidably move therein. Accordingly, in this particular embodiment, a yank force that arises during an extraction can be at least partially transferred to a downward motion of support element 120 and then to a deformation of elastic element 140 . Thus, the risk of a yank force causing the strain on electrical wiring 170 during an extraction to exceed the breaking strength of the wiring can be reduced by transferring the yank force, at least in part, to elastic element 140 , which in this embodiment deforms via compression. It should be noted that deformation of elastic element 140 can alternatively or conjunctively be by stretching, bending, twisting, and/or any other form of deformation consistent with the present invention.
Notably, according to the present invention, base extension 112 need not have a hollowed portion, and support element 120 can include a hollowed portion, such that support element 120 can be adapted to move downwardly and around base extension 112 . Further, while the exemplary configuration of FIG. 1 illustrates base extension 112 and the engaging portion of support element 120 as being cylindrical, they need only be shaped in a manner complementary to each other, such that movable engagement between base extension 112 and support element 120 can be achieved to transfer yank forces to elastic element 140 . Further, complementary shapes need only be functionally compatible and need not be adapted such that one must necessarily fit in or around another, such as when one engages another along a side, for example and not in limitation. Further, moveable engagement can additionally include movement such as leaning, for example and not in limitation, such as where support element 120 and base extension 112 are connected to elastic element 140 , and the support element can bend towards an arising yank force, with elastic element deforming to accommodate such leaning.
Further, exemplary cross-sectional shapes of support element 120 and base extension 112 are not limited to round shapes, as illustrated in FIG. 1 , but can be oval, square, triangular, hexagonal, oblong, or any other symmetric or asymmetrical shape, including partial or whole variations thereof.
In an exemplary aspect of the present invention, elastic element 140 is illustratively shown as a spring 140 in FIG. 1 , but can be provided as any one or more elastic structures, materials, and/or systems adapted to at least partially absorb a yank force via deformation, such as compression and/or stretching, such as, for example and not in limitation, any one or more of any type of shock, strut, spring, torsion bar, or dampener.
Thus, elastic element 140 can include, in whole or in part, any one or more, and/or any known or apparent combinations and variations of, an elastic material, elastic band, elastic cord, elastic bushing, spring, torsion bar, hydraulic shock, pneumatic shock, magnetic shock, spring shock, hydropneumatic shock, tension spring, extension spring, compression spring, torsion spring, constant spring, variable spring, coil spring, flat spring, machined spring, cantilever spring, helical spring, conical spring, volute spring, hairspring, balance spring, leaf spring, v-spring, Belleville spring, constant-force spring, gas spring, ideal spring, mainspring, negator spring, progressive rate coil spring, spring washer, and/or wave spring.
Further, elastic element 140 can be shaped cylindrically, as illustratively shown in FIG. 1 , but can be provided in any other functionally compatible shape consistent with the present invention, including but not limited to, a sphere, a cube, a parallelogram, a cylinder, a pyramid, an oblong shape, a conical shape, a barrel shape, a convex shape, a concave shape, or any other symmetric and/or asymmetric shape.
FIGS. 3 and 4 illustrate exemplary optional aspects of the present invention, one or more of which can be combined with the basic invention as described above.
As illustrated in FIG. 3 , spindle 130 can optionally include a spindle lock 337 and a safety latch 338 , which can cooperatively prevent the spindle from rotating in at least one of a clockwise direction and a counter-clockwise direction. As illustrated in FIG. 4 , spindle lock 337 can include a plurality of teeth 439 a , and can be connected to spindle 130 such that the lock and spindle rotate together. As further illustrated in FIG. 4 , safety latch 338 can be pivoted to a locked position, such that it engages at least one of teeth 439 a , in which latch 338 can abut at least one of teeth 439 a , which prevents spindle lock 337 (and accordingly, spindle 130 ) from rotating in one or both directions. Further, safety latch 338 can be pivoted to an unlocked position, such that it is disengaged from teeth 439 a , which allows spindle lock 337 (and accordingly, spindle 130 ) to rotate freely.
Optionally, safety latch 338 can be spring-biased towards a locking position via spring mechanism 439 b . Additionally, teeth 439 a can optionally be angled in one of a clockwise and counterclockwise direction, such that when safety latch 338 is in a locked position, spindle lock 337 can be rotated in the other of the clockwise and counterclockwise direction, with safety latch 338 being adapted to pivot away from teeth 439 a and slide over teeth 439 a , and further being biased to reset in a locked position after the other the clockwise and counterclockwise rotation stops.
As also illustrated in FIG. 3 , support element 120 can include a wire guide 322 that can be positioned between spindle 130 and well casing 150 . Wire guide 322 can include a rounded edge 324 against which electrical wiring 170 can slide before being wound around spindle 130 , which can allow wiring 170 to self-distribute itself along spindle 130 . Notably, wire guide 322 is illustratively shown to be connected to support element 120 , but alternatively or conjunctively can be connected to base 110 .
FIG. 3 also illustratively shows an optional pipe guide 325 for guiding water pipe 180 directionally during a well pump extraction. Pipe guide 325 can have at least one frame element 326 that defines an opening 327 , which can be positioned between well casing 150 and spindle 130 , and can be sized greater than water pipe 180 . Accordingly, as electrical wiring 170 is pulled from well casing 150 towards spindle 130 , water pipe 180 can be directed through opening 327 , which guides the water pipe via frame element 326 , which provides an abutment function.
Notably, pipe guide 325 is illustratively shown to be connected to support element 120 , but alternatively or conjunctively can be connected to base 110 . Further, frame element 326 is illustrated as having a U-shape, but can be provided in alternative shapes, in whole or in part, such as a whole or partial circle, square, rectangle, oval, oblong shape, or any other symmetric or asymmetric shape that provides abutment-based guidance of water pipe 180 during a well pump extraction.
As further illustrated in FIG. 3 , support element 120 can optionally include a pipe catch 390 having at least one rigid flap 392 adjacent to opening 327 . A flap 392 can include a first flap end 393 hingedly connected to pipe guide 325 , and a second flap end 394 having a concave shape. A flap 392 can be biased, via a spring or gravity, towards a locking position, in which second end 394 of flap 392 covers at least a portion of opening 327 , such that the effective size of opening 327 is smaller than water pipe 180 . From such a position, a flap 392 can hinge upwardly towards spindle 130 , so as to be in an unlocking position, and second end 394 sufficiently exposes opening 327 such that water pipe 180 can move upwardly through the opening. Accordingly, during an extraction, water pipe 180 can be disposed within opening 327 , and a second end 394 of flap 392 can be angled upwardly (or towards spindle 130 ), such that water pipe 180 can move upwardly through the opening as electrical wiring 170 is wound around spindle 130 . In the event water pipe 180 is thereafter moved downwardly, second end 394 of flap 392 , in conjunction with pipe guide 325 and/or a second flap (not shown), can lock the water pipe in a static position by abutting the water pipe and creating static friction therewith. Thus, if electrical wiring 170 mechanically fails during an extraction, pipe catch 390 can prevent a well pump from falling by locking the water pipe 180 , which is connected to the well pump, in a static position. Notably, a second end 394 of a flap 392 can include an acute, right, or obtuse angled edge.
Referring now to FIG. 4 , as illustrated, support element 120 can optionally include a drill abutment 495 adapted to abut at least one of the right and left side of a drill (not shown). Accordingly, when a drill is utilized to rotate rotation element 134 , drill abutment 495 can abut the left or right side of the drill, which will depend on the direction in which the drill is rotating. As further illustrated, drill abutment 495 can be connected so as to swivel between an active position and a stored position. Notably, drill abutment 495 is illustratively shown to be connected to support element 120 , but alternatively can be connected to base 110 .
Reference is now made to FIG. 5 , which illustrates another embodiment of the present invention, in which a well pump puller for extracting a well pump from within a well casing can include a rigid base 110 a , a pipe guide 325 , and a pipe catch 390 . Notably, the exemplary aspects of this embodiment generally mirror those described above, except base 110 a is defined to encompass the support element, as this embodiment lacks an elastic element in its broadest form.
As illustrated, base 110 a can include an engagement element 111 adapted to engage a well casing 150 and/or the ground surface 160 , and a base extension 112 , extending upwardly, and rotatably supporting a spindle 130 having a rotation element 134 and an optional notch 132 . Notably, this exemplary embodiment can include any one or more of the basic and optional aspects herein described in connection with any other exemplary embodiment of the present invention, with the same functioning similarly or the same.
It will be apparent to one of ordinary skill in the art that the manner of making and using the claimed invention has been adequately disclosed in the above-written description of the exemplary embodiments and aspects. It should be understood, however, that the invention is not necessarily limited to the specific embodiments, aspects, arrangement, and components shown and described above, but may be susceptible to numerous variations within the scope of the invention. Moreover, particular exemplary features described herein in conjunction with specific embodiments and/or aspects of the present invention are to be construed as applicable to any embodiment described within, enabled hereby, or apparent herefrom. Thus, the specification and drawings are to be regarded in a broad, illustrative, and enabling sense, rather than a restrictive one.
Further, it will be understood that the above description of the embodiments of the present invention are susceptible to various modifications, changes, and adaptations, and the same are intended to be comprehended within the meaning and range of equivalents of the appended claims.
|
A well pump extractor, which includes a base rotably supporting a spindle, a pipe guide, and a pipe catch, extracts a well pump from within a well by winding electrical wiring attached to the pump around the spindle. During an extraction, a pipe guide guides the path of water pipe connected to a pump. If the electrical wiring fails mechanically during an extraction, the pipe catch catches the water pipe, which prevents the pump from falling to the bottom of the well.
| 4
|
FIELD OF THE INVENTION
This invention relates to toys, and more particularly, to toys (e.g., robots, animated characters) that may be readily created and modified by changing the die cut shape of flexible packages for holding products (e.g., food stuffs) in a hermetically sealed condition (e.g., isolated from the ambient atmosphere).
BACKGROUND OF THE INVENTION
Toy manufacturers are inherently concerned with production expenses. Often in preparing plastic toys for mass production, a manufacturer goes through a lengthy mold making process. Injection molding is a primary process for manufacturing plastic parts for toys. Injection molding involves taking plastic of your choice in the form of pellets or granules and heating the plastic until a melt is obtained. Then the melt is placed into a split-die chamber/mold where it is allowed to cool and harden into the desired shape. The mold is then opened and the part is ejected, at which time the cycle may be repeated. While the cost per part is fairly low, the tooling is expensive.
Thermoforming is a technology that produces a three-dimensional structure from a two-dimensional thermoplastic sheet. The three-dimensional structure is formed by heating a thermoplastic sheet and then pulling it down onto a mold surface to shape the sheet. The structure is formed to the shape of the mold surface by vacuum forming. Then the structure is cooled and released from the mold.
A significant contributing factor to the costs of toy making is the speed of machining. Once a designer has conceived an approved design, it is imperative to convert the design concept into a prototype mold quickly since selling seasons are short. The life cycles of many toys are so short that the designers often work on very tight time schedules. Therefore, it would be beneficial to manufacture toys using a more economical solution.
Children today reap the benefits of the number of toys in the marketplace, with many children having thousands of toys to choose from at a store and hundreds of toys at their house. Despite the many available toys, a child generally has only a couple favorite toys. The other toys are either put into storage or sit around waiting for the child's attention, which is often fleeting. While many parents have ample space for their children's toys, there are some environments where space is limited. For example, children have limited space for playing with their toys in confined environments (e.g., a car), especially when space in the cramped environment is also needed to store luggage or groceries. For example, there may not always be ample space in a car for the car to hold groceries or luggage, and also to have space for many toys for the child to play with. Accordingly, it would be beneficial to provide toys that children can play with that can be used for holding a product.
SUMMARY OF THE INVENTION
These and other objects of this invention are achieved by providing a toy having an interior for holding a product (e.g., candy, coffee, cookies, foodstuff, etc.) therein. The toy is formed of a flexible material suitable for being hermetically sealed with the product located within its interior. The toy comprises a base having a bottom section arranged for moving against a surface (e.g., floor, wall, table top), and a stand-up sealable package that opens to define the interior. Preferably, the bottom section includes wheels or a transporting mechanism that rotates to roll or otherwise move the base in a predetermined manner. The base also includes an upper section having a predetermined circumference. The sealable package includes a bag or pouch having a front panel and a rear panel sealed to each other along their side edges. Each of the panels includes a lower lip having an outside surface and an inside surface. The inside surface is open to form a lower mouth therebetween. The toy is formed upon coupling the lower mouth about the circumference of the upper section of the base.
In a preferred embodiment, the package also comprises a flexible floor panel sealed to the pouch along the lower lip. The floor panel extends between the base and the interior of the package to close off and isolate the interior of the pouch from the base. In another preferred embodiment, the lower lips of the pouch are directly sealed to the base, preferably about the peripheral sides of the base. The pouch may also include a sealable upper section that opens to provide access to the interior of the pouch. The sealable section is arranged for closing and sealing the product in the interior of the package upon closure of the section. The sealable section may also include a fitment secured to the pouch. The fitment 40 preferably includes a connector (e.g., spout, valve) and a cap. The connector is hermetically sealed to the pouch and provides a conduit for access to the interior of the package. The cap securely attaches to the connector to seal the interior and disconnects from the connector to expose the interior for access therein.
The base preferably includes a motor that turns the wheels as desired to move the base against the surface. The base may also include a steering mechanism to control the direction and speed of rotation of the wheels. The steering mechanism can be adapted to control the wheels based on a signal received from a remote controller.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be described in conjunction with the following drawings in which like-referenced numerals designate like elements and wherein:
FIG. 1 is an isometric view of one exemplary embodiment of a flexible toy in accordance with a first preferred aspect of the invention;
FIG. 2 is an exploded isometric view of the flexible toy of FIG. 1;
FIG. 3 is a partial isometric view of the bottom of the pouch shown in FIG. 1;
FIG. 4 is a side elevational view partially in section of the flexible toy taken along line 4 — 4 of FIG. 1;
FIG. 5 is a partial side elevational view of the flexible toy of FIG. 1;
FIG. 6 is a longitudinal view of the base of the flexible toy shown in FIG. 1;
FIG. 7 is a side elevational view of a flexible pouch in accordance with a second exemplary preferred embodiment of the invention;
FIG. 8 is a side elevational view of a flexible pouch in accordance with a third exemplary preferred embodiment of the invention;
FIG. 9 is a sectional view of a snap closure of the pouch taken along line 9 — 9 of FIG. 8;
FIG. 10 is a side elevational view of a flexible pouch 16 having the shape of a toy in accordance with a fourth exemplary preferred embodiment of the invention; and
FIG. 11 is a side elevational view of another flexible pouch having the shape of a toy in accordance with a fifth exemplary preferred embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1-3 there is shown at 10 a toy constructed in accordance with a first preferred embodiment of the invention. The toy 10 basically comprises a flexible package 12 (e.g., container) and a base 14 . The package 12 is arranged to hold any particular material (e.g., candy, snack food, coffee, foodstuffs) and is suitable for packaging small amounts of such materials or for holding large amounts of such materials.
The package 12 includes a pouch 16 (e.g., bag) formed of a web of any conventional, flexible material, such as a laminated film. The pouch 16 basically includes a front panel 18 , a rear panel 20 , a sealable upper section 22 and a lower section 24 . The sealable upper section 22 of the pouch 16 terminates in a top marginal edge 26 . The lower section 24 of the pouch 16 terminates in a bottom marginal edge 28 . Preferably the pouch 16 is die cut to form its shape, as will be described below.
As illustrated at FIGS. 1 and 2, the front and rear panels 18 , 20 of the pouch 16 are coupled together at outer sides of the panels. The panels 18 , 20 are coupled by any conventional sealing method, for example, heat sealing, ultrasonic sealing, adhesive (e.g., epoxy sealing, etc.). The coupling of the front and rear panels 18 , 20 forms outer flanges or fins 30 . Preferably the fin 30 extends longitudinally along the sides of the pouch 16 from the top marginal edge 26 to the bottom marginal edge 28 . The fin 30 is formed by portions of the web material contiguous with the side vertical edges of the front and rear panels 18 , 20 which are brought into engagement with each other and are secured to one another via the conventional sealing technique. In addition to providing a hermetic seal between the panels, the fins 30 increase the stability of the pouch 16 , especially along portions of the pouch 16 closest to the fins 30 .
The pouch 16 is shown in FIGS. 1 and 2 in an open configuration illustrating the hollow interior 32 . The pouch 16 is flexible so that it can be economically formed and stored in a flattened configuration, with both the front and rear panels 18 , 20 abutting each other to consume a minimal amount of space. When the pouch 16 is in its open configuration, the lower section 24 can bend as desired to conform to the shape of the base 14 to fit and seal the pouch 16 to the base 14 as will be described below. As shown in FIGS. 1 and 2, the sealable upper section 22 of the flexible pouch 16 is arranged to permit ingress to the product in the interior 32 of the package 12 and to seal the product from the ambient atmosphere. When the pouch 16 is formed as described above by coupling the front and rear panels 18 , 20 , the top marginal edge 26 forms an upper mouth 34 . The upper mouth 34 includes an inner wall 36 along the inner circumference of the upper mouth 34 , and an outer wall 38 along the outer circumference of the upper mouth 34 .
As an example of a sealable upper section 22 , FIGS. 1 and 2 show a fitment 40 comprising a connector 42 and a removable cap 44 . As best shown in FIG. 2, the connector 42 includes an upper rim 46 , a dome-shaped intermediate section 48 and a lower rim 50 . The upper rim 46 forms a first opening and the lower rim 50 forms a second opening. The lower rim 50 is coupled at its circumference to the top marginal edge 26 of the pouch 16 to form a hermetic seal therebetween. The lower rim 50 is shown having a circumference slightly less than the circumference of the top marginal edge 26 . This enables the lower rim 50 to fit snugly about the inner wall 36 of the upper mouth 34 . It is also within the scope of this invention to provide a lower rim 50 that fits about the outer wall 38 of the upper mouth 34 or to provide a lower rim 50 that abuts the top of the upper mouth 34 , as long as the connector 42 and the pouch 16 are hermetically sealed.
In this embodiment, the connector 42 is formed of any conventional lightweight material (e.g., plastic) and is semi-rigid having a dome-like shape. The intermediate section 48 extends from the lower rim 50 to the upper rim 46 , and has a circumference that decreases toward the upper rim 46 . The connector's upper rim 46 is basically cylindrical in shape and has a circumference less than the circumference of the lower rim 50 . Coupling the connector 42 to the upper mouth 34 of the pouch 16 increases the stability of the pouch 16 towards the upper section 22 of the pouch 16 . In other words, the upper section 22 of the flexible pouch 16 becomes more sturdy when it is attached to the semi-rigid connector 42 as is readily understood by a person skilled in the art. This increased stability enables the package 12 to stand and retain its shape for better use as a toy 10 .
The removable cap 44 is arranged to seal the interior 32 of the package 12 from the atmosphere external to the package 12 . As can best be seen in FIG. 2, the exemplary cap 44 has a flat disc-like top 43 and a cylindrical shaped flange 45 longitudinally extending from the underside of the top adjacent its outer rim. The cylindrical flange 45 is constructed to frictionally engage the upper rim 46 of the connector 42 . For example, as shown in FIGS. 1 and 2, the cylindrical flange 45 couples about the upper rim 46 of the connector 42 when the cap 44 is placed upon the connector 42 . The cap 44 connects to the connector 42 using any conventional method (e.g., screw or push on). This exemplary cap 44 is a push on lid with a flange 45 having an inner circumference about equal to the outer circumference of the upper rim 46 of the connector 42 such that the flange 45 frictionally extends about the outer circumference of the upper rim 46 to secure the cap 44 to the connector 42 . The cap 44 can be placed on and taken off of the connector 42 as desired to access the contents of the interior 32 of the flexible pouch 16 .
For safety purposes, the fitment 40 may also include a removable safety cover that forms a tamper-proof seal. This cover is placed over the first opening defined by the upper rim 46 of the connector 42 and provides a one-time seal notwithstanding the seal provided by the cap 44 placed over the upper rim 46 of the connector 42 . The safety cover is preferably placed over the upper rim 46 after the package 12 is initially filled with a product and is removed by the user after purchase. Prior to its removal, the cover can be inspected to ensure that the package 12 was not tampered with by another prior to purchase.
As can be seen in FIGS. 3 and 4, the package 12 also includes a flexible floor panel 52 for sealing the lower section 24 of the package 12 . The floor panel 52 is preferably formed of the same material as the front and rear panels 18 , 20 (e.g., laminated film). The floor panel 52 is sized to extend across the interior 36 and abut the inner wall 36 of the front and rear panels 18 , 20 . The floor panel 52 is secured to the inner wall 36 of the lower section 24 using any conventional sealing technique (e.g., heat sealing, welding, adhesive, etc.) to form a hermetic seal between the entire perimeter of the floor panel 52 and the lower section 24 .
When the package 12 is flat, the floor panel 52 folds along a crease 54 and is substantially flat. When the package 12 is open, as shown in FIGS. 3 and 4, the floor panel 52 unfolds and forms a cup-like shaped layer having a vertically extending wall 68 sealed along the inner wall 36 of the lower section 24 . In this manner, the floor panel 52 provides a layer between the interior 32 of the package 12 and the atmosphere external to the package 12 to seal the product in the package 12 .
As can be seen clearly in FIGS. 4-6 the base 14 preferably has a cylinder-like shape and is rounded off of its bottom edge 56 . The base 14 includes an upper region 58 , a lower region 60 , wheels 62 , a motor 64 and a battery 66 . As shown in FIGS. 4 and 5, the upper region 58 is fitted and secured within the inner wall 36 of the package 12 . In FIG. 4, the upper region 58 is secured to the vertically extending wall 68 of the floor panel 52 . In FIG. 5, the upper region 58 is sealed directly to the inner wall 36 of the lower section 24 . While the upper region 58 can be sealed to the package 12 using any conventional method as discussed above for securing the panels together, the exemplary bases shown in FIGS. 4 and 5 are sealed to the package 12 with a layer of epoxy cement 74 between the radial peripheral side of the upper region 58 and the adjoining inner wall 36 of the floor panel 52 (FIG. 4) or lower section 24 (FIG. 5 ).
The wheels 62 of the base 14 rotate for rolling the toy 10 against a surface (e.g., floor, wall, table top). The battery 66 communicates with the motor 64 and provides power to the motor 64 for driving at least one of the wheels 62 . The driving wheels 62 are attached to the motor 64 via axles 70 extending between the attached wheels 62 and the motor 64 . The axles 70 rotate based on the motor 64 and turn the driving wheels 62 . The base 14 may also include a steering mechanism 72 for turning the toy. The exemplary base 14 shows the steering mechanism 72 integrated with the motor 64 . It is also within the scope of this invention to provide the steering mechanism 72 separate from the motor 64 and communicating with at least one of the wheels 62 to turn the toy as it moves along a surface. The motor 64 may also operate based on input from a remote controller as known to a skilled artesian for operating the movement of the toy.
As discussed above in FIG. 5, the pouch 16 is sealed directly to the base 14 to create a hermetic seal. The inner wall 36 of the lower section 24 surrounding the package 12 is preferably permanently sealed to the base 14 along a seam line formed between the periphery of the base 14 and the lower section 24 as described above and shown in FIG. 5 . This approach provides the benefit of a hermetic seal formed along the bottom marginal edge 28 of the package 12 without the floor panel 52 shown in FIGS. 3 and 4.
FIG. 6 is a longitudinal view of the lower region 60 of the base 14 . The lower region 60 includes a base floor 76 , which supports the motor 64 and includes openings 77 through which each of the wheels 62 extend. In this example, the driving wheels 62 are connected to the axles 70 inside of the base 14 and extend through the openings 77 in the base floor 76 where they can roll along a surface. The free wheels 62 are rotatably coupled to the base 14 , preferably at the base floor 76 .
FIG. 7 shows a second exemplary preferred embodiment of the flexible pouch 16 In FIG. 7, the pouch 16 a is formed by the front and rear panels 18 , 20 of web material sealed along the peripheral sides and a lower section 24 . The lower section 24 is sealed at the bottom marginal edge 28 along a curved seam line (FIG. 7) such that when the pouch 16 a is opened, the lower section 24 rotates under the pouch 16 a and forms a somewhat bowl-like configuration. Using this configuration, the pouch 16 a preferably attaches to the top surface of the base 14 or within upwardly extending outer peripheral walls of the base 14 . It is understood that the pouch 16 a is securely sealed to the base 14 to prevent any unwanted separation during handling of the toy.
Another example of a flexible pouch is shown at FIG. 8 . The pouch 16 b basically comprises a front panel 18 , a rear panel 20 and a gusseted floor panel 52 . The front and rear panels 18 , 20 have side edges 78 , a top end portion 79 and a bottom end portion 81 . The top end portions of the front and rear panels 18 , 20 terminate in a top marginal edge 26 . The bottom end portion of the front and rear panels 18 , 20 terminate in a bottom marginal edge 28 . The side edges 78 are hermetically sealed and form fins 30 using any conventional sealing technique as discussed above. As shown, side edges 78 of the front and rear panels 18 , 20 are sealed from the top marginal edge 26 to the bottom end portion 81 .
The gusseted floor panel 52 of the flexible pouch 16 b is an integral portion of a single sheet or web of the flexible material, of single or multiple ply or layers. The floor panel 52 has a width terminating at side edges 78 . The width is substantially equal to the width of the front and rear panels 18 , 20 . The floor panel 52 also includes bottom edges that extend approximately to the bottom marginal edge 28 of the pouch 16 b. The floor panel 52 is folded and seamed to form a floor layer having a crease 54 similar to the floor layer shown in FIG. 3 . The floor panel 52 extends from the crease 54 to the bottom edges.
In this exemplary pouch 16 b, the floor panel 52 is hermetically sealed to both the front panel 18 and the rear panel 20 along the side edges 78 and bottom marginal edge 28 , thereby forming a gusseted bottom. An unfolded floor panel 52 forms a flattened floor layer similar to the floor layer shown in FIGS. 3 and 4. In this position, the pouch 16 b becomes cylindrical at its bottom end portion 81 , and the bottom marginal edge 28 of the front and rear panels 18 , 20 is sufficiently planar so the pouch 16 b can stand on its bottom marginal edge 28 . In other words, when the pouch is opened, the gusseted bottom separates about its crease 54 to form a floor layer and vertically extending wall 68 as can be seen in FIG. 3 . The flexible pouch 16 a shown in FIG. 7 is an exemplary non-gusseted stand up package 12 , and the flexible pouch 16 b shown in FIG. 8 is an exemplary gusseted type stand up package 12 .
FIG. 9 illustrates an exemplary integrated snap closure 80 for reclosing and resealing the pouch 16 of FIG. 8 after the pouch 16 has been opened. As can be seen in FIGS. 8 and 9, the front and rear panels 18 , 20 include an upper section 22 , which between the panels 18 , 20 define an opening 82 in the pouch 16 . The snap closure 80 is provided within this opening 82 . The snap closure 80 basically comprises a pair of snap strip members 84 , 86 secured to respective portions of the front and rear panels 18 , 20 . Each of the strips 84 , 86 is formed of a flexible material (e.g., a plastic material, such as high or low density polyethylene or polypropylene or some other material) which is slightly flexible to enable it to be bent out of its original shape by the application of force thereto, but returns to its original shape after removal of that force. Each strip 84 , 86 extends the width of the panel 18 , 20 to which it is secured. Each strip 84 , 86 is arranged to be fixedly secured, e.g., welded or permanently adhesively secured to the inner surface of the upper section 22 of the respective panel 18 , 20 adjacent the top marginal edge 26 and across the full width of the strip 84 , 86 .
The strip 84 basically consists of an elongated tongue-shaped member 88 . In particular, this strip 84 includes an elongated planner upper flange section 90 , an elongated planner lower flange section 92 and an intermediate projecting tongue section 94 . The tongue section projects perpendicularly upward from respective planner flange sections 90 , 92 and has a transversely cylindrical shape that appears bulbous in its cross section (FIG. 9 ).
The strip 86 basically consists of an elongated channel or recess-shaped member 96 . In particular, the strip 86 includes an elongated planner upper flange section 98 , an elongated planner lower flange section 100 and a generally C-shaped intermediate section 102 defining a groove or recess 104 therein.
The material forming the strips 84 , 86 is somewhat elastic and/or flexible to enable the tongue 88 of the strip 84 to snap fit into the groove or recess 104 of the strip 86 , and to be locked therein against accidental disconnection, yet which enable the tongue 88 to exit that recess 104 when the strips 84 , 86 are pulled apart. It must be pointed out that the strips 84 and 86 can be mounted and secured to the rear panel 20 and front panel 18 , respectively, instead of to the front panel 18 and rear panel 20 , respectively. It must also be pointed out that the strips 84 , 86 can be mounted and secured to the front and rear panels 18 , 20 of the flexible pouch 16 a shown in FIG. 7 . Thus, the embodiments of FIGS. 7 and 8 are merely exemplary.
Notwithstanding their slight elasticity, the strips 84 , 86 are substantially rigid so that when they are snapped together, the strips 84 , 86 serve to hold the upper section 22 of the front panel 18 tightly against the top portion of the rear panel 20 . The recess 104 of strip 86 tends to reinforce the strips 84 , 86 and keep them linear to further insure that the opening 82 of the package 12 is sealed closed when the strips 84 , 86 are snap connected to each other. Thus when the strips 84 , 86 are snapped together, the contents of the pouch 16 are effectively isolated from the ambient surroundings so that it can be kept fresh over an extended period of time.
Other exemplary embodiments of the toys constructed in accordance with this invention are shown in FIGS. 10 and 11. The toy 110 shown in FIG. 10 is cut in the shape of an animal and includes a pouch 16 c constructed in a substantially similar manner to that of the pouches and packages shown at FIGS. 1, 2 , 7 and 8 , and described heretofore. The shape of the pouches are defined by the shape of the die. The toy 120 shown in FIG. 11 is formed in the shape of an angel and includes a pouch 16 d constructed in a substantially similar manner to that of the pouches and packages described heretofore. The pouches shown in FIGS. 10 and 11 are provided as examples of alternative toy figures that provide playful pleasure to a child. Both pouches can be filled with a product (e.g., candy, foodstuffs) and fixed to the base 14 as described above as a combination toy with food package 12 . By providing a combination toy and food package 12 in one product, a child can play with the toy without taking up extra space for the product stored in the pouch 16 . Accordingly, space is used more efficiently, because the same space is occupied as both a food package 12 and a toy.
It should be apparent from the aforementioned description and attached drawings that the concept of the present application may be readily applied to a variety of preferred embodiments, including those disclosed herein. Thus, as will be appreciated by those skilled in the art, the closures of this invention, the shapes of the package 12 and features of the toy 10 can be modified insofar as its construction and/or material composition is concerned in order to accommodate the preferred uses of the toy 10 . For example, the package 12 can also have the shape of a robot or a vehicle (e.g., car, truck, airplane, train, etc.). In addition, the base can include other types of rolling members (e.g., one wheel, ball bearings, rollers, tractor treads, spoked hubs, etc.). The rolling member could also be placed horizontally (with a vertical axis) and rotate the toy about the axis. Moreover, the package need not be hermetically sealed. In fact other resealable approaches could be used in addition to the fitment and snap closure described herein. For example, the package could be provided with an easy opening top or tab. Further, the package could have a seal separate from the fitment such that the fitment is used after the package is initially opened by the user.
Without further elaboration the foregoing will so fully illustrate our invention that others may, by applying current or future knowledge, adopt the same for use under various conditions of service.
|
A toy including stand up flexible pouch or other flexible type pouch affixed to a rollable mechanical base and method of making the toy. When assembled, the toy may be manually or remotely controlled to roll or move about in a predetermined direction or fashion. The flexible pouch is shaped and printed to resemble a desired character while still maintaining its ability to contain a product. The base apparatus includes rolling members, e.g., wheels, to allow the base to be rolled or otherwise moved across a surface. The pouch and base are joined together, for example, by heat sealing, ultrasonic sealing, adhesives, etc. The rollable base may include a battery or other power source and/or electronics allowing for remote controllability of the assembled toy. The flexible pouch may contain a separate food or other product and a fitment, snap closure or other type of reclosure as desired.
| 8
|
This is a continuation-in-part application of application Ser. No. 07/901,412 filed Jun. 19, 1992 now abandoned.
FIELD OF THE INVENTION
The present invention relates in general to a turbine transferring energy between a moving fluid and a rotating shaft, and more specifically to the shape of an axial flow turbine which controls turbulence and which balances axial, angular and static pressures of the fluid as the fluid travels along the length of the turbine.
BACKGROUND OF THE INVENTION
Existing axial flow turbines such as Kaplan, Brauer (U.S. Pat. No. 1,065,208 6/1913), and propeller types have a specific range of pressures and fluid velocities which they can be efficiently operated in. Outside of this range these turbines will either become inefficient due to internal generation of turbulence, or cease to function because of the phenomenon known as cavitation. Such prior art axial flow turbines are unable to preclude cavitation because gradients in these turbines become too large when these turbines are operated outside their range. Further, present day turbo machine technology does not provide an axial flow turbine capable of transferring power between its rotor section and a gas while maintaining the static pressure of the gas, its density and temperature substantially constant.
Furthermore, an axial flow turbine as described by Johnson, U.S. Pat. No. 2,808,225 10/1957, does not contemplate a substantial reduction of the air axial and angular velocities. On the contrary, this turbine, as well as existing steam turbines, all work on the pressure drop and the corresponding expansion and acceleration of the gas as it moves along the length of their rotors. Due to its intended application as a high speed dental drill, the Johnson turbine does not consider efficiency as an important design criterion.
SUMMARY AND OBJECTS OF THE INVENTION
It is an object of the invention to provide an axial flow turbine design that maintains the static pressure along the rotor section of the turbine substantially constant. This feature will allow us to preclude cavitation in high pressure applications involving liquids, and will allow us to design an axial flow turbine that can be applied over a wide range of combinations of volume flow and pressure. This substantially constant static pressure along the rotor section of the turbine will also allow us, in applications involving a gas, to exchange power between the rotor and the gas without changing the static pressure, the density and the temperature of the gas.
Turbulent flow is the cause of some of the power losses in an axial flow turbine. These losses are caused by velocity, vectors in the fluid going in directions different from the desired direction which produces an inefficient power exchange between the turbine and the fluid. It is also an object of the invention to provide design criteria to minimize power losses due to turbulence in an axial flow turbine.
Cavitation occurs in applications involving a liquid when the static pressure, at any point in the turbine, drops below certain limits which are determined by the operating temperature, the vapor pressure of the liquid at the operating temperature and the gases dissolved in the liquid. Under this low static pressure the liquid forms a void or bubble of vapor which will later collapse at another point along the turbine where the static pressure increases above the limits which caused the bubble to form. The collapse of the bubble will produce a shock wave that carves or erodes the turbine at the point of collapse, causing permanent damage. Also the formation of the bubble will produce a reduction of the density and a corresponding loss of power, thus lowering the efficiency of the turbine. It is also another object of the invention to provide design criteria for the control of cavitation in an axial flow turbine.
Changes in density and temperature in a gas while the gas is exchanging power with a turbine rotor will cause loss of power and thus cause a corresponding loss of efficiency. It is yet another object of the invention to provide design criteria for minimization of thermodynamic power losses in an axial flow turbine when it is used in applications involving a gas.
According to the invention, a fixed section preferably is provided in the high static pressure side of the turbine wherein a core or hub, and a jacket or pipe cooperate to provide a variation in the magnitude of cross sectional area left for fluid transit. This variation of area left for fluid transit produces an axial acceleration of the fluid and provides a corresponding static pressure gradient. The invention also provides simultaneously, in the fixed section, for fixed helicoid blades having a varying angle of inclination with respect to the axis of the turbine and located in the area left for fluid transit. Such varying angle of inclination of the blades along the length of the fixed section provides a smooth angular acceleration of the fluid and a corresponding static pressure gradient additional to the static pressure gradient caused by the axial acceleration of the fluid mentioned above.
The invention also provides simultaneously a rotor (movable) section in the low pressure side of the turbine wherein a rotor core or hub and a rotor jacket or pipe cooperate to provide a variation in the magnitude of cross sectional area left for fluid transit. Such variation of area is designed to cause an axial acceleration of the fluid and provide a corresponding static pressure gradient opposite in sign to the variation of static pressure caused by the variation of area left for fluid transit in the fixed section. The invention also provides simultaneously (in the rotor section), for helicoid blades having a varying angle of inclination with respect to the axis of the turbine and located in the area left for fluid transit. Such blades causing an angular acceleration of the fluid opposite in sign to the acceleration caused by the blades in the fixed section, but creating a pressure gradient of the same sign as the pressure gradient created by the blades in the fixed section. In the rotor section, the pressure gradient created by the axial acceleration of the fluid is opposite in sign to the pressure gradient created by the angular acceleration of the fluid. Both of these pressure gradients in the rotor section will cancel each other and thus, the static pressure will be maintained substantially constant along the rotor section, while most of the power will be exchanged between the fluid and the rotor.
A set of different embodiments of the invention are disclosed using an axial flow turbine as noted above. Besides the features of the invention described above, all embodiments disclosed herein will provide no acceleration of the fluid at the entrance and exit points of the different sections, and will provide a sinusoidal distribution, preferably a half sinusoidal wave, of the axial and angular accelerations along the length of each section. This sinusoidal distribution of accelerations will maintain turbulence at low levels, and will also determine the shape of the hubs, the jackets and the helicoid blades.
The various features of the novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and specific objects attained by its uses, reference is made to the accompanying drawings and descriptive matter in which preferred embodiments of the invention are illustrated.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIGS. 1a, and 1b are diagrams showing the cooperation of a hub 10 and a Jacket 11 to provide acceleration of a passing fluid, by means of a continuous reduction of the cross sectional area left for fluid transit;
FIGS. 1c-1e are graphs of pressure, velocity, and acceleration of the fluid as it travels through the passage of FIGS. 1a or 1b from point 1 to point 2;
FIG. 2a and 2b is a diagram showing the cooperation of a hub 10 and a Jacket 11 to provide deceleration of a passing fluid, by means of a continuous increase of the cross sectional area left for fluid transit.
FIGS. 2c-2e are graphs of pressure, velocity, and acceleration of the fluid as it travels through the passage of FIGS. 2a or 2b from point 1 to point 2;
FIG. 3a is a diagram showing a fixed blade passage that angularly accelerates a passing fluid, by means of a fixed helicoid blade 12, which continuously increases its angle of inclination with respect to the axial direction;
FIGS. 3b-3d are graphs of pressure, velocity, and angular acceleration of the fluid as it travels through the passage of FIG. 3a from point 1 to point 2;
FIG. 4a is a diagram showing a fixed blade passage that angularly decelerates a passing fluid, by means of a fixed helicoid blade, which continuously decreases its angle of inclination with respect to the axial direction;
FIGS. 4b-4d are graphs of pressure, velocity, and angular acceleration of the fluid as it travels through the passage of FIG. 4a from point 1 to point 2;
FIG. 5a is a diagram showing a rotatable blade passage that receives a fluid with an angular velocity and angularly decelerates the fluid by means of a rotatable blade which increases its angle of inclination with respect to the axial direction;
FIGS. 5b-5d are graphs of pressure, velocity, and angular acceleration of the fluid as it travels through the passage of FIG. 5a from point 1 to point 2;
FIG. 6 is a diagram showing a turbine of the present invention;
FIG. 7 is a diagram showing a mass of fluid contained between two rings.
FIG. 8 is a diagram showing a turbine of the present invention used as a hydraulic motor or as a pump.
FIG. 9 is a diagram showing a turbine of the present invention used as a propeller for a water vehicle.
FIG. 10 is a diagram showing a turbine of the present invention used as an air driven motor or as a fan.
FIG. 11 is a diagram showing a turbine of the present invention used as an internal combustion engine.
FIG. 12 is a diagram showing a turbine of the present invention used to produce power from flowing fluid.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, and in particular to FIGS. 1 and 2, we may appreciate how a core 10 or hub and a jacket 11 or pipe cooperate to produce an axial acceleration of the fluid and a corresponding static pressure change. The axial variation of diameters of the hub and/or the jacket cause a variation of the cross sectional area left for fluid transit. This variation of area left for fluid transit produces the changes in axial velocity of the fluid, as the fluid travels along the length or the devices. Pressure (P), velocity (V), and acceleration (A) distribution curves are shown (under the conceptual device drawings), to facilitate understanding of the changes which take place, as the fluid travels along the length of the devices.
In FIGS. 1a and 1b, the fluid is accelerated and the static pressure drops as the fluid advances along the length of the device. We may say that static pressure is being converted into axial dynamic pressure. We may also say that a positive axial acceleration of the fluid and a corresponding negative static pressure change are taking place as the fluid moves along the length of the device. The changes in static pressure can be calculated according to the following formula:
P.sub.2 -P.sub.1 =1/2σ(V.sub.2.sup.2 -V.sub.1.sup.2) (1)
Where σ represents the density of the fluid, P 1 and P 2 the static pressures at the entrance and exit points respectively, and V 1 and V 2 the axial velocities of the fluid at the entrance and exit points respectively.
The power corresponding to axial velocity (Pow v ) is:
Pow.sub.v =1/2Fm(V.sub.1.sup.2 -V.sub.2.sup.2) (2)
Where Fm represents the mass rate of flow, or volume rate of flow Q times the density σ.
In FIG. 2a and 2b, the fluid is decelerated and the static pressure increases as the fluid advances along the length of the device. We may say that axial dynamic pressure is being converted to static pressure. We may also say that a negative axial acceleration of the fluid and a corresponding positive static pressure change are taking place as the fluid moves along the length of the device. Formula 1 can also be used to calculate the pressure change.
In the case of the fluid being axially accelerated, (as in FIG. 1) the result of Formula 1 will be negative, representing a static pressure drop. If, on the other hand, the fluid is axially decelerated (as in FIG. 2), then the result of Formula 1 will be positive, representing a static pressure increase.
In the fixed section of FIG. 6, we convert all the available static pressure into a well balanced set of axial and angular dynamic pressures. A set of well balanced dynamic pressures means that they are equivalent in magnitude. In other words, it means that the power represented by the change in angular velocity is equivalent to the power represented by the change of axial velocity. Therefore, as the axial and angular velocities are lowered in the rotor section (in a hydraulic motor), they will progressively cancel each other from entrance to exit. Under these conditions of dynamic pressure balance, the rotor section will not experiment a substantial static pressure variation from its entrance to its exit points. This feature of the herein proposed axial flow turbine is important for precluding cavitation in high pressure applications which deal with liquids and for maintaining substantially unaltered the thermodynamic state of the fluid in applications involving gases.
FIGS. 3a, 4a, and 5a, represent a Brauer type turbine blade, modified to include varying angle of inclination (helicoid) blades 12, instead of the helical (constant angle) blades proposed by Brauer. The varying angle of inclination of the blades will allow us to procure a smooth (controlled) angular acceleration of the fluid as it travels inside the device. No variation of the axial velocity of the fluid takes place in these arrangements, since there is no variation of the area left for fluid transit along the length of the devices and the mass flow rate must be constant. The angle of inclination of the blade 12 at any point along the axis of the device, and taken at the rotational center of mass radius Rcm, can be calculated using the following formula:
α=Arctangent(V.sub.t /V) (3)
where V t is the tangential velocity of the fluid and V is the axial velocity of the fluid.
FIG. 3, represents a fixed (nonrotational) device in which the fluid enters with no angular velocity and is angularly accelerated by the blades as it travels along the length of the device. The angular acceleration of the fluid with respect to axial distance will produce a static pressure drop along the length of the device as shown in FIG. 3b. Thus, the fluid will exit the device at a lower static pressure and with angular velocity as shown in FIG. 3c. We may say that a positive angular acceleration and a corresponding negative static pressure change are taking place as the fluid travels along the length of the passage of FIG. 3a. We may also say that static pressure is being converted to angular or rotational dynamic pressure as the fluid travels along the length of the device. The pressure change can be calculated according to the following formula:
P.sub.2 -P.sub.1 =1/2σ(V.sub.t2.sup.2 -V.sub.t1.sup.2)(4)
Where V t1 and V t2 represent the tangential velocities of the fluid as taken at an average rotational center of mass radius (Rem). This center of mass radius can be calculated using the following formula:
Rcm=2(R.sub.e.sup.3 -R.sub.i.sup.3)/3(R.sub.e.sup.2 -R.sub.i.sup.2)(5)
Where R e represents the external radius of the fluid transit area, or the internal radius of the jacket and R i the internal radius of the fluid transit area or the external radius of the hub.
The tangential velocities can be calculated as:
V.sub.t =RcmW (6)
Where W represents the angular velocity of the fluid.
FIG. 4a represents a fixed (nonrotational) blade passage in which the fluid enters with angular velocity and exits with no angular velocity. As the angular velocity of the fluid diminishes, the static pressure increases. We may say that angular dynamic pressure is being converted to static pressure as the fluid travels along the length of the device. Formula 2 can be used to calculate the pressure change.
FIG. 5a represents a rotational device (rotor) in which the fluid enters with an angular velocity equal to the angular velocity of the blade 12 or rotor and exits with no angular velocity. As seen from outside of the device, the fluid is loosing angular velocity. But, for an observer who is rotating with the device at the upstream end, the fluid enters with no angular velocity and is being angularly accelerated in an opposite direction to the rotation of the rotor as it travels towards the exit. This angular acceleration of the fluid (as seen by the rotating observer) requires a static pressure drop. In the situation as seen from an external static observer, we are lowering the angular velocity of the fluid, and at the same time, lowering the static pressure. We may then say that a rotational dynamic pressure in combination with a static pressure drop are transferring power to the rotating device. This power Pow and the corresponding torque τ can be calculated using the following formulas:
Pow=Pow.sub.w +Pow.sub.p (7)
Pow.sub.w =1/2Fm(V.sub.t1.sup.2 -V.sub.t2.sup.2) (8)
Pow.sub.p =Q(P.sub.1 -P.sub.2) (9)
Where Q represents volume rate of flow, and Pow w and Pow p represent the power corresponding to angular velocity and pressure respectively.
Tao=Pow/W.sub.s
Where W s represents the angular velocity of the shaft.
In a Brauer type turbine as shown in FIG. 5, the change in pressure from the input to the output could cause cavitation and corresponding turbulence if it became too large. Therefore, Brauer type turbines can only operate under specific conditions where the pressure drop would not be too large.
FIG. 6 represents a turbine constructed using different combinations of the passages in FIGS. 1-5 to obtain the desired features that are being proposed in the present invention. In particular the passage of FIG. 2 is combined with the passage of FIG. 5 to form the rotor section of the turbine of the present invention. The present invention adjusts the cross sectional area of FIG. 2 and the angle of the blade in FIG. 5 in order to have the pressure gradients to be substantially complementary. Therefore the static pressure along the rotor section of the present invention will be substantially constant. The upstream and downstream portions of the rotor section can be fitted with combinations of the passages in FIGS. 1-5 in order to properly condition the fluid flowing through the rotor section in such parameters as proper cross sectional area, angular velocity, and pressure.
In FIG. 6, and particularly referring to the fixed section, the combination of the device described in FIG. 1a and 1b, especially FIG. 1a, with the device described in FIG. 3a, forms a fluid accelerator. In this fixed section, static or head pressure is converted to axial and angular dynamic pressures as the fluid travels from the entrance to the exit of this fixed section. The total static pressure drop that is converted to axial and angular dynamic pressures can be calculated by adding the results of applying formulas 1 and 4 and can be seen by combining the graphs of FIGS. 1c and 3b.
Also in FIG. 6, and particularly referring to the rotor section, we may appreciate that the rotor proper is formed by the combination of the passage described in FIG. 2a with the passage shown in FIG. 5a. As was earlier explained, the passage in FIG. 5 (a modified Brauer rotor), decelerates the fluid angularly (as seen by an external observer), but simultaneously there is a static pressure drop. Now, as indicated in the section where FIG. 2 was described, there is a static pressure increase when the fluid experiences a decrease in axial velocity. Therefore, the combination of both passages to form a rotor will produce a rotor capable of processing the fluid without substantially modifying the static pressure.
In the fixed section of FIG. 6, we convert all the available static pressure into a well balanced set of axial and angular dynamic pressures. A set of well balanced dynamic pressures means that they are equivalent in magnitude. In other words, it means that the power represented by the change in angular velocity is equivalent to the power represented by the change of axial velocity. Therefore as the axial and angular velocities are lowered in the rotor section (in a hydraulic motor), they will progressively cancel each other from entrance to exit. Under these conditions of dynamic pressure balance, the rotor section will not experience a substantial static pressure variation from its entrance to its exit points. This feature of the herein proposed axial flow turbine is important for precluding cavitation in high pressure applications which deal with liquids and for substantially maintaining the thermodynamic state of the fluid unaltered in applications involving gasses.
FIG. 6 can also represent a pump (instead of a turbine) if the direction of fluid flow is reversed. In this case, power must be applied to the shaft by an external motor. The rotor will produce axial and angular dynamic pressures in the fluid, while maintaining the static pressure substantially constant. The fixed section will subsequently convert both axial and angular dynamic pressures into static or head pressure, by diminishing the axial velocity and stopping the angular motion of the fluid.
FIG. 7 shows two concentric pipe segments which enclose a mass (m) of fluid in the shape of a ring Oust as an imaginary ring of fluid mass at any section perpendicular to the axis along the turbine shown in FIG. 6). The center of the fluid mass (symbol cm, FIG. 7) coincides with the center of both circumferences at the internal and external boundaries of the ring of fluid. Symbols R e and R i represent those external and internal radii respectively. The Rotational Center of Mass Radius (symbol Rcm) of the mass of fluid is the radius of the circumference (drawn in dotted line) between the boundaries of the ring of fluid. Symbol Rcm represents the radius of the circumference at which the mass of fluid (m) can be thought of as being concentrated for angular acceleration calculations.
By applying a static pressure on one side of the ring of mass, we produce a pressure wave traveling in the direction of the lower static pressure particles which conform our a ring of mass, increasing their motion vectors in the direction in which the wave is traveling. The final result will be that our ring of mass will start moving in the direction opposite to the higher pressure side, at a velocity proportional to the static pressure difference. If we see the set of particles as concentrated in the center of mass (cm), we may say that the center of mass has now an axial velocity. This velocity can be calculated according to the following formal:
V=√(2(P.sub.2 -P.sub.1)/σ) (11)
We may then interpret, according to the Kinetic Theory of Fluids, that by applying a pressure difference to a mass of fluid, we may have increased its energy content and this energy has been used in orienting internal micro-motion into macro-motion of the entire mass. But, the motion vectors that we have affected are only the components in the direction perpendicular to the plane of the pressure. The vector components parallel to this plane, have not been affected.
Turbulence can be considered as a set of motion vectors going in directions other than the desired direction. Micro-motion can also be considered as turbulence at particle levels. In order to orient these vectors in a particular useful direction (thus improving efficiency), we must interpose a blade that is inclined at an angle with respect to the axial motion of our ring of mass. On the surface facing higher pressure, this blade will convert static pressure to angular velocity. On the surface facing lower pressure, it will orient the radial motion components into motion components going in the axial direction. If the blade is made to cover one half of a revolution, then all radial motion vectors (regardless of their original direction) will be processed as our ring of mass travels along the axial distance covered by the blade. At the end of the blade our ring of mass will have axial and angular motion and little turbulent motion. The energy carried by the resulting axial and angular velocities can be subsequently changed to pressure or other types of energy as explained above, when describing FIGS. 1-6.
The conclusion is that a blade that extends for one half of a revolution will process motion vectors going in all possible radial directions. Also, if we use two blades in a configuration such as shown in FIG. 6, the solidity of the passage will be equal to one, and all possible axial motion vectors will be processed by the blades, as well. The result of the combination of all the considerations explained above, is the preferred embodiment of the present invention. The present invention however is not limited to only two blades. A single blade or more than two blades can be used and still incorporate the fundamental ideas set forth in this invention.
FIGS. 8 and 12 represent a use of the turbine proposed herein as a hydraulic motor. The fixed section has blades that angularly accelerate the fluid throughout one half of a revolution. This processing of the fluid for one half of a revolution is done to make sure that all motion vectors of the fluid particles are made to go in the desired directions. The rotor section processes the fluid without substantially changing the static pressure. This substantially constant static pressure will allow for operation of the turbine without cavitation, and the minimum static pressure conditions will be determined by the height of the turbine above the spill level and the suction created by the exhaust cone (if used). Both of these conditions are under control of the designer.
In this hydraulic turbine, two elbows guide the fluid into the fixed section and out of the rotor section. They also allow the shaft to pass to the exterior, hold the seals to prevent leakage, and provide support to the shaft bearings. The same configuration can be used as a pump if the fluid direction is reversed and power is applied to the shaft.
FIG. 9 represents the propeller for a vehicle in water. The rotor is located at the fluid entrance side and the fixed section at the fluid exit side. The rotor accelerates water axially and angularly, while maintaining the static pressure substantially constant. The fixed section will further accelerate the water axially by removing the angular component by means of blades that straighten the flow. Thus, the power available as angular velocity is converted to axial velocity by reducing the area left for fluid transit in the fixed section. The fluid will then exit the fixed section as a jet which produces thrust. The fixed section may also contain support bearings for the shaft.
FIG. 10 represents an eolic application of the turbine proposed herein. This embodiment can be used as an air driven motor, and can be applied, for example, to produce electric power by attaching a generator to its shaft. The reverse is also possible and this embodiment can function as a fan if power is applied to the shaft. In this case, the direction of air flow is the reverse as in the air driven motor. Please notice that the jacket or pipe in the rotor section of this application is attached to the blades and rotates with the blades and the core. It was chosen to be attached in order to attain more rigidity of the moving structure and therefore a lighter piece.
FIG. 11 represents a use of the turbine proposed herein as an internal combustion engine. It is formed using two fixed sections and two rotatable sections. The rotatable sections are connected by a shaft.
The first section is the rotatable air accelerator. It is built by an increasing diameter hub with decreasing angle of inclination blades attached to it. This combination of hub and blades, in cooperation with a fixed jacket, produces angular and axial acceleration of the air while keeping the static pressure, the density and the temperature substantially constant.
Following the accelerator section is a fixed (non-moving) pressurizer section built with a cylindrical hub and diminishing angle of inclination blades attached to the hub and to the fixed external jacket. This combination of parts produces pressurization of the air by decelerating the air rotationally while keeping the axial velocity substantially constant. It is in this pressurizer section where thermal energy is added to the air, before it enters the turbine section. A small part of the air at the end of the accelerator section is taken into the burner section which surrounds the external jacket. This air is pressurized by slowing it down axially and angularly. Fuel is injected to the burner section and the products of combustion are fed into the pressurizer section through bores on the external jacket. Bearings for the shaft are included inside the hub of this section.
The rotatable turbine section is built using a combination of a cylindrical hub with increasing angle of inclination blades attached to it (a modified Brauer turbine). The hub was chosen to be cylindrical to facilitate construction and also to illustrate the possibility of different arrangements of the turbine, but a diminishing diameter hub can also be implemented in this section. The blades in this section cover one half of a revolution, in order to process all pressure wave vectors as the air moves from the entrance to the exit of the section, as was shown in other applications described above. Air enters this section at high axial velocity and with no angular velocity. It is angularly accelerated in a direction opposite to the angular velocity of the accelerator section, thus producing torque in the shaft to move the air accelerator and to produce mechanical power outside the motor.
The final section of the internal combustion engine is the fixed (nonrotatable) exit section. It is built using a diminishing diameter hub and blades of diminishing angle of inclination attached to the hub and the jacket. A small diameter cylindrical hub can be implemented in this section if the hub of the previous (turbine) section is chosen to have a diminishing diameter. Air enters this section, when built as shown in FIG. 11, at high axial velocity and high angular velocity and is slowed axially and angularly. As it is slowed, a pressure increase is obtained towards the exit point. Since the pressure outside the motor is atmospheric pressure, the pressure increase created by the blades and the hub in the exit section is seen as a suction, which signifies an additional pressure drop across the turbine section. The power given by this pressure drop is extra power available through the shaft. The hub of this section may also include bearings for the shaft.
CALCULATION SAMPLE OF A HYDRAULIC TURBINE ACCORDING TO THE INVENTION
Refer to the illustrations in FIGS. 8 and 12.
1) SYSTEM CONFIGURATION
2) GIVEN PARAMETERS
Head (h): 12 m
Power (Pow): 7.5 kw
Atmospheric Pressure (Po): 101,000 Pa
Minimum Allowable Internal Pressure (Pmin): 42,000 Pa
Fluid Velocity at the Spill Point (vs): 3 m/s
Minimum Hub Internal Radius (Rmin): 0.025 m
Water Density (a): 1000 Kg/m 3
Gravitational Acceleration Constant (g): 9.78 m/s 2
Turbine Height Above the Spill Point (hs): 3.61 m
b) CALCULATED PARAMETERS
Total available pressure (P total ) in the system configuration as illustrated in FIG. 12 is the product of the density (σ) times the acceleration of gravity (g) times the total head (h):
P.sub.total =σgh; 1000×9.78×12=117,360 Pa(5-1)
Dynamic pressure (P s ) (due to the fluid exit velocity) at the spill point is the product of one half the density (σ) times the velocity (V s ) squared:
P.sub.s =σV.sup.2.sub.s /2; 1000×3.sup.2 /2=4500 Pa(5-2)
Maximum theoretical efficiency (η) is the difference of the total available pressure (P total ) and the dynamic pressure at the spill point (P s ) divided by the total available pressure (P total ).
η=(P.sub.total -P.sub.s)/P.sub.total ; (117,360-4,500)/117,360=0.9616(5-3)
Note: Dynamic pressure at the spill point (P s ) times volume flow (Q) represent a power loss. This power loss places a maximum upper limit on the theoretical efficiency (η) that this particular application may attain.
Net available pressure (P N ) is the total pressure (P total ) minus the dynamic pressure (P s ):
P.sub.N =P.sub.total -P.sub.s 117,360-4,500=112,860 Pa (5-4)
Volume flow (Q) required is determined by dividing the power (Pow) by the net available pressure (P N ):
Q=Pow/P.sub.N ; 7,500/112,860=0.06645 m.sup.3 /s (5-5)
The suction pressure (P H ) created by the turbine being above the spill point level is determined by the product of the density (σ) times the acceleration of gravity (g) times the height (hs) of the column of fluid between the turbine and the spill point level.
P.sub.H =σghs; 1000×9.78×3.61=35,306 Pa (5-6)
Available working pressure (Paw) is the atmospheric pressure (Po) minus the minimum allowable internal pressure (P min ).
Paw=Po-P.sub.min ; 101,000-42,000=59,000 Pa (5-7)
Maximum entrance axial dynamic pressure (p v1 ) is the difference of the available working pressure (Paw) and the suction pressure (P) plus the addition of the dynamic pressure (P s ).
P.sub.v1 =Paw-P.sub.H +P.sub.s ; 59,000-35,306+4,500=28,194 Pa(5-8)
Notes: P v1 is the dynamic pressure due to velocity (V 1 ) of the fluid at the entrance to the turbine.
P s is the dynamic pressure due to velocity (V s ) of the fluid at the spill point.
Fluid entrance velocity (V 1 ) is determined by taking the square root of twice the maximum entrance axial dynamic pressure (P v1 ) divided by the density (σ).
V.sub.1 =√(2P.sub.v1 /σ; √(2×28,194/1000)=7.509 m/s
Fluid entrance area (A 1 ) to the turbine is determined by the division of the volume flow (Q) by the entrance velocity (V 1 ).
A.sub.1 =Q/V.sub.1 ; 0.06645/7.509=0.008849 m.sup.2 (5-10)
2) AXIAL FLOW TURBINE DIMENSIONS
Hub entrance area (A H1 ) is determined by the product of π times the square of the minimum hub internal radius (R min ).
A.sub.H1 =πR.sup.2.sub.min ; 3.1416×0.025.sup.2 =0.001963 m.sup.2( 5-11)
Jacket internal entrance radius (R e ) is determined by taking the square root of the sum of the hub entrance area (A H1 and the fluid entrance area (A 1 ) divided by π.
R.sub.E =√((A.sub.H1 +A.sub.1)/π); (5-12)
√((0.001963+0.008849)/3.1416)=0.05866 m
At this point, for this calculation sample, enough data is available to determine a balanced set of axial and angular dynamic pressures generated at the fixed (stator) section, before the fluid enters the rotor (movable section). P N represents all the static pressure that has to be converted to axial (P A ) and angular (P w2 ) dynamic pressures. The power represented by the product of the volume flow (Q) and the difference of the axial dynamic pressures (P v1 ), must equal the power represented by the product of the volume flow (Q) and the angular dynamic pressure (P w ). The balance of axial and angular pressures allows for the interchange of power between the fluid and the rotor, without substantially modifying the static pressure along the length of the rotor section. Cavitation is thus precluded by the maintenance of a constant static pressure along the rotor section.
P.sub.A =σ(V.sub.2.sup.2 -V.sub.1.sup.2)/2 (5-13)
P.sub.w2 =σR.sup.2.sub.cm W.sup.2.sub.2 (5-14)
Since both axial and angular dynamic pressures must be equal, then the axial dynamic pressure (P A ) is therefore equal to half of the net pressure (P N ).
P.sub.A =P.sub.w2 =P.sub.N /2; 112,860/2=56,430 Pa (5-15)
Axial velocity (V 2 ) will be the square root of twice the pressure Pa divided by the density (σ) plus velocity V 1 squared.
V.sub.2 =√(2P.sub.A /σ+V.sub.1.sup.2); √(2×56,430/1000+7.509.sup.2)=13.01 m/s (5-16)
Area left for fluid transit at point 2 is determined by the division of the volume flow by the velocity V 2 .
A.sub.2 =Q/V.sub.2 ; 0.06645/13.01=0.00511 m.sup.2 (5-16)
Dynamic pressure due to V 2 is one half the density (σ) times V 2 squared.
P.sub.v2 =σV.sub.2.sup.2 /2; 1000×13.01.sup.2 /2=84,630 Pa(5-17)
Radius of the hub at point 2 (R 2 ) is determined as the square root of the jacket internal radius squared minus area A 2 divided by π.
R.sub.2 =√(R.sub.E.sup.2 -A.sub.2 /π); (5-18)
Rotational center of mass radius (Rcm) is determined by taking two thirds of the quotient of the difference of the cubes of the jacket (Ro) and hub R 2 radii divided by the difference of their squares. ##EQU1## 3) OPERATING PARAMETERS
Rearranging formula (5-14), the angular velocity at point 2 is obtained as follows:
W=√(2P.sub.w2 /σRcm.sup.2.sub.2); (5-20)
√(2×56,430/1000×0.05105.sup.2)=208.1 Rad/s
Rotational speed would then be:
RPM=30W/π;30×208.1/3.1416=1987 RPM
Mass flow (M) is the product of the density (σ) and the volume flow (Q).
M=σQ; 1000×0.06645=66.45 kg/s (5-21)
Torque (Tao) is determined as the product of the mass flow (M) times the square of the rotational center of mass radius (Rcm 2 ) times the angular velocity (W).
Tao=MRcm.sub.2.sup.2 W; 66.45×0.05105.sup.2 ×208.1=36.04 N-m(5-22)
Torque (Tao) is also determined as the quotient of power (Pow) and the angular velocity (W).
Tao=Pow/W; 7,500/208.1=36.04 N-m (5-23)
Note: Calculating torque (Tao) using two different sets of values (formulas 5-22 and 5-23) serves the purpose of verifying most of the previous calculations that deal with pressures, velocities, volume flow, etc.
4) TURBINE CONSTRUCTION PARAMETERS
The constructional data that determine the shapes of the stator and rotor hubs and blades are obtained from a sinusoidal distribution (FIGS. 1, 2, and 3, 4, 5) of the axial and angular accelerations. This particular distribution of axial acceleration was chosen in order to obtain hubs and blades that do not change the axial and angular velocities of the fluid at the entrance and exit points of the stator and rotor sections. This keeps the generation of turbulence (at the input and output points of each section) at a minimum, since the velocities are unaltered at those points.
The procedure to determine the shape of the hubs and the blades is based on a sinusoidal distribution of the angular dynamic pressure. This angular dynamic pressure has values that vary between zero (at the entrance), a maximum value (P w 2 )(at the interface of stator and rotor) and back to zero (at the exit point).
a) CALCULATIONS FOR THE FIXED (STATOR) SECTION
The formula for the calculation of angular dynamic pressure (Pwx) at any point (X) along the length (L) of the stator is:
Pwx=P.sub.w.sup.2 (1+cos(πx/L))/2; (5-24)
The axial pressure (Pvx) is equal to the angular dynamic pressure plus the dynamic pressure corresponding to V 1 .
Pvx=Pwx+Pv.sub.1 ; (5-25)
Axial velocity (Vx) is determined by taking the square root of twice the axial dynamic pressure (Pvx) divided by the density (σ).
Vx=√(2Pvx/σ); (5-26)
Area left for fluid transit (Ax) is the quotient of volume flow (Q) and the axial velocity (Vx).
Ax=Q/Vx; (5-27)
Hub radius (Rx) is the square root of the square of the jacket radius (Ro) minus the area left for fluid transit (Ax) divided by π.
Rx=√(Ro.sup.2 -Ax/π); (5-28)
Rotational center of mass radius (Rcmx) is two thirds of the quotient of the cube of the jacket radius (Ro) minus the cube of the hub radius (Rx) divided by the square of the jacket radius (Ro) minus the square of the hub radius (Rx). ##EQU2##
Angular velocity (Wx) is determined as the square root of twice the angular dynamic pressure (Pwx) divided by the density (σ) times the square of the rotational center of mass radius (Rcmx).
Wx=√(2Pwx/(σRcmx.sup.2); (5-30)
Tangential velocity (Vtx) is calculated as the product of the rotational center of mass radius (Rcmx) and the angular velocity (Wx).
Vtx=RcmxWx; (5-31)
Angle of inclination of the blades (αx)(taken at the rotational center of mass radius) is the arctangent of the quotient of the axial velocity (Vx) and the tangential velocity (Vtx).
αx=Tan.sup.-1 (Vx/Vtx); (5-32)
b) CALCULATIONS FOR THE ROTOR SECTION
All the calculations for the rotor are the same as the calculations for the stator, except that the distribution of the axial and the angular dynamic pressures goes from higher to lower values. This type of distribution is done by changing the plus sign in formula 5-24 to a minus sign, as follows:
Pwx=Pw.sub.2 (1-cos(πX/L))/2: (5-33)
Note: Although a sinusoidal distribution of the axial and angular accelerations was chosen for the above calculations, other acceleration distribution criteria could be chosen without departing from the essence of this Patent Application.
While specific embodiments of the invention have been shown and described in detail to illustrate the application of the principles of the invention, it will be understood that the invention may be embodied otherwise without departing from such principles.
|
A rotor is provided wherein an rotor core and a jacket cooperate to provide a continuous variation of area left for fluid transit. This continuous variation of area left for fluid transit produces a continuous axial acceleration of fluid and provides a first pressure gradient. The invention also provides simultaneously for blades having a continuously varying angle provided in the area left for fluid transit and causing a second pressure gradient. The varying of the fluid transit area and the angle of the blade are designed to have the first and second pressure gradients to be complementary and maintain the pressure of the fluid substantially constant. Such a continuous varying angle of inclination of the blades provides a continuous angular acceleration of the fluid and corresponding torque. The blades of continuously varying angle of inclination rotate together with the rotor core producing the torque.
| 5
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to systems for degassing liquids to remove unwanted permanent air gasses, as for example boiler feed water or removal of contaminants such as hydrogen sulfide, unwanted carbon dioxide, and radon. It further relates to systems for scrubbing contaminants from other gasses by contacting the contaminated gasses with relatively clean water, and extends this field to one wherein the liquid used for scrubbing is virtually completely cleaned of all dissolved gasses or volatile contaminants so that the scrubbing may be very complete and rapid. It further relates to the separation of dissolved gasses from industrial liquids, as for instance in removing dissolved hydrocarbon gasses from crude oil or removing dissolved gasses such as helium for storage and later use. It also relates to the instant evaporation of dissolved volatiles such as solvents contained in a liquid and removing them in the equipment to be described or suggested.
2. Description of the Prior Art
The three main types of systems which the present invention intends to improve on are (a) Deaerating devices such as open-air heated tanks for partial removal of dissolved permanent air gasses and other contaminants which may become gaseous in a boiler and reduce a boiler or other piece of industrial equipment's efficiency. (by Systems for holding a contaminated liquid under a partial vacuum, with or without heating, to volatilize and remove the contaminants by diffusion. (c) Systems generally known in the chemical industry as scrubbers, wherein a liquid contaminated with undesired permanent gasses or volatile liquids are sprayed to form drops or spread on high-surface area configurations, allowing diffusion of the undesired dissolved materials to the relatively uncontaminated gas with which it is placed in contact, usually but not necessarily air.
Under the process of the prior art, the liquid to be decontaminated is spread over a very large, thin layer that expedites degassing according to Fick's law of diffusion. A disadvantage of this prior art process is that it facilitates the evaporation of large and largely uncontrolled quantities of the liquid being cleaned. Since the vapor produced by evaporation carries with it the contaminant, a secondary stream of condensate is produced when the vapor is condensed out to facilitate the production of a vacuum. This condensate stream is more highly contaminated than the original liquid being cleaned. Thus this new liquid stream creates a second source of liquid with a concentrated contamination that must be treated. For instance, if the original contaminated liquid, say water, is initially contaminated with a noxious hydrocarbon such as benzene in the amount of 10 -8 molecules of benzine per molecule of water, and further that the quantity of evaporation of water is 0.01 that of the contaminated feed stream, then a contaminated stream of condensate results, containing concentrated benzene in the amount of 10 -6 molecules of benzene per molecule of condensate water. The net effect is that present systems using extended thin films on high-area surfaces provide a system that is very expensive to build., and which requires excessive refrigeration to condense the excess liquid evaporated. Further, as above this secondary stream produces a new source of highly contaminated liquid with a new and exaggerated disposal problem.
SUMMARY OF THE INVENTION
The present invention is a process for rapidly removing dissolved permanent gases and volatile contaminants from a liquid. This is accomplished by forcing the contaminated liquid stream through a cavitating venturi designed to not only free the dissolved air or other gasses and evaporate volatile contaminants, but then to coalescea sizeable fraction of the gas released, typically found in very small bubbles, to larger bubbles. The micro-bubbles are difficult to separate or break because their buoyancy is small compared with their resistance to rising under gravity. The larger bubbles coalesced are easily separated by low centrifugal forces and are relatively easily broke. By designing the equipment so that the liquid is not exposed in thin films, or for extended times and large areas to the low-pressure mixture of vapor and gas, the gas being released when the bubbles break, excessive evaporation is avoided. In the best case almost the only vapor that will be released is that necessary to saturate the gas bubbles. This is minimal because of the very high specific volume of wet steam at its very low partial pressures found in the system. Additional components of the system to accomplish the desired processes of separating the large bubbles, breaking them and removing their gaseous contents without additional significant evaporation are described in the patent specification. Their function is to not only separate the large, coalesced bubbles from the main stream carrying the micro-bubbles not coalesced, but to break them, at the same time isolating the main stream, which then can be further processed in second third stages or more stages while limiting contact of the liquid streams from the low pressure air-vapor released thereby limiting further evaporation. For example, the liquid may flow through one or more turns of tubing following its initial processing through title cavitating venturi. After centrifugal separation, the stream containing the large, soft bubbles is stripped from the main stream 12 in FIG. 1 and sent to one of several types of secondary bubble breakers and separators.
Because evaporation of the contaminated liquid can occur only at a free vapor-liquid surface or interface, it is the method and intention of this invention to limit insofar as practicable evaporation except to the gas bubbles. This process can best be understood by examining in some detail the total process and equipment design as they relate to Fick's law of diffusion: ##EQU1## where dn is the number of molecules moving, across an interface of thickness δ, of area A, in a time dt, driven by a concentration gradient, C 1 -C 2 at a rate determined by an experimental diffusion constant, D. One caveat. Eq.(1) is generally understood without qualification to be at constant pressure, and the concentration gradient the number of molecules, say of gas, per unit of liquid. Not so in this case where the concentration gradient is replaced by a solubility factor. With the large reduction in pressure--it may be by a factor to as high as 1/100th or greater in the throat of the cavitating venturi--the solubility is very low and the dissolved constituents--gas or volatile molecules--move from wherever they occur in the contaminated liquid against the concentration gradient until a new solubility saturation in the liquid at the lower pressure is achieved. For instance, in the practical case we approach in our design, a reduction in pressure to, say 1/30th of an atmosphere, or about 0.03 bar, the dissolved gas and volatilized contaminants will exit the liquid until a solubility saturation value at the lower pressure is reached, irrespective of the actual concentration. No matter; so far as is known, Equal.(1) holds in this case, where the moving force is as now re-defined in terms of solubility and solubility change with a change in pressure.
To reexamine the state of the art contactor, a large pressure vessel with extended surfaces supporting thin films of liquid, would be dictated by Eq.(1). The through-put of contaminated liquid is maximized by paying attention to the demands of diffusion as shown here. Just so in my new system, except that the diffusion is limited, insofar as practicable, to the bubbles (mostly air but containing the contaminant as a vapor). The large area, A, is achieved in the very large surface area of the bubbles of air, large and small. The diffusion distance, δ, is minimized by the close spacing (due to their very large numbers) of the micro-bubbles formed in the venturi's throat: So far as is known, neither the diffusion constant, D nor the concentration gradient (or in its place the solubility deficit, as I now choose to call it) is changed by the new hardware I propose. In any case, diffusion to incipient micro-nuclei inherent in most liquids is extremely rapid; the entire removal down to the new solubility level is accomplished in a distance of tens of mms and a time of a few thousandths of a second. The further coalescence of these very small (hard) micro-air bubbles to large, soft air bubbles occurs in a further short time of perhaps a few or tens of thousands of a second, depending on equipment size, i.e. the length of the straight coalescing section 6 in FIG. 1.
To recap to this point. Micro air bubbles carrying the dissolved volatile or gaseous contaminant are formed in the intake section of the CV, then coalesced in the very large steam bubbles formed in the straight throat. These large steam bubbles, now containing air from the coalesced micro air bubbles are then condensed abruptly in the cavitating diffuser of the CV 8 in FIG. 1, which causes a rapid pressure rise to above the saturation pressure of the liquid being cleaned. The portion of the flow carrying the large air bubbles is then separated in a centrifugal separator for example, 10 in FIG. 1 from the part of the flow carrying the micro-bubbles not coalesced 16 in FIG. 1. The stream carrying the large bubbles is sent to a breaking device such as 24 in FIG. 2, and the bubbles'0 contents sent to the vacuum system. The equipment is designed to avoid insofar as practicable further contact of the degassed liquid with the low pressure air stream flowing to the vacuum system and further to keep that liquid in thick sections, effectively maximizing δ while minimizing A to prohibit insofar as is practicable evaporation of the liquid being cleaned. In the best possible design, almost no steam would be released except for the very small amount needed to saturate the air bubbles. The volume of the air bubbles then controls the total vapor released, and this is the heart of this patent application.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1, shows a schematic of a longitudinal cross section of the Cavitating Venturi (CV) with three sections identified, the entrance nozzle 2, the straight section 6 and the diffuser 8, which empties into a centrifugal separator 10 in which the large air-vapor bubbles formed in the straight section are removed from the remainder of the liquid charge 16. The fraction of the liquid containing the large, easily broken bubbles 20 are then sent via duct 12 to a simple device for breaking the bubbles, releasing their contents which then go to the vacuum system not shown. The portion of the flow carrying very small micro-bubbles not coalesced in the first CV are then passed to a second CV, or more if necessary, allowing continuous staging to reduce the gas content of the liquid to virtually any desired level.
FIG. 2 shows a simple device 24 for breaking the large bubbles separated in the centrifugal separator shown in FIG. 1, useful in systems of limited through-put. This device also is usable as a simple centrifugal separator obviating, in some cases the need for the centrifugal separator 10 of FIG. 1.
FIG. 3, shows a more complex device 38 capable of handling very large through-puts in large capacity systems. Like that in FIG. 2, it is capable of separating the large and very small bubbles following the CV, but it is believed that a best design would use a number of stages, each as shown in FIG. 1
FIG. 4, shows an alternative separator and large bubble breaker 11 in section, with an impeller projecting through the inner layer of liquid carrying the large bubbles separated from the remainder carrying the micro-bubbles as shown in section in FIG. 1.
FIG. 5, shows a cross-section through a cavitating venturi, and above it possible pressure along its length.
FIGS. 6A, 6B, and 6C show three combinations of the novel components shown in earlier FIGS. 1 through 4, with each combination achieving the desired processes of the invention.
DETAILED DESCRIPTION OF THE INVENTION
The functions of the various parts of the invention is as follows. First, referring to FIG. 1, the contaminated or gas-saturated liquid is introduced at a preferred velocity and pressure through the duct 2, which empties into the nozzle portion of the cavitating venturi (CV),which is made up of 4, 6 and 8. The straight section 6 is maintained It a suitable absolute pressure just below the saturation pressure of the liquid, as determined by the liquid's temperature. The stream is diffused to a final desired pressure in the conical section, the diffuser 8, designed according to Bernoulli's principle. The entry section of a CV can release dissolved gasses from solution into very small bubbles (estimated to be of 1μin diameter). One inventive aspect of the invention derives from the phenomena of small bubbles coalescing in a low-pressure throat of a CV.
Upon exit from 8, the stream now consists of a mixture of liquid, very small (uncoalesced) air-gas vapor bubbles and large bubbles coalesced in the straight section 6. The stream exiting 8 is rotated rapidly in a suitable circular duct 10, in which the large bubbles are moved by centrifugal force to the inner portion of 10 and 16, and from which the liquid stream containing the large bubbles is stripped from the flow into duct 12 in a suitable elbow 14. The remainder of the liquid flow, containing micro-bubbles of air, gas and vapor are passed to the next stage or stages, each of which consists of a CV and separation system as shown in this, FIG. 1.
