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BACKGROUND OF THE INVENTION
Field of the Invention
[0001] The invention relates to a process for the treatment of a cellulosic molded body, in particular of cellulose fibers for textiles or non-woven fabrics.
[0002] In particular the invention relates to a process for modifying the properties of cellulosic molded bodies by means of chitosan.
[0003] Chitin and chitosan are natural, biodegradable, non-toxic, non-allergenic, bioactive and biocompatible polymers with a structure similar to that of cellulose. Chitin is gained from the shells of crustaceans, a waste material of the crab and shrimp industries. The worldwide interest in the range of use for chitin has seen an enormous increase in recent years as it is regarded as the second largest resource of natural polysaccharides beside cellulose.
[0004] Chitosan consists of poly-(1,4)-2-amino-2-desoxy-beta-D-glucose and is produced by deacetylation of chitin (poly-(1,4)-2-acetamide-2-desoxy-beta-D-glucose). For reasons of solubility—chitin is insoluble in water, organic solvents, diluted acids and bases—chitosan, which is soluble in diluted acids, aqueous methanol and glycerol, has the by far greater significance.
[0005] Areas of application for chitin and chitosan are the immobilization of cells and enzymes in biotechnology, the treatment of wounds in medicine, the use as nutritional supplement and preserving agent in the food industry, the preservation of seeds in agriculture, the use as flocculating agent and chelating agent with heavy metals in sewage systems.
[0006] However, a modification of the chitin/chitosan has to be carried out for most areas of application in order to improve the solubility in aqueous systems.
[0007] The use of chitosan in the textile industry is divided into three fields of application:
the production of 100% chitosan fibers and the production of “man-made fibers” with incorporated chitosan, respectively the finishing and coating of textile fibers auxiliary process agents for the textile industry
[0011] Due to their antibacterial properties and inhibitory effects on the growth of pathogenic germs, chitosan fibers are used in the field of medicine, for instance as wound coverage and surgical sutures. Chitin and chitosan, respectively, can be broken down enzymatically or hydrolytically by endogenic ferments and therefore are reabsorbable fibers. The effect of such natural polymers on the healing of wounds consists in the gradual release of N-acetyl-glucosamine, the mucopolysaccharide organization of the collagen as well as the beneficial effect on the tissue growth during wound healing (e.g., EP 0 077 098, U.S. Pat. No. 4,309,534, JP81/112937 and JP84/116418).
[0012] The disadvantage of fibers made of 100% chitosan, however, consists in that they exhibit low dry strength (chitosan fibers of Messrs. Innovative Technology Ltd., Winsford, England: titer 0.25 tex; fiber strength conditioned 9 cN/tex; fiber elongation conditioned 12.4%; chitosan fibers of Messrs. Korea Chitosan Co. LTD: fiber strength conditioned 15 cN/tex; fiber elongation conditioned 26%), that they are extremely brittle and that the wet strength amounts to merely 30% of the dry strength. Therefore, either chitosan fibers are admixed to other man-made fibers, or chitosan is already added to the spinning mass during the manufacturing process of, e.g. viscose fibers.
[0013] Viscose fibers with incorporated chitin/chitosan (in the following: “chitosan-incorporated viscose fibers”) are commercially available, e.g. under the trade names Crabyon (Messrs. Omikenshi Co) and Chitopoly (Messrs. Fuji Spinning Co.). Those fibers are produced, for instance, by dispersing chitosan or acetylated chitosan in powder form with a grain size of less than 10 μm in water in an amount of 0.5 to 2% by weight and by adding it to the viscose dope (U.S. Pat. No. 5,320,903). Thereupon, fibers are produced in accordance with the conventional viscose process or also the polynosic process.
[0014] Further manufacturing processes for chitosan-incorporated viscose fibers are described in U.S. Pat. No. 5,756,111 (complex pre- and after-dissolution processes at low temperature in order to obtain alkaline chitin-chitosan solutions to be added to the viscose solution) and in U.S. Pat. No. 5,622,666 (addition of microcrystalline chitosan and a water- and/or alkali-soluble natural polymer, e.g. sodium alginate, which can form ionic bonds with the chitosan, as a dispersion to the viscose dope) and in PCT/FI90/00292 and FI 78127 (addition of micro-crystalline chitosan to the spinning mass), respectively.
[0015] AT 8388 U describes the use of a cellulose fiber incorporating a chitosan or a chitosan salt and/or having a chitosan or a chitosan salt at its surface, in a non-woven textile and/or absorbent toiletries.
[0016] The chitosan-incorporated viscose fibers exhibit an increased dye affinity, an increased water retention value, fungicidal and odor-reducing properties, but also the low wet strength viscose fibers are known for. Since chitosan prevents the growth of bacteria harmful to the skin and eliminates allergic effects, for instance, fabrics made of Chitopoly are particularly suitable for dermatitis patients.
[0017] The drawback of all the methods described consists in that the fibers thus obtained contain very fine chitosan particles, since the chitosan is not soluble in the spinning mass.
[0018] The secondary agglomeration of the chitosan in the spinning mass or the inhomogeneous distribution, respectively, results in a deterioration of the spinning properties, spinning of fibers with low titres is extremely difficult. For that reason, it is also impossible to increase the amount of incorporated chitosan, since, in doing so, there would be an immediate loss of textile data or, already during spinning, numerous fiber breakages would occur. Furthermore, leakages of chitosan occur in the spinning bath, since chitosan is soluble in acids. For the incorporation of chitosan, additional complex steps are necessary.
[0019] In order to guarantee the effect of chitosan in the final product, there has to be incorporated an amount of at least 10 w % of chitosan in the fibers, as only then there will be existent enough chitosan at the fiber surface. The chitosan incorporated inside the fibers is inaccessible and hence not effective.
[0020] Subsequently, it also was attempted to incorporate chitosan in solvent-spun cellulose fibers produced in accordance with the amine-oxide process (so-called “Lyocell fibers”), in particular because of the high wet and dry strength of Lyocell fibers.
[0021] In DE 195 44 097, a process for the fabrication of molded bodies made from polysaccharide mixtures is described, wherein cellulose and a second polysaccharide are dissolved in an organic polysaccharide solvent mixable with water (preferably NMMO), which may also contain a second solvent.
[0022] Furthermore, in KR-A 9614022, the production of chitin-cellulose fibers, referred to as “chitulose”, is described, wherein chitin and cellulose are dissolved in a solvent from the group comprising dimethyl imidazoline/LiCl, dichloro acetate/chlorinated hydrocarbon, dimethyl acetamide/LiCl, N-methylpyrrolidone/LiCl, and yarns are produced according to the wet spinning process. NMMO is not mentioned in the claims.
[0023] In EP-A 0 883 645, among other things, the addition of chitosan to the solution as a modified compound for increasing the elasticity of wraps for foodstuff is claimed. The modifying compounds must be miscible with the cellulose/NMMO/water solution.
[0024] KR-A-2002036398 describes the incorporation of chitosan derivatives with quaternary ammonium groups, which are rather difficult to produce, into fibers.
[0025] In DE-A 100 07 794, the production of polymer compositions is described, comprising a biodegradable polymer and a material consisting of sea weeds and/or the shells of sea animals, as well as the production of molded bodies therefrom. The addition of a material made of sea weeds, sea animals in powder form, in the form of a powder suspension or in liquid form to the cellulose solution produced according to the Lyocell process is also claimed. Furthermore, the material may also be added after or during the shredding of the dry cellulose as well as at any stage of the manufacturing process. Despite the addition of the additive, the fibers exhibit the same textile-mechanical properties as they would without the additive. In the Examples, only Lyocell fibers that have a brown algae powder incorporated are described, wherein, for the production of the spinning mass, the brown algae dust, NMMO and pulp and a stabilizer are mixed and heated to 94° C.
[0026] Furthermore, in the final report “Erzeugnisse aus Polysaccharidverbunden” (Taeger, E.; Kramer, H.; Meister, F.; Vorwerg, W.; Radosta, S; TITK—Thüringisches Institut für Textil-und Kunststoff-Forschung, 1997, pp. 1-47, report no. FKZ 95/NR 036 F) it is described that chitosan is dissolved in diluted organic or inorganic acids and is then precipitated in an aqueous NMMO solution. Thus, a suspension of fine chitosan crystals is obtained in the cellulose solution, which then is spun. According to said document, the chitosan remains in the solution in the form of fine crystals even after the dissolution of the cellulose. That leads to the formation of a micro-heterogeneous two-phase system in the fiber. The strength of the fiber is low (with 10% chitosan: fiber strength conditioned 19.4 cN/tex; fiber elongation conditioned 11.5%).
[0027] WO 04/007818 proposes the incorporation of a chitosonium polymer (a chitosan salt with an inorganic or organic acid), which is soluble in the spinning solution, by means of adding to the spinning solution or a precursor thereof into the Lyocell fiber.
[0028] Alternatively to incorporation, there is provided the possibility to provide textile fabrics with chitosan in the course of their preparation and production. Applying chitosan onto already fabricated fibers or textile articles containing these, is in the following also designated as “impregnation”. A fundamental problem in this connection, however, is that the chitosan applied in this way is not fixed and may be washed out rather quickly, in this way losing its positive effects.
[0029] In order to provide a solution to this problem, there is proposed in EP 1 243 688 the use of chitosan nano-particles for the fabrication of fibers, yarns, knitted and textile fabrics. Nano-chitosans are nearly spherical firm bodies having a mean diameter in the range of 10 to 300 nm, which are arranged inbetween the fibrils due to their small particle diameter. The fabrication of nano-chitosans is realized by means of spray drying, evaporation technique or depressurizing of supercritical solutions.
[0030] WO 01/32751 describes a process for the production of nano-particular chitosan for cosmetic and pharmaceutical preparations having a particle diameter of 10 to 1,000 nm, wherein the pH of an aqueous, acid chitosan solution in the presence of a surfactant is increased until the chitosan will precipitate. Furthermore, there is described in WO 91/00298 the preparation of micro-crystalline chitosan dispersions and powders with a particle diameter of 0.1 to 50 μm, wherein the pH of an aqueous, acid chitosan solution is increased until the chitosan will precipitate.
[0031] WO 97/07266 describes the treatment of a Lyocell fiber with a 0.5% acetic chitosan solution.
[0032] WO 2004/007818 describes, apart from the incorporation of a chitosonium polymer in Lyocell fibers, also the treatment of never-dried Lyocell fibers with the solution or suspension of a chitosonium polymer. It has been shown that this process is only suitable for the treatment of never-dried Lyocell fibers.
[0033] The term “never-dried” designates the status-quo of a freshly-spun fiber that has never been subjected to a drying step.
[0034] The treatment of other fiber types than never-dried Lyocell fibers (e.g. Modal fibers and viscose fibers) is not possible with the process according to WO 2004/007818.
[0035] In the Austrian patent application A 82/2008 (not pre-published) there is described a process, wherein a cellulosic molded body is contacted with an alkaline dispersion containing non-dissolved chitosan particles.
SUMMARY OF THE INVENTION
[0036] The present invention aims at providing a process for the treatment of cellulosic molded bodies, wherein the above mentioned problems of incorporating chitosan in fibers do not exist and which is suitable for different cellulosic fiber types, in a dried as well as never-dried state. The chitosan is to be fixed in particular at the fiber surface of cellulose regenerate fibers (Lyocell fibers, Modal fibers, viscose fibers, polynosic fibers) preferably in the fabrication process, so that the chitosan will still be existent at the final product even after a series of domestic washing processes.
[0037] This aim is reached by means of a process for the treatment of a cellulosic molded body, wherein the molded body is contacted with an acid solution of a chitosan, which is characterized in that the chitosan has a deacetylation degree of at least 80%, a nitrogen content of at least 7 w %, preferably at least 7.5%, a weight average molecular weight M w (D) of 10 kDa to 1000 kDa, preferably 10 kDa to 160 kDa and a viscosity of 1 w % solution in 1 w % acetic acid at 25° C. of 1000 mPas or less, preferably 400 mPas or less, particularly preferably 200 mPas or less.
[0038] Surprisingly, there has been shown that it is possible to sustainably apply chitosan to the surface of cellulosic molded body, if the molded body is treated with an acid solution containing the above specified chitosan. In particular, there was found a surprising correlation between the viscosity of chitosan in acid solution and the amount of coating obtainable in the treatment of the molded body: The lower the viscosity of a chitosan in acid solution is, the higher (this is: significantly higher) is the obtainable amount of coating on the molded body.
[0039] In this way, there may be obtained sufficient amounts of coating with comparably little effort.
[0040] The term “solution of a chitosan” means that the chitosan is present in a completely dissolved form. This term, however, does not exclude the presence of further, optionally undissolved ingredients in the treatment liquid.
[0041] For the use in the process according to the invention, chitosans with a viscosity of 1% solution in 1% acetic acid at 25° C. of 1000 mPas or less, preferably 400 mPas or less, particularly preferably 200 mPas or less, measured with a Brookfield Viscosimeter at 30 rpm, are suitable.
[0042] Furthermore, the deacetylation degree of the chitosan is of importance, too: the higher the deacetylation degree is, the better suitable is the chitosan for a use in the process according to the invention.
[0043] Suitable chitosans may in particular have a polydispersity (ratio between weight average and number average of the molecular weight) of 2 to 4.
[0044] In the literature, there is not given a uniform definition for distinguishing between chitin and chitosan.
[0045] For the purpose of the present invention, the term “chitin” is meant to indicate a β-1,4-bound polymer of 2-acetamido-2-desoxy-D-glucose having a degree of deacetylation of 0%. Also for the purpose of the present invention, the term “chitosan” indicates an at least partially deacetylated β-1,4-bound polymer of 2-acetamido-2-desoxy-D-glucose.
[0046] The process according to the invention has the advantage in comparison to the known processes for the incorporation of chitosan that an incorporated chitosan within the molded body is not accessible. Only chitosan at the surface of the molded body may come into contact with the skin and, in this way, devolve its positive effects. In order to obtain the same amount of chitosan as in the impregnation at the surface of a molded body, there have to be used significantly larger amounts of chitosan than for incorporation.
[0047] In comparison to the use of nano-chitosan, the high production costs of nano-chitosan are in particular advantageous.
[0048] In regard to the process described in WO 2004/007818, the process according to the invention has the advantage that the therein described impregnation with an acid solution of a chitosonium polymer does not work in the treatment of never-dried viscose, Modal or polynosic fibers with subsequent vapor treatment. There are obtained only very little amounts of chitosan coating, while this process cannot be performed without the reconstruction of already existing plants.
[0049] In addition, the process according to the invention is cheaper than the process described in WO 2004/007818, as there may preferably be used cheaper types of chitosan (see further below).
DESCRIPTION OF THE FIGURES
[0050] For a more complete understanding of the present invention, and the advantages thereof, reference is made to the following descriptions taken in conjunction with the accompanying FIGURE, in which
[0051] FIG. 1 is a graph showing the amount of chitosan coating on cellulose fibers in accordance with an exemplary embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0052] According to a preferred embodiment of the process according to the invention, the content of chitosan particles in the solution is 0.1 to 10 w %, particularly preferable 1 to 4 w %.
[0053] The molded body that is treated according to the invention is preferably present in the form of fibers. The fibers may in particular be Lyocell fibers, Modal fibers, polynosic fibers and/or viscose fibers.
[0054] The generic name “Lyocell” was issued by the BISFA (The International Bureau for the Standardisation of Man Made Fibers) and stands for cellulose fibers, which are prepared from cellulose solutions in an organic solvent. Tertiary amine oxides, in particular N-methyl-morpholine-N-oxide (NMMO), are preferably used as solvents. A process for the production of Lyocell fibers is e.g. described in U.S. Pat. No. 4,246,221.
[0055] Viscose fibers are fibers obtained from an alkaline solution of the cellulose xanthogenate (viscose) by means of precipitation and regeneration of the cellulose.
[0056] Modal fibers are cellulose fibers characterized according to the BISFA definition by high wet strength and a high wet modulus (the force necessary to expand a fiber in its wet state by 5%).
[0057] For the treatment with the chitosan solution, the fibers may be present already in dried form, in particular as integral part of a textile article, preferably a yarn, a knitted fabric, a piece of cloth produced therewith or a non-woven article.
[0058] “Already dried” fibers are fibers which have been subjected in the course of their process of production to a drying step at least once.
[0059] Preferably, however, the fibers may be present in never-dried form. A fiber is designated as “never-dried” if it has never been subjected to a drying step in the course of its fabrication. The fibers may be present in particular in the form of a fiber fleece, as it is produced in the course of the production of Lyocell, Modal and polynosic staple fibers as an intermediary product.
[0060] This variant has the advantage that the treatment may be implemented without requiring changes or modifications in apparatuses in an existing plant for the production of Lyocell, viscose, Modal or polynosic fibers. A treatment with never-dried viscose, Modal or polynosic fibers with chitosan during the process of production has not been possible so far.
[0061] The fibers may have residual moisture of 50% to 500% before treatment.
[0062] After treatment with the chitosan solution, the molded body may be subjected to a treatment with hot vapor. In this way, there may be obtained additional fixation of the chitosan on the surface of the molded body.
[0063] In order to produce the solution, there is preferably dissolved chitosan in an inorganic or organic acid.
[0064] The acid is preferably selected from the group consisting of mono-, di- or tricarboxylic acids with 1 to 30 C-atoms, preferably lactic acid, acetic acid, formic acid, propionic acid, glycolic acid, citric acid, oxalic acid and mixtures thereof.
[0065] It has been shown that the amount of acid necessary for the dissolution of the chitosan is dependent on the deacetylation degree.
[0066] The amount of acid necessary for the dissolution of the chitosan is calculated, dependent on the deacetylation degree of the chitosan used, as follows:
[0000]
TABLE 1
Deacetylation
Mol acid
degree chitosan in %
per g chitosan
80%
0.00493
85%
0.00525
90%
0.00555
95%
0.00586
100%
0.00617
[0067] For the preparation of the chitosan solution there are added the above described necessary amounts of acid and water to the respective amount of chitosan under stirring, and the ingredients are then stirred until a clear solution is formed.
[0068] The chitosan solution obtained in this way may be contacted with an initially moist regenerated cellulose fiber fleece, which is adapted to a defined moisture of 50% to 500% by means of pressing. The fiber fleece may e.g. be soaked by means of spraying. For this reason, in plants for the production of viscose fibers and Modal fibers the so-called bleach field may be used, without the necessity of restructuring the existent production plants.
[0069] After impregnation, the fiber fleece may be pressed to a defined moisture of 50%-500%, and subsequently the pressed treatment liquor may be returned into the impregnation cycle.
[0070] Thereafter, the fiber fleece will either be treated with hot vapor and subsequently neutrally washed, or it will be neutrally washed without hot vapor treatment, lubricated and dried.
[0071] The determination of the amount of chitosan coating is carried out by means of measuring the nitrogen content using the LECO FP 328 nitrogen analyzer by burning up the sample. By means of FITC (fluorescein-isothiocyanate) staining of the fibers and subsequent examination of the fibers using the fluorescence microscope, the chitosan distribution on the fiber surface may be observed.
[0072] In another preferred embodiment, the molded body will be subjected to the treatment with a crosslinking agent before or after the drying step.
[0073] The present invention in addition relates to a molded body, which is obtainable by the process according to the invention.
[0074] The molded body according to the invention has a chitosan content with the above defined specifications, wherein the chitosan is essentially completely distributed at the surface of the molded body (and not in an essential amount also inside the molded body).
[0075] The molded body according to the invention may be present particularly in the form of fibers, preferably Lyocell fibers, Modal fibers, polynosic fibers and/or viscose fibers.
[0076] One feature of the molded body obtainable by the process according to the invention is that the chitosan is film-like distributed on the surface of the molded body.
[0077] The molded body according to the invention has preferably a chitosan content of 0.1 w % and more, preferably 0.2 w % to 1 w %, particularly preferably 0.4 to 0.6 w %. It has been shown that there is obtained in particular a good antibacterial effect of the molded body according to the invention already at small amounts of coating starting at 0.1 w %.
[0078] The present invention also relates to the use of a molded body according to the invention as an antibacterial product, as odour-reducing product, as wound healing, styptic and blood coagulation promoting product, in non-woven products and/or as a filling fiber. Preferred areas of use and application of chitosan containing regenerated cellulose fibers according to the invention comprise, due to the mildly antibacterial, odour-reducing and skin-friendly properties, textiles that are worn close to the skin, e.g. underwear or socks, textiles for individuals with sensitive skin (neurodermatitis), bed lining and homewear goods. As a filling fiber, the fiber according to the invention may be used alone or also in mixtures with other fibers, e.g. cotton, polyester fibers and non-modified cellulose fibers (e.g. Lyocell fibers).
[0079] In particular there was found out that regenerated cellulose fibers according to the invention have a significantly antibacterial effect already at an amount of chitosan coating of 0.1% in the Shake Flask Test and that they are cell proliferation promoting in the regenerating epidermis (tested in the porcine ex-vivo wound healing model).
[0080] The present invention, hence, relates in another aspect also to a molded body according to the invention, in particular with a chitosan content of 0.2 w % to 1 w % for the specific use as wound healing product, in particular as a product promoting the cell proliferation in the regenerating epidermis.
[0081] In the following, the invention is further explained in greater detail by means of nonlimiting examples and the figures.
[0082] For this reason, FIG. 1 shows the amounts of chitosan coating obtained on various cellulose fibers using the process according to the invention, in dependency of the viscosity of the used chitosan.
EXAMPLES
Example 1
[0083] There were used the following chitosan types for the treatment of cellulose fibers:
[0000]
TABLE 2
Viscosity
Deacetylation
Company
Type
Batch n o
mPas
degree %
Primex
ChitoClear cg110
TM2881
159
82
Primex
ChitoClear cg110
TM3013
108
80
Primex
ChitoClear cg110
TM3089
58
81
Primex
ChitoClear cg10
TM2963
19
81
Primex
ChitoClear fg95LV
TM3091
15
96
Primex
ChitoClear
TM2875
9
85
fg95ULV
Heppe
85/200/A1
200
85
Heppe
85/400/A1
400
85
Heppe
90/10/A1
6
90
[0084] From these chitosan types, there was prepared respectively a 1 w % chitosan solution in aqueous lactic acid. The respective amount of lactic acid used was defined according to the above table 1 in dependency on the deacetylation degree of the used chitosan.
[0085] Fiber Samples Used:
[0086] 1.3 dtex Lyocell fiber, NMMO-free washed, never dried
[0087] 1.3 dtex Modal fiber, not bleached, never dried
[0088] 1.3 dtex viscose fiber, not bleached, never dried
[0089] Approach for the fiber treatment:
[0090] The never-dried fibers were impregnated with the respective chitosan solution for 5 minutes at room temperature in a liquor ratio of 1:10, pressed with 1 bar, then steamed for 5 minutes at 100° C./100% relative moisture, washed and dried at 60° C.
[0091] The results of the tests are summarized in the following table.
[0000]
TABLE 3
Amount of
Chitosan type
chitosan coating in w %
Batch N o /Type
Lyocell
Modal
Viscose
TM2881
0.34
0.25
0.27
TM3013
0.30
0.23
0.25
TM3089
0.33
0.21
0.22
TM2963
0.42
0.25
0.33
TM3091
0.41
0.26
0.36
TM2875
0.53
0.32
0.38
85/200/A1
0.31
0.24
0.28
85/400/A1
0.26
—
—
90/10/A1
0.66
0.65
0.63
[0092] All fiber samples thus prepared were subjected to hot water treatment in a liquor ratio of 1:20 for 40 minutes at 90° C. The chitosan coatings were shown to be permanent.
[0093] The determination of the amount of chitosan coating on the fiber is carried out by measuring the N content (LECO FP 328 nitrogen analyzer) through burning the sample.
[0094] A FITC (fluorescein-isothiocyanate) staining of the fibers and subsequent examination of the fibers using the fluorescence microscope were performed in order to analyze the chitosan distribution on the fiber surface.
[0095] From the following table, there may be clearly seen for all three fiber types that—in the case of the same w % concentration of chitosan—the lower the viscosity of the solution is, the higher the obtained amount of chitosan coating o will be. Furthermore, the highest amounts of chitosan coating will be obtained at the Lyocell fiber, as these have evidently a better accessible pore system in their initially moist state.
[0000]
TABLE 4
Viscosity of the
Amount of
chitosan solution
chitosan coating in w %
1% in acetic acid mPas
Lyocell
Modal
Viscose
400
0.26
Not tested
Not tested
200
0.31
0.24
0.28
159
0.34
0.25
0.27
108
0.30
0.23
0.25
58
0.33
0.21
0.22
19
0.42
0.25
0.33
15
0.41
0.26
0.36
9
0.53
0.32
0.38
6
0.66
0.42
0.47
[0096] This correlation is presented in a diagram in FIG. 1 .
Example 2
Preparation of a Lyocell Fiber in a Production Test
[0097] There was treated a Lyocell fiber with a titer of 1.3 dtex and 38 mm cutting length with chitosan.
[0098] The never-dried Lyocell fiber prepared according to the teaching in WO 93/19230 was impregnated according to the process described in example 1 with 1 w % chitosan solution in lactic acid (chitosan type: TM2875, see table 1) in a liquor ratio of 1:20 for an intended amount of coating of 0.4 w % chitosan, vapored, lubricated and dried. From the thus prepared fibers, there was spun yarn n° 50 and processed into a textile fabric (Single jersey knitted fabric), which was shown to have an amount of chitosan coating of 0.45%.
[0099] These knitted samples were, in comparison to bleached cotton and Lyocell fibers not treated with chitosan, tested in the porcine ex-vivo wound healing model in the University Hospital Hamburg Eppendorf, Cell-Biological Laboratories, on the portion of proliferative cells at the wound edge in the regenerating epidermis and the part of the epidermis not involved. There were found significantly more proliferative cells at the wound edge and in tendency also more proliferative cells in the regenerating epidermis of the chitosan containing fiber than in a not-treated Lyocell fiber and cotton.
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The present invention relates to a process for the treatment of a cellulosic molded body, wherein the molded body is contacted with an acid solution of a chitosan. The process according to the invention is characterized in that the chitosan has a deacetylation degree of at least 80%, a nitrogen content of at least 7 w %, preferably at least 7.5 w %, a weight average molecular weight M w (D) of 10 kDa to 1000 kDa, preferably 10 kDa to 160 kDa, and a viscosity in 1 w % solution in 1 w % acetic acid at 25° C. of 1000 mPas or less, preferably 400 mPas or less, in particular preferably 200 mPas or less.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to circuits for measuring the time between two voltage transitions, and more particularly to a circuit for converting a time period to a dc voltage proportional to such period.
2. Description of the Prior Art
There are many requirements in the electronic art for obtaining quantitative measurements of time periods such as propagation delay, rise time, pulse widths, and periods of repetitive waveforms. A typical technique is described in U.S. Pat. No. 3,588,699 to Pysnik which measures the time between two signals utilizing voltage-controlled multivibrators. Janowitz et al in U.S. Pat. No. 3,999,128 teach the use of a comparator and sample and hold circuitry in driving a digital voltmeter. Other relevant U.S. patents are as follows: U.S. Pat. Nos. 3,461,392 to Hughes et al; 4,025,848 to Delagrange et al; 3,537,018 to Modiano; 4,246,497 to Lawsen et al; 3,940,693 to Brown; 3,787,765 to Morrow et al; and 3,805,153 to Gallant.
SUMMARY OF THE INVENTION
The present invention utilizes a constant current source to charge a reference capacitor via high speed analog switches. The current source is in series with first switch and the reference capacitor and in parallel with a second switch. When the first switch is closed and the second switch is open, the capacitor will accept a charge from the current source producing a linear voltage ramp across the capacitor proportional to the charging time.
When the second switch and first switch are closed, the capacitor will discharge. The analog switches may be controlled by two input signals. Assuming that both switches are closed and the capacitor is discharged, the second switch is opened and the first switch is closed by a first input signal permitting the capacitor to charge linearly. A second input signal opens the first switch and closes the second switch, diverting the constant current and leaving a charge on the capacitor. As may now be understood, the voltage across the capacitor is a measure of the length of time between the occurrence of the first and second input signals.
The capacitor voltage may be measured by means of a suitable voltmeter which may be calibrated in time increments.
In a preferred embodiment of the invention, the two inputs drive high-speed voltage comparators which control the analog switches. A high-input impedance voltage follower is connected across the capacitor to permit the voltage to be read out without excessive loading.
When periodic signals are applied to the inputs, both switches will close between signals, discharging the capacitor. A sample and hold circuit connected to the voltage follower may be used to hold the output voltage for measurement thereof.
It is therefore a principal object of the invention to provide a time to voltage converter for measuring time characteristics of electronic waveforms.
It is another object of the invention to provide a constant current source for charging a capacitor via switches controlled by electronic waveforms to be measured.
It is still another object of the invention to provide a time measurement circuit that can be implemented by an integrated circuit module.
These and other objects and advantages of the invention will become apparent from the following detailed description when read in conjunction with the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a simplified equivalent circuit of a portion of the invention used to illustrate the principle thereof;
FIG. 2 is a set of waveform diagrams relating to FIG. 1;
FIG. 3 is a state table relating the waveforms of FIG. 2 to the circuit of FIG. 1;
FIG. 4 is a block diagram of a preferred embodiment of the invention;
FIG. 5 is a more detailed schematic diagram of the circuit of FIG. 4; and
FIG. 6 is a schematic diagram of the invention implemented as an integrated circuit chip.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The principle of the time to voltage converter may be explained with reference to FIGS. 1 through 3. In FIG. 1 is shown an equivalent circuit diagram of the voltage generating portion of the invention having a constant current source 5 which may be 10 milliamps for exemplary purposes. Constant current source 5 is in series with reference capacitor 10 (C) and first switch 6 designated as S 1 . A second switch 8 designated as S 2 is in parallel with constant current source 5.
The operation of the circuit of FIG. 1 may be understood with reference to FIG. 2 in which the time between the occurrence of two pulses is to be measured. The first waveform at input A is seen to have a transition at t 0 while a second waveform on input B has a transition at t 1 . Prior to the occurrence of the transition on input A at t 0 , it is assumed that first switch 6 and second switch 8 are both closed as indicated in the chart of FIG. 3. As will be described in more detail hereinafter, the invention includes means associated with second switch to cause it to open when the transition on input A occurs at t 0 . Similarly, means are included associated with second switch 8 to cause it to close at a transition of the waveform on input B and with first switch 6 open at the transition such as indicated at t 1 . Thus, at t 0 , switch 6 (S 1 ) will be closed and switch 8 (S 2 ) will be open.
Assuming that a transition occurs in the waveform on input B τ seconds later at t 1 , switch 6 opens and switch 8 closes. Therefore, capacitor 10 ceases to charge. As may be noted from waveform V c , capacitor 10 starts charging at t 0 , with voltage V c rising linearly to time t 1 . V c thereafter will remain charged to a value V 1 until discharged.
At time t 2 , a transition occurs in the waveform at A with the opposite polarity to the transition at t 0 , causing switch 6 to close, discharging capacitor 10 through switches 6 and 8, causing V c to drop to zero.
As may now be understood, a first waveform occurring at input A will trigger comparator 15, causing current source 5 to start charging capacitor 10 via switch 20. A second, later waveform at input B triggers comparator 16, causing switch 20 to open. Capacitor 10 will hold the charge accumulated thereon between the time of occurrence of the first waveform and the time of occurrence of the second waveform. The voltage across capacitor 10 is applied to a high impedance input voltage follower 24 to produce an output to a suitable indicator.
If the inputs on A and B are periodic waveforms, the output will be a series of periodic pulses such as shown on line V c of FIG. 2. To be able to measure the voltage V 1 , a sample and hold circuit 22 is provided. Sample and hold control circuit 26 is sensitive to the slope of the pulses on input A and B. High speed analog switch 28 is controlled to transfer the ouput from voltage follower 24 to capacitor 30 (C 2 ) which holds the charge after V 1 has dropped to zero, for example, at t 2 . Voltage amplifier 32 isolates the voltage across capacitor 30 from the sample and hold output.
As will now be apparent, the time between t 0 and t 1 has been converted to a voltage V 1 . As will be discussed below, the voltage V 1 can be sampled and held for operation of a voltmeter calibrated in time.
Assume that capacitor 10 in FIG. 1 has a capacity of 1000 pF, current source 5 produces 10 ma and a voltage of 1 volt occurs across capacitor 10. The time τ between t 0 and t 1 is: ##EQU1##
Thus, in this example, the calibration is one nanosecond per 0.01 volts.
Turning now to FIG. 4, a block diagram of a preferred embodiment of the invention is shown suitable for measuring time intervals between a signal on input A and a signal on input B. The A signal is applied to an input of comparator 15. A threshold for triggering comparator 15 is set by control potentiometer 17. When the waveform on input A experiences a transition which exceeds the selected threshold, the logic level at the output of comparator 15 will change from ONE to ZERO or vice versa, depending upon the direction of the transition. The B signal drives comparator 16 having its threshold controlled by potentiometer 18. High speed analog switch 18 is opened by the logic level produced by triggering of comparator 15 and high speed analog switch 20 is similarly controlled by comparator 16. A constant current source 5 is provided to charge capacitor 10 when switch 20 is closed and switch 18 is open.
In FIG. 5, a detailed schematic of the preferred embodiment of the invention is presented. Comparator 15 includes comparator amplifier 25 and exclusive OR gate 21. Comparator 15 may be a type NE527 and gate 21 may be a type 74F86. Similarly, comparator 16 includes comparator amplifier 27 and exclusive OR gate 23. Comparator 15 controls high speed analog switch 18 while comparator 16 controls switch 20. Switches 18 and 20 may be types SD214.
Constant current source 5 is implemented by transistor 50 which may be a type 2N2907 in which the base bias is regulated by regulator 51. Sample and hold control 26 utilizes an exclusive OR gate 35 driven from gate 21 and exclusive OR gate 37 driven from gate 23. Gates 35 and 37 may be types 74F86. These gates control high speed analog switch 28 which may be a type SD214. Voltage follower 24 is connected to capacitor 10 and voltage follower 32 is connected to sample and hold capacitor 30 and may be types CA3140.
As will be noted, comparator amplifiers 25 and 27 each have a negative bias. To select the slope of the signals on inputs A and B which will produce an enabling logic level to switches 18 and 20, excusive OR gates 21 and 23 are controlled by manual selector switches 63 and 64. As will be recognized, a negative-going transition of the waveforms on input A may produce either a ONE or a ZERO at the control electrode of switch 18, depending upon the setting of switch 63.
The various solid state integrated circuits or equivalents shown in FIG. 5 are available as chips. By assembling such chips on a substrate 60, an LSI circuit shown in FIG. 6 may be fabricated. As will be noted, constant current adjustment 61 (R 1 ) is outboard of LSI circuit 60 to permit calibration of the output signal. Similarly, logic level adjustment 62 (R 2 ) is external to permit setting of the turn-on level of switch 18. Slope selector switches 63 and 64 are outboard of substrate 60 as are threshold controls 17 and 19. Advantageously, the LSI circuit may be made available to the industry for inclusion in a wide variety of instruments and electronic devices where measurements of time intervals or control related to time intervals are required.
Although the invention has been disclosed with reference to a specific circuit and preferred components, it will be obvious to those of skill in the art to make various changes and substitutions without departing from the spirit and scope of the invention.
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A constant current source is provided to charge a reference capacitor. The current is switched to the capacitor by a first high-speed analog switch when a first event occurs and the current is turned off by a second high-speed analog switch when a second event occurs. The voltage produced by the charge on the capacitor is proportional to the time between events. A sample and hold circuit maintains the maximum voltage on the capacitor when the events are periodic.
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BACKGROUND OF THE INVENTION
The invention relates to an improved automatic straight knitting machine.
DESCRIPTION OF THE PRIOR ART
As is known, the needle beds of an automatic straight knitting machine are provided with slits that are equidistant and perpendicular to the direction in which the carriage moves. Provided in each slit, starting at the top and working downwards, there is, in the order stated, a needle, an intermediate blade element and a bottom blade element that is destined to carry the blade in operation (obviously with the synchronous movement of the intermediate blade element).
The bottom blade element is provided with a first butt and a second butt, the latter destined, in cooperation with a corresponding selector element with which the carriage is equipped, to select the appropriate blade element. The said selection is defined by a predetermined upward movement on the part of the blade element that is sufficient to position the first butt in the path of one or more fixed cams, integral with the carriage, which by intercepting the said first butt carry upwards the bottom blade element (and consequently the also the intermediate blade element) plus the corresponding needle, causing this to be set in action.
In each carriage, and for each needle bed, provision is made for one or more sets of selector elements, and in each of these the elements are perpendiculatly to the direction in which the carriage moves. Controlled for example by an electromagnet, each selection element is able to move between a non-operative position and an operative position, the latter bringing about the interception of the second butt of the corresponding bottom blade element. Obvious is the advisability of increasing the number of selector elements in each set since, with each working travel of the carriage, each said set is able to select an identical number of blade elements.
The foregoing necessitates the use of selector elements of a volume height-wise (that is to say, in the direction perpendicular to that in which the carriage moves) that is limited; in other words, such as to allow each element to be inserted between a pair of second butts belonging to two consecutive blade elements, in such a way that the said element intercepts the corresponding butt and not that of the following (or preceding) blade element. The said requirement leads necessarily to limiting the upward movement of the second blade element (if selected) and thus to very narrow tolerances, one with respect to the other, in the positioning of the blade elements, the selector elements and the fixed cams.
In the event of the selector element operating sluggishly on the corresponding butt, or intercepting this imperfectly, the upward movement of the blade element is below the preestablished value causing either non-interception of the first butt on the part of the fixed cam (the less disastrous hypothesis), whereby the corresponding needle is not carried into operation, or the breakage of the said first butt against the front end of the said cams.
SUMMARY OF THE INVENTION
The object of the invention is, therefore, to make available an improved automatic straight knitting machine whose conformation is such as to simplify the necessary sequence for carrying the needles into operation, and to do so in a way that is extremely functional, briefly timed, and exercises a notably positive effect on the operating speeds of the said machine, without any danger of the blade elements breaking.
The said object is achieved with the machine according to the invention, comprising, among other things, at least one flat longitudinal needle bed provided with transverse equidistantly made slits, in each of which is inserted, commencing at the top and working downwards, a needle with the corresponding blade element, the latter provided with at least two butts, namely a first butt and a second butt, that project from the front side of the needle bed, a carriage being connected to this, able to reciprocate longitudinally, in turn comprising: firstly, selector elements, symmetrical with respect to a transverse plane and movable between two positions, that is to say, a non-operative position and an operative position, the latter for intercepting the first butt of a corresponding blade element, with the consequent raising of this from a neutral position to a first intermediate position; secondly, means destined to raise the said blade element from the first intermediate position to a second intermediate position; thirdly, means for intercepting the said second butt in order, first of all, to raise the said blade element from the second intermediate position to a maximum elevated position, with the corresponding needle sent into operation, and then to lower the said blade element down to the said neutral position; the said machine being characterized by the fact that the said means for raising the said blade element from the first inter mediate position to the second intermediate position comprise, on each blade element, a third butt oriented in like fashion to the other butts, positioned beneath the second butt and connected thereto through a tailpiece restrained to elastic means such as to permit the said tailpiece to undergo oscillations over the transverse plane of the slit in which the said blade element is received; the said raising means also comprising an operating cam, integral with the carriage, that exerts an effect on the said third butt in order to uplift the corresponding blade element from the said first intermediate position to the said second intermediate position solely when the said blade element is in the said first position, or in order to guide the said third butt, and thus the corresponding blade element, into the said neutral position or into a position in between this and the first intermediate position.
BRIEF DESCRIPTION OF THE DRAWINGS
The characteristics of the machine according to the invention will become more apparent from the description of two preferred embodiments given hereinafter, with reference to the accompanying tables of drawings, in which:
FIGS. 1 and 1a each show, in a lateral view, a blade element and the elastic means connected thereto;
FIG. 2 shows, diagrammatically in a front view, the carriage and the most significant positions adopted by a blade element selected by the said carriage;
FIG. 3 shows, in a perspective view, a first embodiment for the fixed operating cam that is destined to raise the blade element from the first to the second intermediate position, and also shows, with an unbroken line and in dashes, the most significant positions adopted by a blade element with respect to the said fixed cam;
FIGS. 4a and 4b show, diagrammatically, a view along the line I--I and along the line II--II in FIG. 2, respectively, with the operating cam depicted in FIG. 3;
FIGS. 5a and 5b show, diagrammatically, the commencement and end of the interception of a selector element against the first butt of the corresponding blade element;
FIG. 6 shows, in a perspective view, a second embodiment for the fixed operating cam;
FIG. 7 shows, again in a perspective view, an enlarged part of the cam depicted in FIG. 6, as well as certain positions the said cam obliges a blade element, not selected in an optimum way, to adopt.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to FIGS. 1 to 5, shown at 1 a diagrammatic view is a carriage of an automatic straight knitting machine, that slides above a needle bed (not illustrated since of a known type) in which are provided slits 3 (one of which is shown with dashes) perpendicular to the direction in which the carriage moves (directions T1 and T2).
Freely inserted in each slit at the top is a blade element 4 (shown partially with dashes), the upper part of which is provided with a (non-illustrated) needle of a known type.
Below a butt 4a of the blade element 4, freely inserted in the said slit is a blade element 5 provided, commencing at the bottom and working upwards, with a butt 2 and subsequently with three butts 6,7 and 8, namely a first butt, a second butt and a third butt, the last mentioned one of which is carried by a tailpiece 35 in which, transversely, there is suddenly a reduced area 35a: this allows the said tailpiece to bend (direction H) in the presence of corresponding stress pressing on the third butt 8.
In the support structure of the carriage 1 are provided sets of bushes 9 (eight per set in the case under examination), the axes of the bushes in each set being situated in a plane perpendicular to the directions T1 and T2. Freely inserted in the said bushes are corresponding rods 10 provided with selector elements 11, each of which having two inclined surfaces 11a and 11b, respectively, that are symmetrical with respect to the said plane.
Each said rod is rendered movable from a non-operative position I to an operative position O, more about which will be said below.
Provision is made beneath the selector elements 11 in each set for a fixed operating cam 12, symmetrical with respect to the vertical plane of simmetry of the said elements 11, so positioned as to define, between the upper end 12a thereof and the lowest element 11 in the said set, a longitudinal housing 20 through which, as will be said in the ensuing text, the second butt 7 can pass. In the cam 12 there is a longitudinal race 16 (constituted by a central horizontal section 16a and two inclines 16b, one for entering and the other for leaving the said central section) positioned in such a way as to intercept the third butt 8 when the blade element 5 is in the neutral position R. The said interception causes the tailpiece 35 to undergo elastic flexure, in the direction H as stated above, in the plane of the corresponding slit 3.
In the cam 12 there is, above the race 16, a cutaway 40, the lower part of which is delimited by a central horizontal section 40a, at a right angle, adjacent to and inside with respect to the said horizontal section 16a, by two ascendant inclines 40b (that fork symmetrically with respect to the central section 40a) and, lastly, by two upper horizontal sections 40c.
In between a group of selector elements 11 and the one following on, or previous thereto, placed in an inside position with respect to the upper sections 40c of two consecutive cams 12, is a set of fixed cams 50 consisting, in the case under examination, of three cams 13, 14 and 15 symmetrical with respect to a plane equidistant from the planes of symmetry of two consecutive groups of selector elements 11.
Each selector element 11 is destined, when in the operative position O, to intercept the first butt 6 of the corresponding blade element 5. In the case described herein, the butt 6 of a blade element is intercepted by the selector element 11 that is the last but one from the bottom.
While in reality the blade element 5 is stationary, the carriage moves in the direction T1 or T2. Since this a question of relative motion between the blade element and the carriage, in FIG. 2 the carriage is supposed to be stationary and the blade element 5 to be moving in the direction T2, which is equivalent to considering the blade element 5 to be stationary and the carriage to be moving in the direction T1.
A description is now given of the operation of the improved machine according to the invention, with particular reference to the two characteristic situations, namely when a blade element is selected or not selected.
The former situation occurs with the selector element 11 in the non-operative position I (FIG. 4b). In this case, the blade element 5 stays in the neutral position R, the butt 7 passes through the longitudinal housing 20, while the interception against the butt 8 of the race 16 causes in the tailpiece, in the order stated, a gradual increase in deflection (ingoing incline 16b), constant deflection (central section 16a) and, lastly, a gradual decrease in deflection until zeroed (outgoing incline 16b).
For the latter situation, the selector element 11 is in the operative position O (FIGS. 5a and 5b). An examination follows of the various displacements to which the blade element is subjected (with reference to FIGS. 2, 3, 5a and 5b). The butt is intercepted by the ingoing incline 16b of the race 16 and, subsequently, by the central section 16a thereof. This causes, as will be recalled, the deflection of the tailpiece 35 towards the inside of the corresponding slit. With the butt 8 intercepted by the initial part of the section 16a, the lower part of the butt 6 is intercepted by the surface 11a of the selector element 11; this causes the blade element 5 to be raised from the neutral position R to a first intermediate position R1.
In consequence of the said elevation, the butt 8 is jerked into insertion in the cutaway 40 (this being facilitated by the elastic pressures of the tailpiece 35 previously subjected to flexure by the ingoing incline 16b): this is illustrated in FIG. 3 through the positions H11 and H2 (shown with dashes) of the blade element 5 prior to and after the butt 8 being jerked into insertion in the cutaway 40.
With the blade element in position R1 the interception takes place (because of the movement in direction T1 of the carriage) of the ascendant incline 40b against the lower part of the butt 8 (for example position H3 shown with dashes in FIG. 2). This brings about a further elevation of the blade element 5 which is carried into a second intermediate position R2 defined by the said upper horizontal section 40c.
The interception of the surface 13a of the cam 13 against the lower part of the butt 7 occurs when the blade element is in position R2 (again as a consequence of the movement in direction T1 of the carriage). This causes a further, final, elevation of the blade element 5 from position R2 to position R3 (the maximum raised position) whereby the corresponding needle (with which the blade element 4 is provided) is carried into operation.
Finally, with the movement in the direction T1 of the carriage, the interception takes place of the surfaces 14a and 15a of the cams 14 and 15, respectively, against the upper part of the butt 7 whereby the blade element 5 is lowered from position R3 down to the said neutral position R.
Since the cams 12,13,14 and 15, and the selector elements 11 are symmetrical with respect to corresponding vertical planes, the same considerations as above apply as regards the movement in the direction T2 of the carriage.
It is stressed that the raising of the blade element from position R1 to position R2 is dependent on the insertion into the cutaway 40 of the butt 8 which, moreover, is aided by the elastic pressure of the tailpiece 35. This is of the utmost importance since, should the elevation (from R to R1) effected by the selector element 11 be below a predetermined value, the butt 8 continues to stay on the race 16, while the blade element is only raised a little from the position R and so the interception of the cam 13 against the butt 7 fails. Subsequently it will be up to the cam 15 to realign the blade element 5 in the neutral position R.
In other words, unsatisfactory action on the butt 6 on the part of the selector element 11 causes solely the needle connected to the selected blade element "not to be sent into operation" without any danger of the breakage of the butts of the said element, this remaining sound and suitable to be selected (eventually) by the group of selector elements 11 that succeds the previous group.
The lower part of the cam 12 is provided, in the second embodiment (FIGS. 6 and 7), with a longitudinal race 53 interrupted centrally by a re-entrant part 54 that is symmetrical with respect to the vertical plane of symmetry of the selector elements 11. The said re-entrant part 54 divides the race into two parts 53a and 53b, respectively, and these commence with a rectilinear section that joins, without any break in continuity, an upward curved section.
Above the race 53 there is, in the cam 52, a cutaway 55, the lower part of which runs into the re-entrant part 54. The cutaway is delimited laterally by two ascendant inclines 55a (that fork symmetrically starting at the re-entrant part 54), and by two upper horizontal parts 55b. The surfaces of the said inclines 55a and of the said horizontal parts 55b are perpendicular to the base 55c of the cutaway that is oriented longitudinally. It is stressed that the lower edge 55d of the base 55c (namely the edge common to the part 54) slopes, as can be seen in FIG. 7.
Apparent, when viewing the cam 52 head-on, are the upper end 52a and the base 55c of the cutaway 55: the said cutaway defined by two blocks 56 in between which the re-entrant part 54 is formed. The lower longitudinal surface of the said blocks constitutes the said race 53, while in the surfaces of the said blocks are machined the said inclines 55a and the said parts 55b.
Commencing at the re-entrant part 54, the inner parts of the said blocks 56 are provided with one sloping section 57 per part, each defined by a vertical surface that originates at the said re-entrant part and is transversely of a depth that, proceeding longitudinally towards the outside of the cam, increases. The said sloping sections 57 constitute the initial part of corresponding longitudinal tracks C1, more about which will be said hereinafter.
The operation of the second embodiment of the improved machine will now be described with particular reference to the two characteristic situations, namely when a blade element is selected or not selected, assuming this to be a blade element 5 of the type illustrated in FIG. 1.
The former situation occurs with the selector element 11 in the non-operative position I (FIG. 4b.) In this case, the blade element 5 stays in the neutral position R, the butt 7 passes through the longitudinal housing 20, while the butt 8 skims over, in the order stated, the rectilinear sections of the parts 53a and 53b of the race 53: in the said situation, the tailpiece 35 of the blade element is not subjected to any stress at all.
With the latter situation, the selectior element 11 is in the operative position O (FIGS. 5a and 5b). An examination follows of the various displacements to which the blade element 5 is subjected (with reference to FIGS. 2, 5a, 5b and 6). The selector element 11 is carried into the operative position O when the blade element 5 in question is located in the region of the re-entrant part 54, and it thus ensues that the butt 8 skims over the rectilinear section of the part 53a situated upstream of the re-entrant part 54, with respect to the movement direction of the carriage, prior to being positioned therein (position P1 in FIG. 6).
The interception of the surface 11a of the selector element 11 against the lower part of the butt 6 causes the blade element 5 to be raised from the neutral position R (FIG. 5a) to a first intermediate position R1 (FIG. 5b); the said position is shown at P2 in FIG. 6.
The said elevation (in no way obstructed by the base 55c of the cutaway 55 but aided by the lower edge 55d of the said base) carries the butt 8 into the inside of the cutaway 55 without any stress applied to the tailpiece 35.
With the blade element in position R1, the interception takes place (because of the carriage moving in direction T1) of the ascendant incline 55a against the lower part of the butt 8 (for example, the position F3 shown with dashes in FIG. 6). This brings about a further elevation of the blade element 5 whereby this is carried into a second intermediate position R2 defined by the said upper horizontal part 55b.
The interception then occurs, with the blade element in position R2, (again in consequence of the movement of the carriage in the direction T1), of the surface 13a of the cam 13 against the lower part of the butt 7. This causes a further, and a final, elevation of the blade element 5 from position R2 to position R3 (the maximum raised position) whereby the relevant needle (provided in the blade element 4) is carried into operation.
Then with the carriage still moving in the direction T1, the interception takes place of the surfaces 14a and 15a of the cams 14 and 15, respectively, against the upper part of the butt 7. This causes the blade element 5 to be lowered from position R3 down to the said neutral position R.
In the event of the elevation of the blade element 5 brought about by the interception of the selector element 11 against the butt 6 not being sufficient to cause the subsequent interception of the incline 55a against the lower part of the butt 8, thanks to the particular conformation of the cam 12, the said butt is not subjected to breakage. The front surface of the butt 8 is, in fact, intercepted, in the situation to which reference has just been made (position K1 in FIG. 7), by the sloping section 57 and this results in a consequent gradual elastic flexure of the tailpiece 35 (the said deflection being made possible by the suddenly reduced area 35a). Because the butt is intercepted by the track C1 of the block 56 (position K2 in FIG. 7), the deflection continues: the curved section of the part 53a of the successive cam 12 then has the task of re-aligning the blade element 5 in the neutral position R.
When use made of the blade element 5 depicted in FIG. 1a, instead of undergoing flexure, the tailpiece 35 oscillates with respect to the axis thereof, in contrast with the corresponding spring 60.
The cams 12,13,14 and 15 the selector elements 11 are symmetrical with respect to corresponding vertical planes, and thus the same considerations as above apply also to the movement in the direction T2 of the carriage.
To conclude, the particular conformation of the blade element 5 and of the cam 12 depicted in FIGS. 6 and 7 enables the under mentioned advantages to be obtained:
the blade element 5 is not subjected to any stress in the event of the non-selection thereof;
the blade element 5 is not subjected to any stress when selected correctly: in fact the cam 12 attends to raising the element in question from the first to the second intermediate position;
the blade element 5 undergoes stress or oscillates should, in the embodiments depicted in FIGS. 1 and 1a, the selector element 11 operate unsatisfactorily: this merely involves the needle connected to the blade element selected "not being sent into operation", without any danger of breakage to the butts of the said blade element, this continuing to be sound and suitable to be selected (eventually) by the group of selector elements 11 that succeeds the previous group.
An advantage in both embodiments is obtained in consequence of one single selector element being used instead of two as in conventional solutions.
Both blade elements depicted in FIG. 1 and are provided also with the upper butt 2 that is rested against a corresponding fixed cam 30 (shown with dashes in FIG. 2 and placed above the selector elements 11) during the elevation of the blade element concerned from position R1 to position R2.
It is understood that the foregoing description has been gieven purely as an unlimited example and thus that any variants in the above technical solution in no way prejudice the framework of protection afforded to the invention as claimed hereinafter.
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Inserted is each slit of the needle bed of this machine is a needle underneath which is placed a blade element that is provided with three butts, namely a first butt at the top, a second butt below, and a third butt at the bottom. The said third and last butt is carried by a tailpiece able to oscillate or undergo flexure, in contrast with elastic means, inside the corresponding slit.
The selection of a blade element is defined by the operation of a selector element, integral with the carriage, whereby the first butt is intercepted causing the blade element to be raised from the neutral position.
Through action exerted on the third butt by an operating cam, the blade element is raised further in cases when the selection operation is fully satisfactory; should this not be the case, as also when the blade element is in the neutral position, the cam acts as a guide for the said third butt in order to reach, or maintain, the said neutral position.
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[0001] This application is a continuation-in-part of U.S. patent application Ser. No. 13/404,874, filed Feb. 24, 2012, which claims priority from U.S. Provisional Application Ser. No. 61/449,877, filed Mar. 7, 2011, both of which are hereby incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to an arrangement for opening and closing coverings for architectural openings such as Venetian blinds, pleated shades, cellular shades, and vertical blinds.
[0003] Usually, a transport system for a covering that extends and retracts in the vertical direction has a fixed head rail which both supports the covering and hides the mechanisms used to raise and lower or extend and retract the covering. Such a transport system is described in U.S. Pat. No. 6,536,503, Modular Transport System for Coverings for Architectural Openings, which is hereby incorporated herein by reference. In the typical covering product that retracts at the top and then extends by moving downwardly from the top (top/down), the extension and retraction of the covering is done by lift cords suspended from the head rail and attached to the bottom rail. In a Venetian blind, there also are ladder tapes that support the slats, and the lift cords usually run through holes in the middle of the slats. In these types of coverings, the force required to raise the covering is at a minimum when the covering is fully lowered (fully extended), since the weight of the slats is supported by the ladder tapes, so that only the bottom rail is being raised by the lift cords at the outset. As the covering is raised further, the slats stack up onto the bottom rail, transferring the weight of the covering from the ladder tapes to the lift cords, so progressively greater lifting force is required to raise the covering as it approaches the fully raised (fully retracted) position.
[0004] Some window covering products are built to operate in the reverse (bottom-up), where the moving rail, instead of being at the bottom of the window covering bundle, is at the top of the window covering bundle, between the bundle and the head rail, such that the bundle is normally accumulated at the bottom of the window when the covering is retracted and the moving rail is at the top of the window covering, next to the head rail, when the covering is extended. There are also composite products which are able to do both, to go top-down and/or bottom-up. In the top-down/bottom-up (TDBU) arrangements, the window shades or blinds have an intermediate movable rail and a bottom movable rail.
[0005] Known cord drives have some drawbacks. For instance, the cords in a cord drive may be hard to reach when the cord is high up (and the blind is in the fully lowered position), or the cord may drag on the floor when the blind is in the fully raised position. The cord drive also may be difficult to use, requiring a large amount of force to be applied by the operator, or requiring complicated changes in direction in order to perform various functions such as locking or unlocking the drive cord. There also may be problems with overwrapping of the cord onto the drive spool, and many of the mechanisms for solving the problem of overwrapping require the cord to be placed onto the drive spool at a single location, which prevents the drive spool from being able to be tapered to provide a mechanical advantage.
[0006] It often is desirable to hide the cords so there are no loose cords. However, this can be difficult, especially when there is more than one movable rail, which generally means that there are many cords that have to be hidden.
SUMMARY
[0007] Various arrangements are presented for moving a covering from one position to another using lift cords that are hidden and eliminating loose cords. In one embodiment, the user actuates a mechanism on a handle on a movable rail, and then raises or lowers the movable rail to extend or retract the covering. Release of the handle mechanism automatically locks the movable rail in the position it was in when the handle mechanism was released.
[0008] In another embodiment, an indexing mechanism, functionally connected to the lift rod of the movable rail, functions to automatically rotate lift stations in the movable rail to wind up or unwind the lift cord as the movable rail is raised or lowered without requiring a motor to rotate the lift rod. (A motor could be used to assist the indexing mechanism, if desired.)
[0009] In another embodiment, an upper movable rail rides up and down on the lift cords of a lower movable rail.
[0010] In still another embodiment, an upper movable rail is suspended on a first set of lift cords that extend upwardly to fixed points, and a lower movable rail is suspended from the upper movable rail by a second set of lift cords. This embodiment includes an arrangement that prevents the lower movable rail from extending beyond the bottom of the architectural opening when the upper movable rail is fully extended.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a perspective view of a cellular shade incorporating a lock mechanism shown in the locked position;
[0012] FIG. 2 is a perspective view of the shade of FIG. 1 , with the lock in the unlocked position;
[0013] FIG. 3 is a partially exploded perspective view of the shade of FIG. 1 , showing the components that are housed in the movable rail;
[0014] FIG. 4 is a plan view of the lock mechanism of FIG. 1 , with the top cover omitted for clarity, and showing the lift rod;
[0015] FIG. 5 is the same view as FIG. 4 , but with the lock mechanism in the unlocked position;
[0016] FIG. 6 is an exploded perspective view of the lock mechanism of FIG. 1 ;
[0017] FIG. 7 is a rear perspective view of the slide element of the lock mechanism of FIG. 6 ;
[0018] FIG. 8 is a front view the lock mechanism of FIG. 1 ;
[0019] FIG. 9 is a section view along line 9 - 9 of FIG. 8 ;
[0020] FIG. 10 is a perspective view of the cellular shade of FIG. 1 , but adding a pivot support attachment to aid in unlocking the shade if the lock mechanism is not readily accessible to the user;
[0021] FIG. 11 is a perspective view, similar to FIG. 10 , showing a lock release wand engaging the pivot support attachment for aiding in unlocking the shade;
[0022] FIG. 12A is a broken-away, section view along line 12 A- 12 A of FIG. 11 ;
[0023] FIG. 12B is the same view as FIG. 12A , but with the lock mechanism in the unlocked position;
[0024] FIG. 13 is a perspective view of the pivot support attachment of FIG. 11 ;
[0025] FIG. 14 is a perspective view of the tip of the lock release wand of FIGS. 10 and 11 ;
[0026] FIG. 15 is a perspective view of the tip of the lock release wand of FIG. 14 , as seen from a different angle.
[0027] FIG. 16 is a perspective view of a top-down bottom-up cellular shade;
[0028] FIG. 17 is an exploded perspective view of the head rail of the cellular shade of FIG. 16 ;
[0029] FIG. 18 is a perspective view of a top-down bottom-up cellular shade with a movable rail including a lock;
[0030] FIG. 19 is a partially broken away, perspective view of the cellular shade of FIG. 18 , with the rails omitted for clarity;
[0031] FIG. 20 is an exploded perspective view of the cellular shade of FIG. 18 , with the lift cords omitted for clarity;
[0032] FIG. 21 is a bottom-end perspective view of one of the windlass assemblies of FIG. 20 ;
[0033] FIG. 22 is a top-end perspective view of the windlass assembly of FIG. 21 ;
[0034] FIG. 23 is an exploded perspective view of the windlass assembly of FIG. 22 ;
[0035] FIG. 24 is section view along line 24 - 24 of FIG. 22 ;
[0036] FIG. 25 is a perspective view of the windlass of FIG. 24 ;
[0037] FIG. 26 is section view along line 26 - 26 of FIG. 22 ;
[0038] FIG. 27 is a perspective view of an alternate windlass assembly which may be used in the cellular shade of FIG. 20 ;
[0039] FIG. 28 is an exploded perspective view of the windlass assembly of FIG. 27 ;
[0040] FIG. 29 is a plan view showing the housing of the windlass assembly of FIG. 28 ;
[0041] FIG. 30 is a plan view showing the housing cover of the windlass assembly of FIG. 28 ;
[0042] FIG. 31 is a section view along line 31 - 31 of FIG. 27 ;
[0043] FIG. 32 is a front perspective view of a cellular shade, similar to that of FIG. 1 , but with a different drive mechanism;
[0044] FIG. 33 is a rear perspective view of the cellular shade of FIG. 32 ;
[0045] FIG. 34 is a partially exploded perspective view of the cellular shade of FIG. 32 ;
[0046] FIG. 34A is a view similar to FIG. 34 , but using a rack and pinion arrangement instead of a bead chain;
[0047] FIG. 34B is a view similar to FIG. 34 , but using a cord and windlass instead of a bead chain;
[0048] FIG. 35 is a section view along line 35 - 35 of FIG. 34 , but with the sprocket mounted onto the end cap;
[0049] FIG. 36 is a section view along line 36 - 36 of FIG. 35 ;
[0050] FIG. 37 is a perspective view of the end cap of FIG. 34 ;
[0051] FIG. 38 is a perspective view of the sprocket of FIG. 34 ;
[0052] FIG. 39 is a perspective view of a cellular shade, similar to that of FIG. 32 , but with index drive mechanisms at both ends of the shade;
[0053] FIG. 40 is a schematic of a top down/bottom up shade with an automatic variable stroke limiter, with both movable rails in their retracted positions;
[0054] FIG. 41 is a schematic of the shade of FIG. 40 with the upper movable rail in its fully extended position and the lower movable rail in its fully retracted position;
[0055] FIG. 42 is a schematic of the shade of FIG. 40 with the upper movable rail in a partially extended position and the lower movable rail in a partially extended position;
[0056] FIG. 43 is a schematic of the shade of FIG. 40 with the upper movable rail in a partially extended position and the lower movable rail in its fully retracted position; and
[0057] FIG. 44 is a schematic of the shade of FIG. 40 but showing a covering extending from the upper movable rail to the lower movable rail and including brakes on both movable rails.
DESCRIPTION
[0058] FIGS. 1 through 10 illustrate one embodiment of a horizontal covering for an architectural opening (which may hereinafter be referred to as a window covering or blind or shade). This particular embodiment is a cellular shade 10 , with a lock mechanism 12 (illustrated in further detail in FIGS. 4 through 9 ). The user applies an outside force to de-activate the lock mechanism 12 for raising or lowering the shade (retracting and extending the expandable material). When the shade is in the desired position, the user stops applying the outside force, and the lock mechanism automatically locks and holds the shade in place. This same lift arrangement could be used for a Venetian blind.
[0059] The shade 10 of FIGS. 1-3 includes a head rail 14 , a bottom rail 16 , and a cellular shade structure 18 suspended from the head rail 14 and attached to both the head rail 14 and the bottom rail 16 . Lift cords (not shown) are attached to the head rail 14 , extend through openings in the cellular shade 18 , and terminate at lift stations 20 housed in the bottom rail 16 . A lift rod 22 extends through the lift stations 20 and through the locking mechanism 12 . The lift spools on the lift stations 20 rotate with the lift rod 22 , and the lift cords wrap onto or unwrap from the lift stations 20 to raise or lower the bottom rail 16 and thus raise or lower the shade 10 . A spring motor 24 is functionally attached to the lift rod 22 to provide an assisting force when raising the shade.
[0060] These lift stations 20 and spring motor 24 , and their operating principles are disclosed in U.S. Pat. No. 6,536,503 “Modular Transport System for Coverings for Architectural Openings”, issued Mar. 25, 2003, which is hereby incorporated herein by reference. Very briefly, the lift rod 22 is rotationally connected to an output spool on the spring motor 24 . A flat spring (not shown) in the spring motor 24 has a first end connected to the output spool (having a first axis of rotation) of the spring motor 24 . The second end of the flat spring in the spring motor 24 is either connected to a storage spool (not shown) having a second axis of rotation, or is coiled about an imaginary axis defining this second axis of rotation. The flat spring is biased to return to its “normal” state, wound around the second axis of rotation, and typically this corresponds to when the shade 10 is in the fully raised position (retracted). As the shade 10 is pulled down (extended) the flat spring unwinds from the second axis of rotation and winds onto the output spool, increasing the potential energy stored in the spring. When the shade 10 is raised (retracted) the spring winds back onto the storage spool, using some of the potential energy to assist the user in raising the shade 10 by rotating the output spool and thus the lift rod 22 connected to the output spool of the spring motor 24 .
[0061] In this embodiment, the main purpose of the spring motor is to wind up the lift cord as the shade 10 is raised. To operate the shade, the user applies an external force to unlock the locking mechanism 12 and manually positions the rail 16 . He then releases the external force, and the locking mechanism 12 automatically locks to hold the rail 16 in the desired position regardless of the relationship of the spring power to the weight of the shade. The spring may be underpowered (having enough power to wind up the lift cord but not enough power to raise the shade) or it may be overpowered (having enough power to wind up the lift cord and additional power to raise the shade).
[0062] In one embodiment for a Venetian-type blind, this spring motor 24 includes a spring with a negative power curve such that, when the force required to raise the blind is at a minimum (when the Venetian blind is fully extended), the spring provides the least assist, and as a progressively greater lifting force is required to raise the slats of the blind (as the Venetian blind approaches the fully retracted position) the spring provides more of an assist. This spring with a negative power curve is disclosed in U.S. Pat. No. 7,740,045 “Spring Motor and Drag Brake for Drive for Coverings for Architectural Openings”, issued Jun. 22, 2010, which is hereby incorporated herein by reference.
[0063] Each lift station 20 includes a lift spool which rotates with the lift rod 22 . The lift stations 20 , lift rod 22 , and spring motor 24 are mounted in the bottom rail 16 . When the lift rod 22 rotates, so do the lift spools of the lift stations 20 , and vice versa. One end of each lift cord is connected to a respective lift spool of a respective lift station 20 , and the other end of each lift cord is connected to the top rail 14 , such that, when the lift spools rotate in one direction, the lift cords wrap onto the lift spools and the shade 10 is raised (retracted), and when the lift spools rotate in the opposite direction, the lift cords unwrap from the lift spools and the shade 10 is lowered (extended).
Lock Mechanism
[0064] FIGS. 4-9 show the details of the lock mechanism 12 of FIG. 3 . Referring to FIG. 6 , the lock mechanism 12 includes a housing 26 , a slide element 28 , a coil spring 30 , a splined sleeve 32 , and a housing cover 34 .
[0065] The housing 26 is a substantially rectangular box having a flat back wall 36 , a flat front wall 38 which defines an opening 40 , and a forwardly extending fixed tab 42 secured to the front wall 38 . The side walls 44 , 46 define aligned, U-shaped openings 48 , 50 which rotationally support the splined sleeve 32 . The left side wall 44 also defines an inwardly extending projection 52 sized to receive and engage one end 54 of the coil spring 30 . The other end 56 of the coil spring 30 is received in a similar projection 58 on the slide element 28 (See FIG. 7 ), as will be described in more detail later.
[0066] The bottom wall 60 defines a ridge 62 which extends parallel to the front and rear walls 38 , 36 . The bottom edge 64 of the slide element 28 is received in the space between the ridge 62 and the front wall 38 , so the ridge 62 and front wall 38 form a track that guides the slide element 28 for lateral, sliding displacement parallel to the flat front wall 38 of the housing 26 . A recessed shoulder 66 along the front of the housing cover 34 also extends parallel to the front wall 38 . The top edge 68 of the slide element 28 is received between the front wall 38 and the shoulder 66 to provide a similar linear, lateral guiding function for the top edge 68 of the slide element 28 , as described in more detail later.
[0067] Referring to FIG. 7 , the slide element 28 is a substantially T-shaped member with the leg of the “T” being a slide tab 70 which is substantially identical to the fixed tab 42 of the housing 26 , except that there is a through opening 27 through the slide tab 70 , the purpose of which is described later. As best appreciated in FIGS. 4 and 5 , the fixed tab 42 and the slide tab 70 are substantially parallel to each other when the lock mechanism 12 is assembled, and the slide element 28 slides to the left (as seen from the vantage point of FIGS. 4 and 5 ) toward the fixed tab 42 to unlock the lock mechanism 12 , as described in more detail later.
[0068] Again referring to FIG. 7 , the slide element 28 defines a wing projection 71 substantially opposite the spring-receiving projection 58 . As described in more detail later, this wing projection 71 slides between the splines of the splined sleeve 32 to prevent the splined sleeve 32 from rotating.
[0069] The splined sleeve 32 (See FIGS. 6 and 9 ) is a hollow, generally cylindrical body with an internal bore 72 having a non-circular profile. In this particular embodiment, it has a “V” projection profile. The lift rod 22 has a complementary “V” notch 22 A. The lift rod 22 is sized to nearly match the internal profile of the bore 72 , with the “V” projection of the bore 72 being received in the “V” notch 22 A of the lift rod 22 , such that the splined sleeve 32 and the lift rod 22 are positively engaged to rotate together. Thus, when the splined sleeve 32 is prevented from rotation, the lift rod 22 is likewise prevented from rotation.
[0070] The splined sleeve 32 also defines a plurality of splines 74 extending radially at the right end portion of the splined sleeve 32 (as seen from the vantage point of FIG. 6 ). The left end portion 76 of the splined sleeve 32 is a smooth, spline-less, cylindrical surface having the same outside diameter as the base from which the splines 74 project.
Assembly:
[0071] Referring to FIGS. 4-6 , to assemble the lock mechanism 12 , the first end 54 of the coil spring 30 is placed over the projection 52 on the housing 26 . The slide element 28 is then assembled such that the slide tab 70 projects through the opening 40 in the front wall 38 of the housing 26 , with the bottom edge 64 of the slide element 28 fitting in the space between the ridge 62 and the front wall 38 of the housing 26 . The second end 56 of the coil spring 30 receives the projection 58 (See FIG. 7 ) of the slide element 28 , so the coil spring 30 is trapped between and is held in position by the two projections 52 , 58 .
[0072] The coil spring 30 acts as a biasing means which urges the slide element 28 to the right (as seen from the vantage point of FIG. 4 ). To install the splined sleeve 32 , the user pushes the slide element 28 to the left, to the position shown in FIG. 5 , such that the wing projection 71 clears the splines 74 of the splined sleeve 32 . The splined sleeve 32 is then dropped into place so that its ends rest on the curved bottoms of the openings 48 , 50 in the side walls 44 , 46 , which support the splined sleeve 32 for rotation. (Shoulders 73 near the ends of the splined sleeve 32 lie inside the housing 26 adjacent to the side walls 44 , 46 and ensure that the splined sleeve 32 remains in the proper axial position relative to the housing 26 .) Finally, the housing cover 34 snaps on top of the assembly to keep the components together, with top edge 68 of the slide element 28 being received between the shoulder 66 of the housing cover 34 and the front wall 38 of the housing 26 , and the lift rod 22 is slid through the bore 72 of the splined sleeve 32 and through the lift stations 20 and into the spring motor 24 , as shown in FIG. 3 .
[0073] The assembled lock mechanism 12 , lift rod 22 , lift stations 20 , and spring motor 24 , are then mounted in the movable rail 16 . In this embodiment, the movable rail 16 is the bottom rail 16 , but it alternatively could be an intermediate rail, located between the head rail and a bottom rail (not shown). As another alternative, the entire mechanism, including the spring motor 24 , lift rod 22 , lift stations 20 and lock 12 could be located in the fixed head rail 14 , with the lift cords secured to the movable bottom rail, extending through the shade 18 , and winding up on the spools of the lift stations 20 in the fixed head rail.
Operation:
[0074] Referring to FIGS. 1, 2, 4, and 5 , to raise or lower the shade 10 , the user pinches together the tabs 42 , 70 of the lock mechanism 12 , which pushes the slide element 28 to the left (as seen in FIG. 5 ), against the biasing force of the coil spring 30 . The wing projection 71 on the slide element 28 also moves to the left until it clears the splines 74 of the splined sleeve 32 , which frees the splined sleeve 32 and allows it to rotate. The lift rod 22 , which is functionally and positively connected to the splined sleeve 32 , now is also free to rotate. When the user is raising the shade 10 , the spring motor 24 assists the user by supplying some of the force required to rotate the lift rod 22 and with it the lift spools of the lift stations 20 to wind any lift cords onto these lift spools.
[0075] The spring on the spring motor 24 may be overpowered (more powerful than required to overcome the force of gravity acting on the shade 10 so that it raises the shade 10 ), or it may be underpowered, so that the user has to provide some of the lifting force to raise the shade 10 . As discussed earlier, the spring in the spring motor 24 may include a spring with a negative power curve such that, when the force required to raise the blind is at a minimum (when the blind is fully extended), the spring motor 24 provides the least assist, and as a progressively greater lifting force is required to raise the blind (as the blind approaches the fully retracted position) the spring motor 24 provides more of an assist.
[0076] When the user releases the tabs 42 , 70 of the lock mechanism 12 , the coil spring 30 automatically pushes the slide element 28 to the right, as shown in FIG. 4 , which slides the wing projection 71 to the right, so that it enters between two of the splines 74 , as shown in FIG. 9 . This prevents the splined sleeve 32 from rotating further. Since the lift rod 22 is directly connected to the splined sleeve 32 , this also prevents the lift rod 22 and the lift stations, which are functionally connected to the lift rod 22 , from rotating, so the lift cords cannot unwind from their lift stations 20 , and the shade 10 remains in the position where it was released by the user.
[0077] FIGS. 10-15 depict the shade 10 with an enhancement that may be added to make the lock 12 more readily accessible, especially when it might otherwise be too high up to reach.
[0078] Referring to FIGS. 10 and 11 , the enhancement includes a pivot support attachment 78 and a lock release wand 80 . Referring to FIG. 13 , the pivot support attachment 78 has a substantially flat horizontal surface 82 , defining a circular through opening 84 , and two downwardly projecting ears 86 , 88 defining countersunk openings 90 , 92 , for receiving screws to secure the attachment 78 to the movable rail 16 . As seen in FIGS. 10 and 11 , the pivot support attachment 78 is attached to the front, outside surface of the bottom rail 16 via screws 94 .
[0079] FIGS. 14 and 15 show the engagement tip 96 , which is secured to the top of the lock release wand 80 (See FIG. 11 ). This engagement tip 96 defines a first frustoconical surface 98 coaxial with the longitudinal axis of the lock release wand 80 , and a second frustoconical surface 100 mounted on an arm 102 which projects radially from the engagement tip 96 . The second frustoconical surface 100 is oriented perpendicular to the arm 102 . The bottom of the engagement tip 96 defines an opening 104 which receives the end of the lock release wand 80 , as seen in FIG. 10 .
[0080] If it is desirable to have means for extending the reach of the user to raise or lower the shade 10 , the pivot support attachment 78 is attached (using screws 94 , for instance) to the outer surface of the bottom rail 16 such that the two ears 86 , 88 straddle the lock 12 and the ear 86 abuts the fixed tab 42 of the lock 12 . The lock release wand 80 is then inserted into the pivot support attachment 78 such that the first frustoconical surface 98 goes into the opening 84 , as shown in FIGS. 10 and 11 . This first action properly locates the lock release wand 80 relative to the pivot support attachment 78 in preparation for controlling the lock 12 .
[0081] Once the lock release wand 80 is in position, as shown in FIG. 11 , it is rotated in a counter-clockwise direction about its longitudinal axis, as depicted by the arrow 106 in FIG. 10 , until the second frustoconical surface 100 projects into the opening 27 (See FIG. 12A ) in the slide tab 28 of the lock 12 , and the arm 102 is pressing against the slide tab 28 . Further rotation in the same counter-clockwise direction results in the arm 102 pushing the slide tab 28 toward the fixed tab 42 , which unlocks the lock 12 (See FIG. 12B ). The shade 10 may now be raised or lowered by raising or lowering the lock release wand 80 . The second frustoconical surface 100 projecting through the opening 27 of the slide tab 28 creates a positive engagement between the lock release wand 80 and the lock 12 such that the lock release wand 80 does not separate from the lock 12 even when pulling down on the lock release wand 80 .
[0082] Once the shade 10 is in the desired position, the user rotates the lock release wand 80 in a clockwise direction which allows the spring 30 to urge the slide tab 28 back to the locking position. Further rotation of the lock release wand 80 pulls the second frustoconical surface 100 out of the opening 27 in the slide tab 28 and allows the user to pull down on and remove the lock release wand 80 .
Top-Down, Bottom-Up Shade
[0083] FIGS. 16 and 17 show a top-down, bottom-up cellular shade 10 ′. This general type of shade 10 ′ is described in the aforementioned U.S. Pat. No. 7,740,045 “Spring Motor and Drag Brake for Drive for Coverings for Architectural Openings”, issued Jun. 22, 2010, which is hereby incorporated herein by reference.
[0084] The shade 10 ′ includes a head rail 14 ′, a movable intermediate rail 15 ′, a movable bottom rail 16 ′, and a cellular shade structure 18 ′ suspended from the intermediate rail 15 ′ and attached to both the intermediate rail 15 ′ and the bottom rail 16 ′.
[0085] There is a first set of lift cords 108 ′ that extend from the head rail 14 ′ to the intermediate rail 15 ′. These first lift cords 108 ′ have first ends attached to lift stations 21 ′ located in the head rail 14 ′ and second ends attached to the intermediate rail 15 ′. These first lift cords 108 ′ are raised and lowered with the rotation of a first lift rod 23 ′. There is a second set of lift cords 110 ′ that extend from the head rail 14 ′ to the bottom rail 16 ′. These second lift cords 110 ′ have first ends attached to lift stations 20 ′ in the headrail 14 ′, extend through the intermediate rail 15 ′ and through the covering 18 ′ and have second ends attached to the bottom rail 16 ′. These second lift cords 110 ′ are raised and lowered with the rotation of a second lift rod 22 ′. Other components include spring motors with drag brakes 24 ′, as described below.
[0086] The first lift rod 23 ′ extends through the lift stations 21 ′. A spring motor with drag brake 24 ′ is functionally attached to the first lift rod 23 ′ to provide an assisting force when raising the intermediate rail 15 ′ of the shade 10 ′. When the first lift rod 23 ′ rotates, the lift spools on the lift stations 21 ′ also rotate, and the lift cords 108 ′ wrap onto or unwrap from the lift stations 21 ′ to raise or lower the intermediate rail 15 ′.
[0087] The second lift rod 22 ′ extends through the lift stations 20 ′ in the headrail 14 ′. A spring motor with drag brake 24 ′ is functionally attached to the second lift rod 22 ′ to provide an assisting force when raising the bottom rail 16 ′ of the shade 10 ′. When the second lift rod 22 ′ rotates, the lift spools on the lift stations 20 ′ also rotate, and the lift cords 110 ′ wrap onto or unwrap from the lift stations 20 ′ to raise or lower the bottom rail 16 ′.
[0088] This arrangement results in two sets of lift cords 108 ′, 110 ′ extending adjacent to each other, with both of these two sets of lift cords 108 ′, 110 ′ being exposed as the intermediate rail 15 ′ travels down toward the bottom rail 16 ′.
[0000] Arrangement with Intermediate Rail Riding on Lift Cords of Lower Rail:
[0089] FIGS. 18-20 show a top-down/bottom-up cellular shade 10 *, which eliminates one of the sets of lift cords from the embodiment of FIG. 16 . As explained in more detail below, a single set of lift cords 108 * extends from the head rail 14 *, through the intermediate rail 15 *, through the covering 18 *, and on down to the bottom rail 16 *.
[0090] The shade 10 * of FIGS. 18-20 includes a head rail 14 *, an intermediate rail 15 *, a bottom rail 16 *, and a cellular shade structure 18 * suspended from the intermediate rail 15 * and attached to both the intermediate rail 15 * and the bottom rail 16 *.
[0091] Single lift cords 108 * are attached to the head rail 14 *, extend through a set of windlass assemblies 112 * in the intermediate rail 15 *, and then on through openings in the cellular shade 18 *, to terminate at lift stations 20 * housed in the bottom rail 16 *. A lift rod 22 * extends through the lift stations 20 * in the bottom rail 16 *. When the lift rod 22 * rotates, the lift spools on the lift stations 20 * also rotate, and the lift cords 108 * wrap onto or unwrap from the spools on the lift stations 20 * to raise or lower the bottom rail 16 *. A spring motor with drag brake 24 * is functionally attached to the lift rod 22 * to provide an assisting force when raising the bottom rail 16 * and to hold the bottom rail 16 * in place when released by the user.
[0092] A connecting rod (or lift rod) 23 * in the intermediate rail 15 * extends through the locking mechanism 12 * and through the windlass assemblies 112 * to functionally interconnect them as described later.
[0093] The spring motor with drag brake 24 * in the movable bottom rail 16 * of FIGS. 19 and 20 is identical to the spring motor with drag brake 24 ′ of FIG. 17 , including the possibility of incorporating overpowered or underpowered springs, as well as the possibility of incorporating a spring with a negative power curve as has already been discussed. The lift stations 20 * of FIGS. 19 and 20 are substantially identical to the lift stations 20 ′, 21 ′ of FIG. 17 , which has already been described. Finally, the locking mechanism 12 * of FIGS. 19 and 20 is substantially identical in design and operation to the locking mechanism 12 of FIG. 3 , which already has been described.
[0094] The windlass assemblies 112 * shown in FIGS. 19 and 20 are shown in more detail in FIGS. 21-26 . Each windlass assembly 112 * includes a windlass (or capstan) 116 * and a windlass housing 118 *. The windlass (or capstan) 116 * is a spool that rotates within the windlass housing 118 *. The windlass housing 118 * is a substantially rectangular housing with a top wall 120 *, a front wall 122 *, a rear wall 124 *, a right wall 126 *, and a left wall 128 *, which define a hollow cavity 130 * for rotationally housing the windlass spool 116 *. The windlass spool 116 * is assembled to the windlass housing 118 * through the bottom of the windlass housing 118 * as discussed below.
[0095] The right and left walls 126 *, 128 * include arms 132 *, 134 * respectively, which, in turn, define ramps 136 *, 138 * respectively which rotationally support the windlass spool 116 *, as described in more detail later. The top wall 120 * defines a cord entry port 140 *, and the bottom of the windlass housing 118 * defines a cord outlet port 142 *. Finally, a biasing member 144 *, resembling a paddle or a flat finger, projects downwardly inside the cavity 130 *, adjacent the windlass spool 116 *, as best appreciated in FIGS. 21, 23, and 24 . As explained in more detail later, the purpose of the biasing member 144 * is to press the windings of the lift cord 108 * against the ribs 145 * (See FIG. 23 ) of the windlass spool 116 * to prevent slippage between the lift cord 108 * and the windlass spool 116 *, that is, to prevent the possibility of the lift cord 108 * surging the windlass spool 116 *.
[0096] Referring to FIGS. 23 and 25 , the windlass spool 116 * is a hollow, cylindrical body with an internal bore 146 * having a non-circular profile. In this particular embodiment, it has a “V” projection profile. The connecting rod 23 * has a “V” notch and it is sized to nearly match the internal profile of the bore 146 *, with the “V” projection of the bore 146 * being received in the “V” notch of the connecting rod 23 *, such that the windlasses (or capstans) 116 * of the windlass assemblies 112 * and the connecting rod 23 * are positively engaged to rotate together. The windlass spool 116 * defines two coaxial frustoconical surfaces 152 *, 154 * tapering from a larger diameter at the end to a smaller diameter toward the center, and these surfaces are interconnected by a coaxial, generally cylindrical surface with a plurality of friction-enhancing, spaced apart ribs 145 *.
[0097] To assemble the windlass assembly 112 *, a first end of the lift cord 108 * is fed up through the cord exit port 142 in the bottom of the housing 118 * into the cavity 130 * of the housing 118 *, then is pulled downwardly out through the open bottom of the housing 118 * and is wound one or more times around the central portion of the windlass spool 116 * (as shown in FIG. 25 ) and then is fed back into the open cavity 130 * and upwardly through the entry port 140 * out of the windlass housing 118 * and is secured to the head rail 14 ′. The windlass spool 116 * is then installed in the windlass housing 118 * by pushing the windlass spool 116 * upwardly into the open cavity 130 * through the bottom of the windlass housing 118 *. The stub shafts 148 *, 150 * (See FIGS. 23 and 26 ) of the windlass spool 116 * slide up the ramps 136 *, 138 * and push outwardly against the arms 132 *, 134 *, gradually prying them apart as the windlass spool moves upwardly until the windlass spool 116 * clears the tops of the arms 132 *, 134 *, at which point the arms 132 *, 134 * snap back to their original positions, securing the windlass spool 116 * in the housing 118 * as shown in FIGS. 21, 22 and 26 . The second end of the lift cord 108 * is then extended through the covering 18 * and is secured to the respective lift station 20 * in the bottom rail 16 *.