FIG. 2 shows in section (all parts are circular in cross-section except for the scoop 46 in FIG. 3) a simple device for reversing the flow from a number of stages, through each stage's duct 12, combined into 20. The flow from 20 goes to bubble breaking devices such as are shown in FIGS. 2 and 3. In FIG. 2 1 show a stationary device with no moving parts that receives the stream 20 consisting of liquid carrying large bubbles or a mixture of large and small bubbles if the separator 10 is not used, which impinges on a surface of rotation 26. This breaks the bubbles by splashing and further by sending the reversed stream, now traveling downward, through a suitable metal screen 28. The liquid now separated from the gasses flow from the separator 24 through a duct 30 for final disposal, use, or further processing. The separated gasses, (vapor and contaminating gasses) are sent to the vacuum system for discharge and final disposal Note that if separator such as 10 is not used, the flow from 30 would go to a subsequent or stage or stages, each starting with a suitably sized CV to handle the flow, which now has part of its dissolved gasses and volatiles removed. Any number of stages may be utilized to achieve the desired level of decontamination or degassification.
An alternative separator suitable for very large systems (large contaminated liquid flows) is shown in FIG. 3. Here, the large bubble carried in a liquid stream as from 12 FIG. 1, is introduced through a rotating annular duct 36 discharging into a rotating cylinder 38, lined with a suitably shaped co-rotating parabolic cone 40. The bubbles 42 are rapidly separated to the outer surface of the cone 40 to its top, where the bubbles are broken as the stream is flung outward into a co-rotating annulus 44. From 44, the liquid now largely gas-free, is scooped up by a stationary scoop 46 by impact and the cleansed liquid is discharged from the system through a stationary duct 48. A note on the design on the approximately parabolic cone of rotation 40: The water would, without this solid cone assume a parabolic surface shown as a dashed line just inside 40 which would have the unfortunate trait of providing a large free surface for evaporation of the liquid exposed to the low pressure of the vacuum system. To avoid this undesired and uncontrolled evaporation, the cone is made slightly larger in diameter at every point than it would be if it coincided with the free surface of rotation. Thus the separated air-liquid (a foam) rising to the cone's top is sized to be fully wetted by the bubble-liquid mixture, so avoiding the undesired evaporation, a major function of this invention. Only in a very narrow annulus 44 at the top of the system is the liquid exposed to the vacuum system, and then in heavy layers and only very briefly. In terms of the lesson taught by Eq. (1), those factors promoting evaporation according to Fick's law are minimized, except as they relate to the formation of gas-vapor bubbles in the CV, where they are maximized. To a first approximation, the only liquid evaporated (none is desired for reasons stated earlier) is that necessary to saturate the air bubbles. The volume of vapor released to the air bubbles is the same as the volume of the volume of air in the bubbles, according to Dalton's law of partial pressures. When and if we learn to rapidly break very small micro-bubbles, that vapor will further be reduced as the permanent air gasses in the micro-bubbles is compressed, and so too the air's volume. According to Dalton's law of partial pressures, the volume of the vapor would be that of the air which since it must be compressed in the vacuum system, is minimized, thus reducing equipment size and power to drive the vacuum pumps.
Another device 11 for separating and breaking the large bubbles is shown in FIG. 4, which shows an impeller 50 with half-vanes projecting through the inner, liquid layer containing large air-steam bubbles. The outer half-annulus of water contains those micro-bubbles not coalesced in the CV as in FIG. 1, as 54. The impeller is driven through a shaft 56, which is supported and sealed with a combination bearing and seal, 58. Experience has shown that the large air-steam bubbles are stable when rotating rapidly and under centrifugal force. The half-surface impeller acts as a centrifugal pump, expelling the liquid in the septa forming the bubbles to the outer layer, leaving the gasses behind. These separated gasses proceed to the vacuum system through duct 60, which performs as does 20 in FIG. 1. For large systems, this design has powerful advantages justifying the additional complexity, in that one device, similar in some respects to a centrifugal pump, can handle the output of any number of stages, as each consisting of the apparatus shown in FIG. 1.
One very important benefit of the system disclosed here is that the permanent gasses and volatile contaminants can be separated from the main liquid stream at a pressure much lower than necessary to volatilize the contaminating volatiles. The pressure is then raised in the diffuser of the cavitating venturi to a pressure just below that required to keep them in the gas mixture in the bubbles. Since most volatile liquids do not have an exact evaporation point--gasoline, for instance, is a mixture of many compounds--the result is that we can achieve maximum separation of the volatiles at a very low pressure while then raising them to as high a pressure as practicable. This has the very important advantage that the pressure increase in the vacuum pump, and so the power to drive it, will be minimized. The size of the compressor, an important cost factor, also can be minimized. This is illustrated for discussion in FIG. 5, to approximate scale, where the pressure along the length of a cavitating venturi is shown. In section A, the converging nozzle section a large portion of the dissolved gasses to be released are moved to very small bubbles. In the center, or coalescing section, C, massive steam bubbles are formed by dropping the pressure to any chosen value below the saturation temperature of the liquid. Much of the gasses in the micro bubbles formed in section A are incorporated into the massive steam bubbles (which can attempt, unsuccessfully of course, to achieve diameters of infinity if the pressure is just below the saturation pressure of the liquid) In the diffuser section, C, the pressure is raised to any desired value according to Bernoulli's theorem, avoiding excessive condensation (if that is the correct term) that would re-incorporate the volatilize gasses into the liquid. By controlling the pressure at the exit of the diffuser by suitably dimensioning the diffuser and discharging it at the desired pressure in the vacuum system, we can compress, for instance at a low pressure, D, or over-expand to a too-high pressure E or in a correct design, to a preferred pressure F, just high enough to avoid recondensation or perhaps re-solution in the liquid. Note also that the coalescing section of the cavitating venturi, B, need not be straight nor the pressure constant, but can be adjusted to reach almost absolute zero pressure, then increased to just below the saturation pressure to achieve maximum steam bubble size and so coalescence of the micro-gas bubbles. The steam re-condenses very early in the diffuser, section C, when the pressure rises above the liquid's saturation pressure.
FIGS. 6A, 6B, and 6C show 3 combinations of novel components revealed in the earlier FIGS. 1 through 4. Each combination achieves the important functions of releasing micro bubbles of gas from solution, coalescing part of them, then breaking the large bubbles formed by coalescence and sending their contents to a vacuum system in such a way as to avoid excessive evaporation of the liquid being cleansed or stripped of its permanent gasses.
The strength of the system can be understood by considering a possible need for separating helium, a permanent gas, and one or more of the more volatile fractions, say benzene, naphtha, etc, from a stream of crude oil. In the first stage, the final pressure at the discharge of the cavitating venturi's diffuser might be so high that any light fractions would be re-condensed and returned to the main stream, while the helium and other permanent gasses(for instance, air) are separated. The next stage could be designed to separate a more volatile fraction, the third stage a less volatile component, etc.
|
A system is described for rapidly removing dissolved permanent gasses or dissolved volatile contaminants from a liquid, in which the liquid is forced through a cavitating venturi, designed and operated in a fashion to produce micro-bubbles in the high-shear, converging flow section at its entry, to coalesce a significant fraction of these micro-air bubbles in a nominally straight section of maximum restriction following the inlet section, then in a final section, a diffuser, the steam bubbles condense, having during their lives caused coalescence of a significant fraction of the micro air bubbles, which are then, with the water carrying them separated from the remaining stream and its micro-bubbles. The stream separated carries large, easily broken air bubbles which then are broken in a suitable device (four are shown, each with a proposed best design for a specific size of system). The bubbles' contents, a mixture of air, volatiles and vapor are then sent to a vacuum system for processing to the atmosphere.
| 1
|
CROSS REFERENCE TO RELATED APPLICATIONS
This application is related to:
U.S. application Ser. No. 08/195,231 which is a continuation of abandoned U.S. application Ser. No 722,713 filed on Jun. 27, 1991 in the name of Chase and Taylor and entitled "Electronically interpolated integral photographic system";
U.S. application Ser. No. 885,217 filed on May 19, 1992 in the name of Syracuse, Kent and Taylor and entitled "Method and Apparatus for improving electronic recording of depth images";
U.S. application Ser. No. 974,441 filed on Nov. 12, 1992 in the name of Taylor and entitled "CRT printer for lenticular photographs"; and
all incorporated by reference herein.
FIELD OF THE INVENTION
The invention relates to the field of stereoscopic photographs and more particularly to a stereoscopic picture having an improved arrangement of the left and right perspective views for convenient and unambiguous viewing of stereo pairs printed on a photographic receiver (film or paper) and aligned with a lenticular faceplate for display. The invention relates also to a method for producing such a stereoscopic photograph.
BACKGROUND OF THE INVENTION
Three-dimensional photography is comprehensively described in Three-Dimensional Imaging Techniques by Takanori Okoshi (New York: Academic Press, 1976, translated from the Japanese edition published in 1972) which provides a basis for describing the attributes and advantages of this invention. Okoshi initially distinguishes between truly three dimensional imaging and stereoscopic imaging on the basis of the amount of information involved. The quantity of information for a stereoscopic (or binocular) image is only twice that of a planar (one-dimensional) image, is much greater information is present for a truly three-dimensional image (which is often called an autostereoscopic image). Images of the latter type are truly spatial images that gradually show more of the right side of the object when the observer moves rightward, and more of the left side of the object when the observer moves leftward (which is often referred to as a "look around" capability). Integral photography is a method of recording a complete spatial image, that is, one viewable from a multiplicity of directions, upon a single flat photographic plate. The principles of integral photography were described by G. Lippman in 1908 in a paper read to the French Academy of Science. Integral photography thus has a long history of theoretical consideration and demonstration, but has enjoyed only limited commercial success.
Integral photography refers to the composition of the overall image as an integration of a large number of small photographic image components. Each photographic image component is viewed through a separate small lens usually formed as part of a mosiac of identical spherically-curved surfaces embossed or otherwise formed onto the front surface of a plastic sheet of appropriate thickness. The plastic sheet is subsequently bonded to or held in close contact with the emulsion layer containing the photographic image components. Lenticular photography is a special case of integral photography wherein the small lenses are formed as sections of cylinders running the full extent of the print area in the vertical direction. Recent commercial attempts at lenticular photography have included a multi-lensed 35 mm three-dimensional camera sold by Nimslo Corp., Atlanta, Ga., and a similar camera manufactured by Nishika Optical Systems, a division of Nishika Corp., Henderson, Nev. Though a sense of depth is clearly visible in prints made from these cameras, the resulting images have limited depth realism and appear to the viewer to "jump" as the print is rocked or the viewer's vantage relative to the print is changed.
The product of integral photography, that is, an integral photograph, can be further thought of as an X-Y array of microscopic slide projectors cascaded over the area of the print material. Each tiny lens, or lenslet, projects a microscopic view of the scene from a slightly different perspective than the one next to it. If the viewer's eye was concentrated on a singular lenslet surface, it would see only that portion of the view behind that lenslet which is angularly aligned with the line of sight to that lenslet. If the eye is moved laterally and continues to look at the same lenslet, it will see progressively different laterally angular portions of the view behind that lenslet. However, because the lenslets are made very small relative to the normal viewing distance, their apparent angular diameters may approach or subserve the angular resolution of the eye, with the result that features of the lenslets themselves are not apparent to the viewer, while the light emanating from them is.
The viewer then is able to mentally construct the entire array of optical beams from all lenslets into a recognizable scene without distraction from lenslet features. Since the right eye sees the array from a different vantage than the left eye, autostereoscopic depth perception is also present. By shifting the head laterally relative to the print surface, a changing autostereoscopic view is seen resulting in a "look around" capability which adds to the realism of the display. Integral photography also allows a "look around" capability in the vertical direction as well as the horizontal direction and an autostereoscopic view would also result if the print were rotated ninety degrees such that horizontal lines recorded from the original scene are now extending from bottom of the print to the top.
Since it is likely that most viewers prefer to view their photographs as models or reminders of the real world, it is not likely that they will choose to rotate the print for viewing. It was recognized as early as Lippman that instead of spherical lenslets, long cylindrical lenses extending from the top of the print to the bottom could be used to provide autostereoscopic views (and resultant "look around") in the horizontal direction only. This is sufficient to give a realistic three-dimensional model of the real world. Moreover, since vertical film space is not used to record alternative vertical views, the vertical detail recorded improves and approaches the film resolution limit, giving an improved impression of print quality. The long cylindrical lenses are called lenticules, and the principles of integral photography apply equally well to lenticular photography as long as one views the layouts or optical schematics in planes perpendicular to the cylindrical axis of the lenticules.
Since there are no restrains preventing any given lenticule from projecting information recorded behind adjacent lenticules and being seen by a viewer as the print is rotated about a vertical axis or when his head is moved laterally, the recorded sequence of perspective views will be repeated in viewer space. The maximum space for information to be printed behind a lenticule without extending into the recording space of an adjacent lenticule is the reciprocal of the lenticule pitch. The angle through which this information from a given lenticule is seen is called the primary angle. The images seen to each side of the primary angle are called satellite images. The pseudoscopic viewing occurs when one eye is within the primary image region (angle) and the other eye is in the satellite region (beyond the primary angle).
An optical method of making lenticular photographs is described by Okoshi in Chapter 4 of the aforementioned book.
It was determined through magazines such as Stereo World published by the National Stereoscopic association and from museums such as the Eastman House in Rochester N.Y., that sizable collections of stereoscopic photos of historical and societal interest exist unbeknownst to the general public. As such, these photos consist of only one stereo pair and are therefore not capable of reproducing the "look around" effect (which require many laterally separated views of a scene). The earliest patent describing this general technique of stereo pair recording is U.S. Pat. No. 1,128,979 issued to Hess on Feb. 16, 1915 and which describes the simplest optical system wherein the left L and right R views of a stereo pair are placed in plate holders held at angles symmetrical to a normal surface of a sheet of cylindrical lenses 100 (See FIG. 1). The cylindrical lens elements serve to focus sections of the images onto a photographic film 101. After development, the film was presumably carefully aligned and reaffixed to the cylindrical lens sheet for viewing. The image reversal induced by the lenticules in projecting the information is compensated by printing the Right view R to the left of the Left view L.
A principal problem with this type of image display is that the viewer is free to move laterally to a position beyond the primary angle where pseudoscopic viewing occurs thereby inverting the normal depth relationships as described earlier. This is illustrated in FIG. 2 where the left eye sees the Right image (R') aligned under the adjacent lenticule 102 and the right eye sees the Left image (L) under the reference lenticule 103.
By 1978, when the Nimslo camera was developed and marketed, four views of a scene were projected, comprising two left views and two right views. The inverse perspective pseudoscopic problem had still not been solved. This is illustrated in FIG. 3. As illustrated, four views are present under each lenticule: two Right views R 1 -R 2 (reference lenticule 105), R' 1 -R' 2 (adjacent lenticule 106) and two Left views L 1 -L 2 (reference lenticule 105), L' 1 -L' 2 (adjacent lenticule 106). An observer's eyes can move laterally relative to any given reference lenticule 105, for example as an arc 110 if the print is simply tilted in the viewer's hand. There are two positions A and B close to a normal to the print where correct perspective correlation viewing is possible. At position A, the right eye sees Right image R 1 while the left eye sees Left image L 2 . At position B, the right eye sees Right image R 2 while the left eye sees Left image L 1 . However, if the head moves further so that position C or D is reached, pseudoscopic viewing is experienced. In position C, the right eye sees Left image L 1 while the left eye sees Right image R' 2 . In position D, the right eye sees Left image L 2 while the left eye sees Right image R' 1 .
U.S. Pat. No. 4,800,407 describes an optical method of making three view parallax panoramograms. The three lens camera for 3D images described in this patent is still subject to the pseudoscopic image problem.
U.S. Pat. No. 4,852,972 introduces the concept of varying the exposure of views exposed by an optical method for the purpose of compensating for the transmission losses as the angle view increases.
U.S. Pat. No. 4,807,965 recognizes the pseudoscopic image problem and corrects it by preventing the observer from seeing pseudoscopic images by utilizing a mechanical system of Louvres, a constraint that would be expensive to implement and would act as an annoyance to consumers.
U.S. Pat. No. 4,959,641 also recognizes the pseudoscopic image problem and corrects it by independently controllable and discrete light sources provided in fixed relation to a lenticular screen. The problem of such a solution lies mainly in the complexity of the system.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide an improved stereoscopic picture as well as a new method for producing such an improved stereoscopic picture that eliminate the problems mentioned in the above discussion with respect to conventional techniques.
This object is achieved by providing an improved stereoscopic picture, comprising:
(a) a lenticular faceplate material having a predetermined number of lenticules, the lenticules having a given pitch and a given subtended primary angle; and
(b) a photographic receiver mounted on the lenticular faceplate material and on which are recorded sets of right and left perspective views of a first pair of stereoscopic pictures, the sets of right and left perspective views being of a given width, the lenticular faceplate material and the photographic receiver being aligned so that each set on the photographic receiver corresponds to an associated given lenticule of the lenticular faceplate material, the width of the sets being less than the pitch of the lenticules.
It is also another object of the invention to provide a method for producing an improved stereoscopic picture, comprising the steps of mounting on a lenticular faceplate material having a predetermined number of lenticules of a given pitch and of a given subtended primary angle, a photographic receiver on which are recorded sets of right and left perspective views of a first pair of stereoscopic pictures, the sets of right and left perspective views being of a given width, the lenticular faceplate material and the photographic receiver being aligned so that each set on the photographic receiver corresponds to an associated lenticule of the lenticular faceplate material, the width of the sets being less than the pitch of the lenticules.
These and other objects of the present invention will become more apparent when taken in conjunction with the following description and drawings wherein like characters indicate like parts and which drawings form a part of the present description.
The following are advantages of the invention: it provides a very simple and inexpensive solution to the pseudoscopic image problem.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 represents a PRIOR ART stereoscopic picture obtained according to the teaching of U.S. Pat. No. 1,128,979;
FIG. 2 illustrates the pseudoscopic image problem which occurs with the PRIOR ART stereoscopic picture of FIG. 1;
FIG. 3 and 3a represent another stereoscopic picture of the PRIOR ART;
FIG. 4 and 4a represent a first embodiment of the stereoscopic picture according to the invention;
FIG. 5 is a another representation of the stereoscopic picture of FIG. 4;
FIG. 6 and 6a show a second embodiment of the stereoscopic picture according to the invention; and
FIG. 7 and 7a illustrate a third embodiment of the stereoscopic picture of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 4 to which it is now made reference illustrates a first embodiment of the stereoscopic picture according to the invention. Typically such a stereoscopic picture comprises a lenticular faceplate material 100 mounted in alignment with an image receiver 101 on which are recorded a plurality of sets 107 of right and left perspective views of a pair of stereoscopic pictures. Typically, the assemblage is made of a sheet of photographic material oriented with its emulsion side in intimate contact with the flat back side of a clear plastic sheet of appropriate thickness having lenticules embossed or otherwise formed into its front side. Alternatively, the assemblage may be comprised of a lenticular material with an emulsion coating on its rear surface.
According to an important feature of the invention, the image area recorded behind each lenticule, i.e. the set of right and left perspective views does not occupy the whole width of the corresponding lenticule. As an example, when printing a depth image containing 20 views (1-20) in conjunction with a lenticular sheet designed with a primary angle of 20 degrees, it was found that a simple stereo pair could be used to fill only the central five to seven recording sites (7-14) behind each lenticule while leaving the rest of film (1-6 and 15-20) unexposed so that, according to this embodiment, two successive sets of right and left perspective views of a stereo pair occupy 13 to 16 degrees and are separated by four to seven degrees of black. An alternative would be to expose the areas between recording sites with information different from the stereo pairs. For example, graphics, colors other than black, etc. Obviously, the invention is not limited to these particular numbers of exposed and unexposed views. In this particular example, observed at a viewing distance of 3 feet, the width of the black band was just at or beyond the 2.5 inches of human eye separation. Therefore, positioning the head so that pseudoscopic viewing is enabled, is extremely unlikely. This is illustrated in FIGS. 4 and 5. In FIG. 4, the viewer's head is close to a normal to the lenticular screen 100 and the left eye sees the Left image projected from sites 11, 12, 13, or 14 while the right eye sees the Right image projected from sites 7,8,9 or 10. Therefore, since the images seen by the eyes correlate with the Left and Right perspectives that originally provided the images (such as a stereo camera), correct perspective correlation viewing is enabled.
As shown in FIG. 5, if the viewer's head is moved laterally to the right (or conversely to the left), the right eye sees no image to conflict with the image still seen by the left eye image. In fact, it sees a black image 108. Since the overall impression when one eye moves into the black region, is one of diminished image brightness (as summed by the mind over both eyes), the viewer quickly associates adjusting his head laterally to a position where maximum brightness is seen, which is also the viewing zone where stereoscopic vision is enabled.
Alternatively, two successive sets of right and left views of a first stereo pair are separated by a set of right and left views of a second stereo pair, instead of a black area. As an example, the second stereo pair consists of graphics. Advantageously, such graphics include words or symbols for describing the first pair of stereoscopic pictures. Alternatively, such graphics are words or symbols used to help the viewer correctly locate the viewing zone where a correct perspective correlation is enabled. Such a feature is illustrated in FIG. 6 wherein a first stereo pair is recorded in sites 2 to 9 and a second stereo pair is recorded in sites 12 to 19. The two stereo pairs are separated by an unexposed area (dark band) corresponding to sites 10 and 11.
In order for such a technique to work optimally, the lenticular material should be preferably provided with a total subtended primary angle that is substantially greater than the angular separation of a viewer's eyes at the intended viewing distance. Preferably, such a primary angle is at least four times the angular separation of a viewer's eyes at the intended viewing distance. For example, the subtended primary angle of the lenticular material is of at least 20 degrees. Preferably, the writing technique has a resolution sufficient to permit the recording of a stereo pair within a 5 degrees portion of that primary angle.
As another feature of the present invention, the subsets of right and left perspective, views of a set of views are formed of varying brightness level views, the brightness level increasing as the viewer moves towards the viewing zone of the stereoscopic picture where a correct perspective correlation is enabled. In fact, it was determined that if the outer or lateral views of a set (See views 7 and 14; FIG. 7) are printed with reduced exposure, the resulting darker images become an additional intuitive clue to the viewer to move his head laterally in a direction making the views brighter and more visible, and concurrently, that viewing zone is slightly widened where the stereoscopic vision is enabled. As shown in FIG. 7, according to another advantageous feature of the invention, central views 10 and 11 (one right view and one left view) are printed with increased exposure, causing these views to look brighter than the normally exposed views 8-9 and 12-13 and than the under-exposed views 7 and 14. The viewer then quickly learns to find the place where the left and right views have balanced exposure with high contrast, which is exactly the right position to enable correct perspective correlation.
Reference is made again to FIG. 6 which represents an embodiment of the invention that combines all the above mentioned advantageous features of the invention. In this embodiment, the stereoscopic picture is comprised of two separate stereo pairs (sites 2-9 and sites 12-19).The two stereo pairs are separated by a dark band (sites 10 and 11). Each stereo pair is comprised of views of varying exposure levels (first stereo pair: sites 2 and 9 under-exposed, sites 3-4 and 7-8 normally exposed, and sites 5-6 over-exposed; second stereo pair: sites 12 and 19 under-exposed, sites 13-14 and 17-18 normally exposed, and sites 15-16 over-exposed).
Various known techniques can be used for recording the stereo pairs on the photographic receiver. According to a preferred embodiment, a LVT (Light Valve Technology) writer is used. The LVT printer can be used to print directly on a film to be attached to a lenticular faceplate material after development, or directly on an emulsion layer coated on the rear surface of a lenticular faceplate material. To this end, the methods and apparatus described in the above mentioned U.S. applications, Ser. Nos. 08/195,231 and 885,217 can be used. Advantageously, the teaching of the above mentioned U.S. application, U.S. Pat. No. 5,278,608 can also be used to improve the viewing angle at the desired viewing distance. In particular, a system can be used which determines the number of scan lines for each image of a view based on the resolution of the recording media, the number of or pitch of the lenticules and the number of views desired or necessary to minimize the angular transitions between view. The viewing range is also increased by aligning the image lines with respect to the lenticules such that the image lines can be positioned under adjacent lenticules as the distance from a central viewing position increases.
As an alternative printer, the stereo pairs can be recorded by using a CRT printer. Such a CRT printer, usable for the present invention, has been described in great detail in the above mentioned application, Ser. No. 974,441.
Having described the invention in detail and by reference to the preferred embodiment thereof, it will be apparent that other modifications and variations are possible without departing from the scope of the invention defined in the appended claims.
PARTS LIST
100 Lenticular faceplate material
101 Photographic receiver
102 Adjacent lenticule
103 Reference lenticule
105 Reference lenticule
106 Adjacent lenticule
107 Set of right and left perspective views
108 Black image
110 Arc
|
An improved stereoscopic picture, comprising:
(a) a lenticular faceplate material having a predetermined number of lenticules, the lenticules having a given pitch and a given subtended primary angle; and
(b) a photographic receiver mounted on the lenticular faceplate material and on which are recorded sets of right and left perspective views of a first pair of stereoscopic pictures, the lenticular faceplate material and the photographic receiver being aligned so that each set on the photographic receiver corresponds to an associated given lenticule of the lenticular faceplate material, the width of the sets of right and left perspective views being less than the pitch of the lenticules.
| 6
|
RELATED APPLICATIONS
This application is a continuation-in-part of co-pending, commonly assigned U.S. patent application TIME OF CENTURY COUNTER SYNCHRONIZATION USING A SCI INTERCONNECT, Ser. No. 08/720,332, filed Sep. 27, 1996.
TECHNICAL FIELD OF THE INVENTION
This invention relates generally to counter synchronization in multi-processor systems, and more specifically to compensation for "skew" in the synchronization of such counters on a scalable basis according to the size and/or complexity of such systems.
BACKGROUND OF THE INVENTION
In multi-processor systems having multiple nodes, each node typically has a clock counter and each processor on that node reads that clock counter. Unfortunately, each clock driving these counters, and hence each node, runs at a slightly different clock rate. This difference arises as a result of slight differences in clock frequencies, the crystals in each clock being not exactly identical. The different crystal frequencies cause the clocks, and therefore the counters, to drift apart in their measurement of time. The physical differences in the crystals cannot be controlled.
Periodic resynchronization is therefore required. A master clock is typically identified within the system, which in turn sends out a synchronization pulse (hereinafter "sync pulse") to the other clocks to resynchronize with the master.
This resynchronization mechanism is affected directly by the size of the system involved. It takes more time for the sync pulse to reach topologically distant counters than it does to reach topologically nearer counters. This latency would not be so significant if the destination counters were substantially topologically equidistant from the master. Typically, however, a measurable "skew" arises when the sync pulse is distributed to remote clocks, the skew representing the time difference between the maximum latency (for a topologically distant counter) and the minimum latency (for a topologically near counter). This skew increases as the system enlarges physically. This skew further increases as the amount of traffic in the system increases. It just takes longer for a sync pulse to reach topologically remote counters over busy processing connections such as buses or interfaces.
Software running on the system, no matter what size of system, would like all counters in the system to be perfectly synchronous all the time. Software can nonetheless tolerate small variations in counter accuracy, up to a predefined limit. Absent skew, these small variations (usually attributable to marginally different crystal oscillation rates) are correctable through periodic sync pulse distributions from the master clock. However, when the skew in a system exceeds the predefined skew limit for the system, sync pulse distribution cannot correct clock discrepancies by itself. The software further cannot tolerate the discrepancies and errors can occur.
Systems of the prior art, which are often fixed in size and topology, typically account for skew by selecting and implementing a fixed system counter accuracy just once at system design time, where the selected accuracy can be predicted with confidence always to exceed the expected skew. A problem has arisen, however, with the emergence of scalable systems, allowing a system's architecture and topology to be selectively varied from one hardware implementation to the next according to the needs or desires of different users. Clearly, as the system enlarges or becomes more complex, it becomes much harder to predict a single counter accuracy that will always absorb the likely skew in the selected hardware implementation. One solution is to select a single, very coarse accuracy that no matter how large or complex the system gets, will always absorb the expected skew. Selection of such a coarse accuracy also degrades the potential performance of the system, however, by limiting, at the outset, the potential precision with which the system may run. This is particularly disadvantageous for smaller or less complex hardware configurations which must now run on an overly coarse accuracy.
Another solution is to select a finer accuracy and hope that it is still sufficient to absorb the potential skew of a system configured near the maximum scalable capacity of the system. Under this alternative, the system risks loss of counter synchronization in larger and more complex hardware configurations, an event which usually precipitates a processor interrupt and a requirement to re-initialize the system.
There is therefore a need in the art to be able to select system counter accuracies on a scalable basis corresponding to the size and/or complexity of the hardware configuration. An accuracy can then be selected to absorb the skew expected in a particular hardware configuration, while still enabling optimally precise counter accuracy in smaller or less complex systems.
The solution also advantageously should be "invisible" to software, in that counters continue to have a fixed resolution with selectable accuracy. There is also a need in the art to compensate for counter sync pulse skews which may exceed the counter resolution predefined by the system, where such compensation is accomplished without changing the accuracy presented to software.
SUMMARY OF THE INVENTION
The above and other needs are met by a system and method in which counter accuracy is a variable whose value in a particular hardware configuration corresponds to the skew expected in that configuration. In a preferred embodiment, although not mandatorily, the accuracy value is defined to the system at initialization time. Advantageously, the accuracy value is selected according to the result of a skew-calculating algorithm having variables representing skew-affecting parameters (such as system topology or system processing traffic levels, for example).
The present invention is thus scalable. As the topological size and complexity of the system increase, the accuracy value is selected according to the corresponding level of skew expected in the hardware configuration. At the same time, the accuracy value need not be selected any coarser than is required to absorb the skew in the configuration. Counter accuracy for particular hardware configurations is thus optimized.
It will be appreciated that according to the present invention, the resolution of counter references visible to software stays fixed (preset at system design time) while the counter accuracy can be varied to compensate for expected skew. In a preferred embodiment, the software resolution defines a specific bit in a clock-counting register, where software will always identify that bit as the least significant bit in reading a time-of-century ("TOC") counter. Depending on the accuracy value defined to the system at initialization time, however, counters may be rounded at synchronization time to a different bit from this resolution bit. This means that in a system having coarse counter accuracy, the software may see a counter rounded to 1 or more bits greater in significance that the fixed resolution bit. This loss of counter precision to software is nonetheless tolerable in most systems, so long as it is well known and can be taken into account in assessing reliability of counter references. The advantageous "trade-off" against this possible loss of precision is that counter accuracies can be scalably selected to absorb skew.
The inventive counter synchronization mechanism is implemented in a preferred embodiment by enabling a prescale register (which normally just converts clock increments into counter increments) to participate in the counter rounding process at synchronization time. Prescaling and counter synchronization are generally separate operations in systems of the current art, since counter synchronization is generally a function of a fixed counter accuracy value. By allowing the prescale register to participate in the counter synchronization process, however, the software-visible part of the register remains constant, but is subject to the variable-accuracy rounding process described herein.
It is therefore a technical advantage of the present invention to allow for skew in clock synchronization on a scalable basis.
Another technical advantage of the present invention is that compensation for skew is "invisible" to software.
Another technical advantage of the present invention is that in scalable systems, counter accuracy may be traded off on a "sliding scale" against the ability of system synchronization mechanisms to absorb expected skews. Larger and more topologically complex hardware configurations will precipitate larger expected skews, and so counter accuracy may be coarsened to allow counter synchronization mechanisms to absorb such skews without loss of synchronicity. Smaller systems may enjoy a finer counter accuracy corresponding to the smaller expected skew.
A further technical advantage of the present invention is that in a preferred embodiment, a parameter representing counter accuracy may be input at system initialization time to correspond with the expected skew within the system. The parameter may be derived from an algorithm having variables representing skew-affecting factors such as topological size of the system, or expected processing complexity.
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 hereinafter which forms the subject of the claims of the invention. It should be appreciated by those skilled in the art that the conception and the specific embodiment disclosed 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.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, and the advantages thereof, reference is now made to the following descriptions taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic diagram illustrating two nodes within an exemplary architecture and topology on a system on which the present invention may be embodied;
FIG. 2 is a schematic diagram illustrating further exemplary topological interconnection of the architecture of FIG. 1;
FIG. 3 is a schematic diagram of an exemplary system having 112 nodes;
FIG. 4 is a schematic diagram showing the sync pulse distribution arrangement;
FIG. 5 is a block diagram illustrating processing of sync pulses in accordance with the present invention; and
FIG. 6 is a representation of an exemplary register storing clock counts and TOC counts according to the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following description is made with reference to exemplary architecture and topology used in connection with a Hewlett-Packard SPP2000 multi-processor system. This architecture may have as many as 112 nodes. It will nonetheless be understood that the principles of the present invention, as exemplified by the following description of specific aspects of the SPP2000 system architecture, are not limited to such examples, and apply to any architecture in which remote counter synchronization is subject to problems with skew.
Turning first to FIG. 1, depicts a schematic overview of the architecture and topology of two nodes in the exemplary SPP2000 multi-processor, specifically nodes 0 and 1. FIG. 2 depicts a single node. FIG. 3 illustrates a 112 node system, in which nodes 24 are organized as seven X-dimension rings 26 by four Y-dimension rings 27 forming a wall 23. Four of such walls are interconnected by four Z-dimension rings 28. A bridge node (not illustrated) is used to connect a Y-dimension ring to a Z-dimension ring. As noted above, it will be appreciated that the topologies illustrated in FIGS. 1, 2 or 3 are exemplary only, and that the present invention applies to other topologies.
Returning to FIG. 1, two processors 10 are advantageously connected to processor agent chip ("PAC") 11. PAC 11 has an input/output (I/O) subsystem and is coupled to cross bar 12.
One function of the PAC 11 is to transmit requests from the processors 10 through the cross bar 12 and to memory access controllers ("MACs") 14, and then to forward the responses back to requesting processor 10. MACs 14 control access to coherent memory. In the exemplary architecture described herein, each MAC 14 supports up to 2 Gbytes in 4 banks, each bank 29 with 512 Mbytes. The memory banks comprise SIMMs of synchronous direct random access memory (SDRAMs).
With continuing reference to FIG. 1, when processor 10 generates a request to access memory or other resource, PAC 11 examines the request address to determine the proper MAC 14 for handling the request, and then PAC 11 sends the request through RAC 12 to the appropriate MAC 14. If the MAC 14 determines the node ID is not to a local memory address, then MAC 14 forwards the request to the ring interface controller (also known as a toroidal access chip, or "TAC") 15. If the MAC 14 determines the request address is on the local node (i.e. controlled by that MAC 14), the MAC 14 accesses the appropriate memory 29.
Each PAC 11 contains a time of century ("TOC") counter 13. This counter counts according to the local clock frequency. Each node has a single crystal clock and the TOCs on the same node operate from that clock. Each processor attached to a PAC 11 has access to TOC 13 with relatively equal latency between the processors, such that if the two different processors read TOC 13 at substantially the same time, each processor reads approximately the same value, or at least within an acceptable tolerance limit.
It is well-known, however, that no two crystals are identical, and minute imperfections and variations in the oscillation rates of supposedly identical clocks cause those clocks to keep time at slightly different rates. In the exemplary architecture described herein, each node has a different clock, and so TOCs 13 operating on the different nodes are likely to be counting at slightly different rates. Accordingly, TOCs 13 throughout an entire system need to be synchronized periodically, such that when a processor on a remote node reads or accesses the memory or other device on the local node, both local and remote TOC references may be expected to be in synchronicity.
It will be further appreciated that synchronization throughout the system must be with respect to a base, or "master" TOC 13. As shown in FIG. 4, a preselected TOC M within a designated PAC 11 on a single node 30, usually node 0, is designated to be the master. The PAC 11 holding master TOC M generates synchronization ("sync") pulses to be sent to other PACs on both local and remote (or "slave") nodes 31 to keep those TOCs on those other PACs in synchronicity with master TOC M.
Designated PAC 11 distributes sync pulses to PACs on the local node 30 via pathway 21, and to remote nodes 31 via pathway 16. In a preferred embodiment, internodal pathway 16 is a Scalable Coherent Interconnect ("SCI") ring, although the present invention is not specific to any particular pathway between nodes. Once the sync pulse is received at remote nodes 31, pathways 22 within those remote nodes deliver the sync pulse to PACs within those nodes.
FIG. 5 depicts a block diagram illustrating an exemplary synchronization process used by TOCs 13 shown at each PAC on FIG. 4. In a preferred embodiment, clock 35 and clock generator 36 generate ticks at a rate of 16 MHz. Prescale/synchronizer 37 receives these ticks, and, in a preferred embodiment, divides by 16 to increment TOC counter register 38 at a rate of 1 MHz. This equates to one increment of TOC counter register 38 every μsec. It will be appreciated that this division-by-16 process is accomplished by (1) prescale/synchronizer incrementing a prescale register with clock ticks, and then (2) software ignoring the four least significant bits in the register in defining the least significant bit of TOC counter references. This prescale operation thus defines a fixed resolution counter visible to software, preset at system design time. In the example above, the fixed resolution visible to software is 1 μsec.
As discussed above, this TOC counting mechanism needs to be synchronous throughout the system. With momentary reference back to FIG. 4, this is achieved by designating one PAC 11 on one node to have the master TOC M and distributing sync pulses from TOC M to other TOC counters throughout the system.
With reference now to FIG. 5, the sync pulse distribution mechanism at each PAC is responsive to reception of a sync pulse by prescale/synchronizer 37 from TOC sync pulse distribution logic 34. The operation of TOC sync pulse distribution logic 34 depends on whether the local TOC is the master TOC M or not. If it is the master, then TOC sync pulse generator 32 sends a sync pulse to distribution logic 34 at a predetermined interval (in a preferred embodiment every 256 ticks of clock generator 36). If it is not the master, then TOC sync pulse generator 32 is dormant and TOC sync pulse distribution logic 34 receives a pulse from the master located elsewhere on another PAC. TOC sync pulse generator 32 knows whether or not it is the master (and therefore, whether or not to generate a pulse) responsive to a control signal from TOC sync master 33. In a preferred embodiment, TOC sync master 33 is a Control and Status Register ("CSR") bit whose condition ("1" or "0") designates whether or not TOC sync pulse generator 32 is the master, and thus, whether or not it should generate a pulse.
According to the present invention, the sync pulse received by TOC sync pulse distribution logic 34 is then fed to prescale/synchronizer 37 and to TOC sync pulse checker 39. As noted above in the "Summary" section, feeding the sync pulse to prescale functionality in this way is an operation not usually found in current systems. In a preferred embodiment, prescale/synchronizer 37 synchronizes (i.e., resets TOC counter register 38 up or down) according to the information in the sync pulse, and a control signal from TOC sync accuracy 40. The control signal informs prescale/synchronizer 37 of the system's predefined counter accuracy. As will be described below, this accuracy may not be the same as the fixed resolution visible to software. In a preferred embodiment, the predefined counter accuracy can be found in two CSR bits.
According to the present invention, the accuracy ordained by TOC sync accuracy 40 may be varied. Advantageously, the accuracy is set for a particular hardware configuration by assigning a value to a parameter at system initialization time.
Calculation of the parameter's value may be accomplished at system initialization time by reference to an algorithm. The algorithm ideally includes variables representing skew-affecting factors such as topological size and processing complexity of the system. For example, with momentary reference to FIG. 4, in an embodiment in which nodes are linked by an SCI interface, the topological size of a system can be measured in terms of "hops" required to be made by a sync pulse from TAC to TAC in order to travel from master TOC M to the most remote node 31. Other methods of measuring topological remoteness are possible, and the present invention is not limited in this regard.
A second measurable variable contributing to latency in the delivery of a sync pulse is the expected processing time required by the system to perform certain processing steps in delivering a sync pulse. Table 1 below shows exemplary processing times for such steps in a preferred embodiment.
TABLE 1______________________________________ ExpectedStep in delivering sync pulse signal processing time______________________________________Synchronize core logic clock signal 1 cycleSynchronize master node sync pulse 2 cyclessignalSynchronize slave node sync pulse 2 cyclessignal1 TAC hop 12 cycles______________________________________
Other processing steps and/or expected processing times are possible, and the present invention is not limited in this regard. Moreover, cycle time is a variable in itself. In the Hewlett-Packard SPP2000 system used in the preferred embodiment, cycle time is 8.33 nanoseconds ("ns"). This value will vary from system to system on which the present invention is enabled.
Using the parameters suggested above in reference to the SPP2000 system, an exemplary skew-calculating algorithm is
t=41.65+12 n nanoseconds
where t is the expected level of skew (latency in delivering a sync pulse) and n is the number of TAC hops required to reach the furthest node from the master node.
Other algorithms to determine a level of skew for a delivered sync pulse may also be derived. Additional variables, such as expected clock crystal error may also be used. The present invention is not limited to specific forms or variables in deriving an algorithm to compute an expected level of skew. The results of these calculations, however, may be used to select a corresponding counter accuracy to be held by TOC sync accuracy 40 on FIG. 5 when sending control signals to prescale/synchronizer 37.
Returning now to FIG. 5, it will be seen that prescale/synchronizer is receiving sync pulse information from distribution logic 34, accuracy information from TOC sync accuracy 40, and local clock information from clock generator 36. Prescale/synchronizer 37 is now disposed to synchronize TOC counter register 38 with the master TOC M from FIG. 4. The operation of prescale/synchronizer 37 is in this regard further explained with reference to FIG. 6. Register 601 is a register counting clock ticks. As already noted, in a preferred embodiment, this is at a rate of 16 MHz. Also as already noted, prescale functionality in prescale/synchronizer 37 on FIG. 5 is causing the four least significant bits of register 601 to be invisible to software (i.e., dividing local clock counts by 16). The software thus sees a fixed resolution of 1 μsec in counter references.
Let it now be assumed that the predefined system accuracy ordained by TOC sync accuracy 40 on FIG. 5 is also 1 μsec. Synchronizer functionality in prescale/synchronizer 37 on FIG. 5 must therefore ensure that at least the fifth bit 602 of register 601 on FIG. 6 is synchronous with other counters in the system. Accordingly, when a sync pulse arrives, prescale/synchronizer 37 rounds the value of register 601 according to the information in the sync pulse. Since fifth bit 602 is the least significant bit in the predefined counter accuracy of 1 μsec, the four bits to the right of fifth bit 602 represent a "window" of time in which sync pulse delivery time can be affected by skew without affecting the rounded value of fifth bit 602. In a preferred embodiment in which sync pulses are delivered nominally every 16 μsec in a system governed by a 16 MHz clock, this window is ±7 ticks either side of expected pulse delivery time, which equates to ±437.5 ns. So long as sync pulse continue to be received within this window, the local counters can be expected with confidence to be synchronous with the rest of the system up to the predefined counter accuracy of 1 μsec.
In this example, the software sees counter references that may be relied upon as synchronous to the same level of accuracy as the fixed counter resolution of 1 μsec.
Now let it be assumed that the accuracy ordained by TOC sync accuracy 40 on FIG. 5 is 2 μsec (following entry of a different value for the corresponding parameter at initialization time). In this case, synchronizer functionality in prescale/synchronizer 37 need only ensure that at least the sixth bit 603 of register 601 on FIG. 6 is synchronous with other counters on the system to maintain synchronicity. The "window" in which skew will not affect the accuracy of sixth bit 603 has now increased to five bits, or ±15 ticks either side of expected pulse delivery time.
The compensation for skew thus becomes scalable, trading off accuracy for increased ability to compensate for skew without affecting counter synchronicity or resolution as seen by software. Table 2 below highlights this further by reference to the examples used in the preferred embodiment.
TABLE 2______________________________________ Check Range 16 MHz clockAccuracy Nominal 16 μsec sync pulse interval______________________________________1 μsec 256 ± 7 clock ticks (±437.5 ns)2 μsec 256 ± 15 clock ticks (±937.5 ns)4 μsec 256 ± 31 clock ticks (±1.938 μsec)______________________________________
In this example of an accuracy value of 2 μsec, however, the software is still looking at register 601 on FIG. 6 with a resolution of 1 μsec (i.e., ignoring the four least significant bits). The precision of counter accuracy seen by software is thus less reliable, since the counter has been rounded at synchronization time to bit 603, which is the second bit in significance visible to software. As noted above, this potential loss of precision is nonetheless tolerable in systems where the loss is predefined, known about and accountable for. The inventive mechanism has allowed skew to be absorbed as a "trade off" for this potential loss of precision.
It will be seen that although the invention is described above with reference to two examples of clock accuracy, the invention will apply to any selected accuracy. The coarser the accuracy selected, the less precise the counter references seen by software will tend to be. The finer the accuracy selected, the more precise they will tend to be. Of course, when an accuracy selected is so fine that counter synchronization accuracy exceeds the fixed counter resolution seen by software, the system will continue to run to the precision of the fixed counter resolution.
Completing the discussion of FIG. 5, TOC sync pulse checker 39 ensures that the accuracy ordained by TOC sync accuracy 40 is within the skew seen by the system. TOC sync accuracy 40 informs pulse checker 39 of the predefined resolution. Pulse checker 39 makes sure that successive sync pulses arrive within the corresponding "window" as illustrated above in Table 2. Upon detection of sync pulse arrival outside of the window, pulse checker 39 sends an interrupt to the processor informing the processor of the error condition. Generally, reinitialization of the system will be required, with perhaps selection of a coarser accuracy for TOC sync accuracy 40, or possibly system analysis for a broken wire or excessive noise on sync pulse delivery pathways.
The preceding description has disclosed the invention with reference to a scalable mechanism for compensating for skew on a system-by-system basis. Consistent with the present invention, it will be appreciated that a second embodiment will allow scalable selection of counter accuracy on a node-by-node basis, according to levels of skew expected within those nodes.
It will be appreciated that the present invention may be embodied on software executable on a general purpose computer having a central processing unit, a memory, and a mass storage device.
Although the present invention and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
|
A scalable mechanism operable on a multi-processor, multi-node system to compensate for "skew" in synchronizing topologically remote counters. The skew is caused by different latencies inherent in the system in delivering a synchronization ("sync") pulse to remote counters. The invention permits entry, advantageously at system initialization time, of a parameter defining the counter accuracy that will be visible to software in making counter references. The value of the parameter may be derived from an algorithm advantageously including variables representing, for example, skew-affecting factors such as topological remoteness of the furthest node from the master, and/or the anticipated processing times for processing steps to deliver the sync pulse. The invention is thus scalable. As the topological size and complexity of the system increase, the accuracy value is selected according to the corresponding level of skew expected in the hardware configuration. At the same time, the accuracy value need not be selected any coarser than is required to absorb the skew in the configuration. Counter accuracy for particular hardware configurations is thus optimized. In a preferred embodiment, prescale and synchronizer functionality are combined to allow prescale registers to participate in the counter-rounding process at synchronization time. Software reads the prescale registers down to a predefined, fixed resolution. This is accomplished by software ignoring a fixed number of least significant bits of clock increments in the prescale register. At the same time, synchronizer functionality rounds the prescale register at synchronization time according to the selected counter accuracy described above.
| 6
|
RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 14/238,695 filed Feb. 12, 2014, entitled “Device and Method to Accurately and Easily Assemble Glass Slides,” which claims priority to 35 USC §371 of PCT Application Serial No. PCT/US2012/51400, filed Aug. 17, 2012, entitled “Device and Method to Accurately and Easily Assemble Glass Slides,” which claims priority to U.S. Provisional Application No. 61/525,056, filed Aug. 18, 2011, entitled “Device and Method to Accurately and Easily Assemble Glass Slides,” which are each incorporated herein in their entirety by reference.
TECHNICAL FIELD
[0002] Embodiments of the present invention relate generally to laboratory devices and more specifically to systems and methods for the preparation and assembly of slide arrays for further experimentation.
SUMMARY OF THE EMBODIMENTS
[0003] According to some embodiments of the present invention, a device accepts a slide array that is to be assembled. A book-like hinged device can be constructed such that two surfaces with location points are exposed to facilitate the loading of two separate slides. One leaf of the book-like device is constructed such that it is a fixed mounting surface placed upon a bench top or other such piece of furniture. The other leaf of the book-like device is moveable from a fully open configuration to a full closed configuration, approximately 180 degrees of motion. Upon closing the hinge, the action brings two slides together in an accurate, repeatable, and easily managed manner. In the preferred configuration, a vacuum chuck on the moveable leaf of the book-like device holds a moveable slide firmly in place prior to its placement on top of a fixed slide. A spring loaded catch on the upper, moveable portion of the device can also maintain a hold on a slide during operation. The vacuum is applied on command of the operator. The closing of the book-like device brings the moving slide and the fixed slide into close but not intimate contact. Once the operator releases the vacuum upon command, the two slides are brought into final, resting position with a minimum of impact.
[0004] According to some embodiments of the present invention, the slide array is to be assembled inside of a separate carrier to allow further processing. The fixed slide is to be assembled inside of the carrier and then placed on a tooled spot on the fixed leaf of the book-like device. Further processing can include the application of an additional carrier on the top slide and the addition of a screw-type clamp to fixate the slide array.
[0005] According to some embodiments of the present invention, the slides described herein are composed of a transparent glass. The invention is not limited to the size of glass slide normally encountered in normal laboratory operations. The slides can be of a large variety of sizes and shapes. The slides need not be of identical sizes, smaller slides can be placed on a larger slide or vice versa. The slides need not be composed of transparent glass, other materials such as metals or plastics can be accurately assembled using the herein described device.
[0006] Various modifications and additions can be made to the exemplary embodiments discussed without departing from the scope of the present invention. For example, while the embodiments described above refer to particular features, the scope of this invention also included embodiments having different combination of features and embodiments that do not include all of the above described features.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1 illustrates an accurate slide assembly device 100 , according to the embodiments of the present invention.
[0008] FIG. 2 illustrates an accurate slide assembly device 100 , with a Hybridization chamber base installed in the loading position, according to the embodiments of the present invention.
[0009] FIG. 3 illustrates an accurate slide assembly device 100 , with a hybridization gasket slide loaded into the Hybridization chamber base, according to the embodiments of the present invention.
[0010] FIG. 4 illustrates an accurate slide assembly device 100 , with an experimental slide loaded into the vacuum chuck on the moveable arm, according to the embodiments of the present invention.
[0011] FIG. 5 illustrates an accurate slide assembly device 100 , with the vacuum producing cylinder depressed, according to the embodiments of the present invention.
[0012] FIG. 6 illustrates an accurate slide assembly device 100 , with the vacuum producing cylinder extended after release, producing a vacuum under the experimental slide, according to the embodiments of the present invention.
[0013] FIG. 7 illustrates an accurate slide assembly device 100 , with the moveable arm partly rotated into the slide dropping position, according to the embodiments of the present invention.
[0014] FIG. 8 illustrates an accurate slide assembly device 100 , with the moveable arm further deployed into the slide dropping position, according to the embodiments of the present invention.
[0015] FIG. 9 illustrates an accurate slide assembly device 100 , with the moveable arm in its final position prior to the release of the experimental slide, according to the embodiments of the present invention.
[0016] FIG. 10 illustrates a detailed view of an accurate slide assembly device 100 , with the experimental slide still held on the vacuum chuck slightly above the hybridization gasket slide just prior to final placement, according to the embodiments of the present invention.
[0017] FIG. 10 A is a close up view of the indicated portion of the accurate slide assembly device of FIG. 10 .
[0018] FIG. 11 illustrates an accurate slide assembly device 100 , with the experimental slide and the hybridization gasket slide in contact after the release of the vacuum in the vacuum chuck, according to the embodiments of the present invention.
[0019] FIG. 11 A is a close up view of the indicated portion of the accurate slide assembly device of FIG. 11 .
DETAILED DESCRIPTION
[0020] Unless otherwise indicated, all numbers expressing quantities of ingredients, dimensions reaction conditions and so forth used in the specification and claims are to be understood as being modified in all instances by the term “about.”
[0021] In this application and the claims, the use of the singular includes the plural unless specifically stated otherwise. In addition, use of “or” means “and/or” unless stated otherwise. Moreover, the use of the term “including,” as well as other forms, such as “includes” and “included,” is not limiting. Also, terms such as “element” or “component” encompass both elements and components comprising one unit and elements and components that comprise more than one unit unless specifically stated otherwise.
[0022] With reference to FIG. 1 , the Accurate Slide Assembly Device (ASAD) 100 consists of a base 101 whereby the static slide assembly tooling base 102 is solidly affixed in place, according to the embodiments of the present invention. Attached to the tooling base 102 is the moveable arm 103 via hinge 105 that keeps the respective tooling points, lower hybridization tooling area 108 and upper slide chuck 110 , in accurate registration or alignment with one another, according to the embodiments of the present invention.
[0023] With reference to FIGS. 1 , 2 , and 4 , Groove 107 (as shown in FIG. 1 ) allows the placement of a flexible seal 111 (as shown in FIG. 2 ), such as an o-ring, into the upper slide chuck 110 to provide a vacuum to be held in the vacuum space 106 once an experimental slide 113 (as shown in FIG. 4 ) has been placed in the upper slide chuck 110 , according to the embodiments of the present invention. With reference to FIG. 4 , hard tooling points 115 fix the experimental slide 113 in a tightly constrained location, according to the embodiments of the present invention.
[0024] With reference to FIG. 3 , lower slide receiver 112 is the part of the Hybridization chamber base fixture that receives the hybridization gasket slide 114 . Hybridization gasket slide 114 preferably includes several of chambers thereon in which material for processing may be added. Each chamber may be surrounded by a gasket or a flexible seal (similar to the flexible seal 111 above). Once the hybridization gasket slide 114 has been prepared by adding material to the surface, the operation of the ASAD 100 can commence, according to the embodiments of the present invention.
[0025] With reference again to FIG. 4 , the experimental slide 113 is held in place against the o-ring 111 (as shown in FIG. 2 ) after a vacuum is imposed in the open volume or vacuum space 106 (as shown in FIGS. 1 & 2 ). In the present configuration, as illustrated in FIGS. 4-6 , the vacuum is generated by manually pushing button 109 down on the spring return cylinder 104 and then releasing the button 109 to allow the spring to drive the piston inside of the cylinder 104 upwards. A flexible tube 117 connects the cylinder generated vacuum to the open volume or vacuum space 106 (as shown in FIGS. 1 & 2 ) in the moveable arm 103 , according to the embodiments of the present invention.
[0026] With reference to FIGS. 7-9 , once the experimental slide 113 is firmly seated against the o-ring 111 (as shown in FIG. 2 ) and sufficiently registered in the hard tooling points 115 , the moveable arm 103 can be articulated by rotation and the experimental slide 113 can be placed over the hybridization gasket slide 114 and inside of the lower slide receiver 112 , according to the embodiments of the present invention. The moveable slide (e.g., experimental slide 113 in this embodiment) is located in a controlled position so that as the slides (e.g., experimental slide 113 and hybridization gasket slide 114 in this embodiment) are brought into close proximity with each other, there will be no interference with the removable tooling (e.g., lower slide receiver 112 in this embodiment) or the stationary slide (e.g., hybridization gasket slide 114 in this embodiment). This location is provided in the present, preferred configuration by raised surfaces that are carefully designed to press against the periphery of the moveable slide, without interfering with the rest of the tooling or the fixed slide.
[0027] With reference to FIGS. 10 & 11 , the experimental slide 113 can then be released by depressing the button 109 (as shown in FIGS. 1-9 ) and allowing the cylinder spring to drive the cylinder 104 to its neutral state. This action causes the vacuum to be released to atmospheric pressure and the experimental slide 113 falls onto the hybridization gasket slide 114 under the force of gravity, according to the embodiments of the present invention.
[0028] With reference again to FIG. 10 , the small distance 118 between the experimental slide 113 and the hybridization gasket slide 114 allows the eventual placement of the experimental slide 113 and the hybridization gasket slide 114 (as illustrated in FIG. 11 ) to be gentle and non-disruptive event, according to the embodiments of the present invention. In this embodiment, the distance 118 is preferably, but not limited to, a distance on the order of about 1 millimeter or less.
[0029] With reference once more to FIG. 1 , the grooves 116 that are placed in static slide assembly tooling base 102 are present to allow a clamp (not shown) to be applied onto a stack of hybridization base, hybridization gasket slide, printed slide and the hybridization chamber top in order to fixate the two slides (as shown in FIG. 11 ) one on top of the other and held in place by the hybridization top in order to facilitate further processing, according to the embodiments of the present invention. Once gravity has brought the upper slide (i.e., experimental slide 113 ) into contact with the lower slide (i.e., hybridization gasket slide 114 ), it is possible to clamp the slides together without disturbing the orientation thereof. The device may now be used to repeatably fixate other pairs of slides.
[0030] The Accurate Slide Assembly Device (ASAD) 100 is intended to take a first prepared or otherwise unused slide (including, but not limited to, experimental slide 113 ) and place it in close proximity in a parallel attitude to a second prepared or otherwise unused slide (including, but not limited to, hybridization gasket slide 114 ). Prior to positioning in either upper slide chuck 110 or the lower slide receiver 112 , either of the first and second slides may be used or unused, prepared or unprepared, already processed or not yet processed.
[0031] In the above-described embodiment, vacuum was provided using the assembly—comprising the manually actuated button 109 and spring return cylinder 104 —that is connected to the o-ring-lined upper slide chuck 110 via flexible tube 117 . This, however, is not the only method of supplying a vacuum to the ASAD 100 . Other sources of vacuum include, but are not limited to, an external source that can be piped to the instrument, an on-board source that can be generated with a bulb commonly found in laboratories used for operating pipettes, and an air cylinder that is manually operated to provide a sufficient vacuum to pull the slide against an o-ring. The required vacuum pressure is on the order of inches of water (or about 2.5 to 25 mbar).
[0032] For the above-described embodiment, releasing the vacuum to atmospheric pressure may be accomplished via use of one of numerous valving options that are known to those skilled in the art.
[0033] In the above-described embodiment, the device is manually operated, but the device may be configured to operate robotically in ways known to those skilled in the art. In the above-described embodiment, a single hinge 105 is used, because it is the easiest configuration, but a combination of hinges and slides may also be built into the device to accomplish the same or similar task. Either slides, hinges, or both fit the task.
[0034] Although the above-described embodiment utilizes a hybridization chamber base, the device need not have a hybridization chamber base, but may simply be used to assemble the slides.
[0035] In some embodiments, the upper slide chuck 110 may be configured to be adjustably shifted along any direction within a plane that is parallel to the surface of the moveable arm 103 , in order to allow for ease of alignment between the experimental slide 113 and hybridization gasket slide 114 when the moveable is rotated to a position above the static tooling base.
[0036] Various embodiments of the disclosure could also include permutations of the various elements recited in the claims as if each dependent claim was a multiple dependent claim incorporating the limitations of each of the preceding dependent claims as well as the independent claims. Such permutations are expressly within the scope of this disclosure.
[0037] While the invention has been particularly shown and described with reference to a number of embodiments, it would be understood by those skilled in the art that changes in the form and details may be made to the various embodiments disclosed herein without departing from the spirit and scope of the invention and that the various embodiments disclosed herein are not intended to act as limitations on the scope of the claims. All references cited herein are incorporated in their entirety by reference.
|
Embodiments provide a slide assembly device having a static tooling base which is statically and solidly affixed to a base such as a table and a moveable tooling arm that is rotatable about a hinge connected to the static tooling base, so that moveable tooling arm rotates about the hinge in a manner similar to a book cover opening and closing. The embodiments further provide an upper slide chuck that is removably attachable to the moveable tooling arm and a lower slide receiver that is removably attachable to the static tooling base. The upper slide chuck is configured to hold an experimental slide via a vacuum mechanism to engagedly hold the experimental slide to the upper slide chuck while the moveable tooling arm is rotated about the hinge from an open-book position to a closed-book position.
| 1
|
BACKGROUND OF INVENTION
This invention relates to an apparatus and method for forming cylindrical magnet assemblies for rotating electrical machines.
In many forms of rotating electrical machines, there is provided a cylindrical shell that contains a plurality of circumferentially spaced permanent magnets. Generally these magnets are retained within the shell by a magnet case that is complimentary to the shell. However, recently the use of high energy neodymium based magnets has replaced ferrite based magnets. By using these high energy neodymium based magnets, it is possible to increase the magnetic intensity while at the same time, reducing the size of the components. However, because of their high magnetic strength, it is necessary to insure that the magnets are rigidly held within the cylindrical shell.
One way it is proposed to maintain the magnets in position is to deform or fold the edge of the shell into engagement with the magnets so that they are trapped between two flanges thus formed on the shell. However, the previous methods for forming this have resulted in a cumbersome operation which has been difficult to obtain automatically and required two separate forming steps in different stations.
It is, therefore, a principle object to this invention to provide an improved and simplified apparatus and method for assembling the permanent magnets of a rotating electrical machine.
It is a further object to this invention to provide an improved method and apparatus for retaining the permanent magnets in position within a cylindrical shell, which is versatile and can be adapted for use with various sized shells.
SUMMARY OF INVENTION
A first feature of the invention is adapted to be embodied in a machine for folding over a peripheral flange of a cylindrical shell. The apparatus comprises a support for the shell, a forming tool having a pre-bending section and a final bending section angularly related to each other about a plane extending parallel to the support and a drive. The drive is effective to cause relative axial movement of the support and the forming tool to bring the forming tool into engagement with a peripheral flange of a shell positioned on the support. The drive also effects relative radial movement of the support and the forming tool for determining which of section of the forming tool engages the peripheral flange of the shell positioned on the support. In addition, the drive effects relative rotation of the support and the forming tool to deform a circumferential portion of the peripheral flange of the shell positioned on the support. A control operates the drive for first partially bending the peripheral flange of the shell positioned on the support around a circumferential area by the pre-bending section of the forming tool and then completes the bending thereof by the final bending section of the forming tool.
Another feature of the invention is embodied in a method of forming a magnet assembly for a rotating electrical machine. The method comprises the steps of forming a shell having a cylindrical section open at one end and at least partially closed at its other end by a radially extending end wall extending radially inwardly from the cylindrical section and an extending section thereof at the open end of said shell. A plurality of magnetic sections are placed within the shell with their outer periphery in engagement with the inner surface of the cylindrical section and one end thereof in engagement with the end wall. The extending section of the shell is initially bent toward the magnetic sections by bringing a first section of a forming tool into axial contact therewith and then continuing to bend a circumferential extent of the extending section by effecting relative rotation between the shell and the forming tool around the axis of the cylindrical section. Then the extending section is finally bent of into locking engagement with the magnetic sections by bringing a second section of the forming tool into contact with the extending section and effecting relative rotation between the shell and the forming tool around the axis of the cylindrical section.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a front elevational view of an apparatus constructed in accordance with the invention and capable of performing the method of the invention.
FIG. 2 is a side elevational view of the apparatus.
FIG. 3 is an enlarged view looking in the same direction as FIG. 1 with portions shown broken away and in section.
FIG. 4 is a perspective view, with a portion broken away, of a cylindrical shell which forms the magnet carrier.
FIGS. 5-7 are is a cross sectional view looking in the same general direction as FIG. 3 and show the steps in the forming operation.
FIG. 5 shows the forming tools before engagement with the work piece.
FIG. 6 shows the initial pre-bending forming operation.
FIG. 7 shows the final bending operation.
DETAILED DESCRIPTION
Referring now in detail to the drawings and initially to FIGS. 1 through 3, an apparatus for performing the method of the invention and embodying the invention is indicated generally by the reference numeral 11 . The apparatus 11 includes four corner pillars 12 , which are adapted to be supported on the floor. The pillars 12 are connected to each other at their upper ends by cross pieces 13 and at their lower ends by cross pieces 14 to form a rigid frame for the apparatus 11 .
A support plate 15 is affixed to the pillars 12 at an appropriate height and is adapted to support a work piece in the form of a cylindrical ferrous material having a shape best shown in FIG. 4 and identified generally by the reference numeral 16 . Referring now to FIG. 5, the workpiece 16 includes a cylindrical shell portion 17 that is at least partially closed at one end thereof by a radially inwardly extending end wall 18 . The end wall 18 forms an opening 19 to pass a shaft in the completed rotating electrical machine.
A cylindrical inner surface 21 of the shell 17 is adapted to receive a plurality of circumferentially spaced permanent magnets, which may be carried in a magnet carrier of any suitable type. These magnets and carrier are positioned to engage the cylindrical surface 21 with their lower ends being supported on the end wall 18 .
A ledge 22 is formed at the upper end of the surface 21 and is coextensive with the upper ends of the magnets and their carrier. A thinner peripheral flange 23 is formed on the shell and in the illustrated embodiment forms a continuation of the cylindrical section 17 . This peripheral edge 23 has a length that is greater than the radial dimension of the end surface 22 for a reason which will become apparent shortly.
Referring again to the apparatus 11 and specifically FIGS. 1 through 3, the support plate 15 has mounted on it a fixture 24 that is adapted to receive the shell 16 and hold it against transverse movement. This fixture 24 is rotatably connected to a drive shaft 25 that is driven by a rotary motor 26 which may be hydraulically operated.
A moveable forming tool apparatus, indicated generally by the reference numeral 27 , is supported for vertical movement in the directions indicated by the arrow A on guide rails 28 formed on the pillars 12 . This moveable forming tool apparatus 27 has a base portion 29 that is connected to the piston rod of a reciprocating hydraulic cylinder assembly 31 . The cylinder housing of this assembly 31 is fixed to the upper cross pieces 13 by a fastener arrangement 32 .
A feed screw, indicated generally by the reference numeral 33 , is rotatably journalled on the underside of the base portion 29 and has a pair of axially spaced threaded portions 34 and 35 which are of opposite hand. This feed screw 33 is journalled in a pair of spaced bearing assemblies 36 and is driven by the shaft 37 of a further rotary hydraulic motor 38 .
Referring now primarily to FIG. 3, a pair of forming tool assemblies, each indicated generally by the reference numeral 39 , are associated with the feed screw portions 34 and 35 . These assemblies 39 include recirculating ball nuts 41 each of which cooperates with a respective one of the feed screw portions 34 and 35 , so that when the feed screw 33 is rotated in one direction or the other, the assemblies 39 will move toward each other or away from each other in the directions indicated by the arrow B.
Each nut 41 has a supporting brackets 42 , each of which journals a pair of shafts 43 . Rotatably supported on the shafts 43 are forming tools 44 . Each forming tool 44 has an angularly inclined surface 45 , which forms a pre-bending section and a generally cylindrical portion 46 which forms the final bending operation. These operations will be described shortly in more detail.
Referring now back primarily to FIGS. 1 and 2, the apparatus further includes a control panel 47 that controls the operation of the reciprocating hydraulic motor 31 and the rotating hydraulic motors 26 and 38 . The hydraulic system for these operations is shown schematically at 48 and is contained within a hydraulic circuit assembly.
An operator start switch 49 is conveniently positioned on the machine so that the operator can initiate the forming operation, which will now be described by primary reference to FIGS. 5 through 7. As may be best seen in FIGS. 5 through 7, the forming tool forming sections 45 and 46 are disposed at an angle to each other. In the illustrated embodiment, the section 45 is a cone of revolution and thus has a planar configuration in cross section. It is also to be understood that this shape could be of a concave curve and in any event terminates at the section 46 , which extends parallel to the work piece face 18 and surface 22 .
In operation, a work piece 16 with the permanent magnets and the magnet carrier in place is positioned on the support 24 and specifically in confronting relationship to the forming tools 39 . It should be noted that the permanent magnets may magnetized before being inserted into the shell or may be magnetized thereafter.
Initially, the feed screw 33 is rotated in a direction to cause the forming tools 39 to be positioned so that their pre-forming sections 45 are disposed immediately above the extending flange 23 of the shell 16 . Then, the device is lowered by actuation of a hydraulic cylinder 31 so as to bring the sections 45 of the forming tools into engagement with the flange 23 as shown in FIG. 6 so as to partially deflect it. The workpiece 16 is rotated so that the entire circumferential extent of the flange 23 is pre-bent.
Then, the feed screw is rotated so as to move the forming tools 39 away from each other and to bring the final forming sections 46 into registry above the top of the bent flange 23 . Then, the device is further lowered and rotated so as to complete the forming operation.
Thus, it should be readily apparent that the apparatus prevents both the pre-forming and final bending to be accomplished in the same station and in successive steps. Also, because of this construction the apparatus is capable of affixing magnet carriers having widely different diameters. Of course, the foregoing description is that of preferred embodiment of the invention and various changes and modifications may be made without departing from the spirit and scope of the invention, as defined by the appended claims.
|
An apparatus and method for forming cylindrical magnetic assemblies for rotating electrical machines. The apparatus and method pre-bends and finally bends a flange of the supporting shell to lock the permanent magnets in place. This is done in a single station and in two steps by way of an apparatus that permits handling of cylindrical bodies of considerably different diameters and lengths.
| 8
|
BACKGROUND OF THE INVENTION
1. Technical Field
The present invention relates to dispensing apparatus and in particular to a portable self-contained pneumatic gun for dispensing metered and/or mixed single or plural-component flowable materials. More particularly, the invention relates to a portable dispensing pneumatic gun which is self-contained and internally muffled for delivering flowable materials from single or two-component packages wherein the flowable materials are metered and/or mixed closely adjacent to the point of dispensing or application.
2. Background Information
An ever increasing number of products used in everyday life require the dispensing of liquid or semi-liquid flowable materials in one form or another for their manufacture. These flowable materials typically comprise two-component reactive resins: however, single component flowable materials are also frequently employed in such manufacture. The types of materials dispensed include virtually any flowable liquid, semi-liquid, or paste such as epoxies, polyurethanes, silicones, polyesters, acrylics, polysulfides and phenolics, for example. Common commercial manufacturing processes in which such materials are used include injecting precise amounts of mixed resins into molds, encapsulating electric components with insulating resins, applying continuous beads of structural adhesives, injecting polyesters into closed molds, sealing joints with two-part polysulfides, and numerous other functions requiring accurate material control and delivery. Examples of product applications for these materials and processes include under-the-hood electronic assemblies and safety devices for the automotive and trucking industry; encapsulation of magnetic and other advanced electrical devices for the aerospace industry; component mounting, security potting and gun-type applications for circuit board assemblies and components and apparatus such as switches, power supplies, heating assemblies, and other electronic components for the appliance industry.
Thus, as the aforesaid flowable materials continue to be consumed in increasing quantities the demand for precise liquid and semi-liquid dispensing apparatus is also growing at an accelerated rate. The industry is continually searching for more reliable, efficient and accurate metering and/or mixing and dispensing apparatus for flowable materials for a variety of purposes. For example, a particular application may require that an apparatus efficiently and accurately dispense such materials ranging in amounts from less than 1 cubic centimeter to many gallons. However, although, the industry is calling for more exacting apparatus, it is also requiring that the apparatus design be simple, straightforward and capable of being operated by production personnel or conveniently integrated with automation devices such as robots and conveyor systems. Problems currently exist because many prior art metering, mixing and dispensing apparatus are immobile, requiring that the work be brought to the apparatus which most often is inefficient and impractical.
Moreover, the design of many types of the prior art metering, mixing and dispensing apparatus, due to their bulky nature and the inability to position the apparatus in close proximity to the work, include lengthy hoses for transport of the metered and/or mixed material, the components of which often begin to react prematurely, sometime before it is actually dispensed which is highly undesirable. Rather, it is preferable that the flowable materials be metered and/or mixed as closely as possible to the point of dispensation or application to avoid premature reaction of the materials. Also, locating the metering and mixing components of the apparatus as closely as possible to the dispensing point increases metering accuracy and control.
A most common problem with known dispensing guns is the matter of overrun discharge or dribbling of the flowable materials when dispensation is stopped or terminated. The slow release of pressure on the piston member causes the materials to continue to flow at a decreased rate until pressure is fully relieved resulting in inaccurate dispensing and improper ratios of mixed materials. Where two-component materials are dispensed simultaneously, they may have different flow and viscosity characteristics accentuating the inaccuracy of desired delivery. Loss of precise delivery of desired amounts is a frequent problem especially where small volumes are dispensed.
The structure of the subject apparatus is different from the prior art equipment. The subject improved dispensing gun of the pneumatic type of this invention is portable and self-contained. The need exists for an improved metering, mixing and/or dispensing apparatus in which single or plural-component flowable materials are metered and/or mixed adjacent to the point of dispensing and/or application, and which is portable enough to be handled by a human operator and/or which may be readily integrated with robotic or automation systems.
SUMMARY OF THE INVENTION
Accordingly, it is an objective of the present invention to provide a metering, mixing and dispensing pneumatic gun in which plural-component liquids, semi-liquids or pastes are delivered from prefilled packages or cartridges and released at a dispensing or applying location by readily portable simplified apparatus.
Another object of the invention is to provide a self-contained pneumatic gun which is portable and self-muffled for quiet operation and is easily handled by a human operator and which can be conveniently integrated into robotic and/or automation systems.
A further object of the invention is to provide a self-contained pneumatic gun for metering or mixing, and dispensing flowable materials in which the gun is internally muffled and provides for quick release of pressurized operating gas for positive control of material delivery.
Still another objective of the invention is to provide a self-contained dispensing gun of the pneumatic type which can dispense either unitary or a plurality of flowable materials having a wide range of viscosities and cure times from prefilled packages containing the flowable materials.
A still further objective of the invention is to provide a metering, mixing and dispensing gun which allows for accurate volume and delivery rate variability and which can accurately dispense flowable materials contained in single or multiple component packages or cartridges.
Another object of the invention is to provide a self-contained quietly operable pneumatic gun for flowable materials for dispensing such materials in properly metered and/or mixed relationship in which solvent purging of the mixer element is eliminated by the use of an integral disposable static mixer.
A still further objective of the invention is to provide a metering or mixing and dispensing gun of the pneumatic type which is operative by either relatively low-pressure or high-pressure compressed air or other gas and which is accurate in dispensing small volume output shots from prefilled packages. The gun is consistent and reliable for delivering the materials to both accessible and relatively inaccessible locations, the gun being portable, lightweight, compact and durable.
These objectives and advantages are obtained by the subject self-contained quietly-operable pneumatic gun for metering or mixing and dispensing at least two combined flowable materials from prefilled packages, the exact nature of the gun which may be stated as including at least one hollow chamber adapted to receive and retain the material-containing package and having a piston chamber for retaining an operating piston and its operative pressurized gas. The piston being hollow is located in an aligned second hollow chamber which is pressurized by a compressed gas delivered to the head of the hollow piston by a flexible internally-disposed tubular member connected to a quick-release valve mounted on the piston head for rapid discharge of the pressurized gas interiorly of the hollow piston and body member. The opposite end of the elongated piston is adapted to contact the cartridge for delivery of the material therefrom. The quick-release valve is mounted internally of the gun for discharge of the operative gas internally of the gun for its operation at minimal noise levels. The gun has a support handle mounted centrally between the package and piston chambers, the flexible tubular member for the introduction of pressurized gas being mounted spirally around the hollow piston for its collapse around the piston between the gun body member and the quick-release valve. The subject gun is fabricated from essentially non-machined moldable components for economical and simplified manufacture at very economical cost. The gun may be employed to dispense flowable materials from a wide variety of prefilled packages or cartridges which can have a great disparity in shape and cross-sectional contour. The packages may be cylindrical or rectangular in shape, or be comprised of side-by-side parallel attached chambers or other configurations known in the art. The packages may be formed of rigid, semi-rigid or flexible bag-like plastic materials. The package retention chamber of the gun can be modified as desired to accept and retain the package for dispensing therefrom without substantial change of the operative components of the gun. Such packages may be described as axial, co-axial, parallel or side-by-side.
BRIEF DESCRIPTION OF THE DRAWINGS
A preferred embodiment of the invention, illustrative of the best mode in which applicant has contemplated applying the principals and functions of the subject portable self-contained gun is set forth in the following description and is shown is the drawing and is particularly and distinctly pointed out and set forth in the appended claims.
FIG. 1 is a perspective view of the self-contained, self-muffled portable pneumatic gun of the present invention;
FIG. 2 is a longitudinal vertical sectional view of the pneumatic gun taken along a central axial region of the gun shown in FIG. 1;
FIG. 3 is a top plan view partially in fragmentary horizontal section of the gun shown in FIGS. 1 and 2;
FIG. 4 is an enlarged fragmentary sectional view of a portion of the piston head shown in dotted outline in FIG. 2 showing one operative position of the quick-release valve of the gun piston shown FIG. 2 for its positive movement;
FIG. 4A is an enlarged fragmentary sectional view similar to FIG. 4 showing the quick-release valve in its discharge position with the discharged compressed fluid exiting into the hollow piston of FIG. 2; and
FIG. 5 is a schematic view of the quick-release valve of the gun.
Similar numerals refer to similar parts throughout the drawings.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The pneumatic gun of the present invention is indicated generally at the numeral 10 and is shown in FIGS. 1 to 5 of the drawings. Gun 10 is primarily intended for delivering plural components from a prefilled two-component package or cartridge which is mounted within a package or cartridge chamber 11 located at the forward delivery end of the gun. The nature of the packages or cartridges is not intended to be a unique feature of the present invention since they have been previously described is the known prior art. Such packages or cartridges are employed in a wide range of manufacturing processes such as resin transfer molding, electrical potting and encapsulation structural bonding, sealing, casting and filling. However, if desired, gun 10 can be used for accurately metering or mixing and dispensing flowable single or plural types of materials from prefilled cartridges containing the constituents. It is primarily designed for dispensing paired types of flowable materials which are inter-reacted at the point of use and are especially useful in the manufacture of everyday commercial products such as components for use in the automotive and truck industry, as well as transformers, cable connectors, de-scrambler modules and components for the telecommunications industry.