[0098] The connecting rod 23 * is inserted through both windlass assemblies 112 * and through the splined sleeve 32 * of the locking mechanism 12 *, as shown in FIG. 19 .
[0099] As was discussed with respect to the locking mechanism 12 of FIGS. 3-5 , when the user squeezes the slide tab 70 * and fixed tab 42 * together, the wing that is fixed to the slide tab 70 * moves away from the splined portion of the splined sleeve 32 *, unlocking the locking mechanism 12 * and allowing rotation of the connecting rod 23 * and associated windlass spools 116 *.
The Operation of the Shade 10 * is as Follows:
[0100] To raise the bottom rail 16 *, the user grabs the bottom rail 16 * (See FIG. 20 ) and lifts it up. The spring motor with drag brake 24 * located in the bottom rail 16 * assists in raising the bottom rail 16 *. The spring motor 24 * causes rotation of the spools in the lift stations 20 * in order to wind up any excess lift cord 108 * onto the spools as the bottom rail 16 * is raised. When the user releases the bottom rail 16 *, the drag brake portion of the spring motor with drag brake 24 * holds the bottom rail 16 * in place. Since the spools in the lift stations 20 * rotate together, they keep the bottom rail 16 * horizontal as it travels up and down.
[0101] To lower the bottom rail 16 *, the user pulls down on the bottom rail 16 *. The lift cords 108 * are attached to the head rail 14 *, are cinched tightly around their respective windlasses (or capstans) 116 *, and extend to the spools on the lift stations 20 * in the bottom rail 16 *. Since the locking mechanism 12 * has not been released, the connecting rod 23 * is locked against rotation, as are the windlass spools 116 *, so the intermediate rail 15 * remains stationary. The lift cords 108 * unwind from the lift stations 20 * in the bottom rail 16 *, and the bottom rail 16 * is lowered. Again, once the user releases the bottom rail 16 *, the drag brake portion of the spring motor with drag brake 24 * holds the bottom rail 16 * in position.
[0102] To raise the intermediate rail 15 *, the user squeezes the tabs 42 *, 70 * together, which releases the splined sleeve 32 * for rotation. Since the connecting rod 23 * and the windlass spools 116 * are keyed to the splined sleeve 32 *, they also can rotate. If the user lifts up on the intermediate rail 15 * while squeezing the tabs 42 *, 70 * together, the windlass spools 116 * will rotate in their respective windlass housings 118 *, travelling upwardly along the lift cord 108 * as they transfer a portion of the lift cord 108 * that is above the windlass assemblies 112 * to below the windlass assemblies 112 *, so the intermediate rail 15 * also travels upwardly along the cords 108 *. Once the intermediate rail 15 * is in the desired location, the user releases the tabs 42 *, 70 * of the locking mechanism 12 *, which locks the splined sleeve 32 *, and therefore the connecting rod 23 * and the windlass assemblies 112 *, against further rotation, thereby locking the intermediate rail 15 * in place.
[0103] To lower the intermediate rail 15 *, the procedure is the reverse of that for raising the intermediate rail 15 * described above. The user squeezes together the tabs 42 *, 70 * of the locking mechanism 12 *, which releases the splined sleeve 32 * for rotation, which allows the connecting rod 23 * and the windlass assemblies 112 * to rotate. While squeezing together the tabs 42 *, 70 *, the user pulls down on the intermediate rail 15 *. The windlass spools 116 * rotate in the opposite direction, and the intermediate rail 15 * travels downwardly along the lift cords 108 *. Once the intermediate rail 15 * is in the desired position, the user releases the tabs 42 *, 70 * of the locking mechanism 12 *, which locks the intermediate rail 15 * in place. Since the windlass spools (or capstans) 116 * are tied together by the rod 23 * and rotate together, they keep the intermediate rail 15 * horizontal as it travels up and down.
[0104] It should be noted that the bottom rail 16 * remains in position as the intermediate rail 15 * is raised and lowered, since the position of the bottom rail 16 * is determined by the rotation of the spools on the lift stations 20 *, not by the position of the intermediate rail 15 *.
[0105] The tapered surfaces 152 *, 154 * on the windlass spools 116 * ensure that the lift cords 108 * remain centered on the windlass spools 116 *, and the ribs 145 * on the windlass spools 116 * together with the biasing leg 144 * which presses the lift cord 108 * against the ribs 145 * ensures that the cord 108 * does not slip relative to the windlass spools 116 *, so the cord 108 * serves as a type of indexing mechanism which automatically rotates the rod 23 * as the rail 15 * is raised and lowered without requiring a motor. This helps ensure that the intermediate rail 15 * remains horizontal as it travels up and down along the lift cords 108 *.
Alternate Embodiment of a Windlass
[0106] FIGS. 27-31 show an alternate embodiment of a windlass assembly 112 ** which may be used in the cellular shade of FIGS. 18-20 instead of the windlass assembly 112 *. As best appreciated in FIG. 28 , the windlass assembly 112 ** includes a windlass spool (or capstan) 116 **, a windlass housing 118 **, and a windlass housing cover 119 **.
[0107] The most important difference between this windlass assembly 112 ** and the windlass assembly 112 * described above is that this windlass assembly 112 ** does not have a biasing member 144 *. Instead, and as best appreciated in FIGS. 28, 29, 30 and 31 , the windlass housing 118 ** and the windlass housing cover 119 ** each have semi-circular surfaces 156 **, 158 ** which define circumferential guiding grooves 160 **, 162 ** respectively, which tightly guide the lift cord 108 * around the windlass spool 116 **, pressing the lift cord 108 * against the ribs 145 ** (See FIGS. 28 and 31 ) of the windlass spool 116 ** to prevent slippage between the lift cord 108 * and the windlass spool 116 **, that is, to prevent the possibility of the lift cord 108 * surging the windlass spool 116 **.
[0108] The operation of the cellular shade 18 using this second embodiment of a windlass assembly 112 ** is identical to the operation described earlier with respect to the first embodiment of the windlass assembly 112 *.
[0000] Alternate Embodiment of a Cellular Shade with a Drive with a Lock Mechanism
[0109] FIGS. 32-38 depict an embodiment of a cellular shade 10 ′, similar to the shade 10 of FIG. 1 , except that an indexing mechanism 164 ′ is used to automatically rotate the lift rod 22 as the movable rail 16 ′ is raised and lowered without requiring a spring motor. (It should be noted that a windlass 172 B and cord 168 B could be substituted as an alternative indexing mechanism, as shown in FIG. 34B .)
[0110] FIGS. 32, 33, and 34 show the cellular shade 10 ′ which includes a top rail 14 ′, bottom horizontal movable rail 16 ′, a cellular shade structure 18 ′, and an anchoring ledge 166 ′. It should be noted that the anchoring ledge 166 ′ may be part of the frame of the window opening and serves the purpose of providing an anchoring point to secure a bead chain 168 which extends from the top rail 14 ′ to the anchoring ledge 166 ′.
[0111] As shown in FIG. 34 , the bottom rail 16 ′ houses a slide lock mechanism 12 , lift stations 20 , and a lift rod 22 , which are identical to the corresponding items in the cellular shade 10 of FIG. 3 . The most important difference is the absence of the spring motor 24 (See FIG. 3 ) which has been replaced by the indexing mechanism 164 ′ (See FIG. 34 ), as explained in more detail below.
[0112] Referring to FIGS. 35-38 , the indexing mechanism 164 ′ includes a bottom rail end cap 170 ′ and a sprocket 172 ′, and utilizes the bead chain 168 ′ to rotate the lift rod 22 when the bottom rail 16 is raised or lowered, as explained later. The sprocket 172 ′ and lift rod 22 cause the lift spools 20 to rotate together, which keeps the rail 16 ′ horizontal as it travels up and down.
[0113] Referring to FIG. 37 , the bottom rail end cap 170 ′ defines ramped approaches 174 ′, 176 ′ to guide the bead chain 168 ′ to the sprocket 172 ′, as may also be appreciated in FIG. 35 . The end cap 170 ′ also includes flat projections 178 ′, 180 ′, 182 ′, and 184 ′ which project inwardly from the end cap 170 ′ and which are used to releasably secure the end cap 170 ′ to the bottom rail 16 ′. Finally, the end cap 170 ′ also includes a support shaft 186 ′ with an enlarged diameter, barbed end 188 . The support shaft 186 ′ rotationally supports the sprocket 172 ′, as shown in FIG. 36 .
[0114] FIG. 38 shows the sprocket 172 ′ which includes a plurality of semi-circular, circumferentially-arranged, evenly-spaced and alternatingly-opposed cavities 190 ′ designed to receive and engage the beads of the bead chain 168 ′ as the indexing mechanism 164 ′ is raised or lowered together with the bottom rail 16 ′. The hollow shaft 192 ′ of the sprocket 172 ′ has a non-cylindrical cross-sectional profile 194 ′ which matches up with a similarly shaped cross-sectional profile on the lift rod 22 for positive rotational engagement between the sprocket 172 ′ and the lift rod 22 . The portion of the hollow shaft 192 ′ that is located inside the sprocket “teeth” 190 ′ has a reduced inside diameter portion 193 ′ (See FIG. 36 ), which helps retain the sprocket 172 ′ onto the shaft 186 ′ as describe below.
[0115] To assemble the indexing mechanism 164 ′ to the shade 10 ′, the sprocket 172 ′ is first rotationally mounted to the shaft 186 ′ on the end cap 170 ′ by pushing the sprocket 172 ′ onto the shaft 186 ′ and compressing the barbed end 188 ′ until the reduced diameter portion 193 ′ of the sprocket 172 ′ passes the barbed end 188 ′, at which point the barbed end 188 ′ snaps open to its non-compressed position, locking the sprocket 172 ′ onto the shaft 186 ′, as shown in FIG. 36 . Then, one end of the bead chain 168 ′ is fed through the ramped approach 174 ′ (See FIG. 37 ) and the sprocket 172 ′ is manually rotated to feed the bead chain 168 ′ around the sprocket 172 ′, with the beads on the bead chain 168 ′ engaging the cavities 190 ′ on the sprocket 172 ′. The bead chain 168 ′ wraps around the sprocket 172 ′ and then exits the end cap 170 ′ via the ramped approach 176 ′. The indexing mechanism 164 ′ is then pressed onto the end of the bottom rail 16 ′, with the lift rod 22 being inserted into and engaging the non-cylindrical cross-sectional profile 194 ′ of the shaft 192 ′ of the sprocket 172 ′. The end of the bead chain 168 ′ is then secured to the anchoring ledge 166 ′ such that the bead chain 168 ′ is fairly taut between the top rail 14 ′ and the anchoring ledge 166 ′.
Operation:
[0116] To raise the shade 10 ′ the lock 12 is unlocked, as explained earlier with respect to the embodiment described in FIGS. 1-3 , and the operator manually raises the bottom rail 16 ′ to the desired height. As the bottom rail 16 ′ is raised, the bead chain 168 ′ rotates the sprocket 172 ′ in a first direction, which also rotates the lift rod 22 and the lift stations 20 , so as to gather up the lift cords (not shown) onto the spools of the lift stations 20 in the movable rail 16 ′. When the operator releases (lets go of) the lock mechanism 12 , it locks the lift rod 22 against further rotation, holding the bottom rail 16 ′ where it was released, as described earlier with respect to the shade 10 of FIGS. 1-3 .
[0117] To lower the shade 10 ′, the operator again unlocks the lock 12 and lowers the bottom rail 16 ′ to the desired position. As the bottom rail 16 ′ is lowered, the bead chain 168 ′ rotates the sprocket 172 ′ in the opposite direction which then also rotates the lift rod 22 and the lift stations 20 in the opposite direction, unwinding the lift cords (not shown) from the spools of the lift stations 20 . When the operator releases (lets go of) the lock mechanism 12 , it locks the lift rod 22 against further rotation, holding the bottom rail 16 ′ where it was released.
[0118] FIG. 39 shows yet another embodiment of a cellular shade 10 ″ which is very similar to the shade 10 ′ described above, except that it has two indexing mechanisms 164 ′, one on each end of the bottom rail 16 ′, which ride along their corresponding bead chains 168 ′. Other than this difference, the shade 10 ″ is identical to the shade 10 ′ and operates in the same manner. It should be obvious that other indexing mechanisms may be used instead of the bead chain and sprocket mechanism shown in the figures. For instance, as shown in FIG. 34A , a rack and pinion arrangement may be used in which the rack 168 A replaces the bead chain and the pinion 172 A replaces the sprocket. Any indexing mechanism that is used to automatically rotate the lift rod as the movable rail is raised and lowered without requiring a motor may be used to replace the bead chain and sprocket mechanism described above.
[0000] Two Movable Rail Shade with Automatic Variable Stroke Limiter
[0119] While the embodiment shown in FIGS. 18-20 is one way to arrange for raising and lowering two (or more) movable rails without the addition of a second set of lift cords 110 ′ as in FIG. 16 , another way to achieve this result is shown in FIGS. 40-44 .
[0120] FIGS. 40-44 are schematics of a shade 200 with two movable rails in which the upper rail is suspended by lift cords that extend to fixed points above the upper rail, and the lower rail is suspended by lift cords that extend down from the upper rail.
[0121] With this type of arrangement, the issue arises that if the lower rail lift cords are long enough so the lower movable rail can extend to the bottom of the architectural opening when the upper rail is at the top of the opening, then the lower movable rail may extend below the bottom of the architectural opening when the upper rail moves down. Of course, this is not desirable. For that reason, an automatic variable stroke limiter has been incorporated into this design.
[0122] As explained in more detail later, the automatic variable stroke limiter controls the overall length of the shade 200 so that the bottom rail will not extend beyond a desired position, such as beyond the bottom of the opening, regardless of the position of the upper movable rail.
[0123] Referring to FIG. 40 , the shade 200 includes a head rail 202 , an upper movable rail 204 , and a lower movable rail 206 . Extendable covering materials 208 (See FIG. 44 ) such as a pleated shade material or a plurality of slats supported by ladder tapes may be secured to the upper and lower rails 204 , 206 , so that, when the rails move up and down, they extend and retract the covering materials. For example, in FIG. 44 , the covering material 208 extends between the upper movable rail 204 and the lower movable rail 206 . As another possibility, a first covering material 208 could extend from the head rail 202 to the upper movable rail 204 , and a second covering material 208 could extend from the lower movable rail 204 to the bottom of the architectural opening.
[0124] The upper movable rail 204 houses first and second cord spools 212 , 214 mounted for rotation together on an elongated upper rail lift rod 216 . The cord spools 212 , 214 may be located anywhere along the upper rail lift rod that is desired. For example, if a pleated shade material is extending between the head rail 202 and the upper movable rail 204 , the cord spools 212 , 214 will be located inwardly far enough to ensure that the pleated shade material remains under control and does not “blow out”. If no covering material is extending between the head rail 202 and the upper movable rail 204 , then it may be desirable to move the cord spools 212 , 214 further outwardly so the cords that wrap around them do not interfere with the user's line of sight.
[0125] First and second upper rail lift cords 218 , 220 have their first ends secured to the head rail 202 at fixed points 218 a , 220 a and their second ends secured to the cord spools 212 , 214 . As an alternative, the head rail 202 may be omitted and the first set of lift cords may be secured directly to the frame of the window opening at the fixed points 218 a , 220 a . It also should be noted that the fixed points 218 a , 220 a may alternatively be points on a movable rail located above the upper movable rail.
[0126] In these schematics, the angled arrows on the cord spools (such as the arrow 222 on the cord spool 212 in FIG. 40 ) indicate the extent to which the lift cord is wrapped onto the cord spool. If the lift cord is shown coming off of the respective spool at the end near the tip of the arrow, that means it is fully wound onto that spool. If it is shown coming off the respective spool at the opposite end, that means it is unwound from that spool.
[0127] For example, in FIG. 40 , the lift cord 218 is fully wrapped onto the cord spool 212 , while in FIG. 41 the same lift cord 218 is fully unwrapped from the cord spool 212 , and in FIG. 42 the same lift cord 218 is approximately half way wound onto the cord spool 212 .
[0128] Referring again to FIG. 40 , two counterwrap cord spools 224 , 226 are mounted on the same upper rail lift rod 216 , between the first and second cord spools 212 , 214 , for rotation together with the lift rod 216 . These counterwrap cord spools 224 , 226 may be located anywhere along the lift rod 216 , as desired. Lower rail lift cords 238 , 240 are counterwrapped onto these additional cord spools 224 , 226 (wrapped in the direction opposite to the direction of the wrap on the first and second cord spools 212 , 214 ) so that, as the upper lift rod 216 rotates to wind up the upper rail lift cords 218 , 220 onto the first and second lift spools 212 , 214 , it causes the lower rail lift cords 238 , 240 to unwind from their respective counterwrap spools 224 , 226 . Similarly, as the upper rail lift rod 216 rotates in the opposite direction, to unwind the upper rail lift cords 218 , 220 from their lift spools 212 , 214 , it causes the counterwrapped lower rail lift cords 238 , 240 to wrap onto the counterwrap spools 224 , 226 .
[0129] It should be noted that, while the lift spools 212 , 214 and counterwrap spools 224 , 226 are shown as separate pieces mounted on the upper lift rod 216 and individually movable along that lift rod 216 , it would be possible for two (or even more) of the cord spools to be made as a single piece. Also, while the first and second upper rail lift cords 218 , 220 are shown in this schematic as being separate from the first and second counterwrap cords 238 , 240 , it is understood that the first upper rail lift cord 218 and the first counterwrap cord 238 could actually be a single cord, and, similarly that the second upper rail lift cord 220 and the second counterwrap cord 240 could be a single cord.
[0130] A motor 228 , such as the spring motor 24 of FIG. 3 , also is mounted on the upper rail lift rod 216 to assist in wrapping the lift cords 218 , 220 onto their respective cord spools 212 , 214 when raising the upper movable rail 204 . (The motor 228 could alternatively be a battery-powered electric motor.)
[0131] The shade 200 also includes a lower movable rail 206 which houses two cord spools 230 , 232 mounted on a lower rail lift rod 236 for rotation together with the rod 236 . As with the previous cord spools, these lower rail cord spools 230 , 232 may be located anywhere along the lower rail lift rod 236 . The two lower rail lift cords 238 , 240 have their first ends secured to the counterwrap cord spools 224 , 226 , respectively, and their corresponding second ends secured to the corresponding cord spools 230 , 232 on the lower movable rail 206 . The vertical line 242 shown on the left side of FIGS. 40-43 represents the full length of the window opening on which the shade 200 is installed.
[0132] Referring to FIG. 40 , the shade 200 is shown with both the upper movable rail 204 and the lower movable rail 206 in the fully retracted positions. That is, the upper movable rail 204 is all the way up against the head rail 202 , and the lower movable rail 206 is all the way up against the upper movable rail 204 . When the rails are in this position, the first and second upper rail lift cords 218 , 220 are fully wrapped onto their respective first and second cord spools 212 , 214 . The lower rail lift cords 238 , 240 are fully wrapped onto their respective lower rail cord spools 230 , 232 and fully unwrapped from their respective counterwrap cord spools 224 , 226 .
[0133] The user now may lower the upper rail until it is fully extended, while the lower movable rail 206 remains all the way up against the upper movable rail 204 , as shown in FIG. 41 . In this instance, as the upper movable rail 204 is lowered, the first and second upper rail lift cords 218 , 220 unwrap from their corresponding first and second cord spools 212 , 214 and, as they do so, they cause the upper rail lift rod 216 to rotate, which causes the counterwrap cord spools 224 , 226 to rotate, which causes the lower rail lift cords 238 , 240 to wrap onto the counterwrap cord spools 224 , 226 . Since the lower rail 206 already is abutting the upper rail 204 and therefore cannot move up any further relative to the upper rail 204 , as the user pulls down on the upper movable rail 204 , he is also pushing down on the abutting lower movable rail 206 , so the lower rail lift cords 238 , 240 unwrap from the lower rail cord spools 230 , 232 as they wrap onto the counterwrap cord spools 224 , 226 .
[0134] In FIG. 41 , the upper movable rail 204 is in the fully extended position, with the upper rail lift cords 218 , 220 fully unwound from their spools 212 , 214 . The lower movable rail 206 is abutting the upper movable rail 204 , with the lower rail lift cords 238 , 240 fully wound onto the counterwrap spools 224 , 226 and fully unwound from the lower rail spools 230 , 232 . The total length of the shade 200 matches the length of the opening (depicted by the arrow 242 ), so the lower movable rail 206 is at the bottom of the architectural opening. The lower movable rail 206 cannot be lowered any further relative to the upper movable rail 204 because the lower rail lift cords 238 , 240 are already fully unwrapped from the lower rail cord spools 230 , 232 .
[0135] It might be suggested that the lower rail lift cords 238 , 240 could unwrap from the counterwrap cord spools 224 , 226 to further lower the lower movable rail 206 . However, in order to unwrap the lower rail lift cords 238 , 240 from the counterwrap cord spools 224 , 226 the counterwrap spools 224 , 226 would have to rotate together with the upper rail lift rod 216 and the first and second cord spools 212 , 214 , which would wind the upper rail lift cords 218 , 220 onto the first and second cord spools 212 , 214 to raise the upper rail 204 . Thus, rotating the upper lift rod 216 to extend the lower rail lift cords 238 , 240 would also retract the upper rail lift cords 218 , 220 by the same distance, such that the lower movable rail 206 would remain stationary relative to the head rail 202 ; it would not drop below the length of the opening (depicted by the arrow 242 ).
[0136] Referring now to FIG. 42 , the user has raised the upper movable rail 204 to an intermediate position approximately half way between the fully retracted position (shown in FIG. 40 ) and the fully extended position (shown in FIG. 41 ). The upper rail lift cords 218 , 220 are approximately half way wrapped onto their corresponding first and second cord spools 212 , 214 . The lower rail lift cords 238 , 240 are approximately half way unwrapped from the counterwrap cord spools 224 , 226 on the upper movable rail 204 and are fully unwrapped from the lower rail cord spools 230 , 232 . Again, the lower movable rail 206 cannot be lowered any farther than the bottom of the opening 242 . The lower rail cord spools 230 , 232 already are fully unwrapped. Therefore, any lengthening of the lower rail extension cords 238 , 240 would have to come from their unwrapping from the counterwrap cord spools 224 , 226 . However, these counterwrap cord spools 224 , 226 are tied to the first and second cord spools 212 , 214 by the upper rail lift rod 216 , so any unwrapping of the lower rail lift cords 238 , 240 from the counterwrap cord spools 224 , 226 would only occur along with corresponding wrapping of the upper rail lift cords 218 , 220 onto their corresponding first and second cord spools 212 , 214 , thus shortening these upper rail lift cords 218 , 220 by the same distance the lower rail lift cords 238 , 240 are lengthened. Thus, while the lower movable rail 206 would move some distance away from the upper movable rail 204 , the upper movable rail 204 would be moving the same distance toward the head rail 202 , resulting in the lower movable rail 206 remaining in the same position relative to the fixed points 218 a , 220 a.
[0137] Comparing FIGS. 42 and 43 , it may be appreciated that in both figures the lower rail lift cords 238 , 240 are wrapped halfway onto the counterwrap cord spools 224 , 226 . In FIG. 42 , the lower rail lift cords are fully unwrapped from the lower rail spools 230 , 232 , so the balance of the lower rail lift cords 238 , 240 spans the distance between the upper movable rail 204 and the lower movable rail 206 . When the lower movable rail 206 is raised to the position shown in FIG. 43 , where it abuts the upper movable rail 204 , the counterwrap cord spools 224 , 226 do not move, so no more cord is wrapped onto them. All the excess of the lower rail lift cords 238 , 240 resulting from the raising of the lower movable rail 206 wraps onto the lower rail cord spools 230 , 232 , which, in FIG. 43 , are shown to be half-way wrapped with the lower rail lift cords 238 , 240 .
[0138] In this embodiment, the motors 228 , 234 provide at least enough force to wrap any excess cords onto their respective spools as the movable rails are raised. The motors 228 , 234 may also provide additional force to aid the user in lifting the movable rails so as to reduce the catalytic force required from the user to raise the movable rails. In this embodiment, the forces acting to raise the shade 200 (essentially the force provided by the motors 228 , 234 ) are close enough to forces acting to lower the shade 200 (essentially the force of gravity acting on the components) that the friction and inertia in the system are sufficient to prevent the rail from moving up or down once the rail is released by the user.
[0139] As an alternative embodiment, the number 228 , which represents a motor in the upper movable rail 204 , could instead represent a lock that is operable by the user, such as the lock 12 shown in FIG. 1 . In that case, if the user begins with the shade 200 in the position shown in FIG. 42 , when the user releases the lock in the upper movable rail 204 and raises the upper movable rail from the position shown in FIG. 41 , the lower rail lift cords 238 , 240 will pull on the counterwrap spools 224 , 226 and cause them to unwind, which will act as an indexing mechanism to automatically rotate the upper rail lift rod 216 and the upper rail lift spools 212 , 214 , winding up the upper rail lift cords 218 , 220 onto the spools 212 , 214 without requiring a motor. Then, when the user releases the upper rail 204 , the lock will hold the upper rail 204 in position. Similarly, if the user begins with the shade 200 in the position shown in FIG. 42 , when the user releases the lock in the upper movable rail 204 and pushes downwardly on the upper rail 204 , the upper rail lift cords 218 , 220 will pull on the upper rail lift spools 212 , 214 , causing those spools to unwind, which, in turn, will cause the lower rail lift cords 238 , 240 to wind up onto the counterwrap spools 224 , 226 .
[0140] Of course, either or both of the upper and lower rails 204 , 206 could have both a motor and a releasable lock functionally connected to their respective lift rods 216 , 236 .
[0141] FIG. 44 shows a shade 200 * which is similar to the shade 200 of FIGS. 40-43 except that it shows the covering material 208 and has brakes 210 , 211 acting on their corresponding lift rods 216 , 236 . The brakes 210 , 211 and their corresponding motors 228 , 234 may be a combination spring motor and drag brake, similar to the spring motor and drag brake 24 * of FIG. 20 to selectively stop the rotation of their corresponding lift rods 216 , 236 . A brake could be used on one or more of the lift rods, as needed, depending upon the forces involved.
[0142] It will be obvious to those skilled in the art that additional movable rails may be added, with each movable rail being suspended from the next adjacent movable rail above it, and with each pair of adjacent movable rails having its corresponding automatic variable stroke limiter to ensure that the overall length of the resulting shade does not exceed a desired length, which is usually the length of the opening to which it is mounted.
[0143] It should also be noted that the lift mechanisms in either of the movable rails may alternatively make use of other known mechanisms that provide for the cord spools to rotate together. For instance, U.S. Pat. No. 7,117,919 “Judkins” shows interconnected spools and spring motors. U.S. Pat. No. 7,093,644 “Strand” shows gear driven spools.
[0144] It also will be obvious to those skilled in the art that additional modifications may be made to the embodiments described above without departing from the scope of the invention as claimed.
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A covering for an architectural opening has a horizontal movable rail supported by cords, with a variety of configurations which allow the movable rail to be moved up and down while concealing the cords.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a scroll type compressor and more particularly, to an improvement for making a compressor more compact.
2. Description of the Related Art
Conventional scroll type compressors (hereinafter simply referred to as "compressors"), have a fixed scroll that is fixed in a shell and an orbiting scroll that is supported for revolving movement in the shell. The fixed scroll includes a fixed end plate and a fixed spiral element formed integrally with one side of the fixed end plate. The inner and outer walls of the fixed spiral element form involute curves. The orbiting scroll includes an orbiting end plate and an orbiting spiral element formed integrally with one side of the orbiting end plate. The inner and outer walls of the orbiting spiral element also take the form of involute curves. The fixed spiral element and orbiting spiral element are joined with the phase of the latter spiral element shifted by 180° from that of the former spiral element. A compression chamber is therefore formed between the scrolls.
In a compressor of this type, rotation of a drive shaft causes revolution of the orbiting scroll. Consequently, the compression chamber moves toward the center while its volume is decreased, thereby discharging a compressed fluid into a discharge chamber.
Further, as shown in FIG. 4, the inner wall of a fixed spiral element 82 from a tip portion 82b to a base portion 82a is formed along an inner involute curve I in . The outer wall of the fixed spiral element 82 is formed along an outer involute curve I out . This outer wall extends from the tip portion 82b to a position where the involute angle of this position is smaller by almost 180° than that of the base portion 82a. Since the outer wall of the fixed spiral element 82 is connected to an arc E that forms the inner wall of a shell 81, the fixed spiral element 82 is connected integrally with the shell 81. The inner and outer walls of an orbiting spiral element 83 are likewise formed along the involute curves I in and I out , respectively.
According to this compressor, the orbiting spiral element 83 and fixed spiral element 82 must be made to contact each other within a predetermined involute angle in accordance with revolution of the orbiting scroll in order to form the compression chamber. The center O of the shell 81 is designed to be coincident with the center S O of an involute generating circle S for the fixed spiral element 82. In addition, the center P O of an involute generating circle P for the orbiting spiral element 83 moves on a revolution circle C concentric to the center O (center S O ) of the shell 81, permitting the orbiting scroll to revolve.
However, when the center O of the shell 81 coincides with the center S O of the involute generating circle S for the fixed spiral element 82, a wasted space will be formed between the inner wall of the base portion 82a of the fixed spiral element 82 and the inner wall of the shell 81. This will be discussed more specifically below.
A distance W 8 between the inner wall of the base portion 82a of the fixed spiral element 82 and the inner wall of the shell 81 is expressed by the following equations:
a+W.sub.8 =R.sub.or +a+t+c
W.sub.8 =R.sub.or +t+c
where
t: is the thickness of the base portion 83a of the orbiting spiral element 83,
c: is the minimum clearance between the outer wall of the base portion 83a and the inner wall of the shell 81,
a: is the distance between the center P O of the involute generating circle P for the orbiting spiral element 83 and the inner wall of the base portion 83a of the orbiting spiral element 83 (=distance between the center S O of the involute generating circle S for the fixed spiral element 82 and the inner wall of the base portion 82a of the fixed spiral element 82, and
R or : is the radius of orbital revolution.
The minimum diameter D 8 of the shell 81 is therefore expressed as follows:
D.sub.8 =2(a+R.sub.or +t+c).
This conventional type of compressor therefore has a wasted space formed inside, increasing the diameter of the shell 81, which inevitably requires larger space to mount the compressor in a vehicle or the like.
One attempt to reduce this shortcoming is the compressor shown in FIG. 5, which is disclosed in Japanese Unexamined Patent Publication No. 55-51987. In this compressor, the center O of a shell 91 is shifted by R or /2 from the center S O of the involute generating circle S for a fixed spiral element 92 in a direction opposite to the direction toward a base portion 92a of the fixed spiral element 92. In the compressor disclosed in this Japanese publication, the inner and outer walls of the fixed spiral element 92 and an orbiting spiral element 93 are also formed along the involute curves I in and I out , respectively. As the center P O of the involute generating circle P for the orbiting spiral element 93 moves on a revolution circle C concentric to the involute generating circle S for the fixed spiral element 92, the orbiting scroll revolves.
With t, c, a and R or defined as given above, a distance W 9 between the inner wall of the base portion 92a of the fixed spiral element 92 and the inner wall of the shell 91 is expressed by the following equations:
R.sub.or /2+a+W.sub.9 =R.sub.or -R.sub.or /2+a+t+c
W.sub.9 =t+c
The minimum diameter D 9 of the shell 91 is expressed by:
D.sub.9 =2(a+R.sub.or /2+t+c).
This compressor can therefore reduce the wasted space by an amount expressed by the following equation as compared with the above-described typical compressor. ##EQU1## Likewise, the minimum diameter of the shell can be reduced by an amount expressed by the following equation. ##EQU2## As apparent from the above, the compressor can be made more compact, so that this compressor is more easily mounted in a vehicle or the like than the aforementioned compressor.
However, the compressor disclosed in the above publication still has a wasted space W 9 expressed by the formula:
W.sub.9 =t+c
The wasted space is between the inner wall of the base portion 92a of the fixed spiral element 92 and the inner wall of the shell 91. The minimum diameter of the shell 91 is thus limited to:
D.sub.9 =2(a+R.sub.or /2+t+c)
Accordingly, the disclosed compressor is not an adequate solution to the wasted space problem.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a compressor which is designed to have as small a wasted space as possible between the inner wall of the base portion of its fixed spiral element and the inner wall of its shell, and to have a smaller minimum diameter for further improvement on the mounting of the compressor into a vehicle or the like.
To achieve this object, a compressor embodying the present invention has interleaved fixed and orbiting spiral elements that have substantially involute shaped curves. The orbiting spiral element is revolved relative to the fixed spiral element at an orbital radius R or , with its rotation restricted. As the orbiting spiral element revolves, the volume of a compression chamber between the spiral elements decreases. Accordingly, a fluid in the compression chamber is compressed to then be discharged outside the shell.
The axial center (O) of the shell is displaced from the involute center (S O ) of the fixed spiral element in a direction towards the base end portion of the orbital scroll by a displacement distance (X) in the range of,
1/2R.sub.or <X≦1/2R.sub.or +1/2(t+c)
wherein "t" is the thickness of a base end portion of the orbiting spiral element and "c" is the minimum clearance between an outer wall of the orbital scroll's base end portion and the inner wall of the shell.
In a preferred embodiment, the maximum diameter of the orbiting spiral element (D O ) is substantially expressed by the equation: (D O )=2a+t=(c+R or ), wherein "a" is the distance between the center of the involute generating circle for the orbiting spiral element and the inner wall of the base portion of the orbiting spiral element. In another preferred embodiment, the maximum inner diameter of the shell (D s ) is substantially expressed by the equation: D s =2a+t+c+R or .
BRIEF DESCRIPTION OF THE DRAWINGS
The invention, together with objects and advantages thereof, may best be understood by reference to the following description of the presently preferred embodiments together with the accompanying drawings in which:
FIG. 1 is a longitudinal cross section of a compressor according to a first embodiment of the present invention;
FIG. 2 is a lateral cross section of the compressor according to the first embodiment;
FIG. 3 is a lateral cross section of a compressor according to a second embodiment;
FIG. 4 is a lateral cross section showing a typical prior art compressor design; and
FIG. 5 is a lateral cross section showing a second conventional compressor design.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
First and second embodiments of the present invention will now be described referring to the accompanying drawings.
First Embodiment
In the first embodiment of the invention shown in FIG. 1, a fixed scroll 2 includes a disk-shaped fixed end plate 21, a shell 22 formed integrally with the fixed end plate 21, and a fixed spiral element 23 formed on one side the fixed end plate 21. An orbiting scroll 4 includes a disk-shaped orbiting end plate 41 shown in FIG. 1, and an orbiting spiral element 42 formed on a side the orbiting end plate 41 that faces the fixed scroll.
When the fixed scroll 2 is joined with the orbiting scroll 4, a plurality of compression chambers 39 are formed. The shell 22 of the fixed scroll 2 serves as the outer housing of the compressor. A front housing 30 is coupled to the shell 22 by a tightening means.
In the front housing 30, a drive shaft 33 is rotatably supported by bearings 31 and 32. An eccentric pin 34 is provided at the inner end of a larger diameter portion of the drive shaft 33 at a position eccentric from the axis of the drive shaft 33. A bushing 36 is fitted over the eccentric pin 34. The orbiting scroll 4 is supported by the bushing 36 through a bearing 38, and only the revolution of the orbiting scroll 4 is allowed by the cooperation of the bushing 36 with a rotation preventing device 37. A counter weight 35 is attached to the eccentric pin 34 to absorb the dynamic imbalance of the orbiting scroll 4. The rotation preventing device 37 is linked through its movable ring to the orbiting end plate 41.
A discharge port 11, which communicates with the compression chambers 39 in a discharge process, is formed through the center portion of the fixed end plate 21 of the fixed scroll 2. A rear housing 10 having a discharge chamber 13 therein is fixed in the fixed scroll 2. The discharge port 11 communicates through a discharge valve 12 with the discharge chamber 13, which communicates with an external system such as a refrigeration circuit (not shown). A suction port 8, formed through the front housing 30, faces the peripheral portion of the counter weight 35 and communicates with the external system.
The fixed spiral element 23 of the fixed scroll 2 is formed along an involute curve defined by an involute generating circle S for a center S O as shown in FIG. 2. The inner wall of the fixed spiral element 23 from a tip portion 23b to a base portion 23a is formed along an inner involute curve I in . The outer wall of the fixed spiral element 23 is formed along an outer involute curve I out , and extends from the tip portion 23b to the vicinity of an involute point A whose involute angle is smaller by 180° than that of the base portion 23a. The inner wall of the shell 22 is formed along an arc E with a point O as a center.
The outer wall of the fixed spiral element 23 is connected to the inner wall (arc E) of the shell 22 through a small arched wall at the involute point A of the outer involute curve I out . The fixed spiral element 23 is thus integrally formed with the shell 22. A broken line in FIG. 2 indicates part of the arc E at the portion where the fixed spiral element 23 and the shell 22 are formed integral with each other.
The inner and outer walls of the orbiting spiral element 42 from a tip portion 42b to a base portion 42a are formed respectively along the inner and outer involute curves I in and I out based on an involute generating circle P for the center P O .
In the thus constituted compressor the rotation of an engine (not shown) is transmitted via an electromagnetic clutch (not shown) to the drive shaft 33 shown in FIG. 1. Consequently, a revolution momentum is given to the orbiting scroll 4 by the cooperation of the bushing 36 with the rotation preventing device 37. That is, the center P O of the orbiting spiral element 42 in FIG. 2 moves clockwise on the revolution circle C concentric to the involute generating circle S for the fixed spiral element 23.
In the status shown in FIG. 2, refrigerant gas is sucked from the base portion 42a of the orbiting spiral element 42 to an intermediate portion 42c (position whose involute angle is smaller by 180° from the base portion 42a). If the orbiting scroll 4 revolves by 180° from the position shown in FIG. 2, the outer wall at the intermediate portion 42c starts contacting the base portion 23a of the fixed spiral element 23. In the subsequent revolution, the volumes of the compression chambers 39 in FIG. 1 change. As a result, the pressure of the refrigerant gas rises in the compression chambers 39 sequentially, opening the discharge valve 12, so that the refrigerant gas is discharged from the discharge port 11 to the discharge chamber 13.
Referring to FIG. 2, the sizes of the individual portions are expressed as follows:
t: thickness of the base portion 42a of the orbiting spiral element 42,
c: minimum clearance between the outer wall of this base portion 42a and the inner wall of the shell 22,
a: distance between the center P O of the involute generating circle P for the orbiting spiral element 42 and the inner wall of the base portion 42a of the orbiting spiral element 42 (=distance between the center S O of the involute generating circle S for the fixed spiral element 23 and the inner wall of the base portion 23a of the fixed spiral element 23), and
R or : is the radius of orbital revolution.
In this case the center O of the shell 22 which is the center of the arc E is displaced by R or /2+t/2 from the center S O of the involute generating circle S in a direction opposite to the direction toward the base portion 23a of the fixed spiral element 23.
Therefore, a distance W 2 between the inner wall of the base portion 23a of the fixed spiral element 23 and the inner wall of the shell 22, or wasted space in the compressor is expressed as follows:
W.sub.2 +R.sub.or /2+t/2+a=R.sub.or -(R.sub.or /2+t/2)+a+t+c
W.sub.2 =R.sub.or -(R.sub.or /2+t/2)+a+t+c-(R.sub.or /2+t/2+a)
W.sub.2 =c
The minimum diameter D 2 of the shell 22 is expressed as follows: ##EQU3## This compressor can therefore reduce the wasted space by "t" as follows, as compared with the above-described compressor disclosed in the Japanese publication. ##EQU4## Likewise, the minimum diameter of the shell can be reduced by "t" as follows. ##EQU5## With t=4 mm, for example, the minimum diameter of the shell can be reduced by 4 mm.
This compressor is therefore designed to have a smaller diameter and be lighter, further improving the ease of the mounting of the compressor into a vehicle or the like.
In the compressor according to the first embodiment, the inner and outer walls of each of the fixed and orbiting spiral elements 23 and 42 are formed respectively along the involute curves I in and I out . Those inner and outer walls may be formed not along the inner and outer involute curves I in and I out , but along curves whose distances from the respective centers decrease as the involute angle increases.
Further, the tip portions 23b and 42b of the fixed and orbiting spiral elements 23 and 42 may be formed along on arc to improve their strengths, thereby increasing the wall thicknesses.
Second Embodiment
As shown in FIG. 3, a compressor according to the second embodiment differs from the compressor according to the first embodiment in the shapes of its fixed spiral element 53, its shell 52, and its orbiting spiral element 62. Both embodiments are the same in the other structure, so that a description of the same structure will not be given below.
The inner and outer walls of the fixed spiral element 53 of the fixed scroll 5, like those of the first embodiment, are formed from a tip portion 53b to a base portion 53a along inner and outer involute curves I in and I out . It is to be noted that the inner involute curve I in defining the inner wall of the fixed spiral element 53 is directly and smoothly coupled to an arc E that defines the inner wall of the shell 52, so that both inner walls are made integral. In FIG. 3, a broken line indicates part of the arc E at the portion where the fixed spiral element 53 and the shell 52 are formed integral with each other.
The inner wall of the orbiting spiral element 62 from a tip portion 62b to a base portion 62a is formed along the inner involute curve I in . The outer wall of the fixed spiral element 62 from the tip portion 62b to an intermediate portion 62c short by an involute angle of 180° of the base portion 62a, is formed along the outer involute curve I out . The portion from the intermediate portion 62c to the base portion 62a is formed along an arc F which has a radius equal to the distance between an involute point B and a point Q with Q as its center. The outer involute curve I out from the intermediate portion 62c to the involute point B is indicated by a broken line.
As apparent from the above, the orbiting spiral element 62 from the intermediate portion 62c to the involute point B is made thinner. This does not however raise any problem because a fluid compressing action will not be effected at this portion.
In FIG. 3, the sizes of the individual portions are represented by t, c, a and R or , which have also been used in the description of the first embodiment. In the second embodiment, the center O of the shell 52 is displaced by R or /2+t/2+c/2 from the center S O of the involute generating circle S for the fixed spiral element 53 in a direction opposite to the direction toward the base portion 53a of the fixed spiral element 53.
Therefore, the minimum diameter D 5 of the shell 52 around the center O or the center of the arc E is expressed as follows:
D.sub.5 =2(a+t/2+R.sub.or /2+c/2)=2a+t+c+R.sub.or.
If the center O is shifted simply by the above displacement, part of the orbiting spiral element 62 from the intermediate portion 62c to the involute point B interferes with the inner wall of the shell 52.
To prevent the interference, this compressor is designed so that the orbiting spiral element 62 has a maximum diameter D 6 expressed below, which has the following relation with the aforementioned minimum diameter D 5 .