Gun 10 preferably includes a generally cylindrical body member indicated generally at numeral 12 as shown in FIGS. 1 to 3. Body member 12 is preferably right-cylindrical in shape and includes a projecting handle member 13 adapted to supporting and controlling the portable gun. Body 12 has a cylindrical cartridge chamber 11 retailed thereon projecting forwardly adapted to receive and retain a complementally-contoured cartridge 14 shown in dotted outline. Chamber 11 has an open forward end through which the cartridge may be axially inserted into the chamber 11 from its forward end. The cartridge may or may not have an on/off valve 16 as shown on FIGS. 1 and 2 on its delivery end for opening and closing the delivery end of the cartridge by a projecting handle 16a. Package or cartridge chamber 11 need not be right-cylindrical in shape, but may be oval, square or rectangular in cross-sectional shape to retain a complementally-shaped package of similar size and shape depending upon known and newly-developed packages for a wide variety of flowable materials. The retention chamber 11 may be changed or replaced as desired or required by its separation from the body 12 and replacement by a different size and shape. The terts package or cartridge are used interchangeably herein since both are so used by skilled artisans in the subject art.
The cartridge 14 is retained in place by a hinged bifurcated retention member 17 which is swingably connected to body member 12 and is employed to retain the delivery end of the cartridge in cartridge cylinder 11. Other known retention members may also be utilized to retain the cartridge in place depending upon the cartridge design. On/off valve actuator 16a which is shown projecting from the cartridge cylinder in FIG. 2 is retained by retention member 17. A disk-shaped flanged member 18 is connected to retention member 17 at the delivery end of chamber 11, the flanged member having a central cut-out aperture 19 adapted to surround cartridge valve actuator 16a. The cutout area of disk 18 is adapted to retain cartridges of several types whether or not a valve 16 is mounted on the delivery end. A disposable mixing nozzle 20 is connected to the delivery end of the cartridge valve by a threaded connection and retention nut 21 to connect the disposable mixing nozzle to valve 16. Thus, a positive connection is maintained between the cartridge and delivery nozzle as known in the prior art. The cartridge has a diameter and length adapted to be fitted within the cartridge chamber so that it essentially fills the chamber in snugly seated relation. The cartridge retaining chamber may consist of a rigid, tubular member having a diameter and length closely matching the cartridge or an apertured mesh-type basket or other shape for such positive retention. The chamber may have a split flanged member at its terminus end for grasping the cartridge at or near its discharge end. Such elements can be widely varied.
Body member 12 of the gun has a slightly enlarged right cylindrical second chamber 25 projecting from its opposite end in axial alignment with the first cylindrical chamber 11 for retaining the cartridge. Chamber 25 is positively connected to the body member containing an elongated hollow piston member 26 which is forcibly movable toward the cartridge by a contained pressurized gas such as compressed air or carbon dioxide. The enlarged left hand end of the elongated piston 26 comprises the piston head 27 which is sealingly engaged with the inner wall of chamber 25 by a sealing O-ring 28. An annular groove 28a is formed in piston head 27 to seat and retain the O-ring 28. Piston head 27 has quick-release valve 29 mounted with its connector 30 projecting interiorly of the hollow piston head 27 to introduce pressurized gas into the quick-release valve 29.
The opposite end 32 of the piston is contoured to be complementally shaped to the opposite filling end of the cartridge from its delivery end. The cartridge has a contoured movable cap with a depressed central region surrounded by an integral annular ring-type portion which is common to multiple component cartridge caps. The inner or rearward piston head 27 is connected to the outer or forward piston head 32 adapted to contact the cartridge by tie rod 33 which is threadably connected to both ends of the elongated hollow piston. The tie rod 33 extends between the opposing spaced-apart ends of the hollow piston in an axial position, the piston end members being preferably molded of plastic materials.
The quick-release valve 29 is mounted within one portion of the piston head 27 with its connector 30 projecting interiorly of the hollow piston. Pressurized gas is delivered to the quick-release valve by a flexible tubular member 34 such as a flexible plastic tube or hose extending around the exterior of the hollow piston. Such hose member 34 is loose or spirally wrapped around the piston exterior from a source of pressurized gas to the quick-release valve. The gas hose 34 is connected to the source of pressurized gas preferably extending into the handle. The gas hose has a relatively small diameter and is collapsible around one piston during its movement from left-to-right as shown in FIG. 2. The completely interior mounting of the gas hose protects it from abuse and wear due to abrasion. The coiled gas line having a small diameter provides smoother loading of gas pressure on the piston and cartridge.
The handle may or may not contain a second gas valve 35 which may or may not be operable by a trigger 40 mounted within the handle to control delivery of pressurized gas to the pressure chamber 36 within the second hollow chamber 25 and air piston 27. A second connector 37 having a quick-release type fitting is mounted at a lower extremity of the handle 13 for connection to a source of pressurized gas. A second tubular member 50, such as an air hose, extends within the handle from connector 37 to air valve 35 to deliver pressurized gas to the handle area and to the pressurizable chamber 36. The handle 13 is also provided with a trigger guard 38 to protect the trigger 40 from accidental or unintended operation. The gas hose may also project exteriorly through the support handle and connect directly to a quick-release gas coupling which is connectable to the source of pressurized gas. In this alternate co-struction, second gas valve 35 and trigger 40 may be eliminated for gas pressure to be applied directly to quick-release valve 29. The flow of materials from the cartridge or package is controlled by valve 16 with the gas-pressure being maintained on the piston during on-off operation of valve 16.
The tie-rod 33 having threaded receiving openings at its ends is utilized to join the two ends of rigid tubular member 41 of the hollow piston 26 by threaded members connecting the two ends to the tie-rod with threaded metal bolts designated as 41a and 41b. Thus the hollow piston which comprises a hollow tube 41 can be formed of essentially an enlarged air piston head 27 at its left end and a second smaller head 32 at its other end having a configuration complemental to the cap portion of the filled cartridge. The smaller end has a contour including a central disc portion 42 and a surrounding annular ring portion 43 complementally contoured to the cartridge cap end for delivery of the materials from a two-component cartridge. The piston head 32 is replaceable to substitute various modified types of cartridge-contacting surfaces depending upon the type of cartridge being employed. This portion of the piston head 27 can be readily removed from the piston through chamber 11 for the replacement.
The tubular flexible hose 34 for pressurized air extends from second valve 35 mounted within the handle to the quick-release valve 29 in the piston head 27. The hose is spirally wrapped around the hollow piston for its collapse upon itself as the piston penetrates the cartridge for pressurized material delivery.
The quick-release valve 29 mounted in a localized lower region of piston head 27 may be comprised of one of various types of conventional quick-release valves. As shown in FIG. 4 when pressurized air or other gas is introduced into the quick-release valve through connector 30, an internal flexible diaphragm 45 comprised of a disk of elastomeric material is moved from right-to-left to close the outlet port 46 of piston head 27. Such outlet 46 extends from the diaphragm 45 through piston head 27 opening interiorly of the hollow piston. When the pressurized air is so introduced the air flows around the periphery of the diaphragm 45 through multiple channels 47 into pressurizable chamber 36 to move the piston head from left-to-right as shown in FIG. 2. Such operation is effected by depression of trigger 40 or connection to a pressurized gas source to operate air inlet valve 35 through air hose 34 and the quick-release valve 29. Upon release of the trigger 40, quick-release valve 29 is again operated to move the flexible diaphragm 45 from the position shown in FIG. 4 to that shown in FIG. 4A. The diaphragm 45 is then moved from left-to-right to seal the inlet port 48 of the valve. At that time the pressurized gas within chamber 36 is permitted to exhaust through outlet port 46 through the hollow piston and into the interior of the gun body. The pressurized gas is released very rapidly into the hollow gun body without excessive noise associated with conventional gun operation. Thus, when movement of the piston is stopped by release of the triggers or disconnection of pressurized gas, the pressurized air is exhausted into the gun interior through the quick-release valve. The exhaust air is muffled by its interior release within the hollow gun to provide quiet and vibration-free operation. Any airborne particles such as solids or droplets or oil contained in the released gas are retained within the gut body. Such gas exits through outlet passages 51 in the piston tubular body portion and into the body member and handle of the gun. The muffling is self-contained without any additional components being provided to achieve this function.
As shown in FIG. 3 an indicator rod 51 is attached to the larger piston head 27 in rigid relation extending through chamber 25 parallel to the piston. Its projecting end passes through an aperture in body member 12 and forwardly exteriorly thereof, the rod having a length preferably extending to the cap area of the cartridge. The indicator rod has marked indicia thereon such as a volumetric scale to provide a readable measure of volume delivery of material from the cartridge. Indicia on the rod may extend for essentially the full length of the indicator rod to deliver both small and large volumes of the cartridge material.
Upon quick release of the pressurized air, pressure on the cartridge is immediately released so that no overflow of the cartridge is effected. Thus, positive control of the delivered material is maintained so that no dribbling or overrun from the cartridge is permitted to occur. Small shots of the material such as from one to a small number of cubic centimeters of the material are ejected through and from the static mixer nozzle 20. The gun is quietly operated, operation is essentially vibration-free and extremely quiet for long term use of the gun without deleterious effects upon the operator or surrounding location. FIG. 5 illustrates the flow of pressurized air to and from quick-release valve 29. The letter P indicates the supply of air to chamber 36 through inlet channel 47. The letter A indicates the flow of air from chamber 36 through outlet channel 46, and the letter R indicates its exhaust position with a check valve i.e. the diaphragm, permitting quick release of air.
A disposable mixer eliminates the need for solvent purging as required in many prior art apparatus. It is an important feature of the subject gun that plural component liquids are metered and/or mixed adjacent to the dispensing location for increased accuracy which is particularly important when dispensing small volumes of material. An important feature of the gun is its self-contained components and quiet operation enabling it to be easily handled by a human operator or to be conveniently integrated into automation or robotic systems. The subject self-contained self-muffled gun of the present invention has a simplified structure which provides an effective, safe, inexpensive and efficient delivery apparatus which eliminates difficulties encountered with prior dispensing apparatus.
In the foregoing description, certain terms have been used for brevity, clearness and understanding but no unnecessary limitations are to be implied therefrom beyond the requirements of the prior art because such terms are used for descriptive purposes and are to be broadly construed.
Moreover, the description and illustration of the invention is by way of example and sets forth a best mode for practicing the invention the scope of the invention being not limited to the exact details shown or described.
Having now described the features, discoveries and principles of the invention the manner in which the improved self-contained self-muffled dispensing gun is constructive and used the characteristics of the construction, and the advantages will in useful results obtained and a new and useful structures, devices, elements, arrangements, parts and combinations are set forth in the appended claims.
|
A self-contained self-muffled pneumatic gun for dispensing one or two combinable flowable materials from a prefilled package or cartridge. The gun has a first hollow chamber for retaining the package in fixed relation, the package containing the materials to be dispensed and either having a dispensing valve thereon or not as known in the art. A second hollow chamber of the gun retains an axially-movable hollow tubular piston for pneumatically forcing discharge from the gun and through a metering, mixing and/or dispensing nozzle. The hollow piston has a quick-release valve mounted internally in its head portion for rapid release of pressurized gas internally of the gun body for its relatively quiet operation. Internal release of the gas pressure within the head portion serves to prevent noisy operation of the gun. The gun is capable of economical manufacture with the valve components being formed from essentially non-machined moldable components.
| 1
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a tool electrode driving unit of an electric discharge machine, and in particular, to a driving unit including an electrode actuator for rapidly moving the tool electrode toward and away from a workpiece.
2. Description of the Related Art
During electric discharge machining, concentration of discharge and resulting state of continuous arc discharge occurs sometimes when the clearance between the workpiece and the tool electrode has become inappropriate. Such continuous arc discharge will cause conspicuous mark to be left on the spot of the workpiece where the concentration of discharge has occurred, thereby making defective the machined surface of the workpiece. In addition, the concentrated discharges cause machining fluid to be resolved to produce pyrolysis products. As a consequence, the tool electrode and the workpiece short-circuit each other through the pyrolysis products to hinder the further progress of the machining.
In order to avoid occurrences of such situation, it is known to rapidly move the tool electrode toward and away from the workpiece to forcedly introduce the machining fluid between the workpiece and the tool electrode, thereby preventing an occurrence of concentrated discharge. More particularly, occurrence of the continuous arc discharge can be prevented by a squeeze effect of the machining fluid.
Conventionally, in order to provide a mechanism for enabling rapid retreating and approaching of the tool electrode relative to the workpiece, the tool electrode is rigidly attached to the distal end of the quill (spindle) in the electric discharge machine through a piezoelectric element, which functions as an actuator to utilize strain caused by the piezoelectric element, thereby causing a jump motion of the tool electrode to occur. However, such a motion of the tool electrode by the piezoelectric element is an impactive rapid one, that is, high-acceleration motion, so that a large impactive reaction force acts on the portions at which the tool electrode is supported. For instance, a tool electrode having a weight of 50 kg in total will cause a force of about 1200 kgf to act on the quill or column when the piezoelectric element operates. This great reaction force causes the quill or column supporting the tool electrode to be bent to absorb and consume considerable part (about 25%) of displacement generated by the piezoelectric element to pull up the tool electrode. Therefore, according to the conventional arrangement, the displacement generated by the piezoelectric element cannot be fully utilized for generating a jump motion of the tool electrode. Besides, a force caused by an impactive motion and transferred to a head or column of the electric discharge machine causes damage to feed screws, etc., thereby shortening the service life of the machine.
SUMMARY OF THE INVENTION
An object of the present invention is to provide an electric discharge machine, which prevents an impactive high-speed motion from propagating to a quill side of an electric discharge machine when an electrode actuator rapidly pulls up a tool electrode, as well as to enable the rapid retreat of the tool electrode by the electrode actuator to be performed efficiently.
To achieve the above object, according to the present invention, there is provided an electric discharge machine including a quill having a distal end portion to which a tool electrode is attached, the machine comprising: a support body to which the tool electrode is connected through an electrode actuator including constituted of an element adapted to be deformed when an external energy is applied thereto, the support body being non-rigidly connected to the quill with respect to an axial direction of the quill; and a counter weight fixed to the support body for absorbing an impact force toward the quill, the impact force being caused by a motion of the tool electrode, which is caused by deformation of the electrode actuator.
Preferably, the support body has an upper portion thereof arranged within a space formed in the distal end portion of the quill and supported by elastic supporting element mounted in the space. The support body has a lower portion thereof disposed outside the space. The lower portion is integrally formed with the counter weight, and is formed with a member for fixing the electrode actuator.
Preferably, an upper flange is formed at the upper portion of the support body, the upper flange being arranged within the space in the distal end portion of the quill, and upper and lower surfaces of the upper flange are supported by a plurality of pre-load springs mounted within the space to constitute the elastic supporting element. In addition, an oil damper is interposed between an inner wall defining the space in the distal end portion of the quill and a top surface of the upper flange.
More preferably, the element adapted to be deformed when an external energy is applied thereto has a reverse piezoelectric effect, electric strain effect, or magnetic strain effect. Alternatively, the element may be made of a shape memory alloy.
As mentioned above, according to the present invention, when the electrode actuator operates, the counter weight having a considerable large weight is kept at a functionally fixed point, though a great external force caused by deformation of the actuator acts on the electrode, whereby the quill or column is prevented from being deformed. Moreover, the deformation occurs in the direction toward the electrode, so that the action caused by the electrode actuator can be fully utilized for the jumping motion of the tool electrode, whereby the continuous arc discharge can surely be prevented by a squeeze effect of the machining fluid. Thus, keeping the quill or column of the electric discharge machine from the effect of the deforming force will contribute to the improvement in machining accuracy and a longer machine life.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front view schematically showing a main part of a machine according to an embodiment of the present invention; and
FIGS. 2 to 5 are enlarged views schematically showing examples of various modification of the elastic supporting means shown in the aforesaid embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a first embodiment. A tool electrode 4 is attached to a distal end portion of a quill 1 of an electric discharge machine. A space 5 having a circular section is defined in the distal end portion of the quill 1, as shown in the drawing. The space 5 is partitioned vertically by a circumferential flange 6 which projects in a horizontal direction from an intermediate portion of an inner wall which defines the space 5. Further, a through hole 8 is formed at a bottom wall 7 of the quill 1, and a piston 11 of a support body 12, which will be described later, extends therethrough. The whole of the support body 12 is made of stainless steel, and comprises a cylindrical piston 11, which extends vertically, and disk-like upper and lower flanges 9 and 10, which are integrally formed with upper and lower end portions of the piston 11, respectively. Further, an upper half of the support body 12 is received in the space 5 of the quill 1, while a lower half thereof is disposed outside the space, and an electrode actuator 3 is attached to the lower flange 10, as shown in FIG. 1. The tool electrode 4 is rigidly fixed to the electrode actuator 3.
The upper half of the support body 12 received in the space 5 of the quill is supported by elastic supporting means 2 arranged in the space 5 at a position where an outer side surface of the upper flange 9 of the support body 12 is opposing an inner side surface of the flange 6 which projects from the inner wall defining the space 5. That is, the support body 12 is not directly connected to the quill 1 but non-rigidly connected thereto through the elastic supporting element 2. However, the tool electrode 4, which is fixed to the lower flange 10 of the support body 12 through the electrode actuator 3, is designed so that it can be ordinarily controlled to a command position by perfectly corresponding with movement of the quill 1 during machining.
The elastic supporting element 2 comprises a plurality of springs 15 and 16, which are fixed to the top inside surface and bottom inside surface of the wall, oil dampers 17, and pressure bars 13 and 14. The thickness of the upper flange 9 of the support body is the same as that of the circumferential flange 6 on the quill side. The upper and lower surfaces of the upper flange 9 are urged downward and upward respectively by the force of a plurality of springs 15 and 16 applied, through pressure bars 13 and 14, from one end of the springs 15 and 16 of which the other ends are fixed respectively to the top inside surface and the bottom inside surface of the wall defining the space 5. That is, the springs 15 and 16 function as preload springs for the support body 12. Further, the oil dampers 17 together with spring 15 are interposed between the top inside surface of the wall and the upper surface of the upper flange 9 through the pressure bars 13.
The support body 12 is supported by the elastic supporting element 2 constructed as mentioned above, and hence movement of the quill 1 is restricted by the upper or lower springs 15 or 16 when the support body attempts to move in the upper or lower direction. Further, when the quill 1 of the electric discharge machine is moved in the vertical direction to control the position of the tool electrode 4, the support body 12 (and hence the tool electrode 4) perfectly follows the movement of the quill. That is, the springs 15 and 16, and oil dampers 17 constitute the elastic supporting element 2, and support the support body 12 in a non-rigid manner.
The lower flange 10 of the support body 12 has a peripheral edge with wall thickness increased to form an annular counter weight 18. Due to the provision of this counter weight 18, the support body 12 has a mass (weight) of about three times as much as the total weight (normally 100 kg or below) of the electrode actuator 3 and tool electrode 4.
In this embodiment, the electrode actuator 3 for causing a jump motion of the tool electrode 4 comprises a piezoelectric element. The piezoelectric element used here is an ordinary type comprising a plurality of blocks 19 of ceramic pellets made of titanic acid barium crystal piled in several layers, are interposed between base and operating plates, and these plates are arranged vertically so that expansion and contraction of the element due to piezo effect is performed in the vertical direction. The piezoelectric element or electrode actuator 3 is fixed to the center portion of the lower surface,of the lower flange 10 in the supporting body 12.
Operation of the electrode actuator 3 is controlled by means of an NC unit included in the electric discharge machine. The NC unit has a function of driving the electrode actuator 3 when it detects continuous arc discharges. More specifically, in the present embodiment, the piezoelectric element of the electrode actuator 3 is kept deformed or elongated as long as it is energized, but, when the power supply is interrupted, it will contract to cause the rapid retreat of the tool electrode.
The tool electrode 4 is formed for diemilling, and is rigidly fixed to the lower surface of the electrode actuator 3.
When continuous arc discharge is detected during the electric discharge machining using the tool electrode 4, power supply to the electrode actuator 3 will be interrupted according to a command supplied from the NC unit which has received the detection signal. At this moment, the piezoelectric element will contract instantaneously to cause the tool electrode 4 to be pulled up rapidly (by about 30 microns). This will cause a clearance between the workpiece and tool electrode to be increased instantaneously, so that machining fluid moves in and out of the clearance at a high speed, and then the continuous arc discharge is interrupted by the squeeze effect mentioned above. Such contraction of the piezoelectric element occurs as an impulsive high-speed motion to last about 500 micro seconds, so that a great force, as a reaction force to pull up the tool electrode 4, will be applied on the side of the support body 12.
However, since the support body 12, rigidly supporting the tool electrode 4, has a small natural frequency and a great inertia due to the provision of the counter weight 18, the supporting body 12 is kept at a fixed point while an acting force generated upon contraction of the piezoelectric element is exerted on the side of the electrode. Therefore, the reaction force is absorbed by the counter weight 18, whereby an impact to the quill 1 can be prevented. Moreover, the high-frequency impactive high-speed motion, caused by the contraction of the piezoelectric element, is exerted in a manner such that the support body 12 functionally serves as a fixed point, and this motion substantially acts on the side of the electrode, so that most of this motion can be used for pulling up the tool electrode 4.
However, the movement of the electric actuator 3 includes components other than the aforesaid impactive high-speed motion such as the longitudinal vibration or the like occurring in the tool electrode 4 or the support body 12. Since such a motion cannot be absorbed fully by the counter weight 18, vibration occurs in the support body 12 after the tool electrode 4 is rapidly pulled up by the piezoelectric element. However, the vibration is absorbed and buffed by the springs 15 and 16, which urge the upper and lower surfaces of the upper flange 9 in the support body 12, and is rapidly damped by the oil dampers 17. Therefore, the support body 12 does not actually vibrate, and thus no deformation occurs in the quill 1.
FIG. 2 shows a second embodiment. In the first embodiment, the elastic supporting element 2 comprises the springs 15 and 16, oil dampers 17 and the like. As shown in FIG. 2, the elastic supporting element includes springs 15 and 16, but the oil dampers 17 among these components can be omitted, if inertias (moving energy) of the tool electrode 4 and support body 12 are sufficiently absorbed by the springs 15 and 16. Furthermore, the piston 11 of the support body 12 may be constituted non-rigidly to dispense with the springs 15 and 16.
FIG. 3 shows a third embodiment. According to this embodiment, the space delimited by the upper portion of the support body 12 and the bottom of the flange 9 within the space 5 in the distal end portion of the quill 1 is filled with a fluid and is made to communicate with an accumulator 21. The accumulator pressure is adjusted so as to be balanced with the weight of the support body 12. Oil seal 22 is provided between the circumference of the upper flange 9 and the inner surface of the wall defining the space 5, while oil seal 23 is provided between the piston 11 and the circumference of the bottom wall 7. Thus, the support body 12 can be elastically supported by the fluid pressure. In this case, the fluid performs functions equivalent to those of the springs 15 and 16 and dampers 17.
FIG. 4 shows a fourth embodiment. In this embodiment, the upper flange 9 of the support body 12 is freely movable in the vertical direction in the space 5 of the distal end portion of the quill, and is supported by an elastic member 20 interposed between the upper flange and the bottom wall 7. The elastic member 20 has an elasticity whose degree is set so as not to hinder the positioning of the tool electrode 4. More specifically, the tool electrode 4 is arranged to be hanged down from the quill 1 in the axial direction, however, the support body 12 has a weight that is large enough for the positioning of the tool electrode 4.
Therefore, according to the fourth embodiment, a downward component of vibration caused by the motion of the electrode actuator 3 is absorbed and damped by the elastic member 20. On the other hand, an upward component of the vibration is not subject to the damping effect, so that this component will not give any adverse effect on the machining operation, though it sometimes causes the support body 12 to bounce upward. Furthermore, this embodiment enables the structure of the elastic supporting means to be simplified.
FIG. 5 shows a fifth embodiment. In this embodiment, elastic members 21 and 20 respectively fill the spaces both above and below the upper flange 9, which is arranged in the space 5 of the distal end portion of the quill 1 unlike the case of the fourth embodiment, to absorb and dump the vibration of the support body 12 caused by deformation of the electrode actuator 3. Furthermore, according to this embodiment, not only the structure of the elastic supporting element 2 can be made simpler but also the tool electrode 4 can be supported more stably compared with the fourth embodiment.
In addition, the electrode actuator 3 is not restricted to an element of a type providing reverse piezoelectric effect or electric strain effect, and may be of any type of element, such as magnetic strain effect element and shape memory alloy, which causes rapid physical deformation when an external energy of some kind is applied.
|
An electric discharge machine designed to prevent an impactive high-speed motion generated upon actuation of an electrode actuator from propagating to a quill, as well as to enable the rapid retreat of a tool electrode by the electrode actuator to be performed efficiently. The tool electrode is attached to a quill through an elastic supporting element and a piezoelectric actuator, with the elastic supporting element disposed on the side of the quill. The elastic supporting element has an elasticity whose degree is set so as not to adversely affect normal positioning of the tool electrode, and the piezoelectric actuator facilitates rapid retreat of the tool electrode. A support body includes a counter weight having a weight large enough to absorb the component of the impactive high-speed motion of the electrode actuator which acts toward the quill.
| 1
|
TECHNICAL FIELD
[0001] The invention relates to the technical field of polymer materials, in particular to surface treatment composition, insulating fiber, yarn, rope and preparation methods thereof.
BACKGROUND
[0002] Currently, insulating ropes available at the market are mainly prepared by weaving and stranding silk or synthetic fiber. In the field of live working, given requirements for the insulation property and deformation of ropes, silk ropes and synthetic fiber ropes are mainly adopted. The damp-proof treatment of silk ropes and synthetic fiber ropes generally adopts physical attachment via damp-proof agents instead of chemical bond connection, so after being washed for certain times, the damp-proof performance of the ropes is reduced significantly, leading to a short service life. Furthermore, with erection of UHV transmission lines, the size and weight of various fittings on the transmission lines increase, while the fittings need to be lifted in the live working process; however, the strength of the existing silk ropes and synthetic fiber ropes cannot meet requirements of live working to some extent, and as a result, some working projects fail to proceed successfully.
[0003] Therefore, it is necessary to develop new insulation ropes for live working. Compared with the silk ropes and existing synthetic fiber ropes, the new insulation ropes should have better and more stable damp-proof performance, higher strength and better ultraviolet aging resistance. The novel high-strength, damp-proof and ultraviolet aging resistant insulation ropes can transfer large-tonnage stress of the live working items on a tower onto the ground, thereby reducing the labor intensity of operators on the tower and ensuring working safety. The successful development of the insulation ropes will bring the third revolution of UHV live working.
[0004] PBO fiber is a polyparaphenylene benzobisoxazole fiber whose fibrils are composed of PBO molecular chains orienting in the direction of the fiber axis with diameter between 10 and 50 nm and there are many capillary pores between the fibrils, which are connected to each other by means of cracks between the fibrils or openings of the fibrils.
[0005] PBO fiber has a perfect comprehensive performance, known as ultra-high performance fibers of the new era. Its tensile strength, monofilament strength of up to 5 Gpa, the tensile modulus of up to 300 Gpa, is twice that of the para-aramid fiber and 10 times that of the steel wire of the same diameter, and its density is only ⅕ of steel wire. The wear resistance on metal is better than that of aramid fiber, and the deformation coefficient is small, its thermal expansion coefficient is only −6 ppm/° C. The thermal degradation temperature in the air is about 650° C., and 700° C. in the nitrogen or argon gas environment, which is 100° C. higher than the aramid fiber; the limit of oxygen index of the PBO fiber is 68, highest among the polymers; it is smoldering even in open flame, so that it has self-flame retardancy. In addition, it has high impact resistance, and the energy needed to penetrate through its fabric is 2 times as much as that for penetrating Kevlar fiber. Therefore, PBO fiber is not only widely used in fields of national defense, aerospace and other advanced fields, but also can be widely applied to replace the conventional industrial production process and the upgrades of products with high temperature resistance, flame retardant, high performance, such as fiber reinforced material, high tensile strength such as rope or cable material, bridge cable, cable, sailing sailboat the operating lever and rowing with canvas, bullet-proof vests, nautical clothing, anti-high temperature & cut resistant gloves, high temperature and high pressure resistant gloves, PBO fiber composite materials are applied to aircrafts, space crafts, rocket outer structures and internal force bearing structures.
[0006] Given its excellent mechanical property and heat stability, BPO fiber becomes the first choice for insulation ropes for live working. Although PBO fiber has many advantages, there are still some serious drawbacks, such as PBO fiber is highly hydroscopic, and prone to deep fibrillation after damp, resulting in slip of PBO fibrils, and a sharp decline in mechanical properties; in addition, PBO fiber in the ultraviolet light irradiation can be prone to rapid aging phenomenon. The existence of these defects makes the PBO fiber rope's life shorter and cost higher, and severely limits its scope of application.
[0007] The surface treatment measures commonly used in the prior art is to deal with the PBO fiber with the help of a waterproofing agent and an ultraviolet absorber, or a shield agent. However, due to the absence of weak chemical bonds in the PBO molecular structure and a lack of the active groups, its surface is smooth and the free energy is low, making it difficult to connect with other functional groups, such as waterproofing group, anti-ultraviolet radiation group, etc. Therefore, these prior art methods have no obvious effects, and it is difficult to effectively solve the technical problems such as easy moisture absorption, decrease of strength and rapid aging in outdoor application.
SUMMARY
[0008] In order to solve the above technological problems, the invention aims to provide a surface treatment composition for insulating fiber, the insulating fiber obtained by surface treatment of the composition, and the preparation method thereof.
[0009] The invention also aims to provide an insulating yarn and an insulating rope prepared by the insulating fiber.
[0010] Based on the above purposes, the first aspect of the present invention provides a fiber surface treatment composition comprising a silane coupling agent, a polymer and a water-proofing agent, wherein the polymer is a copolymer of a polyurethane/polyacrylics, and the polyacrylics are selected from polyacrylic acid, polyacrylates or acrylic acid-acrylic ester copolymers.
[0011] In a preferred specific embodiment, the polymer may be a core-shell structure in which the core is a polyurethane and the shell is an polyacrylics.
[0012] In a preferred embodiment, when the polyacrylics are selected from polyacrylates or acrylic acid-acrylic ester copolymers, the alcohol forming the acrylic ester in the acrylate monomer is a straight chain alcohol having a carbon chain length of at least carbon atoms, for example, the acrylate monomer may be selected from at least one of octyl acrylate, decyl acrylate, and lauryl acrylate.
[0013] In a preferred embodiment, the polymer comprises nanoparticle having a particle size ranging from 5 to 200 nanometers.
[0014] In a preferred embodiment, the polymer may be in the form of a polymer suspension or a polymer emulsion, wherein the polymer forms dispersion particles.
[0015] In a preferred embodiment, the polyurethane is formed by polymerizing a diisocyanate monomer with a polyol, wherein the diisocyanate monomer may be selected from isophorone diisocyanate.
[0016] In a preferred embodiment, the silane coupling agent may be selected from the group consisting of KH series silane coupling agents, for example, at least one selected from KH550, KH560, KH570, and KH792.
[0017] In a preferred embodiment, the waterproofing agent may be selected from the group consisting of a perfluor C6 chain waterproofing agent and a perfluor C8 chain waterproofing agent.
[0018] In a preferred embodiment, the composition further comprises a cationic dye, which may be selected from at least one of C. I. Basic Yellow 24 and C. I. Basic Yellow 28.
[0019] The second aspect of the present invention provides an insulating fiber, wherein the insulating fiber has said composition adhered on the surface of the insulating fiber.
[0020] In a preferred embodiment, the insulating fiber is selected from polyparaphenylene benzobisoxazole (PBO) fiber.
[0021] In a preferred embodiment, the composition on the surface of the insulating fiber comprises 1 to 20% by weight of the insulating fiber.
[0022] In a preferred embodiment, the waterproofing agent on the surface of the insulating fiber comprises 1 to 18% by weight of the insulating fiber.
[0023] In a preferred embodiment, the cationic dyes on the insulating fiber comprises 0.001 to 0.002% by weight of the insulating fiber.
[0024] The third aspect of the present invention provides a method for preparing the insulating fiber as claimed in the second aspect of the present invention, including the steps as follows:
1) contacting the composition with a fiber to make the composition to be adhered to the surface of the fiber; and 2) baking the fiber to which the composition is attached.
[0027] The fiber may be polyparaphenylene benzobisoxazole (PBO) fiber.
[0028] In a preferred embodiment, the step of contacting comprises impregnating the fiber sequentially in the silane coupling agent, the polymer emulsion and the waterproofing agent.
[0029] In a preferred embodiment, the step of contacting comprises impregnating the fiber in a mixture of the silane coupling agent and the polymer emulsion, and then washing, drying and finally immersing the fiber in the waterproofing agent.
[0030] In a preferred embodiment, the step of contacting is carried out at a temperature of about 100 to 130° C. and for about 60 to 120 minutes.
[0031] In a preferred embodiment, the baking temperature is 180-250° C.
[0032] The fourth aspect of the present invention relates to an insulating yarn which can be made of the insulating fiber in the second aspect of the present invention through textile processing.
[0033] As an alternative, the insulating yarn may also be made by a method comprising the steps as follows:
1) processing a fiber into a yarn; 2) contacting the composition with the yarn to make the composition to be adhered to the surface of the yarn; and 3) baking the yarn to which the composition is adhered, to obtain the insulated yarn.
[0037] In a preferred embodiment, the fiber is polyparaphenylene benzobisoxazole (PBO) fiber.
[0038] The fifth aspect of the present invention relates to an insulating rope which can be made of the insulating yarn in the fourth aspect of the present invention.
[0039] In an alternative embodiment, the insulating rope can also be made through a method comprising the steps as follows:
1) processing the fiber into a yarn by weaving; 2) processing the yarn into a 12-strand loose primary rope; 3) contacting the 12-strand loose primary rope with the composition, so that the composition is adhered to the surface of the 12-strand loose primary rope; 4) baking the 12-strand loose primary rope to which the composition is attached, to obtain a 12-strand loose insulated primary rope; and 5) subjecting the 12-strand loose insulated primary rope to a shaping treatment, and wrapping it with the insulating yarn in the fourth aspect of the present invention to obtain the insulating rope.
[0045] In a preferred embodiment, the fiber is polyparaphenylene benzobisoxazole (PBO) fiber.
Technical Effect
[0046] The fiber surface treatment composition of the invention comprises a silane coupling agent, a polymer and a waterproofing agent, and the synergistic effect is produced by the interaction among them, which can effectively solve the technical problems in the prior art.
[0047] The specific functions of the individual components of the above compositions are described as follows:
Silane Coupling Agent:
[0000]
1) It can prevent the occurrence of fibrillation slip. PBO fiber due to its own chemical structure has the tendency to fibrillate, thus the use of silane coupling agent for its surface treatment can significantly reduce this trend. The —SiOH group formed by hydrolysis of the silane coupling agent can form chemical bonds with N atom and form hydrogen bonding with O atoms on the fiber to form cross-links between the microfibrils and prevent the fibrillation slip of the fibrils. This effect is conducive to maintaining strength.
2) It provides active sites for the attachment of the polymer to the surface of the fiber. Residual reactive groups such as —NH 2 , —OH, —OC 2 H 5 and the like after hydrolysis of the silane coupling agent can react with residues on the latex particles of the polymer emulsion, such as a carboxyl group, to form an amide bond, an ester bond, etc., thereby providing sites at which the polymer can be attached to the surface of the fiber.
Polymer:
[0000]
3) The polyurethane part of the polymer has good film-forming and coating property, and can play the role of physical protection and water barrier.
4) The polyacrylic acid moiety in the polymer or the anionic groups introduced on the fiber by the hydrolysis of polyacrylates, such as —COO − , is advantageous for the cationic waterproofing agent such as a perfluor C6 chain waterproofing agent and a perfluor C8 chain waterproofing agent being adsorbed or bonded thereto. This effect enhances the adhesion of the waterproofing agent to the fiber surface, and improves the washing resistance and the durability of the waterproofing performance of the fiber.
5) Due to the film forming and coverage of the polymer on the fiber surface, it can significantly change the refractive index and is conducive to increasing the reflection and refraction of UV light, thereby enhance the fiber's ability to resist UV.
Waterproofing Agent:
[0000]
6) The bonding rate and the binding amount of the weak cationic/cationic water repellent adhering to the surface of the fiber can be remarkably increased due to the presence of the anionic polymer on the fiber surface, thereby remarkably improving the water repellency of the fiber. In addition, the adhesion force between the waterproofing agent and the polymer is remarkably higher than that of the waterproofing agent and the surface in the prior art, thus the washing resistance of the fiber can be remarkably improved.
[0054] In a further preferred embodiment, the present invention also has the following advantages:
7) The polymer in the composition takes the form of a polymer emulsion which facilitates the stability of the polymer, prevents coagulation when mixed with other components, and facilitates the control of the particle size distribution. 8) Due to the large number of nano-pores between the PBO fibrils, nanometer-size polymer particles can effectively fill these pores, effectively increasing the contact area between the polymer and PBO fibrils. 9) Since the waterproofing agent is bonded to the acrylic group of the polymer so that the water repellent molecules are sandwiched between the side chains of the acrylate segments, and when the side chains are above C8, it can advantageously improve the water repellent capacity of the waterproofing agent, in particular, can remarkably improve the water repellency of the perfluor C6 chain waterproofing agent.
[0058] Waterproofing agents commonly used in the art are perfluor C6 chain waterproofing agent and perfluor C8 chain waterproofing agent, wherein the water repellency of the former one is lower than that of the later one. However, PFOS (perfluorooctane sulfonyl compounds) and PFOA (perfluorooctanoic acid) are produced by perfluor C8 chain waterproofing agent and the European Union has completely banned the use of chemicals containing PFOS and PFOA, so the use of the perfluor C8 chain waterproofing agent has been greatly limited. The invention can improve the water repellency of the perfluor C6 chain waterproofing agent by clamping the waterproofing molecules with at least C8 side chains on the polymer so as to effectively replace the perfluor C8 chain waterproofing agent by using the perfluor C6 chain waterproofing agent.
10) Polyurethane synthesized from isophorone diisocyanate and polyol has excellent resistance to ultraviolet radiation, which is conducive to preventing fiber ultraviolet aging. 11) The coverage of fiber yarn on 12-strand loose primary fiber rope can further enhance the wear resistance and moisture resistance of insulating rope.
[0061] The present invention overcomes the drawbacks of the prior art and provides a fiber surface treatment composition capable of remarkably improving the moisture resistance and UV resistance of the fiber, and the insulating fiber obtained by the surface treatment of the composition. The invention can be applied to the large scale industrial process to produce qualified products, and thoroughly breaks through the previous technical dilemma and barriers. The damp-proof insulating rope made by the PBO fiber is easy to store and transport and safe to use, and is a high-strength insulation rope for live working capable of being used in high-humidity environment.
[0062] The key technical principle of the invention is that through waterproof treatment on the fiber, strength reduction caused by relative slippage of fibril after fiber absorbing water molecules is prevented; by anionic coating and shielding on fiber surfaces through the mixed conditioning fluid, the refractive index can be changed; after adding a tiny amount of high light-resistant cationic dyes to absorb and transfer ultraviolet light energy, the anti-ultraviolet performance of BPO fiber is improved.
[0063] The preparation method has the advantages of having a simple process and operation convenience. The insulated wire obtained in this way can be greatly improved in strength, moisture resistance, UV resistance, and the like, and can be suitable for large-scale industrial production.
DETAILED DESCRIPTION
[0064] In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be described in more detail with reference to specific embodiments.
EXAMPLE 1
Preparation of Aqueous Polyurethane/Polyacrylic Acid-Octyl Acrylate Nanoemulsion
[0065] Adding 50 g of polyethylene glycol into a 3-mouth flask, removing water by extraction filtration for 2 h at 110° C., then cooling to 80° C., adding 100 g of isophorone diisocyanate, pumping with nitrogen, and stirring at constant temperature for 2 h; cooling to 70° C., adding 9 g of dimethylolpropionic acid, 1.5 g of trimethylolpropane, 300 ml of solvents of N-methyl-2-pyrrolidinone and acetone, and appropriate amount of catalyst of dibutyltin dilaurate, heating to 80° C. to react for 7 h, stopping nitrogen, cooling to 60-65° C., adding triethylamine for terminating, keeping constant temperature for 4 h, cooling to 50° C. and adding triethylamine for neutralization for 20 min; adding distilled water to stir and emulsify for 2-3 h at room temperature to obtain milky white semitransparent emulsion; removing acetone by extraction filtration at 65° C. for 1-2 h, and then adding equivalent of deionized water to stir for 10 min; heating to 80-85° C. in the condition of stirring and nitrogen, slowly dripping 10 g of acrylic acid, 20 g of octyl acrylate monomer and initiator of azobisisobutyronitrile (total for about 2 h), keeping constant temperature for 4 h, then cooling to 50-60° C., adding emulsifiers Span 80 and Tween 80 for stirring and emulsifying, till the emulsion is blue transparent, discharging to obtain waterborne polyurethane/polyacrylic acid-octyl acrylate nano-emulsion, with particle size distributed in a range of 50-100 nanometers.
EXAMPLE 2
Preparation of Aqueous Polyurethane/Polyacrylic Acid-Decyl Acrylate Nanoemulsion
[0066] Adding 50 g of polyethylene glycol into a 3-mouth flask, removing water for 2 h at 110° C., then cooling to 80° C., adding 100 g of isophorone diisocyanate, pumping with nitrogen, and stirring at constant temperature for 2 h; cooling to 70° C., adding 9 g of dimethylolpropionic acid, 1.5 g of trimethylolpropane, 300 ml of solvents of N-methyl-2-pyrrolidinone and acetone, and appropriate amount of catalyst of dibutyltin dilaurate, heating to 80° C. to react for 7 h, stopping nitrogen, cooling to 60-65° C., and adding triethylamine for terminating, keeping constant temperature for 4 h, cooling to 50° C., and adding triethylamine for neutralization for 20 min; adding distilled water to stir and emulsify for 2-3 h at room temperature to obtain milky white semitransparent emulsion; removing acetone by extraction filtration at 65° C. for 1-2 h, and then adding equivalent of deionized water to stir for 10 min; heating to 80-85° C. in the condition of stirring and nitrogen, slowly dripping 10 g of acrylic acid, 20 g of acrylate monomer and initiator of azobisisobutyronitrile (total for about 2 h), keeping constant temperature for 4 h, then cooling to 50-60° C., adding emulsifiers of Span 80 and Tween 80 for stirring and emulsifying, till the emulsion is blue transparent, discharging to obtain waterborne polyurethane/polyacrylic acid-decyl acrylate nanoemulsion, with particle size distributed in a range of 30-100 nanometers.
EXAMPLE 3
Preparation of aqueous polyurethane/polyacrylic acid nanoemulsion
[0067] Adding 45 g of polyethylene glycol into a 3-mouth flask, filtering water for 2.5 h at 120° C., then cooling to 78° C., adding 95 g of isophorone diisocyanate, pumping with nitrogen, and stirring at constant temperature for 1.8 h; cooling to 72° C., adding 9 g of dimethylolpropionic acid, 1.8 g of trimethylolpropane, 280 ml of solvents of N-methyl-2-pyrrolidinone and acetone, and appropriate amount of catalyst of dibutyltin dilaurate, heating to 75° C. to react for 6.5 h, stopping nitrogen, cooling to 60-65° C., adding triethylamine for terminating, keeping constant temperature for 5 h, cooling to 45° C., and adding triethylamine for neutralization for 20 min; adding distilled water to stir and emulsify for 1-2.5 h at room temperature to obtain milky white semitransparent emulsion; removing acetone by extraction filtration at 62° C. for 1-2 h, and then adding equivalent of deionized water to stir for 15 min; heating to 82-88° C. in the condition of stirring and filling in nitrogen, slowly dripping 32 g of acrylic acid monomer (total for about 2.5 h), keeping constant temperature for 5 h, then cooling to 50-55° C., adding emulsifiers of Span 80 and Tween 80 for stirring and emulsifying, till the emulsion is blue transparent, discharging to obtain the waterborne polyurethane/poly acrylic acid nanoemulsion, with particle size distributed in a range of 5-100 nanometers.
EXAMPLE 4
Preparation of Aqueous Polyurethane/Poly(Lauryl Acrylate) Nanoemulsion
[0068] Adding 55 g of polyethylene glycol into a 3-mouth flask, removing water for 1.8 h at 105° C., then cooling to 83° C., adding 105 g of isophorone diisocyanate, pumping with nitrogen, and stirring at constant temperature for 2.5 h; cooling to 65° C., adding 10 g of dimethylolpropionic acid, 1.6 g of trimethylolpropane, 350 ml of solvents of N-methyl-2-pyrrolidinone and acetone, and appropriate amount of catalyst of dibutyltin dilaurate, heating to 82° C. to react for 7.2 h, stopping nitrogen, cooling to 60-65° C., adding triethylamine for terminating, keeping constant temperature for 3.5 h, cooling to 53° C., and adding triethylamine for neutralization for 25 min; adding distilled water to stir and emulsify for 2-2.5 h at room temperature to obtain milky white semitransparent emulsion; removing acetone by extraction filtration at 68° C. for 1.5-2 h, and then adding equivalent of deionized water to stir for 8 min; heating to 85-90° C. in the condition of stirring and nitrogen, slowly dripping 28 g of lauryl acrylate monomer and initiator of azobisisobutyronitrile (total for about 2 h), keeping constant temperature for 3.5 h, then cooling to 53-60° C., adding emulsifiers Span 80 and Tween 80 for stirring and emulsifying, till the emulsion is blue transparent, discharging to obtain the waterborne polyurethane/polyacrylates nanoemulsion, with particle size distributed in a range of 20-200 nanometers.
EXAMPLE 5
Preparation of a Moisture-Proofing and Fast-Drying PBO Insulating Fiber
[0000]
1) Evenly mixing 5 kg of aqueous polyurethane/polyacrylic acid-octyl acrylate octyl emulsion and 15 kg of silane coupling agent KH 792 to prepare a mixed conditioning fluid, and soaking 200 kg of PBO fiber into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 125° C., and the treatment time is 35 min.
2) Taking out the PBO fiber from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO fiber into 10 kg of perfluor C8 chain waterproofing agents (TG-581), and adding 4 g of C.I.Basic Yellow 28 in the perfluor C8 chain waterproofing agent, wherein the temperature of the perfluor C8 chain waterproofing agent is controlled at 110° C., and the treatment time is 50 min.
4) Baking the waterproof treated PBO fiber at a high temperature to obtain the insulating PBO fiber, wherein the temperature is controlled at 220° C.
EXAMPLE 6
Preparation of Moisture-Proofing and Quick-Drying PBO Insulation Yarn and Insulating Rope
[0072] The PBO insulating fiber in example 5 is subjected to a textile processing to form the PBO insulating yarn by stranding and twisting.
[0073] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 2.43%, after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below the water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 12.50%.
EXAMPLE 7
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Yarn and Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare the PBO yarn.
2) Evenly mixing 1.5 kg of waterborne polyurethane/polyacrylic acid-octyl acrylate nano-emulsion prepared in example 1, with 2 kg of silane coupling agent KH 550 and 1 kg of Silane coupling agent KH 570 to prepare the mixed conditioning fluid, and soaking 150 kg of PBO yarn into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 115° C., and the treatment time of PBO yarn is 52 min.
3) Taking out the PBO yarn from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO yarn into 22.5 kg of perfluor C6 chain waterproofing agent (TG-5521), and adding 1.95 g of C.I.Basic Yellow 24 in the perfluor C6 chain waterproofing agent, wherein the temperature of the perfluor C6 chain waterproofing agent is controlled at 118° C. and the treatment time is 36 min.
4) Baking the waterproof treated PBO yarn at a high temperature to obtain the insulating yarn, wherein the temperature is controlled at 222° C.
[0078] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope.
[0079] The moisture absorption rate of the insulated ropes is 1.21% after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below the water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 10.25%.
EXAMPLE 8
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Yarn and Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare the PBO yarn.
2) Evenly mixing 1 kg of waterborne polyurethane/polyacrylic acid-decyl acrylate nano-emulsion prepared in example 2, with 10 kg of silane coupling agents KH 550 to prepare the mixed conditioning fluid, and soaking 110 kg of PBO yarn into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 120° C. and the treatment time of PBO yarn is 40 min.
3) Taking out the PBO yarn from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO yarn into 12 kg of perfluor C6 chain waterproofing agent (TG-5521), and adding 1.32 g of C.I.Basic Yellow 24 in the perfluor C6 chain waterproofing agent, wherein the temperature of the perfluor C6 chain waterproofing agent is controlled at 130° C. and the treatment time is 45 min.
4) Baking the waterproof treated PBO yarn at a high temperature to obtain the insulating yarn, wherein the temperature is controlled at 200° C.
[0084] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 1.15%, after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below the water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 8.21%.
Embodiment 9
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Yarn and Insulating Rope
[0000]
1) Stranding and twisting the fiber to prepare the PBO yarn.
2) Evenly mixing 7 kg of waterborne polyurethane/polyacrylic acid nano-emulsion prepared in example 3, with 20 kg of silane coupling agents KH 560 to prepare the mixed conditioning fluid, and soaking 150 kg of PBO yarn into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 105° C., and the treatment time of the PBO yarn is 60 min.
3) Taking out the PBO yarn from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO yarn into 7.5 kg of perfluor C6 chain waterproofing agent (TG-5521), and adding 1.5 g of C.I.Basic Yellow 24 and 0.6 g C.I.Basic Yellow 28 in the perfluor C6 chain waterproofing agent, wherein the temperature of the perfluor C6 chain waterproofing agent is controlled at 102° C., and the treatment time is 55 min.
4) Baking the waterproof treated PBO yarn at a high temperature to obtain the insulating PBO yarn, wherein the temperature is controlled at 250° C.
[0089] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 1.56%, after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below the water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 8.4%.
Embodiment 10
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Yarn and Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare the PBO yarn.
2) Evenly mixing 2 kg of waterborne polyurethane/poly(lauryl acrylate) nano-emulsion prepared in example 4, with 2 kg of silane coupling agent KH 550 and 2kg of silane coupling agent KH 560 to prepare the mixed conditioning fluid, and soaking 50 kg of PBO yarn into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 116° C., and the treatment time of PBO yarn is 41 min.
3) Taking out the PBO yarn from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO yarn into 2.5 kg of perfluor C6 chain waterproofing agent (TG-5521), and adding 0.8 g of C.I.Basic Yellow 24 in the perfluor C6 chain waterproofing agent, wherein the temperature of the perfluor C6 chain waterproofing agents is controlled at 128° C., and the treatment time is 45 min.
4) Baking the waterproof treated PBO yarn at a high temperature to obtain the PBO insulating yarn, wherein the temperature is controlled at 180° C.
[0094] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulated rope is 1.41% after being washed for 10 times and immersed for 15 minutes at 10˜20 cm below the water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 7.83%.
Embodiment 11
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Yarn and Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare the PBO yarn.
2) Evenly mixing 5 kg of waterborne polyurethane/polyacrylic acid-octyl acrylate nano-emulsion prepared in example 1 with 15 kg of silane coupling agent KH 792 to prepare the mixed conditioning fluid, and soaking 200 kg of PBO yarn into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 125° C., and the treatment time of PBO yarn is 35 min.
3) Taking out the PBO yarn from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO yarn into 10 kg of perfluor C8 chain waterproofing agent (TG-581), and adding 4 g of C.I.Basic Yellow 28 in the perfluor C8 chain waterproofing agent, wherein the temperature of the perfluor C8 chain waterproofing agent is controlled at 100° C., and the treatment time is 50 min.
4) Baking the waterproof treated PBO yarn at a high temperature to obtain the PBO insulating yarn, wherein the temperature is controlled at 220° C.
[0099] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 1.15% after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below water surface; when the harsh condition of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 8.21%.
Embodiment 12
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Yarn and Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare the PBO yarn.
2) Evenly mixing 10 kg of waterborne polyurethane/polyacrylic acid nano-emulsion prepared in example 3 with 44 kg of silane coupling agent KH 550 to prepare the mixed conditioning fluid, and soaking 300 kg of PBO yarn into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 118° C., and the treatment time of PBO yarn is 45 min.
3) Taking out the PBO yarn from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO yarn in 24 kg of perfluor C8 chain waterproofing agent (TG-581), wherein the temperature of the perfluor C8 chain waterproofing agent is controlled at 114° C., and the treatment time is 52 min.
4) Baking the waterproof treated PBO yarn at a high temperature to obtain the PBO insulating yarn, wherein the temperature is controlled at 220° C.
[0104] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 1.42%, after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 10.18%.
Embodiment 13
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Yarn and Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare the PBO yarn.
2) Evenly mixing 1.5 kg of waterborne polyurethane/polyacrylic acid-decyl acrylate copolymer nano-emulsion prepared in example 2 with 2 kg of silane coupling agent KH 550 and 1 kg silane coupling agent KH 570 to prepare the mixed conditioning fluid, and soaking 150 kg of PBO yarn into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 115° C., and the treatment time of PBO yarn is 52 min.
3) Taking out the PBO yarn from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO yarn in 22.5 kg of perfluor C8 chain waterproofing agent (TG-581), and adding 1.95 g of C.I.Basic Yellow 24 in the perfluor C8 chain waterproofing agent, wherein the temperature of the perfluor C8 chain waterproofing agent is controlled at 118° C., and the treatment time is 36 min.
4) Baking the waterproof treated PBO yarn at a high temperature to obtain the PBO insulating yarn, wherein the temperature is controlled at 225° C.
[0109] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 1.18%, after being washed for 10 times and immersed for 15 minutes at 10˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 8.33%.
EXAMPLE 14
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Yarn and Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare the PBO yarn.
2) Evenly mixing 2 kg of waterborne polyurethane/poly(lauryl Alcrylate) nano-emulsion prepared in example 4 with 7.6 kg of silane coupling agent KH 792 to prepare the mixed conditioning fluid, and soaking 80 kg of PBO yarn into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 112° C., and the treatment time of PBO yarn is 38 min.
3) Taking out the PBO yarn from the mixed conditioning fluid, washing with water and then drying it; soaking the PBO yarn in 4 kg of perfluor C8 chain waterproofing agent (TG-581), and adding 1.04 g of C.I.Basic Yellow 28 in the perfluor C8 chain waterproofing agent, wherein the temperature of the perfluor C8 chain waterproofing agent is controlled at 122° C., and the treatment time is 48 min.
4) Baking the waterproof treated PBO yarn at a high temperature to obtain the PBO insulating yarn, wherein the temperature is controlled at 192° C. and the insulating PBO yarn is obtained;
[0114] The PBO insulating yarn is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 1.37% after being washed for 10 times and immersed for 15 minutes at 10˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 8.21%.
EXAMPLE 15
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare a 12-strand loose primary PBO fiber rope.
2) Evenly mixing 0.5 kg of waterborne polyurethane/polyacrylic acid-octyl acrylate copolymer nano-emulsion prepared in example 1 with 1.5 kg of silane coupling agent KH 792 to prepare the mixed conditioning fluid, and soaking 200 kg of the 12-strand loose primary PBO fiber rope into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 100° C., and the treatment time is 60 min.
3) Taking out the 12 strand loose primary PBO fiber rope from the mixed conditioning fluid, washing with water and then drying it; soaking the 12-strand loose primary PBO fiber rope into 6 kg of perfluor C6 chain waterproofing agents, and adding 2 g of C.I.Basic Yellow 28 into the perfluor C6 chain waterproofing agent, wherein the temperature of the perfluor C6 chain waterproofing agent is controlled at 128° C., and the treatment time is 30 min.
4) Baking the waterproof treated 12-strand loose primary PBO fiber rope at a high temperature to obtain the 12-strand loose primary PBO fiber insulating rope, wherein the temperature is controlled at 182° C.
5) After stabilized finish of the 12 strand loose primary PBO fiber rope, the rope is wrapped by the fiber yarn prepared in example 9 to obtain the final insulating rope.
[0120] The moisture absorption rate of the PBO fiber insulating rope is 1.08% after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 5.14%.
EXAMPLE 16
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare a 12 strand loose primary PBO fiber rope.
2) Evenly mixing 0.5 kg of waterborne polyurethane/polyacrylic acid-decyl acrylate nano-emulsion prepared in example 2 with 14 kg of silane coupling agent KH 792 and 10kg of silane coupling agent KH 70 to prepare the mixed conditioning fluid, and soaking 160 kg of the 12-strand loose primary PBO fiber rope into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 105° C., and the treatment time is 52 min.
3) Taking out the 12-strand loose primary PBO fiber rope from the mixed conditioning fluid, washing with water and then drying it; soaking the 12-strand loose primary PBO fiber rope into 17.6 kg of perfluor C6 chain waterproofing agent, and adding 1.6 g of C.I.Basic Yellow 24 into the perfluor C6 chain waterproofing agent, wherein the temperature of the perfluor C6 chain waterproofing agent is controlled at 130° C., and the treatment time is 44 min.
4) Baking the waterproof treated 12-strand loose primary PBO fiber rope at a high temperature to obtain the 12-strand loose primary PBO fiber insulating rope, wherein the temperature is controlled at 180° C.
5) After stabilized finish of the 12-strand loose primary PBO fiber rope, the rope is wrapped by fiber yarn prepared in example 10 to obtain the final insulating rope.
[0126] The moisture absorption rate of the PBO fiber insulating rope is 1.22%, after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 8.06%.
EXAMPLE 17
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare a 12-strand loose primary PBO fiber rope.
2) Evenly mixing 0.5 kg of waterborne polyurethane/polyacrylic acid nano-emulsion prepared in example 3 with 4 kg of silane coupling agent KH 570 to prepare the mixed conditioning fluid, and soaking 90 kg of the 12-strand loose primary PBO fiber rope into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 125° C., and the treatment time is 58 min.
3) Taking out the 12-strand loose primary PBO fiber rope from the mixed conditioning fluid, washing with water and then drying it; soaking the 12-strand loose primary PBO fiber rope into 7.2 kg of perfluor C6 chain waterproofing agents, and adding 0.32 g of C.I.Basic Yellow 28 into the perfluor C6 chain waterproofing agents, wherein the temperature of the perfluor C6 chain waterproofing agents is controlled at 122° C., and the treatment time is 41 min.
4) Baking the waterproof treated 12-strand loose primary PBO fiber rope at a high temperature to obtain the 12-strand loose primary PBO fiber insulating rope, wherein the temperature is controlled at 250° C.
5) After stabilized finish of the 12-strand loose primary PBO fiber rope, the rope is wrapped by fiber yarn prepared in example 11 to obtain the final insulating rope.
[0132] The moisture absorption rate of the PBO fiber insulating rope is 1.17% after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 4.88%.
EXAMPLE 18
Preparation of Moisture-Proofing and Quick-Drying PBO Insulating Rope
[0000]
1) Stranding and twisting the PBO fiber to prepare a 12-strand loose primary PBO fiber rope.
2) Evenly mixing 0.8 kg of waterborne polyurethane/poly (lauryl Alcrylate) nano-emulsion prepared in example 4 with 1.9 kg of silane coupling agent KH 5670 to prepare the mixed conditioning fluid, and soaking 90 kg of the 12-strand loose primary PBO fiber rope into the mixed conditioning fluid, wherein the temperature of the mixed conditioning fluid is controlled at 112° C., and the treatment time is 52 min.
3) Taking out the 12-strand loose primary PBO fiber rope from the mixed conditioning fluid, washing with water and then drying it; soaking the 12-strand loose primary PBO fiber rope into 16 kg of perfluor C6 chain waterproofing agent, and adding 1.53 g of C.I.Basic Yellow 24 into the perfluor C6 chain waterproofing agent, wherein the temperature of the perfluor C6 chain waterproofing agents is controlled at 110° C., and the treatment time is 45 min.
4) Baking the waterproof treated 12-strand loose primary PBO fiber rope at a high temperature to obtain the 12-strand loose primary PBO fiber insulating rope, wherein the temperature is controlled at 222° C.
5) After stabilized finish of the 12-strand loose primary PBO fiber rope, the rope is wrapped by fiber yarn prepared in example 11 to obtain the final insulating rope.
[0138] The moisture absorption rate of the PBO fiber insulating rope is 1.30% after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 3.3%.
Comparative Example 1
[0000]
1) Stranding and twisting the PBO filament to prepare a PBO line.
2) Washing 80 kg of the PBO lines with water and then drying it; soaking the PBO line into 4 kg of perfluor C8 chain waterproofing agent, wherein the temperature of the perfluor C8 chain waterproofing agent is controlled at 122° C., and the treatment time is 48 min.
3) Baking the waterproof treated PBO line at a high temperature, wherein the temperature is controlled at 192° C.
[0142] The PBO line is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 10.37% after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 35.89%.
Comparative Example 2
[0000]
1) Stranding and twisting the PBO filament to prepare a PBO line.
2) Washing 80 kg of the PBO line with water and then drying it; soaking the PBO line into 4 kg of perfluor C6 chain waterproofing agent, wherein the temperature of the perfluor C6 chain waterproofing agent is controlled at 122° C. and the treatment time is 48 min.
3) Baking the waterproof treated PBO fiber line at a high temperature, wherein the temperature is controlled at 192° C.
[0146] The PBO line is subjected to further processing such as weaving to obtain an insulating rope. The moisture absorption rate of the insulating rope is 13.76% after being washed for 10 times and immersed for 15 minutes at 15˜20 cm below water surface; when the harsh conditions of environment temperature at 30° C., relative humidity at 85%, ultraviolet wavelength at 340 nm and the irradiation smaller than or equal to 50 W/m 2 are simulated and kept for 150 h, the result of the accelerated aging test is that the tensile strength is reduced by 23.21%.
[0147] In summary, the PBO insulation ropes treated with the fiber surface treatment composition of the present invention are significantly improved in water repellency after repeated laundering and anti-aging performance, compared with the PBO insulated ropes treated with the water repellant only of the comparative examples. Thus, the fiber surface treatment composition of the present invention has an unexpected technical effect on improving the water repellency, the ultraviolet resistance and the aging resistance of the fiber. The insulation fiber and the insulation ropes which are surface-treated by the composition thoroughly break through the predicament and the barrier of the existing technology, and their storage and transportation is more peace of mind, long-term use more secure, and can be used for a long time in live working under high humidity environment.
[0148] Those skilled in the field should understand that the discussion on any above embodiment is illustrative instead of implying that the scope (including claims) of the invention is limited to these examples; based on the idea of the invention, the technical characteristics of the above embodiments or different embodiments can be combined, the steps can appear according to any sequence, and there shall be many variants of different aspects of the invention as described above, which however are not provided in details for the purpose of conciseness. Therefore, any omission, modification, equivalent replacement and improvement within the sprit and principle of the invention shall be included in the protection scope of the invention.
|
The present invention discloses a fiber surface treatment composition, characterized in that the composition is comprised of a silane coupling agent, a polymer and a water repellent agent, wherein the polymer is a copolymer of a polyurethane/acrylic acid polymer, wherein the acrylic polymer is selected from the group consisting of polyacrylic acid, polyacrylates or acrylic acid-acrylic acid ester copolymers. The invention also discloses an insulating fiber having the composition on its surface, the preparation method for it, and an insulating yarn and an insulated cord. The insulated fibers, yarns and ropes of the invention have the advantages of moisture resistance, washing resistance, ultraviolet aging resistance and the like. Particularly, the insulated ropes can be applied to the charging work of transmission lines, especially the UHV transmission lines.
| 3
|
FIELD OF THE INVENTION
[0001] The present invention relates to apparatus for use on unmanned vehicles.
BACKGROUND
[0002] Unmanned aircraft are powered aerial vehicles that do not carry a human operator. They may fly autonomously or be piloted remotely.
[0003] A data link employed to facilitate communication between an unmanned aircraft and its operator, e.g. a satellite data-link, may have uncertain performance, availability, and integrity.
[0004] In manned armed aircraft, the weapon control is typically performed by the airborne operator. The airborne operator interprets relevant Rules of Engagement to ensure weapons release is authorised. Typically, the weapon is released using a control sequence to release a series of electro-mechanical safety critical switches. The control sequence is usually performed on the aircraft. The data-link employed within a manned aircraft for the control of the weapon systems is typically robust, reliable, and of high integrity relative to a data link used for communication between an unmanned aircraft and its operator.
SUMMARY OF THE INVENTION
[0005] In a first aspect, the present invention provides a method performed by apparatus, the apparatus being mounted on an unmanned vehicle and arranged to act upon a payload, the payload being mounted on the unmanned vehicle and, under an action of the apparatus, able to be activated, the method comprising receiving an activation instruction from an entity, the entity being remote from the unmanned vehicle, determining whether or not the received activation instruction is valid by performing a validation process, and in response to determining that the received activation instruction is valid, activating the payload.
[0006] The method may further comprise, in response to determining that the received activation instruction is not valid, preventing or opposing the activation of the payload.
[0007] The apparatus may comprise, or has access to, validation information, and the validation process may comprise comparing the received activation instruction to the validation information.
[0008] The activation instruction may comprise a code, and the validation information may be a further code, the further code being stored in the apparatus.
[0009] The activation instruction may comprise an indication of a time that the activation instruction was sent from the entity to the unmanned vehicle, and the validation process may comprise determining that the activation instruction is not valid if a time period between the indicated time and a time that the validation process is performed is longer than a pre-determined threshold.
[0010] The apparatus and the entity may each comprise multiple codes, each code being related to a payload activation event. Once completed, information pertaining to each payload activation event may be stored in the apparatus. The information may comprise valid, actioned codes. An event history may, thus, be generated and the next anticipated code may readily be identified. Time synchronisation data may be provided to and stored in each of the entity and the apparatus. Time synchronisation data may be used in combination with the event history to enable system re-synchronisation to be performed. System re-synchronisation may be required following a period of degradation in data communications between the apparatus and the entity, for example a UAV and its ground station.
[0011] The activation instruction may comprise an indication of the next anticipated valid code. The validation process may comprise comparing the received anticipated code with the corresponding code stored in the apparatus.
[0012] The method may further comprise receiving target details from a further entity, the further entity being remote from the unmanned vehicle, and, using the received target details, facilitating a payload controller to direct the payload towards the target.
[0013] The further entity may be the entity.
[0014] The method may further comprise measuring a parameter of an area of terrain, the area of terrain comprising a target, and providing, for use by the entity, the measurements of the parameter.
[0015] The step of measuring may be performed using at least one of a visible light detecting camera, an infra-red camera, a ultra-violet camera or a radar sensor.
[0016] The method may further comprise, in response to activating the payload, providing for the entity an indication that the payload has been activated.
[0017] The unmanned vehicle may be an aircraft.
[0018] The payload may be a weapon.
[0019] The method may further comprise, if in response to activating the payload the payload fails to be activated, providing for use by the entity an indication that the payload has failed to be activated.
[0020] In a further aspect, the present invention provides apparatus mounted on an unmanned vehicle and arranged to act upon a payload, the payload being mounted on the unmanned vehicle and, under an action of the apparatus, able to be activated, the apparatus being arranged to receive an activation instruction from an entity, the entity being remote from the unmanned vehicle, determine whether or not the received activation instruction is valid by performing a validation process, and, in response to determining that the received activation instruction is valid, activate the payload.
[0021] In a further aspect, the present invention provides a program or plurality of programs arranged such that when executed by a computer system or one or more processors it/they cause the computer system or the one or more processors to operate in accordance with the method of any of the above aspects.
[0022] In a further aspect, the present invention provides a machine readable storage medium storing a program or at least one of the plurality of programs according to the above aspect.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] FIG. 1 is a schematic illustration (not to scale) of an example scenario in which an aircraft implements an embodiment of an aircraft weapon system;
[0024] FIG. 2 is a schematic illustration (not to scale) of the aircraft;
[0025] FIG. 3 is a schematic illustration (not to scale) of an embodiment of the weapon system of the aircraft; and
[0026] FIG. 4 is a process flow chart showing certain steps of a process for implementing the weapons system to attack the target.
DETAILED DESCRIPTION
[0027] FIG. 1 is a schematic illustration (not to scale) of an example scenario in which an aircraft 2 implements an embodiment of an aircraft weapon system.
[0028] In this scenario, the aircraft 2 is an unmanned aircraft (UAV).
[0029] In this scenario, the aircraft 2 has been launched under the control of a ground station 4 .
[0030] In this scenario, the ground station 4 is located on the ground 6 .
[0031] FIG. 1 shows the aircraft 2 airborne (i.e. after its launch from the ground 6 ).
[0032] In this scenario, the aircraft 2 is launched under the control of the ground station 4 with an intention of attacking (using a weapon launched from the aircraft 2 as described in more detail later below) a target 8 .
[0033] In this embodiment, the aircraft 2 follows a pre-programmed navigation route. The aircraft 2 does not deviate from this route unless the aircraft 2 is commanded to “loiter” by the ground station 4 , the aircraft is commanded to “return” by the ground station, or the aircraft 2 experiences a communications failure (in which case the aircraft 2 returns to the ground 6 ).
[0034] In this scenario, the target 8 is located on the ground 6 . Also, the target 8 is located at a position on the ground 6 that is remote from the ground station 4 .
[0035] In this scenario, the aircraft 2 and the ground station 4 are in two-way communications. The aircraft 2 and the ground station 4 communicate via a communications satellite, hereinafter referred to as “the satellite 10 ”. The two-way communication of the aircraft 2 and the ground station 4 is represented in FIG. 1 by dotted two-headed arrows. Also, the two-way communication of the aircraft 2 and the ground station 4 is described in more detail later below with reference to FIG. 4 .
[0036] FIG. 2 is a schematic illustration (not to scale) of the aircraft 2 .
[0037] In this example, the aircraft 2 comprises a transceiver 12 and a weapon system 14 .
[0038] In this example, messages received by the aircraft 2 from the ground station 4 (via the satellite 10 ) are received by the transceiver 12 . Furthermore, in this embodiment messages sent by the aircraft 2 to the ground station 4 (via the satellite 10 ) are sent by the transceiver 12 .
[0039] In this example, the transceiver 12 is connected to the weapon system 14 such that messages received at the transceiver 12 from the ground station 4 (via the satellite 10 ) are sent from the transceiver 12 to the weapon system 14 . Furthermore, the transceiver 12 is connected to the weapon system 14 such that messages may be sent from the weapon system 14 to the transceiver, which may then be sent from the transceiver 12 to the ground station 4 (via the satellite 10 ).
[0040] In this embodiment, the aircraft 2 comprises an Armament Control Safety Break (not shown in the Figures) which provides an additional safety interlock whilst the aircraft 2 is on the ground 6 .
[0041] FIG. 3 is a schematic illustration (not to scale) of an embodiment of the weapon system 14 of the aircraft 2 .
[0042] In this embodiment, the weapon system 14 comprises a sequencer 16 and a weapon 18 .
[0043] In this embodiment, the sequencer 16 is fitted in the aircraft such that, when certain criteria are satisfied (i.e. when certain messages have been received by the aircraft 2 from the ground station 4 ) the sequencer 16 controls the power, pre-launch, and firing commands to the weapon 18 .
[0044] The sequencer 16 is connected to the weapon 18 such that the weapon 18 can be powered and controlled by the sequencer 16 .
[0045] In this embodiment, prior to the launch of the aircraft 2 (i.e. prior to the aircraft 2 taking off from the ground 6 ) a pre-determined “firing code” is stored in the sequencer 16 , e.g. by hardwiring the code into a storage device which is connected to a port on the sequencer 16 . The same code is also stored in a further storage device which is kept by mission crew at the ground station 4 . This firing code is used to initiate the firing of a weapon from the aircraft 2 as described in more detail later below with reference to FIG. 4 .
[0046] Alternatively, the firing code could by synchronised between the ground station 4 and the sequencer 16 by transmitting the firing code via the satellite 10 , whilst the aircraft 2 is on the ground.
[0047] In this example, the ground station 4 and the sequencer 16 are time synchronised using an incrementing time code, transmitted with the firing code from the ground via the satellite 10 and the transceiver 12 . The firing code should comprise sufficient digits to satisfy the safety requirements of the system.
[0048] A new/different firing code is used for each new aircraft sortie.
[0049] Multiple firing codes may be stored in the sequencer 16 to enable many different events to be instructed by the ground station 4 within a single sortie. The multiple firing codes may be transmitted from the ground station 4 via the satellite 10 and transceiver and stored in the sequencer 16 .
[0050] The process by which the sequencer 16 powers, controls and fires the weapon 18 is described in more detail later below with reference to FIG. 4 .
[0051] In this embodiment, the weapon 18 is a relatively lightweight, precision strike, low collateral damage weapon. However, in other embodiments the weapon is a different type of weapon, or other type of payload. For example, in other embodiments, the weapon is a different type of lethal effector, such as an unpowered laser guided bomb. In other embodiments, the weapon may use any appropriate method to be guided to the target, e.g. a beam rider method, or the weapon may detect reflected laser light on the ground and steer towards that. In other embodiments the payload may be a non-lethal effector, e.g. a communications jamming device, a locator beacon, or equipment for friendly ground-based troops.
[0052] FIG. 4 is a process flow chart showing certain steps of a process for implementing the weapons system 14 to attack the target 8 .
[0053] In this embodiment, the aircraft 2 is airborne following its launch from the ground 6 , as described above with reference to FIG. 1 .
[0054] At step s 2 , as the aircraft 2 flies above the ground 6 , images of the ground 6 are captured by the aircraft 2 using an aircraft-mounted camera (not shown in the Figures).
[0055] At step s 4 , the captured images of the ground 6 are relayed from the transceiver 12 of the aircraft 2 to the ground station 4 . In this embodiment, these images are sent via the satellite 10 .
[0056] At step s 6 , the camera images received at the ground station 4 are displayed (on a screen) to a human operator at the ground station 4 .
[0057] At step s 8 , the operator identifies the target 8 within the displayed images.
[0058] At step s 10 , the operator sends details about the target 8 (e.g. a global position of the target 8 ) from the ground station 4 to the aircraft 2 .
[0059] In this embodiment, these target details are sent via the satellite 10 .
[0060] At step s 12 , the firing code that is stored at the ground station 4 is sent from the ground station 4 to the aircraft 2 by the operator.
[0061] In this embodiment, the ground station's firing code is sent via the satellite 10 .
[0062] In this embodiment, the ground station's firing code is transmitted to the aircraft 2 at the same time as the target details are transmitted to the aircraft 2 (as described above at step s 10 ). However, in other embodiments, the firing code and the target details are sent to the aircraft 2 at different respective times.
[0063] At step s 14 , the ground station's firing code and the target details received at the transceiver 12 of the aircraft 2 is transmitted to the sequencer 16 of the weapon system 14 .
[0064] In this embodiment the time between the ground station's firing code and target details being sent from the ground station 4 , and the time these signals are received at the sequencer 16 is typically less than 10 seconds. Preferably, the time delay in this communication is less than 10 seconds, for example, less than 1 second. In other embodiments, for example, when multiple satellite links are used in the communications path, the delay is greater than 10 seconds.
[0065] At step s 16 , it is determined whether the firing code received by the aircraft 2 from the ground station 4 is valid.
[0066] In this embodiment, the sequencer 16 checks the validity of the ground station's firing code.
[0067] As described above, a firing code is stored in a storage device which is connected to a port on the sequencer 16 . This stored firing code is compared to the firing code received by the aircraft 2 from the ground station 4 to determine the validity of the firing code received from the ground station 4 .
[0068] In this embodiment, if the firing code received from the ground station 4 is identical to the firing code stored at the sequencer 16 , the received code is determined to be valid.
[0069] However, if the firing code received from the ground station 4 is not identical to the firing code stored at the sequencer 16 , the received code is determined to be invalid.
[0070] Also, in this embodiment the sequencer 16 is arranged to only process a valid firing code if the code carries a recent time code. In this embodiment, a valid code is rejected by the sequencer 16 , i.e. declared “invalid”, if it has been delayed by a pre-determined time period, for example, greater than the maximum expected communication delay. This tends to alleviate problems caused by the firing code command being kept in the aircraft data buffer for several minutes prior to it being processed by the sequencer 16 . For example, the problem of the weapon 18 receiving a significantly delayed power and trigger command tends to be reduced.
[0071] In practice, it tends to be very unlikely that there is a significant delay in processing the firing code. In this embodiment, a misfire (Hang-Up) is assumed to have occurred if there is a firing delay longer than the maximum expected communication delay.
[0072] If, at step s 16 , it is determined by the sequencer 16 that firing code received by the aircraft 2 from the ground station 4 is valid, the process proceeds to step s 18 .
[0073] However, if, at step s 16 , it is determined by the sequencer 16 that firing code received by the aircraft 2 from the ground station 4 is not valid, the process proceeds to step s 22 .
[0074] At step s 18 , the target details transmitted to the sequencer 16 at step s 14 are transmitted from the sequencer 16 to the weapon 18 .
[0075] In this embodiment, the determination that the firing code is valid and the transmission of the target details from the sequencer 16 to the weapon 18 is performed in less than 30 ms.
[0076] At step s 20 , the weapon 18 is launched from the aircraft 2 .
[0077] In this embodiment, after launch the weapon 18 is controlled in a conventional manner dependent on the type of weapon.
[0078] In this embodiment, if a weapon misfire (Hang-Up) occurs during firing, the weapon system 14 reports this via the transceiver 12 to the ground station 4 . This report is sent via satellite 10 .
[0079] The aircraft-mounted camera may be used to advantageously provide a visual aid for confirming if the weapon 18 has successfully fired.
[0080] After performing step s 20 , the process for implementing the weapons system 14 to attack the target 8 ends.
[0081] Returning now to step s 16 , if at this step it is determined by the sequencer 16 that firing code received by the aircraft 2 from the ground station 4 is invalid, the process proceeds to step s 22 .
[0082] At step s 22 , after an invalid code is received by the sequencer 16 , the sequencer 16 ignores the firing code and target details are not provided to the weapon 18 via the sequencer 16 .
[0083] At step s 24 the weapon system 14 reports via the transceiver 12 to the ground station 4 that an invalid firing code has been received. This report is sent via satellite 10 .
[0084] After step s 24 , the process for implementing the weapons system 14 ends.
[0085] Thus, a process for implementing the weapons system 14 to attack the target 8 is provided.
[0086] Once a valid action or event has been completed, the ground station 4 may send an indication of the next anticipated valid firing code to the sequencer 16 (e.g. via the satellite 10 and transceiver 12 ). The sequencer 16 may return a confirmation of the anticipated next valid firing code to the ground station 4 .