D.sub.6 =2(a+t/2-R.sub.or /2-c/2)=2a+t-(R.sub.or +c)
D.sub.6 =D.sub.5 -2(R.sub.or +c)
The center Q of the maximum diameter of the orbiting spiral element 62 is displaced by R or from the center O of the shell 52.
Therefore, a distance W 5 between the inner wall of the base portion 53a of the fixed spiral element 53 and the inner wall of the shell 52 is expressed as follows: ##EQU6## No wasted space therefore exists between the inner wall of the base portion 53a of the fixed spiral element 53 and that of the shell 53. This compressor can therefore reduce the wasted space as follows, as compared with the above-described compressor disclosed in the Japanese publication.
W.sub.9 -W.sub.5 =t+c.
Likewise, the minimum diameter of the shell can be reduced as follows. ##EQU7## With t=4 mm and c=1 mm, for example, the minimum diameter of the shell can be reduced by 5 mm. The compressor in the second embodiment is therefore designed to have a smaller diameter and be lighter than the compressor of the first embodiment, further improving the ease of the mounting of the compressor into a vehicle or the like.
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A relatively small diameter scroll type compressor is disclosed. The axial center of the compressor's shell is displaced from the involute center of the fixed spiral element in a direction towards the base end portion of the orbital scroll. More specifically, the displacement distance (X) is in the range of: 1/2R or <X≦1/2R or +1/2(t+c), wherein "t" is the thickness of a base end portion of the orbiting spiral element and "c" is the minimum clearance between an outer wall of the orbital scroll's base end portion and the inner wall of the shell.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 61/225,331, filed on Jul. 14, 2009. The disclosure of the above application is incorporated herein by reference in its entirety.
FIELD
[0002] The present disclosure relates to a fuel system for a vehicle and more particularly to determining an error in a pressure sensor of a fuel system.
BACKGROUND
[0003] The background description provided herein is for the purpose of generally presenting the context of the disclosure. Work of the presently named inventors, to the extent it is described in this background section, as well as aspects of the description that may not otherwise qualify as prior art at the time of filing, are neither expressly nor impliedly admitted as prior art against the present disclosure.
[0004] Internal combustion engines combust an air/fuel (A/F) mixture within cylinders to drive pistons and to provide drive torque. Air is delivered to the cylinders via a throttle and an intake manifold. A fuel injection system supplies fuel from a fuel tank to provide fuel to the cylinders based on a desired A/F mixture. To prevent release of fuel vapor, a vehicle may include an evaporative emissions system which includes a canister that absorbs fuel vapor from the fuel tank, a canister vent valve, and a purge valve. The canister vent valve allows air to flow into the canister. The purge valve supplies a combination of air and vaporized fuel from the canister to the intake system.
[0005] Closed-loop control systems adjust inputs of a system based on feedback from outputs of the system. By monitoring the amount of oxygen in the exhaust, closed-loop fuel control systems manage fuel delivery to an engine. Based on an output of oxygen sensors, an engine control module adjusts the fuel delivery to match an ideal A/F ratio (14.7 to 1). By monitoring engine speed variation at idle, closed-loop speed control systems manage engine intake airflows and spark advance.
[0006] Typically, the fuel tank stores liquid fuel such as gasoline, diesel, methanol, or other fuels. The liquid fuel may evaporate into fuel vapor which increases pressure within the fuel tank. Evaporation of fuel is caused by energy transferred to the fuel tank via radiation, convection, and/or conduction. An evaporative emissions control (EVAP) system is designed to store and dispose of fuel vapor to prevent release. More specifically, the EVAP system returns the fuel vapor from the fuel tank to an engine for combustion therein. The EVAP system is a sealed system to meet zero emission requirements. More specifically, the EVAP system may be implemented in a plug-in hybrid vehicle with minimum engine operation that stores fuel vapor prior to being purged to the engine.
[0007] The EVAP system includes an evaporative emissions canister (EEC), a purge valve, and a diurnal control valve. When the fuel vapor increases within the fuel tank, the fuel vapor flows into the EEC. The purge valve controls the flow of the fuel vapor from the EEC to the intake manifold. The purge valve may be modulated between open and closed positions to adjust the flow of fuel vapor to the intake manifold.
[0008] Determining whether a fuel leak occurs is important in a closed system. However, adding additional pressure sensors increases the cost of the system.
SUMMARY
[0009] The present disclosure provides a method and system for determining the accuracy of a fuel tank pressure sensor using components found in a vehicle fuel system.
[0010] In one aspect of the disclosure, a method includes opening a diurnal control valve, switching on an ELCM diverter valve, generating a fuel tank pressure signal, generating an ELCM pressure signal, correlating the ELCM pressure signal and the fuel tank pressure signal and generating a fault signal in response to correlating.
[0011] In another aspect of the disclosure, a control module includes a diurnal control valve module that opens a diurnal control valve and an ELCM diverter valve control module that switches on an ELCM diverter valve. The control module includes a correlation module performs a correlation of a ELCM pressure signal and a fuel tank pressure signal and that generates a fault signal in response to the correlation when the DCV valve is open and the ELCM diverter valve is on.
[0012] Further areas of applicability of the present disclosure will become apparent from the detailed description provided hereinafter. It should be understood that the detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the disclosure.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] The present disclosure will become more fully understood from the detailed description and the accompanying drawings, wherein:
[0014] FIG. 1 is a functional block diagram of an engine system of a vehicle according to the present disclosure;
[0015] FIG. 2 is a functional block diagram of an engine control module according to the principles of the present disclosure; and
[0016] FIG. 3 is a flowchart depicting exemplary steps performed by the engine control module according to the principles of the present disclosure.
DETAILED DESCRIPTION
[0017] The following description is merely exemplary in nature and is in no way intended to limit the disclosure, its application, or uses. For purposes of clarity, the same reference numbers will be used in the drawings to identify similar elements. As used herein, the phrase at least one of A, B, and C should be construed to mean a logical (A or B or C), using a non-exclusive logical or. It should be understood that steps within a method may be executed in different order without altering the principles of the present disclosure.
[0018] As used herein, the term module refers to an Application Specific Integrated Circuit (ASIC), an electronic circuit, a processor (shared, dedicated, or group) and memory that execute one or more software or firmware programs, a combinational logic circuit, and/or other suitable components that provide the described functionality.
[0019] Referring now to FIG. 1 , a functional block diagram of an exemplary engine system 100 of a vehicle is shown. The engine system may be for a conventional Spark-ignited (SI) engine, a Homogeneous Charge Compression Ignited (HCCI) engine or an extended range electric vehicle engine which is used as a generator for generating electric power for charging a battery pack. The engine system 100 includes a fuel system 102 , an EVAP system 104 , and an engine control module 106 . The fuel system 102 includes a fuel tank 108 , a fuel inlet 110 , a fuel cap 112 , and a modular reservoir assembly (MRA) 114 . The MRA 114 is disposed within the fuel tank 108 and pumps liquid fuel to a fuel injection system (not shown) of the engine system 100 to be combusted. A fuel tank pressure sensor 164 generates a fuel tank pressure signal corresponding to the pressure within the fuel tank.
[0020] The EVAP system 104 includes a fuel vapor line 116 , a canister 118 , a fuel vapor line 120 , a purge valve (PV) 122 , a fuel vapor line 124 , an air line 126 , a diurnal control valve (DCV) 128 , and an air line 130 .
[0021] The fuel tank 108 contains liquid fuel and fuel vapor. The fuel inlet 110 extends from the fuel tank 108 to enable fuel filling. The fuel cap 112 closes the fuel inlet 110 .
[0022] Fuel vapor flows through the fuel vapor line 116 into the canister 118 , which stores the fuel vapor. The fuel vapor line 120 connects the canister 118 to the PV 122 , which is initially closed in position. The engine control module 106 controls the PV 122 to selectively enable fuel vapor to flow through the fuel vapor line 124 into the intake system (not shown) of the engine system 100 to be combusted. Air flows through the air line 126 to the DCV 128 , which is initially closed in position. The engine control module 106 controls the DCV 128 to selectively enable air to flow through the air line 130 into the canister 118 .
[0023] The air line 126 may include an evaporative leak check module (ELCM) 140 . An ELCM filter 141 may filter the air flow to the ELCM 140 . The evaporative leak check module 140 may include an ELCM diverter valve 142 , a vacuum pump 144 and an ELCM pressure sensor 146 . A reference orifice 148 may also be included within the evaporative leak check module 140 . The diverter valve 142 includes a first path 150 and a second path 152 therethrough. In the first position 150 , as illustrated, air is directed through the diverter valve directly from the input to the DCV 128 . In the second position 152 , the diverter valve 142 is controlled upward so that the vacuum pump 144 is in use and air travels through the vacuum pump 144 to the diurnal control 128 . In either case, the pressure sensor 146 generates a pressure signal corresponding to the pressure within the ELCM 140 .
[0024] The engine control module 106 regulates operation of the engine system 100 based on various system operating parameters. The engine control module 106 controls and is in communication with the MRA 114 , the fuel tank pressure sensor 164 , the PV 122 , the DCV 128 and the ELCM 140 .
[0025] Referring now to FIG. 2 , a functional block diagram of the engine control module 106 is shown. The engine control module 106 includes a correlation module 200 , a fuel tank pressure module 202 , a PV control module 204 , an evaporative leak check module (ELCM) pressure module 206 , a DCV control module 208 and an ELCM control module 210 .
[0026] The fuel tank pressure module 202 receives the fuel tank pressure signal and determines a fuel tank pressure based on the fuel tank pressure signal.
[0027] The ELCM pressure module 206 generates a pressure corresponding to the evaporative leak check module pressure sensor 146 of FIG. 1 . The ELCM pressure signal and the fuel tank pressure are provided to the correlation module 200 . The correlation module 200 provides control signals to the purge valve control module 204 that controls purge valve 122 . The correlation module 200 also provides control signals to the diurnal control valve control module 208 . The purge valve control module 204 controls the purge valve 122 as will be described below during a correlation of the pressure sensors. Likewise, the DCV control module 208 controls the DCV 128 during correlation of the pressure sensors.
[0028] The ELCM control module 210 includes an ELCM vacuum pump control module 220 and an ELCM diverter valve control module 222 . The ELCM vacuum pump control module 222 controls the ELCM vacuum pump 144 and the ELCM diverter valve control module controls the ELCM diverter valve 142 .
[0029] The correlation module 200 controls the operation of the purge valve 122 , the diurnal control valve 128 , the ELCM diverter valve 142 and the vacuum pump 144 in a predetermined manner to provide a sensor correlation between the fuel tank pressure and the pressure measured at the ELCM pressure sensor 146 of FIG. 1 . The correlation module 200 may, for example, determine a plurality of differences between the fuel tank pressure and the ELCM pressure and generates an average difference signal. The average difference signal may be compared to a correlation value or threshold. When the difference between the fuel tank and ELCM pressure is outside of a correlation range, an error indicator 230 may be activated. The error indicator 230 may provide an error signal through an on-board diagnostic system, or the like. The error indicator 230 may also be used to provide an audible or visual indicator as to an error to the vehicle operator.
[0030] Referring now to FIG. 3 , a method for operating the present disclosure is set forth. In step 310 , the initial positions of the various valves are initiated. It should be noted that the present disclosure may be performed both in engine-running and engine-off states. In step 310 , the initial positions correspond to the purge valve being closed, the diurnal control valve being closed, the diverter valve being off and the ELCM vacuum pump being off. At this point, no sensor correlation is taking place.
[0031] In step 312 , the ELCM diverter valve is turned on which places the ELCM diverter valve in the upper-most position 152 illustrated in FIG. 1 . In step 314 , the DCV valve is opened. In step 316 , the system waits for a stabilization time. The stabilizing time allows the system to equalize prior to pressure measurement. In step 318 , the pressure sensor signals are correlated.
[0032] The correlation of the pressure sensors in step 318 includes many steps including step 320 that measures the fuel tank pressure from the fuel tank pressure sensor. In step 322 , the pressure at the ELCM pressure sensor is determined. In step 324 , a difference of the measured fuel tank pressure and the measured ELCM pressure is determined. The difference may be obtained several times over a range of times and an average difference may be determined. When the average difference is greater than a calibration threshold (CAL) in step 324 , step 326 generates an error signal. In step 324 , when the difference is not greater than a calibration, a correlation signal is generated in step 328 . After step 328 , the DCV valve is closed in step 330 and the ELCM diverter valve is closed in step 332 .
[0033] As will be evident to those skilled in the art, an additional pressure sensor for verifying the proper operation of the fuel tank pressure sensor is not provided. By providing the same pressure to the fuel tank pressure sensor and the ELCM pressure sensor, both of the sensors are exposed to the same pressure/vacuum environment and therefore a correlation of the two sensors may be performed.
[0034] Those skilled in the art can now appreciate from the foregoing description that the broad teachings of the disclosure can be implemented in a variety of forms. Therefore, while this disclosure includes particular examples, the true scope of the disclosure should not be so limited since other modifications will become apparent to the skilled practitioner upon a study of the drawings, the specification, and the following claims.
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A control module and method for operating the same includes a diurnal control valve module that opens a diurnal control valve (DCV) and an evaporative leak check module (ELCM) diverter valve control module that switches on an ELCM diverter valve. The control module includes a correlation module performs a correlation of a ELCM pressure signal and a fuel tank pressure signal and that generates a fault signal in response to the correlation when the DCV valve is open and the ELCM diverter valve is on.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a forging machine of the type known as a radial forming machine, having four rams which are disposed in a cruciform manner in a single operating plane and are movable radially to the longitudinal axis of the workpiece and are provided with tools.
2. Description of the Prior Art
It is known to design forging machines of the cruciform type mentioned above.
BRIEF SUMMARY OF THE INVENTION
In the order that the tools may form a closed pass in the inner end positions of the stroke of the rams, the tools are connected to the rams by crosspieces which are adjustable transversely to the rams in the operating plane and which with the rams form a support, the adjustment being effected, as a function of the setting of the ram stroke end position, by an amount such that each tool is covered, on the unused width of its operative surface, by a lateral surface of an adjacent tool, and itself covers with its lateral surface the unused width of the operative surface of the other adjacent tool. In order to keep the time for adjusting the tools to a minimum, the crosspieces are connected to the rams by releasable clamping devices which produce a mutual biassing of the crosspiece and ram by the force of a spring and release the clamping device by a piston-cylinder unit acting against the spring force. The clamping devices require a considerable outlay in production, and their location in the vicinity of the tools and the workpiece with its heat radiation is disadvantageous, while the crosspiece is adjusted relative to the ram by way of a shaft which connects the drive, arranged at the end of the ram remote from the crosspiece on account of the considerable space required, of the adjustment device to the crosspiece on the end face of the ram and passes through an axial bore in the ram.
An object of the invention is to provide a clamping and adjustment device between the crosspiece and its ram, which is less expensive structurally and is remote from the region of direct heat radiation.
According to the invention, each ram and the crosspiece associated therewith are traversed by a tie rod which is provided with collars and which with the collars embraces the crosspiece, the ram and a tensioned spring disposed below the collar at the free end of the ram when the crosspiece is tensioned against the ram, a piston, which can be biased against the spring force in a cylinder connected to the ram and which then releases the tensioning of the crosspiece against the ram, bears against the collar under which the spring is disposed, and the tie rod is extended beyond the collar under which the spring is disposed and is connected rotationally rigidly but axially displaceably to a rotary drive supported on the machine frame by way of the cross member for adjusting the stroke position.
Because according to the invention, the shaft passing through the ram serves also as a tie rod, the spring and the countervailing piston-cylinder unit which form the clamping device can be relocated at the end of the ram remote from the tool and crosspiece, i.e. in the area which is remote from the heat radiation and which is less restricted in terms of space.
According to a further feature of the invention, the tie rod collar associated with the crosspiece, is constructed as a lever arm which is provided with a pin parallel to the tie rod and a slide block mounted pivotably on the pin, the crosspiece being provided with a slotted guide which extends transversely to its direction of displacement and into which the slide block engages. In this design, the crosspiece with the slotted guide, the lever with the slide block and the tie rod are particularly suitable for transmitting high clamping and displacement forces.
The surface of the crosspiece, which is provided only with a collar of the tie rod and which is covered in a protective manner by a cover supporting the tool, also permits an easy-to-manufacture, robust design of the connexion of the crosspiece to the ram, in that the crosspiece is guided relative to the ram by guide blocks which in one part (ram or crosspiece) lie in grooves and in the other part are guided in grooves providing space for the adjustment of the crosspiece. In order to produce positive locking between the ram and the crosspiece, inter-locking members are provided which lie in recesses in the ram and the crosspiece respectively and are provided on mutually opposite faces, with fine teeth which mesh with one another when the crosspiece is clamped against the ram.
In order to permit the spring associated with the outer collar of the tie rod to be accommodated in a structurally advantageous manner and to be mounted simply, according to a further feature of the invention a spring cup is provided which can be connected to the ram and in which the spring or set of springs is disposed between spring plates and axial bearings supporting the latter, a cover of the spring cup being constructed as an annular cylinder in which is guided an annular piston which is operatively connected to the axial bearing of the spring plate connected to the collar of the tie rod. The arrangement of the axial bearings permits the tie rod to turn for the lateral adjustment of the crosspiece with respect to the ram, as soon as the spring or set of springs is compressed by biasing the piston, whereby the crosspiece is pushed away from the ram and the fine teeth of the inter-locking members are disengaged.
To enable the tie rod to be used in a simple manner for the transverse displacement of the crosspiece with respect to the ram, according to a further feature of the invention the outer end of the tie rod, projecting from the ram, is provided with a multiply splined pin with which it engages in a multiply splined hub which is connected to a rotary drive by way of a coupling which compensates for radial displacement. In particular, a gearwheel moved by two opposed plunger pistons by way of toothed racks is provided as the rotary drive.
Rams of different design are possible within the scope of the invention.
Thus, according to one embodiment of the invention, a cylinder guided axially movably in the machine frame and provided with a central shaft is provided as a ram, the annular piston, which is associated with the cylinder and which surrounds the shaft, being supported by way of a cross member which is adjustable with respect to the machine frame for adjusting the stroke position.
According to one another embodiment of the invention, a piston which is guided in the bore of a cylinder connected to the machine frame and which is provided with a shaft is provided as a ram, a stopper, which surrounds the piston shaft and which closes the cylinder bore, being supported by way of a cross member which is adjustable with respect to the machine frame for adjusting the stroke position.
According to a further embodiment of the invention, a piston guided in a cylinder and provided with a shaft passing through the cylinder base is provided as the ram, the cylinder being adjustable in the machine frame for adjusting the stroke position.
Finally, according to yet another embodiment of the invention, a central shaft, which is guided in the machine frame and is provided with an annular flange on which piston-cylinder units engage, is provided as the ram, the piston-cylinder units being supported by way of a cross member which is adjustable with respect to the machine frame for adjusting the stroke position.
In each case, whether the shaft forms part of a piston or part of a cylinder, or whether it forms the ram per se, it has a through bore for receiving the tie rod. The rotary drive connected to the tie rod is advantageously mounted in a bracket to the cross member, so that with the cross member it participates in the adjustment of the stroke position, so that between the tie rod and its rotary drive only the operating stroke has to be compensated and not the total stroke, as would be necessary if the rotary drive were supported directly on the machine frame.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be described in detail with reference to the accompanying drawings wherein:
FIG. 1 is an elevational general axial view of a forging machine in accordance with the invention with the workpiece shown in cross section;
FIG. 2 is an enlarged cross-sectional view of one of the rams of the machine of FIG. 1, generally in a plane transverse to the longitudinal axis of the workpiece;
FIG. 3 is a further enlarged cross-sectional view showing details of the upper part of FIG. 2;
FIG. 4 is a cross-sectional view taken along line A-A in FIG. 3;
FIG. 5 is a further enlarged cross-sectional view showing details of the lower part of FIG. 2;
FIG. 6 is a cross-sectional view taken along section line B-B in FIG. 5; and
FIGS. 7, 8 and 9 are schematic reduced cross-sectional views corresponding to FIG. 2 illustrating further embodiments of the invention.
DETAILED DESCRIPTION
A forging work-piece 1 to be forged is shown in cross-section in FIG. 1. The cross-sectional size is determined by the respective inner end position of the stroke of the tools relative to one another and the position of the tools 2 corresponding thereto. It can be seen that only part of the end surface of each ram is used, the unused width of the operative end surface of each tool 2 being covered in one stroke end position by the lateral surface of one adjacent tool 2. The greatest available cross-section, determined by the width of the tool, and the smallest cross-section, determined by the maximum mutual covering of the tools 2, are shown in broken lines in FIG. 1.
The tools 2 are supported and moved by rams 3, which are arranged axially movably in the machine frame 4. Four rams 3 are provided, which are arranged in a cross in a single common plane, at right angles to the longitudinal axis of the workpiece, and are moved radially to the workpiece 1. The lateral setting of the tools 2 relative to the rams 3 is carried out by means of movable crosspiece 5, which together with the rams 3 form supports, such that the crosspieces 5 can be adjusted and fixed transversely to the axes of the rams in the operating plane. The stroke end position of a tool 2, which depends on the cross-section sought, determines the lateral setting of an adjacent tool, which with its lateral surface covers the unused width of the operative surface of the first tool 2.
In the embodiment shown in FIGS. 1 to 6, each ram 3 is constructed as a cylinder 6 which is guided in the machine frame 4 in guide members 7 and 8, which can be constructed as round or flat guides, in the latter case to prevent the cylinder 6 from rotating in the machine frame 4. A shaft 9, which is secured to the cylinder 6 by a nut 10, is inserted into the cylinder base, which has a through bore. An annular piston 11, which surrounds the shaft 9, is supported on the machine frame 4 by way of a cross member 12. For this purpose, tie rods, which are extended to form spindles 13 with threaded shafts 14, are mounted into the machine frame 4. Nuts 20, which are provided with toothing 19 on the outside and with threads on the inside, are mounted rotatably in the cross members 12 and are held by split bearing plates 21. The four nuts 20 of one cross member 12 are turned jointly by a toothed ring 22 which can be rotated on balls 23 on a bearing ring 24 centered and mounted on the cross member 12. A motor 28 with a pinion is provided for driving the toothed ring 22. By turning the toothed ring 22 and thus the nuts 20, the position of the cross member 12 along the spindles 13 changes and thus the position of the annular piston 11 changes with respect to the cross member 12 and the stroke position of the associated ram 3. The operating stroke of the cylinder 6 or ram 3 respectively is limited by the stroke path of a pull-back piston 30. For this purpose a plate 31, in which are formed the cylinders 32 which receive the pull-back pistons 30, is mounted on the cross member 12, and a further cross member 33, on which the pistons 30 abut to limit the stroke path of the ram 3 and cause it to return, is connected to the shaft 9.
The shaft 9 is bored through its entire length and in its bore 35 receives a tie rod 36 which is provided with collars 37 and 38 at opposite ends. The tie rod 36 also passes through the crosspiece 5 mounted on the end face of the ram 3. The collar 37 is mounted on the inner end (relative to the workpiece) of the tie rod 36 and is connected to it by wedges 39, and bears against the crosspiece 5. The collar 37 is constructed as a lever, on which is a pin 40 and a slide block 41 is mounted on the pin 40. The pin 40 and slide block 41 engage in one arm, constructed as a slotted guide 42, of a T-shaped recess in the crosspiece 5, while the other arm, in the form of slotted guide 43 (the crosspiece of the T), forms the passage for the tie rod 36. Guide blocks 44, which guide the crosspiece 5 by engaging guide grooves 45 in it, are formed in recesses on the end face of the ram 3. Inter-locking members 46, which have fine toothed racks 47 on their opposed faces, are inserted in further recesses on the end face of the ram 3 and in corresponding recesses in the crosspiece 5. The recess in the crosspiece 5, which receives the collar 37, is closed by a cover 48, which encloses the collar 37 and also acts as a support plate for the tool 2.
A spring cup 50, which accommodates a set of springs 51, is secured to the shaft 9. Spring plates 52 and 53 support the set of springs 51, by way of axial bearings 54 and 55, at one end on the base of the spring cup 50 and at the other end on the outer collar 38 of the tie rod 36. A cover 56 of the spring cup 50 is constructed with an annular cylinder 57, in which an annular piston 58 is guided. When the cylinder 57 is pressurized the tie rod 36 is displaced axially by means of the collar 38, tie rod 36, via the cover 48, pushes the crosspiece 5 away from the ram 3 so that the intermeshing toothing 47 of the locking members 46 disengages, and by turning the tie rod 36 the crosspiece 5 can be displaced transversely to the axis of the ram in the operating plane, by way of the collar 37, the pins 40 and the slide block 41.
At its outer end the tie rod 36 is extended and is formed as a multiply splined pin 59 and the latter engages in a multiply splined hub 60, which is mounted axially fixed with radial clearance in a bracket 61 mounted on the cross member 12. A gearwheel 62, which is connected rotationally rigidly to the hub 60 by way of an Oldham coupling 63, is mounted in the bracket 61. The gearwheel 62 is driven by two plungers 64 and 65 which operate in opposite directions and which are connected to toothed racks 66 which mesh with the gearwheel 62.
When annular piston 58 is pressurized, thereby displacing the rod 36 and cross piece 5, compressed air is fed by way of a supply line (no shown) into the bore 35, and emerges by way of bores 67 and the gap existing between the end face of the ram and the crosspiece 5 and prevents contamination.
The actuation of the turning apparatus, i.e. the pressurizing of the plungers 64, 65 is possible only when the annular piston 58 is also pressurized to release the crosspiece 5 from engagement with the ram by toothing 47. The displacement of the tools 2 by the plungers 64 and 65 is performed as a function of the stroke position setting of the adjacent ram 3 by the motor 28.
Further embodiments are shown diagrammatically in FIGS. 7, 8 and 9, the same reference numerals being used for corresponding parts.
In the embodiment illustrated in FIG. 7 the machine frame 4 is constructed as a cylinder or is rigidly connected to the cylinder. The ram 3a is constructed as a piston 68 and the cylinder is closed by a stopper 15, through which the shaft 69 of the piston 68 passes. The stopper 15 is connected to a cross member 17 which is displaceable along the spindles 13 for setting the stroke position.
In the embodiment illustrated in FIG. 8, the ram 3b, constructed as a piston 70, is guided in a cylinder 71 which is guided and adjustable in the machine frame 4, for which purpose the cylinder 71 is provided with a neck 72 which has a thread and is adjustable by a nut 73 mounted in the machine frame for setting the stroke position.
In the embodiment illustrated in FIG. 9, the ram 3c is guided directly in the machine frame 4. The piston-cylinder units 74 which move the ram 3c and which are connected to the ram 3c by way of an annular flange 75, are supported on the machine frame 4 by way of a cross member 76, for which purpose the cross member 76 is longitudinally adjustable by spindles 74, in order to set the stroke position.
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A forging machine having rams arranged in the form of a cross carry respective tools adjustable transversely to the ram axes and partly overlapping one another, so that a closed pass can be formed for any size of the forging pass. To adjust the tools transversely, each tool is carried on a respective crosspiece which can be clamped against the ram end or can be released and moved transversely on the ram. The clamping and releasing and the adjustment movement are all effected by a rotary tie rod extending through the crosspiece and through the ram, having one end coupled to the crosspiece for clamping it and moving it transversely to the ram, and the other end coupled to a clamping mechanism and to a rotary adjustment drive.
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This application claims the benefit of Provisional application Ser. No. 60/196,517, filed Apr. 11, 2000.
BACKGROUND
1. Technical Field
The present disclosure relates generally to the field of endoscopic surgical devices. More specifically, the present disclosure relates to an endoscopic fastener applying device for repairing torn tissue such as torn meniscus tissue.
2. Background of Related Art
One known technique for repairing torn meniscus tissue involves the use of a pair of surgical needles which are inserted through cannuli into the knee on opposite sides of a meniscal tear. The ends of the needles include a length of suture material which is pushed down through the cannuli and across the tear. An incision is made in the skin at the point where the needle exits the knee joint so that the leading end of each needle may be grasped and pulled through the joint. The ends of the sutures are then grasped after the needles are removed from the suture ends and the suture is then tied so that a horizontal suture is created in the meniscus. This procedure is repeated for placement of as many sutures as necessary to repair the meniscus tear. As is apparent, this process is both time consuming and difficult to effect.
A subsequent improvement over this procedure is outlined in U.S. Pat. No. 5,002,562, the contents of which are incorporated herein by reference. In this procedure, a barbed clip and an instrument for applying the clip are utilized. The instrument has a pair of opposed arcuate jaws which are shaped to hold a complementary-shaped curved surgical clip therebetween, such that the barbs of the clip are retained within notches in the jaws until the clip is inserted. The legs of the clip are joined by a flexible suture material. The jaws are biased in a normally open position, and as the jaws are pushed into the tissue, the jaws are scissored or closed together until they preferably overlap to move the legs of the clip together until they cross. The jaws are then reopened and backed out of the tissue, with the barbs of the clip retaining the clip in position in the tissue.
A further refinement to meniscal repair is illustrated in U.S. Pat. No. 5,997,552, the contents of which are incorporated herein by reference. This patent details a meniscal fastener applying device which applies fasteners sequentially from a longitudinally extending magazine. An advancing mechanism is operatively associated with an elongated body portion of the device for sequentially advancing surgical fasteners from a fastener supply to a firing position in alignment with a firing mechanism. The fastener includes a pair of anchor members whose proximal-most ends are connected by a suture material offset from the central longitudinal axis thereof. Because of the parallel over-under orientation of the firing mechanism and the longitudinally extending fastener magazine, the elongated body portion of the device requires a substantial cross-sectional area and necessarily requires a correspondingly wide distension of the knee joint to access the meniscal tissue to be repaired.
SUMMARY
A single shot meniscal repair device is provided which incorporates a minimally sized elongate body portion configured to hold a single fastener adjacent a distal end thereof. The elongate body portion is part of a disposable loading unit structure which facilitates up to 360° rotation about the longitudinal axis of the elongate body portion. In an alternate embodiment, at least a distal portion of the elongate body portion is angled off axis to enhance the versatility of the device. The fastener applied by the device includes a pair of anchor members interconnected by a flexible material. The flexible material extends from a respective side of the anchor members, thus maintaining the proximal ends thereof clear to receive the full driving force from the firing assembly without the risk of damaging the connecting flexible material.
BRIEF DESCRIPTION OF THE DRAWINGS
Various embodiments are described herein with reference to the drawings, wherein:
FIG. 1 is a perspective view of one embodiment of the meniscal repair device of the present disclosure;
FIG. 2 is a perspective view with parts separated of the meniscal repair device of FIG. 1;
FIG. 3 is a perspective view showing the elongate body portion of the meniscal repair device of FIG. 1;
FIG. 4 is a perspective view showing a 10° upsweep version of the elongate body portion in accordance with one embodiment of the meniscal repair device of the present disclosure;
FIG. 5 is a perspective view showing a 30° left/right bend version of the elongate body portion in accordance with one embodiment of the meniscal repair device of the present disclosure; and
FIG. 6 is an enlarged perspective view showing the fastener used in the meniscal repair device of the present disclosure.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Preferred embodiments of the presently disclosed stapler will now be described in detail with reference to the drawings, in which like reference numerals designate identical or corresponding elements in each of the several views.
Referring now to the drawings, FIG. 1 illustrates a first embodiment of the fastener applying device shown generally as 10 . Briefly, the staple applying device 10 includes a housing assembly 12 and a disposable loading unit 13 having an elongated body portion 14 defining a longitudinal axis thereof. The elongated body portion 14 is preferably minimally dimensioned for arthroscopic utilization.
The components of the housing assembly 12 of the fastener applying device 10 are best illustrated in FIG. 2 . The housing assembly 12 includes a housing formed from molded housing half-sections 12 a and 12 b within which the components of the housing assembly 12 are positioned. The housing assembly 12 further includes a movable handle 22 and a stationary handle 24 which is formed from portions extending from housing half-sections 12 a and 12 b to form a pistol grip type handle. Movable handle 22 and stationary handle 24 facilitate remote actuation of a firing assembly 52 through the elongated body portion 14 to effect the ejection of a surgical fastener 30 from the distal end of the elongated body portion 14 .
The movable handle member 22 is secured to the housing half sections 12 a and 12 b by a pin 26 which permits rotation of the movable handle 22 relative to the stationary handle 24 . A handle spring 28 is connected to the movable handle 22 by a pin 20 and to the housing 12 by a pin 34 so as to bias the movable handle 22 to an open position. The pin 20 is dimensioned to be received in openings 21 formed in the movable handle 22 .
An actuation arm member 32 is operatively associated with the movable handle 22 and is pivotably connected to the lower end of the stationary handle 24 by pin 34 . A cam roller member 36 is rotatably mounted to the movable handle 22 and is configured to engage and move along a cam path surface 38 defined on the actuation arm member 32 by the proximal facing outer surface thereof. Engagement between the cam roller member 36 and the cam path surface 38 effectuates counter-clockwise rotation of the actuation arm member 32 about pin 34 when the instrument is viewed from the right side, as shown in FIG. 2 .
A latch member 40 is pivotably mounted to the top portion of the actuation arm 32 by pivot members 41 . The latch member 40 is dimensioned and configured to detachably engage with a firing block 42 which is slidably mounted in the housing assembly 12 . An engaging spring 46 connects the latch member 40 to the actuation arm member 32 so as to pivot the latch member 40 about pivot members 41 into engagement with the firing block 42 . The latch member 40 has a hook member 49 pivotable about pivot members 41 into engagement with a post 51 formed on the firing block 42 .
As mentioned above, the firing block 42 is slidably mounted in the housing assembly 12 and is movable in response to corresponding movement of the movable handle member 22 . A mounting projection 50 extends from the end of the firing block 42 and is dimensioned and configured so as to detachably engage with the proximal end 53 of firing plate 52 .
A bearing washer 60 is received about and engages a central portion 55 of the firing block 42 , and a snap washer 62 is fixedly attached to the distal end portion 42 b of the firing block 42 to capture and retain a compression spring 58 therebetween. Upon actuation of the handle assembly, the compression spring 58 is compressed between bearing washer 60 and snap washer 62 creating a force urging firing block 42 in a distal direction. Additional washers 65 for sealing, spacing and fitting purposes may be operatively associated with the distal end portion 42 b of the firing block 42 .
As described above, proximal movement of the movable handle 22 causes the cam roller 36 to engage the cam path surface 38 and rotate actuating arm member 32 and latch member 40 in a counter-clockwise direction when viewing the instrument from the right side, as shown in FIG. 2 . The hook member 49 formed on the latch member 40 engages post 51 formed on the firing block 42 to slide the firing block 42 proximally as latch member 40 and actuating cam member 32 rotate counter-clockwise in response to proximal movement of handle 22 . The proximal movement of the firing block 42 causes bearing washer 60 to engage a bearing surface 64 defined on the interior of the housing assembly 12 (See FIG. 2 ). As the firing block 42 is moved proximally, the compression spring 58 is compressed between the washer 60 and the snap washer 62 creating a force urging firing block 42 in a distal direction. After the spring 58 has been compressed, the latch member 40 contacts a camming wall 66 defined in the proximal end portion of the housing assembly 12 which, in turn, causes the latch member 40 to pivot clockwise about members 41 to disengage hook member 49 from post 51 . The release of stored energy from the compression spring 58 urges the firing block 42 to move distally resulting in corresponding distal movement of the firing plate 52 .
As firing plate 52 moves distally, it engages rod holder 70 and continues in combined distal movement to drive parallel push rods 72 distally to engage and eject fastener 30 . Upon completion of the firing motion, handle 22 is relaxed thus withdrawing firing block 42 and firing plate 52 proximally relative to rod holder 70 and push rods 72 .
The disposable loading unit 13 includes rotational housing 80 formed of housing half-sections 80 a and 80 b. Mounted within housing 80 are the firing plate 52 and rod holder 70 . The elongate body portion 14 is mounted to housing 80 by pins 82 and extends distally therefrom. Push rods 72 are attached to rod holder 70 and are disposed within the elongate body portion 14 . A new fastener 30 is disposed adjacent a distal end 74 of elongate body portion 14 .
Once firing is completed, the expended disposable loading unit 13 is rotated relative to the housing 12 effectively disengaging firing plate 52 from mounting projection 50 on firing block 42 . The expended disposable loading unit is then withdrawn distally from housing 12 and discarded. A new disposable loading unit is inserted into housing 12 and rotated to engage mounting projection 50 with proximal end 53 of mounting plate 52 . The device 10 is then ready for subsequent firing.
Referring to FIG. 3, the elongate body portion 14 is illustrated in a series of views. Rods 72 are configured and dimensioned to travel coaxially within the elongate body portion 14 . The cross-sectional dimensions of elongate body portion 14 are minimized to more easily facilitate introduction to the operative site. A locating barb 76 can be positioned at a distal end of the elongate body portion 14 to assist in stabilizing the device at the firing point.
FIGS. 4 and 5 illustrate alternate embodiments of elongate body portion 14 wherein the distal portion is upswept by 10° (FIG. 4) or bent left/right by 30° (FIG. 5 ). Elongate body portions shown in FIGS. 4 and 5 are otherwise substantially the same as shown in FIG. 3 .
A fastener 30 for use in device 10 is illustrated in FIG. 6 in a series of views. Fastener 30 includes a pair of anchor members 90 linked by a flexible member 92 . Preferably, the entire fastener is formed of bioabsorbable material which resorbs at an appropriate rate to facilitate healing of a tear in the meniscus. Each of the anchors 90 has a tapered distal end 94 and a planar proximal end 96 . Flexible member 92 extends between adjacent side surfaces 98 of anchors 90 spaced between the proximal end 96 and the distal end 94 thereof. This configuration protects the flexible member 92 from inadvertent damage caused by the rods 72 . Each anchor member 90 is further provided with a series of radial projections 100 on its periphery to inhibit withdrawal of the anchor members 90 once they have been positioned within body tissue.
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A surgical fastener application apparatus for applying surgical fasteners of general U-shape to body tissue is provided which includes a housing having a handle portion and a trigger mechanism, an elongated body portion extending from the housing, the elongated body portion having generally annular cross-sectional area substantially along the length thereof and defining a longitudinal pathway therein, and a firing mechanism operatively connected to the housing and including a pair of substantially parallel push rods positioned within the longitudinal pathway of the elongated body portion, the firing mechanism being capable of driving a surgical fastener inserted in a distal end portion of elongated body portion to the body tissue in response to operation of the trigger mechanism.
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FIELD OF THE INVENTION
This invention relates to a device for cleaning air hoses and more particularly to an open ended airway tube designed to be attached to a continuous positive airway apparatus, such as a respirator and similar devices.
TECHNICAL BACKGROUND
The use of respirators and similar breathing apparatus have become a regular part of life for many. In addition to those needing respirators and similar devices for a medical condition, such asthma and emphysema, new strategies for healing illnesses are being developed that use oxygen therapy. Oxygen therapy relies heavily on such breathing apparatus because the cost of a hyperbaric chamber is prohibitive for most folks.
The breathing apparatus is referred to herein as a continuous positive airway apparatus CPAP. This apparatus develops a concentrated oxygenated air stream within the apparatus using the environmental air. The CPAP apparatus includes an output. Connected to the output of the CPAP is a hose or an airway tube. The subject of this invention is the cleaning of the airway tube.
Typically manufacturers of such tubular airways recommend cleaning with the use of a mild soap. The mild soap is mixed with water and then applied to the internal surfaces of the tube to wash away any contaminants. Typically, the soapy water is swished about the inside of the tube and the tube rinsed off and left to air dry.
As readily apparent, this kind of method may be at least somewhat inefficient and very time consuming. Additionally, after repeated usage soap residue builds up on the interior walls of the tube and degrade the tube. Additionally, the water left to its own device does not completely dry before the user is ready for its next use. The user is then left with a wet hose or additional waiting time.
What is needed is a method and device for thoroughly and efficiently cleaning the airway tube.
SUMMARY OF THE INVENTION
Accordingly to overcome the above mentioned disadvantages of the known devices and to solve the long felt needs in the art, it is a general object of the instant invention to provide a kit and a method for using the kit to efficiently and effectively clean hoses intended for use with CPAP apparatus.
It is an additional object of the method and kit of the instant invention to provide a device, which is easily assembled and easy to use to efficiently and effectively clean such hoses.
It is an additional object of the method in accordance with this invention, which enables a user to simply and effectively clean open ended airway tubes.
In accordance with the objects set forth above and as will be described more fully below, the device for cleaning an airway hose, defining an open ended tube, the airway hose specifically adapted for attachment to a continuous positive airway apparatus, in accordance with this invention, comprises:
a cleaning member for cleaning the inside of the open ended tube; a support member, the cleaning element attached to the support member, the support member including means for attaching the cleaning element to the support member and for retaining the cleaning element to the support member during cleaning; and
one end of the support member capable of being fixed during cleaning.
In an exemplary embodiment, the cleaning element comprises a cotton swab having a central opening and is replaceably attached to the support member.
In another exemplary embodiment, the support member is made from a nylon-like material, which provides enough rigidity to be threaded through the central opening of the cleaning element.
In another exemplary embodiment in accordance with this invention, the method of using the device according to the invention comprises the steps of:
supplying a support member having proximal and distal ends and a cleaning member; attaching the cleaning member to the support member such that the cleaning member is in close proximity to the proximal end; inserting the distal end of the support member through the open ended airway tube; securing the distal end of the support member; and
pulling open ended airway tube over the cleaning member.
It is an advantage of the device and method of the invention to provide a kit which enables the user to efficiently and effectively clean tubing intended for use with a CPAP.
It is an additional advantage of the device and method of the invention to provide an economical and readily usable kit which enables the user to efficiently and effectively clean tubing intended for use with a CPAP.
BRIEF DESCRIPTION OF THE DRAWING
For a further understanding of the objects and advantages of the present invention, reference should be made to the following detailed description, taken in conjunction with the accompanying drawing, in which like parts are given like reference numerals and wherein:
FIG. 1 is a plan view illustrating an exemplary embodiment of the cleaning device in accordance with this invention ready for use;
FIG. 2 is a plan view of the cleaning element;
FIG. 3 is a plan view of an exemplary embodiment of the support member and support member with the cleaning element in accordance with this invention;
FIGS. 4 & 5 illustrate an exemplary embodiment of the cleaning device in accordance with this invention in use; and
FIG. 6 illustrates an exemplary embodiment of the full kit of the cleaning device in accordance with this invention.
DETAILED DESCRIPTION OF THE INVENTION
In order to appreciate the invention herein, one must appreciate the need in the art as set forth in the Background and the objects and advantages as described in the Summary of the Invention, above. Most importantly, the structure of the instant invention herein resolves the long felt need to provide the user of a CPAP apparatus with a method and device for efficiently and effectively cleaning the airway supply hose.
With particular reference to FIG. 1 , there is shown the structure of invention, generally indicated by the numeral 20 . The exemplary embodiment of instant invention shown in FIG. 1 includes a cleaning element 22 and a support member 24 . As shown particularly in FIG. 2 , the cleaning element 22 has a central opening 26 providing the means for attaching the cleaning element 22 to the support member 24 .