[0087] If degradation in the communication link occurs, say, due to a temporary loss of or problem with the satellite connection, the data transmitted by the ground station to the transceiver (or by the transceiver to the ground station) may be corrupted. The ground station 4 may then request that the firing code and time synchronisation data for the last successfully completed action be transmitted by the sequencer 16 via the transceiver 12 and satellite 10 to the ground station 4 , such that end-to-end re-synchronisation of the ground station 4 and the sequencer 16 can be achieved.
[0088] An advantage provided by the above described system and method is that failure modes of the system tend to be easy to identify and plan for.
[0089] The following information details certain possible failure modes of the above described system, and certain actions that may be performed in the event of those failures occurring.
[0090] A first failure mode is where the weapon 18 misfires as result of sequencer 16 not relaying codes to the weapon 18 (i.e. there is fault in the sequencer 16 ). The weapon system 14 reports via the transceiver 12 to the ground station 4 that a misfire has occurred. Any relevant data on this misfire may also be reported to the ground station 4 . This report is sent via the satellite 10 .
[0091] A second failure mode is where the weapon 18 misfires e.g. as a result of a failure of the release mechanism for releasing the weapon 18 from the aircraft 2 . In other words, the weapon is initiated, but not fired. In this event, the weapon system 14 reports via the transceiver 12 to the ground station 4 that a misfire has occurred. Any relevant data on this misfire may also be reported to the ground station 4 . This report is sent via the satellite 10 .
[0092] A further advantage of the above described system and method is that a fully autonomous vehicle is used to launch payloads at a target. Thus, a human operator on the vehicle (i.e. a pilot) is not used, and the risks to such an operator are negated. Nevertheless, in the event of an emergency, manual control of the aircraft may be reverted to.
[0093] A further advantage of the above described system is that the aircraft can be fitted with a variety of different payloads depending on the requirements of the scenario.
[0094] A further advantage of the above described system is that the aircraft tends to be inherently stable in all three axes (roll, pitch, and yaw).
[0095] The above described system and method tends to provide for real time monitoring of the state of the weapon on the aircraft.
[0096] The satellite link between the ground station and the aircraft advantageously tends to provide for Beyond Line Of Sight (BLOS) communication. In other embodiments, a different type of data link, e.g. a Line Of Sight (LOS) data link, is used instead of or in addition to the BLOS data link.
[0097] A further advantage provided by the above described system and method is that end-to-end control of the weapon system tends to be maintained even when the data link employed (between the ground station and the aircraft) has uncertain performance, availability, and integrity.
[0098] Apparatus, for implementing the arrangement described above with reference to FIGS. 1-3 , and performing the method steps described above with reference to FIG. 4 , may be provided by configuring or adapting any suitable apparatus, for example one or more computers or other processing apparatus or processors, and/or providing additional modules. The apparatus may comprise a computer, a network of computers, or one or more processors, for implementing instructions and using data, including instructions and data in the form of a computer program or plurality of computer programs stored in or on a machine readable storage medium such as computer memory, a computer disk, ROM, PROM etc., or any combination of these or other storage media.
[0099] It should be noted that certain of the process steps depicted in the flowchart of FIG. 4 and described above may be omitted or such process steps may be performed in differing order to that presented above and shown in FIG. 4 . Furthermore, although all the process steps have, for convenience and ease of understanding, been depicted as discrete temporally-sequential steps, nevertheless some of the process steps may in fact be performed simultaneously or at least overlapping to some extent temporally.
[0100] In the above embodiments, the aircraft weapon system is implemented in the particular scenario described above with reference to FIG. 1 . However, in other embodiments the aircraft weapon system is implemented in a different scenario. For example, in other embodiments a scenario in which the weapon system is implemented may comprise a different number of aircraft, ground stations, satellites, and/or targets that interact in the same or a different appropriate way to that described above.
[0101] In the above embodiments, the autonomous vehicle used to deliver the payload is an aircraft. However, in other embodiments the vehicle is a different type of autonomous vehicle, for example, an autonomous land-based or water-based vehicle.
[0102] In the above embodiments, communications between the ground station and the aircraft are via a single satellite. However, in other embodiments the ground station and the vehicle communicate in a different way, for example, via a different number of satellites, or directly, or using an airborne relay.
[0103] In the above embodiments, the aircraft follows a pre-programmed navigation route. However, in other embodiments the vehicle may follow a different type of route, for example a series of way-points may be uploaded to the aircraft while the aircraft is airborne, or the aircraft may determine its own route.
[0104] In the above embodiments, the firing code is stored in a storage device which is connected to a port on the sequencer. The same code is also stored at the ground station. The firing code may be stored in computer memory of the respective sequencer and ground station. However, in other embodiments a different appropriate system is implemented to provide relatively secure and robust way in which the sequencer (or equivalent) can validate firing codes and target details. For example, in other embodiments two respective firing codes can be relayed to the aircraft from two respective ground stations. The sequencer (or equivalent) may compare the two received codes in order to validate an attack instruction.
[0105] In the above embodiments, the ground station is located on the ground. However, in other embodiments, the ground station, i.e. a location that the operator that controls the aircraft's weapon systems is at, is located at a different location remote from the aircraft, e.g. in a different aircraft or other vehicle.
[0106] In the above embodiments, an aircraft-mounted camera is used to capture images of the ground for use by the operator at the ground station. However, in other embodiments, a different type of sensor (mounted on the aircraft or remote from the aircraft) is used to provide data to the operator for the purpose of target selection. For example, a visible light-detecting camera, an infra-red camera, a ultra-violet camera, a radar sensor, etc. may be used.
|
An apparatus, and a method performed by the apparatus, are disclosed wherein the apparatus can be mounted on an unmanned vehicle and arranged to act upon a payload. The payload can be mounted on the unmanned vehicle and, under an action of the apparatus, is able to be activated. The method can include receiving an activation instruction from an entity remote from the unmanned vehicle; determining whether or not the received activation instruction is valid by performing a validation process; and in response to determining that the received activation instruction is valid, activating the payload. In response to determining that the received activation instruction is not valid, activation of the payload may be prevented or opposed.
| 5
|
BACKGROUND OF THE INVENTION
This is a continuation-in-part application of Ser. No. 247,421 filed Apr. 25, 1972, now abandoned.
This invention relates to a process for polymerizing cycloolefins using a novel catalyst.
In the prior art, it has been reported that as polymerization catalysts for cycloolefins, catalysts have been used containing salts of transition metals of the IVB group or the VIB group, such as tungsten hexachloride and organo aluminum compound. But these are soluble homogeneous catalysts. (G. Natta et al., Makromole, Chem. 91, 87 (1966); Japanese Patent Publication No. 20784/1967; N. Calderon et al., J. Polychem. Sci. A-1, 5, 2209 (1967).
Also, Bell U.S. Pat. No. 3,772,255 teaches a method for ring opening polymerization of cycloolefins using as a catalyst a mixture of tungsten oxide and either aluminum chloride or alkyl aluminum dichloride in the ratio of 3:2 to 2:3. The polymerization rate, however, leaves much to be desired; the rate is very low.
SUMMARY OF THE INVENTION
On the other hand, catalysts used in the present invention are inhomogeneous, i.e. heterogeneous, catalysts containing tungsten trioxide which is not essentially a salt of a transition metal, and a Lewis acid; or a system containing organoaluminum compound in order to increase their activity, such as inhomogeneous, i.e. heterogeneous, solid catalyst containing tungsten trioxide, Lewis acid and organo aluminum compound, which was found to be an extremely highly active catalyst system.
A salt of a transition metal such as tungsten hexachloride, is known to be used as a polymerization catalyst. But, such salt has many disadvantages in that it is expensive and careful handling is required because it reacts with moisture in air easily.
On the other hand, the tungsten trioxide used in the present invention is extremely stable compound. It is known that tungsten trioxide reacts with Lewis acid, such as aluminum chloride to form oxi-chloride at extremely high temperatures. However, surprisingly using the present invention, it was confirmed that cycloolefins were polymerized with the inventive catalyst under conditions where no oxichloride was formed.
In addition, it has been proven in the Examples set forth herein that the catalyst of the present invention has extremely interesting properties and the use of tungsten salt is not necessary. Cycloolefins were polymerized with heterogeneous catalyst containing tungsten trioxide and organometallic compound containing no halogen atom, such as triethyl aluminum.
In contrast to the above-mentioned Bell, the present invention employes tungsten trioxide and Lewis acid in the ratio of 1/3 to 1/30, preferably. It was discovered by the present inventors that the polymerization rate was unexpectedly substantially greater than use of the ratio of 2/3 to 3/2 as in Bell. The amount of increase was over 8 fold, ranging from 25% to 65% per hour, in contrast to Bell which produced polymerization rates of about 3% per hour at the ratio of 1/1.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The invention encompasses the polymerization of cycloolefins. As the cycloolefins, one may select cyclic unsaturated hydrocarbons containing at least one double bond in a ring of C 7 to C 12 . For example, 1,5-cyclooctadiene; 1,5,9-cyclododecatriene, cyclooctene and the like may be used. The catalyst of the present invention advantageously enables the polymerization to proceed with better stereo regularity in considerable extent, as well as being economical and easy handling. For example, 1,4-polybutadiene containing 80% of cis double bonds and 20% of trans double bonds was obtained from cis, cis-1, 5-cyclooctadiene. Polymer of 1,4-polybutadiene structure containing almost 100% of trans double bond was obtained from 1,5,9-cyclododecatriene containing cis, trans, trans- and trans, trans-1,5,9-cyclododecatriene in a ratio of 40:60.
Although no definite results were obtained from infrared spectra, polyoctenamer containing cis double bond in most part was obtained as semi-solid or viscous oily product from cis-cyclooctene.
The results mentioned above indicate important particularities of the heterogeneous solid catalyst of the present invention and the stereo regularity mentioned above is not so distinguished for the system containing homogeneous catalyst.
As Lewis acid to be used in the present invention, AlCl 3 , AlBr 3 , TiCl 4 , VCl 4 , VOCl 3 , and the like can be selected, though the selection is not limited to these compounds. Among these, AlCl 3 is especially preferred for industrial use.
Aluminum trichloride used in the present can be added, without any treatment, to the system but yield may be preferably improved by adding aluminum trichloride, which is mixed and kneaded with tungsten trioxide for several hours before use.
A small amount of weak Lewis base such as diethyl ether or nitro-compound may be added to the catalyst systems above mentioned. Favorable results were obtained with organo aluminum compounds such as C 2 H 5 AlCl 2 , (C 2 H 5 ) 2 AlCl, (C 2 H 5 ) 3 Al, and the like. Especially good conversion was found to be obtained with C 2 H 5 AlCl 2 .
Of course, C 2 H 5 AlCl 2 , (C 2 H 5 )AlCl and (C 2 H 5 ) 3 Al are classified as Lewis acid, and catalyst systems composed of these compounds and tungsten trioxide gave highly stereoregular polymer with good yield. l
The mixing ratio of tungsten trioxide and Lewis acid is preferably from 1:3 to 1:30. This range produced high polymerization activity and rate. Anhydrous tungsten trioxide may be used without any treatment, or favorably, used with a carrier.
In a tri-component heterogeneous catalyst of tungsten trioxide, Lewis acid (excluding organo aluminum compound), and organo aluminum compound, the mole ratios to each other are preferably in the range of 1:(3 to 30):(3 to 30). The mole ratio of tungsten trioxide to organo aluminum compound is preferably between 1:3 to 1:30. Use of a lower ratio may possibly cause gel formation and is not necessary. Mixing of WO 3 and Lewis acid was at a temperature below 80°C. with no reaction therebetween.
The mole ratio of tungsten trioxide to monomer is advantageously as small as possible, but it is preferably within the range of from 1:100 to 1:10000 monomer.
According to the present invention, polymerization can be accomplished with or without the presence of diluting agent. Aliphatic hydrocarbon, aromatic hydrocarbon or halogenated hydrocarbon may be used as a diluting agent.
Polymerization reaction may be performed at a temperature within the range of from -50°C to 80°C and, more preferably, from 0°C to 60°C for more desirable results.
Polymers manufactured according to the present invention may be used as elastomer or plastics.
The principles of the invention are further illustrated by the following actual examples.
EXAMPLE 1.
Polymerization was accomplished in a flask equipped with a stirrer and tubes for introducing nitrogen and reagents.
Into the flask was added 0.1 m mole (0.0232 gram) of tungsten trioxide and then 0.3 m mole (0.400 gram) of aluminum chloride and then the content was mixed completely for one hour at room temperature. Then, 3 ml of anhydrous cis, cis-1,5-cyclooctadiene was added to the mixture and allowed to react for one hour at room temperature. The reaction was stopped by addition of methanol-benzene (1:9) solution of phenyl-β-naphthylamine (50 mg in 30 ml). The polymer obtained thereby was separated from solid catalyst by filtration, and then purified by precipitation with methanol. The rubber like product thus obtained was dried under vacuum at room temperature for complete removal of the solvent. Yield of the product was 0.64 gram. The polymerization rate for this mixing ratio of WO 3 to AlCl 3 was 24.5 % per hour. The ratio was 1/3.
The infrared spectrum of this polymer indicated the presence of 80% of cis-1,4- and 20% of trans-1,4-polybutadiene compounds in the polymer. No 1,2-polybutadiene group was found in the infrared spectrum. Its intrinsic viscosity in toluene at 30°C was found to be 0.16. Aluminum chloride used herein refers to AlCl 3 .
EXAMPLE 2.
The same procedure was conducted as in Example 1. To a catalyst consisting of 0.1 m mole (0.0232 gram) of tungsten trioxide and 0.3 m mole (0.0400) of aluminum chloride were added 3 ml of cis, cis-1,5-cyclooctadiene and then 3 m mole of ethylaluminum dichloride (1 ml of toluene solution), and the mixture was subjected to reaction at room temperature for 1 hour. The product was purified with the same procedure as Example 1 to produce a rubber like polymer of 1.5 grams. The infrared spectrum of this polymer indicated the presence of the same components as in Example 1. The intrinsic viscosity thereof in toluene at 30°C was found to be 0.05.
EXAMPLE 3.
The same procedure as Example 1 was performed. To a catalyst consisting of 0.1 m mole (0.0232 gram) of tungsten trioxide and 0.3 m mole (0.0400 gram) of aluminum chloride were added 3 ml of cis, cis-1,5-cyclooctadiene and then 0.6 m mole of diethyl aluminum chloride (0.2 ml of toluene solution) and the mixture was subjected to reaction at room temperature for 1 hour. The product was purified with the same procedure as in Example 1 to produce a rubber like polymer of 0.71 gram. Infrared analysis of the product indicated that the resulting polymer contained 85% of cis-1,4 and 15% of trans-1,4-polybutadiene. The intrinsic viscosity of the polymer in toluene at 30°C was 0.13.
EXAMPLE 4.
The procedure of Example 1 was repeated except using 1,5,9-cyclododecatriene containing cis-trans-trans-isomer and trans-trans-trans-isomer in a 40/60 ratio in place of cis,cis-1,5-cyclooctadiene. To a catalyst of 0.1 m mole (0.0232 gram) of tungsten trioxide and 0.3 m mole (0.0400 gram) of aluminum chloride was added 2 ml of 1,5,9-cyclododecatriene. After reacting at room temperature for 1 hour, the product produced thereby was purified by the same procedure mentioned above, to give 0.122 gram of white solid polymer. Infrared analysis indicated that the polymer contained about 100% of trans-1,4-polybutadiene. The intrinsic viscosity of the polymer in toluene at 30°C was 0.06.
EXAMPLE 5 (CONTRAST)
Reaction was performed following the procedure of Example 1. To a catalyst of 0.1 m mole (0.0232 gram) of tungsten trioxide and 0.1 m mole (0.01348 gram) of aluminum chloride was added 2 ml of 1,5,9-cyclododecatriene. After reacting at room temperature for 1 hour the product thereof was purified by the same procedure mentioned above, to give 0.0523 gram of white solid polymer. The polymer had the same infrared spectrum as that of the polymer in Example 4. The intrinsic viscosity of the polymer in toluene at 30°C was the same as in Example 4. However, the polymerization rate for the ratio of WO 3 to AlCl 3 of 1/1 was only 3% per hour.
EXAMPLE 6.
The procedure of Example 1 was repeated except to use ethyl aluminum dichloride in place of aluminum chloride as Lewis acid. There was then added to the reaction mixture 0.1 m mole (0.0232 gram) of tungsten trioxide, 3 ml of 1,5,9-cyclododecatriene and then dropwise 3 ml of ethyl aluminum dichloride (1 ml of toluene solution), followed by subjecting the mixture to reaction at room temperature for 2 hours. The product thereof was purified by the same procedure as that in Example 1 to give 0.84 gram of white solid polymer. The polymer had the same infrared spectrum as that in Example 4. The intrinsic viscosity of the polymer in cyclohexane at 20°C was 0.04.
EXAMPLE 7.
The procedure of Example 1 was repeated using triethyl aluminum as Lewis acid. To a reaction vessel were added, 0.1 m mole (0.0232 gram) of tungsten trioxide, 3 ml of 1,5,9-cyclododecatriene and dropwise 6 m mole (2 ml of toluene solution) of triethyl aluminum. After reacting at room temperature for 3 hours, the reaction was stopped by conventional procedure to give 1.20 gram of polymer containing mostly gelled part. The infrared spectrum indicated that ungelled fraction of the polymer was exclusively trans-isomer as in Example 4. The gelling was caused by the mixing ratio being above the preferred range, namely 1/60.
EXAMPLE 8.
Reaction was performed following the procedure of Example 1. With additions of 0.1 m mole (0.0232 gram) of tungsten trioxide, 0.3 m mole (0.0400 gram) of aluminum chloride, then 0.01 ml of diethyl ether as a catalyst, and 3 ml of 1,5,9-cyclododecatriene, the mixture thereof was subjected then to reaction at room temperature for 1 hour. The resulting white solid polymer was 0.124 gram. The infrared spectrum was the same as in Example 4. The intrinsic viscosity of the polymer in toluene at 30°C was 0.08.
EXAMPLE 9.
Following conventional method, 0.1 m mole (0.0232 gram) of tungsten trioxide, 0.3 m mole (0.0400 gram) of aluminum chloride, 3 ml of 1,5,9-cyclododecatriene and 0.3 ml of diethyl aluminum chloride (0.1 ml of toluene solution) were added and the mixture thereof reacted at room temperature for 1 hour, to thereby give 0.080 gram of white solid polymer. The infrared spectrum of the polymer was the same as in Example 4. The intrinsic viscosity of the polymer in toluene at 30°C was 0.02.
EXAMPLE 10.
Following the procedure in Example 1, reaction was performed. To 0.1 m mole (0.0232 gram) of tungsten trioxide was added 2 ml of 1,5,9-cyclododecatriene and then dropwise 3 m mole of ethyl aluminum dichloride (1 ml of toluene solution), followed by reacting the mixture at room temperature for 1 hour. The product was purified in the same manner as in Example 1 to give 1.13 gram of white solid polymer. The infrared spectrum of this polymer was the same as in Example 4. The viscosity (intrinsic) of the polymer in toluene at 30°C was 0.08. The polymerization rate for the molar ratio of WO 3 to ethyl aluminum dichloride of 1/3 was 65% per hour.
EXAMPLE 11.
The procedure of Example 1 was repeated except to use cis-cyclooctene as a monomer in place of cis-cis-1,5-cyclooctadiene, 0.1 m mole (0.0232 gram) of tungsten trioxide and 0.3 m mole (0.0400 gram) of aluminum chloride was well mixed and added thereto was 3 ml of cis-cyclooctene. After reacting the mixture at room temperature for 3 hours, the reaction was stopped by a conventional means to give 0.61 gram of semi-solid or oil-like polymer. The infrared spectrum of the polymer indicated that there were bands attributed to cis-oct-enamer as a major component and to trans-octenamer as a minor component.
EXAMPLE 12.
The reaction was performed following the procedure of Example 1. There was added 0.1 m mole (0.0232 gram) of tungsten trioxide, 0.3 m mole (0.0400 gram) of aluminum chloride as catalyst and 3 ml of cis-cyclooctene. Further added thereto dropwise was 3 ml of ethyl aluminum dichloride (1 ml of toluene solution). Then the mixture was reacted at room temperature for 2 hours to give 1.52 gram of semisolid polymer.
EXAMPLE 13.
Following conventional method, 0.1 m mole (0.0232 gram) of tungsten trioxide, 0.3 m mole (0.0400 gram) of aluminum chloride, 0.2 ml of 1,5,9-cyclododecatriene and 0.1 m mole of ethyl aluminum dichloride (0.1 ml of chlorobenzene solution) were added and the mixture thereof reacted at room temperature for 1 hour, to thereby give 0.11 gram of white solid polymer. The infrared spectrum of the polymer was the same as that for Example 4.
By mixing the tungsten trioxide and Lewis acid or Lewis acid and organo aluminum compound at a temperature of below 80°C, the compounds do not react with each other. The catalyst components are termed "heterogeneous". The catalyst are active during polymerization. Its components are not reacted with each other during initial mixing.
The foregoing description is intended to be illustrative of the principles of the invention. Numerous modifications and variations thereof would be apparent to the worker skilled in the art. All such modifications and variations are to be considered to be within the spirit and scope of the invention.
|
A Process for polymerizing cycloolefins by ring opening reaction using heterogeneous catalyst containing tungsten trioxide and Lewis acid or tungsten trioxide, Lewis acid and organoaluminum compound as the polymerization catalyst.
| 2
|
BACKGROUND
The present invention relates generally to gimbal control systems, and more particularly, to a gimbal control system that employs inner and outer control loops.
Conventional systems for spacecraft antenna control do not simultaneously use autotrack and resolver references. Many systems do not have resolvers at all and in the absence of autotrack sensor signals steer the antenna by open-loop counting of steps. Conventional antenna control systems that use resolvers for closed-loop control of gimbal position in the absence of an autotrack signal would, upon detection of the autotrack signal, commence to use that signal exclusively; that is, they would either use the autotrack or the resolver reference, but not together. This limits system performance by not using all the available sensor information.
Heretofore, a variety of gimbal control systems have been developed for use in controlling the pointing direction of satellite antennas. For example, a gimbal control system employed on the MILSTAR spacecraft has resolvers and autotrack receivers. However, they use one or the other, never both at the same time. The current-generation TDRSS satellite uses an autotrack receiver as a pointing reference for its gimbal. However, it does not have a resolver. When performing "program track" (or open-loop) pointing, it keeps track of the antenna's position by counting motor steps. Gross updates of the antenna's position are available from potentiometers, but are not used in any closed-loop algorithms. Satellites such as INTELSAT VI or AUSSAT-B use ground-based beacons as pointing references for their antennas. These beacon tracking systems are much like the TDRSS design, in that they do not have a resolver but keep track of antenna position by counting steps.
Other gimbal systems with very high performance requirements (such as those developed for laser pointing) often have a highly accurate high bandwidth sensor such as a gyro on the payload (i.e., mounted on the object that is steered by the gimbal). In these cases, that sensor (the gyro or other sensor on the payload) is the primary or only sensor used to control the gimbal. The gyro may be supplemented with a lower-bandwidth target tracking loop. This is the opposite of the design concept of the present invention, where a payload-mounted sensor is only used to provide low-bandwidth correction to a control loop using the resolver.
U.S. Pat. No. 5,062,592, granted to H. Kishimoto, issued Nov. 5, 1991, entitled "Orientation Control Apparatus for Space Vehicle", describes a spacecraft with a gimballed antenna. The antenna has an RF autotrack sensor to sense its inertial position. There is also a rate sensor for sensing the rate of the spacecraft main body (not the antenna), and both sensors are used simultaneously for controlling the antenna gimbal. This differs from the present invention because there is no sensor (such as a resolver) for measuring the relative orientation between the spacecraft and the antenna.
A number of papers relating to control of gimballed payloads have been presented at the annual SPIE Conference on Acquisition, Tracking, and Pointing. For example, a paper entitled "Design and Performance of a Satellite Laser Communications Pointing System," by R. Deadrick, Proc. 8th Annual Rocky Mountain Conference, Keystone, Colo., 1985, is an example of numerous papers that describe gimbal control systems with both resolvers and sensors for measuring payload pointing (quadrant detector in this case), but both sensors are not utilized simultaneously: the resolver is used only in acquisition mode, and the quadrant detector is used only in track mode. Another paper entitled "Acquisition and Tracking System for a Ground-Based Laser Communications Receiver Terminal," E. Clark & H. Brixley, SPIE Vol. 295, Control and Communication Technology in Laser Systems, 1981, pp. 162-169 describes a similar system.
A paper entitled "Attitude Acquisition and Tracking Capabilities of the Instrument Pointing System," by J. Busing and P. Urban, in the First SPIE Conference on Acquisition, Tracking and Pointing, April 1986, describes a control system for a gimballed telescope which simultaneously uses gyros, optical sensors, resolvers, and accelerometers. The optical sensor is used to calibrate gyro rate drifts, and thus the gyro is an inherent part of this control system. The detailed control architecture is not shown.
A paper entitled "Azimuth/Elevation Servo Design of the W. M. Keck Telescope," by M. Sirota and P. Thompson, in the Second SPIE Conference on Acquisition, Tracking and Pointing, January 1988, describes a system for controlling a gimballed telescope with simultaneous feedback of accelerometer, tachometer, and encoder measurements. No optical or RF reference is used.
A paper entitled "The Enhancement of Armored Vehicle Fire Control (Stationary and Fire-on-the-Move) Performance Using Modern Control Techniques," J. Groff, presented at the Third SPIE Conference on Acquisition, Tracking and Pointing, March, 1989, describes a system for controlling a gun turret using (simultaneously) a gyro, a tachometer, a potentiometer, and an optical gimbal angle encoder. The control compensation and architecture appear to be significantly different and more complicated than the present invention.
A paper entitled "A Low-Cost Alternative to Gyroscopes for Tracking System Stabilization," by D. Laughlin et al., in the Fourth SPIE Conference on Acquisition, Tracking and Pointing, April 1990, describes a gimbal control system using a gyro or magnetohydrodynamic device mounted on the payload for measuring angular rate, and closing a high-bandwidth inner "stabilization" feedback control loop, and simultaneously using an optical or RF sensor for closing a low bandwidth outer "track" feedback control loop. No resolver or other relative angle sensor is used. Several other papers describing the same configuration are found in the SPIE conference proceedings.
A paper entitled "A New Generation Control System for Ultra-Low Jitter Satellite Tracking," by W. Verbanets and D. Greenwald, in the Fifth SPIE Conference on Acquisition, Tracking and Pointing, April 1991, describes a gimbal system with simultaneous feedback of accelerometer and position encoder measurements. The compensation is different from the present invention and no inertial optical or RF sensor is employed.
A paper entitled "Optimization of Gimbal Scanned Infrared Seeker," by E. Williams, R. Evans, K. Brant, and L. Stockum in the Fifth SPIE Conference on Acquisition, Tracking and Pointing, April 1991, describes a control system for a seeker that simultaneously uses resolver and gyro feedback. However, the paper does not describe the control compensation.
A paper entitled "Universal Beam Steering Mirror Using the Cross Blade Fixture," by M. Meline, J. Harrell, and K. Lohnes, presented at the Sixth SPIE Conference on Acquisition, Tracking and Pointing, April 1992 includes a block diagram of a system for controlling a gimballed mirror which has an inner control loop using a measurement of the relative angle between the mirror and the basebody. However, this feedback loop has a lower bandwidth than the main outer optical control loop and has the express purpose of canceling the mirror control motor's back EMF, but does not provide any control of the mirror angle beyond that.
While several of the control systems for gimbals described above share certain characteristics with the present system, all of them are different in some fundamental way. The fundamental characteristics of the present system that do not appear in any of these papers are: (1) the simultaneous use of gimbal position measurements relative to both the spacecraft and the target (i.e., resolver and optical or RF tracking sensor measurements); the systems in the published references either do not use these measurements simultaneously, or use some other combination of measurements; and (2) the control filtering used to combine these measurements to account for biases between a programmed (open-loop) command reference and the measured target position from the optical or RF tracking sensor.
Accordingly, it is an objective of the present invention to provide for a gimbal control system that simultaneously uses measurements of relative and inertial gimbal position and a control filtering scheme to combine these measurements to account for biases between the programmed (open-loop) command reference and the measured target position from the optical or RF tracking sensor.
SUMMARY OF THE INVENTION
The present invention is a control system for a gimballed antenna that employs devices for measuring the absolute line-of-sight of the antenna (provided by an autotrack receiver or beacon tracker) and the relative angular position of the antenna (provided by a resolver). The gimbal control system uses both signals simultaneously, thereby increasing the performance and pointing accuracy capability. There are two control loops that operate simultaneously to provide for optimum performance. The first or inner loop is a high-bandwidth control loop that uses the relative gimbal angle measurement to control the antenna pointing along a precommanded profile. The inner loop may run alone to provide for coarse pointing. When available, the line-of-sight measurement is used in a low-bandwidth outer loop to provide corrections to the command profile of the inner loop. Control logic is provided that takes advantage of the control loop structure to allow switching between several control modes. By using the present invention, antenna tracking control performance is maximized, especially in the presence of attitude disturbances of the spacecraft or significant flexible interactions.
The present two-loop control system is especially valuable in cases where a control loop using one of the sensors has an inherently limited bandwidth. For example, in some cases the autotrack sensor creates a relatively noisy but accurate measurement of the absolute inertial position of the target and a control loop using just the autotrack sensor would have a limited bandwidth. The bandwidth of an autotrack loop is also limited if there is significant flexibility in the structure between the gimbal and the antenna where the autotrack sensor measurement is taken, or if the gimballed inertia interacts with the spacecraft structural dynamics. In either of these cases, it is advantageous to use the autotrack sensor to provide a low-bandwidth correction to the high-bandwidth inner control loop that uses the resolver as is provided in the present invention.
Another advantage of using the resolver measurement even when the autotrack reference is available is that resolver feedback enables improved damping of gimbal flexibility. This enables a lighter-weight gimbal with less stiffness to provide an equivalent performance capability.
As spacecraft antenna pointing requirements become more stringent due to increased communication bandwidths, it will become more important to have antenna control systems with the highest possible performance and pointing accuracy. The present system provides improved performance by using all available information from the resolver and autotrack receiver in the spacecraft to control antenna pointing. Also, including the resolver in the feedback control system at all times makes the system less susceptible to missed steps in a stepper motor gimbal. This is important because, as step sizes become smaller, stepper drive motors are more likely to miss steps.
BRIEF DESCRIPTION OF THE DRAWINGS
The various features and advantages of the present invention may be more readily understood with reference to the following detailed description taken in conjunction with the accompanying drawings, wherein like reference numerals designate like structural elements, and in which:
FIG. 1 illustrates a gimbal drive system that employs a gimbal control system in accordance with the principles of the present invention;
FIG. 2 is a block diagram illustrating the details of the gimbal control system in accordance with the principles of the present invention;
FIG. 3 is a block diagram illustrating compensation for a stepper drive gimbal that may be employed in the gimbal control system of FIG. 2;
FIG. 4 is a block diagram illustrating compensation for a direct drive gimbal that may be employed in the gimbal control system of FIG. 2; and
FIG. 5 is a state diagram illustrating antenna mode control used in the gimbal control system of FIG. 2.
DETAILED DESCRIPTION
Referring to the drawing figures, FIG. 1 depicts a gimbal control system 10 in accordance with the principles of the present invention that is adapted to steer an antenna 11 that is mounted on a gimbal 13. In the illustrative embodiment of FIG. 1, the gimbal 13 and the antenna 11 are disposed on a spacecraft 12. The gimbal 13 may be either a stepped or direct ("continuous") drive design. The gimbal 13 is typically a two-axis gimbal, but in certain cases may have one or three controlled axes. A typical example of a stepper-motor driven gimbal 13 is shown in FIG. 1.
The gimbal 13 includes an accurate, low-noise measuring device for measuring the relative angular position of the gimbal 13 and producing a relative position angle measurement signal 18a. This device is typically a resolver 14, but an inductosyn or an optical encoder may also be employed. The relative position signal 18a is indicative of the position error of the gimbal 13 and is typically resolved into two mutually orthogonal components (azimuth and elevation) by the resolver 14. Given that the antenna 11 and gimbal 13 are mounted on the spacecraft 12, the resolver 14 measures the relative angle between the spacecraft 12 and the antenna 11 pointing direction. The relative angle data, along with data indicative of the attitude of the spacecraft 12, determines the pointing direction of the antenna 11 in inertial space. Azimuth and elevation actuators 17 are disposed on the gimbal 13 and are used to move the antenna 11 to its commanded position.
The spacecraft 12 includes a receiver signal processor 19 for receiving and electronically processing a communications signal 18c defining antenna 11 angular position error relative to an absolute reference. Typically, this reference is the desired pointing direction of the antenna 11, and may be generated on the earth or on another cooperating satellite with which the spacecraft 12 communicates (known as a crosslink). The signal processor 19 is commonly part of or ancillary to the main communication receiving electronics of the spacecraft 12. The drive control and resolver processing unit 9 produces gimbal position and resolver signals 18a that are applied to the gimbal control processor 15. The control processor creates gimbal commands 18b that are executed by the drive control and resolver processing unit 9.
In one commonly used design, the received communications signal is used for the pointing reference (typically in a noncoherent receiver), and an autotrack receiver is used to extract the azimuth and elevation error signals. In another commonly used design, some part of the received communications signal is used to create a position reference signal, and the receiver is coherent. This position reference signal is a reference beacon and the electronics that decodes the azimuth and elevation error signals forms a beacon tracker. Other types of sensors that perform this function include: laser communication devices, quadrant detectors, or a payload which derives its own line-of-sight measurement, for example, using an optical telescope.
The drive control and resolver processing unit 9 is coupled between the control processor 15 and the gimbal 13. A receiver demodulator 19 is coupled between the antenna 11 and the control processor 15. The receiver demodulator is adapted to demodulate an autotrack RF signal 18c and produce azimuth and elevation tracking error signals 18d that are processed by the control processor 15.
FIG. 2 is a detailed block diagram of the gimbal control system 10, which employs an outer control loop 23, and an inner control loop 21 that includes the resolver 14. More particularly, the gimbal control system 10 of FIG. 2 is used to control one axis of the gimbal 13. The gimbal control system 10 for the other axis is similar or substantially identical to the gimbal control system 10 shown in FIG. 2.
The inner control loop 21 is comprised of the resolver 14 and a resolver processing circuit 22. The resolver 14 is adapted to provide an output signal 51 indicative of gimbal angles relative to the spacecraft 12. The resolver processing circuit 22 is adapted to process the resolver measurement and provide an output signal 18a indicative of the relative angular position of the antenna 11 (the measured gimbal angle). The inner control loop 21 also comprises a compensation circuit 25, a step generator 26, or motor driver 26, that is adapted to generate step commands, and a gimbal drive 27 that produces a desired gimbal angle signal that drives the gimbal 13.
The gimbal motion, along with spacecraft bus motion, is coupled to the spacecraft and payload dynamics. The inertial orientation of the antenna boresight is a consequence of the spacecraft and payload dynamics. The output of the spacecraft dynamics 31 is processed by an autotrack receiver 19 which produces an autotrack error signal 18d. The autotrack error signal is processed by an anti-aliasing filer 33 and then digitized in an analog-to-digital converter 34. The output of the analog-to-digital converter 34 is applied to a P-I (proportional-integral) compensation circuit 35. First second and third switches 36, 37, 38, are serially coupled between the P-I compensation circuit 35 and the summing device 24. Various command signals that are determinative of control modes provided by the gimbal control system 10 are shown coupled to selected terminal of the switches 36, 37, 38 and include a program track profile 41, a compensated ground command 42, a spacecraft motion compensation signal 43, uncompensated ground command 44, and a store position command 45.
The gimbal control system 10 uses the measurement provided by the resolver 14 for feedback control, and the inner control loop 21 is always active. The inner control loop 21 is a servo loop that controls the antenna 11 to a commanded orientation with respect to the spacecraft 12. The measurement provided by the resolver 14 is processed by a resolver processing circuit 22 and is compared with a commanded gimbal angle in a summing device 24. The error between the measurement provided by the resolver 14 and the commanded gimbal angle is provided as an error output signal from the summing device 24. The error signal is processed by a compensation circuit 25, optionally filtered by an optional digital or analog filter 28 (shown in FIGS. 3 and 4), and then processed by a step generator 26 or motor driver 26 to provide a step rate command for a stepping gimbal 13 or a torque command for a direct-drive gimbal 13. The step command is then sent to gimbal drive 27.
The resolver feedback signal provided by the resolver 14 provides a measurement of the relative angle between the spacecraft 12 and the gimballed antenna 11. This allows for stabilization of gimbal compliance by phase-lead compensation. In theory, derivative feedback may increase the damping of a flexible mode to any desired value. This allows for at least one or two flexible modes to be within the bandwidth of the gimbal control system 10 and therefore a higher-bandwidth gimbal control system 10 may be designed. Thus, even if the gimbal 13 is significantly flexible, an accurate high-bandwidth measurement of the gimbal angle enables improved performance, and more accurate control of the antenna 11. Since a stiffer gimbal drive tends to be heavier, the use of the resolver 14 enables antenna 11 control accuracy to be maintained with a lighter weight gimbal 13.
If the gimbal 13 is driven by a stepper motor, for example, the drive motor causes the gimbal 13 to move exactly to the commanded position. Ignoring flexible modes, the transfer function of the gimbal dynamics is unity. The purpose of feedback control in this case is to use the measurement provided by the resolver 14 to enable the gimbal 13 to track the position command, expressed in degrees of angle instead of relative step counts. In the stepper drive case, and in the preferred implementation, the inner control loop 21a (or compensation loop 21) is as shown in FIG. 3. FIG. 3 is a block diagram illustrating an inner control loop 21a (compensation loop 21) for a stepper drive gimbal 13 that may be employed in the gimbal control system 10 of FIG. 2.
The compensation provided by the inner control loop 21a includes a proportional-double-integrator-derivative (PIID) compensation device 25a that provides for tracking of a commanded position that has a "ramp" characteristic (i.e., a moving target with equation of time a 0 +a 1 t) with no steady-state error. The double integrator compensation device 25a has the added benefits of filtering high-frequency noise and flexible dynamics. The inner control loop 21a also includes the optional notch filter 28 that provides phase lead or a derivative feedback term to stabilize the closed-loop control system 10, and an optional roll-off filter 28a to stabilize flexible modes in the gimbal 13 or antenna 11.
In one possible implementation, the inner control loop 21 outputs a stepping rate command, and the motor drive electronics (which may include a numerically controlled oscillator) integrates this command to derive individual step commands. The inner control loop 21 may be implemented using either analog or digital electronics, or a microprocessor.
If the gimbal 13 is driven by a continuous-drive motor, the inner control loop 21b as shown in FIG. 4 may be employed. FIG. 4 is a block diagram illustrating the inner control loop 21b for a direct drive gimbal 13 that may be employed in the gimbal control system 10 of FIG. 2. In this case, the double integrator characteristic required for the inner control loop 21b to be able to track a ramp input is inherent in the gimbal dynamics. The inner control loop 21b comprises a PID (proportional-integrator-derivative) type integrator 25b as is shown in FIG. 4. This inner control loop 21b allows the control system 10 to achieve zero steady-state error in the presence of constant or slowly-varying friction in the gimbal 13. As before, the inner control loop 21b may also include a notch filter 28 or additional phase lead to stabilize flexible modes in the gimbal 13 or antenna 11, and may be implemented with either analog or digital electronics, or a microprocessor.
Referring again to FIG. 2, possible gimbal control modes using resolver feedback will now be discussed. By changing the position of the switches 36, 37, 38 shown in FIG. 2, it is possible to control the antenna 11 in any of several modes. The switch positions referred to below are numbered as follows. Switch 1 (36), connects to either the Store Position Command 45 (position 1), Uncompensated Ground Command, 44 (position 2) or Spacecraft Motion Compensation, 43 (position 3). Switch 2 (37) connects to either Compensated Ground Command, 42 (position 1) or Program Track Profile, 4 (position 2). Switch 3 (38) connects either to P-I compensation, 35 (position 2) or is open (position 1). The gimbal control modes are summarized in Table 1 below.
TABLE 1______________________________________Antenna Mode Switch 1 (36) Switch 2 (37) Switch 3 (38)______________________________________Store Position 1 -- --Ground Commanduncompensated 2 -- --compensated 3 1 --Program Track 3 2 1(corrected)Acquisition 3 2 1Autotrack 3 2 2______________________________________
If the first switch 36 (switch 1)is in position 1, the antenna 11 is in a "store" mode and is steered to a predetermined desired orientation with respect to the spacecraft 12 and then left there. This position may be such as to minimize solar torques on the spacecraft 12. If the first switch 36 is in position 2, the gimbal 13 is in an "uncompensated ground command mode," and is steered to a ground-commanded desired position with respect to the spacecraft 12. If the first switch 36 is in position 3 and the second switch 37 (switch 2) is in position 1, the gimbal 13 is in a "compensated ground command mode." In this mode, the gimbal 13 is served to a desired ground-commanded inertial orientation, and spacecraft 12 motion is compensated for by adding in a signal representing the orientation of the spacecraft 12 ("spacecraft motion compensation"). The orientation of the spacecraft 12 is typically derived by sensors disposed on the spacecraft 12 (for example, star sensors or gyros). The accuracy of the control provided by this mode is limited by the accuracy of the sensors and the accuracy of knowledge of target position.
If the first switch 36 is in position 3 and the second switch 37 is in position 2, (with the third switch 38 open in position 1 ), the gimbal 13 is in a "corrected program track mode." This mode is similar to the compensated ground command mode, except that instead of a real-time ground commanded position, a stored commanded position profile is used. This profile may, for example, be stored in the form of a table lookup or as a polynomial function that is evaluated on the spacecraft 12. This is a "program track" mode of operation.
"Acquisition" mode is functionally equivalent to the "corrected program track mode, " in that all switch positions are the same, except that a target search profile is superimposed onto the program track profile.
The inner and outer loop autotrack reference provided by the gimbal control system 10 will now be described. Assume that the gimbal control system 10 is in the corrected program track mode (i.e., the first switch 36 is in position 3, the second switch 37 is in position 2, and the third switch 38 is in position 1). If the target toward which the antenna 11 is steered is an autotracking target (i.e., if it has a communications signal that is used as an autotrack reference), then the autotrack signal strength is monitored by the autotrack receiver 19. When the autotrack signal strength has exceeded a predetermined threshold, the autotrack reference is declared present and the third switch 38 is closed (position 2). At that instant, an autotrack error signal is available for controlling the gimbal 13. As is shown in FIG. 2, the autotrack signal is a direct measurement of the boresight angle of the antenna 11 with respect to the target. The description below illustrates how the autotrack signal is used in combination with the resolver signal to control the gimbal 13.
The autotrack error signal from the autotrack receiver 19 is typically processed by a low-pass analog filter or anti-aliasing filter 33 to remove high-frequency noise. It is often the case that the autotrack receiver 19 uses analog electronics and thus the raw autotrack error signal is analog, while the remainder of the control algorithms are performed digitally. If this is the case, the autotrack error signal is digitized (A/D converted) by an A/D converter 34 prior to further processing. In this case, it is important that the analog low-pass filter 33 have its cutoff frequency set below half the sample frequency of the ND converter 34. After A/D conversion, the signal may be low-pass filtered by a second low-pass filter (not shown).
In prior art control systems, the autotrack error signal is used directly in place of the resolver signal in the gimbal control loop. The distinguishing feature of the present invention is that even when the autotrack error signal is present and is used, the resolver signal and the program track reference command are used simultaneously. How this is done is described in detail below.
In the gimbal control system 10 of the present invention, following low-pass filtering of the autotrack signal in the filter 33 and conversion to a digital signal in the A/D converter 34, it is passed through a P-I (proportional-integral) filter 35. The P-I filter 35 has a continuous-time transfer function given by ##EQU1##
The equivalent of the P-I filter 35 may be digitally implemented. The output of the P-I filter 35 is then added to the program track profile 41 following the third switch 38, and from that point the remainder of the gimbal control system 10 is as described previously, in that the third switch 38 is closed but the program track profile 41 is still used.
The combination of the anti-aliasing low-pass filter 33 and the P-I filter 35 ideally result in a low-bandwidth reference signal, in that this signal has its cutoff frequency below that of the inner-loop 21 incorporating resolver feedback used in the gimbal control system 10. In this case, the autotrack signal results in an accurate, but slowly-varying, correction to the stored program track profile 41 equal to the deviation of the actual target position from the stored program track profile. In the steady-state, the output of the P-I filter 35 is exactly this difference. In the steady-state, the input to the P-I filter 35 is zero because the closed-loop action of the two-loop gimbal control system 10 causes the antenna 11 to track exactly on the target, and the sensed autotrack error to be zero. The output of the P-I filter 35 is equal and opposite to the program track error. In the steady-state, the sum of the program track profile 41 and the output of the P-I filter 35 define the exact target position. This summed signal is the input to the inner control loop 21. As the target moves, this input signal matches the target's position with small deviations due to disturbances and noise. The inner control loop 21 servoes the gimbal 13 to track this commanded profile, and the compensation provided by the P-I filter 35 corrects the commanded profile to null the small deviations from the exact target position, resulting in exactly the gimbal motions necessary to track the target.
The benefit of using the inner control loop 21 in combination with the outer control loop 23 even after acquiring the autotrack reference signal is that the resolver is an inherently less noisy sensor than the autotrack signal and allows for a higher-bandwidth, higher-performance control system 10 than that which could be obtained using the autotrack signal 18c alone. Gimbal control may be performed with the commanded program track profile 41 as a reference to the resolver-based inner control loop 21. The inner control loop 21, along with the use of spacecraft motion compensation, tracks out most disturbances resulting from the body of the spacecraft 12 ("spacecraft bus motion"). The autotrack signal provides a low-bandwidth correction signal for the relatively fast inner control loop 21 to correct for unknown biases and unknown motions of the target.
An added benefit of using the output of the resolver 14 as the main feedback signal is that the control system 10 is less sensitive to flexibility of the gimbal 13 or antenna 11, since the resolver 14 is co-located with the gimbal 13. An alternative is to use the autotrack receiver 19 as the primary feedback sensor, augmented with feedforward of the spacecraft bus motion. This combination offers no direct measurement of gimbal deflections due to flexibility, and the control bandwidth is more limited by the need to stabilize gimbal flexible interactions. Thus, using the resolver 14 in the inner control loop 21 allows for active control of the gimbal flexible dynamics and therefore a higher-bandwidth control system 10 with the same gimbal stiffness, or an equal bandwidth control system 10 with a lighter-weight, less stiff gimbal 13. The above discussion refers to flexibility between the resolver and the autotrack sensor. Resolver feedback does not mitigate flexibility between the gimbal drive and resolver feedback (this would typically be flexibility in the gear train).
If the program track profile disappears (for example, if the commands are inadvertently exhausted), the present gimbal control system 10 still operates. Assuming that the most recent value of the program track profile 41 is stored, after the program track ceases to be updated, the output of the P-I filter 35 steadily grows to equal the difference between the current target position and the most recent value of the program track profile. Depending on how the parameters of the gimbal control system 10 are selected, it may be made to behave arbitrarily close to the behavior of a control loop with autotrack feedback alone.
Logic that provides for automatic mode control will now be described. FIG. 5 is a state diagram showing an example of mode control and transitioning logic 60 which may be supported by the gimbal control system 10 described herein. All but one of the antenna control modes shown in FIG. 5 are as in Table 1. "Slew" mode is a special case of program track mode, in which the antenna 11 tracks a predetermined profile using only the resolver reference but compensates for the attitude of the spacecraft 12. The slew mode is used to steer the antenna 11 over large angles to its next target, and is only different from program track mode in that the control gains may be different (typically higher). Also, as stated above, the "acquisition" mode is another special case of the program track mode, during which the autotrack electronics are searching for the autotrack signal. The acquisition mode may include a search pattern superimposed on the program track profile, and again the control gains could be different (typically higher).
FIG. 5 is believed to be relatively self-explanatory. Starting from store mode 61, upon receipt of a command to begin (or return to) service and the appropriate steering profile, the control system 10 is switched to slew mode 62. Then, when the antenna 11 has reached the nominal position of its target, the logic 60 is switched to program track mode 63. If autotrack service is requested, the electronics searches for the autotrack present signal and switches to acquisition mode 64. Upon receipt of the autotrack present signal, control is switched to autotrack mode 65. If the autotrack signal is lost, control is switched back to acquisition mode, and if the signal does not reappear within some length of time, control is switched back to program track mode 63. If the service times out, the antennas may be stopped where they are or may be commanded to store mode 61. Provision is also provided for direct ground command of the gimbal, shown as 67 in FIG. 5.
In one alternative implementation of the present invention, the spacecraft attitude is not available. This might be true, for example, if the antenna 11, the gimbal 13, and its control electronics are delivered as an independent package to be integrated with the spacecraft 12 at a later time. In this case, the best that can be done is to assume the spacecraft motions are negligible and set the spacecraft motion compensation signal of FIG. 2 to zero.
Thus there has been described a new and improved gimbal control system that employs inner and outer control loops. It is to be understood that the above-described embodiment is merely illustrative of some of the many specific embodiments which represent applications of the principles of the present invention. Clearly, numerous other arrangements can be readily devised by those skilled in the art without departing from the scope of the invention.
|
A multi-loop control system for a gimballed antenna that employs devices for measuring both absolute line-of-sight (an autotrack receiver or beacon tracker) and relative angular position (a resolver). The control system uses both signals simultaneously, thereby increasing the performance and pointing accuracy capability. Two control loops operate simultaneously to provide for optimum performance. The first loop is an inner high-bandwidth control loop that uses the relative gimbal angle measurement to control pointing of the antenna along a precommanded profile. The inner loop may run alone to provide for coarse pointing. When available, the line-of sight measurement is used in a low-bandwidth outer loop to provide corrections to the command profile of the inner loop. Control logic is provided that allows switching between several control modes. By using the present invention, antenna tracking control performance is maximized, especially in the presence of attitude disturbances of a spacecraft or significant flexible interactions.
| 1
|
TECHNICAL FIELD
[0001] The present invention relates to exhaust emission control systems for internal combustion engines; more particularly, to methods for regenerating a particulates filter for exhaust gas in an engine exhaust system; and most particularly, to a method for optimizing timing of such regeneration and for controlling temperature in a particulates filter during regeneration thereof to prevent thermal damage to the filter.
BACKGROUND OF THE INVENTION
[0002] Internal combustion engine exhaust emissions, and especially diesel engine exhaust emissions, have recently come under scrutiny with the advent of stricter regulations, both in the U.S. and abroad. While diesel engines are known to be more economical to run than spark-ignited engines, diesel engines inherently suffer disadvantages in the area of emissions. For example, in a diesel engine, fuel is injected during the compression stroke, as opposed to during the intake stroke in a spark-ignited engine. As a result, a diesel engine has less time to thoroughly mix the air and fuel before ignition occurs. The consequence is that diesel engine exhaust typically contains incompletely burned fuel known as particulate matter, or “soot”.
[0003] It must be noted that other types of internal combustion engine ignition processes are also known to produce soot in the exhaust, for example, direct injection gasoline engines. Hence, the problem addressed by the present invention is broader than just diesel exhaust soot, although that is the largest application for the present invention at the present time. For this reason, the terms “catalytic diesel particulate filter (CDPF)” and “diesel particulate filter (DPF)” as used herein should not be limited to diesel engines but rather must be taken to mean a particulate filter for capturing soot particles in any internal combustion engine exhaust.
[0004] It is known to use catalytic particulate filters which physically trap soot particulates. However, such particulate filters progressively load up with accumulated soot and therefore must be repeatedly regenerated by burning off the trapped particulates, typically on a fixed schedule and by fuel and oxygen enrichment of the exhaust stream entering the CDPF and catalytically ignited in an integral diesel oxygen catalyst (DOC).
[0005] Typically, prior art regeneration systems are temperature based with the primary filter protection strategy being limitation of the quantity of soot allowed to accumulate. As shown below, such a strategy can under-utilize the filter capacity by frequent regeneration on a conservative schedule and thus result in a penalty in fuel economy.
[0006] A currently challenging durability issue in the CDPF art is cracking or melting of a CDPF substrate due to large temperature excursions within the bed of the filter during regeneration, especially when using an economical filter such as a cordierite monolith. These temperature excursions are caused by the exothermic reaction of carbon and oxygen due to the combined effects of the mass loading and distribution of wet volatile and dry soot within the CDPF, the operating condition of the engine, and the exhaust gas temperature and flow rate through the CDPF. Diesel engine exhaust temperatures are normally in the range of 200-500° C., depending in part on the amount of exhaust gas recirculation, throttle plate position (MVRV—Manifold Vacuum Regulator Valve) and fueling. These engine control parameters, in combination with the manipulation of both fuel quantity and timing in the main fueling and post fueling events, may be used to increase exhaust gas temperature in the range of 500-700° C. as an effective means of initiating a regeneration event and as a means of controlling exhaust gas temperatures supplied to the CDPF during the regeneration process. During regenerative events, when the exhaust gas contains sufficient available oxygen to support the O 2 transport process (typically, 5-11%) and an adequate (actual mass depends upon wet/dry soot ratio and total mass) non-homogeneous distribution of wet and dry soot is resident within the CDPF, a highly non-uniform uncontrolled reaction can occur within the CDPF. This rapid, non-uniform reduction of wet and dry soot within the CDPF under various conditions of engine load and exhaust gas temperature and flow may result in excessive thermal gradients and peak monolith temperatures that exceed the material capabilities of the substrate material. This combination of events (rapid oxidation and inadequate heat transfer due insufficient exhaust gas flow) can result in excessive filter temperature and/or temperature gradients, resulting in substrate failure.
[0007] A factor not recognized in prior art CDPF regeneration is the relative combustibility difference between “wet” soot and “dry” soot, both of which can be present in a CDPF. By “wet soot” is meant soot particles coated with residual diesel fuel, such as may be generated during periods of high engine load but low engine speed, for example when pulling a heavy vehicle load up a substantial incline in a relatively high gear. Conversely, dry soot may be generated during periods of low engine load and high engine speed, such as at constant highway vehicle speeds. Wet soot burns substantially hotter that dry soot during catalytic regeneration. Indeed, wet soot is inherently rich in hydrocarbons that can explosively ignite, either spontaneously or when regeneration is started, and create an intense exothermic reaction within the CDPF in which temperatures can rise rapidly and uncontrollably (“flash-over”). Further, such intense combustion may occur nonuniformly over a CDPF, creating thermal stresses that can cause cracking or melting of the monolith, resulting in filter failure. Such flash-over is analogous to a creosote fire in a wood stove or fireplace chimney flue.
[0008] U.S. Pat. No. 6,735,941 B2 discloses a method for calculating the total soot mass accumulated in a CDPF by measuring differential pressure across the CDPF. This method does not recognize the functional (combustibility) difference between wet soot and dry soot; does not determine the percentage of total soot that is wet soot; and does not provide a strategy for burning off the wet soot in a controlled manner before completing oxidation of the dry soot, to protect against thermal damage to a CDPF.
[0009] What is needed in the art is a method for continuously calculating the total soot load and the wet soot fraction of the soot load in a CDPF and determining a relative Combustibility Index for the overall soot content.
[0010] It is a principal object of the present invention to prevent damage to a CDPF substrate by overheating during regeneration thereof, by continuously calculating a Combustibility Index for the soot load within a CDPF.
[0011] It is a further object of the present invention to improve engine fuel economy by conducting CDPF regeneration only when needed, as indicated by the Combustibility Index, rather than on a fixed schedule.
SUMMARY OF THE INVENTION
[0012] Briefly described, a method in accordance with the invention for triggering a new regeneration event in a soot-trapping device disposed in an exhaust gas stream of an internal combustion engine comprises the steps of:
[0013] a) determining instantaneous engine speed and engine load;
[0014] b) determining instantaneous mass fractions for wet soot and for dry soot in said exhaust gas stream for said instantaneous engine speed and load;
[0015] c) determining instantaneous concentrations of wet and dry soot particles in said exhaust gas;
[0016] d) determining the rates of accumulation of wet soot and dry soot in said soot-trapping device;
[0017] e) determining the total amounts of wet soot and dry soot accumulated in said soot-trapping device during all engine operation conditions since the latest previous regeneration event; and
[0018] f) triggering said new regeneration event when said total amounts of wet soot and dry soot exceed a permissible value.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The present invention will now be described, by way of example, with reference to the accompanying drawing, in which:
[0020] FIG. 1 is table showing percentages of wet soot and dry soot in diesel exhaust under varying engine operating conditions of speed and load; this table may be used as a means of determining instantaneous engine out volatility; in a full control embodiment, this table would be utilized in an interpolated format.
[0021] FIG. 2 is a table showing concentrations of wet soot and dry soot in diesel exhaust under the engine operating conditions shown in FIG. 1 ; this table may be used as a means of relating instantaneous wet soot equivalent accumulation rate (parts/million) as a function of instantaneous volatility index; in a full control embodiment, this table would be utilized in an interpolated format.
[0022] FIG. 3 is a set of graphs showing the allowable total mass accumulation as a function of wet/dry composition of the soot over a period of engine operation (accumulation time); and
[0023] FIG. 4 is a graph showing the total allowable soot mass to trigger a regeneration event as a function of the instantaneous percent of wet soot resident on a DPF.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0024] The present invention recognizes that combustibility of a soot load in a CDPF at any point in time during operation of a diesel engine is a function of both the Total Soot Mass and the Wet Soot Percentage. In addition, a forecast of instantaneous combustibility in the near future may be made by determining the rate of change in the Wet Soot Percentage and the Equivalent Accumulation Rate of soot in the CDPF.
[0025] Referring to FIG. 1 , the table 10 shows that the percent wet soot and percent dry soot that is produced and emitted per unit time by an engine under different operating conditions of speed and load, and can be used in a calculation of soot volatility. The soot fractions in each region will always total 1.0. The soot components produced by the engine are fundamentally related to the engine operating conditions based primarily on torque/engine load versus RPM (revolutions per minute). As engine power has a fundamental relationship with these parameters, the nature of the combustion occurring under various conditions of load affect both the amount and the chemical composition of the soot particulates that are formed based upon such combustion parameters as oxygen availability, flame front propagation and temperature, quenching, and various other reactions within the chamber environment. As such, the method disclosed herein relates the empirical productive soot output in the exhaust stream to the load conditions to which the engine is responding.
[0026] Presently, there exist no modeling or predictive representations that can accurately estimate exhaust stream particulate emissions or soot distribution within the DPF. However, as these tools are developed they may be directly applied to this methodology. Additionally, the selection of nine regions for the maps 10 , 20 depicted in FIGS. 1 and 2 is arbitrary and may be expanded to meet the control resolution requirements for a particular application. As the wet soot fraction, defining a Wet Soot Volatility Index value, is an indicator of soot volatility within a DPF, this parameter can be used as an indicator of flashover potential (excessive exothermic release) that exists based upon the total soot composition that is resident in the DPF at any time.
[0027] Referring to FIG. 2 , once the primary engine map 10 for soot composition is known ( FIG. 1 ), the fractional values can be applied through molar conversion to obtain the dry soot mass and wet soot mass components 20 in parts per million (ppm) of exhaust gas as a function of mass flow rate of air and fuel through the engine.
[0028] As any given accumulation of wet and dry soot produced by the engine is time dependent, the total mass of wet and dry soot per unit time can be determined by integration of the respective components (ppm or micrograms/sec) over discrete time steps within the control embodiment on the order of ten milliseconds (0.01 seconds) or less. Consequently, the mass quantity of both wet soot and dry soot can be determined for a measured period of operation. Additionally, since the effect of exhaust gas temperature and flow on wet soot phase conversion are known (conversion of wet soot in the CDPF to dry soot by exhaust drying), these integrators (up/down) can be modified to account for wet soot drying and reduction effects and allow for even greater accuracy.
[0029] Once the fractional relationship of wet soot and dry soot production for each region of FIGS. 1 and 2 is known and the complimentary soot mass is known, the soot composition and respective mass values resident on the filter can be accurately estimated for any given point in the DPF control cycle. This information can then be used to determine the best accumulation and regeneration strategy to be employed in order to minimize the potential for flashover that can result in excessive temperature rise, thermal gradients, or catastrophic filter failure. An additional benefit is realized from this strategy as the filter capacity can be efficiently utilized, the number of regeneration cycles minimized, and fuel penalty for active regenerations reduced.
[0030] Since volatility is the primary indicator for DPF control decisions in this strategy, the Effective Volatility of the soot emissions produced by the engine for any given time interval is arrived at by means of the following relationship:
[0000]
To calculate effective_volatility; integrate Instantaneous volatility (Table I) over time;
effective_volatility
=
f
t
t
+
dt
mass_flow
*
vol_index
(
Tq
,
RPM
)
*
Total_ppm
*
dt
f
t
t
+
dt
mass_flow
*
Total_ppm
*
dt
To calculate soot mass accumulated by DPF;
m
soot_inside
_DPF
=
C
eff
f
mass_flow
*
ppm
*
dt
Where: C eff = Filtration Efficiency
Total_ppm = Total soot parts per million; where:
Total_ppm = wet_soot_emission (Tq, RPM) + dry_soot_emission (Tq, RPM); Ref. FIG. 2
[0031] This measure of instantaneous effective volatility represents flammability of the physical soot composition accumulated in a DPF and is the indicator that is employed as a decision trigger in various embodiments of DPF control strategies. As effective volatility is a proportion of wet soot fraction to total soot, it will always fall between the values of 0-1.0. Once determined, this index value is a universal value within the control context regardless of the absolute magnitude of mass accumulation.
[0032] How is effective volatility used? Once the Instantaneous Volatility Index Value is known, it can be directly referenced to the Instantaneous Wet Soot Equivalent Accumulation Rate of mass production via the relationship indicated in FIG. 2 and the formula for ppm above.
[0033] How can this virtual soot sensor be utilized? The Wet Soot Mass Up/Down Integrator 30 represented schematically in FIG. 3 continuously integrates the Instantaneous Wet Soot Equivalent Accumulation Rate in micrograms/sec. This allows for both the total soot and the total wet soot mass quantity produced by the engine over a given time period to be known. The Up/Down Integrator 30 incorporates a provision for discounting the portion of the wet soot that is driven out of solution or dried out over time as a function of exhaust gas flow and temperature. By integrating the components of wet and dry engine out soot mass over time as a function of load and speed, a more accurate means of soot load determination for downstream devices (not just the DPF) is known versus using a proxy measure such as delta-pressure. This enables higher storage utility of the DPF and results in a variable state control method indicated by FIG. 3 , which thus is an Equivalent Soot Mass Integrator.
[0034] FIG. 3 is a representation of a multi-slope, multi-threshold control scheme that can be implemented once the instantaneous wet soot fraction and total soot mass is known. This knowledge enables a control scheme that can selectively utilize any of three different primary regeneration strategies based upon the volatility estimate of the soot load produced by the engine over a given time period:
Strategy 1: Active Regen—A regeneration process wherein fuel (hydrocarbons) is added to the exhaust stream and oxidized across a Diesel Oxidation Catalyst to elevate the exhaust gas temperature to the ignition temperature of the soot mass contained within the DPF. Strategy 2: Opportunistic regen—A regeneration process wherein the normal operating condition of the engine produces sufficient hydrocarbons to elevate the exhaust gas temperature to the ignition temperature of the soot mass contained within the DPF. Strategy 3: Preemptive regen—A regeneration process wherein an early active or opportunistic regeneration is allowed to occur based upon the occurrence of a large proportion of wet soot being present in the DPF (a high value of effective-volatility). The term “early” should be taken to mean ahead of the next expected regeneration event.
[0038] Note that pre-emptive regen is necessary whenever adequate wet soot is present on the filter, although not necessarily the allowable based upon the Total Soot Mass Regen Target value, and the engine operating condition is atypical. Such a situation exists in an event such as a diesel pulling a heavy load with a relatively high wet soot mass on the filter. If this vehicle were to chance encounter a steep grade over an extended period of time, the engine will begin to operate at extreme power and rpm levels and produce extreme exhaust temperatures and emission products. This may be adequate to light off the Diesel Oxygen Catalyst and the soot load within the DPF in an uncontrolled manner. The wet soot quantity has not met the Target Soot Mass Regen Target value for the active regen process, but the engine operating condition is at an extreme operating point for an extended period, an outlier condition.
[0039] This is not the only such extreme condition. One cannot base all potential region heuristics on this case as the system would then encounter unnecessary regen cycles under normal, typical, conditions. However, provisions must be made for this type of control scenario as it will occur periodically and can result in a melted or cracked filter monolith if left undetected and uncontrolled.
[0040] In FIG. 3 , a first example 32 , shown as Case A, is a soot accumulation profile wherein dry soot is accumulated for the first 2700 seconds of engine operation. At point 33 , the engine then shifts into a operating regime for the next 800 seconds wherein the soot comprises about 40/60 wet/dry. At point 34 , the engine shifts back to the original dry soot operating condition. An Equivalent Soot Mass Target Load 35 (Point A) of 45 grams is reached after a total operating time of 7200 seconds, triggering a regeneration event before a dangerously combustible condition develops in the DPF.
[0041] A second example 36 , shown as Case B, is a soot accumulation profile wherein 60/40 wet/dry soot is accumulated for the first 1500 seconds of engine operation. At point 37 , the engine then shifts into a operating regime for the next 600 seconds wherein the soot comprises 100% wet soot. At point 38 , the engine shifts to a dry soot operating condition. An Equivalent Soot Mass Target Load 39 (Point B) of 33 grams is reached after a total operating time of 2900 seconds, triggering a regeneration event before a dangerously combustible condition develops in the DPF.
[0042] How are effective volatility, integrated wet and dry soot mass and accumulated wet and dry soot mass values used in a grand control scheme? Once these parameters are known, it is possible to control a downstream device such as a DPF based upon a primary indicator rather than a proxy indicator such as delta-pressure. In this control method, the knowledge of the proportional relationship between wet (very volatile) soot and dry (less volatile) soot is used as a primary indicator of the need for DPF regeneration at any given time. If a relatively low quantity of total soot is resident on the filter monolith, but is composed of a high proportion of wet volatile soot, the control algorithm can intervene and prevent an uncontrolled flashover (high temperature thermal gradient) by initiating an active controlled regeneration process. Additionally, under certain circumstances dependent upon total soot mass, wet soot proportion and engine operating condition, this information can be used to allow an un-commanded, opportunistic regen to occur due to normal exhaust gas temperature rise without incurring the associated fuel penalty of an active regeneration, thus saving on fuel expenditure per unit of engine operating time. Finally, if the filter soot load accumulation is determined to be composed mostly of dry, less volatile soot, with an adequately low proportion of wet volatile soot, the accumulation period can be extended beyond any “scheduled” regeneration trigger to maximize the time between regenerations. This enables full utilization of the DPF capacity (high efficiency operation) resulting in a further reduced fuel penalty by minimizing the total number of regens required over a given operating cycle. This also has the associated benefit of reduced monolith and catalyst aging effects associated with large numbers of regeneration cycles and results in increased filter durability and longevity.
[0043] The threshold at which active regen intervention is required based upon the effective_volatility index-Instantaneous Percent Wet Soot Resident On DPF Filter (%) (fraction) is illustrated in FIG. 4 . From the Regen Equivalent Soot Mass Target, it can be seen that as the proportion 40 of wet volatile soot resident within the filter at any given instant as a function of total soot present increases, the corresponding Total Soot Mass Regen Target 50 goes down. This is due to the necessity of controlling the rate at which exothermic energy is released within the filter. As the proportion of wet soot to total soot increases, the rate at which exothermic heat is released also increases. This rapid, uncontrolled release of heat is what leads high thermal stress gradients, cracked DPF monoliths, and degraded catalyst performance over time.
[0044] In a continuous time domain, the equation form is:
[0000]
wet_soot
_accum
_mass
=
f
t
t
+
dt
M
A
F
*
wet_soot
_emission
(
Tq
,
R
P
M
)
*
d
t
Where
;
(
Tq
,
R
P
M
)
are
referenced
from
Fig
.
2
Soot
ppm
Table
[0000] Where: MAF=instantaneous engine mass air flow value
soot_emission=the value obtained from look up FIG. 2 , interpolated (controller function) as a function of torque and rpm for greater accuracy. dt=time interval.
[0047] Converting this equation form to a discrete time domain that is usable within a controls environment yields:
[0000]
Wet_soot
_accum
_mass
=
n
t
N
t
+
dt
M
A
F
t
=
tN
*
wet_soot
_emission
(
Tq
,
R
P
M
)
t
=
tN
*
d
t
Where
;
(
Tq
,
R
P
M
)
are
referenced
from
Fig
.
2
Soot
ppm
Table
[0048] Case 1: Integration series of instantaneous wet soot mass. The following example illustrates a low wet soot accumulation scenario:
[0049] Engine operation: low load and rpm operations predominately within Regions I, II, III, and IV in FIGS. 1 and 2 .
[0000]
Wet_soot
_accum
_mass
=
n
t
1
t
+
dt
[
(
M
A
F
t
=
t
1
*
wet_soot
_emission
(
Tq
,
R
P
M
)
t
=
t
1
*
d
t
)
+
(
M
A
F
t
=
t
2
*
wet_soot
_emission
(
Tq
,
R
P
M
)
t
=
t
2
*
d
t
)
+
(
M
A
F
t
=
t
3
*
wet_soot
_emission
(
Tq
,
R
P
M
)
t
=
t
3
*
d
t
)
+
(
M
A
F
t
=
t
N
*
wet_soot
_emission
(
Tq
,
R
P
M
)
t
=
t
N
*
d
t
)
]
Where
;
(
Tq
,
R
P
M
)
are
referenced
from
Fig
.
2
Soot
ppm
Table
[0000] Hence, utilizing the data values (non-interpolated) from FIG. 2 :
[0000]
From FIG. 2. Soot ppm Table
Time
Region
Tq
RPM
ws (ppm)
ds (ppm)
t 1
I
68
1250
0.05
0.02
t 2
II
68
1750
0.41
0.17
t 3
III
68
2250
1.40
0.47
t 4
IV
200
1250
0.17
0.04
t 5
II
68
1750
0.41
0.17
Wet_soot
_accum
_mass
=
∏
T1
-5
t
+
dt
[
(
MAF
t
=
t1
*
0.05
ppm
*
dt
)
t
=
t1
+
(
MAF
t
=
t2
*
0.41
ppm
*
dt
)
t
=
t2
+
(
MAF
t
=
t3
*
0.17
ppm
*
dt
)
t
=
t3
+
(
MAF
t
=
t4
*
1.40
ppm
*
dt
)
t
=
t4
+
(
MAF
t
=
t5
*
0.41
ppm
*
dt
)
t
=
t5
+
(
MAF
t
=
tN
*
wet_soot
_emission
(
Tq
,
RPM
)
t
=
tN
*
dt
)
t
=
tN
]
(Note:
Data are drawn from FIG. 2, Region I, Region II,
Region III, Region IV, and Region II consecutively.)
[0050] For a time step equal to 0.2 seconds, the first five elements of the series would represent the operational dither of wet soot production over a period of 1 second. Carrying this series forward over a time of N seconds would result in a wet soot mass value of 4.3 grams.
[0051] Concurrent with the calculation of wet soot mass accumulation, the dry soot mass accumulation is integrated by the same method in the form:
[0000]
dry_soot
_accum
_mass
=
n
t
1
t
+
dt
[
(
M
A
F
t
=
t
1
*
dry_soot
_emission
(
Tq
,
R
P
M
)
t
=
t
1
*
d
t
)
+
(
M
A
F
t
=
t
2
*
dry_soot
_emission
(
Tq
,
R
P
M
)
t
=
t
2
*
d
t
)
+
(
M
A
F
t
=
t
3
*
drt_soot
_emission
(
Tq
,
R
P
M
)
t
=
t
3
*
d
t
)
+
(
M
A
F
t
=
t
N
*
dry_soot
_emission
(
Tq
,
R
P
M
)
t
=
t
N
*
d
t
)
]
Where
;
(
Tq
,
R
P
M
)
are
referenced
from
Fig
.
2
Soot
ppm
Table
[0052] This yields the following:
[0000]
dry_soot
_accum
_mass
=
n
T
1
-
5
t
+
dt
[
(
M
A
F
t
=
t
1
*
0.02
ppm
*
d
t
)
t
=
t
1
+
(
M
A
F
t
=
t
2
*
0.17
ppm
*
d
t
)
t
=
t
2
+
(
M
A
F
t
=
t
3
*
0.04
ppm
*
d
t
)
t
=
t
3
+
(
M
A
F
t
=
t
4
*
47
ppm
*
d
t
)
t
=
t
4
+
(
M
A
F
t
=
t
5
*
0.17
ppm
*
d
t
)
t
=
t
5
+
(
M
A
F
t
=
tN
*
dry_soot
_emission
(
Tq
,
R
P
M
)
t
=
tN
*
d
t
)
t
=
t
N
]
[0000] (Note: Data are drawn from FIG. 2 , Region I, Region II, Region III, Region IV, and Region II consecutively.)
[0053] For a time step equal to 0.2 seconds, the first five elements of the series would represent the operational dither of dry soot production over a period of 1 second. Carrying this series forward over a time of N seconds would result in a dry soot mass value of 38.7 grams.
[0054] As established above, the effective_volatility is a determinant control metric that equates the relative instantaneous volatility of the total soot load resident on the filter as:
[0000]
effective_volatility
=
f
mass_flow
*
vol_index
*
ppm
*
d
t
f
mass_flow
*
ppm
*
d
t
(Note: mass_flow=total air and fuel throughput of the engine)
[0056] As the DPF accumulation times are significant, it is impractical to tabulate the entire time series data; for the purposes of example, the calculated effective volatility over N seconds for the sample case above results in an index value of 0.10.
[0057] Referencing Case 1 in FIG. 4 (item 100 ). Regen Equivalent Soot Mass Target: For an effective volatility value of 0.1, the allowable total mass accumulation target at which active regen is initiated would be equal to approximately 43 grams. This target mass is based on the relative heat release of wet soot and dry soot and the thermal margins necessary to protect the filter monolith from excessive thermal gradients and temperatures.
[0058] Case 2: Integration series of instantaneous wet soot mass.
[0059] Alternately, if the engine is operating in a region of high load, low rpm, the index and accumulation values would be, respectively:
[0000]
Time increment:
t1
t2
t3
t4
t5
Instantaneous engine out index (FIG. 1)
Wet soot:
.50
.60
.32
.30
.20
Dry soot:
.50
.40
.68
.70
.80
(FIG. 2 or FIG. 3 in micrograms/s)
Wet soot ppm:
2.21
0.69
2.65
1.63
0.23
Dry soot ppm:
2.21
0.46
5.62
3.80
2.93
(Note: Data drawn from FIGS. 1 and 2, Region V, Region VI, Region VII, Region VIII, and Region VII consecutively.)
[0060] For a time step equal to 0.2 seconds, the first five elements of this series would represent the operational dither of wet soot production over a period of 1 second. Carrying this series forward over a time of N seconds would result in a wet soot mass value of 7.2 grams.
[0061] For the same period and a time step equal to 0.2 seconds, the first five elements of this series would represent the operational dither of dry soot production over a period of 1 second. Carrying this series forward over a time of N seconds would result in a dry soot mass value of 4.8 grams.
[0062] In this extreme illustration of extended high load operation, for the purposes of example, the calculated effective volatility over N seconds for the sample case above results in an index value of 0.60.
[0063] Referencing Case 2 in FIG. 4 (item 200 ). Regen Equivalent Soot Mass Target: For an effective volatility value of 0.60, the allowable total mass accumulation target at which active regen is initiated would be equal to approximately 10 grams. Due to the relative high wet soot load and potential for highly localized heat release, the DPF must be actively regenerated at a total soot load far less than that of the previous example. This target mass is based on the relative heat release of wet soot and dry soot and the thermal margins necessary to protect the filter monolith from excessive thermal gradients and temperature.
[0064] This, in essence, is the usefulness of the volatility index method of predicting soot production and hence the timing of the next required regeneration event. The metrics of instantaneous volatility and effective volatility are used in conjunction with traditional engine mapping or simulation to produce a method of emission estimation measures for downstream device control and tailpipe emissions.
[0065] While the invention has been described by reference to various specific embodiments, it should be understood that numerous changes may be made within the spirit and scope of the inventive concepts described. Accordingly, it is intended that the invention not be limited to the described embodiments, but will have full scope defined by the language of the following claims.
|
A method for triggering a new regeneration event in a soot-trapping particulates filter disposed in an exhaust gas stream of an internal combustion engine, comprising the steps of determining instantaneous engine speed and engine load; determining instantaneous mass fractions for wet soot and for dry soot in the exhaust gas stream for the instantaneous engine speed and load; determining instantaneous concentrations of wet and dry soot particles in the exhaust gas; determining the rates of accumulation of wet soot and dry soot in the particulates filter; determining the total amounts of wet soot and dry soot accumulated in said soot-trapping device during all engine operation conditions since the latest previous regeneration event; and triggering the new regeneration event when the total amount of wet soot and dry soot exceeds a permissible value.
| 5
|
This application is a continuation-in-part of application Ser. No. 07/992,700 filed on Dec. 18, 1992, now U.S. Pat. No. 5,520,916, 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 new non-woven fabric material comprising hyaluronic acid derivatives, methods of production thereof, and methods of using said material in medical and pharmaceutical applications.
2. Description of Related Art
Hyaluronic acid is a natural heteropolysaccharide composed of alternating residues of D-glucuronic acid and N-acetyl-D-glucosamine. It is a linear polymer with a molecular weight of between 50,000 and 13,000,000 depending upon the source from which it is obtained, and the preparation and determination methods employed. It is present in nature in pericellular gels, in the fundamental substance of connective tissues of vertebrate organisms of which it is one of the main components, in the synovial fluid of joints, in the vitreous humor, in human umbilical cord tissues, and in cocks' combs.
There are known, specific fractions of hyaluronic acid with definite molecular weights that do not present inflammatory activity, and which can therefore be used to facilitate wound healing, to substitute for the endobulbar fluids, or which can be employed in therapy for joint pathologies by intra-articular injections, as described in European Patent No. 0 138 572 granted to Applicants on Jul. 25, 1990.
Also known are hyaluronic acid esters, wherein all or some of the carboxy groups of the acid are esterified, and their use in the pharmaceutical and cosmetic fields and in the area of biodegradable plastic materials, as described in U.S. Pat. Nos. 4,851,521 and 4,965,353 granted to Applicants.
Hyaluronic acid is known to play a fundamental role in tissue repair processes, especially in the first stages of granulation, by stabilizing the coagulation matrix and controlling its degradation, favoring the recruitment of inflammatory cells such as polymorphonuclear leukocytes and monocytes, of mesenchymal cells such as fibroblasts and endothelial cells, and in orienting the subsequent migration of epithelial cells.
It is known that the application of solutions of hyaluronic acid can accelerate healing in patients affected by bedsores, wounds and burns. The role of hyaluronic acid in the various phases that constitute tissue repair processes has been described, by the construction of a theoretical model, by Weigel P. H. et al.: "A model for the role of hyaluronic acid and fibrin in the early events during the inflammatory response and wound healing," J. Theor. Biol., 119: 219, 1986.
Studies aimed at obtaining manufactured products to apply to the skin, composed of hyaluronic acid esters as such or in mixtures with other polymers have led to the creation of various types of products. Among these are fabrics, such as gauzes of varying thickness (number of threads per centimeter), with varying dimensions, and with threads of varying denier (weight per 9000 meters of thread). Films of widely varying thickness have been proposed, as described in U.S. Pat. Nos. 4,851,521 and 4,965,353.
The use of such materials as skin coverings is limited by their stiffness, which is more or less determined according to how they were made. It is always a problem, however, when the material has to mould itself to the surface to be covered. Another drawback to the use of such materials is their poor absorbability, if any, of liquids such as solutions of disinfectants, antibiotics, antiseptics, antimicotics, proteins or wound healing substances in general, even when these are neither thick nor viscous.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide pliable non-woven fabric materials.
It is also an object of the present invention to provide a method for the preparation of such non-woven fabric materials.
The non-woven fabric materials of the present invention include those composed of hyaluronic acid esters, used singly or in combination with one another or with other types of polymers, and those composed of crosslinked hyaluronic acid. Such materials are particularly soft, and can be easily impregnated with various kinds of liquids.
Further scope of the applicability of the present invention will become apparent from the detailed description and drawings provided below. However, it should be understood that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by way of illustration only since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features, and advantages of the present invention will be better understood from the following detailed descriptions taken in conjunction with the accompanying drawings, all of which are given by way of illustration only, and are not limitative of the present invention, in which:
FIG. 1 is a schematic diagram illustrating the steps involved in the production of the non-woven fabric material of the present invention.
FIG. 2 shows the appearance of the non-woven fabric material comprising the benzyl ester of hyaluronic acid, HYAFF 11, produced in Example 27.
DETAILED DESCRIPTION OF THE INVENTION
The following detailed description of the invention is provided to aid those skilled in the art in practicing the present invention. Even so, the following detailed description should not be construed to unduly limit the present invention, as modifications and variations in the embodiments herein discussed may be made by those of ordinary skill in the art without departing from the spirit or scope of the present inventive discovery.
The contents of each of the references cited in the present application are herein incorporated by reference in their entirety.
The objects of the present invention are achieved by non-woven fabrics according to the present invention weighing between about 20 gr/mq and about 500 gr/mq, and between about 0.2 mm and about 5 mm in thickness. The non-woven fabric can be described as a web composed of a large quantity of fibers varying in diameter between about 12 and about 60 micrometers and in length between about 5 mm and about 100 mm, joined together by chemical coagulation or mechanical means, or with the aid of cohesive material.
The non-woven fabric comprises hyaluronic acid esters used singly or in mixtures with each other in varying ratios. Moreover, the present non-woven fabrics can comprise mixtures of fibers of hyaluronic acid esters with fibers of natural polymers, varying in ratio from 1 to 100% of the total, such as collagen, or coprecipitates of collagen and glycosaminoglycans, cellulose, polysaccharides in gel form such as chitin, chitosan, pectin or pectic acid, agar, agarose, xanthan gum, gellan, alginic acid or alginates, polymannan or polyglycans, starches, natural gums, or fibers obtained from semisynthetic derivatives of natural polymers such as collagen cross-linked with agents such as aldehydes or precursors of the same, dicarboxylic acids or halides of the same, diamines, derivatives of cellulose, alginic acid, starch, hyaluronic acid, chitin or chitosan, gellan, xanthan, pectin, or pectic acid, polyglycans, polymannan, agar, agarose, natural gums, glycosaminoglycans, or fibers obtained from synthetic polymers, such as polylactic acid, polyglycolic acid or copolymers of the same or their derivatives, polydioxanes, polyphosphazenes, polysulfone resins, and polyurethane resins.
The non-woven fabrics of the present invention possessing the above-mentioned characteristics can be produced from multifilaments produced by the usual wet and dry spinning methods and then cut into the desired lengths. The mass of fibers is fed into a carding machine which makes it into staples. The staples are then fed into a cross lapper, from which they emerge as webs of a specific weight.
The web can undergo chemical or mechanical cohesive treatment such as soaking in solvents and subsequent coagulation, needle punching treatment, treatment with bonding agents of the same material as constitutes the non-woven fabric, or of a different material, etc.
With respect to mechanical cohesive treatment, the principal of reinforcement of the fibrous web is based on the entangling of the fibers and the increased fiber friction obtained by the consolidation of the fibrous web. The fibers are entangled by piercing the web vertically with felting needles. These needles are mounted in machines, and the fibrous web is fed to the needling machine for needling, and finally to a structuring machine, which carries out the surface structuring.
With respect to treatments with bonding agents, chemical cohesive treatment with bonding agents is performed on the fibrous web when it emerges from the carding machine (FIG. 1, detail 9). The purpose of this treatment is to fix the fibers at their contact points. In the case of non-woven fabrics composed essentially of hyaluronic acid esters, this is achieved by spraying (11) the fibrous web emerging from the carding machine with a solution of hyaluronic acid esters in, for example, dimethylsulfoxide. The dimethylsulfoxide, being a solvent for the fibers comprising the web, dissolves them, and "fuses" them in the subsequent coagulation bath (12). The web thus fixed is then washed (13) and dried (14).
The coagulation baths 3 and 15 are stainless steel, and are in the form of an upturned triangle so that the extracted solubilization material being formed can be kept in contact with fresh coagulation solvent.
The coagulation process is essentially an extraction process by which, from a solution of polymer and solvent, the extraction of the solubilization solvent and the solidification of the polymer can be effected by the addition of a second solvent, for example ethanol, in which the solubilization solvent, for example dimethylsulfoxide, is soluble, and the polymer is insoluble.
The above-described treatments have the effect of fixing the fibers one to the other so as to produce a structure composed of haphazardly placed, matted fibers, constituting a soft, resistant material.
The present invention therefore relates to a new class of products, non-woven fabrics, to be used in the medical/pharmaceutical field as skin coverings. These fabric materials are totally or partially biocompatible and bioabsorbable, and are composed of hyaluronic acid esters used singly or in mixtures with each other, or with other natural or synthetic polymers. Such materials are characterized by their softness, and by their ability to absorb liquids.
Such non-woven fabrics can be impregnated with a liquid or a gel, such as for example, among other things, solutions of antibiotics, antiseptics, antimicotics or proteins. The term "non-woven fabric" covers in practice materials such as webs and felts, etc., composed of a large quantity of fibers, chemically or mechanically stuck together. The material has the appearance of a fabric, even though it is not woven in the strict sense of the word.
For purely illustrative purposes, described hereafter are some examples of how the non-woven fabric material of the present invention can be produced.
The Esters of Hyaluronic Acid
Esters of hyaluronic acid useful in the present invention are esters of hyaluronic acid with aliphatic, araliphatic, cycloaliphatic or heterocyclic alcohols, in which are esterified all (so-called "total esters") or only a part (so-called "partial esters") of the carboxylic groups of the hyaluronic acid, and salts of the partial esters with metals or with organic bases, biocompatible or acceptable from a pharmacological point of view.
The useful esters include esters which derive from alcohols which themselves possess a notable pharmacological action. The saturated alcohols of the aliphatic series or simple alcohols of the cycloaliphatic series are useful in the present invention.
In the above mentioned esters in which some of the carboxylic acid groups remain free (i.e., partial esters), these may be salified with metals or organic bass, such as with alkaline or alkaline earth metals or with ammonia or nitrogenous organic bases.
Most of the esters of hyaluronic acid ("HY"), unlike HY itself, present a certain degree of solubility in organic solvents. This solubility depends on the percentage of esterified carboxylic groups and on the type of alkyl group linked with the carboxyl. Therefore, an HY compound with all its carboxylic groups esterified presents, at room temperature, good solubility for example in dimethylsulfoxide (the benzyl ester of HY dissolves in DMSO in a measure of 200 mg/ml). Most of the total esters of HY present also, unlike HY and especially its salts, poor solubility in water and are essentially insoluble in water. The solubility characteristics, together with particular and notable viscoelastic properties, make the HY esters particularly preferred for use in composite membranes.
Alcohols of the aliphatic series to be used as esterifying components of the carboxylic groups of hyaluronic acid for use in composite membranes according to the present invention are for example those with a maximum of 34 carbon atoms, which may be saturated or unsaturated and which may possibly also be substituted by other free functional or functionally modified groups, such as amine, hydroxyl, aldehyde, ketone, mercaptan, or carboxyl groups or by groups derived from these, such as hydrocarbyl or di-hydrocarbylamine groups (from now on the term "hydrocarbyl" will be used to refer not only to monovalent radicals of hydrocarbons such as the C n H 2n+1 type, but also bivalent or trivalent radicals, such as "alkylenes" C n H 2n or "alkylidenes" C n H 2n ), ether or ester groups, acetal or ketal groups, thioether or thioester groups, and esterified carboxyl or carbamide groups and carbamide substituted by one or more hydrocarbyl groups, by nitrile groups or by halogens.
Of the above mentioned groups containing hydrocarbyl radicals, these are preferably lower aliphatic radicals, such as alkyls, with a maximum of 6 carbon atoms. Such alcohols may also be interrupted in the carbon atom chain by heteroatoms, such as oxygen, nitrogen and sulfur atoms. Preferred are alcohols substituted with one or two of the said functional groups.
Alcohols of the above mentioned group which are preferably used are those with a maximum of 12, and especially 6 carbon atoms, and in which the hydrocarbyl atoms in the above mentioned amine, ether, ester, thioether, thioester, acetal, ketal groups represent alkyl groups with a maximum of 4 carbon atoms, and also in the esterified carboxyl or substituted carbamide groups the hydrocarbyl groups are alkyls with the same number of carbon atoms, and in which in the amine or carbamide groups may be alkylenamine or alkylencarbamide groups with a maximum of 8 carbon atoms. Of these alcohols, specifically preferred are saturated and non-substituted alcohols, such as the methyl, ethyl, propyl, and isopropyl alcohols, normal butyl alcohol, isobutyl alcohol, tertiary butyl alcohol, the amyl, pentyl, hexyl, octyl, nonyl and dodecyl alcohols and, above all, those with a linear chain, such as normal octyl and dodecyl alcohols. Of the substituted alcohols of this group, the bivalent alcohols are useful, such as ethyleneglycol, propyleneglycol and butyleneglycol, the trivalent alcohols such as glycerine, the aldehyde alcohols such as tartronic alcohol, the carboxylic alcohols such as lactic acids, for example glycolic acid, malic acid, the tartaric acids, citric acid, the aminoalcohols, such as normal aminoethanol, aminopropanol, normal aminobutanol and their dimethylated and diethylated derivatives in the amine function, choline, pyrrolidinylethanol, piperidinylethanol, piperazineylethanol and the corresponding derivatives of normal propyl or normal butyl alcohol, monothioethyleneglycol or its alkyl derivatives, such as the ethyl derivative in the mercaptan function.
Of the higher saturated aliphatic alcohols, preferred are cetyl alcohol and myricyl alcohol, but for the aim of the present invention the higher unsaturated alcohols with one or two double bonds, are especially important, such as especially those contained in many essential oils and with affinity to terpene, such as citronellol, geraniol, nerol, nerolidol, linalool, farnesol, phytol. of the unsaturated lower alcohols it is necessary to consider allyl alcohol and propargyl alcohol. Of the araliphatic alcohols, preferred are those with only one benzene residue and in which the aliphatic chain has a maximum of 4 carbon atoms, which the benzene residue can be substituted by between 1 and 3 methyl or hydroxyl groups or by halogen atoms, especially by chlorine, bromine and iodine, and in which the aliphatic chain may be substituted by one or more functions chosen from the group containing fee amine groups or mono- or dimethylated or by pyrrolidine or piperidine groups. Of these alcohols, most preferred are benzyl alcohol and phenetyl alcohol.
The alcohols of the cycloaliphatic or aliphatic-cycloaliphatic series may derive from mono- or polycyclic hydrocarbons, may preferably have a maximum of 34 carbon atoms, may be unsubstituted and may contain one or more substituents, such as those mentioned above for the aliphatic alcohols. Of the alcohols derived from cyclic monoannular hydrocarbons, preferred are those with a maximum of 12 carbon atoms, the rings with preferably between 5 and 7 carbon atoms, which may be substituted for example by between one and three lower alkyl groups, such as methyl, ethyl, propyl or isopropyl groups. As specific alcohols of this group the following are most preferred: cyclohexanol, cyclohexanediol, 1,2,3-cyclohexanetroil and 1,3,5-cyclohexanetriol (phloroglucitol), inositol, and the alcohols which derive from p-methane such as carvomenthol, menthol, and α-γterpineol, 1-terpineol, 4-terpineol and piperitol, or the mixture of these alcohols known as "terpineol", 1,4- and 1,8 terpin. Of the alcohols which derive from hydrocarbons with condensed rings, such as those of the thujane, pinane or comphane, the following are preferred: thujanol, sabinol, pinol hydrate, D and L-borneol and D and L-isoborneol.
Aliphatic-cycloaliphatic polycyclic alcohols to be used for the esters of the present invention are sterols, cholic acids and steroids, such as sexual hormones and their synthetic analogues, especially corticosteroids and their derivatives. It is therefore possible to use: cholesterol, dihydrocholesterol, epidihydrocholesterol, coprostanol, epicoprostanol, sitosterol, stigmasterol, ergosterol, cholic acid, deoxycholic acid, lithocholic acid, estriol, estradiol, equilenin, equilin and their alkylate derivatives, as well as their ethynyl or propynyl derivatives in position 17, such as 17α-ethynl-estradiol or 7α-methyl-17α-ethynyl-estradiol, pregnenolone, pregnanediol, testosterone and its derivatives, such as 17α-methyltestosterone, 1,2-dehydrotestosterone and 17α-methyl-1,2-dehydrotesterone, the alkynylate derivatives in position 17 of testosterone and 1,2-dehydrotestosterone, such as 17α-ethynyltestosterone, 17α-propynyltestosterone, norgestrel, hydroxyprogesterone, corticosterone, deoxycorticosterone, 19-nortestosterone, 19-nor-17α-methyltestosterone and 19-nor-17α-ethynyltestosterone, antihormones such as cyproterone, cortisone, hydrocortisone, prednisone, prednisolone, fluorocortisone, dexamethasone, betamethasone, paramethasone, flumethasone, fluocinolone, fluprednylidene, clobetasol, beclomethasone, aldosterone, deoxycorticosterone, alfaxolone, alfadolone, and bolasterone. As esterifying components for the esters of the present invention the following are useful: genins (aglycons) of the cardioactive glucosides, such as digitoxigenin, gitoxigenin, digoxigenin, strophanthidin, tigogenin and saponins.
Other alcohols to be used according to the invention are the vitamin ones, such as axerophthol, vitamins D 2 and D 3 , aneurine, lactoflavine, ascorbic acid, riboflavine, thiamine, and pantothenic acid.
Of the heterocyclic acids, the following can be considered as derivatives of the above mentioned cycloaliphatic or aliphatic-cycloaliphatic alcohols if their linear or cyclic chains are interrupted by one or more, for example by between one and three heteroatoms, for instance chosen from the group formed by --O--, --S--, --N,and --NH--, and in these, there may be one or more unsaturated bonds, for example double bonds, in particular between one and three, thus including also heterocyclic compounds with aromatic structures. For example the following should be mentioned: furfuryl alcohol, alkaloids and derivatives such as atropine, scopolamine, cinchonine, la cinchonidine, quinine, morphine, codeine, nalorphine, N-butylscopolammonium bromide, ajmaline; phenylethylamines such as ephedrine, isoproterenol, epinephrine; phenothiazine drugs such as perphenazine, pipothiazine, carphenazine, homofenazine, acetophenazine, fluophenazine, and N-hydroxyethylpromethazine chloride; thioxanthene drugs such as flupenthixol and clopenthixol; anticonvulsants such as meprophendiol; antipsychotics such as opipramol; antiemetics such as oxypendyl; analgesics such as carbetidine and phenoperidine and methadol; hypnotics such as etodroxizine; anorexics such as benzidrol and diphemethoxidine; minor tranquilizers such as hydroxyzine; muscle relaxants such as cinnamedrine, diphylline, mephenesin, methocarbamol, chlorphenesin, 2,2-diethyl-1,3-propanediol, guaifenesin, hydrocilamide; coronary vasodilators such as dipyridamole and oxyfedrine; adrenergic blockers such as propanolol, timolol, pindolol, bupranolol, atenolol, metroprolol, practolol; antineoplastics such as 6-azauridine, cytarabine, floxuridine; antibiotics such as chloramphenicol, thiamphenicol, erythromycin, oleandomycin, lincomycin; antivirals such as idoxuridine; peripheral vasodilators such as isonicotinyl alcohol; carbonic anhydrase inhibitors such as sulocarbilate; antiasthmatic and antiinflammatories such as tiaramide; sulfamidics such as 2-p-sulfanilonoethanol.
In some cases hyaluronic acid esters may be of interest where the ester groups derive from two or more therapeutically active hydroxylic substances, and naturally all possible variants may be obtained. Especially interesting are the substances in which two types of different ester groups deriving from drugs of a hydroxylic character are present and in which the remaining carboxyl groups are free, salified with metals or with a base, possibly also the bases being themselves therapeutically active, for example with the same or similar activity as that of the esterifying component. In particular, it is possible to have hyaluronic esters deriving on the one hand from an antiinflammatory steroid, such as one of those mentioned previously, and on the other hand from a vitamin, from an alkaloid or from an antibiotic, such as one of those listed.
Method of Preparing HY Esters of the Invention
Method A
The esters of hyaluronic acid may be prepared by methods known per se for the esterification of carboxylic acids, for example by treatment of free hyaluronic acid with the desired alcohols in the presence of catalyzing substances, such as strong inorganic acids or ionic exchangers of the acid type, or with an etherifying agent capable of introducing the desired alcoholic residue in the presence of inorganic or organic bases. As esterifying agents it is possible to use those known in literature, such as especially the esters of various inorganic acids or of organic sulphonic acids, such as hydracids, that is hydrocarbyl halogenides, such as methyl or ethyl iodide, or neutral sulphates or hydrocarbyl acids, alfites, carbonates, silicates, phosphites or hydrocarbyl sulfonates, such as methyl benzene or p-toluene-sulfonate or methyl or ethyl chlorosulfonate. The reaction may take place in a suitable solvent, for example an alcohol, preferably that corresponding to the alkyl group to be introduced in the carboxyl group. But the reaction may also take place in non-polar solvents, such as ketones, ethers, such as dioxane or aprotic solvents, such as dimethylsulphoxide. As a base it is possible to use for example a hydrate of an alkaline or alkaline earth metal or magnesium or silver oxide or a basic salt or one of these metals, such as a carbonate, and, of the organic bases, a tertiary azotized base, such as pyridine or collidine. In the place of the base it is also possible to use an ionic exchanger of the basic type.
Another esterification method employs the metal salts or salts with organic azotized bases, for example ammonium or ammonium substitute salts. Preferably, the salts of the alkaline or alkaline earth metals are used, but also any other metallic salt may be used. The esterifying agents are also in this case those mentioned above and the same applies to the solvents. It is preferable to use aprotic solvents, for example dimethylsulphoxide and dimethylformamide.
In the esters obtained according to this procedure or according to the other procedure described hereafter, free carboxylic groups of the partial esters may be salified, if desired, in a per se known manner.
Method B
The hyaluronic esters may also be prepared by a method which consists of treating a quaternary ammonium salt of hyaluronic acid with an etherifying agent, preferably in an aprotic organic solvent.
As organic solvents it is preferable to use aprotic solvents, such as dialkylsulphoxides, dialkylcarboxamides, such as in particular lower alkyl dialkylsulphoxides, especially dimethyl-sulphoxide, and lower alkyl dialkylamides of lower aliphatic acids, such as dimethyl or diethyl-formamide or dimethyl or diethylacetamide.
Other solvents however are to be considered which are not always aprotic, such as alcohols, ethers, ketones, esters, especially aliphatic or heterocyclic alcohols and ketones with a lower boiling point, such as hexafluoroisopropanol, trifluoroethanol, and N-methylpyrrolidone.
The reaction is effected preferably at a temperature range of between about 0° C. and 100° C., especially between about 25° C. and 75° C., for example at about 30° C.
The esterification is carried out preferably by adding by degrees the esterifying agent to the above mentioned ammonium salt to one of the above mentioned solvents, for example to dimethyl-sulphoxide.
As an alkylating agent it is possible to use those mentioned above, especially the hydrocarbyl halogens, for example alkyl halogens. As starting quaternary ammonium salts it is preferable to use the lower ammonium tetraalkylates, with alkyl groups preferably between 1 and 6 carbon atoms. Mostly, hyaluronate of tetrabutylammonium is used. It is possible to prepare these quaternary ammonium salts by reacting a metallic salt of hyaluronic acid, preferably one of those mentioned above, especially sodium or potassium salt, in aqueous solution with a salified sulphonic resin with a quaternary ammonium base.
One variation of the previously described procedure consists in reacting a potassium or sodium salt of hyaluronic acid, suspended in a suitable solution such as dimethylsulphoxide, with a suitable alkylating agent in the presence of catalytic quantities of a quaternary ammonium salt, such as iodide of tetrabutylammonium.
For the preparation of the hyaluronic acid esters, it is possible to use hyaluronic acids of any origin, such as for example the acids extracted from the above mentioned natural starting materials, for example from cocks' combs. The preparation of such acids is described in literature: preferably, purified hyaluronic acids are used. Especially used are hyaluronic acids comprising molecular fractions of the integral acids obtained directly by extraction of the organic materials with molecular weights varying within a wide range, for example from about 90%-80% (MW=11.7-10.4 million) to 0.2% (MW=30,000) of the molecular weight of the integral acid having a molecular weight of 13 million, preferably between 5% and 0.2%. Such fractions may be obtained with various procedures described in literature, such as by hydrolyzing, oxydizing, enzymatic or physical procedures, such as mechanical or radiational procedures. Primordial extracts are therefore often formed during these same by publication procedures (for example see the article by Balazs et al. quoted above in "Cosmetics & Toiletries"). The separation and purification of the molecular fractions obtained are brought about by known techniques, for example by molecular filtration.
Additionally useful are purified fractions obtainable from hyaluronic acid, such as for example the ones described in European Patent Publn. No. 0138572.
The salification of HY with the above metals, for the preparation of starting salts for the particular esterification procedure described above, is performed in a per se known manner, for example by reacting HY with the calculated base quantity, for example with alkaline hydrates or with basic salts of such metals, such as carbonates or bicarbonates.
In the partial esters it is possible to salify all the remaining carboxylic groups or only part of them, dosing the base quantities so as to obtain the desired stoichiometric degree of salification. With the correct degree of salification it is possible to obtain esters with a wide range of different dissociation constants and which therefore give the desired pH, in solution or "in situ" at the time of therapeutic application.
PREPARATION EXAMPLES
The following exemplify the preparation of hyaluronic acid esters useful in the composite membranes of the present invention.
Example 1
Preparation of the (Partial) Propyl Ester of Hyaluronic Acid (HY)
50% of the esterified carboxylic groups
50% of the salified carboxylic groups (Na)
12.4 g of HY tetrabutylammonium salt with a molecular weight 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 1.8 g (10.6 m.Eq.) of propyl iodide are added and the resulting solution is kept at a temperature of 30° for 12 hours.
A solution containing 62 ml of water and 9 g of sodium chloride is added and the resulting mixture is slowly poured into 3,500 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed three times with 500 ml of acetone/water 5:1 and three times with acetone and finally vacuum dried for eight hours at 30° C.
The product is then dissolved in 550 ml of water containing 1% of sodium chloride and the solution is slowly poured into 3,000 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed twice with 500 ml of acetone/water (5:1) and three times with 500 ml of acetone and finally vacuum dried for 24 hours at 30° C. 7.9 g of the partial propyl ester compound in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030, (1961)!.
Example 2
Preparation of the (Partial) Isopropyl Ester of Hyaluronic Acid (HY)--50% of Esterified Carboxylic Groups--50% of Salified Carboxylic Groups (Na)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 160,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 1.8 g (10.6 m.Eq.) of isopropyl iodide are added and the resulting solution is kept for 12 hours at 30° C.
A solution containing 62 ml of water and 9 g of sodium chloride is added and the resulting mixture is slowly poured into 3,500 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed three times with 500 ml of acetone/water 5:1 and three times with acetone and finally vacuum dried for eight hours at 30° C.
The product is then dissolved in 550 ml of water containing 1% of sodium chloride and the solution is slowly poured into 3,000 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed twice with 500 ml of acetone/water 5:1 and three times with 500 ml of acetone and finally vacuum dried for 24 hours at 30° C. 7.8 g of the partial isopropyl ester compound in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030 (1961)!.
Example 3
Preparation of the (Partial) Ethyl Ester of Hyaluronic Acid (HY)--75% of Esterified Carboxylic Groups--25% of Salified Carboxylic Groups (Na)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 250,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 2.5 g (15.9 m.Eq.) of ethyl iodide are added and the resulting solution is kept for 12 hours at 30° C.
A solution containing 62 ml of water and 9 g of sodium chloride is added and the resulting mixture is slowly poured into 3,500 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed three times with 500 ml of acetone/water 5:1 and three times with acetone and finally vacuum dried for eight hours at 30° C.
The product is then dissolved in 550 ml of water containing 1% of sodium chloride and the solution is slowly poured into 3,000 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed twice with 500 ml of acetone/water 5:1 and three times with 500 ml of acetone and finally vacuum dried for 24 hours at 30° C. 7.9 g of the partial ethyl ester compound in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030, (1961)!.
Example 4
Preparation of the (Partial) Methyl Ester of Hyaluronic Acid (HY)--75% of Esterified Carboxylic Groups--25% of Salified Carboxylic Groups (Na)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 80,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 2.26 g (15.9 m.Eq.) of methyl iodide are added and the resulting solution is kept for 12 hours at 30° C.
A solution containing 62 ml of water and 9 g of sodium chloride is added and the resulting mixture is slowly poured into 3,500 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed three times with 500 ml of acetone/water 5:1 and three times with acetone and finally vacuum dried for eight hours at 30° C.
The product is then dissolved in 550 ml of water containing 1% of sodium chloride and the solution is slowly poured into 3,000 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed twice with 500 ml of acetone/water 5:1 and three times with 500 ml of acetone and finally vacuum dried for 24 hours at 30° C. 7.8 g of the partial methyl ester compound in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030 (1961)!.
Example 5
Preparation of the Methyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 120,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 3 g (21.2 m.Eq.) of methyl iodide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for twenty four hours at 30° C.
8 g of the ethyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030 (1961)!.
Example 6
Preparation of the Ethyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 85,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 3.3 g (21.2 m.Eq.) of ethyl iodide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for twenty-four hours at 30° C.
8 g of the ethyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030 (1961)!.
Example 7
Preparation of the Propyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 3.6 g (21.2 m.Eq.) of propyl iodide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for twenty-four hours at 30° C.
8.3 g of the propyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030 (1961)!.
Example 8
Preparation of the (Partial) Butyl Ester of Hyaluronic Acid (HY)--50% of Esterified Carboxylic Groups--50% of Salified Carboxylic Groups (Na)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 620,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 1.95 g (10.6 m.Eq.) of n-butyl iodide are added and the resulting solution is kept for 12 hours at 30° C.
A solution containing 62 ml of water and 9 g of sodium chloride is added and the resulting mixture is slowly poured into 3,500 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed three times with 500 ml of acetone/water 5:1 and three times with acetone and finally vacuum dried for eight hours at 30° C.
The product is then dissolved in 550 ml of water containing 1% of sodium chloride and the solution is slowly poured into 3,000 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed twice with 500 ml of acetone/water 5:1 and three times with 500 ml of acetone and finally vacuum dried for 24 hours at 30° C. 8 g of the partial butyl ester compound in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030 (1961)!.
Example 9
Preparation of the (Partial) Ethoxy-carbonylmethyl Ester of Hyaluronic Acid (HY)--75% of Esterified Carboxylic Groups--25% of Salified Carboxylic Groups (Na)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 180,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 2 g of tetrabutylammonium iodide and 1.84 g (15 m.Eq.) of ethyl chloroacetate are added and the resulting solution of kept for 24 hours at 30° C.
A solution containing 62 ml of water and 9 g of sodium chloride is added and the resulting mixture is slowly poured into 3,500 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed three times with 500 ml of acetone/water 5:1 and three times with acetone and finally vacuum dried for eight hours at 30° C.
The product is then dissolved in 550 ml of water containing 1% of sodium chloride and the solution is slowly poured into 3,000 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed twice with 500 ml of acetone/water 5:1 and three times with 500 ml of acetone and finally vacuum dried for 24 hours at 30° C. 10 g of the partial ethoxycarbonyl methyl ester compound in the title are obtained.
Quantitative determination of the ethoxylic ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030 (1961)!.
Example 10
Preparation of the N-pentyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 620,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 3.8 g (25 m.Eq.) of n-pentyl bromide and 0.2 g of iodide tetrabutyl-ammonium are added, the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for twenty four hours at 30° C.
8.7 g of the n-pentyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described on pages 169-172 of Siggia S. and Hann J. G. "Quantitative organic analysis via functional groups" 4th Edition, John Wiley and Sons.
Example 11
Preparation of the Isopentyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethysulfoxide at 25° C., 3.8 g (25 m.Eq.) of isopentyl bromide and 0.2 g of tetrabutylammonium iodide are added, the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for twenty four hours at 30° C.
8.6 g of the isopentyl ester product featured in the title are obtained. Quantitative determination of the ester groups is carried out according to the method described on pages 169-172 of Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups" 4th Edition, John Wiley and Sons.
Example 12
Preparation of the Benzylester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.5 g (25 m.Eq.) of benzyl bromide and 0.2 g of tetrabutylammonium iodide are added, the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for twenty four hours at 30° C.
9 g of the benzyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out according to the method described on pages 169-172 of Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups" 4th Edition, John Wiley and Sons.
Example 13
Preparation of the β-phenylethyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 125,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.6 g (25 m.Eq.) of 2-bromoethylbenzene and 185 mg of tetrabutylammonium iodide are added, and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is thus formed which is then filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for twenty four hours at 30° C.
9.1 g of the β-phenylethyl ester in the title are obtained. Quantitative determination of the ester groups is carried out according to the method described on page 168-172 of Siggia S. and hanna J. G. "Quantitative organic analysis via functional groups" 4th Edition, John Wiley and Sons.
Example 14
Preparation of the Benzyl Ester of Hyaluronic Acid (HY)
3 g of the potassium salt of HY with a molecular weight of 162,000 are suspended in 200 ml of dimethylsulfoxide; 120 mg of tetrabutylammonium iodide and 2.4 g of benzyl bromide are added.
The suspension is kept in agitation for 48 hours at 30° C. The resulting mixture is slowly poured into 1,000 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 150 ml of ethyl acetate and finally vacuum dried for twenty four hours at 30° C.
3.1 g of the benzyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out according to the method described on pages 169-172 of Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups" 4th Edition, John Wiley and Sons.
Example 15
Preparation of the (Partial Propyl) Ester of Hyaluronic Acid (HY)--85% of Esterified Carboxylic Groups--15% of Salified Carboxylic Groups (Na)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 165,1000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethysulfoxide at 25° C., 2.9 g (17 m.Eq.) of propyl iodide are added and the resulting solution is kept for 12 hours at 30° C.
A solution is then added containing 62 ml of water and 9 g of sodium chloride and the resulting mixture is slowly poured into 3,500 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed three times with 500 ml of acetone/water 5:1 and three times with acetone and finally vacuum dried for eight hours at 30° C.
The product is then dissolved in 550 ml of water containing 1% of sodium chloride and the solution is slowly poured into 3,000 ml of acetone under constant agitation. A precipitate is formed which is filtered and washed twice with 500 ml of acetone/water 5:1 and three times with 500 ml of acetone and finally vacuum dried for 24 hours at 30° C. 8 g of the partial propyl ester compound in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas Anal. Chem. 33, 1028-1030 (1961)!.
Example 16
Preparation of the N-octyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170.000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.1 g (21.2 m.Eq.) of 1-bromooctane are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 9.3 g of the octyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 17
Preparation of the Isopropyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170.000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 2.6 g (21.2 m.Eq.) of isopropyl bromide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 8.3 g of the isopropyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method of R. H. Cundiff and P. C. Markunas (Anal. Chem. 33, 1028-1030, 1961).
Example 18
Preparation of the 2,6-dichlorobenzyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170.000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 5.08 g (21.2 m.Eq.) of 2,6-dichlorobenzyl bromide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 9.7 g of the 2,6-dichlorobenzyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 19
Preparation of the 4-terbutylbenzyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.81 g (21.2 m.Eq.) of 4-terbutylbenzyl bromide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 9.8 g of the 4-terbutylbenzyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 20
Preparation of the Heptadecyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 6.8 g (21.2 M.Eq.) of Heptadecyl bromide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 11 g of the Heptadecyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 21
Preparation of the Octadecyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 7.1 g (21.2 m.Eq.) of octadecyl bromide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 11 g of the octadecyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 22
Preparation of the 3-phenylpropyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.22 g (21.2 m.Eq.) of 3-phenylpropyl bromide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 9 g of the 3-phenylpropyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 23
Preparation of the 3,4,5-trimethoxy-benzyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 M.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.6 g (21.2 m.Eq.) of 3,4,5-trimethoxybenzyl chloride are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 10 g of the 3,4,5-trimethoxybenzyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 24
Preparation of the Cinnamyl Ester of Hyaluronic Acid (HY)
12.4 g of Hy tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.2 9 (21.2 m.Eq.) of Cinnamyl bromide are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 9.3 g of the Cinnamyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 25
Preparation of the Decyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.7 g (21.2 m.Eq.) of 1-bromo decane are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 9.5 g of the Decyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
Example 26
Preparation of the Nonyl Ester of Hyaluronic Acid (HY)
12.4 g of HY tetrabutylammonium salt with a molecular weight of 170,000 corresponding to 20 m.Eq. of a monomeric unit are solubilized in 620 ml of dimethylsulfoxide at 25° C., 4.4 g (21.2 m.Eq.) of 1-bromo nonane are added and the solution is kept for 12 hours at 30° C.
The resulting mixture is slowly poured into 3,500 ml of ethyl acetate under constant agitation. A precipitate is formed which is filtered and washed four times with 500 ml of ethyl acetate and finally vacuum dried for 24 hours at 30° C. 9 g of the Nonyl ester product in the title are obtained. Quantitative determination of the ester groups is carried out using the method described in Siggia S. and Hanna J. G. "Quantitative organic analysis via functional groups", 4th Edition, John Wiley and Sons, pages 169-172.
The Esters of Alginic Acid
The alginic acid esters which can be employed in the present invention can be prepared as described in EPA 0 251 905 A2 by starting with quaternary ammonium salts of alginic acid with an etherifying agent in a preferably aprotic organic solvent, such as dialkylsulfoxides, dialkylcarboxamides, such as in particular lower alkyl dialkylsulfoxides, above all dimethylsulfoxide, and lower alkyl dialkylamides of lower aliphatic acids, such as dimethyl or diethyl formamide or dimethyl or diethyl acetamide. It is possible, however, to use other solvents which are not always aprotic, such as alcohols, ethers, detones, esters, especially aliphatic or heterocyclic alcohols and ketones with a low boiling point, such as hexafluoroisopropanol and trifluoroethanol. The reaction is brought about preferably at a temperature of between about 0° and 100° C., and especially between about 25° and 75° C., for example at about 30° C.
Esterification is carried out preferably by gradually adding the esterifying agent to the above-mentioned ammonium salt dissolved in one of the solvents mentioned, for example in dimethylsulfoxide. As alkylating agents, those mentioned above can be used, especially hydrocarbyl halides, for example alkyl halides.
The preferred esterification process, therefore, comprises reacting, in an organic solvent, a quaternary ammonium salt of alginic acid with a stoichiometric quantity of a compound of the formula
A-X
wherein A is selected from the group consisting of an aliphatic, araliphatic, cycloaliphatic, aliphatic-cycloaliphatic and heterocyclic radicals, and X is a halogen atom, and wherein said stoichiometric quantity of A-X is determined by the degree of esterification desired.
As starting quaternary ammonium salts, it is preferable to use lower ammonium tetraalkylates, the alkyl groups having preferably between 1 and 6 carbon atoms. Mostly, the alginate of tetrabutylammonium is used. These quaternary ammonium salts can be prepared by reacting a metal salt of alginic acid, preferably one of those mentioned above, especially the sodium or potassium salt, in aqueous solution with a sulfonic resin salified with the quaternary ammonium base.
One variation of the previously specified procedure consists of reacting a potassium or sodium salt of alginic acid, suspended in a suitable solution such as dimethylsulfoxide, with a suitable alkylating agent in the presence of a catalyzing quantity of a quaternary ammonium salt, such as tetrabutylammonium iodide. This procedure makes it possible to obtain the total esters of alginic acid.
To prepare new esters it is possible to use alginic acids of any origin. The preparation of these acids is described in literature. It is preferable to use purified alginic acids.
In the partial esters, it is possible to salify all the remaining carboxy groups or only part of these, dosing the base quantity so as to obtain the desired stoichiometric degree of salification. By correctly gauging the degree of salification, it is possible to obtain esters with a wide range of different dissociation constants, thereby giving the desired pH in solutions or "in situ" at the time of therapeutic application.
ALAFF 11, the benzyl ester of alginic acid, and ALAFF 7, the ethyl ester of alginic acid, are particularly useful in the present composite membranes.
Example 27
A non-woven fabric comprising hyaluronic acid benzyl ester HYAFF 11, weighing 40 gr/mq, 0.5 mm thick, was produced by the following procedure (see FIG. 1).
A solution of HYAFF 11 in dimethylsulfoxide at a concentration of 135 mg/ml is prepared in a tank (1) and fed by a gear metering pump (2) into a spinneret for wet extrusion composed of 3000 holes each measuring 65 microns.
The extruded mass of threads passes into a coagulation bath (3) containing absolute ethanol. It is then moved over transporting rollers into two successive rinsing baths (4 and 5) containing absolute ethanol. The drafting ratio of the first roller is set at zero while the drafting ratio between the other rollers is set at 1.05. Once it has been passed through the rinsing baths, the hank of threads is blown dry with hot air at 45°-50° C. (6) and cut with a roller cutter (7) into 40 mm fibers.
The mass of fibers thus obtained is tipped into a chute leading to a carding/cross lapping machine (9) from which it emerges as a web, 1 mm thick and weighing 40 mg/mq. The web is then sprayed with a solution of HYAFF 11 in dimethylsulfoxide at 80 mg/ml (11), placed in an ethanol coagulation bath (12), in a rinsing chamber (13), and lastly in a drying chamber (14).
The final thickness of the material is 0.5 mm. Its appearance can be seen in FIG. 2.
Example 28
A non-woven fabric comprising the ethyl ester of hyaluronic acid, HYAFF 7, weighing 200 gr/mq and 1.5 mm thick, was produced by the following procedure.
Fibers of HYAFF 7, 3 mm long, obtained by the spinning process described in Example 27, were fed through a chute into a carding machine, from which they emerged as a 1.8 mm thick web weighing 200 gr/mq. The web is passed through a needle punching machine (FIG. 1, details 16, 17, and 18), which transforms it into a non-woven fabric weighing 200 gr/mq, and 1.5 mm thick.
Example 29
A non-woven fabric weighing 200 gr/mq and 1.5 mm thick comprising a mixture of the ethyl ester of hyaluronic acid, HYAFF 7, and of hyaluronic acid benzyl ester, HYAFF 11, in equal quantities, was obtained by the following procedure.
Fibers of HYAFF 7 and HYAFF 11, measuring 3 mm in length, obtained by the spinning process described in Example 27 were thoroughly mixed in a spiral mixer. The mixture of fibers was fed into a carding machine from which it emerged as a 1.8 mm thick web weighing 200 gr/mq.
The web was put through a needle punching machine (FIG. 1, details 16, 17, and 18), which transformed it into a 1.5 mm thick unwoven fabric weighing 200 gr/mq, with the two materials perfectly mixed together.
Example 30
A non-woven fabric weighing 40 gr/mq and 0.5 mm thick comprising a mixture of hyaluronic acid benzyl ester, HYAFF 11, and a partial (75%) benzyl ester of hyaluronic acid, HYAFF 11p75, in equal percentages, was produced by the following procedure.
HYAFF 11p75 is prepared as follows. 10 g of hyaluronic acid tetrabutylammonium salt, mw=620.76, equal to 16.1 nmole, are solubilized in a mixture of N-methyl pyrrolidone/H 2 O, 90/10, 2.5% in weight, to obtain 400 mls of solution. The solution is cooled to 10° C., then purified N 2 is bubbled through it for 30 minutes. This is then esterified with 1.49 ml (equal to 12.54 mmole) of benzyl bromide. The solution is gently shaken for 60 hours at 15°-20° C.
Subsequent purification is achieved by precipitation in ethyl acetate following the addition of a saturated solution of sodium chloride, and subsequent washings with a mixture of ethyl acetate/absolute ethanol, 80/20. The solid phase is separated by filtration, and treated with anhydrous acetone. 6.8 g of product are thus obtained, equal to a yield of about 95%.
Fibers of HYAFF 11 and HYAFF 11p75, 40 mm long, obtained by the process described in Example 1, were thoroughly mixed in a spiral mixer.
The mixed fibers were fed into a carding machine from which they emerged as a 1 mm thick web weighing 40 mg/mq. The web was then sprayed with a solution of HYAFF 11 in dimethylsulfoxide at 80 mg/ml (FIG. 1, detail 11), placed in an ethanol coagulation bath (12), then in a rinsing chamber (13) containing water or a mixture of water and ethanol in a ratio of from 10 to 95% ethanol, and finally in a drying chamber (14).
The material has a final thickness of 0.5 mm, and the fibers of HYAFF 11 and HYAFF 11p75 are perfectly mixed and adhered together.
Example 31
A non-woven fabric comprising the benzyl ester of hyaluronic acid, HYAFF 11, weighing 200 gr/mq and 1.5 mm thick, impregnated with vancomycin, was produced by the following procedure.
The non-woven fabric obtained as described in Example 28 was immersed for 4 hrs in an aqueous solution of vancomycin at a concentration of 0.1 mg/ml. Subsequently, after treatment in a heated colander, the non-woven fabric is dried for 2 hrs in an oven. In vitro release tests showed that the vancomycin is contained in the material in pharmacologically active quantities.
The non-woven fabrics of the present invention can be advantageously utilized in various types of microsurgical procedures, such as in odontology, stomatology, otorhinolaryngology, orthopedics, neurosurgery, etc., in which it is necessary to employ a substance that can be metabolized by the organism and which is capable of facilitating flap take, reepithelialization of mucous membranes, stabilization of grafts, and the filling of cavities. The new non-woven fabrics can also be employed as buffer media in surgery to the nose and inner ear.
Example 32
Non-woven fabric materials of the present invention can also be produced employing partial or total "inner ester" auto-crosslinked carboxy polysaccharides such as autocrosslinked hyaluronic acid. Such "inner ester" crosslinked carboxy polysaccharides are well known in the art, as disclosed in European Patent Application 0 341 745 A1 and corresponding U.S. Pat. No. 5,676,964, the entire contents of which are herein incorporated by reference. These inner ester auto-crosslinked carboxy polysaccharides include inter-and/or intramolecular esters of acidic polysaccharides, such as hyaluronic acid, containing carboxy functions, in which all or a part of such functions are esterified with hydroxyl groups of the same molecule and/or of different molecules of the acidic polysaccharide. These "inner esters" of acidic polysaccharides are also known as "auto-crosslinked polysaccharides" since the formation of a mono- or polymolecular crosslink is the consequence of the above-mentioned internal esterification.
For the purpose of producing non-woven fabric materials of the present invention, the degree of inner esterification of the carboxyls can vary between about 1% and about 100%, preferably between about 1% and about 30%, more preferably between about 18% and about 22%. All or only a part of the carboxy functions can be "inner" esterified. In partial inner esters, further carboxy functions can be either partially or totally esterified with monovalent or polyvalent alcohols, thus forming "outer" ester bonds, and in the partial esters of both these ester groups, the non-esterified carboxy functions may be free or salified with metals or organic bases. Thus, threads can be formed from mixed "inner" and "outer" esters, where the degree of inner esterification of the carboxyls can vary as noted above. The threads can be formed by partial esters of hyaluronic acid, with a certain percentage of the carboxy groups being crosslinked, and the remaining carboxy groups being salified with alkaline metals, such as sodium or potassium, ammonium salts, cesium salts, or salts of alkaline earth metals, such as calcium, magnesium, or aluminum.
Furthermore, such non-woven fabric materials can be impregnated or saturated with pharmaceutically active substances such as those described above either by means of physical bonds (in the case of salts), or chemical bonds (in the case of alcohols).
Examples of physical incorporation of pharmaceutically active substances are described in Examples 36-37 of European Patent Application 0 341 745 A1, where the preparation of kanamycin and amikacin salts of crosslinked hyaluronic is described.
Examples of chemical incorporation of pharmaceutically active substances are described in Examples 31-33 of the above-noted European Patent Application, where the preparation of cortisone esters of crosslinked hyaluronic acid is described.
Examples of the pharmaceutically active substances with which composite membranes can be impregnated by means of physical (salt) bonds include vitamins, haemostatics, anaesthetics, disinfectants, non-steroid antiinflammatory agents, growth factors, peptides, proteins, and analgesics.
Examples of the pharmaceutically active substances with which non-woven fabric materials can be impregnated by means of chemical reaction in the membrane include steroid drugs such as cortisones, vitamins such as vitamins D 2 and D 3 , growth factors, peptides, proteins, and analgesics.
The preparation of threads using solutions of crosslinked, acidic polysaccharides in dimethylsulfoxide is described at page 11 and in Example 41 of European Patent Application 0 341 745 A1. This is similar to the preparation of threads comprising hyaluronic acid esters, as described in Examples 27-31, supra. Such threads prepared using crosslinked hyaluronic acid can be made into non-woven fabric materials in the manner also described in Examples 27-31, supra.
For example, crosslinked hyaluronic acid can be prepared as follows. 10 g of hyaluronic acid tetrabutylammonium salt, molecular weight 620.76, equal to 16.1 mmole, are solubilized in water in a quantity of 80 mg/ml. The solution is frozen to -40° C., and freeze-dried. The product thus obtained is placed in a reactor with a capacity of 500 ml, and then treated with 300 ml of acetone. To the suspension is added 1.03 g (the quantity required to esterify 25% of the carboxy groups) of 2-chloro-1-methyl pyridine iodide, and the mixture is heated to the boiling point of the acetone reaction solvent. The mixture is left to react for four hours. The product thus obtained is washed several times with acetone, and placed in an aqueous solution of ammonium acetate, where it is left overnight. Subsequent treatment consists of suspending the product in saline.
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.
|
Biomaterials are disclosed comprised of biodegradable, biocompatible, and bioabsorbable non-woven fabric materials for use in surgery for the guided regeneration of tissues. The non-woven fabric materials constitute threads embedded in a matrix, wherein both the matrix and the threads constitute auto-crosslinked hyaluronic acid.
| 3
|
FIELD OF THE INVENTION AND RELATED ART
[0001] The present invention relates to a beam as a microscopic structural member placed in an area which remains filled with liquid or the like, and the method for forming such a beam. In particular, it relates to such a beam that improves in mechanical strength an ink jet recording head which ejects ink to record on recording medium, the method for forming such a beam, an ink jet recording head provided with such a beam, and the method for manufacturing such an ink jet recording head.
[0002] An ink jet recording method (disclosed in Japanese Laid-open Patent Application 54-51837, for example), which generates bubbles by heating ink; ejects ink by utilizing the pressure generated by the growth of the bubbles; and adheres the ejected ink to the surface of recording medium, is advantageous in that it is capable of recording at a high speed, is relatively high in image quality, and is low in noises. This recording method makes it easy to record images in color, and also, makes it easy to recording on ordinary paper or the like. It also makes it easy to reduce the size of a recording apparatus. Further, the ejection orifices of an ink jet recording head can be placed in high density. Therefore, ink jet recording method contributes to the improvement of a recording apparatus in terms of resolution and image quality. Thus, a recording apparatus (ink jet recording apparatus) which employs this liquid ejecting method is used, in various forms, as the information outputting means for a copying machine, a printer, a facsimileing machine, etc.
[0003] In recent years, the demand has been increasing for means for outputting information in the form of an image which is greater in the amount of data, and therefore, the demand has been increasing for means for recording a highly precise image at a high speed. In order to output a highly precise image, it is required to reliably eject minutes ink droplets, and for this purpose, it is necessary to highly precisely form ejection orifices at a high density.
[0004] Japanese Laid-open Patent Applications 5-330066 and 6-286149, for example, propose ink jet recording head manufacturing methods capable of highly precisely forming ejection orifices at a high density. Further, Japanese Laid-open Patent Application 10-146979 proposes a method for forming ribs in the orifice plate having ejection orifices. The ink jet recording heads proposed in these documents are of the so-called side shooter type, from which ink droplets are ejected in the direction perpendicular to the surface of the substrate on which heating members are located.
[0005] In the case of an ink jet recording head of the “side shooter type”, the increase in the density at which ejection orifice are formed, naturally results in the reduction in the distance between the adjacent two ejection orifices, resulting thereby in the reduction in the width of each ink passage to the corresponding ejection orifice. The narrower the ink passage, the longer the time necessary for the ink passage to be refilled with ink after the extinction of the bubbles. In order to reduce this refilling time, it is necessary to reduce the distance between a heat generating member and an ink supplying hole.
[0006] As the method for accurately control the distance between an ink supplying hole and a heat generating member, one of the anisotropic etching methods has been known, which uses water solution of alkali, and utilizes the phenomenon that the etching rate is affected by the orientation of the plane of the silicon substrate. In the case of this method, generally, the distance between a heat generating member and ink supplying hole is controlled by using a piece of silicon wafer, the face orientation of which is ( 100 ), as the substrate, and anisotropically etching the substrate from the back side of the substrate to precisely form the ink supply hole. For example, Japanese Laid-open Patent Application 10-181032 proposes a method for forming the ink supplying hole, which is the combination of the sacrifice layer formed on the surface of the silicon substrate, and the anisotropic etching method.
[0007] In the field of the manufacture of an ink jet recording head, this method of anisotropically etching a silicon crystal has become one of the most useful technologies for precisely forming an ink supplying hole.
[0008] However, in order to record images more precisely and at a higher speed than the levels of precision and speed at which images are recorded by an ink jet recording apparatus in accordance with the prior art, not only must ejection orifices be increased in density, but also, the line in which ejection orifices are aligned must be increased in length, which creates a problem. That is, as the line of the ejection orifice is increased in length, the opening of the ink supplying hole is also increased in length; the greater the number of ejection orifices, the greater the length of the opening of the ink supplying hole. As a result, the ink jet recording head (substrate) is reduced in mechanical strength. The reduction in the mechanical strength of the substrate causes the deformation of the substrate and/or damage to the substrate during the process for manufacturing ink jet recording heads. This in turn makes it possible that such problems as reduction in yield, or unsatisfactory recording performance, will occur.
[0009] In order to solve the above described problems, the idea of providing an ink jet recording head with two or more ink supplying holes has been studied. However, when two or more ink supplying holes were formed by literally using the method disclosed in Japanese Laid-open Patent Application 10-181032, the distances between some of the ejection orifices and corresponding ink supplying hole became different from the distances between the other ejection orifices and the corresponding ink supplying hole, because the openings of the ink supply holes on the back side of the substrate became different in size from those on the front side, reducing thereby the speed at which the ink passages were refilled with ink. As a result, it was difficult to achieve a practical printing speed.
[0010] On the other hand, Japanese Laid-open Patent Application 9-211019 discloses another method for forming a microscopic beam of semiconductor. The beam is roughly triangular in cross section. One of the lateral surfaces coincides with one of the ( 100 ) faces of the semiconductor, and each of the other two lateral surfaces coincides with one of the ( 111 ) faces of the semiconductor. The beam is formed, as an integral part of the primary portion, by etching the substrate (mother member) formed of a single crystal of silicon so that it is supported by the mother member (substrate), by both lengthwise ends. This method for forming a beam can be used for forming a beam narrower at the bottom, or the portion which coincides with the back surface of the substrate, but, it suffers from the problem that the inward side of the beam is dissolved from the peak of the beam, by the etchant with a high pH value used for anisotropic etching.
SUMMARY OF THE INVENTION
[0011] Thus, the primary object of the present invention is to provide an ink jet recording head having corrosion resistant beams, and a method for manufacturing such an ink jet recording head.
[0012] Another object of the present invention is to provide a corrosion resistant beam formable as an integral part of a microscopic structure manufacturable with the use of a manufacturing process which employs an anisotropic etching method.
[0013] According to an aspect of the present invention, there is provided a beam having a base material of silicon monocrystal and at least one projection which is integrally formed so as to be supported at least at one end thereof and which has two surfaces having an orientation plane ( 111 ), comprising a bottom surface in a plane which is common with a plane of said base material; a groove penetrating from said bottom surface to a top of said projection; and a protecting member having a resistance property against a crystal anisotropic etching liquid and covering an inner wall of said groove.
[0014] According to this aspect of the present invention, beams are formed, as integral parts of the substrate, on the inward side of the substrate of an ink jet recording head, more specifically, within the common liquid chamber of the ink jet recording head. Therefore, the ink jet recording head (substrate) in accordance with the present invention is superior in mechanical strength to an ink jet recording head in accordance with the prior art.
[0015] Further, in the case of an ink jet recording head structured in accordance with the present invention, its common liquid chamber is formed so that the common ink supplying hole of the common liquid chamber faces the front side of the substrate. Further, each beam is triangular in cross section, and each of its two lateral surfaces on the front side of the substrate coincides with one of the ( 111 ) faces of the crystal of which the substrate is formed. Therefore, the beam is resistant to the corrosion by ink or the like; it is unlikely to be corroded by ink or the like, from its peak.
[0016] According to another aspect of the present invention, there is provided a method for manufacturing a beam having a base material of silicon monocrystal and at least one projection which is integrally formed so as to be supported at least at one end thereof and which has two surfaces having an orientation plane ( 111 ), said beam comprising a bottom surface in a plane which is common with a plane of said base material, said method comprising the steps of: (A) forming a groove in said base material from said bottom side; (B) forming a protecting member a protecting member having a resistance property against a crystal anisotropic etching liquid and covering an inner wall of said groove; (C) forming a plurality of beam formation grooves with a position of formation of said beam interposed therebetween; and (D) forming a surface other than said bottom surface of said beam by crystal anisotropic etching of a part of said base material which is faced to the beam formation groove.
[0017] The method, in accordance with the present invention, for manufacturing an ink jet recording head, makes it possible to satisfactorily manufacture an ink jet recording head in accordance with the present invention. Further, the shape (vertical measurement, and width of bottom) into which a beam is formed can be easily changed by changing the shape of the grooves formed in the step (e), and the shape of the grooves formed in the step (g) for forming the beams. Further, the surfaces, other than the bottom surface, of each beam, and the surfaces of the side walls of the common liquid chamber, are formed by anisotropic etching. Therefore, these surfaces are parallel to the ( 111 ) face of the crystal of which the substrate is formed, being therefore highly resistant to corrosion.
[0018] According to a further aspect of the present invention, there is provided an ink jet recording head including a silicon substrate having energy generating means for ejecting said ink through an ejection outlet by application of ejection energy to the ink, and a common liquid chamber, formed in said substrate, for storing ink to be supplied to said ejection outlet, said ink jet recording head comprising at least one beam which has at least one projection formed on a back side of said substrate in said common liquid chamber, said projection being integrally formed so as to be supported at opposite ends thereof and having two surfaces having an orientation plane ( 111 ); said beam including a bottom surface in a plane which is common with a plane of said base material; a groove penetrating from said bottom surface to a top of said projection; and a protecting member having a resistance property against a crystal anisotropic etching liquid and covering an inner wall of said groove.
[0019] A beam, in accordance with the present invention, for an ink jet recording head can be applicable to various microscopically structured components other than an ink jet recording head. As described above, a beam in accordance with the present invention is unlikely to be corroded from its peak.
[0020] According to a further aspect of the present invention, there is provided a manufacturing method for manufacturing an ink jet recording head including a silicon substrate having energy generating means for ejecting said ink through an ejection outlet by application of ejection energy to the ink, and a common liquid chamber, formed in said substrate, for storing ink to be supplied to said ejection outlet, said ink jet recording head including at least one beam which has at least one projection formed on a back side of said substrate in said common liquid chamber, said projection being integrally formed so as to be supported at opposite ends thereof and having two surfaces having an orientation plane ( 111 ), said method comprising the steps of (A) forming a groove in said substrate from a back side of said substrate; (B) forming a protecting member a protecting member having a resistance property against a crystal anisotropic etching liquid and covering an inner wall of said groove; (C) forming a plurality of beam formation grooves with a position of formation of said beam interposed therebetween; and (D) crystal anisotropic etching of a part of said substrate facing a beam formation groove to form a beam having at least one projection constituted by two surfaces having an orientation plane ( 111 ) and a bottom surface which is common with a back side of said substrate, and a common liquid chamber having a common ink supply port in a front surface of said substrate.
[0021] The method, in accordance with the present invention, for forming a beam makes it possible to satisfactorily form the above described beam in accordance with the present invention. It is particularly effective if it is used in a process in which a microscopically structured component is manufactured with the use of an anisotropic etching method. It is similar to the above described head manufacturing method in that the shape (vertical measurement, width of bottom, etc.) into which a beam is formed can be easily changed by changing the shape of the grooves formed in the step (a), and the shape of the grooves formed in the step (c) for forming the beams.
[0022] As described above, according to the present invention, an ink jet recording head is improved in mechanical strength by the beams formed in the common liquid chamber of the head. Therefore, the ink jet recording head is prevented from deforming, and therefore, the ejection orifices are prevented from deviating in position. Further, it is possible to manufacture reliable ink jet recording heads which are substantially longer than the ink jet recording heads in accordance with the prior art, making it therefore possible to record more precisely and at a higher speed. Further, the ink jet recording heads in accordance with the present invention are less likely to break while they are manufactured. Therefore, they are higher in yield than the ink jet recording heads in accordance with the prior art. Further, in the case of an ink jet recording head in accordance with the present invention, the opening of the ink supplying hole of the common liquid chamber faces the front side of the substrate, eliminating the problem concerning the refill time. Therefore, the ejection orifices of the ink jet recording head in accordance with the present invention are uniform in ejection frequency, enabling the ink jet recording head to record at a high speed. Further, a beam in accordance with the present invention is unlikely to be corroded from its peak by ink or the like. Therefore, it is well suited for an ink jet recording head. Further, it is also well suited for the beam for a microscopically structured component, in addition to an ink jet recording head, which is always in contact with alkaline liquid or the like, because the beam in accordance with the present invention is resistant to alkali.
[0023] These and other objects, features, and advantages of the present invention will become more apparent upon consideration of the following description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] FIG. 1 is a perspective view of an example of an ink jet recording head in accordance with the present invention.
[0025] FIG. 2( a ) is a sectional view of the ink jet recording head shown in FIG. 1 , at a plane parallel to the widthwise direction of the ink jet recording head, and FIG. 2( b ) is the ink jet recording head shown in FIG. 1 , at a plane parallel to the lengthwise direction of the ink jet recording head.
[0026] FIG. 3 is a schematic drawing for describing the method for improving the ink jet recording head in terms of mechanical strength, with the provision of beams.
[0027] FIG. 4 is a schematic drawing of the apparatus for angularly etching a substrate, which is used for the ink jet head manufacturing method in accordance with the present invention.
[0028] FIG. 5 is a sectional view of the substrate, which was etched with the use of the apparatus shown in FIG. 4 .
[0029] FIG. 6 is a drawing for describing the ink jet head manufacturing method in the second embodiment of the present invention.
[0030] FIG. 7 is an enlarged sectional view of the groove portion, for supplementing the description of the beam forming method in accordance with the present invention.
[0031] FIG. 8 is a drawing for describing the ink jet head manufacturing method in the third embodiment of the present invention.
[0032] FIG. 9 is a drawing for describing the ink jet head manufacturing method in the fourth embodiment of the present invention.
[0033] FIG. 10 is a drawing for describing the ink jet head manufacturing method in the fifth embodiment of the present invention.
[0034] FIG. 11 is a drawing for describing the ink jet head manufacturing method in the sixth embodiment of the present invention.
[0035] FIG. 12 is a drawing for describing the ink jet head manufacturing method in the seventh embodiment of the present invention.
[0036] FIG. 13 is a perspective view of a typical recording apparatus compatible with an ink jet recording head in accordance with the present invention.
[0037] FIG. 14 is a perspective view of a typical head cartridge compatible with an ink jet recording head in accordance with the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0038] Hereinafter, the preferred embodiments of the present invention will be described with reference to the appended drawings.
Embodiment 1
[0039] FIG. 1 is a perspective view of an example of an ink jet recording head in this first embodiment. FIG. 2 is a sectional view of the ink jet recording head shown in FIG. 1 . FIGS. 2( a ) and 2 ( b ) are sectional views at planes parallel to the widthwise and lengthwise directions, respectively, of the ink jet recording head.
[0040] Referring to FIG. 1 , the ink jet recording head 20 in this embodiment comprises a substrate 1 formed of a piece of a single crystal of silicon, and an orifice plate 3 having a plurality of ejection orifices and solidly glued to the substrate 1 . The substrate 1 has: a common liquid chamber 9 from which ink is supplied to the ejection orifices; and a beam 1 a which is on the back side of the substrate 1 , being inside the common liquid chamber 9 .
[0041] Referring to FIG. 2 , the common liquid chamber 9 extends from one end of the substrate 1 to the other. The orientation of the side walls (internal wall) of the common liquid chamber 9 formed of a single crystal of silicon (substrate 1 ) matches that of the ( 111 ) face of the silicon crystal. More specifically, the common liquid chamber 9 is formed by isotropically etching the substrate 1 so that the top and bottom sides of its side walls, which are parallel to the ( 111 ) face of the silicon crystal, meet at the center of the substrate 1 in terms of the thickness direction (direction Z in drawing) of the substrate 1 . Thus, the common liquid chamber 9 is shaped so that the closer to the center of the substrate 1 , in terms of the thickness direction of the substrate 1 , the wider; the common liquid chamber 9 is widest at the center of the substrate 1 in terms of the thickness direction of the substrate 1 .
[0042] Referring to FIG. 2 , the beam 1 a is a structural member for reinforcing the entirety of the ink jet recording head. The beam 1 a has a roughly triangular cross section, and its bottom surface, that is, one of its three lateral surfaces, coincides with the back surface of the substrate 1 . There is no limit for the number of the beam 1 a ; two or more beams 1 a may be provided. The ink jet recording head 20 in the drawing is provided with only one beam 1 a . The beam 1 a is formed so that it extends in the Y direction in the drawing, which is parallel to the front and rear surfaces of the substrate 1 , and is supported by the substrate 1 , by both of its lengthwise ends. The other two of the three lateral surfaces of the beam 1 a , that is, the two surfaces on the top side, face the common liquid chamber 9 , and there are parallel to the ( 111 ) face of the silicon crystal. Referring to FIG. 2( b ), the height of the beam 1 a , that is, the measurement of the beam 1 a in terms of the thickness direction (Z direction in drawing) of the substrate 1 is set to be less than the thickness of the substrate 1 . In other words, the two surfaces of the beam 1 a on the top side constitute parts of the walls of the common liquid chamber 9 , the top side of which is open as an ink supplying hole.
[0043] The bottom surface of the beam 1 a is covered with a protective layer 14 formed of a substance resistant to alkalis. Further, the beam 1 a is provided with a projection 14 a (protective member), which is formed of the same substance as the material for the protective layer 14 , and extends in the direction perpendicular to the bottom surface of the beam 1 a . The top end of the projection 14 a roughly coincides with the top (peak) of the beam 1 a . More precisely, the projection 14 a extends slightly beyond the peak of the beam 1 a . Firstly, this beam protecting layer 14 and projection 14 a have the effect of preventing the beam 1 a from being etched from its peak during the formation of the common liquid chamber 9 , which will be described later. Secondly, they prevent the beam 1 a from being corroded from the peak, by ink.
[0044] The above described ink jet recording head 20 in the first embodiment of the present invention is provided with a beam 1 a (reinforcement structure), which is in the common liquid chamber 9 . Therefore, the it is greater in mechanical strength than an ink jet recording head in accordance with the prior art. Thus, even if the ink supplying opening is substantially increased in length, the substrate 1 is prevented by the beam 1 a from deforming. Therefore, it does not occur that the ejection orifices deviate in position due to the deformation of the substrate 1 . Further, the two lateral surfaces of the beam 1 a , on the top side, are parallel to the ( 111 ) face of the silicon, being slower in the rate at which they are etched by water solution of alkali. In other words, the beam 1 a is less likely to be corroded by alkaline ink. Therefore, the ink jet recording head 20 is superior in terms of corrosion resistance.
[0045] A beam such as the above described reinforcement beam 1 a , and the manufacturing method therefor, are useful for various microscopic structures provided with such a beam, in particular, when an anisotropic etching method is used for the manufacturing process for a given microscopic structure.
[0046] Referring to FIG. 1 or 2 ( b ), the ink jet recording head 20 is structured so that the ink supplying opening 2 of its common liquid chamber 9 is on the top surface side of the substrate 1 . Therefore, the ejection orifices (unshown) are uniform in the distance from the ink supplying opening 2 . In addition, the this distance is relatively short. Therefore, the problematically slow ink refill attributable to the length of the ink passages (distance) is not likely to occur.
[0047] Further, the side walls of the common liquid chamber 9 are parallel to the ( 111 ) face of the silicon substrate 1 . Therefore, it is not likely to be corroded by the alkaline ink, making the ink jet recording head superior in corrosion resistance.
[0048] Referring to FIG. 2 , in the case of the ink jet recording head 20 , in terms of the cross section parallel to the top and bottom surfaces of the substratel, the common liquid chamber 9 is greater at the mid point of the common liquid chamber 9 , in terms of the thickness direction of the substrate 1 , than the sum of the openings of the common liquid chamber 9 located at the bottom surface of the substrate 1 . In comparison, in the case of an ink jet recording head in accordance with the prior art, the common liquid chamber 9 is trapezoidal in vertical cross section, being wider at the bottom; in other words, it gradually reduces in horizontal cross section starting from the bottom side. Therefore, in order to increase the volume of the common liquid chamber 9 , the common liquid chamber 9 had to be increased in the size of its bottom opening. In the case of this ink jet recording head 20 , however, the common liquid chamber 9 is as large in volume as that of an ink jet recording head in accordance the prior art, while being smaller in the size of its bottom opening. In other words, the back side portion of the substrate 1 remains intact by a greater amount than in the case of the ink jet recording head in accordance with the prior art, leaving a greater portion of the substrate 1 as the area to which the liquid passage plate ( FIG. 3 ) is glued.
[0049] Next, referring to FIG. 3 , what occurs as the ink jet recording head in accordance with the present invention is solidly bonded to the liquid passage plate, and the effects thereof, will be described in detail. FIG. 3 is a schematic drawing for describing the increase in the mechanical strength of the ink jet recording head attributable to the provision of the beam 1 a . The ink jet recording head in FIG. 3( a ) is virtually identical in structure to the ink jet recording head 20 shown in FIG. 2 , and is provided with a beam 1 a , which is located on the back side of the substrate 1 . The ink jet recording head in FIG. 3( b ) is also provided with a beam 1 b , which is located roughly in the middle of the head in its thickness direction.
[0050] Both the ink jet recording heads in FIGS. 3( a ) and 3 ( b ) are pasted to the corresponding liquid passage plates 15 , respectively, formed of resin. As the glue for bonding the ink jet recording heads to the corresponding liquid passage plates 15 , adhesive made of thermosetting resin is used. Since the ink jet recording heads are bonded to the liquid passage plates with the use of adhesive made of thermosetting resin, the liquid passage plate gradually contracts as its temperature returns to the normal one after the bonding. Since the material for the substrate 1 is silicon, whereas the material of the liquid passage plate is resin, a substantial amount of shearing stress is generated between the substrate 1 and liquid passage plate 15 , and this stress sometimes causes the substrate 1 to deform or break.
[0051] To compare in structure the ink jet recording head in FIG. 3( a ) and ink jet recording head in FIG. 3( b ), in the case of the head in FIG. 3( a ), one of the lateral surfaces of the beam 1 a coincides with the back surface of the substrate 1 . Therefore, the head in FIG. 3( a ) is greater in the size of the area by which it is bonded to the liquid passage plate 15 than the head in FIG. 3( b ), being therefore more resistant to the abovementioned shearing stress. Regardless of the presence or absence of shearing stress, being greater in the size of the bonding area is desirable from the standpoint of increase in bond strength. In comparison, in the case of the ink jet recording head in FIG. 3( b ), the head is greater in strength compared to the one which is not provided with the beam 1 b . However, compared to the head in FIG. 3( a ), it is smaller in the size of the bonding area, being therefore less resistant to the shearing stress.
[0052] Hereinafter, the manufacturing methods for the reinforcement beam for an ink jet recording head, and an ink jet recording head, in accordance with the present invention will be described with reference to the second to seventh embodiments of the present invention. In the following embodiments of the present invention, in order to simplify the descriptions thereof, the structural components, members, portions, etc., identical in function, will be given the same referential symbols as those given in FIGS. 1 and 2 , and will not be described in detail. Further, the heat generating members, wiring for driving the heat generating members, and ink passages to the ejection orifices, which are on the substrate, in the following embodiments, will not be illustrated, and the steps for forming the heat generating members and wiring will not be described.
[0053] First, referring to FIGS. 4 and 5 , “angular etching method”, or the technology to be used in the seventh embodiment, that is, the method for etching a substrate at an angle relative to the primary surface of the substrate, will be described. FIG. 4 is a schematic drawing of the apparatus used for performing “angularly etching method” used for the ink jet head manufacturing method in accordance with the present invention. FIG. 5 is a sectional view of the substrate 1 etched by such an etching method.
[0054] The etching apparatus 30 , shown in FIG. 4 , for angularly etching the substrate 1 comprises: an ordinary etching apparatus, which uses plasma to etch an object in a vacuum container 32 for forming a vacuumed space; and a jig (holder) 31 placed in the ordinary etching apparatus in order to hold an object (substrate 1 ) at an angle.
[0055] The etching apparatus 30 is structured so that the plasma generated in the plasma generating portion 33 , in the upper portion of the internal space of the vacuum container 32 advances downward. The object is etched in the direction in which the plasma advances. The substrate holding jig 31 is structured so that it can hold the object (substrate 1 ) at an angle of árelative to the plasma advancement direction.
[0056] The substrate 1 covered with a mask 11 is placed on the substrate holding jig 31 as shown in the drawing, and plasma is generated to etch the substrate 1 . As the plasma advances, the substrate 1 is etched at an angle, as shown in FIG. 5 , by the plasma which comes into contact with the substrate 1 through the hole 18 of the mask 11 . As a result, a groove 19 is formed. The side walls of the groove 19 hold the angle of árelative to the primary surface of the substrate 1 , and the groove 19 is roughly uniform in width (w).
[0057] The substrate 1 formed of silicon can be etched at a predetermined angle with the use of atoms of any of carbon, chloride, sulfur, fluorine, oxygen, hydrogen, and argon, or reactive gaseous molecules of any of the preceding elements.
Embodiment 2
[0058] Next, referring to FIGS. 6 and 7 , the method for manufacturing the ink jet recording head and the reinforcement beam therefor, in the first embodiment of the present invention will be described. The manufacturing method, which will be described next, is the manufacturing method for the ink jet recording head 21 shown in FIG. 6( i ).
[0059] The ink jet recording head 21 comprises a substrate 1 , and an orifice plate 3 having a plurality of ejection orifices (unshown) and placed on the substrate 1 , as does the ink jet recording head shown in FIGS. 1-3 . The substrate 1 of the ink jet recording head 21 is provided with three reinforcement beams 1 a similar in configuration to the one shown in FIG. 2( b ).
[0060] The common liquid chamber 9 extends from one end of the substrate 1 to the other, and has one opening (ink supplying hole 2 ), which faces the front side of the substrate 1 . The ink supplying hole 2 is connected to the ink passages (unshown) on the inward side of the orifice plate 3 . With the provision of this structural arrangement, the ink supplied from the common liquid chamber 9 is supplied to each of the ejection orifices (unshown) through the corresponding ink passage.
[0061] The side walls of the common liquid chamber 9 are formed of the same substance as that of which the substrate 1 is formed, and are parallel to the ( 111 ) face of the substrate material.
[0062] On the front and back surfaces of the substrate 1 , there partially remain the layers used during some of the manufacturing steps. The back surface of the substrate 1 is covered with a beam protecting layer 14 , and the front surface of the substrate 1 is covered with the passivation layer 12 , which is between the substrate 1 and orifice plate 3 . The passivation layer 12 is a layer needed during the formation of the ink passages 6 , and is resistant to certain types of etching.
[0063] The ink jet recording head 21 structured as described above is manufactured through the following steps. First, a precursor 21 a such as the one shown in FIG. 6( a ) is formed.
[0064] The precursor 21 a comprises: the substrate 1 ; the passivation layer 12 formed on the front (top) surface of the substrate 1 ; a dissolvable resin layer 13 partially covering the passivation layer 12 ; and the orifice plate 13 placed on the passivation layer 12 in a manner of covering the dissolvable resin layer 13 . The precursor 21 a also comprises a first mask 11 a having three holes 18 a and placed on the back surface of the substrate 1 . The distances among the three holes 18 a have been adjusted so that they roughly match the width of the bottom surface of the beam 1 a.
[0065] To describe in more detail, the precursor 21 a is formed through the following steps.
[0066] First, a silicon substrate is prepared, which has a predetermined thickness, and the primary surface of which is parallel to the ( 100 ) face of the silicon crystal. Then, the entire surface of the substrate 1 is oxidized using oxidization gas, forming a silicon dioxide layer across both the front (top) and back (bottom) surfaces of the substrate 1 . Then, the silicon dioxide layer is removed in entirety from the back side of the substrate 1 with the use of buffered hydrofluoric acid. During this process, a portion of the layer of the thermally oxidized silicon on the front surface of the substrate 1 , more specifically, the portion corresponding to the ink supplying hole 2 , is removed by the buffered hydrofluoric acid.
[0067] Then, a film of silicon nitride is formed as the passivation layer 12 on the front side of the substrate 1 by LPCVD (low pressure chemical vapor deposition). During this process, a silicon nitride film is also formed on the back side of the substrate 1 . However, this silicon nitride film (unshown) on the back side is removed; it can be removed by the etching method which uses reactive gaseous ions of CF 4 , for example.
[0068] Next, the resin layer 13 is formed in the pattern of ink passages (unshown), on the passivation layer 12 .
[0069] Next, the orifice plate 3 is solidly attached to the substrate 1 (passivation layer 12 ), being precisely positioned so that it covers the resin layer 13 .
[0070] Next, the first mask 11 a is formed of photosensitive resist, on the back surface of the substrate 1 , from which silicon is exposed, and the first holes 18 are formed.
[0071] The precursor 21 a is completed through the above described sequential steps.
[0072] Next, first grooves 19 a are formed as shown in FIG. 6( b ). More specifically, first, the substrate 1 is etched with the use of reactive gaseous ions of SF 6 from the back side, to form the first grooves 19 a having a predetermined depth. Incidentally, the opposing two lateral surfaces of each first groove 19 a are parallel to each other. Thereafter, the first mask 11 a is removed by ashing, which uses O 2 gas.
[0073] Next, silicon nitrate is formed by the plasma CVD, in each first groove 19 a and across the entirety of the back surface of the substrate 1 , forming the projections 41 a and beam protection layer 903 , as shown in FIG. 6( c ). Each projection 14 a in FIG. 6 is formed by filling each first groove 19 a with silicon nitride. However, it may be formed by covering the surfaces of each first groove 19 a with silicon nitride (protective member 14 ) as shown, in enlargement, in FIGS. 7( a ) and 7 ( b ). FIG. 7( a ) is an enlarged sectional view of one of the first grooves 19 a and its adjacencies in the state shown in FIG. 6( b ), and FIG. 7( b ) is an enlarged sectional view of the first groove 19 a and its adjacencies in the state shown in FIG. 6( c ).
[0074] Next, a second mask 11 b is formed of photoresist, on the beam protection layer 14 , and the portions of the beam protection layer 14 exposed through the patterned second mask 11 b are removed with the use of solution, the primary ingredient of which is phosphoric acid, in order to form four second holes 18 b , as shown in FIG. 6( d ).