As shown in FIG. 3 , the support member 24 includes a retaining member 28 as a means for retaining the cleaning member 22 on the support member 24 . As will be explained in more detail below, the exemplary embodiment of the retaining member comprises the proximal end of the support member 24 being turned into a knot and fixed in position.
As illustrated in FIG. 1 , in an exemplary embodiment of the structure in accordance with the invention, the support member 24 and the airway supply hoses have predetermined lengths. As illustrated, the support member 24 is a length somewhat greater than the length of the airway supply hose.
The airway supply hose, once removed from the CPAP defines an open ended tube 30 in the exemplary embodiment shown in FIG. 1 . The tube 30 attaches one end to the CPAP apparatus (not shown) and the other end to the user interface. Typically, a face mask (not shown) provides the user interface.
As noted above, FIG. 2 illustrates in detail the cleaning element 22 having central opening 26 . The cleaning element 22 is attached to the support member 24 by threading distal end of the support member 24 through the central opening 26 as clearly illustrated in FIGS. 1 & 3 .
In the exemplary embodiment of the invention shown in FIG. 2 , the cleaning member 22 comprises a cotton swab having predetermined diameter. The predetermined diameter slightly larger, but compatible with the internal diameter of the tube 30 so that during use the interior surfaces of the tube are thoroughly contacted as will be explained more fully below.
FIG. 3 , illustrates in detail, the support member 24 with and without the cleaning member 22 attached. The support member 24 has a first end, defining a distal end 32 and a second end, defining a proximal end 34 . The distal end 32 is threaded through the central opening 26 of the cleaning member 22 . The proximal end 34 includes structure for retaining the cleaning member 22 on the support member defining a retaining member 36 .
In the exemplary embodiment, the support member 24 defines a rope-like chord of nylon mesh. The distal end 32 is singed to provide a structure which eases the access of the support member 24 through the central opening 26 . In further exemplary embodiments, the distal end 32 is shaped and molded into a pointed end further easing the entry of the support member 24 through the central opening 26 . The singed end of the distal end 32 provides additional rigidity to facilitate the insertion of the distal end 32 through the opening 26 .
The proximal end 34 , in the exemplary embodiment shown in FIG. 3 , is formed into a knot as shown. The knot is heat treated, singed again, as with the distal end 32 . The heat treatment fixes the knot and thus defines a member 36 for retaining the cleaning member 22 on the support member 24 during cleaning.
IN USE
With particular reference to FIGS. 4 & 5 , there is shown the method of use of the cleaning device in accordance with this invention. After assembly of the support member 24 and cleaning member 22 , the distal end 32 of the support member 24 is inserted into one end of the tube 30 . The distal end 32 is then affixed to a stationary household article, for example a dresser draw, which is first opened to allow the distal end 32 to be inserted into the drawer and then closed to secure the drawer with the distal end 32 affixed thereto.
Once so affixed, the support member 24 is in position to support the cleaning member 22 as the tube 30 is pulled over the cleaning member 22 . The oversized cleaning member 22 brushes up against the interior walls 40 . This operation can be repeated as often as required. It is suggested that each cleaning include a replacement of the cleaning member 22 . However, depending upon usage and the amount of containments dislodged by the cleaning member 22 , the same cleaning member 22 can be used for the different hoses connected with the same CPAP. However, it is strongly recommended that the cleaning member 30 be changed for each new CPAP.
Since the cleaning member 30 has a diameter greater than the largest tube to be cleaned connected with the CPAP apparatus, only one size cleaning member 30 is needed for the CPAP apparatus. In other words, the device 20 in accordance with the instant invention uses a single size cleaning member regardless of the make or model of the particular CPAP apparatus. And, each of the hoses of the CPAP apparatus can be cleaned with the same size cleaning element, despite the fact that there are different diameters for each of the hoses.
With particular reference to FIG. 6 , there is shown an additional exemplary embodiment of the cleaning device and method in accordance with this invention. In this embodiment, the same elements including support member 24 and a cleaning member 22 are included. However, the device includes an additional member, namely a cleaning fluid 50 . The cleaning fluid is sprayed onto the cleaning member 22 using an aerosol or pump sprayer 52 . By slightly moistening the cleaning member 22 , more containment is picked up by the cotton swab as the tube passes over it.
The cleaning fluid 50 may be of various types and may vary according to need. Accordingly, there is no best fluid to be provided. However, typically, the cleaning fluid has the composition of soap, vinegar and water solution in the ratio of one part soap, one part vinegar and twenty parts water. A low phosphoric soap is preferred so as to be less toxic to the environment. Of course, the cleaning fluid in accordance with the instant invention is non-toxic and safe as a cleaning fluid for human usage.
While the foregoing detailed description has described several embodiments of the method and cleaning device for cleaning an airway breathing hose in accordance with this invention, it is to be understood that the above description is illustrative only and not limiting of the disclosed invention. It will be appreciated there are variations of the support member, nylon works, but other material for the support member are also suitable. And, while the cleaning member is cotton herein, other various materials are similarly suitable for the purposes and functions of the method and device herein. It will be appreciated that the invention is fully disclosed in the exemplary embodiments discussed above and that there are numerous other embodiments that are not mentioned, but within the scope and spirit of this invention. Thus, the invention is to be limited only by the claims as set forth below.
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Disclosed herein is a method and a device for cleaning an open airway ended tube. The tube being designed for attachment to a continuous positive airway apparatus. The device includes a cleaning element for cleaning the inside of the open ended tube and a support member. The cleaning element attached to the support member. The support member including means for attaching the cleaning element to the support member and for retaining the cleaning element to the support member during cleaning. Additionally, one end of the support member capable of being secured during cleaning.
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BACKGROUND OF THE INVENTION
1. Field of the invention:
This invention relates to a method for the growth of single bulk crystals of compound semiconductors such as ZnS, ZnSe, ZnTe, etc., using the sublimation method or the halogen transportation method, and an apparatus used for the said crystal growth method.
2. Description of the prior art:
The vapor phase transportation method in which crystal materials are transported to a seed crystal by the use of halogen gas is preferably used as a single crystal growth method. According to the vapor phase transportation method, even compounds such as ZnS, etc., having a transition point of about 1020° C. that is below the melting point (about 1830° C.) thereof are grown at a low temperature (e.g., below 1000° C.), so that the passage at the transition point and/or the mixing of polytyped crystals into the single crystal, which may arise in the fusing method in which the compounds are grown at a high temperature (e.g., 1800° C.) under a high pressure (e.g., several tens of atmosphere), can be avoided. Therefore, the vapor phase transportation method in which halogen gas is used as a transporting agent is important to the growth of a single bulk crystal of the above-mentioned compounds. However, since halogen elements (i.e., I, Br, Cl and F) are active even at room temperature (namely, I and Br have a high vapor pressure at room temperature and Cl and F are gaseous at room temperature), a charging process for the charge of a crystal growth vessel with halogen elements becomes complicated. Moreover, it is difficult to accurately add a given amount of halogen to the growth vessel without contamination by foreign substances, while the inside of the growth vessel is maintained at a high vacuum level (e.g., less than 10 -6 Torr) in the charging process. In order to remove these problems, an approach in which the volume of halogen required to provide a given amount after vaporization is measured in advance or an approach in which a given amount of halogen is sealed within a small ampule and then the ampule is added to the growth vessel together with crystal materials has been proposed. The former approach requires measurements of a volume of halogen which necessitate vaporization of halogen using a heating process and solidification of halogen using liquid nitrogen, which causes difficulties in preventing the mixing of water vapor and/or air into the growth vessel in the halogen-charging process. In the latter approach, loss in halogen arises when the halogen-ampule is sealed, resulting in an incorrect amount of halogen. Accordingly, these approaches cannot attain the addition of an accurate amount of halogen with reproducibility to the growth vessel.
As mentioned above, in the vapor phase transportation method in which halogen is used as a transporting agent, prevention of mixing gases such as water vapor, air, etc., into the growth vessel when the growth vessel is charged with halogen is difficult in light of the physical properties of halogen, so that the amount of halogen to be added to the growth vessels cannot be maintained at a fixed value for each vessel, which causes difficulties in establishment of reproduceable crystal growth conditions, resulting in an extremely reduced amount of crystal materials to be transported by the halogen or in the growth of polytype crystals.
In order to solve the above-mentioned problems, a crystal growth method has been proposed in which, as shown in FIG. 3, the temperature distribution is maintained to be in the range of T 1 to T 2 and ampules with a specific design is used, and moreover the seed crystal growth section 23 are separated from the single crystal growth section 25 within the growth vessel 22 so as to regulate the crystal growth. Reference numerals 24 and 26 indicate a crystal material and a heater, respectively. Since this method adopts such a crystal growth environment in which the temperature distribution is in a fixed range of T 1 to T 2 so as to improve the reproducibility of the crystal growth, when the conditions under which halogen is supplied to ampules are different and/or water vapor, air, etc., are mixed into the growth vessel, distorted crystals that are inferior in crystallinity are produced. Moreover, if the growth conditions (including the supply of halogen to ampules, growth temperatures, etc.), are changed in view of the physical property control, there is a possibility that they will vary from the optimal single crystal growth conditions. These problems are caused by the phenomenon that distortions of crystals arising from the beginning crystal growth are taken over by the succeeding crystal growth.
SUMMARY OF THE INVENTION
The method for the growth of a compound semiconductor bulk crystal, using the sublimation method or the halogen transportation method, of this invention, which overcomes the above-discussed and numerous other disadvantages and deficiencies of the prior art, comprises maintaining the temperature of a limited portion of the crystal, which has just begun to grow, at a higher level than that of the crystal growth temperature, thereby attaining control of the crystallinity of the crystal at the initial growth stage.
In a preferred embodiment, temperature control is performed using a first heater which creates a temperature distribution over the whole area within a crystal growth vessel including both the crystal growth region and the crystal material storage region and a second heater which controls the temperature of a limited area within the crystal growth vessel corresponding to the desired portion of the crystal that has just begun to grow.
In a more preferred embodiment, transporting mediums used in said halogen transportation method are compounds made of a metallic or submetallic element and a halogen element, said halogen compounds being chemically stable at room temperature and being decomposed at a temperature that is lower than the crystal growth temperature.
The apparatus for the growth of a compound semiconductor crystal, using the sublimation method or the halogen transportation method, of this invention, comprises a crystal growth vessel, a first heater that is wound around the body of the vessel, and a second heater that is disposed movably up and down in a space between the first heater and the vessel, said first heater creating a temperature distribution over the whole area within the vessel and the second heater controlling the temperature of a limited area within the vessel corresponding to the desired portion of a crystal that has just begun to grow.
Thus, the invention described herein makes possible the objects of (1) providing a method for the growth of compound semiconductor crystals in which halogen compounds that meet a specific requirement are used as a transporting medium, thereby attaining extreme simplification of the process for the preparation of ampules required for crystal growth and creating reproduceable inner conditions of the ampules, which results in good quality single bulk crystals on a large scale that are reproduceable; (2) providing a method for the growth of compound semiconductor crystals in which the beginning conditions of the single bulk crystal growth of the II-VI group compound semiconductors such as ZnS, ZnSe, etc., are controlled in a given space for a given period of time, so that a good quality single bulk crystal can be grown with reproducibility; (3) providing a method for the growth of compound semiconductors in which a local portion of the beginning crystal growing from a seed crystal is heated to a high temperature so as to soften the effects of changes in the supersaturation of crystal material gases and/or the effects of the gas flowing on the crystal growth, resulting in a good quality crystal in which distortion has been minimized before the crystal growing from the seed crystal becomes thick, so that the progress of an excellent single-crystal growth can be effected in the succeeding bulk crystallization; and (4) providing an apparatus with a double heating structure for the above-mentioned method, by which despite the difference in the beginning conditions of the single bulk crystal growth for each sample, a good quality single bulk crystal can be grown with reproducibility.
BRIEF DESCRIPTION OF THE DRAWINGS
This invention may be better understood and its numerous objects and advantages will become apparent to those skilled in the art by reference to the accompanying drawings as follows:
FIG. 1 is a schematic diagram showing the basic structure of an apparatus of this invention.
FIG. 2 is a schematic diagram showing an apparatus used in the method for the growth of single bulk crystals of this invention.
FIG. 3 is a schematic diagram showing an apparatus used in a conventional method for the growth of single bulk crystals.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
According to a crystal growth technique using a vapor phase of this invention, the growth of crystals onto a seed crystal progresses depending upon the supersaturation of the crystal material in the low temperature zone in the crystal growth vessel, and accordingly time and spacial changes in the supersaturation of the crystal material influence crystallization of the crystal material, resulting in the growth of crystals containing single crystals, skeleton crystals, dendrites, etc. Especially, when the vapor flows, the supersaturation of the crystal material varies depending upon a variation in temperatures, temperature gradient, time and spatial variation in the vapor flow, and non-uniformity of the vapor flow. The above-mentioned variables within a growth apparatus arise in a transient state of the beginning of the growth stage in light of crystal growth theory, and control in the beginning crystal growth stage is especially important to obtain good quality single bulk crystals.
The main feature of this invention is in that the supersaturation of the crystal material is controlled (that is, time and spatial changes in the supersaturation of the crystal material are reduced) by heating a limited area within the growth vessel corresponding to the desired portion of crystals growing at the beginning, to a temperature that is higher than the temperature at which single crystals grow, so that distortion of crystals arising from the beginning growth can be reduced, which makes possible the progress of a stable growth of good quality crystals onto a seed crystal.
Another feature of this invention is to provide an apparatus with a double heating structure constituted by a first heater that creates a given temperature distribution and a second heater that creates a higher temperature distribution in a limited area within the growth vessel that can be selected as desired in such a manner that the higher temperature distribution formed by the second heater is superposed on the lower temperature distribution formed by the first heater. More particularly, the temperature distribution composed of a material temperature at which the crystal material is vaporized and a growth temperature (this temperature being lower than the material temperature) at which single crystals grow is created by the first heater. Under this temperature condition, crystals grow onto a seed crystal. When the crystals extend to a certain length from the seed crystal, a limited portion of the crystals from the top is heated by the second heater so as to regulate a difference between the crystal surface temperature and the material temperature. The crystals are further heated until they extend to a given length from the seed crystal, and then the operation of the second heater is stopped, after which the growth of the crystals progresses by the use of the first heater alone, resulting in uniform and good quality crystals.
Another feature of this invention is to use halogen compounds that are stable at room temperature and that generate halogen gases at a crystal growth temperature, instead of halogens that are unstable at room temperature at which crystal growth ampules are prepared, as a halogen transporting medium of the vapor phase transportation method. Halogens (i.e., I, Br, Cl and F) that exist in a solid, liquid or gaseous form at room temperature are unstable, which makes their manipulation difficult. If certain halogen compounds XAn (wherein X is the metallic or submetallic elements, A is the halogens and n is an integer such as 1, 2, 3, etc.) that are stable at a temperature in the range of 0° to about 200° C. at which ampules are prepared and that generate halogen gases by thermal decomposition at a growth temperature above 700° C. are selected, the abovementioned problems will be solved. Since the compounds XAn are stable at room temperature, it is possible to set an accurate amount of halogens to be added to the vessel. It is also possible to create a sufficient vacuum of less than 10 -6 Torr inside of the ampules. Moreover, the preparation of the ampules and the equipment therefor can be simplified. In this way, the growth conditions under which single bulk crystals of compound semiconductors grow can be set so that such single bulk crystals can be easily reproduceable.
EXAMPLE 1
This example discloses a method for the growth of single crystals of ZnS and ZnSe using iodine as a transporting medium. This example also discloses a crystal growth apparatus.
FIG. 1 shows the basic structure of a crystal growth apparatus of this invention, using iodine as a transporting medium. The apparatus comprises a growth vessel 111, a first heater 8 that is wound around the body of the vessel 111, and a second heater 9 that is disposed movably up and down in a space between the first heater 8 and the vessel 111. The body of the vessel 111 is constituted by a quartz ampule 1, in which a seed crystal 2, a bulk single crystal 7, etc., are disposed in the upper area and a crystal material 3 such as ZnS or ZnSe is placed in the lower area. The quartz ampule 1 is of a cylindrical shape with a diameter of 30 mm and a length of 100 mm. A heat sink 4 is disposed above the seed crystal 2 in a manner to be in contact with the seed crystal 2. The second heater 9 is connected to a driving system 10 by which the second heater 9 moves up and down. The seed crystal 2 faces the growth space through a hole that is formed in the upper wall of the quartz ampule 1 and a crystal grows through the hole.
The quartz ampule 1 is heated by the first heater 8 to create a temperature distribution over the whole area within the quartz ampule 1 including the crystal material storage region of a temperature T 1 and the crystal growth region of a temperature T 2 , and the crystal growth begins. That is, when the crystal material 3 is heated to a temperature T 1 , it is vaporized together with iodine gas as a transporting medium. As a result, the vaporized crystal material is carried to the seed crystal 2 and deposited thereon. When the crystal grows on the seed crystal 2 to a length of about 5 mm (this state being indicated as a reference numeral 5 in FIG. 1), the second heater 9 operates to heat a limited area within the quartz ampule 1 corresponding to the desired portion of the fine crystal 5 to a temperature T 3 (T 3 >T 2 ). Under these temperature conditions, the fine crystal 5 continues to grow until the length of the crystal 5 becomes 10 to 15 mm. The desired portion of the crystal 5 obtains thermal energy by being heated to a temperature T 3 , so that the mismatch in crystal configuration and/or the crystal defect disappears due to atomic motion by which surface diffusion and/or a lattice match can be carried out. The instability at the initial growth stage can be almost eliminated at the time when the length of the fine crystal 5 becomes greater than 10 mm, and heat from the second heater 9 is reduced or stopped at once and the growth of a single crystal of ZnS or ZnSe further progresses at the growth temperature T 2 which is attained using mainly the first heater 8. By the above-mentioned heating process, the occurrence of defects in the growing crystal can be prevented, resulting in the growth of a good quality crystal 7.
The second heater 9 which is movable up and down can heat a desired portion of the crystal in order to prevent uneven growth of the crystal, so that even when accidental changes in the shape of the crystal arise during growth, heating control can be performed by the second heater 9, which makes the regrowth of a single crystal possible.
The structure of the above-mentioned apparatus is shown in detail in FIG. 2, in which the ampule 1 is connected to a positioning means 44 by a supporting rod 33 and a motor 55. The ampule 1 is positioned in a desired region within the furnace 80. The second heater 9 is also connected to a positioning means 100 by which the second heater 9 is positioned at a desired location to heat a limited area of the crystal during growth. The crystal within the ampule 1 can be observed through windows 66 to which TV cameras 77 are connected. This apparatus can be connected to a computer system 78 by which the growth of crystals is monitored, the crystal growth is automatically controlled to attain optimal conditions, and the data obtained with regard to the single crystal growth are collected and recorded.
EXAMPLE 2
This example discloses a method for the growth of a single crystal of ZnS and ZnSe, using iodine compounds such as AgI (the decomposition temperature thereof being 552° C.), BiI 3 (the decomposition temperature thereof being 500° C.), GeI 4 (the decomposition temperature thereof being 375° C.), etc., as a transporting medium. Each iodine compound is stable at room temperature (that is, it has a low vapor pressure at room temperature) and a certain amount of iodine compound that corresponds to the amount of halogen to be required as a transporting medium can be accurately weighed. The weighed iodine compound is added to an ampule together with a crystal material. The ampule is then subjected to a crystal growth process using the halogen transportation method. The crystal material such as ZnS or ZnSe is vaporized, as mentioned in Example 1, together with iodine gas generated from the iodine compound and grown onto a seed crystal or a nucleus that has spontaneously generated, resulting in a good quality single bulk crystal of ZnS or ZnSe. Temperature control as described in Example 1 is carried out as needed.
When AgI or BiI 3 is used as a transporting medium, since Ag is a monad and Bi is a pentad and they function as an acceptor impurity against ZnS and ZnSe, both of which are a II-VI group compound semiconductor, they compensate I, a donor impurity, to thereby control the conductivity, resulting in a ZnS or ZnSe single bulk crystal having sufficiently high electrical resistance.
EXAMPLE 3
A single-crystal growth of ZnS and ZnSe by the halogen transportation method using bromine as a transporting medium has not yet been reported, but, in this example, SeBr 4 (the decomposition temperature thereof being 75° C.) was used, instead of bromine, as a transporting medium by the same method as in Example 2, resulting in single crystals of ZnS and ZnSe, respectively, grown with reproducibility.
EXAMPLE 4
Instead of iodine that is used in the halogen transportation method, chlorine compounds such as PtCl 4 (the decomposition temperature thereof being 370° C.) and TiCl 3 (the decomposition temperature thereof being 440° C.) were used as a transporting medium in a method for the growth of a single bulk crystal of this example, and good quality single bulk crystals of ZnS and ZnSe, were respectively grown.
It is understood that various other modifications will be apparent to and can be readily made by those skilled in the art without departing from the scope and spirit of this invention. Accordingly, it is not intended that the scope of the claims appended hereto be limited to the description as set forth herein, but rather that the claims be construed as encompassing all the features of patentable novelty that reside in the present invention, including all features that would be treated as equivalents thereof by those skilled in the art to which this invention pertains.
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A method for the growth of a compound semiconductor crystal using the sublimation method or the halogen transportation method, comprising maintaining the temperature of a limited portion of the crystal, which has just begun to grow, at a higher level than that of the crystal growth temperature, thereby attaining control of the crystallinity of the crystal at the initial growth stage, and an apparatus for the said method.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority from International Application No. PCT/EP 99/01817 filed on Mar. 18, 1999, which was published in English as WO 99/49097 on Sep. 30, 1999, and which in turn claims priority from FP 98400721.1 filed on Mar. 26, 1998.
BACKGROUND OF THE INVENTION
The present invention relates to an organic substrate having optical layers deposited by magnetron sputtering, and to a method for preparing it.
In the ophthalmic field, substrates in transparent organic materials obtained, for example, by polymerizing acrylic, allylic, methacrylic or vinylic monomers are in everyday use. Deposition of thin films on lenses, such as ophthalmic lenses, in such organic materials, or in inorganic materials is also in common use. This for example makes it possible to provide anti-reflective treatment, by successive deposition of different thin films. It is necessary, in such applications, to accurately control the nature and thickness of the various layers deposited.
Conventionally, deposition of thin anti-reflective layers on ophthalmic lenses is done by vacuum evaporation. An organic substrate to be coated with or without an anti-abrasive layer, is placed in a vacuum chamber and the material to be deposited is thermally evaporated by heating or by electron bombardment. In order to improve adhesion of the thin films obtained, the substrates to be coated are heated. In the case of an organic material, the substrate must not be heated beyond 100° C.
Such a technique suffers from disadvantages. It is difficult to automate and does not allow continuous flow coating of substrates. Furthermore, stability and reproducibility of the method are not strictly guaranteed.
The layers of the anti-reflective stack can also be deposited by radiofrequency oxide sputtering, but the low rate of deposition renders this technique barely suitable for industrial use. Moreover, this type of method is poorly adapted to the use of targets of large dimensions, thereby limiting the size of the coated substrates.
As against this, cathodic sputtering, which is readily automated, makes it possible to coat substrates of varying dimensions, using continuous or semi-continues flow, while simultaneously ensuring the process is stable. It has thus been proposed to deposit thin films using magnetron sputtering at direct current (DC). This technique consists in vaporizing a solid target which has been brought to a negative potential by the action of a plasma, typically of an inert gas such as argon. Particles detached from the target are deposited on the surface to be coated at a rate, and density, which are far superior to those obtainable with low temperature vacuum deposition. The presence of a magnetic field close to the target, having lines of force parallel to the surface of the target, improves deposition rate by increasing the number of atoms that are vaporized; magnets are used for creating such a field close to the target. The operation is performed in an enclosure under high vacuum, and is called magnetron sputtering.
The technique of magnetron sputtering is well suited to the deposition of metals. In optical applications, it is necessary to deposit layers such as ZrO 2 , SiO 2 , TiO 2 , Nb 2 O 5 , Al 2 O 3 , Ta 2 O 5 , HfO 2 , Pr 2 O 3 , Sb 2 O 5 , Y 2 O 3 , WO 3 , In 2 O 3 , SnO 2 , Cr 2 O 3 and mixtures thereof. However, these materials, which are non conducting, are poorly adapted to direct current magnetron sputtering. It has thus been suggested to use a metal target and a plasma consisting not only of argon, but also of oxygen, so that the metal atoms detached from the target become oxidized. This reactive sputtering technique is difficult to implement, notably in view of the difficulty of accurately maintaining constant the amount of oxygen in the plasma. Correct operating equilibrium is unstable and contamination of the target causes deposition rate to diminish.
In order to improve stability of the system, it is also been proposed to apply an alternating voltage to the cathode, rather than a DC voltage, of a sinewave or square wave type. On the positive half-cycle, the cathode is discharged. This technique is known as pulsed magnetron sputtering (PMS) and is disclosed in patent DE-A-37 00 633.
In order to still further improve operation of such a system, patent DD-A-252 205 or DE-A-38 02 852 discloses the use of two cathodes. An AC voltage is applied to each cathode, one cathode discharging while the other is being charged up under the effect of the voltage applied for vaporizing the target. This technique, called Double Magnetron Sputtering (DMS) or Twin Mag, makes it possible to avoid electric arcs.
In order to avoid excessive contamination of the target by oxygen, during sputtering, and to ensure sufficient oxidation of the layer at substrate level, it has also been proposed in patent DD-A-239 810 to regulate the oxygen throughput in the enclosure, as a function of the intensity of a spectral line of the plasma. The intensity of the spectral line emitted by the excited atoms, removed from the target, is proportional to the state of oxidation of the target. This technique is known as Plasma Emitting Monitoring (PEM).
Another method for controlling oxygen flow consists in adjusting the voltage applied to the cathode with respect to a set value. This technique is described in patent DE-A-4106513 or EP-A-501016.
It has been proposed, for example in U.S. Pat. No. 4,572,842, to introduce the reactive gas only close to the surface to be coated, thereby avoiding contamination of the target to be vaporized. U.S. Pat. No. 4,572,842 discloses the use of a septum separating the process cavity into two zones; this patent discloses an example of anti-reflective deposition on a glass substrate; the high inert gas pressure, used in conjunction with a septum, makes it possible to obtain the best reduction of contamination of the metal target by oxygen. Thus, this patent makes it possible to increase deposition rate while still ensuring operation. Patent DD-A-21 48 65 discloses a method for on-line treatment using high inert gas pressure to avoid contaminating the metal target.
It has also been proposed to proceed sequentially with the deposition of a thin metal layer using sputtering followed by oxidation thereof, this technique of sputtering followed by oxidation makes it possible to deposit a metal film under an inert gas such as argon, while preserving rate of deposition. The practical difficulty in implementing this technique is that of preventing contamination of the metal target by the oxygen used for oxidising the metal layer. An apparatus for implementing such a sequential method is disclosed in U.S. Pat. No. 4,420,385: separation of the deposition and oxidation zones which are adjacent, is achieved by means of baffles. Another apparatus is disclosed in EP-A-0,428,358. This apparatus is marketed by Optical Coating Laboratory Inc. (OCLI) under the trade name Metamode™. The deposition and oxygen zones are elongate zones parallel to the axis of the drum carrying the surfaces to be coated. A further apparatus is disclosed in WO-A-92 13114 in the name of Applied Vision Ltd. This apparatus is marketed by the company under the trade name Plasmacoat ARx10™. Oxidation is achieved using a plasma source.
The invention concerns the new problem of adhesion of thin films deposited on a transparent organic material substrate, optionally having received an anti-abrasive treatment, with use of a magnetron sputtering technique. It applies to techniques in which oxidation is sequential as well as to those using sputtering in a reactive atmosphere.
EP-A-0,428,358 mentions, in example 2, “Glass Eyeglass Lenses” that the sequential deposition and oxidation method makes it possible to obtain anti-reflective films having good abrasion resistance, for surfaces to be treated in inorganic glass. It does not mention results of tests for example 4, corresponding to anti-reflective deposition on an ophthalmic lens in organic material. WO-A-92 13114 does not mention the problem of adhesion.
The invention proposes, in a surprising fashion, to increase the gas pressure during sputtering of the metallic or semi-conducting target in order to improve adhesion of thin films deposited on a transparent organic material substrate, having optionally an anti-abrasive layer. A prejudice exists against increasing inert gas pressure for sputtering.
In one of the reference works of this subject, Deposition Technologies for Films and Coatings , by Rointain F. Bunshah, it is explained, on page 80, that if a film is deposited by sputtering deposition, atoms removed from the target have energies much higher than thermal energies and may be implanted into the surface to an appreciable depth. The physically incorporated atoms may then act as nucleating and bonding sites for further atom deposition. This passage encourages the person skilled in the art to use high energy atoms for favouring implantation and thus adhesion.
On page 229 of the same work, it is stated that the relatively high energies of the sputtered atoms in magnetron sputtering sources operating at low pressure and in ion beam systems may act to some degree act to promote adhesion by mechanisms similar to those in plasma bombardment. Here again, this general teaching in the relevant art, which would urge skilled worker to chose atoms of high energy.
These teachings incite the skilled worker to chose, for magnetron sputtering, low pressures; indeed, it is known that the energy of vaporized atoms decreases when inert gas pressure increases. In the context, see for example, the article by W. D. Westwood, Calculation of Deposition Rates in Diode Sputtering Systems, Journal of Vacuum Science Technology, 15(1), 1978.
In the state of the art, it is suggested to carry out sputtering at gas pressures of the order of 25 to 80 mTorr, equivalent to 3.3 to 10.64 Pa. In this context, see the work by Bunshah, page 230, for the case of plane diodes and DC current. For such diodes, as there is no plasma confinement by means of the magnetic field, a high inert gas pressure is employed, of the order of 2 to 10 Pa, in order to preserve an intense plasma. This teaching does not apply to magnetron sputtering, for which current pressures are of the order of 0.1 to 0.5 Pa.
In EP-A-0,428,358 in the name of OCLI, it is suggested to operate under an argon pressure of 2.0 micron, equivalent to 2.66.10 −1 Pa, for deposition of SiO 2 and TiO 2 on a glass substrate (example 1, table 1). For a substrate in inorganic glass, and films of SiO 2 and Ta2O 5 , it is suggested to operate under an argon pressure of 2.5 micron equivalent to 3.33.10 −1 Pa (example 2, table 2). For a substrate in organic glass and the same films the proposed argon pressure is also 2.5 micron equivalent to 3.33.10 −1 Pa (example 2, table 3). The Applied Vision Ltd. apparatus marketed under the trade name Plasmacoat AR10™ suggest working under an argon pressure of 5.10 −3 mbar, equivalent to 5.10 −1 Pa for depositing Si, with an argon throughput of 12 sccm. For Zr deposition, it is proposed to operate at a pressure of 8.10 −3 mbar, equivalent to 8.10 −1 Pa, with an Ar throughput of 17 sccm.
U.S. Pat. No. 5,170,291 to Leybold discloses a sputtering performed with a magnetron in a reactive gas atmosphere composed of a mixture of Ar and O 2 . The target materials were Ti, Al, and Si. The pressure during the sputtering was as follows:
sputtering from the Ti-target: 5 10 −3 mbar
sputtering from the Al-target: 8 10 −3 mbar
sputtering from the Si-target: 1,2 10 −2 mbar
Thus, the optical layer that is deposited at high pressure is in this case the low refractive index layer.
SUMMARY OF THE INVENTION
The invention proposes, contrary to this practice and teaching, to operate at much higher pressures. It turned out, completely surprisingly, that one can thus improve adhesion of thin films on an organic substrate having optionally an anti-abrasive layer. Also, according to one embodiment, the distance between the substrate and the magnetron is at least 90 mm, preferably between 90 mm and 200 mm, especially between 90 mm and 150 mm. This greater distance between magnetron and substrate allows a lower substrate temperature, which can be highly advantageous, for example when coating temperature-sensitive substrates. Moreover, the layer uniformity, especially on curved substrates, can be further enhanced. If the method of the invention is applied for an inorganic substrate, the excellent results obtained by thermal evaporation are maintained.
More precisely, the invention provides an organic substrate having an optically-active stack on at least one side thereof, characterized in that said optically-active stack comprises at least one optical layer having a high refractive index and at least one optical layer having a low refractive index, at least one of said layers being deposited by magnetron sputtering at high pressure, for example between 0.8 to 5.0 Pa, especially above 1.0 Pa.
Notably, the invention is directed towards an organic substrate having an optically-active stack on at least one side thereof, characterized in that said optically-active stack comprises at least one optical layer having a high refractive index and at least one optical layer having a low refractive index, said at least one high refractive index layer being deposited by magnetron sputtering at high pressure.
Very surprisingly, the adhesion is greatly improved when (only) the high refractive index layer(s) is(are) deposited at high pressure.
Notably, the invention is directed towards an organic substrate having an optically-active stack on at least one side thereof, characterized in that said optically-active stack comprises at least one optical layer having a high refractive index and at least one optical layer having a low refractive index, said at least one high refractive index layer and said at least one low refractive index layer being deposited by magnetron sputtering at high pressure.
Notably, the invention is directed towards an organic substrate having an optically-active stack on at least one side thereof, characterized in that said optically-active stack comprises at least one optical layer having a high refractive index and at least one optical layer having a low refractive index, at least one of said layers being deposited by magnetron sputtering at high pressure between 0.8 to 5.0 Pa, especially above 1.0 Pa, preferably between 1.5 to 3.5 Pa, said sputtering being carried out with the substrate being located at least at 90 mm from the magnetron, preferably between 90 mm and 200 mm, especially between 90 mm and 150 mm,
Specific embodiments correspond to claims 3, 4 and 6 to 18. Specific high sputtering pressure is 1.5 to 3.5 Pa.
The invention applies to substrates having an anti-reflective effect as well as a mirror effect. One or the other effect is obtained by varying the thicknesses of the layers.
The high refractive index is conventionally comprised between 2.0 and 2.6, for example between 2.1 and 2.3, whereas the low refractive index is conventionally comprised between 1.35 and 1.52, for example between 1.35 and 1.46; optionally, the ratio between these two refractive indexes is comprised between 1.5 and 2, for example between 1.5 and 1.7.
The invention also provides a method for producing an organic substrate having an optically-active stack on at least one side thereof, characterized in that said optically-active stack comprises at least one optical layer having a high refractive index and at least one optical layer having a low refractive index, said method comprising the step of depositing at least one of said optical layers by magnetron sputtering at a pressure from 0.8 Pa to 5.0 Pa, for example above 1.0 Pa, preferably 1.5 to 3.5 Pa. The distance between magnetron and the substrate is at least 90 mm, preferably comprised between 90 and 200 mm, especially between 90 mm and 150 mm, this distance being defined as the distance measured between the target and the substrate surface to be coated. Specific embodiments correspond to claims 20 to 35.
In the reactive sputtering in an argon-oxygen mixture embodiment at a pulse rate of from 10 to 100 kHz, the PMS technique as described above may be used. In the pulsed voltage alternating between two neighboring magnetrons embodiment, the DMS technique as described above may be used.
When adjusting the oxygen content of said optical layers by measuring the optical characteristics of the plasma emission, and controlling the oxygen supply as a function of a corresponding signal, the PEM technique as described above may be used. When adjusting the oxygen content of said optical layers by measuring the voltage of the reactive magnetron discharge, and controlling the oxygen supply as a function of a corresponding signal, the method employing comparison with a set value may be used.
The method according to the invention is suitable for the preparation of a substrate according to the invention.
The invention also relates to the use of this method for improving adhesion on thin films deposited on an organic material substrate.
The invention relates finally to the substrate obtained by the method according to the invention especially to an ophtalmic lense.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Further characteristics and advantages of the invention will become more clear from the description which follows of some embodiments of the invention provided solely by way of example.
EXAMPLE 1
Sequential Sputtering and Oxidation
The examples given below were carried out using a Plasmacoat AR10 machine by Applied Vision Ltd., using sequential sputtering and oxidation, of the type described in WO-A-92 13114. Reference should be made to this document for more details regarding the structure of the machine.
In this machine, for thin SiO 2 and ZrO 2 films, the following argon pressures are envisaged for sputtering of metal films:
argon pressure for depositing Si: 4.5.10 −3 mbar, equivalent to 0.45 Pa,
argon pressure for deposition Zr: 6.5.10 −3 mbar, equivalent to 0.65 Pa.
These values correspond to an argon throughput of:
12 sc cm for Si deposition
17 sc cm for Zr deposition.
According to the invention, thin films have been deposited, using the following argon pressures:
argon pressure for depositing Si: 0.9.10 −2 mbar, equivalent to 0.9 Pa,
argon pressure for depositing Zr: 1.1.10 −2 mbar, equivalent to 1.1 Pa.
These values correspond to argon throughputs of:
20 sc cm for Si deposition
25 sc cm for Zr deposition.
The oxygen pressure for oxidation of the thin film deposited was not modified.
This corresponds to an increase in gas pressure of 140% and 100% in the respective cases of Si and Zr. More generally, an increase of for example 50% to 200% makes it possible to achieve satisfactory results.
The distance between the magnetron and the substrate was 120 mm.
By way of a test, anti-reflective coating was carried out on an organic substrate marketed by the applicant under the Orma trademark, on which a varnish was applied. The varnish was of the type disclosed in FR-A-2,702,486 in the name of the applicant. Such a varnish comprises a matrix obtained by polymerization of an optionally hydrolized silane; generally, an epoxysilane is used such as glycidoxypropyltrimethoxysilane, optionally in combination with one or several alkyltrialkoxysilane(s) or tetralkoxysilane. Fillers are added to this matrix, these being for example metal oxides or colloidal silica as well as a catalyst.
A varnish based on acrylates or methacrylates can also be used.
Pre-cleaning of the ophthalmic lens was carried out using an argon plasma. Following this, the following films were successively deposited under the operating conditions set out for the AR10 machine (below: standard ophthalmic lenses) and then under the operating conditions described above (below: ophthalmic lenses according to the invention):
first film : ZrO 2
16 nm
second film : SiO 2
20 nm
third film : ZrO 2 :
108 nm
fourth film : SiO 2 :
84 nm
Tests carried out in the conditions under which they will be worn, practised on standard ophthalmic lenses and on ophthalmic lenses according to the invention showed that wear was more pronounced in the case of standard ophthalmic lenses. Additionally, qualitative tests were carried out on standard ophthalmic lenses and on ophthalmic lenses according to the invention, using the procedure known as the “n10 blow test”. This procedure makes it possible to evaluate adhesion of a film deposited on a substrate, such as an ophthalmic lens.
The substrate to be tested was cleaned with alcohol and placed in a holder. A SELVYT™ cloth supplied by Bergeon & Cie, CH 2400 Le Locle, was placed on the glass. A graduated eraser was brought into contact with the rag. The graduated eraser was subject to a constant force. The eraser and the substrate to be tested were then moved one with respect to the other, using an alternating movement. A cycle means 10 successive to-and-fro movements.
The operator checked the state of the substrate every 3 cycles, by visually inspecting the substrate. He noted the cycle number through which a defect appeared for the first time.
The table that follows gives the results of the “n10 blow test” on the convex face of the standard ophthalmic lens and of the ophthalmic lens according to the invention. In all, nine runs were used, each comprising 10 standard ophthalmic lenses and 10 ophthalmic lenses according to the invention. For each run, two standard ophthalmic lenses and those according to the invention were tested after 24 hours; two standard ophthalmic lenses and ophthalmic lenses were tested after one month. For the test, a PVC eraser plastified with dioctyl phtalate in the following proportions was employed:
PVC: 47.3% by weight
DOP: 47.3% by weight
alumina: 2.8% by weight
Syloid 378: 1.9% by weight
Plastolein: 0.5% by weight
Uvitex OBP: 0.2% by weight.
The eraser had dimensions of 30×25×16 mm, a Shore A hardness of 65, and was obtained by extrusion, such a eraser can be obtained from Maped Mallat, BP 14, 74371 Pringy, France. The face of the 16×25 eraser was in contact with the lens.
Standard
Invention
Standard
Invention
Run
24 h
24 h
1 month
1 month
1
3
12
3
12
2
3
12
3
12
3
3
6
3
6
4
3
20
3
15
5
3
9
3
12
6
3
9
3
nd
7
3
6
3
20
8
3
9
3
30
9
3
12
3
6
Mean
3.00
10.56
3.00
14.13
Standard
0.00
4.25
0.00
7.86
deviation
(nd: not determined)
The result in the table show that the defect appears in the standard glass starting from cycle three. However, on the glass according to the invention, the defects always appear for a number of cycles greater or equal to 6. This table confirms the surprising results of the invention.
Similar results are obtained with a SiO 2 —TiO 2 stack.
Results of the same order could have been obtained on using abrasion or adhesion tests according to the MIL-C-675 standard.
The invention provides better adhesion, in the case of magnetron sputtering and successive oxidation.
The invention also makes it possible to obtain greater adhesion when using magnetron sputtering in a reactive atmosphere. In this type of treatment, according to the invention, the sputtering is done under pressures of 0.8 to 5 Pa, preferably 1.5 to 3.5 Pa.
EXAMPLE 2
Reactive Magnetron Sputtering
The coatings were deposited in an inline sputtering machine equipped with double magnetrons which work at frequencies of 100 KHz as described in patents DD 252 205 and DE 3 802 852.
For example, we obtained excellent results for a TiO 2 —SiO 2 —4—layers stack:
TiO 2 : 11.4 nm
SiO 2 : 30,2 nm
TiO 2 : 101,5 in
SiO 2 : 80,3 nm
The pressure during SiO 2 deposition was 2 Pa and 3.2 Pa for TiO 2 . The magnetron-to-substrat distance was 90 mm.
With these parameters, the following n 10 blow test results have been achieved:
Three lenses were coated per run.
Standard
Invention
Run
Standard 24 h
Invention 24 h
1 month
1 month
1
3
50/15/12
3
25/9/25
2
3
50/20/15
3
15/25/25
3
3
25/9/25
3
12/25/12
4
3
25/20/20
3
25/25/15
Mean
3
23.83
3
19.83
Standard
0.00
13.26
0.00
6.56
Deviation
Similar results have been obtained at a SiO 2 pressure of 2 Pa and a lower TiO 2 pressure of 2 Pa, but with higher magnetron-to-substrat distance of 150 mm. Higher magnetron-to-substrat distance leads to better thickness uniformity on curved substrat.
In either case, it is advantageous to clean the substrate prior to sputtering. For cleaning of the substrate, a cold plasma, generated by direct current, microwave or radiofrequency can be used. A typical gas pressure of 10 −2 to 100 Pa ensures correct cleaning of the substrate. The plasma used in cleaning can be an argon, oxygen plasma or yet again a plasma obtained from a mixture of these two gasses.
A mirror-like stack is obtained in a similar way, with the same materials as above, with the same indexes, by varying the thickness of each layer.
EXAMPLE 3
Reactive Magnetron Sputtering
In the same machine used for example 2, runs with. Nb 2 O 5 instead of TiO 2 as high index material were carried out.
For example, we obtained excellent results for a Nb 2 O 5 —SiO 2 —4—layers stack:
Nb 2 O 5 : 11.6 nm
SiO 2 : 31.5 nm
Nb 2 O 5 : 118 nm
SiO 2 : 80,3 nm
The pressure during SiO 2 deposition was 2.3 Pa. The magnetron-to-substrate distance was 90 mm.
The pressure during Nb 2 O 5 deposition was 3.0 Pa and 1.0 Pa respectively. The magnetron-to-substrate distance was 170 mm.
With these parameters the following n 10 blow test results have been achieved (with 3 lenses per run):
1.0 Pa tested
3.0 Pa tested
1.0 Pa tested
3.0 Pa tested
Run
after 24 h
after 24 h
after 1 month
after 1 month
1
12/3/3
>25/>25/>25
6/12/6
>25/>25/>25
2
25/9/25
>25/>25/>25
25/25/12
>25/>25/>25
Mean
12.8
>25
14.8
>25
Standard
10
0
10
0
Deviation
While results for the stacks deposited at deposition pressures of 1.0 Pa are good, a much higher pressure improved adhesion drastically
Obviously, other embodiments are possible. Equivalent results can be obtained on other machines, like the OCLI machine, for other coatings, or for other types of substrate, as well as for any combination of the conditions described above, for example the pressure and the distance between magnetron and substrate.
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An organic substrate having optically-active layers deposited by magnetron sputtering and a preparation process for it are provided. Gas pressure used for carrying out better adhesion by sputtering is high, comprised between 0.8 and 5.0 Pa. Sputtering is particularly suitable for targets of Si, Ti, Zr and organic substrates with or without anti-abrasive coating. Improved adhesion of thin films is obtained.
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TECHNICAL FIELD
[0001] The present invention relates to a structure for retaining a drive ring rotatable with respect to a nozzle mount in a variable displacement exhaust turbocharger, which is used for an exhaust turbocharger of an internal combustion engine and which is equipped with a variable nozzle mechanism for varying a vane angle of a plurality of nozzle vanes.
BACKGROUND ART
[0002] As one variable displacement exhaust turbocharger which is used for an exhaust turbocharger of an internal combustion engine and which is equipped with a variable nozzle mechanism for varying a vane angle of a plurality of nozzle vanes, the technique of JP 2010-19252 (Patent Document 1) is provided.
[0003] This technique of the related art is illustrated in the attached drawings. FIG. 6A is an illustration of a turbine housing 010 . FIG. 6B is a partial enlarged view of section P of FIG. 6A . FIG. 6C is an exploded view of components of FIG. 6B .
[0004] A variable nozzle mechanism 0100 is configured such that a plurality of guide vanes (nozzle vanes) 080 is positioned between a lower vane ring 020 and an upper vane ring 030 . The guide vane 080 is rotatably supported about an axis to control a flow rate of exhaust gas flowing in a turbine. The distance between the lower vane ring 020 and the upper vane ring 030 is maintained by a stepped spacer 050 which is positioned therebetween. The upper vane ring 030 and the lower vane ring 020 are attached to the turbine housing 010 by nuts 040 and metal fastening members 042 .
[0005] Further, the stepped spacer 050 has a through-hole formed in the center so that the fastening member 042 can pass through the stepped spacer 050 .
[0006] Meanwhile, another technique is disclosed in JP 4545068B (Patent Document 2). A variable displacement exhaust turbocharger of JP 4545068B is configured, as illustrated in FIG. 7 , such that a drive ring 064 is arranged on a peripheral circumferential surface of a guide part 057 of a nozzle mount 055 to be disposed between a side face of a lever plate (not shown, disposed on a left side of the drive ring 064 ) and a side face of the nozzle mount 055 so that they are next to each other in the axial direction and a stud with a flange (a nail pin) 066 is fixed to a side part of the nozzle mount 055 to be in contact with an outer surface 064 a of the drive ring 064 so as to prevent the drive ring 064 from moving in the axial direction, i.e. coming off toward the lever plate side.
[0007] In FIG. 7 , a nozzle vane 068 is provided between the nozzle mount 055 and an annular support plate 070 .
CITATION DOCUMENT
Patent Document
[0000]
[Patent Document 1]
JP 2010-095252 A
[Patent Document 2]
JP 4545068 B (FIG. 3)
SUMMARY
Technical Problem
[0012] However, the stepped spacer 050 described in Patent Literature 1 has the central through-hole for the fastening member 042 to pass through. Further, this stepped space 050 is provided to maintain the distance between the lower vane ring 020 and the upper vane ring 030 where the plurality of guide vanes (nozzle vanes) 080 is arranged.
[0013] Patent Document 1 teaches to use the stepped spacer 050 for positioning. However, there is no disclosure as to the use of the stepped spacer 050 for positioning of the drive ring in a thrust direction by fitting the drive ring for varying a vane angle of the nozzle vane to the guide part of the nozzle mount.
[0014] In the fixing mechanism of Patent Document 2 using the nail pin 066 capable of abutting to the outer surface 064 a of the drive ring 064 , the guide part 057 of the nozzle mount 055 is required to have a space to accommodate a mounting width of the drive ring 064 . Correspondingly, the nozzle mount 055 is required to have a significant width in the axial direction of the nozzle mount 055 . It results in increase of the nozzle mount 055 in size and weight, and this also makes it difficult to manufacture the nozzle mount 055 by press-molding. Moreover, as the width dimension of the guide part 057 of the nozzle mount 055 needs to be machined with high precision in relation to the width dimension of the drive ring 064 , and this causes an increase in the number of the processing steps.
[0015] In view of the above issues, it is an object of the present invention to reduce the weight and production cost of a nozzle mount by pres-fitting a pin with a flange portion into a press-fitting hole formed in an end face of a guide part along a thrust direction so as to retain the drive ring to the guide part of the nozzle mount in the thrust direction and providing an adjusting member (a spacer member) between the flange portion and the end face for adjustment in the thrust direction.
Solution to Problem
[0016] To solve the above issues, the present invention provides a variable displacement exhaust turbocharger which is equipped with a variable nozzle mechanism and is driven by exhaust gas from an engine, and the variable displacement exhaust turbocharger comprises:
[0017] a plurality of nozzle vanes supported rotatably by a nozzle mount which is fixed to a case including a turbine casing of the variable displacement exhaust turbocharger;
[0018] a drive ring which is interlocked with an actuator and is fitted to an annular guide part protruding from a center part of the nozzle mount in an axial direction, the guide part having a width in a thrust direction which is smaller than a width of the drive ring;
[0019] a plurality of lever plates each of which is fitted to a groove formed in the drive ring at one end via a connection pin and is connected to the nozzle vane at the other end;
[0020] a press-fitting pin which has a flange portion facing a side face of the drive ring, the press-fitting pin being press-fitted into a press-fitting hole formed in an end face of the guide part along a thrust direction of the guide part so as to retain the drive ring in the thrust direction; and
[0021] an adjusting member arranged between the flange portion of the press-fitting pin and the end face of the guide part,
[0022] wherein the adjusting member is configured to adjust a distance between the flange portion of the press-fitting pin and a side face of the nozzle mount, the drive ring being sandwiched between the flange portion and the side face of the nozzle mount.
[0023] According to the present invention, by reducing the thrust-directional thickness of the guide part of the nozzle mount and providing the adjusting member for adjustment in the thrust direction between the guide part and the flange portion for restricting rocking of the drive ring in the thrust direction, it is possible to form an appropriate amount of clearance in the thrust direction of the drive ring.
[0024] Therefore, as the guide part can be shortened in the thrust direction by the amount equivalent to the thickness of the adjusting member (in the thrust direction of the guide part), it is possible to achieve weight reduction and cost reduction of materials.
[0025] Further, by reducing the thrust-directional thickness of the guide part of the nozzle mount, it is possible to reduce the thrust-directional thickness of the nozzle mount including the guide part in the thrust direction. This enables production by press working, thereby reducing the production cost.
[0026] It is preferable in the present invention that the adjusting member comprises the press-fitting pin formed integrally with the flange portion.
[0027] By forming the adjusting member integrally with the press-fitting pin, it is possible to simplify the mounting work and production of the adjusting member.
[0028] It is also preferable in the present invention that the adjusting member has an annular shape and is formed by a separate member from the press-fitting pin.
[0029] With this configuration, the adjusting member can be formed separately, and thus it is possible to precisely process the adjusting member to a desired thickness.
Advantageous Effects
[0030] With the configuration that the thrust-directional width of the guide part is made smaller than the width of the drive ring, the adjusting member is sandwiched between the flange portion of the press-fitting pin and the end face of the guide part, the distance between the side face of the nozzle mount supporting the drive ring and the flange portion of the press-fitting pin is adjusted by the adjusting member, an amount of clearance at the guide part in the thrust direction of the drive ring is adjustable using the adjusting member. Thus, compared to the case where the thrust-directional length of the guide part is precisely processed by end mill machining or the like, the production cost can be reduced.
[0031] Moreover, as the thrust-directional length of the nozzle mount can be reduced by the amount of the thickness of the adjusting member (in the thrust direction of the guide part), it is possible to achieve the weight reduction and cost reduction of the materials. Further, by reducing the thrust-directional thickness of the guide part of the nozzle mount, it is possible to reduce the thrust-directional thickness of the nozzle mount including the guide part. This enables production by press working, thereby reducing the production cost.
BRIEF DESCRIPTION OF DRAWINGS
[0032] FIG. 1 is a longitudinal cross-sectional view of a main part of a variable displacement exhaust turbocharger equipped with a variable nozzle mechanism according to an embodiment of the present invention.
[0033] FIG. 2A is a front view of a variable nozzle mechanism according to a first embodiment of the present invention, which is taken from a lever plate side.
[0034] FIG. 2B is a cross-sectional view in A-A of FIG. 2A .
[0035] FIG. 3A is an enlarged cross-sectional view of a part where a nail pin is press-fitted in a nozzle mount according to a first embodiment of the present invention, which is taken in B-B of FIG. 2A .
[0036] FIG. 3B is an enlarged view of a press-fitting hole on a nozzle mount side according to the first embodiment of the present invention.
[0037] FIG. 3C is a schematic view of the nail pin according to the first embodiment of the present invention.
[0038] FIG. 4A is an enlarged cross-sectional view of a section where a nail pin according to a second embodiment of the present invention is press-fitted in the nozzle mount.
[0039] FIG. 4B is an enlarged view of a press-fitting hole on the nozzle mount side according to the second embodiment of the present invention.
[0040] FIG. 4C is a schematic view of the nail pin according to the second embodiment of the present invention.
[0041] FIG. 5 illustrates a schematic configuration of the nail pin according to a third embodiment.
[0042] FIG. 6A illustrates a turbine housing 010 of the related art.
[0043] FIG. 6B is a partial enlarged view of section P of FIG. 6A .
[0044] FIG. 6C is an exploded view of components of FIG. 6B .
[0045] FIG. 7 is an illustration of the related art.
DETAILED DESCRIPTION
[0046] Embodiments of the present invention will now be described in detail with reference to the accompanying drawings.
[0047] It is intended, however, that unless particularly specified, dimensions, materials, shapes, relative positions and the like of components described in the embodiments shall be interpreted as illustrative only and not limitative of the scope of the present invention.
First Embodiment
[0048] FIG. 1 is a longitudinal cross-sectional view of a main part of a variable displacement exhaust turbocharger equipped with a variable nozzle mechanism according to an embodiment of the present invention.
[0049] FIG. 1 illustrates a turbine casing 30 , a scroll 38 of a scroll shape formed in an outer peripheral part of the turbine casing 30 , a turbine rotor of a radial flow type 34 , a compressor 35 , a turbine shaft 32 for connecting the turbine rotor 34 and the compressor 35 , a compressor housing 31 and a bearing housing 36 .
[0050] The turbine shaft 32 connecting the turbine rotor 34 and the compressor 35 is rotatably supported by the bearing housing 36 via two bearings 37 , 37 . The drawing also illustrates an exhaust gas outlet 8 and a rotation axis CL of the exhaust turbocharger.
[0051] A plurality of nozzle vanes 2 is arranged on an inner circumferential side of the scroll 38 at equal intervals in the circumferential direction of a turbine and is supported rotatably by a nozzle mount 5 . A nozzle shaft 2 a is formed on a vane end of the nozzle vane 2 and is rotatably supported by the nozzle mount 5 which is fixed to the turbine casing 30 .
[0052] On an opposite side of the nozzle shaft 2 a from the vane end, a lever plate 1 for varying a vane angle of the nozzle vane 2 by rotation of the nozzle shaft 2 a is connected to the drive ring 3 via a connecting pin 10 .
[0053] An actuator rod 33 is configured to transmit a reciprocating motion from an actuator (not shown). A drive mechanism 39 is configured to convert the reciprocating motion of the actuator rod 33 (a reciprocating motion in a direction substantially perpendicular to the drawing) into a rotational motion by a rotation shaft 15 a, and rotate the drive ring 3 by a drive pin 15 c disposed at an end of a lever 15 b fixed to the rotation shaft 15 a.
[0054] A section 100 surrounded by a dotted line is a part of a variable nozzle mechanism for varying a vane angle of the nozzle vane 2 .
[0055] In the operation of the variable displacement exhaust turbocharger equipped with the variable nozzle mechanism which is configured as illustrated in FIG. 1 , exhaust gas from an internal combustion engine (not shown) enters the scroll 38 and flows into the nozzle vanes 2 while swirling along the scroll shape of the scroll 38 . After flowing past between the nozzle vanes, the exhaust gas flows in the turbine rotor 34 from its outer peripheral side. Then, the exhaust gas flows radially toward the center to perform expansion work in the turbine rotor 34 . After performing the expansion work, the exhaust gas flows out in the axial direction and then guided toward the exhaust gas outlet 8 and sent outside of the turbine rotor 34 .
[0056] In order to control the displacement of this variable displacement turbine, a vane angle of the nozzle vanes 2 at which a flow rate of the exhaust gas through the nozzle vanes 2 a reaches a desired flow rate is set by a vane angle controller (not shown) with respect to the actuator. The reciprocal displacement of the actuator with respect to this vane angle is transmitted to the drive ring 3 via the drive mechanism 39 so as to drive and rotate the drive ring 3 .
[0057] By rotation of the drive ring 3 , the lever plate 1 is caused to rotate around the nozzle shaft 2 a via a connection pin 19 which is described later. By rotation of the nozzle shaft 2 a, the nozzle vane 2 is rotated to the vane angle which is set as to the actuator.
[0058] FIG. 2A is a front view of the variable nozzle mechanism, which is taken from the lever plate 1 side. FIG. 2B is a cross-sectional view in A-A of FIG. 2A . The drawings illustrate a variable nozzle mechanism 100 for varying the vane angle of the nozzle vanes 2 . The variable nozzle mechanism 100 is configured as described below.
[0059] The drive ring 3 formed in a disk shape is externally fitted to a guide part 5 a (see FIG. 2B ) of a cylinder shape which protrudes in the direction of the axis CL of the nozzle mount 5 (in the same direction as the rotation axis of the exhaust turbocharger) to be rotatably supported. Further, grooves 3 y, with which the connection pins 10 engage, are formed in the guide part 5 a at equal intervals in the circumferential direction. The grooves 3 y are described later. The drive mechanism 39 has a drive groove 3 z where the actuator rod 33 engages.
[0060] The same number of the lever plates 1 as the grooves 3 y of the drive ring 3 is provided at equal intervals in the circumferential direction. On the outer peripheral side of each of the lever plates 1 , the connection pin 10 is formed. On the inner peripheral side of each of the lever plates 1 , the nozzle shaft 2 a of the nozzle vane 2 is fixed.
[0061] A nozzle plate 6 of an annular shape is connected to the nozzle mount 5 by a plurality of nozzle supports 61 .
[0062] In the variable nozzle mechanism, as illustrated in FIG. 2B , the lever plate 1 is arranged on an inner side in the axial direction (on the compressor housing 31 side in FIG. 1 ), and between a side face of the lever plate 1 and a side face of the nozzle mount 5 , the drive ring 3 is arranged in the state where the drive ring 3 , the lever plate 1 and the nozzle mount 5 are arranged next to one another in the axial direction.
[0063] The connection pin 10 is formed integrally with a base material by pressurizing one side face of each of the lever plates 1 by a press machine so that a rectangular depression 10 a is formed on the side face and a rectangular protrusion is formed on the other side face by extrusion.
[0064] The drive ring 3 of the variable nozzle mechanism 100 which is formed in the above manner, needs to be retained with respective appropriate clearances between the nozzle mount 5 and the flange portion 20 a of the nail pin 20 , and between the inner peripheral surface of the drive ring 3 and the outer peripheral surface of the guide part 5 a.
[0065] If the clearance is greater than a specified value, the drive ring 3 rocks in the axial direction of the nozzle mount 5 . This can result in one-side hitting of a thrust-direction end of a sliding face of the drive ring 3 against the guide part (one-side contact), which causes fixation.
[0066] On the other hand, if the clearance is smaller than the specified value, the sliding resistance of the nozzle mount 5 increases, which causes fixation of the sliding portion.
[0067] To prevent the fixation, it is desired to ensure an appropriate amount of a thrust-directional clearance L 8 (see FIG. 3B ) in the thrust direction of the nozzle mount 5 and the drive ring 3 . To maintain the appropriate amount of clearance L 8 , a nail pin 20 which is a pin with a flange portion 20 a is press-fitted in the press-fitting hole 5 b formed at an outer peripheral edge part of the end face of the guide part 5 a in the thrust direction, so as to secure an appropriate clearance by means of the flange.
[0068] FIG. 3A is an enlarged cross-sectional view of a part where a nail pin serving as the press-fitting pin is press-fitted in the nozzle mount 5 according to a first embodiment of the present invention, which is taken in B-B of FIG. 2A . FIG. 3B is an enlarged view of a press-fitting hole on the nozzle mount. FIG. 3C is a schematic view of the nail pin to be press-inserted in the press-fitting hole of FIG. 3B .
[0069] At the end face of the guide part 5 a, a nail pin 20 with a flange portion 20 a is press-fitted in a press-fitting hole 5 b. The nail pin 20 has the flange portion 20 a to prevent rocking of the drive ring 3 in the direction of the axis CL of the nozzle mount 5 during rotation of the drive ring 3 .
[0070] In FIG. 3A , the disc-shaped drive ring 3 is externally fitted to the cylindrical guide part 5 a protruding in the direction of the axis CL of the nozzle mount 5 such that there is a small clearance L 7 therebetween in the radial direction.
[0071] The length L 1 of the guide part 5 a (a protrusion amount) is set smaller than a thickness T 2 of the drive ring 3 which is externally fitted to the nozzle mount 5 such that the drive ring 3 contacts a section of the nozzle mount 5 disposed between a contact portion 5 c where the drive ring 3 contacts and the end face of the guide part 5 a.
[0072] A thickness T 1 of the nozzle mount 5 (in the thrust direction) is set to the maximum length that can be machined by press so as to reduce the process cost and weight of the nozzle mount 5 .
[0073] As for the thickness T 1 of the nozzle mount 5 , the press-machining precision is improved, whereby maintaining a fixed strength and a perpendicularity of a stopper pin (not shown) for restricting a swing amount of the lever plate 1 which swings to define a fully-closed position of the vane angle of the nozzle vane 2 and the nail pin which is press-fitted in the nozzle mount 5 .
[0074] FIG. 3B is a detailed view of the press-fitting hole 5 b. FIG. 3C is an illustration of the nail pin 20 to be press-fitted in the press-fitting hole 5 b.
[0075] The press-fitting hole 5 b is formed in the outer peripheral edge part of the end face of the guide part 5 a along the axis CL of the nozzle mount 5 , and a plurality of the press-fitting holes 5 b is arranged at equal intervals in the circumferential direction.
[0076] The press-fitting hole 5 b changes in hole diameter at two stages along an axis of the hole. Specifically, the hole diameter of the press-fitting hole 5 b is ø 1 on an opening side (L 4 area) where the nail pin 20 is inserted and changes to ø 2 on its deeper side (L 3 -L 4 area) to satisfy the relationship of ø 1 >ø 2 .
[0077] The area of the length L 4 of the section with the hole diameter ø 1 extends from a deeper side of the contact portion 5 c (a position on left side of the contact portion 5 c on the drawing) to the end face of the guide part 5 a.
[0078] The nail pin 20 includes a pin portion 20 b to be press-fitted in the press-fitting hole 5 b, the flange portion 20 a, a stepped portion 20 c which is an adjusting member for forming the appropriate clearance L 8 between the drive ring 3 and the flange portion 20 a, and a protruding portion 20 d which protrudes from the flange portion 20 a which is opposite from the flange portion 20 a.
[0079] The nail pin 20 is integrally formed with the stepped portion 20 c.
[0080] By a thrust-directional thickness L 5 of the nail pin 20 , the appropriate amount of the clearance L 8 is formed.
[0081] The hole diameter ø 2 is smaller than a diameter ø 3 of a tip part of the nail pin 20 , and the hole diameter ø 2 and the diameter ø 3 are formed according to a dimensional relationship of press-fitting. The length L 9 of the tip part of the pin 20 (a press-fit margin) which is inserted in the hole diameter ø 2 is long enough to possess a fixing strength to prevent the nail pin 20 from coming out from the press-fitting hole 5 b easily during the operation of the drive ring 3 .
[0082] Further, the outer peripheral surface of the outer diameter ø 4 of the stepped portion is set so as not to project beyond the outer peripheral surface of the guide part 5 a in the radial direction when the nail pin 20 is press-fitted in the press-fitting hole 5 b.
[0083] The protruding portion 20 d is a portion where a press-fitting tool is abutted when press-fitting the nail pin 20 into the press-fitting hole 5 b. Without the protruding portion 20 d, the pin portion 20 b deforms during insertion of the nail pin 20 due to the press-fitting pressure acting on the pin portion 20 b. The deformation of the pin portion 20 b accompanies deformation of the flange portion 20 a. Therefore, the protruding portion 20 d is provided to prevent deformation of the nail pin 20 and facilitate assembling thereof.
[0084] Further, the height L 1 of the guide part 5 a and the thickness L 5 of the stepped portion 20 c are set so that an appropriate clearance L 8 is secured between the flange portion 20 a of the nail pin 20 and the drive ring 3 when the nail pin 20 is press-fitted into the press-fitting hole 5 b.
[0085] Furthermore, in a section where the sliding face width (T 2 ) of the drive ring 3 is located, a space 5 e is formed in L 1 section of the press-fitting hole 5 b.
[0086] Thus, although a section of the press-fitting hole 5 b of the nozzle mount 5 on the drive ring 3 side is thin and has low rigidity, it is possible to prevent outward bulging of the section caused by the press-fitting of the nail pin 20 .
[0087] This is, however, not restrictive and it is not a problem in this embodiment even if the space 5 e is not provided.
[0088] A relief R is provided in a continuous portion between the contact portion 5 c and the guide part 5 a of the nozzle mount 5 so that the edge of the sliding face width (T 2 ) of the drive ring 3 reliably contacts the guide part 5 a.
[0089] By ensuring that the slide face of the drive ring 3 contacts across the guide part 5 a, it is possible to reduce rocking of the drive ring 3 in the thrust direction during rotation of the drive ring 3 , thereby preventing the fixation of the edge of the sliding face width of the drive ring and the guide part 5 a.
[0090] On an outer circumferential side of the relief R of the side face, the contact portion 5 c of a disk shape is formed so that the radial-direction side face of the drive ring 3 contacts the disk-shaped contact portion 5 c. The contact portion 5 c is provided to reduce frictional resistance between the side face of the nozzle mount 5 and the radial-direction side face of the drive ring 3 , thereby enhancing smooth rotation of the drive ring 3 .
[0091] With the above configuration, by press-machining the nozzle mount 5 , the length L 1 of the guide part 5 a of the nozzle mount 5 becomes small and the thrust-directional thickness T 1 of the entire nozzle mount 5 is reduced by an amount of the thickness L 5 of the stepped portion 20 c. Thus, it is possible to achieve the weight reduction and cost reduction of materials.
[0092] The configuration of the nozzle mount 5 (the configuration around the guide part) was conventionally complicated and it required many steps to achieve machining precision when machining the guide part 5 a in the thrust direction (end mill machining). However, with the integral configuration in which the stepped portion serving as the adjusting member is integrally provided in the nail pin 20 , high machining precision can be easily achieved by adopting lathe machining, whereby achieving significant reduction in the machining cost.
[0093] Further, as the space 5 e is formed in L 4 section of the nail pin 20 and the press-fitting hole 5 b, press-fitting of the nail pin 20 does not generate a bulging portion on the surface of the guide part 5 a in the section where the sliding face T 2 of the drive ring 3 is located. Therefore, it is possible to maintain the surface of the guide part 5 a smooth and avoid the fixation of the drive ring 3 and the guide part 5 a.
[0094] In the case where the space 5 e is not provided, the fitting dimension of the pin portion 20 b and the press-fitting hole 5 b in the L 4 section may be adjusted to avoid generation of the bulging portion.
[0095] Moreover, as the diameter of the press-fitting hole 5 b in the L 4 section is large, press-fitting work is facilitated.
Second Embodiment
[0096] A second embodiment will be described in reference to FIG. 4A , FIG. 4B and FIG. 4C .
[0097] The structure is the same as the first embodiment, except for press-fitting of a nail pin 21 in the nozzle mount 51 . Thus, structures such as the variable nozzle mechanism will not be described further herein.
[0098] In addition, for parts of the same shape with the same effect, are assigned the same reference numerals, and a description thereof will be omitted.
[0099] FIG. 4A is an enlarged cross-sectional view of a section where a nail pin according to the second embodiment of the present invention is press-fitted in the nozzle mount. FIG. 4B is an enlarged view of a press-fitting hole on the nozzle mount side. FIG. 4C is a schematic view of the nail pin to be inserted in the press-fitting hole of FIG. 4B .
[0100] FIG. 4A shows a nozzle mount 51 and a lever plate 1 . In FIG. 4A , the drive ring 3 is externally fitted to a guide part 51 a of the nozzle mount 51 .
[0101] FIG. 4B illustrates a press-fitting hole 51 b where a nail pin 21 is press-fitted. FIG. 4C illustrates the nail pin 21 to be fitted to the press-fitting hole 51 b.
[0102] The press-fitting hole 51 b has a diameter a and is formed in the outer peripheral edge part of the end face of the guide part 51 a along the axis CL of the nozzle mount 51 , and a plurality of the press-fitting holes 51 b is arranged in the outer peripheral edge part at equal intervals in the circumferential direction.
[0103] The area of the length L 4 of the section with the hole diameter ø 2 extends from the end face of the guide part 51 a to a deeper side of a contact portion 51 c (a position on left side of the contact portion 51 c on the drawing).
[0104] The length L 1 of the guide part 51 a (a protrusion amount) is set smaller than an amount equivalent to the thickness T 2 of the drive ring 3 which is externally fitted to the nozzle mount 5 such that the drive ring 3 contacts a section of the nozzle mount 51 disposed between the contact portion 51 c where the drive ring 3 contacts and the end face of the guide part 5 a.
[0105] The nail pin 21 comprises a pin tip portion 21 b to be press-fitted in the press-fitting hole 51 b, a reduced diameter part 21 c with smaller diameter than the pin tip portion 21 b, a stepped portion 21 f which is a disc-shape adjusting member having an outer diameter portion does not project beyond the outer peripheral surface of the guide part 51 a in the radial direction, a flange portion 21 a for maintaining an appropriate clearance L 8 (see FIG. 4B ) with respect to the side face of the drive ring 3 and restricting rocking of the side face of the drive ring 3 in the thrust direction, and a protruding portion 21 d from the flange portion 21 a to a side which is opposite from the stepped portion 21 f. The nail pin 21 is integrally formed.
[0106] The nail pin 21 to be press-fitted in the press-fitting hole 51 b is configured so that the pin tip part 21 b has diameter ø 3 and the reduced diameter part 21 c between the pin tip part 21 b and the stepped portion 21 f has diameter ø 5 , and diameter ø 3 >diameter ø 5 .
[0107] The thrust-directional length L 5 of the stepped portion 21 f is determined to secure an appropriate clearance L 8 between the side face of the drive ring 3 and the flange portion 21 a.
[0108] A length L 10 of the diameter ø 3 of the tip part 21 b (press-fit margin) has a length that achieves fixing strength so that the nail pin 21 does not come out from the press-fitting hole 51 b easily at the operation of the drive ring 3 when inserting the nail pin 21 into the press-fitting hole 51 b.
[0109] Further, each of the tip part 21 b of the nail pin 21 and the press-fitting hole 51 b is formed in interference-fitting dimension of a respective elastic deformation region so that the section (L 1 ) of the press-fitting hole 51 b opposing the drive ring 3 does not plastically deform when press-fitting the nail pin 21 into the press-fitting hole 51 b.
[0110] Thus, by press-fitting the nail pin 21 into the press-fitting hole 51 b, the stepped portion 21 b is abutted to the end face of the guide part 51 a to form the appropriate clearance L 8 .
[0111] With this configuration, the thrust-directional thickness T 1 of the nozzle mount 51 is reduced by the amount equivalent to the thickness L 5 of the stepped portion 21 f. Thus, it is possible to achieve the weight reduction and cost reduction of materials.
[0112] The configuration of the nozzle mount 51 (the configuration around the guide part) was conventionally complicated and it required many steps to achieve machining precision when machining the guide part 51 a in the thrust direction (end mill machining). However, with the integral configuration in which the stepped portion serving as the adjusting member is integrally provided in the nail pin 21 , high machining precision can be easily achieved by adopting lathe machining, whereby achieving significant reduction in the machining cost.
[0113] Further, as the space 21 e is formed in L 4 section of the nail pin 20 and the press-fitting hole 5 b, press-fitting of the nail pin 21 does not generate a bulging portion on the surface of the guide part 51 a in the section where the sliding face T 2 of the drive ring 3 is located. Therefore, it is possible to maintain the surface of the guide part 51 a smooth and avoid the fixation of the drive ring 3 and the guide part 51 a.
Third Embodiment
[0114] A third embodiment will be described in reference to FIG. 5 .
[0115] The structure is the same as the first embodiment, except for a shape of the nail pin. Thus, structures except for the nail pin will not be described further herein.
[0116] A nail pin 22 comprises a pin portion 22 b to be press-fitted in the press-fitting hole 5 b (see FIG. 3B ), a flange portion 22 a for restricting rocking of the drive ring 3 (see FIG. 3B ) in the thrust direction, and a press-fitting tool receiving part 22 d where a press-fitting strikes when the nail pin 22 protruding from the flange portion 22 a to a side which is opposite from the pin portion 22 b is press-fitted into the press-fitting hole 5 b. The nail pin 21 is integrally formed.
[0117] Moreover, in a section where the pin portion 22 b contacts the flange portion 22 a, a spacer 23 (corresponding to the stepped portion 20 c of the first embodiment) serving as an adjusting member is press-fitted.
[0118] The dimension of the spacer 23 is adjusted so that the outer peripheral surface of the space 23 does project beyond the outer peripheral surface of the guide part 5 a (see FIG. 3B ) when the nail pin 22 is press-fitted in the press-fitting hole 5 b.
[0119] In this embodiment, the spacer 23 is press-fitted to the nail pin 22 . Thus, by eliminating a gap between an inner peripheral surface of the spacer 23 and the pin portion 22 b and setting the outer diameter of the spacer 23 to the maximum diameter which is twice as large as the distance between the axis of the press-fitting hole 5 b and the outer peripheral surface of the guide part 5 a, it is possible to prevent the spacer 23 from projecting beyond the outer peripheral surface of the guide part 5 a to secure the clearance L 7 (see FIG. 3B ) between the inner peripheral surface of the drive ring 3 and the spacer 23 , prevent fixation of these parts and also secure the clearance L 8 in the thrust direction of the drive ring 3 .
[0120] In this embodiment, the configuration in which the spacer 23 is press-fitted to the pin portion 22 b is described. This is, however, not restrictive, and the spacer 23 may be inserted in a manner other than press-fitting to achieve the same effects as long as, with the clearance between the pin portion 22 b and the inner peripheral surface of the spacer 23 , even if the spacer 23 is disposed closer to the guide part 5 a side when the nail pin 22 is press-fitted in the press-fitting hole 5 b, the outer peripheral part of the spacer 23 is either flush with the outer peripheral surface of the guide part 5 a or slightly closer to the center of the spacer 23 without projecting beyond the outer peripheral surface of the guide part 5 a.
INDUSTRIAL APPLICABILITY
[0121] According to the present invention, it is possible to provide a variable displacement exhaust turbocharger equipped with a variable nozzle mechanism for varying a vane angle of a plurality of nozzle vanes, whereby the drive ring of the variable nozzle mechanism is easily retained to the guide part with an appropriate clearance and fixation of the inner peripheral surface of the drive ring and the outer peripheral surface of the guide part is prevented so as to achieve cost reduction and improved durable reliability.
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It is intended to achieve weight reduction and production reduction of a nozzle mount for pivotably supporting a drive ring constituting a variable nozzle mechanism, and is characterized by: providing on an end face of a guide part 5 a a nail pin 20 having a flange portion and being positioned so as to hold a drive ring 3 of a variable nozzle mechanism 100 to the guide part 5 a of a nozzle mount 5 in the thrust direction, and setting the thrust-directional width of the drive ring 3 smaller than the width of the guide part 5 a, and providing an adjusting member 20 c between the flange portion of the nail pin 20 and the end face of the guide part 5 a to adjust a distance between the side face of the nozzle mount and the flange portion of the nail pin 20.
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INTRODUCTION
[0001] This invention relates generally to the application and utilization of a heat driven engine to improve the efficiency of separation of a brine waste stream. Specifically this invention describes the use of low grade waste heat to drive a novel, single chamber adsorption type heat driven engine that removes the excess solvent, water, from the brine offal of the secondary aluminum smelting process, reducing the need to provide higher quality energy to this separation process. The device is also useful for extracting water from other solute/solvent mixtures.
[0002] Heat driven engines, including adsorption chillers, are well known by those in the art. The work output of an adsorption chiller is typically chilled water used for air conditioning, process cooling or numerous other useful purposes. The chilled water circuit in a typical adsorption chiller is a closed loop, sometimes with the end load in communication with the chiller and often with a heat exchanger in the loop to isolate the chiller from the potential contaminates of the end load. A typical adsorption chiller comprises multiple chambers separated by valved walls or barriers.
[0003] Co-pending application Ser. No. 12/550,290 entitled “Improved Adsorbent—Adsorbate Desalination Unit And Method,” describes an open loop adsorption concentrator system having an internally divided housing and utilizing silica gel and water as the preferred working pair (the “'290 Application”). The '290 Application introduces an economizing heat exchanger and a mist eliminator as new techniques to handle the needs of such an open loop system. As with prior art adsorption chillers, the pressure vessel of the '290 Application is a multi-chambered shell interconnected by a plurality of valves which open and close to intermittently prohibit and allow the flow water vapor from chamber to chamber within the pressure vessel.
[0004] The present invention describes an open loop in the evaporator of a single, open chamber adsorbent/adsorbate system optimized for use as a concentrator for the heavy salt brines found as an offal or waste product of the aluminum smelting industry. The challenges involved in handling and separating such heavy salt brines require further improvements to an open loop system as described in the '290 Application. The construction of the concentrator is simplified to eliminate the internal vapor barriers and moving valves to avoid contamination and malfunction of these features. The elimination of the vapor valves opens the condenser to the uninhibited vapor flow from the evaporator. Another innovation in the present invention is the circulation of cooling water in the condenser at all times, without the cycling typically found in a standard adsorption chiller. After cooling water is run through the condenser, it is selectively used to cool the adsorbent and thus drive the adsorption cycle. In this manner, the isosteric heat of adsorption may then be reclaimed by the cooling water and put back into the concentrator system by feeding it into the brine heat exchanger.
[0005] A wash down feature on the mist eliminator is also added to maintain proper function in light of the high levels of salt drift contamination.
[0006] Another novel feature of the present invention is the use of a brine heat exchanger and an optional degasser, external to the vacuum shell, to heat and de-gas the brine before it is introduced into the evaporator. Recirculation of brine through the brine heat exchanger is essential to maintaining the brine at a temperature above that of the cooling water and the condenser so that a partial pressure differential is maintained between the upper area and lower areas within the shell, thereby creating a continuous vapor flow within the shell.
[0007] Yet another feature of a preferred embodiment of the present invention is the utilization of an evaporator within the shell. Finally, evaporation may also be enhanced by flowing the brine over a high surface area, porous fill media.
[0008] This disclosure will describe specifically a single chamber adsorption concentrator with an open loop in the evaporator for the extraction of water from a solute/solvent mixture having particular application to the brine slurry produced as a waste stream from the aluminum smelting process. For this application, silica gel and water or zeolite and water are the preferred choices for the adsorbent/adsorbate working pair of this invention. The novel modifications of a typical adsorption chiller necessary to support this heavy brine in an open loop system will be evident upon examining the detailed description and associated figures included in this specification.
[0009] While this invention will describe the application of a silica gel and water working pair to the application of separating water from the aluminum brine in an adsorption concentrator, it is understood by the inventors that this same process could be adapted to solvent extraction from many different types of brines, slurries, contaminated streams of solvents and similar mixtures provided that the solute is non-volatile in a vacuum. Silica gel and zeolite are suitable choices where water is the solvent; however other types of adsorption working pairs would also make it possible to extract other solvents from additional types of fluid slurries or mixtures. Such mixtures might be alcohol and water or water and oil.
BACKGROUND OF THE INVENTION
[0010] In the aluminum industry there are two general types of processing plants: primary smelting operations and secondary smelting operations. The primary processing plants start with the mining operations and the conversion of raw alumina ore into the finished aluminum ingots or products. Secondary smelting plants use scrap aluminum as the raw materials to be processed. The two processes share many similarities once the basic aluminum is formed. Both produce a series of waste products that must be cleaned, separated, recycled and reclaimed.
[0011] Aluminum secondary smelting (scrap recycling) accounts for approximately 33% of all aluminum produced in the U.S. There are approximately 68 major secondary processing plants in the U.S. These processing plants are typically located near large urban areas where large supplies of scrap aluminum are available. Such locations, however, also place these plants in areas where the environmental impact of the plant's operations is carefully measured and monitored.
[0012] The re-melting process of the aluminum produces a solute/solvent mixture or brine which typically comprises one or more solvents, typically substantially water, and one or more solutes including but not limited to metallic aluminum (typically about 10% by weight), aluminum oxide (typically about 50% weight), and a mixture of potassium salts and chloride salts, notably potassium chloride and sodium chloride (typically about 40% weight), and other solutes resulting from aluminum smelting processes. In current processes, the salts are separated from the insoluble aluminum oxide in a hot leach step. The solution of saturated potassium chloride and sodium chloride contained in the brine are then crystallized by evaporating the water in an energy intensive process, typically electric motor-driven vapor recompression or fuel-fired thermal brine concentration. The present invention relates to an improved means and method to remove water from the brine, making the process more efficient and economical. The resulting products of the separation, the distilled water and the concentrated salts, can all be reclaimed and recycled.
BRIEF SUMMARY OF THE INVENTION
[0013] This invention describes the application of low grade heat to drive a heat driven engine that will separate water from a brine solution. Specifically, this invention will describe a heat driven engine of the adsorption type using an adsorbent/adsorbate working pair. In this invention, the preferred working pair is silica gel and water and the evaporator section of the device will be an open loop system. The pressure vessel or shell of the present invention is a hollow, single, relatively open space, not divided into compartments or chambers. The solvent is water and the solute is a combination of potassium-chloride and sodium-chloride salts. The water for the working pair will be the water being evaporated from the brine that is continuously or intermittently introduced into the evaporator from other processes.
[0014] Closed loop process fluid (water) will be used to connect the adsorption concentrator heat exchangers to the external sources of the cooling and heating.
[0015] The heat required to drive the adsorption concentrator will be available as low quality waste heat from the smelting process that would otherwise typically be rejected to the atmosphere as a heat sink by means of a heat dump such as a body of water or an atmospheric cooling tower.
[0016] This adsorption concentrator uses an adsorbent-adsorbate working pair of silica gel and water cycling between adsorption and desorption. During the adsorption period, water is evaporated from the brine and adsorbed in the silica gel. The heat of evaporation is removed from the brine. The isosteric heat of adsorption is deposited into the silica gel as it adsorbs the water vapor. This isosteric heat is removed from the adsorbent silica gel during this period by circulating cooling water through the silica gel modules. The heat of evaporation removed from the brine is replaced with isosteric heat by use of an external heat exchanger in the recirculating brine loop.
[0017] When the silica gel is saturated, the adsorption process is halted and the desorption process is initiated. The desorption period dehydrates the silica gel by reintroducing the isosteric heat to the silica gel, warming the silica gel and driving the water vapor from the silica gel. The water vapor is condensed back into liquid water in the condenser. This desorption process creates a demand for low quality waste heat that was previously discarded and provides an opportunity for a gain in efficiency in the overall smelting process.
[0018] In the preferred embodiment, a new supply of source brine is continuously introduced into the evaporator of the adsorption concentrator. Upon introduction, the temperature of the brine will be relatively hot as a result of the smelting process through which it was created. The introduction of relatively hot brine to the evaporator hastens the evaporation of the water from the brine. The water being evaporated from the brine is adsorbed and stored in the silica gel or, since all components are housed within the single chamber of the hollow shell, may be condensed directly by the condenser.
[0019] Water evaporation from the brine results in an increase of the concentration of the solutes in the brine collected in the sump. In other words, the brine not evaporated has a greater solute concentration than the source brine. The un-evaporated brine is recirculated to be sprayed over the evaporator multiple, times with reheating through a brine heat exchanger on each pass. In practice, the temperature of the brine heat exchanger, the rate of introduction of relatively hot source brine, the rate of recycling of un-evaporated brine, and the rate at which concentrated un-evaporated brine is removed from the concentrator can be coordinated in order to achieve a desired equilibrium in the solute concentration of the un-evaporated brine in the sump. These process variables can be optimized to produce a concentrate brine that has a much greater concentration of solutes than the source brine. Constant recirculation and the agitation caused by re-introduction of the brine into the concentrator are essential to achieving the desirable higher concentration of solutes in the concentrated brine. This constant circulation keeps the brine in a uniform concentration and at a relatively high temperature.
[0020] When the silica gel becomes saturated, the adsorption process will be halted and a desorption cycle is initiated. During the desorption cycle, hot water is introduced to the silica gel modules to warm them and drive off the water vapor through desorption. The water vapor will be drawn to the condenser along a vapor pressure differential created between the condenser and the areas surrounding the silica gel and the evaporator. In the condenser, the vapor is condensed to a liquid and withdrawn from the concentrator through a sump as distilled water.