[0075] Next, the substrate 1 is etched from the back side, with the use of reactive gaseous ions of SF 6 , forming four second holes 19 b having a predetermined depth, as shown in FIG. 6( e ). The remaining second mask 11 b is removed by ashing, with uses O 2 gas.
[0076] Next, referring to FIG. 6( f ), the substrate 1 is anisotropically etched from the walls of each second groove 19 b with the use of water solution of TMAH (tetra-methyl ammonium hydroxide). As a result, the substrate 1 is etched in a manner to expose the ( 111 ) face of the substrate 1 , leaving the portions 8 , which are triangular in cross section, above the beams 1 a.
[0077] Next, referring to FIG. 6( g ), as this etching process is allowed to continue, only the portions 8 are etched, whereas the beams 1 a are scarcely etched for the following reason. That is, each beam 1 a has the projection 14 b , which is in the center of the beam 1 a , and once the tip of each projection 14 a is exposed by etching, it prevents the beam 1 a from being etched further. The occurrence of this phenomenon means that the completed beam 1 a is resistant to corrosion; the beam 1 a is unlikely to be etched, because the tip of the projection 14 a is exposed at the top of the beam 1 a.
[0078] In the last step, the portions 8 a are entirely removed, leaving only the beams 1 a standing on the back side of the substrate 1 , as shown in FIG. 6( h ). As a result, the common liquid chamber 9 , which extends from one end of the substrate 1 to the other, is formed. The opening of the common liquid chamber 9 , on the front side of the substrate 1 , serves as the ink supplying hole 2 .
[0079] Next, the passivation layer 12 is etched away through the ink supplying hole 2 , with the use of the reactive gaseous ions of CF 4 , and the resin layer 3 is dissolved away with the solvent capable of dissolving the resin layer 3 . As a result, ink passages (unshown) are formed, as shown in FIG. 1( i ).
[0080] Through the above described sequential steps, the ink jet recording head 21 is manufactured.
[0081] To describe in more detail, each of the structural portions of the ink jet recording head 21 , and each of the above described steps for manufacturing the ink jet recording head 21 , may be as follows:
[0082] The configuration and size of the beams 1 a can be controlled by modifying the configurations of the first groove 19 a or second mask 11 b . When a substrate, the primary surface of which is parallel to the ( 100 ) face of the silicon crystal of which the substrate is made, is used to manufacture the ink jet recording head, there is the following relationship between the depth D of the first groove 19 a and the width W of the second mask 11 b , because the angle between the ( 100 ) face and ( 111 ) face is 54.7°:2D=Wùtan 54.7°. Thus, the configuration and size of the beam 1 a can be adjusted by calculating the measurements of the first groove 19 a and second mask 11 b.
[0083] Further, even when a substrate ( 1 ), the primary surface of which is parallel to the ( 110 ) face of the silicon crystal, is used, the configuration and size of the beam 1 a , in which the beam 1 will be after the anisotropic etching, can be controlled based on the angle between the ( 110 ) face and ( 111 ) face of the substrate ( 1 ).
[0084] Further, although the beam 1 a has the beam protection layer 14 and projection 14 a , they may be removed if necessary. The removal of the beam protection layer 14 and projection 14 a makes it possible to divide a single beam 1 a into multiple beams 1 a (two in the case of ink jet recording head 21 in FIG. 6 ).
[0085] The material for the first mask 11 a has only to be resistant to the step for forming the first groove 19 a . For example, inorganic film such as thermally oxidized film may be used in place of such organic film as photoresist.
[0086] As for the etching method for forming the first groove 19 a and second groove 19 b , any of the following methods may be used: wet etching, plasma etching, sputter etching, ion milling, laser abrasion based on excimer laser, YAG laser, or the like, sand blasting, etc., instead of reactive ion etching.
[0087] The materials for the beam protection layer 14 and projection 14 a do not need to be limited to the aforementioned substances, as long as the substances are resistant to anisotropic etching. In particular, when the beam 1 a having the beam protection layer 14 is formed in an ink jet recording head, it is desired that a substance resistant to ink is selected as the material for the beam protection layer 14 and projection 14 a . As for such materials, there are film of inorganic substance such as metal, oxide, nitride, etc., and film of organic substance such as resin. More specifically, Ti, Zr, Hf, V, Cr, Mo, W, Mn, Co, Ni, Ru, Os, Rh, Ir, Pd, Pt, Ag, Au, Ge, silicon compound, and polyether-amide resin, can be used.
[0088] The beam protection layer 14 and projection 14 a may be formed by thermally oxidizing the surface of the substrate 1 after the formation of the first groove 19 a . Further, they may be formed with the use of such film forming methods as vapor deposition, sputtering, plating, spin coating, burr coating, dip coating, etc., instead of the abovementioned CVD.
[0089] The material for the passivation layer 12 does not need to be limited to the abovementioned one, as long as it is resistant to the etching method for forming the common liquid chamber 9 . Further, in consideration of the fact that the second groove 19 b reaches the passivation layer 12 , the passivation layer 12 needs to be resistant to the etching process for forming the second groove 19 b . As for the method for forming the passivation layer 12 , such a conventional method as the vapor deposition, sputtering, chemical vapor phase epitaxy, plating, or thin film forming technology such as thin film coating, or the like, may be used.
[0090] As for the etching method for forming the common liquid chamber 9 , the method for anisotropically etching the silicon substrate 1 with the use of water solution of alkali as etchant may be used. Instead of TMAH, one among such etching liquids as KOH, EDP, hydrazine, or the like, the etching rate of which are affected by the face orientation of crystal, may be used. In any case, the ink supplying opening 2 can be precisely formed in terms of width (configuration) by using an etching method capable of anisotropically etching the silicon crystal.
[0091] As the method for forming the common liquid chamber 9 which extends through the substrate 1 , a sacrifice layer, the pattern and size of which matches the desired pattern and size of the ink supplying opening 2 , may be formed on the bottom surface of the passivation layer 12 . In such a case, in order to assure that while the silicon substrate 1 is etched for the formation of the common liquid chamber 9 , the sacrifice layer and the silicon (residual portion) immediately below the sacrifice layer are simultaneously etched, the sacrifice layer is to be formed of a substance that is isotropically etched by the etching liquid for forming the common liquid chamber 9 . When the abovementioned process is used, in which the sacrifice layer, which determines the shape in which the opening of the common liquid chamber 9 is formed, is formed on the substrate 1 , and then, the passivation layer 12 is formed on the sacrifice layer, it is possible to prevent the problem that when the substrate 1 is etched from the back side thereof, the ink supplying opening of the common liquid chamber 9 is inaccurately formed in shape and size, because of the deviation in the thickness of the substrate 1 , crystalline defects in the silicon crystal of which the substrate 1 is made, deviation in OF angle, deviation in the density of the etching liquid, or the like factors; in other words, it is possible to control the shape and size of the ink supplying hole 2 by controlling the pattern of the sacrifice layer.
[0092] As the material for the sacrifice layer, various substances, for example, semiconductive substances, dielectric substances, metallic substances, etc., can be used, as long as they are isotropically etched by the etchant used for anisotropically etching silicon crystal, and also, can be formed into thin film. More specifically, such semiconductors as polycrystalline silicon, porous crystalline silicon, and the like, such a metallic substance as aluminum, such a dielectric substance as ZnO, and the like, which are dissolvable into water solution of alkali, are preferable. In particular, polycrystalline silicon film is preferable as the material for the sacrifice layer, because it is superior in terms of the compatibility with an LSI process, and is higher in reproducibility. The sacrifice layer may be as thin as the thinnest film formable with the use of a selected material. For example, when the sacrifice layer is formed of polycrystalline silicon, in a thickness of roughly several hundreds of angstroms, the sacrifice layer can be isotropically etched at the same time as the substrate 1 is anisotropically etched.
Embodiment 3
[0093] Referring to 8 , the method for manufacturing the ink jet recording head and the reinforcement beam therefor, in another embodiment of the present invention, will be described. The manufacturing method which will be described next is for the ink jet recording head (unshown) similar to the ink jet recording head 21 shown in FIG. 6( i ), except that the beam protective layer 14 and projections 14 a of the ink jet recording head in this embodiment are formed of silicon dioxide instead of silicon nitride. The precursor 22 a shown in FIG. 8( e ) is identical in configuration to the precursor 21 a shown in FIG. 6( c ); the former is different from the latter only in the material for the beam protection layer 14 . Thus, the manufacturing steps performed after the step for forming the beam protection layer 14 are the same as the steps performed after the step used for forming the intermediate product shown in FIG. 6( d ), and therefore, they will not be described.
[0094] The process for manufacturing the precursor 22 a is as follows:
[0095] First, the substrate 1 is prepared, and the first mask 11 a is formed on the back surface of the substrate 1 , as shown in FIG. 8( a ), through the same step as the step used for forming the precursor 21 a shown in FIG. 6( a ).
[0096] Next, the first grooves 19 a are formed, as shown in FIG. 8( b ), through the same step as the step used for forming the intermediate product shown in FIG. 6( b ).
[0097] Next, the entirety of the surfaces of the substrate 1 are thermally oxidized with the use of oxidization gas. As a result, not only is a film 14 of silicon dioxide formed on both the front and back surfaces of the substrate 1 , but also, the projection 14 a is formed of silicon dioxide, in each of the first grooves 19 a , as shown in FIG. 8( c ).
[0098] Next, the portion of the film 14 on the front surface of the substrate 1 , which corresponds to the ink supplying opening (unshown), is removed with the use of buffered hydrofluoric acid, as shown in FIG. 8( d ).
[0099] Next, the passivation layer 2 , resin layer 13 , and orifice plate 3 are sequentially formed, as shown in FIG. 8( e ), through the same manufacturing steps as those used for preparing the precursor 21 a shown in FIG. 6( a ).
[0100] Through the above described sequential steps, the precursor 22 a ( FIG. 8( e )), the state of which is virtually identical to that of the precursor 21 a shown in FIG. 6( c ), is formed. This precursor 22 a is used to manufacture the ink jet recording head (unshown) in this embodiment, through the same steps as those carried out after the step used for forming the intermediate product shown in FIG. 6( d ).
Embodiment 4
[0101] Next, referring to FIG. 9 , the method for manufacturing the ink jet recording head and the reinforcement beam therefor, in another embodiment of the present invention will be described. The manufacturing method which will be described next is for the ink jet recording head (unshown), which has the first mask 11 a between the substrate 1 and beam protection film 14 . The process for manufacturing the precursor 23 a shown in FIG. 9( e ) is for forming this ink jet recording head (unshown), and is in the same state as the state of the precursor 21 a shown in FIG. 6( e ), that is, the first mask 11 a has been formed between the substrate 1 and beam protection layer 14 . The manufacturing steps carried out after the step used for forming the intermediate product shown in FIG. 9( e ) are the same as those carried out after the step used for forming the intermediate product shown in FIG. 6( e ), and therefore, will not be described.
[0102] First, referring to FIG. 9( a ), the precursor 23 a is prepared through the same steps as those used for forming the precursor 21 a shown in FIG. 6( a ).
[0103] The precursor 23 a is identical in configuration to the precursor 21 a shown in FIG. 6( a ). However, the first mask 11 a of this precursor 23 a is formed of polyether-amide resin, which is resistant to the anisotropic etching. The first mask 11 a is used as the mask for the anisotropic etching process, which will be described later.
[0104] Next, the first grooves 19 a are formed, as shown in FIG. 9( b ), through the same step as the step used for forming the intermediate product shown in FIG. 6( b ).
[0105] Next, the projections 14 a are formed of resin inside of each first groove 19 a , and the beam protection film 14 is formed of resin film on the first mask 11 a , by a bar code method, as shown in FIG. 9( c ). In the step used for forming the intermediate product shown in FIG. 6( c ), which was described in the description of the second embodiment, the projections 14 a and beam protection layer 14 are formed of silicon nitride, with the use of CVD. In comparison, the projections 14 a and beam protection layer 14 in this embodiment are formed of resinous substance as described above.
[0106] Next, the second mask 11 b having the second holes 18 b is formed on the beam protection layer 14 , as shown in FIG. 9( d ), through the same steps as those used to form the intermediate product shown in FIG. 6( d ).
[0107] Next, the second grooves 19 b are formed, as shown in FIG. 9( e ), through the same step as the one used for forming the intermediate product shown in FIG. 6( e ).
[0108] Through the above described sequential steps, the precursor 23 a ( FIG. 9( e )), the state of which is roughly the same as that of the precursor 21 a shown in FIG. 6( e ), is formed. Then, the precursor 23 a is used to manufacture the ink jet recording head (unshown) in this embodiment through the same steps as the steps carried out after the step used for forming the intermediate product shown in FIG. 6( e ).
[0109] As will be evident from the above description of the preferred embodiments of the present invention, the beam protection layer 14 and projections 14 a can be varied in material. The material for beam protection layer 14 and projections 14 may be a metallic substance (Pt, for example), instead of being one of the resins mentioned above. When the beam protection layer 14 and projections 14 a are formed of a metallic substance, they may be formed by sputtering.
[0110] The shape in which the beam in this embodiment is form can be controlled by modifying the shapes of the beam protection film and projections. Next, examples of beams different in shape from the beams in the preceding embodiments will be described.
Embodiment 5
[0111] It is possible to form a beam, which is pentagonal in cross section, by adjusting the first grooves in depth, and the width of the bottom of the beam.
[0112] Next, referring to FIG. 10 , the method usable for manufacturing an ink jet recording head, the beams of which are pentagonal in cross section, will be described. The manufacturing method, which will be described next, is for manufacturing the ink jet recording head 24 shown in FIG. 10( e ).
[0113] First, a precursor 24 a in the state shown in FIG. 10( a ) is formed through the steps similar to the steps used for forming the intermediate products shown in FIGS. 6( a ) and 6 ( b ).
[0114] Compared to the grooves 19 a of the precursor 21 a in the state shown in FIG. 6( b ), the grooves 19 a of the precursor 24 a in the state shown in FIG. 10( a ) are shallower, being 150 ìm, for example, in depth.
[0115] Next, the precursor 24 a in the state shown in FIG. 10( b ) is formed through the same steps as the steps used to form the precursor 21 a into the states shown in FIGS. 6( c ) and 6 ( d ). The state of the precursor 24 a shown in FIG. 10( b ) is the same as the state of the precursor 21 a shown in FIG. 6( d ); in other words, the second holes 18 b have been formed. The distance between the adjacent two holes 18 a , that is, the width of the portion of the mask 11 b for controlling the width of the bottom of each beam 1 a , is 300 ìm, for example.
[0116] Next, the second grooves 19 b shown in FIG. 10( c ) are formed through the step used for forming the precursor 21 a into the state shown in FIG. 6( e ).
[0117] Next, the substrate 1 is anisotropically etched from the walls of each of the second grooves 19 b through the same steps as those used for forming the precursor 21 a into the states shown in FIGS. 6( f ) and 6 ( g ). As a result, the beams 1 a , shown in FIG. 10( d ), which are pentagonal in cross section, are formed. The reason why the beams 1 a are formed so that they become pentagonal in cross section is that the height of each projection 14 a is less than the width of the bottom of the corresponding beam 1 a . In other words, one of the characteristics of the anisotropic etching that the anisotropic etching progresses in the direction of exposing the ( 111 ) face of the silicon crystal, is utilized to form the beams 1 a which are pentagonal in cross section.
[0118] Next, the same step as the step used for forming the precursor 21 a shown in FIG. 6( h ) is continued to form the precursor 24 a in the state shown in FIG. 10( h ), which has the beams 1 a which are roughly triangular in cross section, and the common liquid chamber 9 . As a result, the ink jet recording head 24 , which is identical in structure as the ink jet recording head 21 shown in FIG. 6( i ) is formed.
Embodiment 6
[0119] As will be evident from the description of the preceding embodiments, the shape in which each beam 1 a is formed in terms of cross section can be varied by adjusting in width the corresponding first groove and the width of the beam 1 a.
[0120] Next, referring to FIG. 11 , the method for forming beams 1 a , the cross sections of which are in the form of letter W placed upside down, will be described. The manufacturing method which will be described next is for manufacturing the ink jet recording head 25 shown in FIG. 11( d ), the cross section of the beams 1 c of which are in the form of letter W placed upside down. More specifically, the precursor of each of the beams 1 a is triangular in cross section, and its two base angles are 54.7°. During the step for forming the beams 1 c , the precursor of each beam 1 c , which is triangular in cross section ( FIG. 11( c )), is etched at an angle of 54.7°, starting from its peak. As a result, a recess is formed between the two projections in the precursor of each beam 1 c . The surfaces of each beam 1 c , other than the bottom surface thereof, are roughly parallel to ( 111 ) face of the substrate 1 .
[0121] First, the precursor 25 a shown in FIG. 11( a ) is formed through the steps similar to the steps used for forming the precursor 21 a into the states shown in FIGS. 6( a )- 6 ( c ).
[0122] The precursor 25 a is virtually the same as the precursor 21 a shown in FIG. 6( c ). It has the beam protection layer 14 , which is on the back surface of the substrate 1 , and two pairs of projections 14 a , which have a predetermined depth and have been extended into the substrate 1 a . The paired projections 14 a are positioned a predetermined distance apart from each other.
[0123] Next, the second grooves 19 b shown in FIG. 11( b ) are formed through the steps similar to the steps used for forming the precursor 21 a into the states shown in FIGS. 6( d ) and 6 ( e ). The second grooves 19 b are formed so that the distance between the adjacent two second grooves 19 b becomes roughly the same as the width of the bottom of the beam 1 a.
[0124] Next, in order to form the precursor 25 a into the state shown in FIG. 11( c ), the substrate 1 is etched through the steps used for forming the precursor 21 a into the state shown in FIG. 6( f ). The beams 1 d in the precursor 25 a in the state shown in FIG. 11( c ) are triangular in cross section, and the peak of each beam 1 d is at the center between the corresponding pair of projections 14 a , in terms of the direction parallel to the primary surface of the substrate 1 .
[0125] Next, the etching process is allowed to progress through the step similar to the step through which the precursor 21 a is formed into the state shown in FIG. 6( f ) to form the beams 1 d in the shape shown in FIG. 11( d ). As a result, the etching begins from the top of the precursor of each beam 1 d , yielding the beam 1 d , the cross section of which is in the form of letter W placed upside down. Further, at the same time as the precursor of each beam 1 d is etched starting from its peak, the common liquid chamber 9 is completed. As a result, the ink jet recording head 25 in this embodiment is yielded.
[0126] The beam 1 d in this embodiment has only one recess, which is located between the two peaks. However, the number of the recesses can be increased by increasing the number of the projections 14 a in each set of projections 14 a . A recess such as the one described above functions as a means for trapping the gas which adversely affects the ink ejection from an ink jet recording head.
Embodiment 7
[0127] In the above described preceding embodiments, the projections 14 a are formed perpendicular to the substrate 1 . However, it is possible to form the projections 14 a at an angle with the use of the “angular etching method” shown in FIGS. 4 and 5 . Therefore, with the use of this etching method, the number of the various shapes in which each beam is formed in terms of cross section can be substantially increased.
[0128] Next, referring to FIG. 12 , the method for manufacturing an ink jet recording head provided with inclined projections will be described. The manufacturing method which will be described next is for manufacturing the ink jet recording head 26 shown in FIG. 12( d ), the projection 14 a in each beam 1 e is tilted relative to the primary surface of the substrate 1 .
[0129] First, the precursor 26 a shown in FIG. 12( a ) is formed through the steps roughly similar to the steps used for forming the intermediate products shown in FIGS. 6( a )- 6 ( c ), except that the first grooves (which corresponds to projection 14 b in FIG. 12( a )) are formed with the use of the angularly etching apparatus 30 shown in FIG. 4 .
[0130] Next, the intermediate product shown in FIG. 12( b ) is formed by forming the second holes 18 b through the step similar to the step used for forming the intermediate product shown in FIG. 6( d ), and then, forming the second grooves 12 b through the step similar to the step used for forming the intermediate product shown in FIG. 6( e ).
[0131] Next, the substrate 1 is etched as shown in FIG. 12( c ) through the step similar to the step used for forming the intermediate product shown in FIG. 6( f ). As a result, the beams 1 e are formed so that their peaks will coincide with the corresponding tips of the projections 14 b.
[0132] Next, the etching is allowed to continue through the steps similar to the steps carried out after the step used for forming the intermediate product shown in FIG. 6( g ). As the etching is allowed to continue, the beams 1 e and common liquid chamber 9 are formed, yielding the ink jet recording head 26 in this embodiment shown in FIG. 12( d ).
[0133] The ink jet recording heads 21 - 26 ( FIGS. 6-12 ) in the second to seventh embodiments, respectively, were manufactured, and were tested to confirm their characteristics.
[0134] For the purpose of confirming their mechanical strength, the ink jet recording heads 21 - 26 ( FIGS. 6-12 ) were compared to an ink jet recording head in accordance with the prior art.
[0135] The ink jet recording head in accordance with the prior art was identical in the measurement of the ejection element to the ink jet recording heads 21 - 26 , but was not provided with the beam. All the ink jet recording heads were subjected to destruction tests in which load is applied to them in the direction parallel to the width direction of the ink supplying hole until the substrates 1 were damaged.
[0136] None of the ink jet recording heads 21 - 26 in accordance with the present invention were damaged by the minimum amount of load which damaged the ink jet recording head in accordance with the prior art. In other words, these tests proved that all of the ink jet recording heads 21 - 26 in the preferred embodiments of the present invention were superior in mechanical strength to the ink jet recording head in accordance with the prior art.
[0137] When images were printed with the ink jet recording heads 21 - 26 , they were uniform in refill characteristic; they were roughly identical in the distance from the ink supplying hole to the heat generating member, and refilling time.
[0138] When the beams with which the ink jet recording heads 21 - 26 were provided were kept in ink for three months, none of the beams changed in shape, and also, the beams 1 c of the intermediate product ( FIG. 10( d )) derived from the precursor 24 a of the ink jet recording head 24 shown in FIG. 10 did not change in shape.
[0139] In the above described preferred embodiments of the present invention, the beams were formed so that they extended in the width direction (direction Y in FIG. 1 ) of the substrate. However, the direction in which the beams extend does not need to be limited. For example, they may be formed so that they extend in the lengthwise direction of the substrate. Further, the beams may be formed so that they form a grid. When forming the beams in a grid pattern, they may be formed at a narrow pitch in one direction or both directions so that they collectively function as a filter to prevent the foreign particles having mixed into ink from entering the common liquid chamber 9 . When the beams are applied to microscopic structures other than ink jet recording heads, it is not mandatory that they are held to the mother member by both of their lengthwise ends; they may be held to the mother member by only one of the their lengthwise ends.
[0140] The beams may be in various forms different from those in the above described embodiments. For example, by shifting the position of the center of each of the first grooves from the center of the second mask in terms of the widthwise direction of the mask, it is possible to form asymmetrical beams. Further, by forming the first grooves, the walls of which are perpendicular to the substrate 1 , at the edge of the second mask, it is possible to form beams, the cross section of which are in the form of a right-angled triangle. In order to form such beams, the projection formed in each of the first grooves becomes the wall of the corresponding beam, which is perpendicular to the bottom surface of the beam. Further, by controlling in shape the first grooves and second mask, it is possible to form such beams that are U-shaped in cross section.
[0141] Further, as described above, the vertical measurement in which each of the above described beams is formed can be easily changed by forming the first grooves so that they extend from the bottom to the peak of the beam. Therefore, the beam can be formed in various shapes. Similarly, the width in which the bottom of each beam is formed can be easily changed by changing the shape of the masking member.
[0142] The structure of each of the ink jet recording heads in the above described embodiments of the present invention is effective when applied to ink jet recording heads which employs the “liquid ejection method of bursting bubble type”, or “bursting bubble liquid ejecting method”.
[0143] The “bubble bursting liquid ejection method” means an ink jet recording method in which the bubbles generated by the film boiling triggered by the heating of ink are allowed to burst into the external air in the adjacencies of the ejection orifices, and has been proposed in Japanese Laid-open Patent Applications 2-112832, 2-112383, 2-112834, 2-114472, and the like.
[0144] The “bubble bursting liquid ejecting method” ensures that the bubbles rapidly grow toward an ejection orifice. Therefore, the “bubble bursting liquid ejecting method” makes it possible to highly reliably record at a high speed, while being assisted by the high rate of ink refilling performance achieved by the provision of the ink supplying hole with no blockage. Further, allowing the bubbles to burst into the external air eliminates the process in which the bubbles shrink. Therefore, the heaters and substrates are not damaged by cavitation. Further, one of the characteristic aspects of the “bubble bursting liquid ejection method” is that, in principle, all the ink on the ejection orifice side of the location, at which bubbles are formed, is ejected in the form of an ink droplet. Therefore, the amount by which ink is ejected per ejection is determined by such factors as the distance from the ejection orifice to the bubble generation point, recording head structure, and the like. Therefore, the abovementioned “bubble bursting liquid ejection method” is stable in the amount by which ink is ejected; it is less likely to be affected by the changes in ink temperature or the like.
[0145] In the case of an ink jet recording head of the side shooter type, the distance between an ink ejection orifice and the corresponding heat generating member can be easily controlled by controlling the thickness of an orifice plate, and this distance is one of the most important factors that determine the amount by which ink is ejected. Therefore, the ink jet recording heads in accordance with the present invention are well suited in structure for the “bubble bursting liquid ejection method”.
[0146] To sum up, not only is the beam in accordance with the present invention well suited for ink jet recording apparatuses, but also, various microscopic structures employing beams. Further, not only is the beam forming method in accordance with the present invention useful for manufacturing an ink jet recording apparatuses, but also, various microscopic structures employing beams. In particular, they are useful when the anisotropic etching method is used during the manufacturing process for a microscopically structured product.
[0147] Lastly, referring to FIGS. 13 and 14 , a typical ink jet recording apparatus and a typical ink jet head cartridge, which are compatible with an ink jet recording head in accordance with the present invention, will be described.
[0148] The ink jet recording apparatus shown in FIG. 13 comprises: a recording sheet feeding portion 1509 from which recording papers are fed into the main assembly of the ink jet recording apparatus; a recording portion 1510 which records on the recording sheet fed from the record sheet feeding portion 1509 ; a delivery tray portion 1511 into which the recording sheet is discharged after an image is recorded thereon. Recording is made by the recording portion 1510 , on the recording sheet fed from the recording sheet feeding portion 1509 , and then, the recording sheet is discharged into the delivery tray portion 1511 after the completion of the recording.
[0149] The recording portion 1510 is supported by a guiding shaft 1506 so that it is allowed to freely slide along the shaft 1506 . It comprises: a carriage 1503 structured so that it can be freely shuttled in the direction parallel to the width direction of the recording sheet; a recording unit 1501 removably mountable on the carriage 1503 ; and a plurality of ink cartridges 1502 .
[0150] The ink jet head cartridge 1501 shown in FIG. 14 is the combination of a holder 1602 and a recording head 1601 attached to the holder 1602 . The recording head 1601 is provided with a plurality of ejection orifices 104 . The holder 1602 is provided with ink passages (unshown) for supplying the ejection orifices 104 of the ink jet recording head 1601 , with the ink from the ink cartridges 1502 .
[0151] While the invention has been described with reference to the structures disclosed herein, it is not confined to the details set forth, and this application is intended to cover such modifications or changes as may come within the purposes of the improvements or the scope of the following claims.
[0152] This application claims priority from Japanese Patent Application No. 416843/2003 filed Dec. 15, 2003, which is hereby incorporated by reference.
|
A beam having a base material of silicon monocrystal and at least one projection which is integrally formed so as to be supported at least at one end thereof and which has two surfaces having an orientation plane ( 111 ), includes a bottom surface in a plane which is common with a plane of the base material; a groove penetrating from the bottom surface to a top of the projection; and a protecting member having a resistance property against a crystal anisotropic etching liquid and covering an inner wall of the groove.
| 1
|
CROSS-REFERENCE TO RELATED APPLICATION
This non-provisional application claims priority under 35 U.S.C. §119(a) on Patent Application No. 2004-318769 filed in Japan on Nov. 2, 2004, the entire contents of which are hereby incorporated by reference.
TECHNICAL FIELD
This invention relates to a method of separating a water-soluble cellulose ether from its suspension in water as a filter cake by pressure filtration, the water-soluble cellulose ether typically having excellent plastic properties and high dissolution temperature. A water-soluble cellulose ether behaves as follows after it is dispersed in hot water. As the dispersion cools, the cellulose ether is slowly dissolved in water so that the water-soluble cellulose ether solution increases its viscosity in proportion. In this course, however, at a certain temperature, the rate of viscosity increase becomes slowed down. The “dissolution temperature” is determined by dispersing a water-soluble cellulose ether in hot water at or above 95° C. in a concentration of 1% by weight, cooling the dispersion (which builds up a viscosity with a lowering of temperature), monitoring the viscosity of the dispersion, and detecting the temperature at which the viscosity makes a substantial change relative to a lowering of temperature (that is, the rate of viscosity increase becomes slowed down).
BACKGROUND ART
Methyl cellulose is prepared by etherifying alkali cellulose with methyl chloride at temperatures of about 50 to 90° C. as described in Examples of JP-B 7-119241. After the etherifying reaction, the reaction mixture is introduced into an agitator vessel containing water at about 95° C. where the salt formed during the reaction is dissolved in water. The suspension exiting the agitator vessel is then subjected to a separation operation in order to obtain the desired pure cellulose ether.
In the separation operation, the use of rotary pressure filters is considered. However, the customary textile filter coverings for rotary pressure filters suffer from the problem that products having a high dissolution temperature penetrate and dwell in the filter so that the filter is clogged and becomes inoperative within a short filtering time. The clogging may be cleared by washing with high-pressure steam or hot water, the customary mesh size filter can be stretched in mesh size or even ruptured. The problem is overcome in U.S. Pat. No. 4,954,268 or Japanese Patent No. 2,895,084 by using a filter of multi-layer sintered metal structure having an increased strength. The multi-layer structure leaves a problem that once the filter is clogged with the product, it is difficult to remove the clogging product by washing.
DISCLOSURE OF THE INVENTION
An object of the present invention is to provide a method of separating a water-soluble cellulose ether from its suspension in water using a filter system while avoiding the filter from being clogged and permitting the filter system to operate effectively over an extended period of time.
The inventor has found that a water-soluble cellulose ether can be separated from a suspension of water-soluble cellulose ether in water without substantial problems by filtering through a filter system using a perforated metal or ceramic filter medium, and cleaning the filter medium with steam, compressed air or water under pressure after the filtration. The filter system is kept operable for a long period. The cleaning of the filter medium after filtration not only prevents the filter medium from being clogged, but also washes out the water-soluble cellulose ether remaining within the filter medium, eliminating any loss of water-soluble cellulose ether.
The present invention provides a method of separating a water-soluble cellulose ether from its suspension, comprising the steps of passing a suspension of water-soluble cellulose ether particles in water through a pressure filter of perforated metallic or ceramic filter medium for leaving a cake of water-soluble cellulose ether on the filter, removing the filter cake from the filter medium, and cleaning the filter medium with steam, compressed air or water under pressure.
Preferably the filter medium is perforated to a pore size substantially corresponding to an average diameter of suspended particles. The filter medium is typically a special steel containing at least 8% by weight of nickel and at least 18% by weight of chromium. The preferred suspension comprises the water-soluble cellulose ether and water in a weight ratio of 10/100 to 50/100. The water-soluble cellulose ether is typically an alkyl cellulose, hydroxyalkyl alkyl cellulose or hydroxyalkyl cellulose.
In a preferred embodiment, the method further comprises the steps of washing the filter cake with one or both of hot water and steam, and back blowing steam, compressed air or water under pressure from the filter medium side to loosen the filter cake from the filter medium, prior to the removal of the filter cake.
In a further preferred embodiment, after the removal of the filter cake from the filter medium, water under pressure is sprayed to the filter medium from a jet nozzle for rinsing the filter medium and the resulting rinse water is recycled for washing the filter cake.
The present invention enables to separate a water-soluble cellulose ether, especially having a high dissolution temperature, from a suspension of water-soluble cellulose ether in water, avoids the filter system from being clogged, and extends the operative time of the filter system.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The method of the invention is for separating a water-soluble cellulose ether from a suspension of water-soluble cellulose ether particles in water using a filter. The filter is made of a perforated metallic or ceramic filter medium.
The filter medium should preferably be perforated to a pore size substantially corresponding to an average diameter of suspended particles. The filter medium with such a pore size can capture even fine particles having a smaller diameter than the pore size.
For corrosion prevention, the metal material used herein may be selected from special steels having corrosion resistance, specifically special steels containing at least 5% by weight of nonferrous metals. For example, special steels which are resistant to salts in water-soluble cellulose ether suspended liquids and filter cake wash liquids are preferred, with special steels containing at least 8% by weight of nickel and at least 18% by weight of chromium being more preferred as the perforated filter medium. The use of such metallic filter medium prevents the occurrence of stress crack corrosion due to the high salt content of the hot suspension.
These perforated materials can be manufactured by known methods as described in T. Terabayashi and K. Kajio, “Study on Electron Beam Machining,” Journal of Precision Engineering Society, vol. 53, No. 5, 1987, pp. 789-794; and K. Kajio, “High-Speed Drilling of Difficult-to-Electron-Beam-Machine Materials,” Machinery Technology, vol. 37, No. 8, pp. 47-52.
The ceramic material may be selected from oxide and non-oxide based ceramic materials having salt resistance, for example, alumina, magnesia, zirconia, and ferrite. Silicon carbide, silicon nitride and similar ceramic materials are also useful. Zirconia is most preferred because of toughness.
The filter medium typically has a thickness of 0.2 to 20 mm, preferably 2 to 10 mm, in the filtrate direction.
The water-soluble cellulose ether used in the present invention preferably has a dissolution temperature of at least 20° C. and may include an alkyl cellulose, hydroxyalkyl cellulose, and hydroxyalkyl alkyl cellulose.
Examples of alkyl cellulose include methyl cellulose having 1.0 to 2.2 of methoxyl group (DS), and ethyl cellulose having 2.0 to 2.6 of ethoxyl groups (DS).
Examples of hydroxyalkyl cellulose include hydroxypropyl cellulose having 0.05 to 3.3 of hydroxypropoxyl group (MS).
Examples of hydroxyalkyl alkyl cellulose include hydroxyethyl methyl cellulose having 1.0 to 2.2 of methoxyl group (DS) and 0.1 to 0.6 of hydroxyethoxyl group (MS), hydroxypropyl methyl cellulose having 1.0 to 2.2 of methoxyl group (DS) and 0.1 to 0.6 of hydroxypropoxyl group (MS), and hydroxyethyl ethyl cellulose having 1.0 to 2.2 of ethoxyl group (DS) and 0.1 to 0.6 of hydroxyethoxyl group (MS).
“DS” is “Degree of Substitution” which means that the average number of alkoxyl groups attached to the anhydroglucose unit of cellulose. “MS” is “Molar Substitution” which means that the average number of moles of hydroxylalkyl groups per mole of anhydroglucose unit of cellulose.
Among them, preferred are hydroxyethyl methyl cellulose and hydroxypropyl methyl cellulose each having a high dissolution temperature (30 to 60° C.).
For collecting the water-soluble cellulose ether in high yields after filtration, the suspension used preferably comprises the water-soluble cellulose ether and water in a weight ratio of 10/100 to 50/100. The suspension should have a concentration enough to pump.
The water-soluble cellulose ether particles in the suspension liquid preferably have an average particle size of 0.1 to 2,000 μm as measured by sifting method.
As described above, the separating method of the invention involves filtering a suspension of water-soluble cellulose ether particles in water through a pressure filter of perforated metallic or ceramic filter medium for leaving a cake of water-soluble cellulose ether on the filter, removing the filter cake from the filter medium, and cleaning the filter medium with steam, compressed air, water under pressure or hot water.
In the step of filtering a suspension of water-soluble cellulose ether particles in water through a pressure filter of perforated metallic or ceramic filter medium, the suspension to be filtered is preferably at a temperature of 20 to 160° C., more preferably 70 to 140° C. because of cost performance, filter protection and prevention of dissolution of cellulose ether. The suspension to be filtered may be a liquid further containing sodium chloride and other salts in a concentration of about 1 to 30% by weight, in the reaction mixture resulting from etherifying reaction for the preparation of water-soluble cellulose ether and containing water-soluble cellulose ether, water, sodium chloride, other salts and organic matters.
For the pressure filtration, the pressure may vary over a wide range although the preferred pressure is generally in a range of about 0.001 to 1 MPa, especially about 0.01 to 0.5 MPa.
As a result of filtration, a cake of water-soluble cellulose ether is left on the filter. The cake is then removed from the filter medium. In the subsequent step, the filter medium is cleaned with steam, compressed air, water under pressure or hot water. The steam used herein is preferably at a temperature of 100 to 185° C., more preferably 100 to 160° C. and a pressure of 0.001 to 1 MPa, more preferably 0.01 to 0.5 MPa. The compressed air used herein is preferably at a pressure of 0.001 to 1 MPa, more preferably 0.01 to 0.5 MPa and a temperature of 10 to 160° C., more preferably 20 to 140° C. The pressurized water used herein is preferably at a temperature of 10 to 160° C., more preferably 20 to 140° C. and a pressure of 0.001 to 15 MPa. The hot water used herein is preferably at a temperature of 50 to 160° C., more preferably 70 to 140° C. and a pressure of 0.001 to 3 MPa.
In a preferred embodiment, after the filtration, the cake is washed with hot water and/or steam, and steam, compressed air or water under pressure is then blown back into the filter from the filter medium side (remote from the cake-depositing side) to loosen the cake from the filter medium, prior to the removal of the cake. By these steps, the foreign materials such as salts are washed out of the filter cake. Then the filter cake is composed essentially of the water-soluble cellulose ether, with the foreign materials such as salts being almost removed.
In a further preferred embodiment, after the removal of the filter cake from the filter medium, a flat jet nozzle is used to spray hot water under a pressure of at least 1 MPa, preferably 1.5 to 2 MPa, and at a temperature of 90 to 212° C., to the filter medium for rinsing the perforated filter medium in the filtrate direction. The resulting rinse water is recycled as the cake washing water (i.e., the source for water under pressure or steam), which becomes an aqueous solution containing salts to serve to reduce the dissolution temperature of the product having a high dissolution temperature, preventing clogging due to dissolution during the washing. In the hot water spraying step, the filter medium is cleaned, and the valuable product remaining in the filter medium is recovered and returned to the process, contributing to an improvement in yield.
While the separating method of the invention involves passing a suspension of water-soluble cellulose ether particles in water through a pressure filter of perforated metallic or ceramic filter medium, the pressure filter used herein may be a rotary pressure filter as illustrated in FIG. 1 of Japanese Patent No. 2,895,084, and filtration operation may be performed by the same procedure as illustrated in FIG. 3 except that the filter medium is different.
EXAMPLE
The invention is illustrated by the following example, which is given for illustration purposes only and is not meant to limit the invention. The filter used is a rotary pressure filter as illustrated in Japanese Patent No. 2,895,084 and manufactured by BHS of Germany.
Example 1
A hydroxyethyl methyl cellulose (HEMC) having 1.46 of methoxyl groups (DS) and 0.32 of hydroxyethyl groups (MS) and a dissolution temperature of 55° C., which was a reaction mixture after etherification reaction, was mixed with an amount of boiling water of 95° C. to produce a suspension containing 12 parts by weight of HEMC in 100 parts by weight of water. The suspension contained salts mainly composed of sodium chloride in a concentration of 6% by weight.
The suspension at 95° C. was fed to a rotary pressure filter, preheated at 100° C., with a filter surface area of 1 m 2 and 1 drum rotation per minute, under a pumping pressure of 0.2 MPa. The filter used was a perforated steel filter (pore size: 0.07 mm in diameter, plate thickness: 0.3 mm, pore pitch in the same direction as filter rotation: 0.30 mm, pore pitch in a direction perpendicular to filter rotation: 0.26 mm, material: stainless steel SUS304) manufactured by Pacific Special Alloy Castings Co., Ltd.
On the filter surface, a closed filter cake of 20 mm thick was formed. It was then intensively blown out with steam at 34° C. and 0.2 MPa.
Prior to the removal of the filter cake, hot water (95° C., 0.2 MPa) washing in the filtrate direction was followed by compressed air (20° C., 5 MPa) blowing in the backward direction to loosen the cake. Then the cake was removed from the filter surface by means of a scraper.
Following removal of the cake, hot water at 90° C. under a pressure of 1 MPa, preferably 1.5 to 2 MPa was sprayed to the perforated filter medium from flat jet nozzles for intensively cleaning matters adhered to the filter medium.
The filter cake was dried at 100° C. for 3 hours, after which the content of residual salts in the filter cake was measured to be 0.1% by weight to the dried hydroxypropyl methyl cellulose as analyzed by the measurement method of a heat loss described in the hydroxypropyl methyl cellulose assay of Japanese Pharmacopoeia, 14th Ed.
Then the cycle described was similarly repeated using the water under pressure at 90° C. consumed in the cleaning of the filter medium as the cake washing water. Performance comparisons over many hours did not reveal declining filter throughput.
Example 2
A hydroxypropyl methyl cellulose (HPMC) having 1.50 of methoxyl groups (DS) and 0.20 of hydroxypropoxyl groups (MS) and a dissolution temperature of 40° C., which was a reaction mixture after etherification reaction, was mixed with an amount of boiling water of 95° C. to produce a suspension containing 50 parts by weight of HPMC in 100 parts by weight of water. The salt concentration in the suspension was 25% by weight.
The suspension was processed as in Example 1 except that the filter used was a perforated zirconia ceramic filter with the same specifications. Following removal of the cake, water under pressure (90° C., 10 MPa) was sprayed to the perforated filter medium from flat jet nozzles for intensively cleaning matters adhered to the filter medium.
The filter cake was dried at 100° C. for 3 hours, after which a heat loss was measured to be 0.01% by weight to the dried hydroxypropyl methyl cellulose as analyzed by the method in the hydroxypropyl methyl cellulose assay of Japanese Pharmacopoeia, 14th Ed. No decline of filter throughput was observed over many hours.
The hydroxypropyl methyl cellulose thus collected had a viscosity of 4,000 mPa·s as measured in a 2 wt % aqueous solution thereof at 20° C. by the HPMC2208 viscosity measurement of US Pharmacopoeia.
The process sequence can also be carried out with the appropriate modifications in pressure filter funnels operating batchwise.
Japanese Patent Application No. 2004-318769 is incorporated herein by reference.
Although some preferred embodiments have been described, many modifications and variations may be made thereto in light of the above teachings. It is therefore to be understood that the invention may be practiced otherwise than as specifically described without departing from the scope of the appended claims.
|
A water-soluble cellulose ether is separated from its suspension by passing a suspension of water-soluble cellulose ether particles in water through a filter of perforated metallic or ceramic filter medium under pressure, removing the filter cake of water-soluble cellulose ether from the filter medium, and cleaning the filter medium with steam, compressed air or water under pressure. The invention enables to separate a water-soluble cellulose ether, especially having a high dissolution temperature, avoids the filter from being clogged, and extends the operative time of the filter.
| 2
|
BACKGROUND OF THE INVENTION
(1) Field of the Invention
This invention relates to quick opening windows such as may be employed to provide a safety exit from an enclosure such as a trailer or mobile home.
(2) Description of the Prior Art
Prior structures of this type are best illustrated in U.S. Pat. Nos. 900,407 and 4,106,236.
In U.S. Pat. No. 900,407 the glazed sash is normally supported on a flexible strap and means is provided for holding the strap in predetermined location. Detaching the strap and lowering the window achieves the essential purpose. No particular weather sealing construction or positive support for the glazed window sash is suggested by the patent.
The U.S. Pat. No. 4,106,236 patent discloses a fire door for a trailer with a quick operating latch which serves to hold a door in fixed position in an opening in a wall. Rotational movement of the latch frees the upper portion of the door which may then be moved outwardly of the opening to provide a suitable exit.
The present invention features a compact relatively small support structure which can be built into a hollow wall of a trailer or mobile home beneath and in communication with a window opening therein and arranged to support a glazed sash in normal closed relation in the window opening. A handle on the inside of the trailer or mobile home provides means for moving the support structure sufficiently to permit the glazed sash to drop downwardly by gravity into the cavity in the wall of the trailer or mobile home to form a safety exit.
The glazed sash itself is frictionally engaged in a conforming channel configuration in the window opening so that it can be moved upwardly to closed position and the support means repositioned thereinunder.
SUMMARY OF THE INVENTION
A quick opening window for trailers and mobile homes comprises a glazed sash movably disposed in a frame defining a window opening in a wall of the trailer or mobile home with a cavity in the wall beneath the window opening of a size and shape sufficient to receive the glazed sash when lowered thereinto. A movable support platform in the lowermost portion of the window opening and beneath the normal frame thereof normally supports the glazed sash in weather-tight relation and means is provided on the interior of the trailer or mobile home for moving the support means relative to its supporting position to permit the glazed shape to drop downwardly into the cavity below the window opening so as to form a safety exit.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a portion of an exterior wall of a mobile home showing the quick opening window installed therein;
FIG. 2 is a cross sectional elevation of the quick opening window and on an enlarged scale;
FIG. 3 is a cross sectional detail on line 3--3 of FIG. 2 with parts broken away and parts in cross section; and
FIG. 4 is a horizontal section in enlarged detail on line 4--4 of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In the form of the invention chosen for illustration and description herein, the quick opening window for trailers and mobile homes may be seen in side elevation in FIG. 1 of the drawings, wherein a side 10 of a trailer or mobile home is illustrated and a window opening therein is defined by a rectangular frame 11. A sash 12 having transparent glazing material such as glass or optical grade plastic 13 is secured in the sash 12 as will be understood by those skilled in the art and broken lines in FIG. 1 indicate a lower alternate or open position of the sash 12 in a cavity beneath the window opening defined by the frame 11.
By referring now to FIG. 2 of the drawings, it will be seen that the glazed sash 12 is positioned between the outer wall 10 of the trailer or mobile home and an inner wall 14 by the frame 11 which is preferably flanged at its inner ends at 15 which position a pair of oppositely disposed resilient gaskets 16 which directly engage the sides of the sash 12.
Still referring to FIG. 2 of the drawings, it will be seen that the sash 12 is directly supported on a resilient strip 17 which is positioned longitudinally of the upper surface of a support bar 18 which extends longitudinally below the sash 12 and has its end portions slidably engaged on the horizontal portions of angle members 19 which are in turn secured to frame members 20 which extend between the inner and outer walls 10 and 14 of the trailer or mobile home as the case may be. The support bar 18 has a pair of sidewardly extending rods 21 on its opposite ends which rods engage a secondary support bar 22 which is positioned in spaced parallel relation to the support bar 18.
The angle members 19 are preferably attached to the frame members 20 by means of fasteners 23.
Plates 24 are positioned partially beneath the lower surfaces of the horizontal sections of the angle members 19 and held in spaced relation to the support bars 18 and 22 by fasteners 25.
By referring now to FIG. 4 in particular, it will be observed that the space between the support bar 18 and the secondary support bar 22 is more than sufficient to permit the glazed sash 12 to move downwardly therebetween at such time as the support bar 18 and the secondary support bar 22 are moved as indicated by the arrows in FIG. 4 of the drawings. In order that such movement may be imparted to the support bar 18 and the secondary support bar 22 so as to move the support bar 18 out from under the glazed sash 12, an angular bracket 26 is attached to the support bar 18 by means of brackets 27 and fasteners 28 respectively. A handle 29 is positioned on the opposite side of the inner walls 14 of the trailer or mobile home construction as heretofore described and is connected by a connecting bar 30 with the angular bracket 26. Movement of the handle 29 will not immediately move the support bar 28 relative to its supporting position beneath the glazed sash 12 until the tension of a friction catch is overcome. The friction catch may best be seen in FIGS. 2 and 3 of the drawings, and by referring thereto it will be seen that a catch device comprises a horizontally disposed body member 31 having a vertical end portion 32 with an outwardly and downwardly inclined angular extension 33. A pair of bolts 34 loosely attach the member 31 to a support base 35 and it in turn is attached to a cross frame member 36 in the wall of the trailer or mobile home. The bolts 34 are both loosely positioned and held in tensioned relation as shown by coil springs 37, the arrangement being such that movement imparted the handle 29 so as to move the support bar 18 from its supporting position relative to the glazed sash 12 must tilt the latch members 31 and 32 and the angular end portion 33 in both instances compressing the coil springs 37 about the loosely positioned bolts 34.
The vertical portion 32 of the latch means will directly engage the end of one of the plates 24 as seen in FIGS. 2 and 3 of the drawings, and motion imparted the handle 29 must therefore overcome the resistance of the springs 37 and permit the latch members 31 32, and 33 to move to permit the plates 24 to slide along with the support bar 18 toward the inner wall 14 of the wall of the trailer or mobile home in which the safety window is installed.
The arrangement is such that when the safety window is to be replaced in closed position in the opening defined by the frame 12, it may be elevated to the position shown in FIGS. 1 and 2 of the drawings and the slide bar 18 repositioned therebeneath where it will again assume a latched and relatively fixed position by reason of the latching device and the parts 32 and 33 thereof in particular.
Those skilled in the art will observe that the frame member 11 while shown in two portions in FIG. 2 of the drawings may comprise a single extruded or stamped aluminum shape or the like with a channel which engages the sides and uppermost portion of the glazed sash 12 with the web of the channel cutaway in the portion of the frame 11 as seen in FIG. 2 of the drawings where the glazed sash 12 will move downwardly when the support bar 18 is withdrawn from its normal support position as hereinbefore explained.
Adjustable stop means to control the travel of the support bar 18 and the secondary support bar 22 are preferably included in the device and are illustrated in FIGS. 2 and 4 of the drawings and indicated by the numerals 38 and a similar adjustment is provided by the movable engagement of the connecting bar 30 with the angular bracket 26 as hereinbefore described.
It will thus be seen that a quick opening window for trailers and mobile homes has been disclosed which may be relatively easily and inexpensively formed and assembled as a unit in a wall cavity immediately beneath a window opening in the wall so as to normally position a glazed sash therein in sealing relation to the wall and yet be movable quickly and easily to permit the glazed sash to drop completely out of the window opening and into a cavity of the wall therebeneath so as to provide a readily accessible usable safety exit from the trailer or mobile home, the construction being such that the glazed sash may be easily repositioned in sealing relation to the window opening and the support means repositioned where it is held against accidental disengagement as necessary in a trailer or mobile home.
|
A quick opening window positions a glazed sash in a window opening in weather sealing relation and supports said glazed sash in closed relation to the opening on a sidewardly slidable support which is moved from its normal position beneath the glazed sash to permit the sash to drop into a hollow cavity beneath the window opening. A tension latch arrangement is provided which must be overcome in moving the glazed sash support from its normal position to prevent the accidental opening of the window.
| 4
|
FIELD OF THE INVENTION
[0001] The present invention relates to a frequency jittering control circuit and a method for using the same, in particular to a frequency jittering control circuit and a method which do not require a digital counter. The omission of the digital counter greatly reduces the complexity of the circuit.
BACKGROUND OF THE INVENTION
[0002] To avoid electromagnetic interference (EMI) generated by high frequency signals, frequency jittering is a method that is often used in high frequency electronic products. Conventionally, frequency jittering is achieved by means of a digital counter; following the counts generated by the digital counter, the frequency shifts within a narrow range. The digital counter may be designed to provide sequential or random counts, and the frequency correspondingly shifts sequentially or randomly. A typical frequency jittering control circuit employing a digital counter may be found in U.S. Pat. No. 6,229,366.
[0003] The drawbacks to use a digital counter are as follows: first, a digital counter is a huge circuit device; it is made of T flip-flops, and T flip-flops heavily consume circuit area. Moreover, in such frequency jittering control circuits, a designer has to design current source devices of different current amounts, and the corresponding control mechanism of the different current source devices by the output of the digital counter. Thus, the conventional circuit employing a digital counter is disadvantageous in that it is costly and complicated.
SUMMARY OF THE INVENTION
[0004] In view of the foregoing, it is an objective of the present invention to provide a frequency jittering control circuit and a method thereof, which do not require a digital counter. The present invention takes advantage of the characteristics of a phase lock loop (PLL) in a very inventive way; by switching the input frequency of the PLL, the output frequency of the PLL swings between two frequency limits to provide the desired frequency jittering function. Moreover, the resulted frequency after frequency jittering is more random and smoother, providing a better anti-EMI effect than that resulting from conventional random counts by a digital counter.
[0005] In accordance with the foregoing and other objectives of the present invention, and as disclosed by one embodiment of the present invention, a frequency jittering control circuit is disclosed, which comprises: at least two oscillators generating different reference frequencies; and a PLL having an input switching between the at least two oscillators.
[0006] As disclosed by another embodiment of the present invention, a frequency jittering control circuit is disclosed, which comprises: a multi-frequency oscillator generating at least two different reference frequencies; and a PLL having an input switching between the at least two reference frequencies.
[0007] According to another aspect of the present invention, a frequency jittering control method is disclosed, which comprises: generating at least two different frequencies, and providing a PLL having an input switching between the at least two reference frequencies so that its output swings between the at least two reference frequencies.
[0008] It is to be understood that both the foregoing general description and the following detailed description are provided as examples, for illustration rather than limiting the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] These and other features, aspects, and advantages of the present invention will become better understood with regard to the following description, appended claims, and accompanying drawings where:
[0010] FIG. 1 is a schematic diagram showing a first embodiment of the present invention;
[0011] FIG. 2 is a circuit diagram showing a typical structure of an oscillator;
[0012] FIG. 3 is a schematic diagram showing a second embodiment of the present invention; and
[0013] FIGS. 4A-4C show three embodiments of the multi-frequency oscillator according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0014] The present invention takes advantage of the characteristics of a PLL in an inventive way. FIG. 1 is a schematic circuit diagram illustrating a first embodiment of the present invention. As shown in the figure, according to the present embodiment, a frequency jittering control circuit 20 includes two oscillators 22 and 24 , which generate two different reference frequencies respectively. A multiplexer 26 receives the outputs from the two oscillators 22 and 24 , and selects one of them. The output of the multiplexer 26 is electrically connected with the input of the PLL 28 , and thus the PLL 28 will gradually adjust its output frequency to be consistent with the output frequency of the multiplexer 26 .
[0015] The circuit shown in FIG. 1 operates as follows. At first, a user may set the reference frequencies of the two oscillators 22 and 24 as the upper and lower limits of the range for frequency jittering. The PLL 28 may start from any frequency, and the multiplexer 26 may start by selecting anyone of its inputs. When or after the PLL 28 synchronizes its output frequency to the output frequency of the multiplexer 26 , a signal S 0 is generated to switch the multiplexer 26 to the other frequency input. Due to the phase lock function of the PLL 28 , the output frequency of the PLL 28 will gradually increase or decrease, until it again synchronizes its output frequency to the output frequency of the multiplexer 26 . At or after this time point, the PLL 28 again sends a signal S 0 to switch the multiplexer 26 to the other frequency input. As such, the output frequency of the PLL 28 will swing between the upper and lower limits of the range, achieving the frequency jittering function.
[0016] In comparison with the conventional frequency jittering method by means of a digital counter, the frequency spectrum of the present invention is smoother. The time point when the signal S 0 is generated could be any point in the waveform of the other frequency, and thus the swing is more random, providing a better anti-EMI effect.
[0017] The above embodiment employs two oscillators with two different reference frequencies. Under the same spirit, it can be readily conceived to use more than two oscillators for the multiplexer 26 to switch among the different inputs. Here it should be emphasized that it is also possible to use only one oscillator, to generate two or more reference frequencies.
[0018] FIG. 2 shows a typical structure of an oscillator. It works as follows. The signal S 2 or S 1 decides whether the circuit charges the capacitor C by the charging current source IC, or discharges the capacitor C by the discharging current source ID. The voltage across the capacitor C is compared with a high-level input VH of a high-level comparator 31 to generate the signal S 1 , and compared with a low-level input VL of a low-level comparator 32 to generate the signal S 2 . The charging and discharging of the capacitor C generate oscillation signals.
[0019] Referring to FIG. 3 and FIGS. 4A-4C , a multi-frequency oscillator 32 can be made by slightly modifying the circuit shown in FIG. 2 . As a first example ( FIG. 4A ), the multi-frequency oscillator 32 is provided with two charging current sources IC 1 and IC 2 of different current amounts, and the signal S 0 sent by the PLL 28 controls a multiplexer 42 to switch between the two charging current sources IC 1 and IC 2 . By this arrangement, the output of the PLL 28 also achieves the desired frequency jittering function. By the same token, similar effect can be achieved by providing two discharging current sources.
[0020] As another example, referring to FIG. 4B , the multi-frequency oscillator 32 is provided with two capacitors C 1 and C 2 of different capacitances, and the signal S 0 sent by the PLL 28 controls a multiplexer 42 to switch between the two capacitors C 1 and C 2 . As yet another example, referring to FIG. 4C , the multi-frequency oscillator 32 is provided with two high-level reference voltage inputs VH 1 and VH 2 , and the signal S 0 sent by the PLL 28 controls a multiplexer 42 to switch between the two inputs VH 1 and VH 2 . (By the same token, the multi-frequency oscillator 32 can be provided with two low-level reference voltage inputs.) All the above arrangements can construct a multi-frequency oscillator 32 that is able to cause the PLL 28 to swing between an upper and a lower limits of a preset range, achieving the desired frequency jittering function more smoothly and more randomly than prior art.
[0021] Although the present invention has been described in considerable detail with reference to certain preferred embodiments thereof, they are for illustrative purpose rather than for limiting the scope of the present invention. Other variations and modifications are possible. For example, one may insert circuit devices which do not affect the primary function of the circuit between two of the illustrated devices. In view of the foregoing, it is intended that the present invention cover all such modifications and variations, which should be interpreted to fall within the scope of the following claims and their equivalents.
|
A frequency jittering control circuit wherein by means of the characteristics of a PLL whose input switches between different frequencies, the output frequency of the PLL swings between the different frequencies to achieve the desired frequency jittering.
| 7
|
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to security devices and, more particularly, to a plug for blocking transmission through a door viewer from a light source.
[0003] 2. Description of Related Art
[0004] For security purposes, and, more particularly, to determine the identity of a person seeking to enter a building, door viewers of various types have been developed. These door viewers generally include a lens system for providing to a person on the inside a wide angle view to the outside. Thereby, the person on the inside has an opportunity to view and identify a person(s) seeking entry prior to permitting entry by opening the door. Generally, the commercially available door viewers for this purpose are adequate in providing the results sought.
[0005] The lens system in commercially available viewers does not permit a person outside to view with any clarity a person or features of the room inside the door. However, the door viewer does transmit light from the inside to the outside. If there is no light source optically aligned with the door viewer, ambient light is transmitted through the door viewer from the inside to the outside. In such event, the intensity of the light transmitted is essentially unaffected by a person on the inside looking through the viewer from a short distance removed therefrom. However, if a light source is optically aligned with the door viewer, any blockage of light from such light source to the door viewer will reduce the intensity of the light transmitted through the door viewer. Thus, a person on the outside can readily determine, by the change in light intensity emanating from the door viewer, that a person is present inside in proximity to the door viewer. While it is impossible for the inside person to be recognized due to the optics of the door viewer, the person on the outside will know that a person is inside the building. This information can be used by a thief or burglar as part of the decision making process of whether to burglarize or break into the building. There have also been reported instances of a thief or burglar injuring the person on the inside by driving an icepick or the like through the door viewer when the person on the inside was looking through it, as would be evident by the change in light intensity emanating from the door viewer.
[0006] There are available lenses which can be used in conjunction with a conventional commercial door viewer that permit a person from the outside to view with clarity the surroundings on the inside of the door. Thus, the privacy intended by a commercially available viewer is compromised. Such compromise and effect thereof is of particular concern in commercial establishments, such as motels and hotels which have door viewers and wherein the occupants are generally viewable as their activities are normally conducted within the room into which the door opens. Moreover, for a person with criminal intentions the opportunity to view and assess the nature of the occupants prior to committing a criminal act may be of significant benefit and to the detriment of the occupants.
[0007] Conventional commercially available door viewers permit transmission of light from the exterior to the interior space of a room into which the door opens. This light transmission will vary from intermittent, partial or complete blockage of light entering the door viewer as persons walk by on the outside. The resulting flickering seen on the inside of a door viewer may be particularly disturbing to a motel or a hotel guest who has turned out the lights and is trying to sleep.
SUMMARY OF THE INVENTION
[0008] The present invention is directed to a portable or permanently installed blockage for precluding light transmission through a door viewer from the inside to the outside. Furthermore, during daylight conditions, removal of the blockage for purposes for of using the viewer will not provide an indication of whether a viewer on the inside is looking through the door viewer.
[0009] It is therefore a primary object of the present invention to provide a portable blockage for precluding light transmission through a door viewer.
[0010] Another object of the present invention is to provide a demountable blockage for a door viewer which is attached to the door viewer.
[0011] Still another object of the present invention is to provide a selectively usable blockage attached to a door viewer for selectively blocking light transmission through the door viewer.
[0012] Yet another object of the present invention is to provide an inexpensive portable or permanently mounted plug for use with a door viewer.
[0013] A further object of the present invention is to provide a selectively removable plug for use with a conventional door viewer.
[0014] A still further object of the present invention is to provide a plug removable from the inside of a door viewer which does not signal use of the door viewer to a person on the outside.
[0015] A yet further object of the present invention is to provide a method for selectively controlling light transmission through a door viewer.
[0016] These and other objects of the present invention will become apparent to those skilled in the art as the description thereof proceeds.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The present invention will be described with greater specificity and clarity with reference to the following drawings, in which:
[0018] [0018]FIG. 1 illustrates the present invention attached to a conventional door viewer mounted in a door;
[0019] [0019]FIG. 2 is a partial cross-sectional view of the present invention mounted in a door viewer; and
[0020] [0020]FIG. 3 illustrates use of the present invention while precluding an indication to a person on the outside that the door viewer is being used by a person on the inside.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0021] Referring jointly to FIGS. 1 and 2, there is shown a conventional door viewer 10 mounted within a door 12 . Usually, the door is the front door of a dwelling or the door to a hotel or motel room. The door viewer has essentially three components. The first component is a cylinder 14 having an annular flange 16 for abutting engagement with outside surface 18 of door 12 . The interior of cylinder 14 includes a lens system 20 , representatively depicted by lenses 21 and 22 . The lens system provides a wide angle view of the area outside of door 12 and essentially distorts the view through the door viewer from the outside into the space behind the door. A sleeve 30 including an annular flange 32 is essentially hollow. The interior of sleeve 30 includes threads 34 for threaded engagement with threads 36 on the exterior of cylinder 14 . With such threaded engagement between the cylinder and the sleeve, a range of widths of door 12 can be accommodated.
[0022] A plug 40 , which may be in the shape of a truncated cone, as illustrated, is demountably mounted within hollow end 42 of door viewer 10 . Following such mounting, transmission of light through the door viewer from a location outside of door 12 is precluded. As particularly shown in FIGS. 1 and 3, plug 40 is readily mounted in or demounted from engagement with the door viewer.
[0023] To insure accessibility of plug 40 and to minimize the likelihood of loss or misplacement, the plug may be attached to the door viewer through a lanyard 44 or the like. As shown, the lanyard may be a chain 46 of metallic material or of manmade material. The lanyard may be attached to a cap 48 , which cap receives and retains one end of plug 40 .
[0024] The other end of lanyard 44 may be attached to door viewer 10 by use of attachment means, such as a cord or a wire 50 , secured to and extending from the lanyard. As discussed above, sleeve 30 is in threaded engagement with cylinder 14 . To assist in threading and unthreading the sleeve, a pair of diametrically opposed slots 52 , 54 may be formed in annular flange 32 . These slots can be engaged by a coin or the like to provide a grip for rotating the sleeve. Upon rotation of the sleeve in one direction, such as counterclockwise, the sleeve will be urged to translate away from the door and provide a space between annular flange 32 and interior surface 38 of the door. By wrapping a section of the attachment means, such as wire 50 , about the sleeve adjacent annular flange 32 , and thereafter rotating the sleeve in a clockwise direction, wire 50 will become captured between annular flange 32 and surface 38 of the door. Thereby, plug 40 and its attached lanyard 44 will remain in proximity with door viewer 10 when the plug is not engaged with the door viewer and loss or misplacement is essentially eliminated. Because of this simple mode of attaching plug 40 , it can be temporarily attached at temporary abodes of the user, such as hotel room and motel room doors. To disengage plug 40 and its attached lanyard 44 , the above described process can be reversed to release wire 50 from between annular flange 32 and surface 38 of door 12 .
[0025] One of the optical characteristics of a conventional door viewer of the type illustrated in FIGS. 1 and 2 is that blockage of a source of light transmitting light directly through the door viewer can be detected by a person outside of the door. However, when ambient light interior of the door is the only light transmitted through the door viewer, no or little change in intensity of the light transmitted is detectable if a person were to place one's head in position to look through the door viewer from the inside to the outside.
[0026] As shown in FIG. 3, it is assumed that a source 60 of light would transmit light directly through door viewer mounted within door 12 . In such event, if a person 62 were to look through the door viewer, the transmission of light from source 60 would be blocked. The resulting change in intensity of light detectable by a person 64 outside of door 12 would provide an indication of the presence of person 62 .
[0027] The present invention is particularly suited to avoid such indication of the presence of a person 62 . When a person 62 decides to look through door viewer 10 , the person would block direct light transmission from source 60 through the door viewer and only ambient light would be available for transmission through the door viewer. When in such position, person 62 would remove plug 40 from the door viewer. The resulting light transmitted through the door viewer would not change as a function of movement of person 62 unless such person's movements would result in transmission of light directly from source 60 . That is, only ambient light would be transmitted through the door viewer and the intensity of such ambient light would remain essentially constant despite some movement of person 62 . Thus, a person 64 on the outside of door 12 would not be aware of whether person 62 was or was not looking through the door viewer and hence the presence of person 62 would be unknown.
[0028] While the invention has been described with reference to several particular embodiments thereof, those skilled in the art will be able to make the various modifications to the described embodiments of the invention without departing from the true spirit and scope of the invention. It is intended that all combinations of elements and steps which perform substantially the same function in substantially the same way to achieve the same result are within the scope of the invention.
|
A readily available conventional commercial door viewer includes a lens at one end for providing a wide angle view and a hollow end through which a person would look. A truncated cone shaped plug fits within the hollow end to block light transmission through the door viewer. The plug is readily manually removable to use the door viewer and includes a removable lanyard to tether the plug in proximity to the door viewer.
| 4
|
BACKGROUND OF THE INVENTION
The present application relates generally to disconnectable threaded joints for interconnecting two components. More particularly, one form of the present application relates to a threaded joint for coupling together gas turbine engine casings. Although the present application was developed for application in gas turbine engines, certain applications may exist in other fields.
Gas turbine engines usually include a number of cylindrical components joined together to define a housing. Within the housing, there is generally a flow of working fluid. Gas turbine engine designers have strived to secure the components of the housing in a way that maintains structural and pressure integrity while at the same time facilitating assembly and disassembly for inspection and/or repair of components.
A conventional system for connecting cylindrical gas turbine engine housing components has been to incorporate circumferential and abutting flanges which are secured to one another by clamps or fasteners extending through aligned openings in the abutting flanges. One limitation of this approach has been that the prior system complexity adds to the cost and potential unreliability of the joint. Further, the flanged, bolted joint and/or clamped joint may lead to an increase in the overall envelope for the engine.
Accordingly, there is a continuing need for an effective disconnectable joint for gas turbine engine components.
SUMMARY OF THE INVENTION
One form of the present invention contemplates an apparatus comprising: a first gas turbine engine component having a first annular portion with an internal thread and a first annular abutment surface spaced from the internal thread; and a second gas turbine engine component having a second annular portion with an external thread and a second annular abutment surface spaced from the external thread and abutting the first annular abutment surface, the first and second components at least partially overlapping one another and the threads interengage to couple the components together and place the abutting abutment surfaces in a first sealing relationship, wherein one of the components is in tension and the other of said components is in compression between the abutting abutment surfaces and the interengaging threads.
Another form of the present invention contemplates a method of assembling a threaded joint between two gas turbine components. The method comprising: orienting a cylindrical portion of the two components in an overlapping relationship, one of the components in the overlapping relationship defining an inner overlapping section having an externally threaded portion and the other component defining an outer overlapping section having an internally threaded portion; creating a differential thermal loading between the inner overlapping section and the outer overlapping section, the outer overlapping section having a greater thermal loading; threading the components together to bring an abutment surface on each of the components into an abutting relationship and establish a seal therebetween that is spaced from the threaded portions; and allowing the components to achieve equal thermal loading thereby increasing the axial preload.
Yet another form of the present invention contemplates an apparatus comprising: a first component having a first cylindrical portion with an internal thread and a first annular abutment surface spaced from the internal thread, the first component including a pair of first pilot surfaces spaced apart from the internal thread; and, a second component having a second annular portion with an external thread and a second annular abutment surface spaced from the external thread and abutting the first annular abutment surface, the first and second components at least partially overlapping one another and the threads interengage to couple the components together and place the abutting abutment surfaces in a first sealing relationship, wherein one of the components is in tension and the other of the components is in compression between the abutting abutment surfaces and the interengaging threads, and further wherein the second component including a pair of second pilot surfaces spaced apart from the external thread and in registry with the pair of first pilot surfaces to form a second sealing relationship.
One object of the present invention is to provide a unique threaded joint for gas turbine components.
Related objects and advantages of the present invention will be apparent from the following description.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows an external side view of a gas turbine engine employing a prior art technique for joining annular components.
FIG. 2 is a fragmentary view of a gas turbine engine, comprising one embodiment of a threaded joint of the present invention.
FIG. 3 is a fragmentary cross-section view of the threaded joint of FIG. 2 .
FIG. 4 is a fragmentary, cross section view of an alternative embodiment of the present invention showing the component joint at the beginning of assembly.
FIG. 5 is a fragmentary cross-section view of the joint of FIG. 4 shown in its assembled position.
FIG. 6 is a fragmentary cross-section view showing a locking mechanism for the threaded joint of FIG. 3 .
FIG. 7 is an illustrative end view taken at arrow A in FIG. 6 .
FIG. 8 is a cross-section view taken on line B-B of FIG. 6 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
For the purposes of promoting an understanding of the principles of the invention, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the invention is thereby intended, such alterations and further modifications in the illustrated device, and such further applications of the principles of the invention as illustrated therein being contemplated as would normally occur to one skilled in the art to which the invention relates.
With reference to FIG. 1 , there is illustrated a gas turbine engine 10 utilizing one embodiment of a threaded joint 36 of the present invention. The gas turbine engine 10 illustrated is purely illustrative and no limitation is intended herein to any specific type of gas turbine engine. The illustrative gas turbine engine comprises an accessory drive/inlet housing 12 , compressor housing 14 , diffuser/combustor housing 16 , turbine housing 18 and exhaust housing 20 . The general operation of gas turbine engines is well known to those of ordinary skill in the art and thus it is unnecessary to describe the operation of compression, combustion and expansion to extract work out of the gas turbine engine by a power turbine providing a rotary output or pure reaction to produce thrust. Gas turbine engines operate with internal pressures at the hundreds of PSI level. In at least one form, discharge pressures can approach 600 PSI on high pressure ratio applications having overall pressure ratios of about 40:1. The capability to withstand high pressures require joints between the various housings to be structurally sound, capable of a pressure seal, and removable for maintenance. The present application is applicable to a wide variety of pressures and is not limited, unless expressed to the contrary, to any particular pressure ranges.
With reference to FIG. 2 , there is illustrated an enlarged fragmentary view of a portion of the gas turbine engine showing the joint 36 coupling the diffuser/combustor housing 16 to the turbine housing 18 . While the joint of the present invention is illustrated between the diffuser/combustor housing 16 and the turbine housing 18 , it is applicable to all joints in the gas turbine engine. Further, the present invention is contemplated for other fields, including but not limited to, rocket motors, steam turbines, liquid carrying tubes/pipes, and gaseous fluid carrying tubes/pipes.
With reference to FIG. 3 , there is illustrated an enlarged fragmentary cross-sectional view of the joint 36 . Housing 18 has an annular portion 38 with an externally threaded portion 40 formed thereon. Housing 16 has an annular portion 42 with an internally threaded portion 44 formed thereon. The portions 42 and 38 overlap, and the threads 40 and 44 interengage when in an assembled state. An end face 48 on annular portion 38 abuts a corresponding shoulder 46 on annular portion 42 . In one embodiment, the interface between shoulder 46 and end face 48 is axially spaced from the interengaging threads 40 and 44 so that when the threads are tightened there is sufficient axial force to drive the end face 48 and shoulder 46 into an abutting relationship and form a seal. The term “seal” or “sealing” as utilized herein describes the reduction of fluid flow between the components coupled together at the joint. The reduction in fluid flow at the joint may be a complete prevention of fluid leakage between the components or a partial prevention of fluid leakage that minimizes fluid leakage between the components at the joint. The interengaging of the threaded joint places at least a portion of the outer annular portion 42 in tension and the inner annular portion 38 in compression.
Radial pilots 100 and 101 are formed on either side of the interengaging threaded joint. The radial pilot 100 comprises an inwardly facing pilot surface 50 formed on annular portion 42 and a corresponding outer facing pilot surface 52 formed on annular portion 38 . Radial pilot 101 comprises an outer facing pilot surface 54 formed on annular portion 38 and an inner facing pilot surface 56 formed on annular portion 42 . In one form the respective surfaces of the pilot surfaces are substantially parallel.
The parameters of the pilot joints, length to the axial abutting surfaces, and thread size are all selected to facilitate assembly/disassembly during a condition where the housings 16 and 18 are subjected to differential thermal conditions. In one non-limiting example the present invention contemplates a ten inch diameter threaded joint where the length from the thread element to the mutually abutting axial surfaces 48 and 46 is about 1½ inches. The thickness of annular portion 42 which is in tension and of annular portion 38 which is in compression is about 0.1 inches. In obtaining about a 0.002 inch deformation in each annular portion, a preload of about 125,000 pounds is generated. A 40,000 PSI bearing stress is generated at the abutting surfaces 48 and 46 . A buttress thread is utilized at the threaded joint. This 125,000 pound load is sufficient to provide a fluid tight coupling with adequate bending stiffness. However, other joint sizes, threads, amount of deformation and preloads are contemplated herein.
In the assembly/disassembly phase, the housing 16 is subjected to a higher localized thermal loading than housing 18 . This can be done by heating the exterior of housing 16 in the proximity of the annular portion 42 or by cooling the annular portion 38 of housing 18 . Preferably, the heating of the housing occurs between the radial pilots 100 and 101 . In this condition, the length from the threaded joint to the mutually abutting axial surfaces 48 and 46 is greater for annular portion 42 than it is for annular portion 38 ; the pilot surfaces 50 and 56 are greater in diameter than the interconnecting surfaces 52 and 54 , and; threads 44 have clearance relative to threads 40 . The heating provides clearance between the components forming the radial pilot 100 and 101 .
The two components are threaded together in the state of differential thermal loading until the surfaces 48 and 46 abut one another. The threads are tightened to create a predetermined loading on these axial end faces. In one form of the invention, the preload is 125000 pounds. As the annular portions 38 and 42 reach equal thermal loading, annular portion 42 reduces in length and diameter relative to annular portion 38 . The result of the cooling of the assembly is to create an axial preload between shoulder 46 and end face 48 and a radial preload between the surfaces 54 and 56 of radial pilot 101 and surfaces 50 and 52 of pilot 100 . The practical effect is to tighten the joint and enhance the seals at the joint between the following pairs of surfaces: 50 and 52 , 46 and 48 , 54 and 56 . To disassemble the joint, the differential thermal loading described above is employed and the annular portions 38 and 42 are unthreaded.
During operation of the gas turbine engine, the working fluid flow path is at least partially adjacent the annular portion 38 so that it is subjected to a higher thermal loading than annular portion 42 . As a consequence, there is thermal growth in annular portion 38 relative to annular portion 42 , thus increasing both the axial and pilot seals. It should be noted that the axial spacing of the pilot joints 50 , 52 and 54 - 56 from the threads 40 , 44 provide increased bending stiffness through the joint. In another embodiment, a secondary seal including, but not limited to, an E-seal, W-seal or C-seal can be employed in the void formed between the aft face 58 of housing 16 and the shoulder on housing 18 .
The joint 46 shown in FIGS. 4 and 5 is substantially similar to the joint 36 , but includes an enhanced self-piloting element. The utilization of like feature numbers is done to represent like features. Annular portion 60 extends from gas turbine housing 18 and has an axial end face 62 . Annular portion 64 is integral with housing 16 and overlaps annular portion 60 . An externally threaded section 66 on annular portion 60 interengages with an internally threaded section 68 on annular portion 64 as the components are threaded together. Lead-in pilot surface 72 on annular portion 60 cooperates with a corresponding pilot 74 on annular portion 64 leading from shoulder 113 . This lead-in pilot surface 72 aids in threading the joint into place in the position shown in FIG. 5 . As the components are assembled, the radial pilot 110 is formed by the engagement of surface 111 of portion 60 with surface 112 of portion 64 . The lead-in pilot surface 72 on portion 60 does not normally contact the surfaces 74 and/or 112 . However, the lead-in pilot surface 74 is located in close proximity to the component 64 in order to provide an alignment guide for the structure. Surface 72 can be set to engage surface 112 and/or 74 prior to threads 66 and 68 engaging to prevent cross-threading at assembly. Surface 62 disposed at the end of portion 60 is brought into an abutting relationship with surface 113 when the components are assembled. The seal is formed between surfaces 62 and 113 , surfaces 111 and 112 , and between surfaces 70 and 114 . It should be noted that the same techniques for differentially thermally loading the joints can be employed for the joint illustrated in FIGS. 4 and 5 .