[0021] Cooling water is circulated through the condenser at all times. After passing through the condenser, the cooling water will be selectively passed through the silica gel modules during the adsorption cycle or passed directly to a cooling tower heat exchanger for cooling and recirculation back to the condenser.
[0022] When the concentrator is in the adsorption period, because the shell is open throughout without any compartmentalization or intermittent barriers such as opening and closing valves, some water vapor will be condensed directly from the evaporator as allowed by the differences in the temperatures and partial pressures. During the desorption period, the area within the shell about the condenser will have the lowest relative partial pressure compared to other areas within the shell because the cooling is continued during the desorption period, resulting in water vapor condensing out of the vapor phase and into the liquid phase.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] The particular features and advantages of the invention as well as other objects will become apparent from the following description taken in connection with the accompanying drawings in which:
[0024] FIG. 1 is a schematic view of the adsorption concentrator of the present invention.
[0025] FIG. 2 is a schematic view of one embodiment of the adsorption concentrator of the present invention.
[0026] FIG. 3A is a schematic diagram of the four-way valve shown in FIG. 2 as reference 65 as positioned during the desorption cycle.
[0027] FIG. 3B is a schematic diagram of the four-way valve shown in FIG. 2 as reference 65 as positioned during the adsorption cycle.
[0028] FIG. 4 is a schematic view of a second embodiment of the adsorption concentrator of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0029] FIG. 1 shows the principal elements of an adsorption concentrator 5 according to the present invention. These elements are housed in a single chamber, substantially hollow, vacuum tight enclosure of a concentrator housing or shell 10 . A vacuum is maintained within the shell 10 . At or near the lower area or lower end 40 of the shell 10 , within the shell 10 , is an open loop evaporator 11 . A source solute/solvent mixture or brine solution to be distilled is fed into an open loop evaporator 11 through the hot brine input line 12 and is substantially continuously distributed about, across or upon the evaporator 11 , such as by spraying it through one or a plurality openings, such as brine spray nozzles 13 positioned about the portion of the hot brine input line 12 within the shell 10 . That portion of the brine that is not evaporated upon introduction into the near vacuum about the evaporator 11 falls and is collected as a concentrated brine in an evaporator sump 14 at the lower end 40 of the concentrator shell 10 where it is pulled, such as by a pump means (not shown), through a vacuum trap or other pressure-maintaining drain 43 designed to allow removal of the concentrated brine solution without significantly affecting or changing the pressure within the shell 10 . The drain 43 is connected to a brine output line 15 and recirculated across the evaporator 11 . The concentrated brine is directed through the brine output line 15 or other appropriate plumbing, either back into the hot brine input line 12 , or, alternately, to a brine output line (not shown in FIG. 1 ). During the start-up of the concentrator 5 , it may be necessary to recirculate all of the concentrated brine until the desired concentration of solutes in the concentrated brine is achieved. Otherwise, once the desired solute concentration is achieved, a portion of the concentrated brine is substantially continuously recirculated while a second portion of the concentrated brine is substantially continuously removed through the brine output line (shown as 26 in FIG. 2 ).
[0030] The evaporator 11 of the present invention may comprise any suitable evaporator common in the art, including both passive or active evaporators 11 . In one preferred embodiment, the evaporator 11 comprises a passive evaporator functioning as a means for maximizing the surface area over which a fluid is distributed. A passive evaporator may comprise any physical structure providing suitable surface area over which fluid can traverse substantially unimpeded under the influence of gravity. Maximizing the surface area over which the brine is sprayed increases the rate of evaporation. Alternatively, the evaporator 11 may comprise an active evaporator such as a heat exchanger connected to an external heating source, such as a flow of hot fluid through the evaporator 11 .
[0031] Returning to FIG. 1 , in one preferred embodiment, the evaporator 11 may comprise a first portion of its surface 17 positioned above the normal operating level 19 of the solute/solvent mixture in the evaporator sump 14 and a second portion of its surface 18 positioned below the normal operating level 19 of the solute/solvent mixture in the sump 14 . In another embodiment, shown in FIG. 2 , the portion 18 of the evaporator 11 below or within the level 19 of the solute/solvent mixture of the sump 14 may further comprise a porous, high surface area fill media 16 intended to add surface area and thereby enhance evaporation of the brine solution from the sump 14 . For purposes of this disclosure, the term “evaporator” 11 may comprise either submerged portion 18 , unsubmerged portion 17 , or both portions 18 , 17 of the evaporator 11 .
[0032] Interposed within the concentrator shell 10 between the evaporator 11 and the adsorbent modules, such as silica gel modules 50 , is a mist eliminator 35 . The mist eliminator 35 functions to substantially prevent brine contaminants from entering the adsorbent modules 50 . Adsorbent modules 50 are positioned within the shell 10 above the mist eliminator 35 , between the mist eliminator 35 and the condenser 75 , proximate to the upper area 41 of the concentrator shell 10 in which the condenser 75 is positioned.
[0033] The mist eliminator 35 functions to prevent passage of water droplets and other brine contaminants and particulates upward from the evaporator 11 to the adsorbent modules 50 or condenser 75 and to collect water droplets and contaminants from the air and vapor stream and divert the liquid and contaminants back to the evaporator 11 and sump 14 . However, the mist eliminator 35 does not materially impede or inhibit the free flow of water vapor within the shell 10 . The mist eliminator 35 provides a large surface area in a small volume of space to collect liquid without substantially impeding air or vapor flow. Mist eliminator 35 may comprise any number of physical structures known in the art for creating a tortured path for an air stream to follow, thereby providing ample surface areas upon which water droplets in the air stream can collect. The results achieved by a mist eliminator 35 will depend on proper specification of mist eliminator type, such as mesh, vane or fiber bed (or a combination of types), orientation, thickness, internal details, support and spacing in the vessel, vapor velocity and flow pattern, and many other considerations. The mist eliminator 35 of the present invention may be designed in one or more elements or screens for easy removal from the shell 10 through a pressure-sealed opening (not shown) for cleaning or replacement.
[0034] A mist eliminator input line 36 is provided to carry and dispense fluid with which to wash the captured contaminants and particulates from the mist eliminator 35 , either periodically or continuously, by injecting a hot fluid, such as the preferred water, or another suitable fluid, through a plurality of openings positioned about the portion of the mist eliminator input line 36 , within the shell 10 such as mist eliminator spray nozzles 37 . The fluid is dispensed upon the width and breadth of the mist eliminator 35 to wash captured contaminants and particulates back into the brine in the brine sump 14 .
[0035] An array of one or more modules carrying an adsorbent which can be regenerated or, for short, adsorbent modules, such as silica gel modules 50 , is located near the upper area 41 of the concentrator shell 10 . The array of adsorbent modules 50 is alternately used for adsorption and desorption of water vapor by altering the temperature of the fluid, such as water, flowing through a module fluid circuit (comprising lines 51 , 52 and modules 50 ) running through the modules 50 . When cooling fluid, such as cooling water, is pumped into the module input line 51 , the cooling fluid passes through the adsorbent modules 50 and the adsorbent will cool and adsorb water vapor rising from the evaporator 11 . Such adsorption creates a relatively lower partial pressure in the area 44 of the shell 10 about the adsorbent modules 50 . When hot temperature fluid, such as the preferred hot water, is pumped into the module fluid circuit, the adsorbent modules 50 will be heated to a higher temperature and will desorb the collected water back into water vapor. Desorption creates a relatively higher partial pressure in the area 44 within the shell 10 about the adsorbent modules 50 and the water vapor will tend to flow away from this zone of higher partial pressure towards the relatively constant area 41 of relatively lower partial pressure about the condenser 75 which is created as water vapor is condensed into water at the condenser 75 .
[0036] To drive condensation, a cooling fluid, preferably water, preferably having a temperature lower than the temperature of the brine, will be circulated through the condenser 75 positioned within the upper area 41 of the concentrator shell 10 substantially continuously during operation of the concentrator 5 . When the adsorbent modules 50 are in the desorption mode, desorbed water vapor will collect in the area 41 about the condenser 75 quickly as it is driven from the higher temperature and higher partial pressure area 44 about the adsorbent modules 50 and will condense back to a liquid form. When the adsorbent modules 50 are in an adsorption mode, the area 41 about condenser 75 may still be at a sufficiently low temperature and partial pressure relative to the area 44 about the modules 50 to continuously attract and condense some water vapor formed at the evaporator 11 , albeit at a slower rate. Additionally, because the shell 10 is not compartmentalized, that is, it is without non-permeable barriers dividing the interior of the shell 10 to restrict or otherwise permanently or temporarily or intermittently inhibit the substantially free flow of gas or water vapor to all areas within the shell 10 (such as with valves that are opened and closed periodically), it is contemplated that at least a portion of the water vapor from the evaporator 11 may bypass adsorption into the silica gel of the adsorbent modules 50 and be directly condensed into water at the condenser 75 .
[0037] The condensate or distilled water from the condenser 75 is collected in a condenser sump 100 where it is directed out of the concentrator shell 10 through a vacuum trap or other pressure-maintaining drain 43 to a condenser drain line 101 . The distilled condensate water leaving the adsorption concentrator 5 represents one of the useful products of the invention. This condensate water is a clean, pure, distilled water that can be used for any desired purpose.
[0038] A vacuum pump 110 is provided to create and maintain the initial vacuum within the shell 10 , and, as needed, to reduce the gas pressure inside the concentrator shell 10 by removing any non-condensable gases that may be introduced into the concentrator shell 10 by the brine. The reduced pressure created by the vacuum pump 110 inside the concentrator shell 10 improves the efficiency of the invention by reducing the temperature at which the water will boil from the brine and enhancing the desorption process. The vacuum pump 110 is connected to the concentrator shell 10 by a vacuum pump line 111 .
[0039] The temperature of the condenser 75 is limited by the temperature of the cooling fluid entering the condenser input line 71 , circulating through the condenser 75 and exiting through the condenser output line 72 . In contrast, the temperature of the adsorption modules 50 varies depending upon whether cooling fluid or heating fluid is circulated through the module fluid circuit. Similarly, because of the heat of the relatively hot source brine and the re-heating by the brine heat exchanger through which it is passed, the recirculated condensed brine is maintained at a temperature higher than the condenser 75 and the cooling fluid by which the condenser 75 is driven. Maintaining the brine and the area 40 within the shell 10 about the evaporator 35 at a higher temperature than the temperature of the condenser 75 and the area 41 within the shell 10 about the condenser 75 creates a temperature gradient and partial pressure differential along which the water vapor will flow continuously during operation of the condenser 5 .
[0040] FIG. 2 illustrates the complete brine concentrator system 30 , including ancillary equipment and components that are used to control the function of the adsorption concentrator 5 . Certain of these components may comprise an integral part (i.e., within the shell 10 ) of the adsorption concentrator 5 unit itself, while other components, such as heat exchangers 20 , 80 and pumps 25 , 70 , 83 and external plumbing would typically be external to the concentrator 5 and are specifically adapted to suit the physical environment in which the concentrator 5 is to operate.
[0041] Brine from a source (not shown) is introduced to the concentrator system 30 through a brine feed line 21 which passes the brine through a conventional degasser 27 . The degasser removes the volatile gases from the brine before it enters the adsorption concentrator 5 , reducing the load on the vacuum pump 110 . The degasser also increases the efficiency of the adsorption concentrator 5 by improving the vacuum level in the evaporator 11 . As illustrated in FIG. 2 , the degasser 27 may be positioned along the brine feed line 21 before the brine heat exchanger 20 .
[0042] The brine is introduced into the shell 10 at a relatively hot temperature from between about 100° F. to about 120° F., typically about 110° F., or such other temperature at which it may be substantially upon being generated through the smelting process. In practice, it is preferable to maintain the brine at a temperature above the temperature of the cooling fluid used to drive the condenser 75 and adsorption in the adsorbate modules 50 .
[0043] A brine feed control valve 22 controls the source of the brine input to the brine heat exchanger 20 by selectively allowing a feed of brine from one or more sources. A portion of the hot brine input line 12 passes into the shell 10 for spraying or disbursing the brine proximate to the evaporator 11 .
[0044] To enhance evaporation of water and separation of water from the solutes in the brine, the brine is substantially continuously recirculated through a brine recirculating circuit between the evaporator sump 14 and the brine heat exchanger 20 and back to the sump 14 after having been disbursed again across the evaporator 11 . The brine is recirculated by a pump means, such as brine recirculation pump 25 in the brine recirculating circuit. The brine recirculating circuit comprises brine output line 15 , pump means 25 , brine recirculation line 23 running to a brine heat exchanger 20 , and evaporator input line 12 for circulating heated brine from the brine heat exchanger 20 back into the area 40 about the evaporator 11 . In this circuit, brine from the sump 14 is reheated then carried back through the evaporator input line 12 for re-distribution across the evaporator 11 . The recirculated brine passes through the brine heat exchanger 20 on each recirculation pass. After initial start-up of the concentrator 5 , once the concentration of solutes in the brine in the sump 14 reaches the desired level, the brine recirculation valve 24 is partially opened to allow a portion of the concentrated brine to be removed from the concentrator system 30 through the brine output line 26 at the desired rate while another portion of the concentrated brine is recirculated. Though not essential to the proper functioning of the concentrator 5 , it is preferable that the operation of the brine recirculation valve 24 and the brine feed control valve 22 be coordinated so that fresh brine is substantially continuously added along with the recirculated concentrated brine. Similarly, through not essential, it is preferable that concentrated brine is continuously removed from the concentrator 5 once the desired concentration has been achieved.
[0045] The area 40 of the adsorption concentrator 5 about the evaporator 11 is maintained at a relatively high temperature by the introduction of relatively hot source brine and the recirculation of concentrated brine through the brine heat exchanger 20 to promote the evaporation of water in the brine. The relatively high temperature of the brine in the evaporator 11 and the evaporation of water from the brine into water vapor produces a relatively high partial pressure in the area 40 about the evaporator 11 within the adsorption concentrator 5 .
[0046] The heat that is added to the brine as it passes through the brine heat exchanger 20 is provided from a hot water supply line 56 that supplies hot water from a hot water source (not shown) to the brine heat exchanger 20 . In one preferred embodiment, heat may also be provided in part by directing all or a portion of the cooling fluid which has gained isosteric heat of adsorption in the adsorption modules 50 as it was used to drive adsorption during the adsorption cycle.
[0047] During the adsorption period of the cycle, the silica gel in the modules 50 is cooled by the introduction of cooling water at a temperature range expected to be between about 50° F. to about 100° F., preferably at a temperature below the temperature of the brine as it is introduced into the adsorption concentrator 5 , such as at about 85° F. to about 90° F. This cooling water removes the isosteric heat of adsorption from the adsorbent modules 50 that has been deposited during the adsorption process. This allows the silica gel itself to create a partial pressure near zero in the area 44 about the modules 50 . The differential pressure between the area 44 within the shell 10 about the adsorbent modules 50 and the area 40 within the shell 10 about evaporator 11 quickly moves the water vapor from the evaporator 11 to the adsorbent modules 50 .
[0048] This rapid flow of the water vapor creates the need to provide a mist eliminator 35 within the shell 10 between the evaporator 11 and the adsorbent modules 50 . The mist eliminator 35 collects mist (water droplets) and airborne contaminants such as the salts from the brine. These airborne contaminants are collected on the mist eliminator 35 and are washed from the surfaces of the mist eliminator 35 from time to time using a wash down feature. In a preferred embodiment, the wash down is accomplished by introducing fluid, such as all or portion of the hot water or cooling water leaving the modules 50 through module output line 50 , through a mist eliminator input line 36 having a plurality of openings, such as mist eliminator spray nozzles 37 that are positioned about that portion of the mist eliminator input line 36 within the shell 10 , to adequately wash the surfaces of the mist eliminator 35 . The wash down fluid is gravitationally pulled to the evaporator 11 where it mixes with the brine and eventually distilled by the concentrator 5 like any other water in the brine.
[0049] The temperature of the adsorbent modules 50 is determined by the temperature of the cooling water that is circulated into the modules 50 through a module fluid circuit comprising module input line 51 , the modules 50 , and module output line 52 . In the preferred embodiment shown in FIG. 2 , whether the fluid passing through the module fluid circuit is hot (for desorption) or cooler (for adsorption) is controlled by four-way valve 65 . During the adsorption cycle, cooling fluid from the condenser 75 is routed through the four-way valve 65 to the module fluid circuit. The module output line 52 of the module fluid circuit connects to the brine heat exchanger 20 and may also include mist eliminator valve 38 to selectively direct all or a portion of the fluid through mist eliminator input line 36 .
[0050] In the adsorption cycle, the cooling fluid will pass through the brine heat exchanger 20 , exiting through brine heat exchanger outlet line 91 to the brine heat exchanger valve 90 which, in the adsorption cycle, directs the cooling fluid to alternate cooling water return line 92 which returns the cooling fluid to the cooling tower heat exchanger 80 where it is cooled for reuse through the condenser input line 71 .
[0051] A cooling tower heat exchanger 80 is included in this path to isolate the cooling water that is run through the adsorption concentrator 5 from the heat sink, such as a body of water (not represented) or, as illustrated here, a cooling tower 82 . Both types of heat sinks are well known sources of contaminants that can be isolated from the cooling water used to drive the heat driven engine 5 with a simple heat exchanger such as the cooling tower heat exchanger 80 .
[0052] The cooling tower water is circulated with a cooling tower pump 83 that draws cooling water from the cooling tower 82 . The water is pumped through a cooling tower output line 84 , to the cooling tower heat exchanger 80 and back to the cooling tower 82 by way of a cooling tower input line 81 . Any waste heat from the condenser 75 and the adsorbent modules 50 that is not taken back into the system as heat added to the recirculating brine in the brine heat exchanger 20 is expelled to the environment, in this case by the air flow 85 through the cooling tower 82 .
[0053] During the desorption cycle, the four-way valve 65 is selected to direct cooling fluid exiting the condenser 75 through cooling water return line 66 connected to the cooling tower heat exchanger 80 . At the same time, the four-way valve 65 directs hot water from hot water supply line 56 to the adsorbent modules 50 through the lines of the module fluid circuit. Hot water exiting the modules 50 is fed to the brine heat exchanger 20 where its heat is utilized to heat the recirculated brine. Again, the mist eliminator valve 38 may direct all or a portion of the hot water into the mist eliminator 35 but otherwise simply directs the hot water to the brine heat exchanger 20 and then on to the brine heat exchanger outlet 91 . In the desorption cycle, brine heat exchanger valve 90 is selected to direct hot water to hot water return line 57 .
[0054] Alternately, circulating both the cooling fluid used to drive the adsorption cycle and the hot water used to drive the desorption cycle through the brine heat exchanger 20 will result in a slight fluctuation of the temperature of the recirculated brine being introduced into the area 40 of the shell 10 about the evaporator 11 , but the temperature fluctuation will not result in the net temperature of the source brine and the recirculated brine in the shell 10 dropping below the temperature of the condenser 75 or the cooling fluid as it passes into and out of the condenser 75 .
[0055] A vacuum pump 110 is operated at all times to remove non-condensable gases from the adsorption concentrator 5 that may be introduced by the brine. The vacuum pump 110 is connected to the concentrator shell 10 by a vacuum pump line 111 . The vacuum pump 110 has a water vapor filter (not shown) to prevent it from pulling water vapor from the concentrator 5 .
[0056] FIGS. 3A and 3B schematically illustrate the flow of fluids through the four-way valve 65 of the brine concentrator system 30 of FIG. 2 . FIG. 3A illustrates the positioning of the four-way valve 65 during the desorption cycle. Cooling fluid leaving the condenser 75 through condenser output line 72 is routed through connector 47 to cooling water return line 66 connected to the cooling tower heat exchanger 80 . Simultaneously, hot fluid from a hot water source (not shown) flowing through hot water supply line 56 is routed through connector 45 to the modules 50 through module input line 51 . During the desorption cycle, connector 46 is not used and is substantially empty.
[0057] When the brine concentrator 30 enters the adsorption cycle, four-way valve 65 switches from the position shown in FIG. 3A to the position shown in FIG. 3B . During the adsorption cycle, connector 46 connects the condenser output line 72 to the module input line 51 allowing cooling fluid leaving the condenser 75 to pass to the modules 50 to drive desorption. The flow of hot fluid through hot water supply line 56 is halted as is the flow of water into cooling water return line 66 . Connectors 46 and 47 are disengaged and remain empty during the desorption cycle.
[0058] FIG. 4 illustrates an alternate embodiment of the brine concentrator system 115 of the present invention.
[0059] Brine is introduced to the concentrator system 115 through a brine feed line 21 which passes the brine through a conventional degasser 27 and a brine heat exchanger 20 . As illustrated in FIG. 4 , the degasser 27 may be positioned along the brine feed line 21 before the brine heat exchanger 20 . However, the degasser 27 may alternately be located after the brine heat exchanger 20 on the hot brine input line 12 if that proves to be more effective and efficient to the operation of the concentrator system 115 .
[0060] The brine heat exchanger 20 is provided on the brine feed line 21 to heat or raise the temperature of the brine before it is introduced into the shell 10 to a temperature from between about 100° F. to about 175° F., preferably to a temperature in the range of about 100° F. to about 120° F.
[0061] A brine feed control valve 22 controls the source of the brine input to the brine heat exchanger 20 by selecting a feed from the brine recirculation line 23 , the brine feed line 21 or allowing a combination of both lines 21 , 23 . Brine heated by the brine heat exchanger 20 is carried from the brine heat exchanger 20 through the hot brine input line 12 . A portion of the hot brine input line 12 passes into the shell 10 for spraying the brine proximate to the evaporator 11 .
[0062] To enhance evaporation of water and separation of water from the solutes in the brine, the brine is substantially continuously recirculated from the evaporator sump 14 by a pump means, such as brine recirculation pump 25 . Brine output line 15 further comprises a brine recirculation line 23 for circulating brine from the sump 14 to the brine heat exchanger 20 for reheating. Recirculated and reheated brine is then carried back through the evaporator input line 12 for re-distribution across the evaporator 11 .
[0063] The heat that is added to the brine as it passes through the brine heat exchanger 20 is provided from a hot water supply line 56 that supplies hot water from a hot water source (not shown) to the brine heat exchanger 20 .
[0064] During the adsorption period of the cycle, the silica gel in the modules 50 is cooled by the introduction of cooling water at a temperature range expected to be between about 50° F. to about 100° F., preferably at a temperature below the temperature of the brine as it is introduced into the adsorption concentrator 5 , such as at about 85° F.
[0065] A mist eliminator 35 is provided within the shell 10 between the evaporator 11 and the adsorbent modules 50 . Airborne contaminants are collected on the mist eliminator 35 and are washed from the surfaces of the mist eliminator 35 from time to time using a wash down feature comprising a mist eliminator input line 36 having a plurality of openings, such as mist eliminator spray nozzles 37 that are positioned about that portion of the mist eliminator input line 36 within the shell 10 .
[0066] The temperature of the adsorbent modules 50 is limited by the temperature of the cooling water that is circulated into the modules 50 through module fluid circuit comprising module input line 51 , the modules 50 , module output line 52 , and a cooling water pump 70 . Cooling water enters through module input line 51 and, once circulated through the adsorbent modules 50 , the cooling water is removed through the module output line 52 . A cooling tower heat exchanger 80 is included in this path to isolate the cooling water that is run through the adsorption concentrator 5 from the heat sink, such as a cooling tower 82 .
[0067] In a preferred embodiment of the present invention, a common control valve body 58 contains two coordinated valves, a module output valve 53 and a module input valve 54 . During adsorption, the module input valve 54 is open to the condenser input line 71 allowing cooling water from the cooling tower heat exchanger 80 to enter the adsorbent modules 50 and remove the isosteric heat of adsorption. That cooling water exits the adsorbent modules 50 and flows through the module output valve 53 where it is directed to the condenser output line 72 and returned to the cooling tower heat exchanger 80 .
[0068] During the desorption process, hot water is directed to the adsorbent modules 50 using the valves 54 , 53 of the common control valve body 58 . The module input valve 54 is open to the hot water line 55 and the hot water supply 56 . Simultaneously, the module output valve 53 is open to the hot water control line 59 that connects the module output valve 53 to the mist eliminator valve 38 . The mist eliminator valve 38 may direct all or a portion of the hot water into the mist eliminator 35 but otherwise simply directs the hot water to the hot water return line 57 .
[0069] Although this invention has been disclosed and described in its preferred forms with a certain degree of particularity, it is understood that the present disclosure of the preferred forms is only by way of example and that numerous changes in the details of operation and in the combination and arrangement of parts may be resorted to without departing from the spirit and scope of the invention as hereinafter claimed.
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A single chamber adsorption concentrator unit is described that utilizes low grade heat to drive an adsorbent/adsorbent working pair to separate a solvent from a solute/solvent mixture. One preferred application of the device of the present invention is separating water from the salt brine produced by the aluminum smelting industry. The brine solution is introduced into a single chamber shell proximate the concentrator evaporator where the water in the brine can freely evaporate and the resulting water vapor freely flow without inhibition to be either absorbed into the adsorbent modules or condensed by the condenser. The free flow of water vapor is facilitated by continuous operation of the condenser and by maintaining the brine solution at a higher temperature than the cooling fluid driving the condenser. A mist eliminator with a wash down feature located intermediate to the evaporator and the silica gel is provided to collect contaminants that may be carried from the evaporator by the vigorous boiling.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to a method of determining subterranean formation fracture orientation, and more particularly, but not by way of limitation, to a method of determining fracture orientation wherein a fracture is created in a formation and a location orientated core containing a portion of the fracture is removed therefrom.
2. Description of the Prior Art
In the production of fluids such as oil, gas and water from a subterranean rock formation penetrated by a wellbore, a commonly used technique for stimulating the production of fluids from the formation is to create and extend fractures therein. Most often, the fractures are created by applying hydraulic pressure on the formation from the wellbore. That is, a fluid is pumped through the wellbore and into the formation to be fractured at a rate such that the resultant hydraulic force exerted on the formation causes one or more fractures to be created therein. The fractures are extended by continued pumping, and the fractures are usually propped open after being formed and extended so that fluids contained in the formation readily flow through the fractures into the wellbore. Fracturing techniques are also used in formations penetrated by injection and production wells which are utilized for carrying out enhanced production procedures therein, e.g., waterflood and other similar recovery procedures, as well as in other oilfield applications.
Subterranean rock formations are usually bounded by formations formed of dissimilar rock materials. Because of this, in carrying out fracture stimulation procedures in a formation from which it is desired to produce fluids, it is often necessary and always desirable to know the direction of the least in situ principal stress in each formation, i.e., the direction in which fractures will extend in the formation, as well as the relative levels of the least in situ principal stresses in the formations. For example, when the formation containing desired fluids is bounded by one or more formations containing undesired fluids, if it is known that the formation containing desired fluids has the lowest least in situ principal stress level, then fractures can be created and extended in that formation without fear of fracturing the formations containing undesired fluids. If the converse situation exists and is known, a production stimulation procedure other than one involving fracturing can be utilized.
In a given field containing a reservoir of desired fluids, it is desirable to know the orientation of fractures induced in formations containing the fluids so that the drilling of wellbores into the formations and the production of fluids therefrom can be optimized and maximum production obtained. In other operations such as in carrying out enhanced production procedures and solution mining procedures where communication between wellbores is required, a knowledge of the orientation of induced fractures is essential to bringing about such communication.
By the present invention a method of determining induced fracture orientation, i.e., the direction of the least in situ principal stress, in one or more subterranean formations is provided. The fracture orientation information obtained can be utilized to determine if fracture techniques should be carried out in the formations, where other wellbores should be drilled, which of two or more formations has the lowest least in situ principal stress level and consequently will fracture first, and the like.
SUMMARY OF THE INVENTION
By the present invention, the orientation of fractures created in a subterranean formation penetrated by a wellbore is determined. A fracture is created in the formation extending from the lower end portion of the wellbore and a location orientated core containing a portion of the fracture is removed from the wellbore. The orientation of the fracture in the core is used to determine the orientation of the fracture in the formation.
After determining the orientation of a fracture created in a first subterranean formation, the method can be repeated to determine the orientation of fractures in one or more other formations and the least in situ principal stress levels in the formations can be determined.
It is, therefore, a general object of the present invention to provide a method of determining the orientation of fractures created in one or more subterranean formations.
A further object of the present invention is the provision of a method for determining the orientation of fractures created in two or more subterranean formations as well as the least in situ principal stress levels of the formations and other information during the drilling of a wellbore penetrating the formations.
Other and further objects, features and advantages of the present invention will be readily apparent to those skilled in the art upon a reading of the description of preferred embodiments which follows when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic illustration of the lower end portion of a wellbore penetrating a subterranean formation just after a fracture has been formed in the formation.
FIG. 2 is a diagrammatic illustration of the wellbore and formation of FIG. 1 showing the location of a core to be removed from the formation.
FIG. 3 is an enlarged top view of a core removed from a fractured formation.
FIG. 4 is a side view of the core of FIG. 3 taken along line 4--4 of FIG. 3.
FIG. 5 illustrates a portion of a typical fracturing chart illustrating a fracturing procedure carried out in accordance with the present invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
The drilling of wellbores penetrating subterranean formations is most commonly carried out using a string of drill pipe having a drill bit attached to the lower end. The drill pipe and drill bit are rotated while drilling fluid is circulated from the surface through the drill pipe and drill bit into the wellbore and then upwardly through the annulus between the wellbore and drill pipe back to the surface. The drilling fluid lubricates the drill bit and carries cuttings to the surface for separation therefrom.
In carrying out the method of the present invention for determining the orientation of fractures created in a subterranean formation during the drilling of a wellbore penetrating the formation, the wellbore is drilled to a point within the formation. That is, the wellbore is drilled into the formation but not through the formation. The string of drill pipe and drill bit are removed from the hole, a conventional open hole packer is connected to the lower end of the drill pipe and the packer and drill pipe are lowered in the wellbore to a point whereby a lower end portion of the wellbore within the formation remains below the packer. The packer is then set so that the lower end portion of the wellbore is isolated from the annulus between the wellbore and the string of drill pipe above the packer.
Referring now to FIG. 1, the lower portion of a wellbore 10 penetrating a subterranean formation 12 is illustrated. A string of drill pipe 14 is disposed in the wellbore 10 and an open-hole packer 16 is positioned in the wellbore 10 so that a lower end portion 18 of the wellbore within the formation 12 remains below the packer. As illustrated, the drill string 14 extends through the packer 16 and terminates therebelow so that fluids introduced into the wellbore 10 by way of the drill string 14 are prevented by the packer 16 from flowing within the wellbore into the annulus 20 between the wellbore and the drill string. While the lower end of the drill string 14 is shown in FIG. 1 positioned just below the packer 16, the drill string 14 can extend into the lower end portion 18 of the wellbore 10 and can extend to the bottom of the wellbore if desired.
After the packer 16 has been set in the wellbore 10, its sealing ability can be tested by pressuring up the annulus 20 above the packer and then pressuring up the lower end portion 18 of the wellbore below the packer to a higher pressure level than the pressure level in the annulus. If the annulus pressure does not increase while the higher pressure level in the wellbore below the packer is held at a substantially constant level, leakage around the packer is not taking place.
Upon setting and testing the packer 16, a fracturing fluid, most conveniently drilling fluid, is pumped through the drill string 14 into the lower end portion 18 of the wellbore 10 whereby hydraulic pressure is applied on the formation 12. The pumping rate and hydraulic force on the formation are increased to the level whereby a fracture 22 is created in the formation. The fracture 22 is generally vertical, as are most hydraulic pressure-induced fractures, and the pumping of the fracturing fluid is continued to extend the fracture in all directions from the lower end portion 18 of the wellbore 10 until communication between the lower end portion 18 and the annulus 20 occurs as shown by the arrows in FIG. 1. That is, when the fracture 22 extends in the formation 12 to a point above the packer 16, communication by way of the fracture between the lower end portion 18 and the annulus 20 takes place and a rise in the annulus pressure level will be noted. The total quantity of fracturing fluid required to be pumped into the lower end portion 18 of the wellbore 10 to create and extend the fracture 22 therein is usually quite small, e.g., in the range of from one to five barrels.
In a preferred technique, downhole pressure level recording instruments are placed in the wellbore 10 as a part of or with the packer 16 whereby the pressure below the packer in the lower end portion 18 of the wellbore 10, hereinafter referred to as the tubing pressure, and the pressure above the packer, i.e., the annulus pressure are continuously recorded. After evidence of the creation and extension of the fracture 22 has been obtained, the pumping of fluid into the lower end portion 18 of the wellbore 10 is terminated and the drill string 14 and wellbore 10 are shut in. The continuous recording of the tubing and annulus pressure levels after the shut-in (referred to in the art as the instantaneous shut-in pressure) provides information concerning the nature of the created fracture and the formation. Preferably, several sequences of pumping fluid into the lower end portion 18 of the wellbore 10 followed by shutting in the wellbore and tubing string are carried out at various pumping rates. If the annulus pressure level stabilizes as soon as pumping is stopped, the instantaneous closure of the fracture is indicated. To further determine fracture closure characteristics, the pressure level in the annulus 20 or the pressure level in the lower end portion 18 of the wellbore 10 can be reduced. If the fracture 22 is completely closed, the reduction of pressure in one of such locations will not cause the lowering of the pressure level in the other location.
During the carrying out of the procedures described above whereby fluid is pumped by way of the drill string 14 into the lower end portion 18 of the wellbore 10 and into the annulus 20 by way of the fracture 22, the pressure in the annulus may increase to a level whereby it is necessary to reduce the annulus pressure. This can be accomplished by flowing fluid out of the annulus by way of a surface valve connected thereto.
Once the fracturing and testing procedures described above have been carried out, the pressures in the annulus and in the lower end portion 18 of the wellbore 10 are relieved and the packer 16 is released from engagement with the walls of the wellbore. The packer 16 and drill string 14 are withdrawn from the wellbore and a conventional core cutting device capable of producing a location oriented core is lowered into the wellbore.
A variety of downhole coring techniques and apparatus have been developed whereby a portion of a selected downhole formation (known in the art as a core or core sample) is removed from the formation and taken to the surface while maintaining a knowledge of or ability to determine the location orientation of the sample. In accordance with the present invention, such an apparatus is utilized to obtain a location oriented core from the bottom of the wellbore 10. That is, the coring apparatus is utilized to cut and remove a vertical core sample 28 from the bottom 24 of the wellbore 10. The location from where the core sample 28 is removed is shown by dashed lines on FIG. 2 and is designated by the numeral 26.
Referring now to FIGS. 3 and 4, the core sample removed from the bottom 24 of the wellbore 10 is illustrated and designated by the numeral 28. Because the vertical fracture 22 extends downwardly from the bottom 24 of the wellbore 10, the core sample 28 obtained thereform contains a portion of the fracture 22. As mentioned above, the core 28 is location orientated so that when the core 28 is brought to the surface, orientated with respect to its original location, and the orientation of the portion of the fracture 22 contained therein observed, the orientation of the fracture 22 within the formation 12 can be determined.
Once the orientation of the fracture 22 in the formation 12 has been determined, the string of drill pipe and drill bit are again lowered into the wellbore 10 and the wellbore 10 is deepened. If it is desirable to determine the orientation of fractures in additional formations penetrated by the wellbore 10, the procedure described above for determining the orientation of fractures are repeated therein including the recording of instantaneous shut-in pressures in each formation. A comparison of the recorded pressure level and other information will, in addition to fracture orientation, reveal differences in the least in situ principal stress levels in the formations. That is, the formation which fractures at the lowest pressure and/or produces the lowest instantaneous shut-in pressure will be the most fracturable and has the lowest least in situ principal stress level.
While the methods of this invention are particularly suitable for determining subterranean fracture orientation during the drilling of a wellbore, the methods can be carried out in a wellbore after drilling has been terminated or after the well has been completed using conventional tools, pumping equipment, conduit strings disposed in the wellbore, etc.
EXAMPLE
Referring now to FIG. 5, a fracturing chart showing tubing pressure, annulus pressure and fracturing fluid rate during a fracturing procedure carried out in accordance with the present invention is illustrated. Segment 1 of the chart illustrates the tubing and annulus pressure maintained for the detection of leaks and testing of the packer which is set at approximately 8132 feet below the surface. A tubing pressure of 1000 psi. is maintained with the annulus pressure being 150 psi.
Segment 2 shows the pumping of fracturing fluid into the lower end portion of the wellbore which causes an immediate increase in tubing pressure to the point of formation breakdown or fracturing. After fracturing the annulus pressure rises almost immediately indicating communication between the lower end portion of the wellbore and the annulus. The average pumping rate is 11 gallons per minute with breakdown taking place at a surface pressure of 2160 psi. corresponding to a downhole pressure of 8177 psi. After breakdown, pumping is continued for a short time, i.e., about 2 minutes, to extend the fracture.
Segment 3 of the chart shows a first shut-in period wherein the tubing pressure drops to about 925 psi. and the annulus pressure rises to about 525 psi. After stabilization, the tubing and annulus pressures remain constant at a pressure differential of about 400 psi. across the packer.
Segment 4 of the chart shows a second pumping of fracturing fluid at a rate of about 8 gallons per minute for a pumping time of about 2 minutes. Again, a clear communication between tubing and annulus is shown.
Segment 5 shows a second instantaneous shut-in pressure which, because the tubing and annulus pressure level stabilized indicates immediate fracture closure.
Segment 6 shows a third resumption of pumping of fracturing fluid at a rate of about 5 gallons per minute. Again, immediate communication between the lower end portion of the wellbore and the annulus occurs. Segment 7 shows a third shut-in.
The orientated core obtained from the bottom of the wellbore after fracturing in the above-described manner contains a downwardly extending portion of the created fracture. The fracture is vertical and extends 3.5 feet below the bottom of the wellbore. The orientation of the fracture in the formation is easily determined from the location orientated core.
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A method of determining the orientation of a fracture or fractures created in a subterranean formation penetrated by a wellbore is provided. The method comprises creating a fracture in the formation extending from a lower end portion of the wellbore and then removing a location orientated core containing a portion of the fracture from the wellbore to thereby determine the orientation of the fracture in the formation.
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FIELD OF THE INVENTION
[0001] The present invention relates to a vehicle and to a method of controlling a vehicle. In particular, but not exclusively, the invention relates to a vehicle having stop/start functionality in which an actuator may be automatically stopped and restarted during the course of a drivecycle. By drivecycle is meant a period during which a vehicle is used to undertake a journey, commencing when the driver initiates starting of the vehicle (or ‘key on’) and ending when the driver initiates shutdown of the vehicle (or ‘key off’).
BACKGROUND
[0002] It is known to provide a motor vehicle having stop/start functionality in which an engine of the vehicle is switched off to save fuel when conditions permit such as when the vehicle is held stationary with a driver-operated brake pedal depressed. The condition in which the vehicle is held stationary with the engine automatically switched off during a drivecycle is known as an ‘eco-stop’ condition.
[0003] When the driver releases the brake pedal the engine may be restarted and a transmission of the vehicle may be re-engaged. That is, under ‘no fault’ normal operating conditions, release of the brake pedal by the driver triggers the engine to be restarted, the driveline to be closed and torque to be transmitted to the drive wheels.
[0004] It is also known to provide a hybrid electric vehicle (HEV) having an engine and an electric motor. In a parallel-type HEV the engine may be used to provide motive power to the vehicle. The engine and electric motor may be maintained in a stopped condition when the vehicle is held stationary by the brake pedal (i.e. in the eco-stop condition) in order to reduce fuel consumption.
[0005] If the vehicle is operating in a parallel mode in which the engine provides drive torque to the wheels, when the driver releases the brake pedal the vehicle may be arranged to restart the engine and re-engage the transmission. Alternatively, if the vehicle is operating in electric vehicle (EV) mode in which the electric motor is used to drive the vehicle and not the engine, if the vehicle is in the eco-stop condition (in which the electric motor is switched off when the vehicle is stationary) the vehicle may be arranged automatically to restart the electric machine when the brake pedal is released.
[0006] It is against this background that the present invention has been conceived. Embodiments of the invention may provide a vehicle or a method which improves upon known systems. Other aims and advantages of the invention will become apparent from the following description, claims and drawings.
STATEMENT OF THE INVENTION
[0007] In a first aspect of the invention there is provided a motor vehicle having an engine, driver-selectable first and second modes of operation and driver-operable means for selecting the first and second modes, when the first mode is assumed the vehicle being operable to implement a stop/start functionality in which the engine is stopped automatically and subsequently restarted during a drivecycle thereby to reduce an amount of time for which the engine is switched on over the drivecycle, when the second mode is assumed the vehicle being arranged to change a value of at least one operating parameter of the vehicle relative to vehicle operation when the vehicle is not in the second mode, the vehicle being operable such that at least one of:
driver selection of the second mode when the first mode has also been selected causes the vehicle to deselect the first mode; subsequent deselection by the driver of the second mode causes the first mode to be reselected automatically by the vehicle; and the vehicle is operable to assume the first mode in addition to the second mode if the first mode is selected by the driver when the vehicle is in the second mode.
[0011] The term “engine” used herein is not intended to be limiting, unless otherwise indicated, and includes, by way of non-limiting example, any suitable prime mover or drive device such as a combustion engine, turbine or electric machine.
[0012] The feature that the first and second modes may both be selected has the advantage that the driver may enjoy the stop/start functionality (and therefore the benefit of improved fuel economy and/or a reduction in an amount of one or more gases emitted by the engine over a given drive cycle) whilst in the second mode.
[0013] The second mode may correspond to a ‘dynamic’ or ‘sports’ mode in which the one or more vehicle operating parameters are changed so as to improve at least one performance characteristic of the vehicle such as a time taken to accelerate from rest to a given speed.
[0014] Alternatively or in addition the second mode may correspond to a mode in which a selected one of a plurality of special vehicle programs are executed. The special vehicle programs may be arranged to control the vehicle according to a methodology, protocol or the like in order to optimise vehicle performance in a given situation. For example one program may optimise vehicle operating parameters for off-road driving, another may optimise vehicle parameters for driving at high speeds whilst turning, another may optimise vehicle parameters for driving on an icy surface, another may correspond to a dynamic or sports mode, and so forth.
[0015] In an embodiment, if the first mode is selected whilst the vehicle is in the second mode the vehicle remains in the first mode when the driver subsequently deselects the second mode.
[0016] In an embodiment, if the first mode is selected by the driver when the vehicle is in the second mode, the vehicle remains in the first mode when the driver subsequently deselects and reselects the second mode.
[0017] Optionally the vehicle is operable wherein if the second mode is deselected by the driver the vehicle assumes the first mode regardless of whether or not the vehicle was in first mode when the second mode was deselected.
[0018] The vehicle may be operable wherein if the second mode is deselected by the driver the vehicle assumes the first mode regardless of whether or not the vehicle is in first mode when the second mode is deselected provided the vehicle was in the first mode when second mode was last selected.