FIGS. 6 , 7 and 8 illustrate an anti-rotation locking mechanism generally indicated at 200 which is illustrated here applied to the joint of FIGS. 2 and 3 . It should be noted, however, that the anti-rotation mechanism may be employed with equal benefit to the other joints including, but not limited to, those set forth in FIGS. 4 and 5 . The anti-rotation device comprises a ring 76 extending over both of annular end portions 42 and 38 . As shown in FIG. 8 , end portion 38 has a plurality of slots 78 (only one of which is shown) spaced around the circumference of annular section 38 . A corresponding number of projections 80 extend from ring 76 into slots formed in portion 38 . Ring 76 includes an annular section 82 which overlaps annular portion 42 , including at least a portion of the slots 84 spaced around the circumference of the portion 42 . When the elements are in their secure position and the projections 80 are lined up in grooves 78 , the thin annular section 82 is deformed at 86 to extend into grooves 84 . Thus, the elements are locked against rotation. Disassembly may take place after sections 86 are bent to clear grooves 84 and permit unthreading of the elements. The present application contemplates other anti-rotation locking mechanisms, such as, but not limited to, local welding for expendable applications, locking pins and lockwire.
While the invention has been illustrated and described in detail in the drawings and foregoing description, the same is to be considered as illustrative and not restrictive in character, it being understood that only the preferred embodiment has been shown and described and that all changes and modifications that come within the spirit of the invention are desired to be protected. It should be understood that while the use of the word preferable, preferably or preferred in the description above indicates that the feature so described may be more desirable, it nonetheless may not be necessary and embodiments lacking the same may be contemplated as within the scope of the invention, that scope being defined by the claims that follow. In reading the claims it is intended that when words such as “a,” “an,” “at least one,” “at least a portion” are used there is no intention to limit the claim to only one item unless specifically stated to the contrary in the claim. Further, when the language “at least a portion” and/or “a portion” is used the item may include a portion and/or the entire item unless specifically stated to the contrary.
|
An assembly including inner and outer overlapping annular elements with interengaging threads. An axial abutment between the two elements is spaced from the threaded section to permit a structural and fluid seal at the joint. Pilot joints are provided to stabilize the joint and provide additional sealing.
| 5
|
BACKGROUND OF THE INVENTION
FIELD OF THE INVENTION
This invention concerns mycophenolic acid derivatives as agents in the treatment of rheumatoid arthritis.
PREVIOUS DISCLOSURES
Rheumatoid arthritis has been treated with a variety of compounds representing many structural classes, including, for example, corticosteroids, aspirin and related compounds, derivatives of arylacetic and arylpropionic acids, relatives of phenylbutazone, gold salts and penicillamine and its derivatives. However, no representative of any of these classes of compounds is regarded as ideal.
Mycophenolic acid is a weakly-active antibiotic found in the fermentation broth of Penicillium brevi-compactum. It has now been discovered that certain mycophenolic acid derivatives and related compounds are useful as agents in the treatment of rheumatoid arthritis.
Compounds somewhat structurally similar to the novel compounds of the present invention (compounds illustrated by Formula II as defined herein) are described in U.S. Pat. Nos. 3,705,894; 3,853,919; 3,868,454; 3,880,995, in Japanese Pat. No. J 57024380, in the J. Antibiot., 29(3), 275-85, 286-91 (1976), and in Cancer Research, 36(8), 2923-7 (1976). The disclosed compounds are described as having anti-tumour, immunosuppressive, anti-viral, anti-arthritic and anti-psoriatic activities.
The present invention includes the discovery that the family of compounds illustrated by Formula I and as defined herein are active in biological models of chronic inflammatory diseases, including models of rheumatoid arthritis in mammals. While many of these compounds are disclosed elsewhere, their usefulness in treating rheumatoid arthritis was not previously known. Compounds similar to or included in Formula I are described in U.S. Pat. Nos. 3,705,894, 3,777,020, and 3,868,454, Japanese Kokai Nos. 57/183776, 57/183777, and 48/86860, South African Application No. 68/4959, Great Britain Pat. No. 1261060, Belgian Pat. No. 815330, and West German Pat. No. 2237549.
SUMMARY OF THE INVENTION
In a first aspect, the invention pertains to a method of treating rheumatoid arthritis which method comprises administering to a mammal in need of such treatment a therapeutically effective amount of a compound of the formula: ##STR4## and the pharmaceutically acceptable salts thereof, wherein:
A is oxygen or sulfur;
R 1 is selected from the group consisting of H, ##STR5## in which Y is oxygen or sulfur:
R 2 is alkyl, haloalkyl or --NR 4 R 5 , where R 4 and R 5 are independently H, alkyl, haloalkyl, cycloalkyl, phenyl optionally monosubstituted with halogen, hydroxy, carboxy, chlorocarbonyl, sulfonylamino, nitro, cyano, phenyl, alkyl, acyl, alkoxycarbonyl, acylamino, dialkylamino or dialkylaminoethoxycarbonyl, phenyl optionally disubstituted with hydroxy, carboxy, nitro or alkyl, or benzyl optionally substituted with dialkylamino;
n is an integer from 0-6;
R 3 is H alkyl or a pharmaceutically acceptable cation;
Q and R are independently H or --CO 2 R 3 ; and
Z is selected from the group consisting of ##STR6## in which X is oxygen or sulfur;
R 7 is H, alkyl, alkenyl, cycloalkyl, optionally substituted phenyl, optionally substituted benzyl or a pharmaceutically acceptable cation; and
R 8 and R 9 are independently H, alkyl or cycloalkyl, or R 8 and R 9 taken together are --(CH 2 ) 4 --, --(CH 2 ) 5 -- or --(CH 2 ) 2 O(CH 2 ) 2 --;
with the proviso that R 1 and R 7 cannot both be H if X and A are oxygen.
In a second aspect, the invention pertains to novel compounds of the formula: ##STR7## and the pharmaceutically acceptable salts thereof, wherein: R 1 is selected from the group consisting of ##STR8## in which Y is oxygen or sulfur;
R 2 is H, alkyl having 1 to 6 carbon atoms or --NR 4 R 5 , where R 4 is H or alkyl having 1 to 6 carbon atoms and R 5 is H, alkyl having 1 to 6 carbon atoms or ##STR9## n is an integer from 0-6; R 3 is H, alkyl having 1 to 6 carbon atoms or a pharmaceutically acceptable cation;
Q and R are independently H or --CO 2 R 3 ; and
X is oxygen or sulfur; and
R 7 is H, alkyl having 1 to 6 carbon atoms, cycloalkyl, optionally substituted phenyl, optionally substituted benzyl or a pharmaceutically acceptable cation;
with the proviso that R 1 cannot be H or COR 2 when X is oxygen.
In two other aspects, the invention relates to a pharmaceutical composition containing a therapeutically effective amount of a compound of Formula II admixed with at least one pharmaceutically acceptable excipient, and to a method of treating rheumatoid arthritis in a mammal by administering to a mammal in need of such treatment a therapeutically effective amount of a compound of Formula II.
Finally, the invention relates to novel processes for preparing the compounds of Formula II and includes the preparation of several novel intermediates.
DETAILED DESCRIPTION OF THE INVENTION
Definitions
As used herein:
"Alkyl" means a branched or unbranched saturated hydrocarbon chain containing 1 to 6 carbon atoms, such as methyl, ethyl, propyl, isopropyl, tert-butyl, butyl, n-hexyl and the like.
"Alkoxy" means the group --OR wherein R is lower alkyl as herein defined. "Cycloalkyl" means cyclopentyl, cyclohexyl or cycloheptyl.
"Optional" or "optionally" means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where said event or circumstance occurs and instances in which it does not. For example, "optionally substituted phenyl" means that the phenyl may or may not be substituted and that the description includes both unsubstituted phenyl and phenyl wherein there is substitution; "optionally followed by converting the free base to the acid addition salt" means that said conversion may or may not be carried out in order for the process described to fall within the invention, and the invention includes those processes wherein the free base is converted to the acid addition salt and those processes in which it is not.
"Optionally substituted phenyl", unless otherwise specified, refers to a phenyl moiety optionally bearing one to three substituents independently chosen from the group consisting of halogen, hydroxy, carboxy, chlorocarbonyl, aminosulfonyl, NO 2 , CN, alkyl having one to six carbon atoms, alkoxycarbonyl, acylamino, and dialkylaminoethoxycarbonyl.
"Optionally substituted benzyl" refers to a benzyl moiety optionally bearing one to three substituent independently selected from the group consisting of halogen, hydroxy, carboxy, chlorocarbonyl, aminosulfonyl, NO 2 , CN, alkyl having one to six carbon atoms, alkoxycarbonyl, acylamino, and dialkylaminoethoxycarbonyl.
Some compounds of Formula I and II may be converted to a base addition salt by virtue of the presence of a carboxylic acid group. The term "Pharmaceutically acceptable cation" refers to the cation of such salts. The cation is chosen to retain the biological effectiveness and properties of the corresponding free acids and to not be biologically or otherwise undesirable. The cations derived from inorganic bases include sodium, potassium, lithium, ammonium, calcium, magnesium and the like. Cations derived from organic bases include those formed from primary, secondary and tertiary amines, such as isopropylamine, diethylamine, trimethylamine, pyridine, cyclohexylamine, ethylene diamine, monoethanolamine, diethanolamine, triethanolamine and the like.
The compounds of Formulas I and II are derivatives of "mycophenolic acid" which has the structure shown as Formula (III) and has a ring system numbered as shown: ##STR10##
The compounds of the invention will be named using the above shown numbering system as 6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoic acid derivatives. The symbol "E" designates the configuration of the side chain double bond. Following are examples of how representative compounds of Formulas I and II are named:
The compound of Formula II in which R 1 is --CO(CH 2 ) 2 CO 2 C 2 H 5 , X is oxygen and R 7 is hydrogen, is named
"E-6-[1,3-dihydro-4-(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid".
A compound of Formula II in which R 1 is ##STR11## is named "methyl E-6-[1,3-dihydro-4-(1,2-dicarbomethoxyeth-2-(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate".
A compound of Formula II in which R 1 is --CYNR 4 R 5 where Y is oxygen, R 4 is hydrogen, R 5 is 4-carboxyphenyl, X is sulfur and R 7 is --C 2 H 5 is named "ethyl (E)-6-{1,3-dihydro-4-[N-(4-carboxyphenyl)carbamoyloxy]-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl}-4-methyl-4-thiohexenoate".
Methods of Preparation
The novel compounds of the invention (compounds of Formula II) are prepared by the procedures detailed below and illustrated in Reaction Schemes 1, 2 and 3, and will be variously designated as compounds of Formulas IIA-IIE.
Many of the compounds of the family illustrated by Formula I are known, and their syntheses are available from the published scientific and patent literature. In particular, methods of preparing the compounds of Formula I are described in U.S. Pat. Nos. 3,705,894, 3,777,020, and 3,868,454, Japanese Kokai Nos. 57/183776, 57/183777, and 48/86860, South African Application No. 68/4959, Great Britain Pat. No. 1261060, Belgian Pat. No. 815330, and West German Pat. No. 2237549, the relevant portions of which are incorporated herein by reference. Compounds of Formula which are novel are described herein as compounds of Formula IIA and IIB.
Compounds of Formulas IIA and IIB
The compounds of Formulas IIA and IIB can be prepared as shown in Reaction Scheme 1. ##STR12##
As shown in Reaction Scheme 1, the compounds of Formulas IIA (compounds of Formula II in which R 1 is hydrogen) and IIB (compounds of Formula II in which R 1 is --CYNR 4 R 5 ) are prepared from mycophenolic acid (A). To prepare the compounds of Formula IIA, the mycophenolic acid of Formula A is first converted to an activated carbonyl derivative of Formula B in which L is a leaving group such as halo, N-carbonylimidazole, alkoxy, acyloxy or the like, chosen to be capable of displacement by a compound of Formula B1 in the presence of a base. The compounds of Formula B are prepared by standard means well known in the chemical arts. For example, the compound of Formula B where L is chloro is made by reaction with from 1.0 to 10 molar equivalents, preferably 4.0 molar equivalents, of an inorganic acid halide such as phosphorus trichloride, phosphorus pentachloride or preferably thionyl chloride, optionally in the presence of a catalytic amount of an N,N-disubstituted amide, such as N,N-dimethylformamide in an inert organic solvent such as benzene, toluene, acetonitrile, tetrahydrofuran, diethyl ether, chloroform or preferably methylene chloride. The reaction is conducted at a temperature of about 0° to 90° C., preferably about 25° C., for about 1-12 hours, preferably about three hours. Compounds of Formula B in which L is another appropriate leaving group such as those mentioned above can also be readily prepared by well known means. No one leaving group is particularly preferred over others.
The product of Formula B is then reacted with about 1-10 molar equivalents, preferably about 4.0 molar equivalents, of a compound of Formula B1 in an inert organic solvent as defined above, preferably dichloromethane. The reaction takes place in the presence of from 1-10 molar equivalents, preferably about 5 molar equivalents, of an inorganic base such as sodium carbonate, potassium bicarbonate or the like, or a tertiary organic base, such as triethylamine, N-methylpiperidine, or preferably pyridine. The reaction is conducted at 0°-25° C., preferably about 5° C., for thirty minutes to six hours, preferably about one hour. The resulting product of Formula IIA is isolated and purified by conventional means.
The compounds of Formula IIB are prepared from the compounds of Formula IIA by conversion to an activated carbonyl or thiocarbonyl derivative of Formula C, in which M is a leaving group chosen to be capable of displacement by an amine of Formula D1. For example, M may be halo, N-carbonylimidazole, trichloromethoxy, optionally substituted phenoxy, such as 2,4-dichlorophenoxy, 4-methoxyphenyl, and the like.
The conversion of the compound of Formula IIA to a compound of Formula C is performed by standard means appropriate to the chosen leaving group. For example, the compound of Formula C where M is chloro is made by reaction of the compound of Formula IIA with from 1-10 molar equivalents, preferably about 2 molar equivalents, of phosgene or thiophosgene in an inert organic solvent as defined above, preferably benzene. The reaction takes place in the presence of from 1-5 molar equivalents, preferably about 2 molar equivalents of a tertiary organic base such as triethylamine or preferably pyridine. The reaction is conducted at from 0°-50° C., preferably about 25° C., for about 1-72 hours, preferably about 18 hours, and then filtered. Evaporation of the filtrate under vacuum affords the compound of Formula C where M is chloro.
Alternatively, the compound of Formula IIA is reacted as above, substituting an appropriately substituted alkyl or aryl chloroformate or chlorothioformate for phosgene or thiophosgene, giving the compound of Formula C where M is the correspondingly substituted alkoxy or aryloxy moiety.
Similarly, the compound of Formula IIA can be reacted as above, substituting N,N'-carbonyldiimidazole or N,N'-thiocarbonyldiimidazole for phosgene or thiophosgene, giving the compound of Formula C where M is N-carbonylimidazole or N-thiocarbonylimidazole.
The products of the reactions described herein can be isolated and purified by any suitable separation or purification procedure, such as, for example, filtration, extraction, crystallization, column chromatography, thin-layer chromatography, thick-layer chromatography, preparative low or high pressure liquid chromatography, or a combination of these procedures. Specific illustrations are described in the Examples. However, other equivalent separation or purification procedures can be used.
The salt products are also isolated by conventional means. For example, the reaction mixtures can be evaporated to dryness and the salts then further purified by standard methods such as those listed above.
The compounds of Formula C are then converted to the desired compounds of Formula II by treating with the appropriate reagent, as decribed below.
Compounds of Formula IIB can be prepared by treating the appropriately substituted compound of Formula C with an appropriate amine of Formula D1, as shown, thereby converting the -OCYM group to the corresponding carbamate or thiocarbamate. To carry out this process, the compound of Formula C is dissolved in an inert organic solvent as defined above, preferably tetrahydrofuran, and reacted with from about 2-5 molar equivalents, preferably about 2-3 molar equivalents, of the appropriate amine of Formula D1 in solution in an inert solvent as defined above, preferably tetrahydrofuran. The reaction takes place at a temperature of about 0°-40° C., preferably about 25° C., for about 1-10 hours, preferably about 4 hours, at a pressure of about 1-5 atmospheres, preferably at atmospheric pressure. When the reaction is substantially complete, the product compound of Formula II is isolated by conventional means and if desired converted to a pharmaceutically acceptable salt.
Alternatively, the reaction is carried out in the presence of from 1-5 molar equivalents, preferably 2 molar equivalents, of a tertiary organic base or an inorganic base, as defined above. The compound of Formula C is reacted with from 1-4 molar equivalents, preferably about 1.2 molar equivalents, of the appropriate amine of Formula D1 in an inert organic solvent, as defined above.
Alternatively, compounds of Formula IIB are made directly from compounds of Formula C, by reaction with an appropriately substituted carbamoyl or thiocarbamoyl chloride or Formula D2. To carry out this process, the compound of Formula C is dissolved in an inert organic solvent as defined above, preferably tetrahydrofuran, and reacted with from 1-4 molar equivalents, preferably about 1.2 molar equivalents, of the appropriate carbamoyl or thiocarbamoyl chloride of Formula D2 in the presence of a tertiary organic base or inorganic base as defined above. The reaction takes place at a temperature of about 0°-40° C., preferably about 25° C., for about 1-10 hours, preferably about 4 hours. When the reaction is substantially complete, the product of Formula IIB is isolated by conventional means.
Compounds of Formula IIB where R 4 is H can also be made by reacting a compound of Formula C with an appropriately substituted isocyanate or isothiocyanate of Formula D3. To carry out this process, the compound of Formula C is dissolved in an inert organic solvent as defined above, preferably toluene, and reacted with from 1-5 molar equivalents, preferably about 2 molar equivalents, of an isocyanate or isothiocyanate of Formula D3. The reaction takes place at a temperature of about 10°-100° C., preferably about 50° C., for about 1-10 hours, preferably about 4 hours. When the reaction is substantially complete, the product of Formula IIB is isolated by conventional means.
Compounds of Formulas IIC and IID
The preparation of compounds of Formula IIC (compounds of Formula II in which R 1 is --COR 2 and R 2 is alkyl), and Formula IID (compounds of Formula II in which R 1 is --CO(CH 2 ) n CO 2 R 3 is shown in Reaction Scheme 2. ##STR13##
The compounds of Formula IIC are prepared directly from compounds of Formula IIA by reaction with an appropriately substituted acyl halide of Formula D4. To carry out this process, the compound of Formula IIA is dissolved in an inert organic solvent as defined above, preferably acetonitrile, and reacted with about 1 to 6 molar equivalents, preferably about 3 molar equivalents, of the appropriate compound of Formula D4, in the presence of about 1 to 6 molar equivalents, preferably about 3 molar equivalents, of an inorganic base or tertiary organic base as defined above, preferably pyridine. The reaction takes place at a temperature of about 0°-25° C., preferably about 5° C., for about 1-10 hours, preferably about 3 hours. When the reaction is substantially complete, the product of Formula IIC is isolated by conventional means.
Similarly, substituting an acyl halide of Formula D5 for an acyl halide of Formula D4, the compounds of Formula IID are prepared. Compounds of Formula IID where --XR 7 is OH are prepared by carrying out the above reaction directly on mycophenolic acid, the compound of Formula A.
Compounds of Formulas IIE and IIF
Compounds of Formula IIE (compounds of Formula II in which R 1 is R--C═C--Q) and Formula IIF (compounds of Formula II in which R 1 is R--C═C--Q, in which R and Q are H or --CO 2 R 3 , where R 3 is H, are prepared as shown in Reaction Scheme 3, below. ##STR14##
Compounds of Formula IIE are prepared directly from compounds of Formula IIA by reaction with an appropriately substituted acetylene of Formula D6. To carry out this process, the compound of Formula C is dissolved in an inert organic solvent as defined above, preferably tetrahydrofuran, and reacted with about 1 to 5 molar equivalents, preferably about 2 molar equivalents, of the appropriate compound of Formula D6 in the presence of about 1 to 5 molar equivalents, preferably about 2 molar equivalents, of a tertiary organic base or inorganic base as defined above, preferably pyridine. The reaction takes place at a temperature of about 0°-50° C., preferably about 5° C., for about 1-48 hours, preferably about 16 hours. When the reaction is substantially complete, the product of Formula IIE is isolated by conventional means.
Compounds of Formula IIF are prepared by hydrolysis of compounds of Formula IIE. To carry out the process, the compound of Formula IIE is dissolved in an inert organic solvent as defined above, preferably tetrahydrofuran, and reacted with about 3 to 15 molar equivalents, preferably about 6 molar equivalents, of an inorganic base such as sodium hydroxide, potassium carbonate, or preferably lithium hydroxide, dissolved in a protic solvent such as methanol, ethanol or preferably water. The reaction takes place at a temperature of about 0°-50° C., preferably about 25° C., for about 1-48 hours, preferably about 20 hours. When the reaction is substantially complete, the product of Formula IIF is isolated by conventional means.
Salts of Compounds of Formula II
Some of the compounds of Formula II may be converted to corresponding base addition salts by virtue of the presence of a carboxylic acid group. The conversion is accomplished by treatment with a stoichiometric amount of an appropriate base, such as potassium carbonate, sodium bicarbonate, ammonia, ethylenediamine, monoethanolamine, diethanolamine, triethanolamine and the like. Typically, the free acid is dissolved in a polar organic solvent such as ethanol or methanol, and the base added in water, ethanol or methanol. The temperature is maintained at 0°-50° C. The resulting salt precipitates spontaneously or may be brought out of solution with a less polar solvent.
The base addition salts of the compounds of Formula II may be decomposed to the corresponding free acids by treating with an exess of a suitable acid, such as hydrochloric acid or sulfuric acid, typically in the presence of aqueous solvent, and at a temperature of between 0° and 50° C. The free acid form is isolated by conventional means, such as extraction with an organic solvent.
Preparation of Starting Materials
The compounds of Formula II are prepared from mycophenolic acid, the compound of Formula A, which is commercially available.
The compounds of Formula B1 and Formula D1 are commercially available, or can be prepared by standard methods known to those skilled in the chemical art. The compounds of Formula B1 which are not commercially available are prepared by means well known to those skill in the art, for example as described in Synthetic Organic Chemistry by Wagner and Zook, pp. 148-225 and 778-786, which is incorporated herein by reference. In general, the compounds of Formula D1 are commercially available. The compounds of Formula D1 wherein R 5 is phenyl having a substituent COOR 3 where R 3 is lower alkyl are prepared from the compounds of Formula D1 where R 3 is H--for example, by reaction of the appropriate compound of Formula D1 with an excess of the alcohol R 3 OH in the presence of an acid catalyst. The reaction is described in greater detail in Organic Functional Group Preparations, 2nd Edition, Vol. I, by Sandler and Karo, pp. 289-309, which is incorporated herein by reference.
The compounds of Formula D2 are either available commercially or can be prepared by, for example, reaction of a secondary amine of Formula D1 with phosgene (Y═O) or thiophosgene (Y═S). Compounds of Formula D2 wherein R 1 is H can be prepared by the reaction of an isocyanate or isothiocyanate of Formula D3 with an excess of dry hydrochloric acid in an inert solvent. These reactions are described in greater detail in Comprehensive Organic Chemistry, Vol. 2, by Barton and Ollis, pp. 1088-1090, which is incorporated herein by reference.
Any alkyl or aryl chloroformates or chlorothioformates that are not commercially available are prepared, for example, by reaction of phosgene or thiophosgene with one equivalent of the appropriate alcohol or phenol in the presence of a base. The reactions are described in greater detail in Comprehensive Organic Chemistry, by Barton and Ollis, Vol 2, pp. 1078-1083 and Vol 3, pp. 432-4, which is incorporated herein by reference.
The compounds of Formula D3 that are not commercially available are prepared by reaction of an appropriately substituted primary amine (R 2 NH 2 ) with phosgene or thiophosgene. The reaction is discussed in further detail in Organic Functional Group Preparations, 2nd Edition, Vol. 1, by Sandler and Karo, pp. 364-365, which is incorporated herein by reference.
The acyl halides of Formula D4 and Formula D5 are prepared from commercially available carboxylic acids or half esters of dicarboxylic acids respectively. For example, the compounds where M is C1 can be prepared by reaction with thionyl chloride in an inert solvent. The reaction is discussed in further detail in Synthetic Organic Chemistry, by Wagner and Zook, pp. 546-547, which is incorporated herein by reference. The half esters of dicarboxylic acids, if not commercially available, can be prepared, for example, by the reaction of the appropriate alcohol and an anhydride formed from a dicarboxylic acid as shown in the reaction scheme below. ##STR15##
The reaction is discussed in more detail in Comprehensive Organic Chemistry, Vol. 2, by Barton and Ollis, p 687, which is incorporated herein by reference.
Acetylenes of Formula D6 are commercially available or are prepared from propiolic acid or acetylene dicarboxylic acid by conventional esterification procedures, which are discussed in more detail in Organic Functional Group Preparations, 2nd Edition, Vol 1, by Sandler and Karo, pp 289-309, which is incorporated herein by reference.
In summary, the compounds of the present invention are made by the procedures outlined below:
(1) The process for preparing compounds of Formula IIA comprises reacting a compound of the formula ##STR16## in which L is a leaving group with a compound of the formula R 7 XH, where R 7 and X are as previously defined.
(2) The process for preparing compounds of Formula IIB comprises:
(a) reacting a compound of the formula: ##STR17##
wherein X, Y, M and R 7 are as defined above, with an appropriate amine of the formula R 4 R 5 NH, wherein R 4 and R 5 are as defined above; or
(b) converting the free acid, where appropriate, of the compound of Formula IIB with a base to a pharmaceutically acceptable salt; or
(c) converting a base addition salt of the compound of Formula IIB with an acid to the corresponding free acid.
(d) converting a base addition salt of the compound of Formula IIB to another pharmaceutically acceptable base addition salt.
(3) Alternatively, a process for preparing a compound of Formula IIB, above, comprises:
(a) reacting a copound of the formula: ##STR18##
where X and R 7 are as defined above with a carbamoyl chloride of the formula R 4 R 5 NCYCl, or an isocyanate of the formula R 5 NCY, wherein R 4 , R 5 and Y are as defined above; or
(b) converting the free acid, where appropriate, of the compound of Formula IIB with a base to a pharmaceutically acceptable salt; or
(c) converting a base addition salt of the compound of Formula IIB with an acid to the corresponding free acid.
(d) converting a base addition salt of the compound of Formula IIB to another pharmaceutically acceptable base addition salt.
(4) The process for preparing a compound of Formula IIC and Formula IID comprises:
(a) reacting a compound of the formula: ##STR19##
where X and R 7 are as defined above with an acyl halide of the formula R 2 COHal; or
(b) converting the free acid, where appropriate, of the compound of Formula IIC or Formula IID with a base to a pharmaceutically acceptable salt; or
(c) converting a base addition salt of the compound of Formula IIC or Formula IID with an acid to the corresponding free acid.
(d) converting a base addition salt of the compound of Formula IIC or Formula IID to another pharmaceutically acceptable base addition salt.
(5) The process for preparing a compound of Formula IIE comprises:
(a) reacting a compound of the formula ##STR20##
where X and R 7 are as defined above, with an acetylene of formula R--C.tbd.C--Q, where R and Q are as defined above; or
(b) converting the free acid, where appropriate, of the compound of Formula IIE with a base to a pharmaceutically acceptable salt; or
(c) converting a base addition salt of the compound of Formula IIE with an acid to the corresponding free acid.
(d) converting a base addition salt of the compound of Formula IIE to another pharmaceutically acceptable base addition salt.
(6) The process for preparing a compound of Formula IIF comprises:
(a) reacting a compound of the formula: ##STR21##
where R and Q are --CO 2 R 3 , where R 3 is alkyl having from 1-6 carbon atoms and X and R 7 are as defined above, with an alkali metal hydroxide followed by a mineral acid; or
(b) converting the free acid of the compound of Formula IIF with a base to a pharmaceutically acceptable salt; or
(c) converting a base addition salt of the compound of Formula IIF with an acid to the corresponding free acid.
(d) converting a base addition salt of the compound of Formula IIF to another pharmaceutically acceptable base addition salt.
UTILITY AND ADMINISTRATION
The compounds of Formulas I and II have been shown in standard laboratory tests to be useful in treating chronic inflammatory diseases, including models of rheumatoid arthritis, in mammals. Accordingly, the compounds of Formula I and II, their salts, and pharmaceutical compositions containing them, may be used in treating inflammatory diseases with an immunologically based component, particularly rheumatoid arthritis, in mammals by administering a therapeutically effective amount of a compound of Formula I or II to a mammal in need thereof. Anti-inflammatory activity can be determined by the method described by C. M. Pearson in Proc. Soc. Exp. Biol. Med., 91:95-101, (1956) utilizing adjuvant-induced arthritis in rats. This method is described in detail in Example 14 hereinbelow. Rheumatoid arthritis is also characterized as an autoimmune disease. Activity against autoimmune diseases can be determined by the method described by Grieg, et al. in J. Pharmacol. Exp. Ther. 173:85 (1970) using experimental allergic encephalomyelitis induced in rats. The method is described in Example 15 below.
Administration of the active compounds and salts described herein can be effected via any medically acceptable mode of administration for agents which control inflammation, rheumatoid arthritis and associated pain. These methods include but are not limited to oral, parenteral and otherwise systemic and topical routes of administration. Oral administration is preferred, depending of course, on the disorder being treated. The compounds are administered in a therapeutically effective amount either alone or in combination with a suitable pharmaceutically acceptable excipient.
Depending on the intended mode of administration, the compounds of this invention may be incorporated in any pharmaceutically acceptable dosage form, such as, for example, tablets, suppositories, pills, capsules, powders, liquids, suspensions, emulsions, aerosols, or the like. Preferably means of administration are unit dosage forms suitable for single administration of precise dosages, or sustained release dosage forms for continuous administration. Preferably the dosage form will include a pharmaceutically acceptable excipient and an active compound of Formula I, or a pharmaceutically acceptable salt thereof, and, in addition, may include other medicinal agents, pharmaceutical agents, carriers, excipients, adjuvants, stabilizers, etc. Depending on parameters such as mode of administration, type of composition, and activity of the compound, the pharmaceutical composition may contain 1-95 percent by weight active ingredient with the remainder being excipient.
For solid dosage forms, non-toxic solid carriers include but are not limited to, for example, pharmaceutical grades of mannitol, lactose, starch, magnesium stearate, sodium saccharin, the polyalkylene glycols, talcum, cellulose, glucose, sucrose, and magnesium carbonate. An example of a solid dosage form of the compounds of this invention is a suppository containing propylene glycol as the carrier. Liquid pharmaceutically administerable dosage forms can, for example, comprise a solution or suspension of an active compound as defined above and optional pharmaceutical adjuvants in a carrier, such as, for example, water, saline, aqueous dextrose, glycerol, ethanol, and the like, to thereby form a solution or suspension. If desired, the pharmaceutical composition to be administered may also contain minor amounts of nontoxic auxiliary substances such as wetting or emulsifying agents, pH buffering agents and the like. Typical examples of such auxiliary agents are sodium acetate, sorbitan monolaurate, triethanolamine sodium acetate, triethanolamine oleate, etc. Actual methods of preparing such dosage forms are known, or will be apparent, to those skilled in this art; for example, see Remington's Pharmaceutical Sciences, Mack Publishing Company, Easton, Pa., 16th Edition, 1980. The composition or formulation to be administered will, in any event, contain a quantity of the active compound(s) in an amount effective to alleviate the symptoms of the subject being treated.
For oral administration, a pharmaceutically acceptable non-toxic dosage form may contain any of the normally employed excipients, such as, for example pharmaceutical grades of mannitol, lactose, starch, magnesium stearate, sodium saccharin, talcum, cellulose, glucose, sucrose, magnesium carbonate, and the like. Such compositions take the form of solutions, suspensions, tablets, pills, capsules, powders, sustained release formulations and the like. Such dosage forms may contain 1%-95% active ingredient, preferably 25-70%.
For topical administration, an appropriate dosage form will comprise an effective amount of a compound of Formula I in admixture with a pharmaceutically acceptable non-toxic carrier. A suitable range of composition would be 0.1%-10%, preferably 1-2% by weight, active ingredient, and the balance carrier. The concentration of active ingredient in pharmaceutical compositions suitable for topical application will vary depending upon the therapeutic activity of the particular active ingredient and the medical condition to be treated. Suitable dosage forms for topical application of the compounds of this invention include but are not limited to creams, ointments, lotions, emulsions and solutions.
For example, a suitable ointment for topical application of compounds of the instant invention may contain 15-45% by weight of a saturated fatty alcohol having 16 to 24 carbon atoms, such as cetyl alcohol, stearyl alcohol, behenyl alcohol, and the like, and 45-85% by weight of a glycol solvent such as propylene glycol, polyethylene glycol, dipropylene glycol, and mixtures thereof. In addition, the ointment may contain 0-25% by weight of a plasticizer (e.g. polyethylene glycol, 1,2,6-hexanetriol, sorbitol, glycerol, and the like), 0-15% by weight of a coupling agent such as a saturated fatty acid having from 16 to 24 carbon atoms, (e.g., stearic acid, palmitic acid or behenic acid) a fatty acid amide (e.g. oleamide, palmitamide, stearamide of behenamide) or an ester of a fatty acid having from 16 to 24 carbon atoms (e.g., sorbitol monostearate, polyethylene glycol monostearate, polypropylene glycol or the corresponding mono-ester or other fatty acids such as oleic acid and palmitic acid), and 0-20% by weight of a penetrant such as dimethyl sulfoxide of dimethylacetamide.
The amount of active compound administered will, of course, depend on the subject being treated, the severity of the affliction, the manner of administration and the judgment of the prescribing physician. However, a therapeutically effective dosage of compounds of the instant invention is in the range of 1-100 mg/kg/day, preferably about 5-30 mg/kg/day, and most preferably about 10 mg/kg/day. For an average 70 kg human, this would amount to 70 mg-7 g per day, or preferably about 700 mg/day.
Preferred Embodiments
Among the family of compounds defined by Formula I, preferred methods of treating rheumatoid arthritis utilize compounds of Formula I in which A is oxygen and R 1 is CONR 4 R 5 . Of these, more preferred methods utilize compounds of Formula I in which Z is COOR 7 in which R 7 is lower alkyl, particularly hydrogen or methyl.
Among the family of compounds defined by Formula II, one preferred group includes those compounds of Formula II in which X is oxygen. Of these, a preferred subgroup are compound of Formula II in which R 7 is hydrogen or methyl. Within this subgroup, one preferred subclass includes compounds of Formula II in which R 1 is CO(CH 2 ) n CO 2 R 3 , especially those in which R 3 is methyl or ethyl. A second preferred subclass within this subgroup includes compounds of Formula II in which R 1 is R--C═CH--Q, particularly those in which R and Q are each CO 2 R 3 where R 3 is hydrogen, methyl or ethyl.
A second preferred group are compounds of Formula II in which X is sulfur. Within this group, a preferred subgroup includes compounds of Formula II in which R 1 is hydrogen or COR 2 , especially where R 2 is --NR 4 R 5 .
At present, the most preferred compounds of Formula II are:
(E)-6-[1,3-dihydro-4-(3-carbomethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid;
(E)-6-[1,3-dihydro-4-(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid;
(E)-6-[1,3-dihydro-4-(2-carbomethoxyethanoyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid;
(E)-6-[1,3-dihydro-4-(4-carbomethoxybutanoyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid;
(E)-6-[1,3-dihydro-4-(5-carbomethoxypentanoyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid;
methyl (E)-[1,3-dihydro-4-(1,2-dicarbomethoxyeth-2-(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate; and
methyl (E)-[1,3-dihydro-4-(1,2-dicarboethoxyeth-2-(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate.
The following examples serve to further illustrate the invention. They are not intended, nor should they be construed, to narrow or limit the scope of the invention as claimed.
EXAMPLE 1
Preparation of ethyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate and related compounds of Formula IIA
(a) To a solution of 5.0 g of mycophenolic acid in 75 ml of methylene chloride was added 5 ml of thionyl chloride and 5 drops of N,N-dimethylformamide. The mixture was stirred overnight at 25° C. and the solvent removed under reduced pressure. The residue was dissolved in 100 ml of methylene chloride, cooled to 50° C. and 4.2 ml of pyridine and 5.43 ml of ethylmercaptan added. The mixture was stirred at 25° C. overnight, then poured into water and extracted with methylene chloride. The organic layer was dried over anhydrous magnesium sulfate, evaporated under reduced pressure and the residue chromatographed on silica gel, eluting with a 1:1 mixture of diethyl ether and hexane. The purified product was recrystallized from a mixture of diethyl ether and hexane to yield ethyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate, having a melting point of 63°-67° C.
(b) Following the procedure described in paragraph (a) above, but using the appropriate compounds of Formula B1, the following compound of Formula IIA was prepared:
Benzyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate, m.p. 80°-82° C.
(c) In a similar manner, the following compounds of Formula IIA where X is sulfur are prepared:
methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
propyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
isopropyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
butyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
sec-butyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
n-pentyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
n-hexyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
cyclohexyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
cyclopentyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
phenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
2-chlorophenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
4-chlorophenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate;
4-methoxyphenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate; and
2,4-dimethoxyphenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate.
(d) Similarly, by following the procedure of part (a) but substituting the appropriate alkyl, cycloalkyl, benzyl alcohol or phenol for the mercaptan, the following compounds of Formula IIA, where X is oxygen, are prepared:
ethyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
propyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
isopropyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
butyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
sec-butyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
n-pentyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
n-hexyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
cyclohexyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
cyclopentyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
phenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
2-chlorophenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
4-chlorophenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate;
4-methoxyphenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate; and
2,4-dimethoxyphenyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate.
EXAMPLE 2
Preparation of ethyl (E)-6-(1,3-dihydro-4-carbamoyloxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate and related compounds of Formula IIB
(a) To a solution of 500 mgs of ethyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate in 10 ml of benzene cooled in an ice bath was added 0.1 ml of pyridine and 6 ml of a 12.5% solution of phosgene in benzene. The solution was stirred at 25° C. overnight, the precipitate filtered off and solvent removed from the filtrate under reduced pressure. The residue was dissolved in 5 ml of tetrahydrofuran and to this solution was added dropwise a solution of ammonia in tetrahydrofuran until the reaction was complete. The mixture was poured into water and extracted with ethyl acetate. The organic solution was dried over magnesium sulfate and evaporated to an oil which was chromatographed on silica gel, eluting with a 1:1 mixture of ethyl acetate and hexane. The purified product was stirred with a mixture of ether and hexane and filtered giving ethyl (E)-6-(1,3-dihydro-4-carbamoyl oxy-6-methoxy-7-methyl-3-oxo-5-iso benzofuranyl)-4-methyl-4-thiohexenoate, mp 145°-147° C.
(b) Following the procedure described in paragraph (a) above, but using the appropriate compounds of Formula C and Formula D1, the following compounds of Formula IIB were prepared:
Benzyl (E)-6-(1,3-dihydro-4-carbamoyloxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate, m.p. 119°-121° C.
Ethyl (E)-6-{1,3-dihydro-4-[N-(4-carboxyphenyl)-carbamoyloxy]-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl}-4-methyl-4-thiohexenoate, m.p. 204°-206° C.
Cyclohexyl (E)-6-{1,3-dihydro-4-[N-(4-carboxyphenyl)-carbamoyloxy]-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl}-4-methyl-4-thiohexenoate, m.p. 205°-206° C.; and
Benzyl (E)-6-{1,3-dihydro-4-[N-(4-carboxyphenyl)carbamoyloxy]-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl}-4-methyl-4-thiohexenoate, m.p. 185°-187° C.;
(c) In a similar manner, but starting as desired with other appropriate compounds of Formula IIA, and substituting as needed other appropriate compounds of Formula D1, the following representative compounds of Formula IIB, in which X is oxygen and R 4 , R 5 , R 7 and Y are as defined below, are prepared.
______________________________________R.sup.4 R.sup.5 R.sup.7 Y______________________________________H 4-carboxyphenyl phenyl OH 4-carboxyphenyl 4-methoxyphenyl OH 4-carboxyphenyl benzyl SH H methyl SH H cyclohexyl OH H isopropyl OH CH.sub.3 n-butyl OH n-propyl n-entyl SCH.sub.3 isobutyl n-hexyl On-hexyl n-hexyl cyclohexy1 Omethyl 4-carboxyphenyl cyclooenty1 OH 4-methoxycarbonylphenyl 2-chlorophenyl Sethyl 4-carboxyphenyl 4-chlorophenyl OH H 2,4-dimethyoxy phenyl O______________________________________
(d) Similarly, the following compounds of Formula IIB, in which X is sulfur and R 4 , R 5 , R 7 , and Y are as defined below, are prepared:
______________________________________R.sup.4 R.sup.5 R.sup.7 Y______________________________________H 4-carboxyphenyl phenyl OH 4-carboxyphenyl 4-methoxyphenyl OH 4-carboxyphenyl benzyl SH H methyl SH H cyclohexyl OH H isopropyl OH CH.sub.3 n-butyl OH n-propyl n-entyl SCH.sub.3 isobutyl n-hexyl On-hexyl n-hexyl cyclohexy1 Omethyl 4-carboxyphenyl cyclooenty1 OH 4-methoxycarbonylphenyl 2-chlorophenyl Sethyl 4-carboxyphenyl 4-chlorophenyl OH H 2,4-dimethyoxy phenyl O______________________________________
EXAMPLE 3
Preparation of ethyl (E)-6-(1,3-dihydro-4-acetoxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexanoate and related compounds of Formula IIC and IID
(a) To a solution of 1.6 g of ethyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate in 120 ml of acetonitrile at 0° C. was added 0.74 ml of pyridine followed by 1.0 ml of acetyl chloride. After stirring for 2 hours the reaction mixture was poured into dilute hydrochloric acid and extracted with ethyl acetate. The organic solution was dried over anhydrous magnesium sulfate and evaporated to an oil, which was triturated with ether to give ethyl (E)-6-(1,3-dihydro-4-acetoxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate, m.p. 81°-84° C.
(b) Following the procedure described in paragraph (a) above but using mycophenolic acid in place of the compound of Formula IIA and the appropriate acyl halide of Formula D5, the following compounds of Formula IID were prepared:
(E)-6-[1,3-dihydro-4-(carboethoxycarbonyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate, m.p. 125°-127° C.
(E)-6-[1,3-dihydro-4-(carbomethoxyethanoyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate, m.p. 112°-114° C.
(E)-6-[1,3-dihydro-4-(carboethoxyethanoyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate, m.p. 99°-101° C.
(E)-6-[1,3-dihydro-4-(3-carbomethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexanoate, m.p., 125°-127° C.
(E)-6-[1,3-dihydro-4-(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexanoate, m.p. 93°-95° C.
(E)-6-[1,3-dihydro-4-(4-carbomethoxybutanoyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexanoate, m.p. 65°-67° C.
(E)-6-[1,3-dihydro-4-(5-carbomethoxypentanoyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexanoate, m.p. 99°-101° C.
(c) In a similar manner, the following exemplary compounds of Formula IIC where X is oxygen and R 2 and R 7 are as defined below are prepared:
______________________________________R.sup.2 R.sup.7______________________________________ethyl ethyln-propyl n-propylisopropyl methyln-butyl isopropylisobutyl n-butyln-pentyl n-hexyln-hexyl cyclohexylmethyl cyclopentylmethyl 2-chlorophenylmethyl 4-methoxyphenylmethyl 2,4-dimethoxyphenyl______________________________________
(d) In a similar manner the following compounds of Formula IIC where X is sulfur are prepared:
______________________________________R.sup.2 R.sup.7______________________________________ethyl ethyln-propyl n-propylisopropyl methyln-butyl isopropylisobutyl n-butyln-pentyl n-hexyln-hexyl cyclohexylmethyl cyclopentylmethyl 2-chlorophenylmethyl 4-methoxyphenylmethyl 2,4-dimethoxyphenyl______________________________________
(e) In a similar manner, but substituting an appropriate acyl halide of Formula D5 for an acyl halide of Formula D4, and starting with the desired compound of Formula IIA, the following compounds of Formula IID where X is oxygen and R 3 and R 7 are as defined below, are prepared:
______________________________________R.sup.3 R.sup.7______________________________________ethyl ethyln-propyl n-propylisopropyl methyln-butyl isopropylisobutyl n-butylsec-butyl n-pentyln-pentyl n-hexyln-hexyl cyclohexylmethyl cyclopentylmethyl 2-chlorophenylmethyl 4-methoxyphenylmethyl 2,4-dimethoxyphenyl______________________________________
(f) In a similar manner, the following compounds of Formula IID where X is sulfur, are prepared:
______________________________________R.sup.3 R.sup.7______________________________________ethyl ethyln-propyl n-propylisopropyl methyln-butyl isopropylisobutyl n-butylsec-butyl n-pentyln-pentyl n-hexyln-hexyl cyclohexylmethyl cyclopentylmethyl 2-chlorophenylmethyl 4-methoxyphenylmethyl 2,4-dimethoxyphenyl______________________________________
EXAMPLE 4
Preparation of methyl E-6-[1,3-dihydro-4-(1,2-dicarbomethoxy-2-(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate and related compounds of Formula IIE
(a) To a solution of 6.72 g of methyl E-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-hexenoate in 100 ml of tetrahydrofuran at -80° C. was added 3.16 ml of pyridine and 4.8 g of dimethyl acetylenedicarboxylate and the mixture was allowed to warm to 25° C. and was stirred for 16 hours. The solution was poured into dilute hydrochloric acid and extracted with diethyl ether. The organic solution was dried over anhydrous sodium sulfate and the solvent removed under reduced pressure. The residue was chromatographed on silica gel eluting with diethyl ether. The purified product was recrystallized from diethyl ether/hexane mixture, to yield methyl E-6-[1,3-dihydro-4-(1,2-dicarbomethoxyeth-2-(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate, m.p. 105°-107° C.
(b) Following the procedure described in paragraph (a) above, but substituting as desired the appropriate compounds of Formula IIA and the appropriately substituted acetylenes of Formula D6 for those used in paragraph (a), the following compound of Formula IIE was prepared:
Methyl-E-6-[1,3-dihydro-4-(1,2-dicarboethoxyeth-2-(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate, m.p. 61°-63° C.
(c) In a similar manner, the following exemplary compounds of Formula IIE where X is oxygen and R 3 and R 7 are as defined below are prepared:
______________________________________R.sup.3 R.sup.7______________________________________ethyl Hn-propyl propylethyl isopropylmethyl n-butylmethyl sec-butylethyl n-pentyln-butyl n-hexylisobutyl cyclohexyln-pentyl cyclopentylmethyl phenylethyl 2-chlorophenylmethyl 4-chlorophenylethyl 4-methoxyphenylmethyl 2,4-dimethoxyphenylethyl benzyl______________________________________
(d) In a similar manner, but starting instead with the appropriate compounds of Formula IIA in which X is sulfur, the following exemplary compounds of Formula IIE are prepared:
______________________________________R.sup.3 R.sup.7______________________________________n-propyl propylethyl isopropylmethyl n-butylmethyl sec-butylethyl n-pentyln-butyl n-hexylisobutyl cyclohexyln-pentyl cyclopentylmethyl phenylethyl 2-chlorophenylmethyl 4-chlorophenylethyl 4-methoxyphenylmethyl 2,4-dimethoxyphenylethyl benzyl______________________________________
EXAMPLE 5
Preparation of (E)-6-[1,3-dihydro-4-(1,2-dicarboxyeth-2-(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid, a Compound of Formula IIF
(a) To a solution of 2.4 g of methyl (E)-6-[1,3-dihydro-4-(1,2-dicarbomethoxy 2(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoate in 50 ml of tetrahydrofuran was added a solution of 1.2 g of lithium hydroxide monohydrate in 50 ml of water. After stirring for 20 hours the solution was poured into dilute hydrochloric acid and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and the solvent removed under reduced pressure. The residue was chromatographed on silica gel, eluting with 0.1% formic acid in ethyl acetate. The purified product was triturated with ether, giving (E)-6-[1,3-dihydro-4-(1,2-dicarboxyeth-2(E)-enyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid, m.p. 203°-205° C.
(b) Following the procedure described in paragraph (a) above, but starting with the appropriate compound of Formula IIE, the following compound of Formula IIF was prepared:
(E)-6-[1,3-dihydro-4-(E)(2-carboxy-ether-1-gloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl]-4-methyl-4-hexenoic acid, m.p. 145°-146° C.
(c) In a similar manner, but starting as desired with other appropriate compounds of Formulas IIE and D6, the following compounds of Formula IIF in which X is oxygen and R, Q and R 7 are as defined below are prepared:
______________________________________R Q R.sup.7______________________________________H CO.sub.2 CH.sub.3 phenylH CO.sub.2 C.sub.2 H.sub.5 4-methoxyphenylH CO.sub.2 isopropyl benzylH CO.sub.2 n-propyl methylH CO.sub.2 sec-butyl cyclohexylH CO.sub.2 n-butyl isopropylH CO.sub.2 n-pentyl n-butylCO.sub.2 CH.sub.3 H n-pentylCO.sub.2 C.sub.2 H.sub.5 H n-hexylCO.sub.2 isopropyl H cyclohexylCO.sub.2 n-propyl H cyclopentylCO.sub.2 sec-butyl H 2-chlorophenylCO.sub.2 n-butyl H 4-chlorophenylCO.sub.2 n-pentyl H 2,4-dimethoxyphenylCO.sub.2 CH.sub.3 CO.sub.2 CH.sub.3 n-pentylCO.sub.2 C.sub.2 H.sub.5 CO.sub.2 C.sub.2 H.sub.5 n-hexylCO.sub.2 isopropyl CO.sub.2 isopropyl cyclohexylCO.sub.2 n-propy1 H cyclopentylCO.sub.2 sec-butyl H 2-chlorophenylCO.sub.2 n-butyl H 4-chlorophenylCO.sub.2 n-pentyl H 2,4-dimethoxyphenyl______________________________________
(d) In a similar manner, but starting as desired with other appropriate compounds of Formulas IIE and D6, the following exemplary compounds of Formula IIF in which X is sulfur and R, Q and R 7 are as defined below are prepared:
______________________________________R Q R.sup.7______________________________________H CO.sub.2 CH.sub.3 phenylH CO.sub.2 C.sub.2 H.sub.5 4-methoxyphenylH CO.sub.2 isopropyl benzylH CO.sub.2 n-propyl methylH CO.sub.2 sec-butyl cyclohexylH CO.sub.2 n-butyl isopropylH CO.sub.2 n-pentyl n-butylCO.sub.2 CH.sub.3 H n-pentylCO.sub.2 C.sub.2 H.sub.5 H n-hexylCO.sub.2 isopropyl H cyclohexylCO.sub.2 n-propyl H cyclopentylCO.sub.2 sec-butyl H 2-chlorophenylCO.sub.2 n-butyl H 4-chlorophenylCO.sub.2 n-pentyl H 2,4-dimethoxyphenylCO.sub.2 CH.sub.3 CO.sub.2 CH.sub.3 n-pentylCO.sub.2 C.sub.2 H.sub.5 CO.sub.2 C.sub.2 H.sub.5 n-hexylCO.sub.2 isopropyl CO.sub.2 isopropyl cyclohexylCO.sub.2 n-propy1 H cyclopentylCO.sub.2 sec-butyl H 2-chlorophenylCO.sub.2 n-butyl H 4-chlorophenylCO.sub.2 n-pentyl H 2,4-dimethoxyphenyl______________________________________
EXAMPLE 6
Conversion of Free Acid to Salt
One molar equivalent of sodium hydroxide in water is added to a methanolic solution of 1.0 g of (E)-6-[1,3-dihydro-4(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzoylfuranyl]-4-methyl-4-hexenoic acid. The solvent is removed under vacuum and the residue recrystallized to give the sodium salt of (E)-6-[1,3-dihydro-4(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzoylfuranyl]-4-methyl-4-hexenoic acid.
EXAMPLE 7
Conversion of Salt to Free Acid
1.0 g of the sodium salt of (E)-6-[1,3-dihydro-4(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzoylfuranyl]-4-methyl-4-hexenoic acid suspended in ether is stirred with 2 molar equivalents of dilute aqueous sulfuric acid until the salt is completely dissolved. The organic layer is separted, washed with water, dried over magnesium sulfuate and evaporated to yield (E)-6-[1,3-dihydro-4(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzoylfuranyl]-4-methyl-4-hexenoic acid.
EXAMPLE 8
Direct Interchange of Basic Salts
1.0 g of the ammonium salt of (E)-6-[1,3-dihydro-4(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzoylfuranyl]-4-methyl-4-hexenoic acid is dissolved in methanol containing one molar equivalent of sodium hydroxide and the solution evaporated to dryness under vacuum. The residue is recrystallized to give the sodium salt of (E)-6-[1,3-dihydro-4(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzoylfuranyl]-4-methyl-4-hexenoic acid.
EXAMPLES 9-13
In Examples 5 through 9, the active ingredient is (E)-6-[1,3-dihydro-4(3-carboethoxypropionyloxy)-6-methoxy-7-methyl-3-oxo-5-isobenzoylfuranyl]-4-methyl-4-hexenoic acid. However other compounds of Formula I and II such as those prepared in Examples 1-5, and the pharmaceutically acceptable salts thereof may be substituted:
EXAMPLE 9
______________________________________ Quantity perIngredients tablet, mgs.______________________________________Active ingredient 25cornstarch 20lactose, spray-dried 153magnesium stearate 2______________________________________
The above ingredients are thoroughly mixed and pressed into single scored tablets.
EXAMPLE 10
______________________________________ Quantity perIngredients tablet, mgs.______________________________________Active ingredient 100lactose, spray-dried 148magnesium stearate 2______________________________________
The above ingredients are mixed and introduced into a hard-shell gelatin capsule.
EXAMPLE 11
______________________________________ Quantity perIngredients tablet, mgs.______________________________________Active ingredient 108lactose 15cornstarch 25magnesium stearate 2______________________________________
The above ingredients are mixed and introduced into a hard-shell gelatin capsule.
EXAMPLE 12
______________________________________ Quantity perIngredients tablet, mgs.______________________________________Active ingredient 150lactose 92______________________________________
The above ingredients are mixed and introduced into a hard-shell gelatin capsule.
EXAMPLE 13
A solution preparation buffered to a pH of 7 is prepared having the following composition:
______________________________________Ingredients______________________________________Active ingredient 0.1 gfumaric acid 0.5 gsodium chloride 2.0 gmethyl paraben 0.1 ggranulated sugar 25.5 gsorbitol (70% solution) 12.85 gVeegum K (Vanderbilt Co.) 1.0 gdistilled water q.s. to 100 ml______________________________________
EXAMPLE 14
Determination of Anti-Inflammatory Activity Utilizing Adjuvant-Induced Arthritis In The Rat
Protocol:
This procedure is a modification of a system initially described by Pearson, C. M., Proc. Soc. Exp. Biol. Med., 91:95-101 (1956).
Female Crl:CD, br (Sprague Dowley derived) rats (Charles River) weighing 165-185 g receive 0.1 ml of a suspension in paraffin oil of heat-killed M. Mycobacterium butyricum (10 mg/ml) by means of an intradermal injection into the proximal 1/4 of the tail on day 0. Beginning on day 1, the test material is administered orally in an aqueous vehicle (1 ml/dose) once a day for 17 days. On day 18 the intensity of the swelling of the four foot pads and tail is determined utilizing a scoring system in which the swelling in the four paws was scored 0-4 for each paw and the tail swelling was scored 0-3, such that the total maximum score is 19. The compounds of the present invention show anti-inflammatory activity when tested by this method.
EXAMPLE 15
DETERMINATION OF AUTOIMMUNE ACTIVITY UTILIZING EXPERIMENTAL ALLERGIC ENCEPHALOMYELITIS
Protocol:
This procedure is a modification of a procedure initially described by Grieg, et al., J. Pharmacol. Exp. Ther. 173:85 (1970). Female Lewis rats, LEW/Cre, br from Charles River, weighing 125-135 g were used.
On day 1, Experimental Allergic Encephalomyelitis is induced by giving an 0.1 ml sub-plantar injection into the dorsum of the right hind paw of an emulsion consisting of 15 mg (wet weight) of syngeneic spinal cord tissue, 0.06 ml of Freund's Incomplete Adjuvant (Difco). 0.04 ml of sterile 0.9% saline, and 0.2 mg of heat killed and dried Mycobacterium butyricum (Difco). Beginning on day 1, the test material is administered orally in 2N aqueaus vehicle (1 ml/dose) once a day for 16 days. On days 12-17, clinical evaluations are obtained for each animal. The animals are considered positive if flaccid hind limb paralysis is present on one or more days. The compounds of the present invention show autoimmune activity when tested by this method.
|
A method of treating rheumatoid arthritis which method comprises administering to a mammal in need of such treatment a therapeutically effective amount of a compound of the formula: ##STR1## and the pharmaceutically acceptable salts thereof, wherein:
A is oxygen or sulfur;
R 1 is selected from the group consisting of H, ##STR2## in which Y is oxygen or sulfur:
R 2 is alkyl, haloalkyl or --NR 4 R 5 , where R 4 and R 5 are independently H, alkyl, haloalkyl, cycloalkyl, phenyl optionally monosubstituted with halogen, hydroxy, carboxy, chlorocarbonyl, sulfonylamino, nitro, cyano, phenyl, alkyl, acyl, alkoxycarbonyl, acylamino, dialkylamino or dialkylaminoethoxycarbonyl, phenyl optionally disubstituted with hydroxy, carboxy, nitro or alkyl, or benzyl optionally substituted with dialkylamino;
n is an integer from 0-6;
R 3 is H alkyl or a pharmaceutically acceptable cation;
Q and R are independently H or --CO 2 R 3 ; and
Z is selected from the group consisting of ##STR3## in which X is oxygen or sulfur,
R 7 is H, alkyl, alkenyl, cycloalkyl, optionally substituted phenyl, optionally substituted benzyl or a pharmaceutically acceptable cation; and
R 8 and R 9 are independently H, alkyl or cycloalkyl, or R 8 and R 9 taken together are --(CH 2 ) 4 --, --(CH 2 ) 5 -- or --(CH 2 ) 2 O(CH 2 ) 2 --;
with the proviso that R 1 and R 7 cannot both be H if X and A are oxygen.
| 2
|
CROSS-REFERENCES TO RELATED APPLICATIONS
This application relates to and claims priority from Japanese Patent Application No. 2008-022675, filed on Feb. 1, 2008, the entire disclosure of which is incorporated herein by reference.
BACKGROUND
1. Technical Field
The present invention relates to a biological sample reaction chip and to a biological sample reaction method for carrying out biological sample reactions such as nucleic acid amplification.
2. Related Art
Growing attention is being focused on methods for carrying out, for instance, chemical analysis, chemical synthesis or bio-related analysis using microfluidic chips in which microchannels are provided in a glass plate or the like. Microfluidic chips, which are also called micro-Total Analytical Systems (micro-TAS), Lab-on-a-chip and the like, are advantageous in that they require smaller amounts of specimens and reagents, have shorter reaction times and generate fewer waste products than existing devices. Thus, microfluidic chips are thus a promising application in a wide range of fields such as medical diagnosis, environmental and foodstuff onsite analysis, and in the manufacture of pharmaceuticals and chemicals, where test costs can be reduced since reaction amounts may be small. Likewise, testing can be made more efficient by considerably shortening also reaction times, since samples and reagents are used in small amounts. When used in medical diagnosis, in particular, microfluidic chips are advantageous in that they can use less of a specimen, for instance a blood sample, which allows easing the burden placed on the patient.
Known methods for amplifying genes such as DNA and RNA, used as samples, include polymerase chain reaction (PCR). In PCR, a mixture of target DNA and reagents is placed in a tube where the reagents and the target DNA are made to react, by repeating a so-called thermal cycle that involves changes of temperature in three stages, for instance, 55° C., 72° C. and 94° C., over several minutes, using a temperature control device. In each temperature cycle the target DNA can be amplified, to roughly a double amount, through the action of an enzyme called polymerase.
So-called real-time PCR, using special fluorescent probes, has come into use in recent years. In real-time PCR, DNA can be quantified while the amplification reaction is taking place. Real-time PCR boasts high measurement sensitivity and reliability, and is hence widely used in research and clinical testing.
Conventional devices, however, were problematic in that the amount of reaction liquid required for PCR is normally of several tens of μl, while basically only one gene could be determined in one reaction system. Some methods allow measuring simultaneously about four genes by introducing plural fluorescent probes and discriminating between respective colors, but determining simultaneously more than four genes inevitably calls for an increase in the number of reaction systems. The amount of DNA extracted from the specimen is normally small, and reagents are expensive. It has been thus difficult to determine simultaneously multiple reaction systems.
JP-A-2006-126010 and JP-A-2006-126011 disclose inventions in which liquid analyte samples such as a PCR reaction solution or blood are accurately introduced into a plurality of chambers, using a rotationally driven device.
JP-A-2000-236876 discloses a method that involves preparing micro-wells integrated on a semiconductor substrate, and carrying out PCR in the wells, to amplify and analyze collectively multiple DNA samples, using small sample amounts.
SUMMARY
An advantage of some aspects of the invention is to provide a biological sample reaction chip and a biological sample reaction method that allow a reaction to be carried out with a small amount of reaction liquid and that allow processing efficiently multiple specimens at a time.
A biological sample reaction chip according to an aspect of the invention includes: a plurality of reaction containers; a reaction liquid introduction channel having a reaction liquid supply opening at a first end and an evacuation opening at a second end; and a reaction liquid quantifying channel, a third end of which is connected to one of the reaction containers, and a fourth end of which is connected to the reaction liquid introduction channel, such that an interior of each of the reaction containers is coated with a reagent that is necessary for a reaction.
In this case, a reaction liquid is fed from the reaction liquid introduction channel into the reaction containers via the reaction liquid quantifying channels. Reactions using extremely small amounts of reaction liquid are made possible thereby, something that is difficult to achieve by pipette quantifying. The cost of reagents and so forth can be reduced when using small amounts reaction liquid. Also, reaction times are shortened considerably, which enhances processes efficiency. Moreover, reactions can take place in multiple reaction containers at a time, which allows conducting multiple tests and the like with good efficiency.
The reaction liquid is introduced into the reaction containers after having resided in the reaction liquid quantifying channels, whereby contamination between reaction containers can be prevented.
Reagents necessary for the reactions are coated on each reaction container, and hence the user can easily conduct tests and the like simply by filling reaction liquid.
A volume of the reaction containers may be smaller than A volume of the reaction liquid quantifying channels.
A biological sample reaction method according to an aspect of the invention is a biological sample reaction method using the above-mentioned biological sample reaction chip, the method including: reducing the pressure inside the reaction containers, the reaction liquid quantifying channels and the reaction liquid introduction channel to a predetermined pressure; filling a reaction liquid into the reaction liquid introduction channel via the reaction liquid supply opening; introducing the reaction liquid into the reaction liquid quantifying channels by reverting the pressure inside the reaction containers, the reaction liquid quantifying channels and the reaction liquid introduction channel to a pressure outside the chip; removing the reaction liquid from the reaction liquid introduction channel; introducing into the reaction containers the reaction liquid in the reaction liquid quantifying channels, by centrifugal force; and carrying out a biological sample reaction process.
In this case, a reaction liquid is fed from the reaction liquid introduction channel into the reaction containers via the reaction liquid quantifying channels. Reactions using extremely small amounts of reaction liquid are made possible thereby, something that is difficult to achieve by pipette quantifying. The cost of reagents and so forth can be reduced when using small amounts reaction liquid. Also, reaction times are shortened considerably, which enhances processes efficiency. Moreover, reactions can take place in multiple reaction containers at a time, which allows conducting multiple tests and the like with good efficiency.
The reaction liquid is introduced into the reaction containers after having resided in the reaction liquid quantifying channels, whereby contamination between reaction containers can be prevented.
In the reduction of the pressure to the predetermined pressure, the pressure is preferably reduced to a pressure ranging from 50% of the pressure outside the chip to less than the pressure outside the chip.
That way, the reaction liquid is prevented from reaching the reaction containers during introduction of the reaction liquid into the reaction liquid quantifying channels. Also prevented is contamination across neighboring reaction containers, via the reaction liquid quantifying channels and the reaction liquid introduction channel, which occurs when certain reagents applied beforehand on the reaction containers leach out into the reaction liquid.
The biological sample reaction process may be a process including nucleic acid amplification, the reaction liquid may have a target nucleic acid, an enzyme for amplifying nucleic acid and nucleotides, at predetermined concentrations, and the reaction containers may be coated beforehand with primers.
When carrying out real-time PCR, fluorescent probes may be applied beforehand in the reaction apparatus.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A is a top-side view diagram illustrating the schematic constitution of a microreactor array according to Embodiment 1 of an aspect of the invention;
FIG. 1B is a cross-sectional diagram of FIG. 1A along line C-C;
FIG. 2 is a schematic diagram illustrating an example of a device for reducing pressure inside the microreactor array;
FIG. 3 is a schematic diagram illustrating another method of reducing pressure inside the microreactor array;
FIG. 4A , FIG. 4B , FIG. 4C , and FIG. 4D are schematic diagrams for explaining a method of filling a reaction liquid into the microreactor array; and
FIG. 5 is a diagram illustrating the schematic constitution of a centrifugation device that imparts centrifugal force on the microreactor array.
DESCRIPTION OF EXEMPLARY EMBODIMENTS
An embodiment of an aspect of the invention is explained below with reference to accompanying drawings.
Embodiment 1
FIG. 1A is a top-side view diagram illustrating the schematic constitution of a microreactor array (biological sample reaction chips) 10 according to Embodiment 1 of an aspect of the invention, and FIG. 1B is a cross-sectional diagram of FIG. 1A along line C-C. As illustrated in the figure, the microreactor array 10 has a transparent plate (first plate) 101 , a transparent plate (second plate) 102 , reaction container 103 , reaction liquid quantifying channels 104 , a reaction liquid introduction channel 105 , a reaction liquid supply opening 106 , and an evacuation opening 107 .
As illustrated in FIG. 1 , the microreactor array 10 is configured by the transparent plate 101 and the transparent plate 102 bonded together. The transparent plate 101 has formed therein the reaction container 103 , the reaction liquid quantifying channels 104 and the reaction liquid introduction channel 105 . The transparent plate 102 has formed therein the reaction liquid supply opening 106 and the evacuation opening 107 . The transparent plates 101 , 102 may be, for instance, resin plates.
The reaction container 103 are formed, for instance, to a circular shape having a diameter of 500 μm and a depth of 100 μm. The reaction liquid quantifying channels 104 and the reaction liquid introduction channel 105 are formed so that the cross section thereof perpendicular to the direction of reaction liquid flow is 100 μm wide and 100 μm deep. The reaction liquid quantifying channels 104 are formed to a length of 3 mm along the direction of reaction liquid flow. The volume of the reaction container 103 is smaller than the volume of the reaction liquid quantifying channels 104 . Preferably, the reaction container 103 , the reaction liquid quantifying channels 104 and the reaction liquid introduction channel 105 are subjected to a treatment that renders the inner wall surfaces thereof hydrophilic, in order to prevent bubble adhesion. Preferably, the inner wall surfaces of the reaction container 103 , the reaction liquid quantifying channels 104 and the reaction liquid introduction channel 105 are subjected to a surface treatment that inhibits nonspecific adsorption of biomolecules such as proteins. Also, the surfaces of the transparent plate 101 and the transparent plate 102 that come into contact with each other are preferably subjected to a surface treatment for imparting liquid repellency, with a view to preventing contamination across neighboring reaction container 103 during preliminary application of primers and fluorescent probes, necessary for PCR reactions, on the reaction container 103 .
A method of filling reaction liquid into the microreactor array 10 is explained next.
Firstly, as illustrated in FIG. 2 , the microreactor array 10 is placed in an airtight container 20 provided with a pressure gauge 23 , and then the pressure is reduced to 60 kPa by way of a vacuum pump 21 . Thereby, the pressure inside the microreactor array 10 (inside the reaction container 103 , the reaction liquid quantifying channels 104 and the reaction liquid introduction channel 105 ) is brought down to 60 kPa. A syringe pump 22 for reaction liquid filling is connected to the reaction liquid supply opening 106 of the microreactor array 10 . With the pressure in the airtight container 20 kept at 60 kPa, the reaction liquid is fed into the reaction liquid introduction channel 105 using the syringe pump 22 .
The reaction liquid includes a target nucleic acid, a polymerase and nucleotides (dNTPs) at predetermined concentrations suitable for reaction.
As the target nucleic acid there may be used, for instance, DNA extracted from biological samples such as blood, urine, saliva or spinal fluid, or cDNA reverse-transcribed from extracted RNA.
The primers may be present in the reaction liquid, although in the microreactor array of the present example the primers are applied beforehand on the reaction container 103 , where they are held in a dry state. Different primers may be applied on respective reaction container 103 , so that multiple PCR reactions can be carried out simultaneously.
Reduction of pressure in the microreactor array 10 may also be accomplished by directly connecting the vacuum pump 21 to the evacuation opening 107 , as illustrated in FIG. 3 , without resorting to an airtight container 20 such as the one illustrated in FIG. 2 .
Next, the pressure inside the microreactor array 10 is brought back to atmospheric pressure. At the stage in which reaction liquid is fed into the reaction liquid introduction channel 105 , the reaction liquid lingers in the reaction liquid introduction channel 105 without flowing into the reaction liquid quantifying channels 104 , as illustrated in FIG. 4A . The purpose of this is to balance capillary forces and atmospheric pressure in the reaction liquid quantifying channels 104 and the reaction container 103 connected thereto. When the pressure inside the microreactor array 10 is reverted to atmospheric pressure, a given amount V of reaction liquid flows from the reaction liquid introduction channel 105 into the reaction liquid quantifying channels 104 , as illustrated in FIG. 4B . The liquid amount V is the amount of reaction liquid that ultimately fills the reaction container 103 .
Herein, the relationship of equation (1) below holds-initially:
V /( V 1 +V 2)=( P 0 −Pc )/ P 0 (1)
wherein Pc denotes the set pressure (in this case 60 kPa) when the interior of the microreactor array 10 is evacuated, V 1 denotes the volume of the reaction container 103 , V 2 denotes the volume of the reaction liquid quantifying channels 104 , P 0 denotes the atmospheric pressure (≈100 kPa) and V denotes the amount of reaction liquid introduction from the reaction liquid quantifying channels 104 into the reaction container 103 .
The liquid amount V can thus be obtained from equation (2) below.
V =( V 1 +V 2)×( P 0 −Pc )/ P 0 (2)
Assuming P 0 =100 kPa, and since Pc=60 kPa, reaction liquid flows into each reaction liquid quantifying channel 104 in an amount of equivalent to 40% of the aggregate volume (V 1 +V 2 ) of the reaction container 103 and the reaction liquid quantifying channels 104 .
Preferably, the set pressure Pc ranges from 50% of the atmospheric pressure P 0 to less than the atmospheric pressure P 0 .
By setting thus the pressure Pc to range from 50% of the atmospheric pressure P 0 to less than the atmospheric pressure P 0 , the amount of liquid introduced from the reaction liquid introduction channel 105 into the reaction liquid quantifying channels 104 is no greater than 50% of the aggregate volume (V 1 +V 2 ) of the reaction container 103 and the reaction liquid quantifying channels 104 . Setting V 1 <V 2 , as described above, and keeping the amount of liquid flowing into the reaction liquid quantifying channels 104 within the above range has the effect of preventing the reaction liquid from reaching the reaction container 103 . If the reaction liquid flows into the reaction container 103 , the reagent applied beforehand in the reaction container 103 may leach out into the reaction liquid, which may result in contamination across neighboring reaction container 103 via the reaction liquid quantifying channels 104 and the reaction liquid introduction channel 105 .
Next, the reaction liquid remaining in the reaction liquid introduction channel 105 is suctioned off and removed using a syringe or the like, as illustrated in FIG. 4C . Subsequently, the reaction liquid supply opening 106 and the evacuation opening 107 are sealed with adhesive sheet or the like, and the microreactor array 10 is rotated using a centrifugation device 30 such as the one illustrated in FIG. 5 .
The microreactor array 10 is placed on a rotary table 31 of the centrifugation device 30 , as illustrated in FIG. 5 . Rotation of the centrifugation device 30 causes then centrifugal force to act in the microreactor array 10 , in the direction running from the reaction liquid quantifying channels 104 towards the reaction container 103 .
The reaction liquid in the reaction liquid quantifying channels 104 moves into the reaction container 103 as a result of the centrifugal force acting on the microreactor array 10 . The specific gravity of the air in the reaction container 103 is smaller than that of the reaction liquid, and hence the air in the reaction container 103 is pushed out into the reaction liquid introduction channel 105 via the reaction liquid quantifying channels 104 . Air is thus replaced with the reaction liquid, which fills as a result the reaction container 103 .
PCR (biological sample reaction treatment) is carried out then, once the reaction liquid is fed into the microreactor array 10 in accordance with the above procedure. To carry out the PCR process, the transparent plate 102 is fixed at a predetermined position and the microreactor array 10 is placed in a thermal cycler. PCR involves ordinarily repeating cycles that has each a step of denaturating double-stranded DNA at 94° C., a subsequent step of annealing with primers at about 55° C., and a step of replicating complementary strands, at about 72° C., using a thermostable DNA polymerase.
When real-time PCR is to be carried out in the microreactor array 10 , the inner walls of the reaction container 103 are coated beforehand with fluorescent probes and the primers used in the PCR reaction, with fluorescence intensity being measured at each cycle using a CCD sensor or the like. The amount of initial target nucleic acid is calculated and measured on the basis of the cycle at which a specific fluorescence intensity is reached. The method for carrying out real-time PCR is not limited to the above one. For instance, fluorescent probes may be rendered unnecessary when using a double-strand binding fluorescent dye such as SYBR(™) Green.
In Embodiment 1, thus, centrifugal force is used to feed reaction liquid into the reaction container 103 via the reaction liquid quantifying channels 104 . Reactions using extremely small amounts of reaction liquid are made possible thereby, something that is difficult to achieve by pipette quantifying. Moreover, the reactions can take place in multiple reaction container 103 at a time, which allows conducting multiple tests with good efficiency.
The reaction liquid is introduced into the reaction container 103 after having resided in the reaction liquid quantifying channels 104 , whereby contamination across reaction container 103 can be prevented.
In Embodiment 1, the microreactor array 10 is used in a reaction apparatus for real-time PCR, but may also be used for various reactions that utilize genetic or biological samples. For instance, the microreactor array 10 may be used in a process for detecting target proteins in a reaction liquid, by coating the reaction container 103 with, for instance, peptides (oligonucleotides) or proteins such as antigens, antibodies, receptors or enzymes that selectively capture (adsorb or bind to) specific proteins.
|
A biological sample reaction chip, including: a plurality of reaction containers; a reaction liquid introduction channel having a reaction liquid supply opening at a first end and an evacuation opening at a second end; and a reaction liquid quantifying channel, a third end of which is connected to one of the reaction containers, and a fourth end of which is connected to the reaction liquid introduction channel, wherein an interior of each of the reaction containers is coated with a reagent that is necessary for a reaction.
| 1
|
BACKGROUND OF THE INVENTION
The subject of this invention is a programmable cylinder lock, namely a lock comprising devices intended to allow providing the initial codification of the lock or, through a change operation, to modify the former lock codification in order to adjust the lock for being operated by a key different from the key to which the lock was formerly adapted.
More particularly, the invention concerns improvements in a kind of programmable cylinder lock which is known from the European Patents Nos. 0.226.252 and 0.900.310.
In a usual cylinder lock, which comprises a stator and a cylindrical rotor mounted inside the stator for rotation around its own axis and having a keyhole extending in the axis direction for the insertion of a key, a number of locking pins are mounted inside the rotor, movable perpendicularly to the axis on the extension of the keyhole plane, and each locking pin is intended to cooperate with a key segment whose codification is represented by the level of a tooth or recess of the key, situated within the considered segment. The fixed length of each locking pin is such that, when it cooperates with the corresponding segment of the correct key, the distal end of the locking pin corresponds to the cylindrical surface of the rotor and does not hinder its rotation, whereby, when all the locking pins are displaced in the respective correct positions by the correct key, the rotor can be rotated for operating the lock. When, on the contrary, one or more locking pins are situated in non correct positions, they (or the corresponding counterpins which may be provided in the stator) extend through the cylindrical rotor surface and hinder its rotation and therefore the lock operation. Because the codification of the lock is represented by the fixed length of the locking pins, that is defined during the manufacture step, the lock can be operated only by a single correct key and cannot be otherwise programmed.
The programmable cylinder locks of the kind considered in this invention and described in the mentioned patents comprise, in the rotor which is rotatably mounted inside the stator, instead of locking pins of a preestablished length, a number of key followers movable along their own longitudinal and transversal directions, said key followers being intended to cooperate with the codification conformations of a key inserted into the rotor keyhole, and a corresponding number of locking pins movable along their own longitudinal direction, which form the blocking members of the lock. The key followers and the locking pins form together a number of pairs each including a key follower and a locking pin, and they are provided with toothings intended to mutually cooperate, in different relative positions, in order to define the lock codification. A transversally displaceable stop bar cooperating with a longitudinal groove of the stator and having projections susceptible of cooperating with notches of the locking pins has the purpose of immobilizing the locking pins when the rotor is made to rotate within the stator and, as a consequence, the stop bar comes out of said groove and engages the locking pins. A change bar, which is transversally displaceable and is slidingly coupled with the key followers, normally keeps the key followers engaged with the locking pins but, when said change bar comes into said groove of the stator, it transversally displaces the key followers and disengages the same from the locking pins, thus allowing to modify the lock codification by means of the replacement of the former key by a different key.
In a lock of this kind it is required that the number of possible codification combinations, namely the number of different keys foreseen for the different locks of the same kind, be the higher possible. One of the parameters which determine the number of possible combinations is the number of codification levels that may be foreseen for the key segments, and this number depends on the pitch of the cooperating toothings of each pair of key followers and locking pins. The more small is this pitch, the more high is the number of possible codifications. However, the pitch of these toothings cannot be reduced below certain limits, on one hand because this would involve greater manufacture difficulties, and on the other hand because the engagement between the pairs of key followers and locking pins would no more have a sufficient mechanical strength.
SUMMARY OF THE INVENTION
The main object of this invention is to improve a lock of the considered kind in order to make up for the stated drawback, by allowing to increase the number of possible codifications levels without having recourse to a reduction of the pitch of the cooperating toothings of the key followers and the locking pins.
This object is attained according to the invention, in a lock of the considered kind, in that one of the two members, which compose at least some of the pairs each including a locking pin and a key follower, is provided with two parallel and adjacent toothings, each toothing having its pitch phase displaced with respect to the pitch phase of the other toothing, and in that at least one of said members which compose the pair including a locking pin and a key follower also has a limited mobility along the direction of the rotor axis, whereby said member is allowed to displace in such a way that the mutual engagement between both members may take place into the one or the other of said two toothings of one of the members forming the pair.
Thanks to this arrangement, the number of relative positions in which may be coupled the locking pins and the key followers forming the pairs is doubled, because in each case use can be made of the one or the other toothing, whose pitch are out of phase. In this manner, without reducing the toothing pitch, a number of codification combinations is obtained which corresponds to the number of codification combinations which could be obtained by halving the toothing pitch. It follows that the number of different keys which can be provided is increased without reducing either the manufacture ease or the mechanical strength of the lock.
Preferably, said two toothings, of the locking pin or of the key follower which together form a pair, are mutually phase displaced of a half of a pitch. In this manner there is obtained a uniform difference among the levels that may be provided by the alternate use of the two toothings.
Preferably, the member of each pair including a locking pin and a key follower, which has two toothings, is the locking pin, whereas the corresponding key follower has a single toothing.
Preferably, both members of each pair including a locking pin and a key follower have a limited mobility along the direction of the rotor axis.
It is of advantage that the teeth of the toothing of one of the members forming each pair including a locking pin and a key follower are provided with a bevel intended to render more easy the relative displacement of the members for mutually engaging the respective toothings.
In case, said teeth bevel can be foreseen for both the toothings of the key followers and of the locking pins.
The different features stated aim to obtain the maximum easy of engagement between the toothings of the pairs of locking pins and key followers.
It is of advantage that the key followers are provided, in the region in which they are slidingly coupled with the change bar, with an extension by means of which they are positively hooked to the change bar. In this way is prevented the possibility that the key followers take by chance any abnormal position capable of compromising a good lock operation.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other features, objects and advantages of the subject of the present invention will more clearly appear from the following description of an embodiment, being a not limiting example, with reference to the accompanying drawings, wherein:
FIG. 1 represents, for the purpose of reference, a cross section of a programmable cylinder lock known from the European Patent No. 0.900.310, in a condition of normal operation.
FIG. 2 shows a cross section corresponding to that of FIG. 1 , but in a condition of change.
FIG. 3 shows in perspective a locking pin of the lock according to the invention, which is provided with two toothings relatively out of phase.
FIG. 4 shows in perspective a key follower of the lock according to the invention.
FIG. 5 shows in perspective the locking pin according to FIG. 3 and the key follower according to FIG. 4 , relatively engaged.
FIG. 6 shows in perspective a portion of a rotor segment and of the key, with a pair comprising a locking pin and a key follower relatively engaged, in a first condition.
FIG. 7 is a plan view of the component parts represented in FIG. 6 .
FIG. 8 shows in perspective a portion of a rotor segment and of the key, with a pair comprising a locking pin and a key follower relatively engaged, in a second condition.
FIG. 9 is a plan view of the component parts represented in FIG. 8 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
At first, reference to FIGS. 1 and 2 will be made in order to recall the general structure and the operation of a lock of the considered kind, for whose particulars reference is made to the cited documents. Number 1 designates a stator inside which there is rotatably mounted a rotor 2 susceptible of receiving in its keyhole a key 3 . Inside rotor 2 are mounted a number of key followers 4 lying in a plane perpendicular to the axis of rotor 2 and having mobility along their own longitudinal and transversal directions. The key followers 4 are intended to cooperate with the codification conformations of key 3 . In addition, inside rotor 2 are mounted a corresponding number of locking pins 6 , each locking pin being coplanar with one of the key followers 4 and having mobility along its own longitudinal direction. In the shown case, the locking pins 6 cooperate with counterpins 8 and, together with them, form the blocking members of the lock. The key followers 4 have a toothing 5 , the locking pins have a toothing 7 , and these toothings are intended to mutually cooperate. This cooperation may take place in different relative positions, in order to determine the lock codification. A stop bar 9 is displaceable in a transverse direction within rotor 2 is susceptible to cooperate with a longitudinal groove 10 of stator 1 , has protrusions intended for cooperating with recesses of the locking pins 6 , and serves for immobilizing the locking pins 6 when rotor 2 is made to rotate within stator 1 and, as a consequence, the stop bar 9 comes out of said groove 10 and engages the locking pins 6 . A change bar 11 which is transversally displaceable in rotor 2 is slidingly coupled with the key followers 4 , and normally the change bar 11 keeps the key followers 4 engaged with the locking pins 6 as shown by FIG. 1 but, when said change bar 11 , due to a rotation of rotor 2 , comes to correspond to said groove 10 of stator 1 and penetrates therein, it transversally displaces the key followers 4 and disengages the same from the locking pins 6 , as shown by FIG. 2 . Then, by means of the replacement of the former key 3 by a different key, it is possible to modify the lock codification.
As it may be remarked, the pitch of toothings 5 and 7 , which determines the possible positions for the lock codification, is not very small, and it cannot be reduced at will because this reduction would involve some manufacture difficulties and a weakening of the engagement between key followers and locking pins. This fact limits the possibility of increasing the number of possible codification positions and, therefore, the number of different keys which can be provided for a lock of this kind.
As already stated, according to the invention one of the two component parts of at least some of the pairs comprising a locking pin and a key follower, preferably the locking pin, is provided with two parallel adjacent toothings, each of these toothings having its pitch phase displaced with respect to the pitch phase of the other toothing. This feature appears in particular from FIG. 3 . As it may be observed, the locking pin 6 , for the remaining substantially conforming the known shapes, instead of having a single toothing 7 , has two parallel adjacent toothings 7 a and 7 b , and the pitches of these two toothings are mutually phase displaced. In the shown example, the phase displacement amounts to a half of a pitch, and this is the preferred condition.
The key follower 4 represented in FIG. 4 has as customary a single toothing 5 . According to the position of the key follower 4 with respect to the locking pin 6 , this toothing 5 is susceptible of engaging the toothing 7 a or the toothing 7 b of the locking pin. For example, according to FIG. 5 , the toothing 5 of the key follower 4 engages the toothing 7 b of the locking pin 6 . Because the two toothings 7 a and 7 b are mutually displaced by a half of a pitch, it ensues that the possible relative positions of the key follower 4 and the locking pin 6 do not differ, as usually, by a toothing pitch, but only by a half of a pitch. Therefore, being equal all other conditions and without any reduction of the toothing pitch, the number of possible relative positions of each key follower with respect to the corresponding locking pin is doubled. Therefrom ensues a very great increase of the number of possible codification combinations of the lock and of the corresponding key.
In order that the key followers 4 , when they are approached to the corresponding locking pins 6 when programming the lock, can engage as needed the one or the other of the toothings 7 a and 7 b , a relative displacement should be allowed between the key followers 4 and the locking pins 6 in the direction of the axis of rotor 2 . For this reason, according to the invention, it is needed that at least one of said two members, the key follower 4 and the locking pin 6 , which compose each pair, has a limited mobility along the direction of the rotor axis, whereby it can displace in such a way that the mutual engagement of the two members takes place as needed in the one or the other of said two toothings of one of the involved component parts. This mobility can be assigned indifferently to the key followers 4 or to the locking pins 6 , but it is preferable that this mobility is assigned to both said component parts, whereby its extension can be reduced in a corresponding way.
If this is considered suitable, said displacement (which however aims spontaneously taking place) may be favored by a light bevel of the teeth of some toothings of the one or the other or both the component parts. This bevel is represented in 5 a in FIG. 4 for the teeth of the key follower 4 .
In the example shown and described, the double toothing 7 a , 7 b has been assigned to the locking pins 6 , whereas the key followers 4 have a single toothing 5 . However it is to be remarked that the same behavior can be obtained by providing a double toothing on the key followers and a single toothing on the locking pins. The selection between these two possibilities can be imposed by a preference of the designer or by a manufacture advisability.
A further clarification of the behavior of the distinctive component parts of the invention is given by FIGS. 6 to 9 , wherein it is supposed that the limited displacement along the direction of the axis of rotor 2 is allowed both to the key followers 4 and to the locking pins 6 . FIGS. 6 and 7 refer to the case in which a key follower 4 is engaging the toothing 7 b of a locking pin 6 , whereas FIGS. 8 and 9 refer to the case in which a key follower 4 is engaging the toothing 7 a of a locking pin 6 . Of course, the one or the other of these cases takes place according to the fact that, in the position in which the key 3 has brought the key follower 4 , the pitch of toothing 5 of the key follower 4 corresponds to the pitch of either one or the other of the toothings 7 a and 7 b of the locking pin 6 .
In the case of FIGS. 6 and 7 , the key follower 4 displaces along the direction of the axis of rotor 2 in the sense of arrow F 1 , whereas at the same time the locking pin 6 displaces in the direction of the axis of rotor 2 in the opposite sense, according to arrow F 2 , whereby the toothing 5 of the key follower 4 aligns with the toothing 7 b of the locking pin 6 and can engage the same.
On the contrary, in the case of FIGS. 8 and 9 , the key follower 4 displaces along the direction of the axis of rotor 2 in the sense of arrow F 3 , whereas at the same time the locking pin 6 displaces in the direction of the axis of rotor 2 in the opposite sense, according to arrow F 4 , whereby the toothing 5 of the key follower 4 aligns with the toothing 7 a of the locking pin 6 and can engage the same.
It is to be remarked that the senses of the two arrows F 1 and F 3 according to which displaces the key follower 4 are opposite in the two cases shown, and like this are opposite in the two cases the senses of the two arrows F 2 and F 4 according to which displaces the locking pin 6 .
It is of advantage that the key followers 4 , as it may be observed in FIGS. 4 and 5 , have an extension 4 a in the region in which they are slidingly coupled with the change bar 11 . By means of the extension 4 a the key followers 4 are positively hooked to the change bar 11 . In this way is prevented the possibility that the key followers, due to their mobility, may take by chance some abnormal position capable of compromising a good lock operation.
Thanks to the application of the invention becomes possible a great increase of the number of possible codification combinations of the lock, and therefore of the possible number of different keys, without resorting to a reduction of the toothing pitch of the component parts, and therefore without causing particular manufacture difficulties or any weakening of the component parts.
All the described features may be applied to all the pairs comprising a key follower and a locking pin of the lock or even, for the reason of simplification, only to some pairs, by accepting in this case a reduction of the extent of advantages offered by the invention.
The characteristics of the invention may be applied to the stated kind of locks, irrespective of they being provided with master keys or not.
It should be understood that this invention is not limited to the embodiment described and shown as an example. Several possible modifications have been pointed out in the course of the description, and others are within the ability of those skilled in the art. These modification and others, and any replacement by technically equivalent means, can be made to what has been described and shown, without departing from the spirit of the invention and the scope of this Patent as defined by the appended Claims.
|
A programmable cylinder lock includes a stator and a cylindrical rotor, mounted therein for rotation around its own axis and having a keyhole, a number of key followers movable along their own longitudinal and transversal directions, intended to cooperate with a key inserted into the keyhole, a number of locking pins movable along their own longitudinal direction, the key followers and locking pins forming together a number of pairs and having toothings cooperating to define the lock codification, the rotor including a stop bar cooperating with a longitudinal groove of the stator and having projections cooperating with notches of the locking pins to immobilize them when the stop bar engages them, and a change bar slidingly coupled with the key followers to normally keep them engaged with the locking pins and to disengage them therefrom when the change bar provides a lock programming position.
| 8
|
PRIORITY CLAIM
[0001] This application is a Continuation In Part Application, claiming the benefit of priority to non-provisional application Ser. No. 10/651,530, filed in the United States on Aug. 29, 2003, and titled “Emission Bag”.
FIELD OF INVENTION
[0002] The present invention relates to a barrier, and more particularly, to an emission bag where a user coughs or sneezes into the emission bag, with the emission bag acting as a barrier such that pathogens ejected from a nose or mouth will be confined to an interior of the emission bag. Additionally, the emission bag has small perforations that are medicated with an anti-septic, such that emissions are sterilized upon passing through the small perforations.
BACKGROUND OF INVENTION
[0003] Pathogens are often transmitted through fluid droplets, such as mucous, saliva, and nasal secretions. Projected through a cough or sneeze, the droplets act as carriers, transferring the pathogen from one individual to another. A single cough may produce anywhere from a few hundred to several thousand droplets, each potentially contaminated with pathogens. Contrasted with a sneeze, a sneeze may produce anywhere from a few hundred to a few million droplets. While some of the droplets produced by a sneeze may be large enough to immediately fall to the floor, others evaporate, forming residues of “droplet nuclei” which may remain airborne for hours or even days.
[0004] Preventing transmission of pathogens is often accomplished through use of barriers. The barriers are used to prevent the droplets from transferring to one's hand or from becoming airborne. The barriers take form as rubber gloves, handkerchiefs, tissues, and mitts. While effective in a sterile setting such as a hospital, rubber gloves are impractical for daily use. If an individual were to sneeze or cough, she would unlikely place a rubber glove over her hands before sneezing into them. While more practical than rubber gloves, handkerchiefs and tissues do little to prevent contamination of the hands since the microorganisms progress through the barrier from one site to another.
[0005] In an attempt to prevent contamination of the hands, a few inventors have created mitts with impervious layers. As disclosed in U.S. Pat. Nos. 5,196,244 and 5,864,883, to Beck and Reo respectively, a mitt-like bag couples an impervious inner layer with an absorbent external layer. As disclosed in Beck and Reo, a user inserts her hand into the mitt-like bag and proceeds to blow her nose, sneeze, or cough onto the absorbent external layer of the mitt-like bag. The user then turns the mitt-like bag inside-out, sealing any pathogens on a now interior portion.
[0006] Although the mitt-like bags are successful in preventing contamination of the hands, they are not entirely successful in preventing pathogens from becoming airborne. When sneezing directly onto the absorbent external layer of the mitt-like bag, it is likely that pathogens will escape. Additionally, because of the impervious inner layer, if a user were to sneeze directly into an internal portion of the mitt-like bag, air would quickly fill the mitt-like bag and cause a blow-back of pathogens onto the user's face.
[0007] Therefore, there exists a need to present a bag where a user may sneeze or cough directly into an internal portion of a sealable bag, the bag being such that it allows air to pass through the bag, while keeping droplets and pathogens in the internal portion. Additionally, because sneezes and coughs often come unexpectantly, it is desirable that the bag be small and portable, allowing a user to carry one bag or a package of several bags. In this regard, the present invention substantially fulfills this need.
SUMMARY OF INVENTION
[0008] The present invention comprises an emission bag for covering a nose and mouth in such a manner that pathogens transmitted from the nose and mouth will be confined to an interior of the emission bag. The emission bag comprises a piece of material with an opening; and a bag attached with the piece of material and opening, such that an entrance to an interior of the emission bag is through the opening.
[0009] In another aspect, a top film is attached with the emission bag, such that manipulating the top film exposes the opening. Additionally, a bottom film is attached with a bottom portion of the piece of material, whereby manipulating the bottom film exposes the bag. In another aspect, the bottom film may also be attached with an exterior surface of the bag, such that pulling on the bottom film pulls open the bag and extends the bag away from the opening.
[0010] In another aspect, the piece of material is constructed from a material selected from a group consisting of plastic, metal and paperboard. Additionally, the piece of material may have perforations, allowing it to fold along the perforations and thereby create two opposing sides.
[0011] In yet another aspect, the piece of material has an enclosure apparatus, such that when the piece of material is folded along the perforations, the enclosure apparatus on the two opposing sides come into contact with each other and thereby seal the emission bag. The enclosure apparatus is selected from a group consisting of adhesive tabs, tape, Velcro, glue, and twist-ties.
[0012] Additionally, the bag is constructed of a material selected from a group consisting of plastic, paper and cloth.
[0013] In another aspect, the bag has small perforations allowing the bag to breathe. The small perforations are medicated with an anti-septic on the interior of the bag, such that emissions are sterilized upon passing through the small perforations.
[0014] Furthermore, the bag has an entrance and a base and the entrance has an area and the base has an area, where the area of the entrance is smaller than the area of the base.
[0015] Finally, a wet napkin may be placed within the interior of the bag and may further be medicated.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The nature of the emission bag described herein will be readily apparent in the following drawings, in which:
[0017] FIG. 1 is a top perspective view of the present invention, showing a piece of material with an opening;
[0018] FIG. 2A is a cross-sectional view of the present invention, taken from line II-II of FIG. 1 , showing the piece of material with a top film and a bottom film attached thereto;
[0019] FIG. 2B is a cross-sectional view of the present invention, taken from line II-II of FIG. 1 , showing an emission bag attached with the piece of material; and
[0020] FIG. 3 is a cross-sectional view of the present invention, taken from line II-II of FIG. 1 , showing the piece of material being folded, with two opposing sides coming into contact with each other and thereby sealing the emission bag.
[0021] FIG. 4 is a cross-sectional view of the present invention, taken from line II-II of FIG. 1 , showing a wet napkin placed within the bag.
DETAILED DESCRIPTION
[0022] The present invention relates to a barrier, and more particularly, to an emission bag where a user coughs or sneezes into the emission bag, with the emission bag acting as a barrier such that pathogens transmitted from a nose or mouth will be confined to an interior of the emission bag. Additionally, the emission bag has small perforations that are medicated with an anti-septic, such that emissions are sterilized upon passing through the small perforations. An inherent advantage of this invention is that it is small and portable, allowing a user to carry a single emission bag or a package containing several emission bags.
[0023] The following description, taken in conjunction with the referenced drawings, is presented to enable one of ordinary skill in the art to make and use the invention. Various modifications will be readily apparent to those skilled in the art, and the general principles defined herein may be applied to a wide range of aspects. Thus, the present invention is not intended to be limited to the aspects presented, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein. Furthermore it should be noted that unless explicitly stated otherwise, the figures included herein are illustrated diagrammatically and without any specific scale, as they are provided as qualitative illustrations of the concept of the present invention.
[0024] Referring to the figures, FIG. 1 illustrates an aspect of the emission bag 100 as piece of material 102 with an opening 104 . The piece of material 102 may be constructed of any suitably semi-rigid material, non-limiting examples of which include plastic, metal and paperboard. For example, the piece of material 102 may be a planar board constructed of paperboard, with the opening 104 as a hole in the planar board. Furthermore, the piece of material 102 may be any suitably portable size, a non-limiting example of which includes Five and one-half inches long by four and one-half inches wide with a thickness of five-ply. Additionally, the piece of material 102 may be comprised of a single layer or multiple layers. The opening 104 may be any suitable size and shape, a non-limiting example of which includes a circular opening with a diameter of two and one-half inches. The piece of material 102 has perforations 106 running from one side of the piece of material 102 to the other, allowing it to fold along the perforations 106 and thereby creating two opposing sides 108 . The number of perforations 106 may be any suitable number allowing the piece of material 102 to be folded, a non-limiting example of which includes three on each side of the opening 104 . Furthermore, the size of the perforations 106 may be any suitable size allowing the piece of material 102 to be folded, a non-limiting example of which includes fourteen gauge holes.
[0025] An enclosure apparatus 110 is attached with the piece of material 102 , such that when the piece of material 102 is folded along the perforations 106 , the enclosure apparatus 110 on the two opposing sides 108 come into contact with each other and thereby seal the emission bag 100 . The enclosure apparatus 110 may be any suitable apparatus for affixing two mediums together, non-limiting examples of which include adhesive tabs, tape, Velcro, glue, and twist-ties.
[0026] As illustrated in FIG. 2A , a top film 200 is attached with the emission bag 100 , such that the top film 200 needs to be peeled off or otherwise manipulated in order to expose the opening 104 . The top film 200 may be attached with the emission bag 100 through any suitable means for affixing two mediums together, non-liming examples of which include staples, tape, adhesive and being in-sewn. The top film 200 may be any suitable size to cover the opening 104 , a non-limiting example of which includes being five and one-half inches long by four and one-half inches wide. Additionally, the top film 200 may be attached with the enclosure apparatus 110 or attached with the piece of material 102 . Furthermore, the top film 200 may be constructed of any suitable material for covering the opening 104 , non-limiting examples of which include a flexible clear plastic film, and paperboard.
[0027] Attached with a bottom portion 202 of the piece of material 102 , is a bottom film 204 . The bottom film 204 may be attached with the bottom portion 202 of the piece of material 102 through any suitable means for affixing two mediums together, non-liming examples of which include staples, tape, adhesive and being in-sewn. The bottom film 204 may be removed or otherwise manipulated to expose a bag 206 , allowing the bag 206 to be extended from the piece of material 102 . In addition to being attached with the piece of material 102 , the bottom film 204 may be optionally attached with an exterior surface of the bag 206 , such that pulling on the bottom film 204 pulls open the bag 206 and extends the bag 206 away from the opening 104 . The bottom film 204 may be constructed of any suitable material for covering or protecting the bag 206 , non-limiting examples of which include a flexible clear plastic film, and paperboard. When paperboard, a piece of plastic would be attached in a center of the bottom film 204 to help prevent any medication from drying out.
[0028] As illustrated in FIG. 2B , the bag 206 is attached with the piece of material 102 and opening 104 , such that an entrance to an interior 208 of the bag 206 is through the opening 104 . The bag 206 may be attached with the piece of material 102 through any suitable means for affixing two mediums together, non-limiting examples of which include staples, tape, adhesive, in-sewn, and being compressed between multiple layers of the piece of material 102 . The bag 206 may be constructed of any suitable material for constructing a bag, non-limiting examples of which include plastic, paper and cloth. The bag 206 has small perforations 210 , allowing the bag 206 to breathe, such that when a user sneezes or coughs into the bag 206 , air is allowed to pass through the small perforations 210 . The number of small perforations 210 may be any suitable number to allow the bag 206 to breathe, a non-limiting example of which includes five perforations. Additionally, the size of the small perforations 210 may be any suitable size to allow the bag 206 to breathe, a non-limiting example of which includes a diameter of one millimeters. Furthermore, the small perforations 210 are medicated with an anti-septic, such that emissions are sterilized upon passing through the small perforations 210 from an interior 208 of the bag 206 to an exterior 212 of the bag 206 . Additionally, the bag 206 may be any suitable size or shape, a non-limiting example of which includes five and one-half inches wide by seven inches long. In another example, the bag 206 has an entrance 214 and a base 216 , where an area of the entrance 214 may be smaller than an area of the base 216 . Furthermore, the bottom film 204 may optionally be attached with the bag 206 , such that pulling on the bottom film 204 pulls open the bag 206 .
[0029] As illustrated in FIG. 3 , the emission bag 100 may be sealed, containing any pathogens inside. When the piece of material 102 is folded along the perforations 106 , the two opposing sides 108 are brought together. When the two opposing sides 108 are brought together, the enclosure apparatus 110 on the two opposing sides 108 come into contact with each other and thereby seal the emission bag 100 . When sealed, any pathogens are trapped in the interior 208 of the bag 206 .
[0030] Illustrated in FIG. 4 is the emission bag 100 with a wet napkin 400 . In this aspect, the emission bag 100 contains a wet napkin 400 placed within the interior 208 of the bag 206 . The wet napkin 400 may be constructed of any suitable material for creating a napkin, non-limiting examples of which include paper and cloth. Additionally, the wet napkin 400 may be any suitable size and thickness, a non-limiting example of which includes being six inches wide by eight inches long, and with a thickness of two-ply. Further, the wet napkin 400 may be medicated with an anti-septic or any other suitable medication. Placement of the wet napkin 400 within the interior 208 of the bag 206 will help to reduce the drying out of the anti-septic associated with the small perforations 210 . Additionally, the wet napkin 400 may be used to wipe ones nose or mouth after a cough or sneeze and thereafter sealed within the interior 208 of the bag 206 .
|
The present invention relates to a barrier, and more particularly, to an emission bag where a user coughs or sneezes into the emission bag, with the emission bag acting as a barrier such that pathogens transmitted from a nose or mouth will be confined to an interior of the emission bag. The emission bag has small perforations allowing it to breathe, so that when a user coughs or sneezes into the emission bag, it doesn't immediately fill full of air and cause a blow-back of the pathogens onto a user's face. Additionally, the small perforations are medicated with an anti-septic, such that emissions are sterilized upon passing through the small perforations.
| 0
|
RELATIONSHIP TO OTHER APPLICATIONS AND PATENTS
[0001] The present application is a Continuation-In-Part of a pending application, Ser. No. 10/442,583, filed May 21, 2003; which is a Continuation-In-Part of an allowed application, Ser. No. 09/883,718 filed Jun. 18, 2001, now matured as U.S. Pat. No. 6,576,145; which is a Continuation-In-Part of an allowed application, Ser. No. 09/451,293 filed Nov. 30, 1999, now matured as U.S. Pat. No. 6,251,290; which is a Continuation-In-Part of an allowed application, Ser. No. 09/304,377 filed May 4, 1999, now matured as U.S. Pat. No. 6,096,227; which is a Continuation-In-Part of an allowed application, Ser. No. 08/971,514 filed Nov. 17, 1997, now matured as U.S. Pat. No. 5,928,522; which is a Continuation-In-Part of an allowed application, Ser. No. 08/807,643 filed Feb. 27, 1997, now matured as U.S. Pat. No. 5,797,701; the relevant disclosures of all of which being herein incorporated by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to methods and apparatus for recovering useful liquid and gaseous hydrocarbons from both naturally-occurring and man-made mixtures of hydrocarbons and mineral substrates; more particularly to methods and apparatus for processing hydrocarbon-containing geologic ores, including tar sands, oil sands, oil sandstones, oil shales, and petroleum-contaminated soils, to recover petroleum-like hydrocarbons, and especially bitumen, kerogen, and/or crude oil, therefrom and to render the mineral substrate residues suitably low in hydrocarbons, acids, and bases for environmentally-acceptable disposal; and most particularly to a method and apparatus for separating bitumen from particulates in tar sand and oil sand grains, using hydrogen peroxide. As used hereinafter, the term “tar sands” shall be taken to mean any or all of the above hydrocarbonaceous ores.
BACKGROUND OF THE INVENTION
[0003] As used herein, hydrocarbonaceous deposit is to be taken to include tar sands, oil sands, oil sandstones, oil shales, and all other naturally-occurring geologic materials having hydrocarbons contained within a generally porous rock-like inorganic matrix. The matrix may be loose, friable, or indurate. The hydrocarbons may be in direct contact with the mineral substrate or may be separated therefrom by a third material, for example, water. Contaminated soil is to be taken to include soils which have been impregnated with hydrocarbons, as is known to occur in petroleum drilling, well operating, storage, refining, transport, and dispensing processes.
[0004] Tar sands are naturally-occurring geological formations found in, for example, Canada (Alberta) and the United States (Wyoming). Such sands have potential for yielding large amounts of petroleum. Tar sands are porous, generally loose or friable, and typically contain substantial amounts of clay and have the interstices filled with high-viscosity hydrocarbons known generally in the art as bitumen. In addition, particles of clay or sand are surrounded typically by bitumen to form discrete grains. Most of these tar-like bituminous materials are residues remaining after lighter (lower molecular weight) hydrocarbons have escaped through geologic mechanisms over geologic time or have been degraded through the action of microorganisms, water washing, and possibly inorganic oxidation.
[0005] Very extensive tar sand deposits occur in northern Alberta, Canada along the Athabasca River and elsewhere. Tar sand layers in this area may be more than 60 meters thick and lie near the surface over a total area of about 86,000 km 2 . They are estimated to contain a potential yield in excess of 1.6 trillion barrels of oil.
[0006] Oil shales are related to oil sands and tar sands; however, the substrate is a fine-grained laminated sedimentary rock typically containing an oil-yielding class of organic compounds known as kerogen. Oil shale occurs in many places around the world. Particularly kerogen-rich shales occur in the United States, in Wyoming, Colorado, and Utah, and are estimated to contain in excess of 540 billion potential barrels of oil.
[0007] Hydrocarbons recoverable from tar sands and oil shales may comprise, but are not limited to, bitumen, kerogen, asphaltenes, paraffins, alkanes, aromatics, olefins, naphthalenes, and xylenes.
[0008] In the known art of petroleum recovery from hydrocarbonaceous deposits, the high molecular weight bituminous or kerogenic material may be driven out of the sands, sandstones, or shales with heat. For example, in a known process for recovering kerogen from oil shale, crushed shale is heated to about 480° C. to distill off the kerogen which is then hydrogenated to yield a substance closely resembling crude oil. Such a process is highly energy intensive, requiring a portion of the process output to be used for firing the retort, and thus is relatively inefficient. Also, a significant percentage of the kerogen may not be recovered, leaving the process tailings undesirable for landfill.
[0009] Other known processes, for recovering bitumen from tar sands for example, require the use of caustic hot water or steam. For example, a process currently in use in Canada requires that a hot aqueous slurry of tar sand be mixed with high concentrations of aqueous caustic soda to separate the bitumen from the sand grains and to fractionate the bitumen into lower molecular weight hydrocarbons which may then be separated from the mineral residues and refined further like crude oil.
[0010] This process has several serious shortcomings. First, it is relatively inefficient, typically recovering 70% or less of the hydrocarbons contained in the sands. “Free” hydrocarbons, that is, compounds mechanically or physically contained interstitially in the rock, may be recovered by this process; but “bound” hydrocarbons, that is, compounds electrostatically bound by non-valence charges to the surface of clays or other fines having high electronegative surface energy, are not readily released by some prior art processes. In fact, high levels of caustic may actually act to inhibit the desired release of organic compounds from such surfaces and are known to emulsify released bitumen with water, forming a stable colloid and making later separation of bitumen from water very difficult. Thus, the prior art process is wasteful in failing to recover a substantial portion of the potential hydrocarbons, and the mineral substrate residue of the process may contain substantial residual hydrocarbon, making it environmentally unacceptable for landfill. Typically, the aqueous colloidal tailings of prior art processes require ponding, sometimes for years, to permit separation of water from the suspended and entrained particles. The volumes and surface areas of such ponds in Alberta are enormous.
[0011] Second, the wet sand and clay residues can be caustic and may not be spread on the land or impounded in lagoons without extensive and expensive neutralization.
[0012] Third, the caustic aqueous residual may contain high levels of dissolved petroleum, which is non-recoverable and also toxic in landfill. Such residual also has a high Chemical Oxygen Demand (COD), making ponds containing such residual substantially anoxic and incapable of supporting plant or animal life and highly dangerous to waterfowl.
[0013] Fourth, oils recovered by the prior art process typically have high levels of entrained or suspended fine particulates which must be separated as by gravitational settling, filtration, or centrifugation before the oils may be presented for refining. These particulates may be emulsified with the oils and can be extremely difficult to separate out.
[0014] Fifth, the present-day cost of oil recovered from Albertan tar sands by prior art process may require a substantial governmental subsidy to match the world spot price of crude oil.
[0015] Sixth, the process is highly sensitive to natural oxidation of ores, being most successful on freshly-mined ores which have not been weathered nor exposed for long to atmospheric conditions. Exposure to air for only a few days can render the ores untreatable by this method.
[0016] Alternatively, it is known to use hydrogen peroxide in an aqueous slurry to separate bitumen from mineral particulates in a tar sand or oil sand.
[0017] Canadian Patent Application No. 2,177,018 (“'018”), laid open for public inspection Nov. 22, 1997, and abandoned Dec. 21, 2000, discloses a batch process for separating oil and bitumen from sand by mixing sand and water in a tank to form an aqueous slurry; adding a water solution of hydrogen peroxide to the aqueous slurry; agitating the slurry containing the hydrogen peroxide; skimming an upper froth layer containing oil and bitumen; and removing a lower clean sand layer and a middle clean water layer from the tank.
[0018] The disclosed process is relatively slow and low in capacity. Mechanical agitation of the slurry is relatively low, being provided specifically by injection of gas bubbles through an air injection assembly. Use of a mechanical mixer, for example, is not suggested. Hydrogen peroxide is taught as “a catalyst initiating a vigorous reaction.” For overall speed, the process relies on the rate at which the hydrogen peroxide attacks the tar sand granules, separating the slurry into “an upper froth layer, a middle clean water layer, a lower clean sand layer, and a clay layer.” The disclosed process does not teach or suggest that vigorous mechanical agitation and/or substantially elevating the temperature above 45° C. may accelerate the process or increase the overall yield.
[0019] U.S. Pat. No. 6,576,145, issued Jun. 10, 2003, discloses a continuous process for separating hydrocarbons from a mixture of hydrocarbons and a particulate mineral substrate by feeding a predetermined amount of the mixture into a mixing vessel; adding a predetermined amount of water to the mixture to form an aqueous slurry; tempering the slurry to about 80° C.; adding a predetermined amount of aqueous hydrogen peroxide to the heated slurry; agitating the heated slurry containing the hydrogen peroxide by passing the slurry through a linear oxidation vessel at a low axial velocity and a high radial and rotational velocity to release hydrocarbons from the mineral substrate and to reduce the molecular weight of some of the hydrocarbons; and passing the slurry through a separator wherein the mineral substrate is separated from the water and the hydrocarbons also are separated from the water.
[0020] The disclosed method improves upon the disclosure of '018 in three ways: first, by recognizing the benefit of elevating temperature substantially above 45° C., which greatly enhances bitumen recovery by reducing viscosity and also speeds up the reaction of hydrogen peroxide; and second, by recognizing the benefit of a continuous process using a plurality of specialized, linked vessels; and third, by recognizing the importance of intense mechanical shear in assisting attack on the sand grains by hydrogen peroxide.
[0021] However, this patent does not disclose or suggest, however, that a period of intense shear of the slurry prior to addition of the hydrogen peroxide may be beneficial in shortening the required reaction time and thus increasing throughput.
[0022] Further, this patent disclosure purports that an important element in separation of bitumen from mineral grain is oxidation and chain-breaking of the bitumen compounds by the peroxide.
[0023] Further, this patent disclosure relies primarily on gravitational separation of the separated reaction products by density difference between bitumen and sand or clay particulates relative to water.
[0024] Further, this patent disclosure teaches to add aliquots of aqueous hydrogen peroxide at a plurality of locations along the flowpath of the slurry.
[0025] It is a principal object of the invention to provide an improved process for recovering hydrocarbons from tar sand and oil sand deposits in greater than 90% yield.
[0026] It is a further object of the invention to provide an improved process for recovering hydrocarbons from such deposits in greater than 99% yield.
[0027] It is a still further object of the invention to provide an improved recovery process which yields higher throughput rates than those of prior art processes.
[0028] It is a still further object of the invention to provide an improved recovery process wherein physical separation of bitumen globules from mineral particulates is assisted by preferential flotation of the bitumen globules.
[0029] It is a still further object of the invention to provide an improved recovery process which is substantially less expensive to operate on a per-unit of ore basis than are known treatment processes.
SUMMARY OF THE INVENTION
[0030] Briefly described, individual grains in an oil-sand or tar-sand ore typically comprise an envelope of bitumen surrounding a mineral substrate particle of clay or sand. In so-called “water wet” ores, a thin water layer is present between the bitumen envelope and the substrate particle. In “oil wet” ores, a water layer is absent or nearly so. As used hereinafter, the term “bitumen” should be understood to mean bitumen itself and, for simplicity in discussion herein, all other hydrocarbonaceous materials including but not limited to kerogen, asphaltenes, paraffins, alkanes, aromatics, olefins, naphthalenes, and xylenes.
[0031] In a bitumen-recovery process in accordance with the invention, the ore is preliminarily screened to eliminate rocks or plant materials which may have been included from the soil overburden of the ore deposit. The screened ore is mixed with water to form a slurry which is heated to about 80° C. or higher. The type of water is non-critical and may include fresh water, salt water, seawater, tailing pond water, recycled process water, and combinations thereof. The hot slurry is strongly agitated at high liquid shear rates, preferably exceeding slurry average velocities of 5 meters per second, for at least one minute and preferably for several minutes, by which action the bitumen envelope is mechanically thinned, distorted, and ultimately fractured, exposing the water layer and/or mineral grain within. Subsequent to the intense shear step, an aqueous solution of hydrogen peroxide is added to the slurry, and agitation is maintained sufficient to rapidly disperse the hydrogen peroxide throughout the slurry. The hydrogen peroxide enters the bitumen envelope through the previously-formed fractures and reacts with the surface of the mineral substrate to reduce wettability of the substrate to hydrocarbons. The hydrogen peroxide is thereby decomposed to oxygen and water, generating free oxygen gas which coalesces into small bubbles attached preferentially to the bitumen envelope. As more oxygen gas is liberated, bubbles continue to form and to expand in the space within the bitumen envelope between the envelope and the substrate, eventually rupturing the envelope and allowing the substrate particle to become separated therefrom. After separation, the particle has a negative buoyancy in the rapidly-degenerating slurry and begins to settle, whereas the bitumen globules with O 2 bubbles attached are quite positively buoyant and rise to the surface where they form a skimmable froth. Both free interstitial hydrocarbons and those hydrocarbons bound electrostatically to the particles are released from the mineral substrate and separated by such oxygen flotation. In general, flocculants or gas sparging in the settling tank are not required to effect excellent separation. The water and rock tailings from the process are substantially free of hydrocarbon contamination and are environmentally suitable for disposal.
[0032] In a further preferred embodiment, the only wastewater from the process is the water contained in the wet tailings of sand and clay. The remainder of the separated water may be recycled into the mixing stage at the head end of the process. The separated sand can provide excellent filtration of clay particles from water being recycled. Such sand filtration is also environmentally beneficial in restoring the original sand/clay relationship to mineral residues eventually landfilled.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] The foregoing and other objects, features, and advantages of the invention, as well as presently preferred embodiments thereof, will become more apparent from a reading of the following description in connection with the accompanying drawings, in which:
[0034] [0034]FIG. 1 is a simplified schematic flowpath of a continuous process for recovering hydrocarbons from hydrocarbonaceous ores or soils in accordance with the invention; and
[0035] [0035]FIG. 2 is a more detailed schematic flowpath of the basic process shown in FIG. 1;
[0036] [0036]FIG. 3 is a more detailed view of a first stage shearing and separating device shown in FIG. 2;
[0037] [0037]FIG. 4 is an elevational cross-sectional view taken along line 4 - 4 in FIG. 3;
[0038] [0038]FIG. 5 is a graph relating bitumen recovery rate as a function of various process aids;
[0039] [0039]FIG. 6 is a bar graph showing relative wetting index of sand solids by 1-propanol without and with prior treatment of the sand with hydrogen peroxide;
[0040] [0040]FIG. 7 is graph showing decomposition rates of hydrogen peroxide in the presence of oil sand, sand, clay, and bitumen; and
[0041] [0041]FIG. 8 is a schematic diagram showing the sequence of states and events by which the process of the invention is believed by the inventors to proceed.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0042] Since ore volumes to be treated can be relatively large, it is preferable to configure the process for continuous throughput, although semi-continuous and batch systems are within the scope of the invention and all such processes may be configured of known apparatus without undue experimentation or further invention. A continuous throughput process in accordance with the present invention is described below.
[0043] The hydrogen peroxide-based process as disclosed in herein incorporated U.S. Pat. No. 6,576,145 ('145) forms the basis for an improved process as described herein for treatment of tar sands and oil sands to more simply and economically recover a high percentage of the hydrocarbon content therefrom.
[0044] Referring to FIGS. 1 through 4, in a hydrocarbon recovery process and apparatus 01 embodying the invention, a hydrocarbon/substrate mixture, referred to generally herein as tar sand ore, preferably has been mined, crushed, ground, screened, or otherwise pre-treated as needed in a conventional preparation zone (not shown) to eliminate large rocks and debris, for example, by a rotary trommel screen, and to yield an ore feedstock 10 having particles preferably less than about 2 mm in diameter (sand and clay size). The ore may be sprayed with water, preferably heated water, during processing by the trommel screen. The ore is charged through a feeder 11 , for example, a screw feeder, into a mixing tank 12 , wherein it is mixed with water to form a pumpable slurry 13 having a weight percent proportion of ore to water of between about 0.5:1 and about 2:1. The slurry is formed and then agitated by mixer 17 and its temperature is adjusted to between about 20° C. and about 150° C. to begin to release free hydrocarbons from the mineral substrate, soften waxy or ashpaltic hydrocarbon solids, reduce the apparent viscosity of the batch, reduce the density of hydrocarbon fractions within the batch, and begin to break surface adhesion of hydrocarbon compounds bound to substrate surfaces. Preferably, the temperature is adjusted to about 80° C.
[0045] As described up to this point, the present process is substantially as disclosed in the '145 patent, except that preferably hydrogen peroxide is not added to the slurry in mixing tank 12 , except via recycled process water as described below.
[0046] Mixing tank 12 is in communication with a subsequent shearing and separating device 14 . For example, connected to mixing tank 12 is agitating and shearing means, preferably in the form of a device 14 into which slurry 13 is preferably pumped by a first transfer pump 15 via line 19 . In some installations, line 19 is a relatively long pipe for transfer of slurry 13 from a mixing facility, which may be near the mine head, to a remote separating facility. In such a pipe, slurry 13 may be exposed advantageously to relatively high shear rates during pumping, preferably about 5 meters per second or higher, during transfer to device 14 . The term “shear” as used herein refers to an average mean fluid velocity in any direction. Slurry 13 may also be transferred by gravity feed; also, tank 12 and device 14 may be configured as different parts or different operating phases in a single vessel (not shown), within the scope of the invention.
[0047] Device 14 is functionally divided into a purely shearing region 29 a and a first stage separation region 29 b . Device 14 is preferably configured as a relatively long tube 80 , preferably disposed horizontally, having both cylindrical 82 and non-cylindrical 84 portions such that a cross-section is substantially in the shape of the inverted letter P or lower-case d (see FIG. 4), such that a plurality of rotary mixing devices, such as mixing means 16 , may be readily installed into apparatus 14 at a plurality of locations along the apparatus (see FIGS. 2 and 3). Mixing means 16 in accordance with the invention may be selected from the group consisting of a propeller, a fluid jet nozzle, jet pump, or any other impelling means. A shrouded propeller (impeller) is currently preferred. The impellers may be individually driven as by individual electric motors or may be ganged together with a common drive as by a chain or belt 29 in known fashion, as shown in FIG. 3. Each impeller is preferably provided with a generally cylindrical shroud 18 to narrow the cone of flow turbulence emanating from the mixer. In a currently preferred embodiment, each mixer 16 preferably is disposed non-radially of the tube axis 86 ; that is, the axis of rotation 88 of the mixer preferably is contained in a first plane and the axis of the tube is contained in a second plane, although both axes may lie in a single plane within the scope of the invention. The axis of rotation forms an angle 90 with the axis of the mixing tube, preferably about 90°. The axis of mixer rotation is preferably generally tangential to the cylindrical portion of the tube, such that the slurry is violently rolled about a horizontal axis (vertical spinning flow while axial flow is horizontal) as it passes horizontally along the tube from an entrance port 20 to an exit port 22 . Preferably, device 14 and pump 15 are sized to provide an axial mass flowrate of slurry 13 along the tube of about 0.13 ft/sec, or about 8 ft/min, where slurry temperature is about 80° C. and the process is operated at atmospheric pressure. Device 14 is preferably closed so that at other pressures, for example, up to 5 atmospheres gauge, other temperatures, for example, up to 150° C., and other suitable times are readily determinable by one of ordinary skill in the chemical engineering arts without undue experimentation.
[0048] Preferably, the instantaneous shear velocity in the highest-velocity direction within the slurry is at least 1 meter per second and preferably exceeds 5 meters per second. Preferably, the time period of intense agitation and shearing of slurry 13 up to this point, combining any such shearing from transfer in pipe 19 with shearing in section 29 a of device 14 , is at least 1 minute and preferably up to 15 minutes or more. Longer shearing times are not believed to adversely affect the slurry or the separation process. Such intense shear is believed by the inventors to distort and ultimately fracture the bitumen layer of each tar-sand grain, exposing the water layer and/or the mineral substrate within to subsequent attack by hydrogen peroxide, as described below.
[0049] In separation section 29 a of device 14 , slurry 13 is blended with an aqueous solution containing hydrogen peroxide to produce a treated slurry having a hydrogen peroxide content between about 0.05% and about 10.0% in the water phase by weight. Sodium peroxide is believed to also be functional in place of hydrogen peroxide, but hydrogen peroxide is the preferred oxidant for ease of handling, cost, and lack of chemical residue. Hydrogen peroxide is easily stored as a solution and ultimately decomposes to water and oxygen, leaving no elemental or mineral residue in the tailings. The peroxide solution is supplied from a storage source 24 through a feed pump 26 into device 14 via an entry port 28 which preferably is located part way along the length of device 14 , as shown in FIG. 2, to permit intense agitation and shearing in device 14 as described above prior the introduction of oxidant. Downstream of entry port 28 , along the length of device 14 , agitation and shearing may be maintained at a high level or may if desired be reduced.
[0050] Device 14 may be conveniently assembled from modular units like unit 14 a shown in FIG. 3. For example, at an axial slurry flowrate of 0.13 ft/sec, a 10-foot module has a slurry residence time of 1.33 minutes. Thus, an assembly of ten such modules in sequence, overall 100 feet long, can accommodate a residence time of greater than 13.3 minutes.
[0051] Referring now to FIG. 8, the following mechanism is presented by the inventors as one theory explaining the success of the invention, although validity of the invention does not rely upon the accuracy of such theory.
[0052] A tar sand grain 102 typically comprises a mineral particulate 104 as a core, usually a sand or clay particle, surrounded by a bitumen envelope 106 . A water layer 108 is commonly present, partially or fully surrounding the mineral particulate. However, the water layer may be completely absent. The tar sand grains 102 in the slurry are subjected to intense shear as described above. Hydrogen peroxide in aqueous solution, when added to the slurry, enters into each tar sand grain 102 via one or more fractures 110 in the bitumen envelope 106 caused by the prior intense shear. Hydrogen peroxide that enters a fractured tar sand grain is decomposed by reaction with the surface of the mineral particulate, forming water plus gaseous oxygen 112 . In a first separation stage 113 for each tar sand grain, the nascent gas phase immediately swells as oxygen bubbles 112 form between the bitumen envelope 106 and the particulate core 104 , disrupting the structure of the tar sand grain and causing the bitumen envelope to become detached from from the mineral particulate. In a second separation stage 115 for the slurry as a whole, the oxygen bubbles 112 remain attached preferentially to the bitumen globules 114 , giving the globules great buoyancy such that they rapidly migrate upwards 116 in the slurry, wherein the apparent viscosity is rapidly decreasing from decomposition of the tar sand grains. (The bubble-buoyant globules 114 are readily observable in the slurry and the bubble surfaces appear to be coated with hydrocarbon.) Conversely, most of the freed particulates 104 in the form of sand and clay fines sediment 118 rapidly, although some fines may be carried by convection upwards into the froth formed at the top of the slurry. Such incorporated sediments may be removed from the bitumen froth conventionally in a succeeding step.
[0053] This proposed mechanism for the process of the invention is supported by laboratory data, as shown in FIGS. 6 and 7.
[0054] Referring to FIG. 6, oil sand solids were obtained by dissolving away the bitumen envelopes with solvent. To evaluate the influence of peroxide on the oil sand grains, solids recovered from bench extractions were packed into a column of 7 mm diameter and 9 cm long. The end of the column was covered with a nylon mesh, which served to retain the solids within the column while providing access for the fluid. The fluid used in these experiments was 1-propanol. After determining an initial imbibition rate for 1-propanol into the column, the column was drained and dried. A 1% hydrogen peroxide solution then was placed in the column for a period of 24 hours. The packed column was then again drained and dried, and the imbibition rate of 1-propanol determined again. The results are shown in FIG. 6. Replicate trials 200 , 300 were conducted. Columns 202 , 302 represent the imbibition rate before peroxide treatment, and columns 203 , 303 represent the imbibition rate after peroxide treatment. The relative wetting index was reduced significantly after treatment with hydrogen peroxide, indicating that the solids were less likely to be wet by the 1-propanol after being exposed to the peroxide. If 1-propanol can be considered to be more “oil-like” than water, then the exposure to hydrogen peroxide appears to render the grain surfaces more hydrophilic; thus, attachment of hydrophobic materials like bitumen to the sand grains would be significantly weakened.
[0055] It was previously believed, as disclosed in the '145 patent, that the observed decomposition of hydrogen peroxide is a result of reaction to a significant degree with the bitumen via Fenton's Reaction to shorten hydrocarbon chain lengths and reduce viscosity. However, further experimentation, as is shown dramatically in FIG. 6, indicates that very little reaction occurs between hydrogen peroxide and the hydrocarbon of a tar sand grain when the mineral substrate has been removed (curve 402 ). However, very rapid decomposition of hydrogen peroxide is seen when the hydrogen peroxide solution is exposed to only a mineral substrate from which the hydrocarbon envelope has been removed, whether the substrate be clay (curve 404 ) or sand (curve 406 ).
[0056] To find the source that is responsible for the decomposition of the peroxide, experiments were conducted on solids recovered from the extraction experiments and using a bitumen-in-water emulsion created in the laboratory. The solids were further separated into two size fractions by screening through a 325 mesh (nominally 45 μm opening) screen. For the solids, approximately 4 g of material were dispersed in 100 ml of water containing peroxide. The bitumen-in-water emulsion was used as formed (approximately 1% by weight). The bitumen-in-water emulsion separated at 80° C., so that portion of the experiment was conducted at 55° C. (For comparison purposes, the decomposition curve 408 for high grade oil sand at 55° C. has also been included.) The low rate of decomposition for the bitumen-in-water emulsion demonstrates conclusively that the decomposition of peroxide occurs when access to the surface of the solids is achieved, not through reaction with the bituminous envelope. A surprising result, however, is that the decomposition for the solids does not show dependence on the size of the solids. It was expected that the smaller size fraction (designated as <45 μm) would show higher decomposition rates. A probable explanation for this observation is that the specific sites that are responsible for the deposition far exceed the amount of peroxide present.
[0057] Continuing with the description of the process, and referring again to FIGS. 1 and 2, device 14 is in communication with a separator tank 30 for carrying out second separation stage 115 . From exit port 22 , the slurry is passed into separator tank 30 via line 27 . Mineral particulates, substantially freed of hydrocarbons, settle out of the slurry to the bottom of the tank. For a continuous process, tank 30 is provided with a substantially flat bottom on which the layer of sand and clay accumulates. The settling particulates can mechanically trap globules of bitumen; therefore, a fluid distribution means such as a sparger bar 32 may be disposed within the tank on the bottom 31 , where sand can settle upon it. A fluid, such as water or compressed air, is delivered from a source 34 to sparger bar 32 and is allowed to bubble up through the settling sand to sweep entrained bitumen up into the water/hydrocarbon phase. Such sparging may be performed continuously or intermittently, preferably at a sufficiently low fluid flow rate that the settling sand is not significantly stirred back into the water phase.
[0058] Alternatively, the sand on bottom 31 may be mechanically agitated by a scuffle bar to allow entrapped bitumen globules to escape.
[0059] Sand that accumulates on bottom 31 may be removed, within the scope of the invention, by any means desired. In a preferred embodiment, as shown in FIG. 2, a drag chain conveyor 36 is disposed in tank 30 in proximity to and above sparger bar 32 . Conveyor 36 comprises a continuous articulated belt 38 of paddles or scoops hinged together and disposed around a plurality of rollers 40 driven by a conventional drive means (not shown) in a pathway having a first portion 42 substantially parallel to bottom 31 , a second portion 44 leading upwards and away from bottom 31 and out of tank 30 , and a third portion 46 leading away from tank 30 . Return paths are parallel and opposite to the exit paths just described. The motion of the conveyor, as shown in FIG. 2, is clockwise. Sand settling to the bottom of the tank and being cleaned of bitumen by the sparger settles through spaces in the conveyor belt and accumulates to a depth at which first conveyor portion 42 is encountered. As cleaned sand continues to accumulate, conveyor 36 sweeps the sand to the left in tank 30 and then drags excess sand up the slope of exit chute 48 and away from tank 30 to a storage site 50 . The sand thus separated is wet with water, is substantially free of hydrocarbons, and is environmentally suitable for direct landfill without further treatment.
[0060] Still referring to FIG. 2, in some ores, significant amounts of bitumen may still be present by entrainment in the sand as removed from tank 30 by conveyor 36 . Such bitumen may be efficiently recovered through use of a second separation tank 30 ′, shown schematically, wherein a new slurry may be formed by addition of water, as needed, to the sand. Commonly, sufficient residual hydrogen peroxide is present in the sand to effect separation, although more hydrogen peroxide may be added from source 24 as desired. The re-cleaned particulates settle rapidly to the bottom of tank 30 ′ and are removed by another drag chain conveyor 36 ′ to storage site 50 . Froth 52 ′ is treated as described below.
[0061] In the liquid phase in first separator 30 , a froth 52 rich in hydrocarbons and buoyed by oxygen bubbles rises to the surface as the aqueous and organic phases partially separate gravitationally. Froth 52 typically contains substantial amounts of entrained water and substrate fines.
[0062] Optionally, such separation may be effected by known means such as centrifugation, filtration, settling, adsorption, absorption, or combinations thereof, of one phase from the other, or of the liquids from the particulates.
[0063] Optionally, such separation may be enhanced by further addition of water to the separator tank.
[0064] The organic phase floating on the aqueous phase near the top of tank 30 following separation therefrom preferably is drawn off via overflow pipe 54 and sent to a storage tank 56 where it is ready for shipment to a petroleum refiner. Bitumen and other hydrocarbonaceous products of the present process may be heated in tank 56 by a hot water or steam heater system 58 to reduce viscosity and promote flow as needed. The cutter stock may be recovered from the bitumen in known fashion by the refiner and returned for reuse.
[0065] Alternatively, froths 52 , 52 ′ may be removed to a separate treatment apparatus (not shown), as is typical for froths separated in accordance with the prior art. To remove most water and fines from the organic phase, the froth may be mixed with cutter stock, preferably at a ratio of about 1:1, to dilute and solubilize the bitumen, causing a further separation of the froth into an aqueous phase containing the fines and an organic phase containing the hydrocarbons. Preferably, in accordance with the invention, the froth may be treated with additional amounts of hydrogen peroxide to assist in breaking the foam. As the froth is degraded, the entrained mineral particulates settle out and the bitumen rises to the surface where it may be skimmed off for further treatment to prepare it for refining. The separated water layer is preferably returned to the head end of the main process for efficient recycle of the heat and peroxide content, as described above.
[0066] Separator tank 30 is further provided with a partial cover 59 which includes along one edge an inverted weir 60 extending from above the surface 62 of the liquid phase downwards into the aqueous phase. The aqueous phase, still typically containing a dispersion of some portion of the clay fines, may be drawn off from tank 30 via a middling outlet port 64 at a flowrate selected such that the organic phase is not drawn under weir 60 . The aqueous phase is directed to a water conditioner 66 which may comprise any of various well-known clarifying devices, including but not limited to a centrifuge, a filter, and a tailings pond. Preferably, conditioner 66 is a sand filter, which may utilize the sand in storage site 50 or other sand medium. Particle-free process water suitable for re-use is recycled from conditioner 66 through water heater system 68 into mixing tank 12 . It is an important feature of the invention that the only water necessarily residual of the process is the water wetting the sand and clay. In many applications, the process water exiting the conditioner 66 may be re-used in its entirety as make-up water in the initial mixing step.
[0067] The present process may also yield gaseous hydrocarbons which are desirably collected for at least environmental reasons, and which may be present in sufficient quantity to have economic significance. Accordingly, a vacuum pump 70 is connected via vacuum lines 72 to a headspace 74 in the oxidizing vessel, a headspace 76 beneath cover 59 of the separator tank, and a headspace 78 in storage tank 56 . The collected vapors 80 may be burned off to the atmosphere or may be directed for combustion in water heating system 68 or may be otherwise used.
[0068] With respect to prior art bitumen recovery processes such as are discussed hereinabove, and referring now to FIG. 5, an important advantage and benefit of a bitumen recovery process employing hydrogen peroxide in accordance with the invention is a much higher initial rate of bitumen liberation from the tar sand grains. In laboratory tests using a recirculation apparatus wherein various addenda were added to a tar sand slurry and recirculated for up to one hour, curve 502 represents the rate of liberation using sodium hydroxide in a slurry at pH 8.78; curve 504 , liberation using hydrogen peroxide addition at two different times; and curve 506 , liberation using hydrogen peroxide at a single point and time, for example, as shown in FIG. 2. The total liberation after an hour is nearly the same for all three methods. However, separation in a commercially viable process must be as rapid as possible; processes requiring more than about 15 minutes are not useful because of the size of the plant required to hold the material for long times and still have high throughput. The much more rapid initial rate of peroxide-aided separation and flotation dramatically reduces the size requirement of a processing plant, resulting in savings which may exceed $100,000,000 per plant.
[0069] From the foregoing description it will be apparent that there has been provided improved methods and apparatus for economically recovering petroleum-like hydrocarbon residues from particulate mineral substrates, especially hydrocarbonaceous ores, and for discharging a substrate residue environmentally suitable for landfill disposal. Variations and modifications of the herein described methods and apparatus, in accordance with the invention, will undoubtedly suggest themselves to those skilled in this art. Accordingly, the foregoing description should be taken as illustrative and not in a limiting sense.
|
Method and apparatus for treating an ore comprising mineral substrate particles surrounded by hydrocarbon compounds, especially tar sand grains and contaminated soils, to recover a hydrocarbon portion and a cleaned substrate portion. In a preferably continuous process, hydrocarbonaceous rock, sand, ore, or soil containing bitumen, petroleum, and/or kerogen may be crushed or otherwise comminuted as needed to provide a particle size of sand or smaller. The ore is mixed with water to form a slurry. The slurry is heated to about 80° C. and is intensively sheared to condition the slurry for separation, preferably by shear-fracture of the hydrocarbon layers surrounding the particles in the grains. The conditioned slurry is blended with a peroxide in aqueous solution, preferably hydrogen peroxide, which enters the grains and is decomposed therein, creating bubbles of free oxygen within the grains which disrupt the hydrocarbon envelope. In decomposing, the peroxide increases the hydrophilicity of the particle surfaces. Both free and bound hydrocarbons in the ore are thereby released from the mineral substrate particles. The resulting hydrocarbon globules are separated from the substrate particles by flotation, accelerated by attached oxygen bubbles. Water and mineral tailings from the process are substantially free of hydrocarbon contamination and are environmentally suitable for landfill disposal.
| 8
|
FIELD OF THE INVENTION
[0001] The present invention relates to crystalline forms of dexlansoprazole designated as Forms A and B, and process for their preparation. The present invention further relates to processes for the preparation of anhydrous dexlansoprazole and dexlansoprazole sesquihydrate using crystalline Forms A and B of dexlansoprazole.
BACKGROUND OF THE INVENTION
[0002] Dexlansoprazole is chemically described as 2-[(R)-{[3-methyl-4-(2,2,2-trifluoroethoxy)pyridin-2-yl]methyl}sulfinyl]-1H-benzimidazole as represented by Formula I.
[0000]
[0003] Dexlansoprazole is useful for healing all grades of erosive esophagitis (“EE”) for up to 8 weeks, to maintain the healing of EE for up to 6 months and for the treatment of heartburn associated with non-erosive gastroesophageal reflux disease (“GERD”) for 4 weeks.
[0004] U.S. Pat. Nos. 6,462,058; 7,285,668 and U.S. Publication 2007/0004779 purportedly describe processes for preparing crystalline forms of dexlansoprazole and its hydrates. WO 2009/117489 purportedly describes process for the preparation of amorphous dexlansoprazole.
SUMMARY OF THE INVENTION
[0005] Crystalline Form A of dexlansoprazole comprising substantially the same XRPD pattern as depicted in FIG. 1 .
[0006] Crystalline Form A of dexlansoprazole having an XRPD pattern comprising d-spacing values substantially at 16.18, 5.41, 4.88, 4.65, 4.15 and 3.93 Å.
[0007] Crystalline Form A of dexlansoprazole according to claim 2 , further comprising d-spacing values substantially at 16.18, 13.26, 11.64, 10.88, 9.76, 8.11, 7.29, 6.76, 6.39, 5.92, 5.83, 5.73, 5.41, 5.17, 5.07, 4.88, 4.83, 4.65, 4.42, 4.27, 4.15, 4.09, 4.01, 3.93, 3.73, 3.61, 3.52, 3.45, 3.41, 3.31, 3.25, 3.21, 3.11, 3.06, 2.98, 2.92, 2.84, 2.72, 2.63, 2.55, 2.44 and 2.36 Å.
[0008] Crystalline Form B of dexlansoprazole comprising substantially the same XRPD pattern as depicted in FIG. 2 .
[0009] Crystalline Form B of dexlansoprazole having an XRPD pattern comprising d-spacing values substantially at 13.86, 11.09, 5.00, 4.77, 4.62, 4.32, 3.94, 3.70 and 3.63 Å.
[0010] Crystalline Form B of dexlansoprazole according to claim 5 , further comprising d-spacing values substantially at 13.86, 11.09, 9.02, 6.92, 6.80, 5.54, 5.20, 5.00, 4.77, 4.68, 4.62, 4.32, 4.29, 4.21, 4.05, 3.94, 3.70, 3.63, 3.57, 3.51, 3.43, 3.40, 3.37, 3.22, 3.09, 3.04, 2.99, 2.94, 2.89, 2.82, 2.78, 2.74, 2.67, 2.59, 2.53, 2.49 and 2.41 Å.
[0011] A process for the preparation of crystalline Form A of dexlansoprazole, wherein the process comprises:
a) treating dexlansoprazole with cyclohexanol; and b) isolating the crystalline Form A of dexlansoprazole from the mixture thereof.
[0014] A process for the preparation of crystalline Form B of dexlansoprazole, wherein the process comprises:
a) treating dexlansoprazole with phenol; and b) isolating the crystalline Form B of dexlansoprazole from the mixture thereof.
[0017] A process for the preparation of anhydrous dexlansoprazole, wherein the process comprises:
a) treating crystalline Form A or Form B of dexlansoprazole with an organic solvent; and b) isolating anhydrous dexlansoprazole which comprises an XRPD pattern having interplanar spacing (d) values substantially at 11.70, 6.78, 5.84, 5.73, 4.43, 4.17, 4.13, 4.09, 3.94, 3.90, 3.70, 3.41 and 3.12 Å.
[0020] A process according to the claim 9 , wherein the organic solvent is an alkanol, an ether or a mixture thereof.
[0021] A process for the preparation of dexlansoprazole sesquihydrate, wherein the process comprises:
a) treating crystalline Form A of dexlansoprazole with water, and b) isolating dexlansoprazole sesquihydrate which comprises interplanar spacing (d) values substantially at 13.22, 9.61, 8.87, 8.04, 6.61, 6.00, 5.91, 5.64, 5.02, 4.51, 3.65, 3.57, 3.51 and 3.00 Å.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] FIG. 1 depicts the X-ray powder diffraction pattern (XRPD) of the crystalline Form A of dexlansoprazole.
[0025] FIG. 1A provides the table of values for the XRPD pattern depicted in FIG. 1 .
[0026] FIG. 2 depicts the X-ray powder diffraction pattern (XRPD) of the crystalline Form B of dexlansoprazole.
[0027] FIG. 2A provides the table of values for the XRPD pattern depicted in FIG. 2 .
[0028] FIG. 3 depicts the X-ray powder diffraction pattern (XRPD) of the anhydrous dexlansoprazole.
[0029] FIG. 3A provides the table of values for the XRPD pattern depicted in FIG. 3 .
[0030] FIG. 4 depicts the X-ray powder diffraction pattern (XRPD) of dexlansoprazole sesquihydrate.
[0031] FIG. 4A provides the table of values for the XRPD pattern depicted in FIG. 4 .
DETAILED DESCRIPTION OF THE INVENTION
[0032] The present invention provides for crystalline Form A of dexlansoprazole. The crystalline Form A of dexlansoprazole has substantially the same XRPD (X-ray powder diffraction pattern) pattern as depicted in FIG. 1 . The crystalline Form A of dexlansoprazole is characterized by an XRPD pattern having interplanar spacing (d) values at 16.18, 5.41, 4.88, 4.65, 4.15 and 3.93 Å. The crystalline Form A of dexlansoprazole is further characterized by an XRPD pattern having interplanar spacing (d) values at 16.18, 13.26, 11.64, 10.88, 9.76, 8.11, 7.29, 6.76, 6.39, 5.92, 5.83, 5.73, 5.41, 5.17, 5.07, 4.88, 4.83, 4.65, 4.42, 4.27, 4.15, 4.09, 4.01, 3.93, 3.73, 3.61, 3.52, 3.45, 3.41, 3.31, 3.25, 3.21, 3.11, 3.06, 2.98, 2.92, 2.84, 2.72, 2.63, 2.55, 2.44 and 2.36 Å.
[0033] The present invention also provides for crystalline Form B of dexlansoprazole. The crystalline Form B of dexlansoprazole has substantially the same XRPD (X-ray powder diffraction pattern) pattern as depicted in FIG. 2 . The crystalline Form B of dexlansoprazole is characterized by an XRPD pattern having interplanar spacing (d) values at 13.86, 11.09, 5.00, 4.77, 4.62, 4.32, 3.94, 3.70 and 3.63 Å. The crystalline Form B of dexlansoprazole is further characterized by an XRPD pattern having interplanar spacing (d) values at 13.86, 11.09, 9.02, 6.92, 6.80, 5.54, 5.20, 5.00, 4.77, 4.68, 4.62, 4.32, 4.29, 4.21, 4.05, 3.94, 3.70, 3.63, 3.57, 3.51, 3.43, 3.40, 3.37, 3.22, 3.09, 3.04, 2.99, 2.94, 2.89, 2.82, 2.78, 2.74, 2.67, 2.59, 2.53, 2.49 and 2.41 Å.
[0034] The present invention also provides a process for the preparation of crystalline Form A of dexlansoprazole. The process includes:
a) treating dexlansoprazole with cyclohexanol; and b) isolating the crystalline Form A of dexlansoprazole from the mixture thereof.
[0037] Dexlansoprazole existing in any solid or non-solid form known in the prior art may be used as the starting material. Dexlansoprazole may be prepared, for example, according to the methods disclosed in WO 96/02535 or WO 97/02261. Dexlansoprazole is treated with cyclohexanol. The treatment with cyclohexanol may be carried out at a temperature of about 10° C. to about 100° C., for example, at about 15° C. to about 50° C. The cyclohexanol may be used alone or in combination with an organic solvent, or the treatment with cyclohexanol is optionally preceded or followed by treatment with an organic solvent. The organic solvent may be a ketone, for example, acetone, or an aliphatic hydrocarbon, for example, n-hexane. The mixture is stirred for a sufficient to time to effect the formation of crystalline Form A of dexlansoprazole. The crystalline Form A of dexlansoprazole may be isolated from the reaction mixture by filtration, cooling, evaporation, decantation, distillation, vacuum drying, or a combination thereof.
[0038] The present invention also provides a process for the preparation of crystalline Form B of dexlansoprazole. The process includes:
a) treating dexlansoprazole with phenol; and b) isolating the crystalline Form B of dexlansoprazole from the mixture thereof.
[0041] Dexlansoprazole existing in any solid or non-solid form known in the prior art may be used as the starting material. Dexlansoprazole may be prepared, for example, according to the methods disclosed in WO 96/02535 or WO 97/02261. Dexlansoprazole is treated with phenol. The treatment with phenol may be carried out at a temperature of about 10° C. to about 100° C., for example, about 15° C. to about 50° C. The phenol may be used alone or in combination with an organic solvent, or the treatment with phenol is optionally preceded or followed by treatment with an organic solvent. The organic solvent may be an ester, for example, ethyl acetate, or an aliphatic hydrocarbon, for example, n-hexane. The mixture is stirred for a sufficient to time to effect the formation of crystalline Form B of dexlansoprazole. The crystalline Form B of dexlansoprazole may be isolated from the reaction mixture by filtration, cooling, evaporation, decantation, distillation, vacuum drying, or a combination thereof.
[0042] The present invention also provides for a process for the preparation of anhydrous dexlansoprazole which is characterized by an XRPD pattern comprising interplanar spacing (d) values at 11.70, 6.78, 5.84, 5.73, 4.43, 4.17, 4.13, 4.09, 3.94, 3.90, 3.70, 3.41 and 3.12 Å. The process includes:
a) treating crystalline Form A or Form B of dexlansoprazole with an organic solvent; and b) isolating anhydrous dexlansoprazole which is characterized by an XRPD pattern having interplanar spacing (d) values substantially at 11.70, 6.78, 5.84, 5.73, 4.43, 4.17, 4.13, 4.09, 3.94, 3.90, 3.70, 3.41 and 3.12 Å.
[0045] The crystalline Form A or Form B of dexlansoprazole may be prepared according to the previous aspects of the present invention. The crystalline Form A or Form B of dexlansoprazole is treated with an organic solvent. The organic solvent may be an alkanol, for example, methanol, or ether, for example, diisopropyl ether or a mixture thereof. The treatment with the solvent may be carried out at a temperature of about −30° C. to about 60° C., for example, about −20° C. to about 55° C. The mixture may be stirred for about 1 hour to about 10 hours. The anhydrous dexlansoprazole may be isolated by filtration, distillation, decantation, vacuum drying, evaporation, or a combination thereof.
[0046] The anhydrous dexlansoprazole so obtained has an XRPD pattern having interplanar spacing (d) values at 11.70, 6.78, 5.84, 5.73, 4.43, 4.17, 4.13, 4.09, 3.94, 3.90, 3.70, 3.41 and 3.12 Å. The anhydrous dexlansoprazole is further characterized by an XRPD pattern having interplanar spacing (d) values at 11.70, 8.47, 7.96, 6.78, 6.53, 5.84, 5.73, 5.12, 4.85, 4.78, 4.43, 4.40, 4.24, 4.17, 4.13, 4.09, 3.98, 3.94, 3.90, 3.85, 3.70, 3.52, 3.41, 3.39, 3.31, 3.26, 3.12, 3.10, 2.97, 2.94, 2.87, 2.84, 2.75, 2.71, 2.60, 2.48, 2.41, 2.38 and 2.30 Å.
[0047] The present invention also provides a process for the preparation of dexlansoprazole sesquihydrate which is characterized by an XRPD pattern with interplanar spacing (d) values at 13.22, 9.61, 8.87, 8.04, 6.61, 6.00, 5.91, 5.64, 5.02, 4.51, 3.65, 3.57, 3.51 and 3.00 Å, wherein the process includes:
a) treating crystalline Form A of dexlansoprazole with water; and b) isolating dexlansoprazole sesquihydrate.
[0050] The crystalline Form A of dexlansoprazole may be prepared according to the previous aspect of the present invention. The crystalline Form A of dexlansoprazole is treated with water. The water may be used alone or in combination with a water-miscible organic solvent. The treatment with water may be carried out at a temperature of about 15° C. to about 100° C., for example, about 20° C. to about 55° C. accompanied by stirring. The stirring may be carried out for about 1 hour to about 5 hours, for example, about 2 hour to 3 hours. The dexlansoprazole sesquihydrate may be isolated by filtration, cooling, distillation, decantation, vacuum drying, evaporation, or a combination thereof. The dexlansoprazole sesquihydrate so obtained has an XRPD pattern having interplanar spacing (d) values at 13.22, 9.61, 8.87, 8.04, 6.61, 6.00, 5.91, 5.64, 5.02, 4.51, 3.65, 3.57, 3.51 and 3.00 Å. The dexlansoprazole sesquihydrate is further characterized by an XRPD pattern having interplanar spacing (d) values at 21.60, 18.04, 13.22, 10.74, 9.61, 8.87, 8.04, 7.15, 6.61, 6.00, 5.91, 5.64, 5.45, 5.02, 4.80, 4.68, 4.51, 4.38, 4.29, 4.23, 4.12, 3.99, 3.85, 3.75, 3.72, 3.65, 3.57, 3.51, 3.47, 3.40, 3.34, 3.28, 3.20, 3.17, 3.11, 3.08, 3.00, 2.88, 2.83, 2.74, 2.66, 2.61, 2.55, 2.50, 2.43 and 2.40 Å.
[0051] XRPD of the samples were determined by using Panalytical X'Pert Pro X-Ray Powder Diffractometer in the range 3-40 degree 2 theta and under tube voltage and current of 45 Kv and 40 mA respectively. Copper radiation of wavelength 1.54 angstrom and Xceletor detector were used.
[0052] While the present invention has been described in terms of its specific embodiments, certain modifications and equivalents will be apparent to those skilled in the art and are intended to be included within the scope of the present invention.
EXAMPLES
Example 1
Preparation of Crystalline Form A of Dexlansoprazole
[0053] Dexlansoprazole (15 g) was dissolved in cyclohexanol (120 mL) at 22° C. to 28° C. The solution was stirred at 22° C. to 28° C. for 15 minutes and at 50° C. to 55° C. for 1 hour. n-Hexane (300 mL) was slowly added at 50° C. to 55° C. in 45 minutes. The solution was stirred at 50° C. to 55° C. for 30 minutes and at 22° C. to 28° C. for 45 minutes. n-Hexane (200 mL) was added at 22° C. to 28° C. and stirred for 2 hours. The mixture was stirred at 10° C. to 15° C. for 30 minutes and at 5° C. to 10° C. for 2 hours. The mixture was filtered and the solid was washed with n-hexane (240 mL). The solid was dried under vacuum at 22° C. to 28° C. for 1 hour to obtain the title compound having an XRPD pattern as depicted in FIG. 1 .
[0054] Yield: 15 g
Example 2
Preparation of Crystalline Form A of Dexlansoprazole
[0055] Cyclohexanol (0.8 g) and acetone (1 mL) were added to dexlansoprazole (2 g) and the mixture was ground at 22° C. to 28° C. for 20 minutes. The mixture was dried under vacuum at 22° C. to 28° C. for 32 hours to obtain the title compound.
[0056] Yield: 2 g
Example 3
Preparation of Crystalline Form B of Dexlansoprazole
[0057] Dexlansoprazole (2 g) was dissolved in ethyl acetate (15 mL) at 22° C. to 28° C. The solution was stirred at 22° C. to 28° C. for 10 minutes. Phenol (1.25 g) in ethylacetate (5 mL) was added drop-wise to the solution. The mixture was stirred at 22° C. to 28° C. for 2.5 hours. n-Hexane (35 mL) was added at 20° C. to 25° C. and the mixture was stirred for 7 hours. The solution was kept at 22° C. to 28° C. for 16 hours. The solution was filtered and dried under vacuum at 22° C. to 28° C. for 1 hour to obtain the title compound having an XRPD pattern as depicted in FIG. 2 .
[0058] Yield: 1 g
Example 4
Preparation of Crystalline Form B of Dexlansoprazole
[0059] A mixture of dexlansoprazole (2 g) and phenol (1.3 g) was ground at 22° C. to 28° C. for 30 minutes. The mixture was dried under vacuum at 22° C. to 28° C. for 20 hours to obtain the title compound.
[0060] Yield: 2.5 g
Example 5
Preparation of Anhydrous Dexlansoprazole
[0061] Dexlansoprazole crystalline Form A (5 g) was dissolved in methanol (12.5 mL) at 22° C. to 28° C. and the solution was stirred for 1 hour. The solution was added drop-wise in 15 minutes to cooled diisopropylether (0° C. to 5° C.; 150 mL). The mixture was stirred at 0° C. to 5° C. for 2 hours and at −20° C. to −10° C. for 45 minutes. The mixture was further stirred at 50° C. to 55° C. for 45 minutes and at 0° C. to 5° C. for 2.5 hours. The mixture was filtered and the solid was washed with n-hexane (25 mL). The mixture was dried under vacuum at 22° C. to 28° C. for 2.5 hours to obtain the title compound having an XRPD pattern as depicted in FIG. 3 .
[0062] Yield: 2 g
[0063] Moisture content: 0.13% w/w
Example 6
Preparation of Anhydrous Dexlansoprazole
[0064] Dexlansoprazole crystalline Form B (3.8 g) was dissolved in methanol (10 mL) at 22° C. to 28° C. and the solution was stirred for 1 hour. The solution was added drop-wise in 15 minutes to hot diisopropylether (50° C. to 55° C.; 100 mL). The mixture was stirred at 50° C. to 55° C. for 1 hour and stirred at 0° C. to 5° C. for 5 hours. Diisopropylether (20 mL) was added to the mixture and the mixture was stirred for 2 hours. n-Hexane (150 ml) was added to the mixture and the mixture was stirred at 0° C. to 5° C. for 1.5 hours. The mixture was filtered and the solid was washed with n-hexane (25 mL). The solid was dried under vacuum at 22° C. to 28° C. for 2.5 hours to obtain the title compound.
[0065] Yield: 2 g
[0066] Moisture content: 0.13% w/w
Example 7
Preparation of Dexlansoprazole Sesquihydrate
[0067] Dexlansoprazole crystalline Form A (4 g) was dissolved in deionized water (100 mL) at 22° C. to 28° C. and stirred at 50° C. to 55° C. for 30 minutes. Deionized water (50 mL) was added to the solution and the solution was stirred at 50° C. to 55° C. for 45 minutes. The mixture so obtained was filtered and the solid was washed with warm water (25 mL). The solid was dried under vacuum at 22° C. to 28° C. for 16 hours to obtain the title compound having an XRPD pattern as depicted in FIG. 4 .
[0068] Yield: 3.5 g
[0069] Moisture content: 7.46% w/w
|
The present invention relates to crystalline forms of dexlansoprazole designated as forms A and B, and their preparation. The present invention further relates to processes for the preparation of anhydrous dexlansoprazole and dexlansoprazole sesquihydrate using crystalline Forms A and B of dexlansoprazole.
| 2
|
Subsets and Splits
No community queries yet
The top public SQL queries from the community will appear here once available.