[0019] In an embodiment, if the second mode is driver selected when the vehicle is not in the first mode, subsequent driver deselection of the second mode results in automatic cancellation of the first mode if the first mode is driver selected whilst in the second mode.
[0020] Optionally if the vehicle is in the second mode and not the first mode and first mode is selected by the driver, the vehicle remains in the first mode if the second mode is subsequently deselected.
[0021] In an embodiment, if the vehicle is in the second mode and not the first mode and the first mode is selected by the driver, the vehicle remains in the first mode if the second mode is subsequently deselected provided the vehicle was in the first mode when the second mode was selected.
[0022] In an embodiment the vehicle may be arranged wherein if the vehicle is in the second mode and not the first mode, driver deselection of the second mode results in the first mode remaining deselected by the vehicle.
[0023] Optionally if the vehicle is in the second mode and not the first mode, driver deselection of the second mode results in the first mode remaining deselected by the vehicle provided first mode was deselected when the vehicle was not in second mode.
[0024] Optionally if the first mode is selected when the vehicle is in the second mode, the vehicle is arranged to assume an override state in which driver selection and deselection of second mode does not cause the vehicle automatically to exit the first mode ( FIG. 2 only).
[0025] In an embodiment when in the override state driver selection and deselection of the first mode does not cause the vehicle automatically to exit the second mode.
[0026] Optionally the stop/start functionality is implemented by means of a stop/start control methodology in which the engine is switched off when the vehicle is stationary.
[0027] In an embodiment in the first mode a throttle map and/or a gear change map are changed relative to operation not in the first mode in addition to stop/start functionality thereby to reduce an amount of fuel consumed by the vehicle over a given drivecycle.
[0028] Thus in some arrangements the first mode is a mode in which one or more operational aspects of the vehicle are optimised for fuel economy and engine emissions, for example throttle maps and/or gear change (or ‘gear shift’) maps.
[0029] Optionally when in the second mode the vehicle is arranged to change a value of at least one operating parameter such that an engine speed at which a gearbox is arranged to execute an upshift is increased relative to operation when not in the second mode.
[0030] In an embodiment, in the second mode the vehicle is arranged to change a value of at least one operating parameter such that a speed assumed by the engine for a given amount of throttle control actuation is increased relative to operation in non-second mode.
[0031] Thus, a target engine speed of the vehicle for a given amount of throttle depression is increased when operating in the second mode.
[0032] In an embodiment, when in the second mode the vehicle is arranged to change a value of at least one operating parameter such that a stiffness of a suspension of the vehicle is increased.
[0033] The stiffness of the suspension may be increased for example by reducing a size of an aperture in a damper of the suspension. Alternatively or in addition a portion of the suspension may comprise a material or fluid the stiffness of which may be changed by changing a value of an electric or electromagnetic field applied to the material or fluid. Other arrangements are also useful.
[0034] In a further aspect of the invention there is provided a method of controlling by means of control means a motor vehicle having an engine, driver-selectable first and second modes of operation and driver-operable means for selecting the first and second modes, when the first mode is assumed the method comprising implementing a stop/start functionality in which the engine is stopped automatically and subsequently restarted during a drivecycle thereby to reduce an amount of time for which the engine is switched on over the drivecycle, when the second mode is assumed the method comprising changing a value of at least one operating parameter of the vehicle relative to vehicle operation when the vehicle is not in the second mode, when the first mode has also been selected and the driver selects the second mode the method comprising controlling the vehicle to deselect the first mode, when the driver subsequent deselects the second mode the method comprising reselecting automatically the first mode, the method further comprising when in the second mode assuming the first mode in addition to the second mode if the first mode is selected by the driver when the vehicle is in the second mode.
[0035] In an embodiment, when in the second mode and the first mode is selected whilst in the second mode, the method comprises the step of remaining in the first mode when the driver subsequently deselects the second mode.
[0036] The method may further comprise the step of controlling the vehicle to remain in the first mode if the driver selects the first mode when the vehicle is in the second mode and the driver subsequently deselects and reselects the second mode.
[0037] In one aspect of the invention there is provided a method of controlling by means of a controller a vehicle having driver-selectable eco and dynamic modes of operation and driver-operable means for selecting the eco and dynamic modes, the method comprising the step of deselecting automatically by means of the controller the eco mode when the driver selects the dynamic mode when the eco mode has also been selected, and reselecting automatically the eco mode by means of the controller if the driver subsequently deselects the dynamic mode.
[0038] Within the scope of this application it is envisaged that the various aspects, embodiments, examples and alternatives, and in particular the individual features thereof, set out in the preceding paragraphs, in the claims and/or in the following description and drawings, may be taken independently or in any combination. For example features described in connection with one embodiment are applicable to all embodiments, unless such features are incompatible.
BRIEF DESCRIPTION OF THE DRAWINGS
[0039] Embodiments of the invention will now be described, by way of example only, with reference to the accompanying figures in which:
[0040] FIG. 1 is a schematic illustration of a stop/start vehicle according to an embodiment of the present invention;
[0041] FIG. 2 is a state diagram showing states of the vehicle of FIG. 1 in respect of selection or deselection of an eco mode and a dynamic mode and a required driver control action to transition between the states;
[0042] FIG. 3 is a state diagram showing states of a vehicle in respect of selection or deselection of the eco mode and the dynamic mode and a required driver control action to transition between the states according to a further embodiment of the invention;
[0043] FIG. 4 is a state diagram showing states of a vehicle in respect of selection or deselection of the eco mode and the dynamic mode and a required driver control action to transition between the states according to a still further embodiment of the invention; and
[0044] FIG. 5 is a state diagram showing states assumed by vehicles configured according to each of the arrangements of FIG. 2 (arrangement 1 , Arr, 1 ), FIG. 3 (arrangement 2 , Arr, 2 ) and FIG. 3 (arrangement 3 , Arr, 3 ) for a set of six example scenarios.
DETAILED DESCRIPTION
[0045] FIG. 1 is a schematic illustration of a vehicle 100 according to an embodiment of the present invention.
[0046] The vehicle 100 has an internal combustion engine 121 arranged to provide torque to a driveline 5 of the vehicle by means of a transmission 123 . The driveline 5 is arranged to drive four wheels 111 , 112 , 114 , 115 of the vehicle 100 .
[0047] In some embodiments the driveline 5 may be arranged to drive only two wheels of the vehicle. In some embodiments the driveline 5 may be operable to drive either two or four wheels of the vehicle. Other numbers of wheels are also useful.
[0048] The vehicle 100 has a controller 140 arranged to control a speed of the engine 121 responsive to an input from a throttle pedal control 121 P.
[0049] The vehicle 100 is also provided with a pair of driver operated mode selectors. A first (eco mode) selector 160 is operable to select and to deselect an eco mode of operation whilst a second (dynamic mode) selector 170 is operable to select and to deselect a dynamic mode of operation. It is to be understood that the vehicle is operable in either or both of the eco and dynamic modes.
[0050] It is to be understood that the eco mode corresponds to a mode in which the vehicle operates according to a stop/start control methodology. That is, when the vehicle is held stationary by means of a brake pedal control 130 P the engine 121 is stopped thereby to reduce fuel consumption and/or an amount of undesirable gases emitted by the vehicle 100 .
[0051] In some embodiments the dynamic mode corresponds to a mode in which a gear shift map of the vehicle 100 is modified, for example by increasing the engine speed at which the transmission 123 of the vehicle 100 performs an upshift, i.e. a shift to a gear that is higher than the gear in which the vehicle 100 is currently operating, when operating in one or more gears.
[0052] In some embodiments a throttle map may also be modified, for example to cause the engine 121 to rotate at a higher speed for a given amount of throttle pedal depression.
[0053] Other arrangements are also useful. For example, other changes to one or more maps or other operating parameters of the vehicle are also useful.
[0054] It is to be understood that in vehicles not employing a map for one or more functions an alternative change may be made in order to achieve a similar change in performance of the vehicle.
[0055] Operation of the vehicle 100 will now be described with respect to selection and deselection of the eco mode (by the driver or the controller 140 ) and of the dynamic mode (by the driver).
[0056] FIG. 2 is a state flow diagram of a vehicle according to an embodiment of the invention. It is to be understood that the vehicle of FIG. 1 may be arranged to operate according to the state diagram of FIG. 2 .
[0057] The description will begin from a default state of the vehicle (state S 101 ) in which the dynamic mode is not selected (i.e. the dynamic mode is OFF) and the eco mode is selected (i.e. the eco mode is ON).
[0058] If whilst in the default state S 101 the driver deselects the eco mode by pressing the eco mode selector 160 the vehicle is arranged to transition to state S 102 in which the dynamic mode is OFF and the eco mode is OFF. If the driver subsequently selects the eco mode the vehicle returns to state S 101 in which the eco mode is ON and the dynamic mode is OFF.
[0059] If whilst in state S 102 the driver presses the dynamic mode selector 170 the vehicle transitions to state S 103 in which the dynamic mode is ON and the eco mode is OFF. If the driver then deselects the dynamic mode, the vehicle transitions back to state S 102 in which the dynamic mode and eco mode are both OFF.
[0060] If whilst in state S 103 the driver selects the eco mode, the vehicle assumes state S 104 in which the eco mode and dynamic mode are both ON. The vehicle also assumes an override condition in which condition deselection and selection of either the eco mode or the dynamic mode in any possible sequence has no effect on whether the other mode is selected or deselected.
[0061] Thus, for example, if whilst in state S 104 the driver deselects eco mode (i.e. turns eco mode OFF), the vehicle assumes state S 105 in which the dynamic mode remains ON and the eco mode is switched OFF.
[0062] Likewise, if whilst in state S 104 the driver deselects dynamic mode the vehicle assumes a state in which the dynamic mode is OFF and the eco mode is ON.
[0063] If whilst in state S 101 the driver selects the dynamic mode, the vehicle is arranged to transition to state S 106 in which the dynamic mode is ON and the eco mode is OFF. That is, when the dynamic mode is selected the vehicle automatically deselects the eco mode. Eco mode is automatically deselected on the basis that a driver selecting dynamic mode is likely to be requiring relatively rapid response to control inputs and less likely to want the engine to turn off when the vehicle is stationary, for example when waiting at traffic lights.
[0064] If the driver subsequently deselects the dynamic mode, the vehicle 100 is arranged automatically to select eco mode and the vehicle 100 assumes state S 101 of FIG. 2 . Eco mode is resumed on the basis that the driver did not deselect eco mode prior to selecting the dynamic mode.
[0065] If whilst in state S 106 the driver selects the eco mode, the vehicle 100 is arranged to assume state S 104 in which the eco mode and dynamic modes are both selected.
[0066] As noted above, once the vehicle 100 enters state S 104 in which eco mode is selected whilst in dynamic mode, the vehicle 100 assumes the override condition in which condition the deselection and selection of either the eco mode or the dynamic mode in any possible sequence has no effect on whether the other mode is selected or deselected. That is, the vehicle does not automatically select or deselect one mode responsive to the selection or deselection of another mode.
[0067] This feature has the advantage that if whilst in dynamic mode the drive selects the eco mode, the vehicle remains in eco mode until the driver deselects eco mode, regardless of how many times the driver deselects of selects dynamic mode.
[0068] In some embodiments arranged according to the state diagram of FIG. 2 the vehicle 100 is arranged to remain in the override condition until the engine 121 is shut down by the driver (and not shut down by the vehicle 100 according to the stop/start functionality).
[0069] It is to be understood that in the arrangement of FIG. 2 , when the vehicle transitions from state S 101 to state S 106 the fact that eco mode is selected when in state S 101 is stored in an eco status memory 141 M of the vehicle. If the vehicle subsequently transitions back to state S 101 from state S 106 the vehicle recalls from the eco status memory 141 M the stored status of eco mode (i.e. whether selected or deselected).
[0070] Similarly, when the vehicle transitions from state S 102 to state S 103 , the fact that eco mode is deselected when in state S 102 is stored in the eco status memory 141 M for later recall if the vehicle transitions back to state S 102 from state S 103 .
[0071] Thus it is to be understood that the vehicle is able to distinguish between states S 106 and S 103 (in both of which the dynamic mode is selected and the eco mode is deselected) by reference to the eco status memory 141 M. In the present embodiment the eco status memory 141 M is a flash memory although other memory devices are also useful.
[0072] FIG. 3 is a state diagram of the operation of a vehicle as shown in FIG. 1 according to a further embodiment of the invention.
[0073] The description will begin from a default state of the vehicle (state S 201 ) in which the dynamic mode is not selected (i.e. the dynamic mode is OFF) and the eco mode is selected (i.e. the eco mode is ON).
[0074] If whilst in state S 201 the driver deselects the eco mode, the vehicle assumes state S 202 in which the dynamic mode and eco mode are both OFF. If whilst in state S 202 the driver selects the dynamic mode the vehicle transitions to state S 203 in which the dynamic mode is ON and the eco mode is OFF. This is similar to the arrangement of FIG. 2 .
[0075] If the driver subsequently selects the eco mode the vehicle transitions to state S 204 in which the dynamic mode and eco mode are both ON.
[0076] If the driver subsequently deselects the eco mode the vehicle returns to state S 203 .
[0077] However if whilst in state S 204 the driver deselects dynamic mode, the vehicle returns to sate S 202 in which the dynamic mode and eco mode are both OFF. That is, deselection of dynamic mode by the driver also results in automatic deselection of eco mode by the vehicle.
[0078] The advantage of this feature is that the vehicle returns to the state it was in prior to selection by the driver of dynamic mode.
[0079] The fact that the driver deselected eco mode whilst not in dynamic mode suggests the driver does not desire eco functionality on the journey and therefore the vehicle transitions from state S 204 to state S 202 rather than to state S 201 .
[0080] Thus, a driver wishing to transition from state S 204 to state S 202 can do so directly and does not have to assume state S 202 via state S 201 or state S 203 . This has the advantage that the workload of the driver in driving the vehicle according to his preferred style may be decreased.
[0081] It is to be understood that if the driver subsequently selects the dynamic mode from state S 202 , the dynamic mode is assumed without also assuming the eco mode (state S 203 ).
[0082] If whilst in state S 201 the driver selects dynamic mode rather than deselecting eco mode, the vehicle assumes state S 206 in which dynamic mode is ON and eco mode is automatically deselected by the vehicle. Subsequent deselection of dynamic mode results in automatic reselection of eco mode by the vehicle.
[0083] The fact that the driver has not deselected eco mode whilst dynamic mode is not selected indicates that the driver most likely wishes to assume eco mode when not in dynamic mode.
[0084] If whilst in dynamic mode in state S 206 the driver selects eco mode, the vehicle assumes state S 207 in which eco mode and dynamic mode are both selected. If the driver subsequently deselects eco mode the vehicle returns to state S 206 whilst if the driver deselects dynamic mode when in state S 207 the vehicle returns to state S 201 .
[0085] Thus if the vehicle assumes the dynamic mode when eco mode has been selected, when dynamic mode is exited the vehicle returns to state S 201 in which the eco mode is selected. Selection and/or deselection of eco mode whilst in dynamic mode therefore has no effect on whether eco mode is selected when the dynamic mode is subsequently deselected. Rather, the vehicle recalls the fact that eco mode was already selected when dynamic mode was last selected and returns to state S 101 when dynamic mode is deselected.
[0086] It is to be understood that if the vehicle makes a transition from state S 201 to state S 206 the vehicle stores the status of the eco mode in the eco status memory 141 M of the vehicle for later recall if the vehicle transitions back to state S 201 from state S 206 or from state S 207 to state S 201 .
[0087] Similarly, if the vehicle transitions from state S 202 to state S 203 the vehicle stores the status of the eco mode in the eco status memory 141 M for later recall when the vehicle transitions from state S 203 back to state S 202 or from state S 204 back to state S 202 .
[0088] It is to be understood that the vehicle is able (by means of the eco status memory 141 M) to distinguish between states S 203 and S 206 (in both of which dynamic mode is selected and eco mode is deselected) and between states S 204 and S 207 (in both of which dynamic mode and eco mode are both selected) by reference to the eco status memory 141 M.
[0089] FIG. 4 is a state diagram of the vehicle 100 of FIG. 1 when operated according to a further embodiment of the invention.
[0090] The arrangement of FIG. 4 is similar to the arrangement of FIG. 3 and like states are provided with like reference signs prefixed numeral 3 instead of numeral 2 .
[0091] The state transitions experienced by the vehicle 100 responsive to selection/deselection of the eco and dynamic modes are similar to those of FIG. 3 with certain differences.
[0092] Of note is that state S 304 (in which dynamic mode and eco mode are both selected) only appears once on the state diagram whereas in the diagram of FIG. 3 it appears twice (S 204 and S 207 ).
[0093] Thus, in the arrangement of FIG. 4 , if when dynamic mode and eco mode are both selected the dynamic mode is deselected, the vehicle always remains in the eco mode regardless of whether eco mode was selected when dynamic mode was last selected.
[0094] In contrast, in the arrangement of FIG. 3 , if when dynamic mode and eco mode are both selected the dynamic mode is deselected, the state assumed by the vehicle depends on the order in which dynamic mode and eco mode were selected by the driver starting at default state S 201 .
[0095] Thus, in the arrangement of FIG. 4 , the fact that the driver has selected eco mode whilst in dynamic mode is taken to indicate that the driver most likely wishes to remain in eco mode when dynamic mode is deselected.
[0096] Secondly, in state S 303 in which the dynamic mode is ON and eco mode is OFF, if the dynamic mode is deselected the eco mode remains deselected regardless of the history of selection of eco mode and dynamic mode.
[0097] This is because in order to arrive at state S 303 from default state S 301 , the driver is required to have deselected eco mode either when the dynamic mode was OFF or when dynamic mode was ON.
[0098] The fact that the driver has specifically deselected eco mode is taken to suggest the driver would not wish to return to eco mode when dynamic mode is deselected.
[0099] Thus, selection of dynamic mode when in eco mode and subsequent deselection of dynamic mode results in a return to eco mode unless eco mode is specifically deselected by the driver whilst in dynamic mode, in which case unless eco mode is specifically reselected whilst in dynamic mode, the eco mode remains deselected when dynamic mode is subsequently deselected.
[0100] It is to be understood that other arrangements are also useful.
[0101] In the arrangement of FIG. 4 , it is to be understood that when the vehicle transitions from state S 301 to state S 306 , the eco mode status is stored in the eco status memory 141 M for later recall if the vehicle transitions back from state S 306 to state S 301 .
[0102] Similarly, when the vehicle transitions from state S 302 to state S 303 , the eco mode status is stored in the eco status memory 141 M for later recall if the vehicle transitions back from state S 303 to S 302 .
[0103] However, if the vehicle transitions from state S 303 to state S 304 by selecting the eco mode, if the dynamic mode is deselected whilst in state S 304 the vehicle remains in the eco mode.
[0104] Thus, in some embodiments if the eco mode is selected when in state S 303 , the eco mode status stored in the eco status memory 141 M is reversed such that if the dynamic mode is subsequently deselected whilst in state S 304 the eco mode remains selected,
[0105] Conversely, if whilst in state S 304 the eco mode is deselected, in some embodiments the eco mode status stored in the eco status memory 141 is reversed such that if the dynamic mode is subsequently deselected whilst in state S 303 the eco mode remains deselected.
[0106] As noted above, FIG. 5 is a state diagram showing states assumed by the vehicle according to each of the arrangements of FIG. 2 (arrangement 1 , Arr, 1 ), FIG. 3 (arrangement 2 , Arr, 2 ) and FIG. 4 (arrangement 3 , Arr, 3 ) for a set of six example scenarios in which a driver makes a series of selections and deselections of the eco and dynamic modes.
[0107] In each case, the state circled with a dashed line is a state in which the eco mode is stored in the eco status memory 141 M of the vehicle for later recall when the vehicle assumes the state circled by a solid line. That is, the eco mode assumed in the state circled with the dashed line is resumed in the state circled with a solid line.
[0108] It is to be understood that whilst some embodiments of the invention have been described wherein the vehicle is operable in an eco mode (or ‘stop/start’ mode) and a second mode (which may be a ‘dynamic’ or ‘sports’ mode), the second mode may in some embodiments correspond to a mode in which a selected one of a plurality of special vehicle programs are executed. The special vehicle programs may be arranged to control the vehicle according to a methodology, protocol or the like in order to optimise vehicle performance in a given situation. For example one program may optimise vehicle operating parameters for off-road driving, another may optimise vehicle parameters for driving at high speeds whilst turning, another may optimise vehicle parameters for driving on an icy surface and so forth.
[0109] Embodiments of the invention include hybrid electric vehicles, conventional stop/start vehicles and any other suitable type of motor vehicle.
[0110] Throughout the description and claims of this specification, the words “comprise” and “contain” and variations of the words, for example “comprising” and “comprises”, means “including but not limited to”, and is not intended to (and does not) exclude other moieties, additives, components, integers or steps.
[0111] Throughout the description and claims of this specification, the singular encompasses the plural unless the context otherwise requires. In particular, where the indefinite article is used, the specification is to be understood as contemplating plurality as well as singularity, unless the context requires otherwise.
[0112] Features, integers, characteristics, compounds, chemical moieties or groups described in conjunction with a particular aspect, embodiment or example of the invention are to be understood to be applicable to any other aspect, embodiment or example described herein unless incompatible therewith.
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The present invention provides a motor vehicle having driver-selectable first and second modes (eco, dynamic) of operation and driver-operable means for selecting the first and second modes. Driver selection of the second mode (dynamic) when the first mode (eco) has also been selected causes the vehicle to deselect the first mode (eco), subsequent deselection by the driver of the second mode (dynamic) causing the first mode (eco) to be reselected automatically by the vehicle. If the first mode (eco) is selected by the driver when the vehicle is in the second mode (dynamic), the vehicle selects the first mode (eco) in addition to the second mode (dynamic). A further aspect is directed to a method.
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FIELD OF THE INVENTION
The present invention relates to transmissions and more particularly, to speed reducers for use in the power train of a motor grader.
BACKGROUND OF THE INVENTION
Motor graders are principally designed to be used in road building, however, due to their large size and stability, they have been adapted for other uses such as bank grading, pavements planning, brush cutting and snow blowing.
As one can appreciate, a grader loses power with age, due to wear, and no longer functions at maximum performance. This drop in power is particularly noticeable at lower engine r.p.m. and the operators tend to compensate for this reduction in power by increasing the engine r.p.m.'s and riding the clutch to avoid stalling the engine.
Although older graders may not be as versatile as new machines, they still find spot duty doing many of the lighter jobs such as light roadgrading, snow removal etc. In most cases the loss of power could be overcome by rebuilding the engine, however, this is normally not a feasible solution as other components of the grader have also worn and the reliability of the grader would not justify this investment. A number of accessories such as snow blowers, pavement planners and pavement rippers are available for a grader, however, the grader must be capable of operating at low vehicle ground speed and hence, low r.p.m.'s which is not always possible, as the power output is low at these engine r.p.m.'s causing the engine to stall when the load is applied.
The present invention overcomes this problem by introducing a speed reducer in the power train of the motor grader, such that the grader can operate at these reduced ground speeds while providing the required torque. When these characteristics are not required, the speed reducer may be disengaged returning the drive train to its original status. The device is particularly useful as the normal transmission ratios may be used for light functions and the speed reducer may be engaged when low ground speed, high torque functions are required. For example, the speed reducer would not be used when the grader is travelling to the job site, however, when on site the speed reducer would be engaged allowing the grader to fulfill the desired function.
SUMMARY OF THE INVENTION
The specification of the present invention discloses a speed reducer or multiplier comprising an input shaft, an output shaft, a planetary gear system and a movable power transfer member adapted to selectively engage either the input shaft and the output shaft whereby the planetary system freely rotates, or the output shaft and the planetary gear system. The arrangement is such that the engagement of said transfer member with the planetary gear system causes the engagement of the input shaft and the planetary gear system thereby changing the speed of the output shaft relative to the input shaft. The engagement of the transfer member with the input shaft causes the disengagement of the input shaft and the planetary system thus providing a non engaged free planetary system.
The speed reducer according to this design uses a moving transfer member which causes the planetary system to be disengaged or engaged at two points. Because of this arrangement, the planetary system is allowed to freewheel when not engaged thereby, reducing wear and reducing the power consumed.
The speed reducer allows an older motor grader to be modified increasing the range of ground speeds in which the grader can operate, thus increasing the versatility and useful life of the grader.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiments of the invention are shown in the drawings wherein:
FIG. 1 is a perspective view of the speed reducer with a portion thereof, cut away;
FIG. 2 is a cross-sectional view taken through the length of the speed reducer when the planetary system is not engaged; and
FIG. 3 is a cross-section taken through the speed reducer when the planetary system is engaged.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
As can be seen in FIG. 1, the speed reducer has an input shaft 1, an output shaft 2, a sliding power input member 3, a sun gear 4, planetary gears 5, a stationary ring gear 6, planetary gear frame member 8, power transfer member 10, power output gear 12 and shifting mechanism 14.
The casing 20 of the speed reducer has been provided with bearings 21 for supporting and positioning the input shaft 1. The power input gear 3, the sun gear 4, and planetary gear supporting structure 22 are all carried on the input shaft 1. The sun gear and the support structure 22 are bearingly supported on this shaft whereas, the power input gear 3 is splined to the input shaft such that it can slide in the axial direction of the shaft but cannot rotate on the shaft.
In the positions shown in FIGS. 1 and 3, the planetary gear system is coupled to the input and output shafts, thereby activating the speed reducer. In this position the power transfer member 10 has been moved forward and is meshing with gear 9 which is secured to the frame 8. The frame member 8 is connected and driven by the axes of the planetary gears. The power transfer member is engaging the power output gear 12 which will be the case regardless of whether the speed reducer is activated or the power is being directly transmitted through the speed reducer.
Due to the position of the power transfer member 10, the power input member 3 has been moved forward on the input shaft 1 such that gear 34 meshes with ring gear 30 which is fixed to the sun gear 4. As shown in the figures the power input members 3 has two gears, 32 and 34 of different diameters. Only one of these gears will be engaged at any one time, gear 34 transmitting power from the input shaft to the planetary gear system and gear 32 transmitting power through the transfer member 10 to the output gear 12.
As shown in FIGS. 2 and 3 a plate member 100 has been secured to the rear face of input member 3 enabling the power transfer member 10 to position the input member of the splined input shaft. When member 10 is moved from the direct drive position shown in FIG. 2 to the planetary gear system shown in FIG. 3 the gear teeth 11 of the transfer member 10 strike the plate member 100 forcing the input member 3 to slide on the input shaft activating the reducer by engaging gears 30 and 34 and disengaging the power transfer member 10 and gear 32. The system is returned to the direct drive position of FIG. 2 by moving the power transfer member in the opposite direction allowing gear teeth 13 to abut the plate member 100, moving the input member disengaging gears 30 and 34 and engaging gear 32 with the power transfer member.
The transfer member 10 comprises two coaxial ring gear portions 41 and 42 having gear teeth 11 and 13 respectively. Separating the ring gear portions is an annular sleeve 43 having a diameter greater than outer diameter of gear 32 and having an axial length greater than the thickness of the teeth of this gear, such that gear 32 may turn within the annular sleeve when not engaged.
The ring gear portion 42 is adapted to mesh with either input gear 32 or gear 9 secured to the frame member 8; gear 32 and gear 9 being of equal diameter.
As shown in FIGS. 1 and 3, the transfer member 10 has been moved forward, forcing gear 34 of the power input member to mesh with the planetary system. In this mode, power transferred from the input shaft to the planetary system via gears 30 and 34, to the power transfer member via gear 9 and subsequently to the output shaft.
In FIG. 2, the speed reducer is not activated and power is being directly transmitted to the output shaft 2. The transfer member 10 has been moved by the shift mechanism 14 such that the transfer member is no longer meshing with gear 9 and has now engaged gear 32 of the power input member 3. The movement of the transfer 10 has also caused the power input member 3 to move a similar axial direction, disengaging ring gear 30 and gear 34 of the power input member. Power is now transmitted from the input shaft to the transfer member 10 via gear 32 and subsequently to the output shaft.
Ring gear 30 and gear 9 of the frame member 8 have been disengaged thereby freeing the planetary gear system. It is only through this double disengagement caused by the movement of the power transfer member 10 and the subsequent movement of the power input member 3 combined with the sun gear bearingly supported on the input shaft that the planetary gear system may be isolated and not driven with the input shaft.
As can be appreciated, all functions do not require this higher torque for a given speed, and thus the operator must be capable of selectively engaging the speed reducer. With double disengagement, the planetary system is completely free to rotate, however, due to the friction within the system the planetary gear system will have little movement when not engaged.
Functions which require these improved torque characteristics at low speed, are often seasonal and therefore, there is no need to have the planetary system driven when the speed reducer is not activated, as power consumption and wear would increase.
The torque available at a given ground speed is increased due to the transmission of forces within the gear system as well as due to the power characteristics of the engine. The speed reducer allows the engine to operate at higher r.p.m.'s for a given ground speed and more power is available as engine speed initially increases. Therefore more power and torque is available due to the characteristics of the engine and speed reducer. The increased engine speed also allows other equipment of the grader such as the heater to function properly which would not be the case if engine speed was low. Thus the speed reducer allows the engine to operate within its normal speed range while allowing the ground speed to be reduced for speciality jobs. It is normally anticipated that a speed reduction of approximately 3 to 1 will operate satisfactorily however, other reduction ratios are also possible. A torque arm (not shown) is secured to the casing of the speed reducer and secured to the grader locking the casing against rotation.
The transfer member 10 is positioned by the shifting mechanism 14 comprising a shifting fork 17 secured to connecting rod 19. The transfer member 10 has an outwardly facing annular groove for insertion of fork 17. The connecting rod will be controlled from the cab of the grader through a linkage mechanism allowing the operator to activate the system. The annular groove and shifting fork 17 provide a suitable connecting means allowing the transfer member to rotate while also allowing the fork member to be fixed with respect to rotation.
In its present application, the speed reducer will normally be positioned between the output of the engine and the transmission of the grader and therefore, the output shaft 2 has been adapted with a splined free end for direct engagement in the transmission of the grader. It is also noted that to avoid extensive modification costs the reducer has been designed to be as small as possible and only requires a gap of approximately 10 inches for insertion.
In adapting the motor grader, the drive shaft from the engine is shortened or replaced and the output shaft of the reducer directly inserted in the transmission. Therefore, the present system results in a very compact, speed reducer which can be quickly inserted in the power train of a motor grader without encountering major modification problems and excessive downtimes.
Because of the unique design of the system the speed reducer can be activated when required and at other times, will not be driven as the planetary system has been completely disengaged from the input and output shafts. Thus the present system is highly reliable and can improve the versatility of graders to allow them to satisfy the specialty functions required of them. This is particularly true of older motor graders which can now be adapted to fulfill these specialty functions in a more efficient manner.
The present invention has been described in relation to one particular application of the device, as a speed reducer in a motor grader, however, the invention could also be used as a speed multiplier if so desired. If used as a multiplier the improved torque characteristics would not be present although the double disengagement would still allow the planetary system to free wheel when not activated.
Although various embodiments of the invention have been described herein, in great detail, it will be appreciated by those skilled in the art that variations may be made thereto, without departing from the spirit of the invention or the scope of the appended claims.
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The present invention discloses a speed reducer or multiplier for use in a motor grader. The unique structure of the reducer allows the device to be easily inserted in the drive train of a grader and thereby improve the feasible ground speeds at which the grader can operate satisfactorily. The structure further allows the speed of the planetary reduction system to remain idle when not in use. Thereby increasing the efficiency and decreasing problems such as wear. This is accomplished by a shifting mechanism which causes at least two gears to be engaged or disengaged.
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FIELD OF THE INVENTION
[0001] This invention relates to heat exchangers and more particularly to combination-type heat exchangers wherein heat exchangers for two or more fluids share a common manifold or header, and in more particular applications, to such heat exchangers as used in vehicular systems, such as automobiles, buses, trucks, etc.
BACKGROUND OF THE INVENTION
[0002] It is known to form a so-called “combination” or “combo” type heat exchanger by including one or more baffles in each of the manifolds or headers of the heat exchanger to divide the interiors of each of the headers into at least a first section for a first working fluid and a second section for a second working fluid with each of the working fluids being directed through the respective heat exchange tubes that are connected to the respective sections of the common manifolds. While such constructions may be suitable for their intended purposes, problems can arise when there are large temperature differentials between the different working fluids in each section of the shared manifold, particularly for constructions where the cores or tubes for each of the working fluids are assembled in the same plane, such as, for example, in parallel flow constructions. Accordingly, there is a continued need for improvement in combo heat exchangers.
SUMMARY OF THE INVENTION
[0003] The invention reduces the strain on heat exchanger core tubes by sectioning or partially sectioning one or both common headers in a combination type heat exchanger. The invention also allows the heat exchanger to be assembled using conventional methods. The invention provides for the possibilities of cutting the headers during or after core assembly, or after brazing. Cutting can be accomplished by various methods such as sawing or punching.
[0004] The option of partially sectioning or cutting the header allows the heat exchanger to be installed intact into a system, and have the header sections break apart during thermal events in the vehicle. Also, partially cutting the headers can be done prior to cores assembly, and the final cutting can be done during or after core assembly.
[0005] In accordance with one form of the invention, a multi-fluid heat exchanger is provided for transferring heat between a first fluid and a common fluid in one part of the heat exchanger and between the second fluid and a common fluid in a second part of the heat exchanger. The heat exchanger includes first and second elongated header pipes, first and second core sections, and a pair of baffles in the first header pipe. The first elongated header pipe has a plurality tube receiving opening spaced along a length of the first header pipe. The second elongate header pipe has a plurality of tube receiving openings spaced along a length of the second header pipe. The first core section includes a plurality of parallel, spaced tubes, each of the tubes having a first end and a second end, with the first end received in a corresponding one of the tube receiving openings of the first header pipe and the second end received in a corresponding one of the tube receiving openings of the second header pipe to direct the first fluid between the first and second header pipes through an interior of the tube. The second core section comprising a plurality of parallel, spaced tubes, each of the tubes having a first end and a second end, with the first end received in a corresponding one of the tube receiving openings of the first header pipe and the second end received in a corresponding one of the tube receiving openings of the second header pipe to direct the second fluid between the first and second header pipes through an interior of the tube. The second core is spaced from the first core along the lengths of the first and second header pipes. The pair of baffles are located in the first header pipe at a location between the first and second cores to divide an interior of the first header pipe into a first fluid manifold for the first fluid and a second fluid manifold for the second fluid. The first header pipe includes a cut portion located between the pair of baffles, the cut portion having at least a majority of a transverse cross section of the header pipe removed in comparison to the immediately adjacent transverse cross sections of the first header pipe.
[0006] In one feature, the cut portion is sized so that any remaining part of the transverse cross section of the first header pipe at the cut portion is severed under thermal cycling of the heat exchanger during operation of the heat exchanger.
[0007] As one feature, all of the transverse cross section of the first header pipe has been removed in the cut portion, so that the first header pipe is separated into two unconnected pieces.
[0008] In accordance with one feature, one of the tube openings of the first header pipe is located at the cut portion.
[0009] In a further feature, the one of the tube openings of the first header pipe doe not have a tube end received therein.
[0010] According to a further feature, the cut portion is defined by at least one saw cut extending through a portion of the header pipe outside of the one of the tube openings.
[0011] As a further feature, the cut portion is defined by a saw cut extending through a side of the header pipe immediately opposite from the one of the tube openings.
[0012] In accordance with a further feature, the cut portion is defined by a saw cut extending through the one of the tube openings.
[0013] In one feature, the cut portion is defined by a pair of saw cuts extending through opposite respective sides of the first header pipe.
[0014] According to one feature, the cut portion is characterized by the absence of any of the tube openings.
[0015] In one feature, there is a serpentine fin extending between the first and second cores and connected to both the first and second cores.
[0016] As one feature, the heat exchanger includes another pair of baffles located in the second header pipe at a location between the first and second cores to divide an interior of the second header pipe into a first fluid manifold for the first fluid and a second fluid manifold for the second fluid, the second header pipe including a second cut portion located between the another pair of baffles, the second cut portion having at least a majority of a transverse cross section of the header pipe is removed in comparison to the immediately adjacent transverse cross sections of the first header pipe.
[0017] In accordance with one feature of the invention, a method is provided for making a multi-fluid heat exchanger for transferring heat between a first fluid and a common fluid in one part of the heat exchanger and between a second fluid and the common fluid in a second part of the heat exchanger. The method includes the steps of:
[0018] a) providing a heat exchanger with first and second parallel flow core sections extending between a pair of elongated header tubes, with each of the tubes having a first fluid manifold for the first core section and a second fluid for the second core section;
[0019] b) providing a cut portion in one of the elongated headers at a location between the first and second manifolds, the cut portion having at least part of the header connecting the first and second manifolds of the header;
[0020] c) thermal cycling the heat exchanger to severe the at least part of the one of the elongated headers so that the first and second manifolds of the header are no longer connected at the cut portion.
[0021] As one feature, step b) includes providing the cut portion after the first and second core seconds are assembled and brazed together with the pair of elongated headers.
[0022] As another feature, step b) includes providing the cut portion before the first and second core seconds are assembled and brazed together with the pair of elongated headers.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] FIGS. 1-5B are views of a combo heat exchanger including a thermal relief mechanism embodying the present invention; and
[0024] FIGS. 6A-11C are views of alternate embodiments of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0025] FIG. 1 shows a portion of a combination cooler embodying a multi-fluid heat exchanger of the present invention. The combo cooler 10 includes a common manifold or header 12 in the form of an essentially cylindrical tube that has pierced tube slots 14 to receive the flattened heat exchanger tubes 16 and 18 , respectively, that direct their respective first and second heat exchange fluids through the combo heat exchanger 10 so that heat can be transferred between the first and second working fluids to a third fluid, typically air, that flows over the exterior of the tubes 16 , 18 and passes through a plurality of serpentine fins 20 that are positioned between adjacent pairs of the tubes 16 and 18 . The manifold 12 includes a first section 22 for the first fluid and a second section 24 for the second fluid, with the first and second sections being separated by a pair of baffles 26 and 28 that have been inserted through cut baffle slots 30 in the manifold 12 and brazed in place during the common brazing operation that brazes all of the tubes 16 , 18 , fins 20 , and headers 12 together. A saw cut 32 is located between the baffles 26 and 28 at the location of a pierced tube slot 14 A. The cut 32 is created after the remainder of the heat exchanger 10 has been assembled and brazed together. This saw cut 32 is further illustrated in FIGS. 5A and 5B , and the full heat exchanger is shown in FIGS. 2-4 . As best seen in FIG. 2 , in some applications it may be desirable to include the saw cut 32 in only one of the headers 12 .
[0026] FIGS. 6A-6B , 7 A- 7 B, 8 A- 8 B, 9 A- 9 B, 10 A- 10 B, and 11 A- 11 C show alternate embodiments to the saw cut of FIGS. 1-5B .
[0027] More specifically, FIGS. 6A and 6B show an alternate embodiment wherein a partial saw cut 34 extends from the side of the manifold 12 opposite the tube slots 14 so as to leave a pair of connection tabs 36 that extend between the tube slot 14 A and the saw cut 34 .
[0028] FIGS. 7A and 7B show an alternate embodiment wherein a partial saw cut 38 is made on the same side of the manifold as the tube slots 14 A so as to leave a circumferential connection tab 40 on the side of the manifold 12 opposite from the tube slots 14 .
[0029] FIGS. 8A and 8B show an optional embodiment wherein the manifold 12 includes a pair of saw cuts 42 and 44 that are made on each side of the manifold adjacent the pierced tube slot 14 A and extend all the way into the slot 14 A so as to remove all of the material except for a circumferential connecting tab 46 on the opposite side of the manifold 12 from the tube slots 14 .
[0030] FIGS. 9A and 9B show an optional embodiment wherein the manifold 12 does not include a pierced tube slot 14 A at the location between the baffles 26 and 28 , but does include a baffle slot 48 that is of the same type as the slots 30 used for the baffles 26 and 28 , and which leaves a pair of connection tabs 50 on each side of the manifold 12 .
[0031] FIGS. 10A and 10B show an alternate embodiment similar to that of FIGS. 9A and 9B , but where the manifold 12 does include a pierced tube slot 14 A at the location of the cut baffle slot 48 .
[0032] FIGS. 11A, 11B and 11 C show yet another alternate embodiment wherein the manifold 12 includes a pierced tube slots 14 A and has saw cuts 52 on each side similar to the embodiment of FIGS. 8A and 8B , but the saw cuts 52 do not extend into the tube slot 14 A, thereby leaving the connection tab 46 and a pair of side tabs 54 .
[0033] For each of the foregoing embodiments that include one or more connection tabs, the heat exchanger 10 can be installed intact, i.e., with the first and second sections 22 and 24 connected together by the connection tabs, and then the header sections 22 and 24 can be separated during operation by thermal stresses that result in the structural failure of the connection tabs.
[0034] It should be appreciated that the tubes 16 , and preferably the associated fins 20 , define a core section 60 for the cooler 10 , and the tubes 18 , and preferably the associated fins 20 , define another core section 62 of the combo cooler 10 . It should also be appreciated that the saw cuts 32 , 34 , 38 , 42 , 44 , 52 and cut baffles slots 48 of each of the foregoing embodiments define a cut portion 64 in the corresponding manifold of the embodiment that is located between the pair of baffles 26 and 28 . It can also be seen in the figures that, for each of the previously described embodiments, at least a majority of the transverse cross section of the header 12 has been removed at the cut portion 64 in comparison to the immediately adjacent transverse cross sections of the header 12 .
[0035] While the above embodiments have been shown for a combination cooler wherein the common manifold has only first and second sections, the invention may prove useful in applications wherein there are more than two sections in the common manifold 12 and therefore more than two of the saw cuts 32 , or the alternate embodiments thereto, in each of the manifolds 12 .
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A multi-fluid heat exchanger and a method of making the same are provided wherein a cut portion is provided in an elongated header of the heat exchanger at a location between a pair of baffles in the elongated header and first and second cores of the heat exchanger. At least a majority of the transverse cross section of the elongated header is removed at the cut portion to allow for relative thermal growth of the first and second cores.
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CROSS REFERENCE TO RELATED APPLICATIONS
This Application claims the right of priority based on Taiwan Patent Application No. 93120116 entitled “AN ELECTRONIC APPARATUS HAVING A SHOCK ABSORBER” filed on Jul. 5, 2004, which is incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to an electronic apparatus having a vibration absorber, and more particularly, to a vibration absorber having a plurality of deformation spaces.
BACKGROUND OF THE INVENTION
Mechanical vibrations are commonly generated from the electronic components in most electronic apparatuses, for example, computers or projectors with cooling fans, or recorder players, CD players or DVD players having motors used to rotate tapes or spin disks. Those undesirable mechanical vibrations propagating within the apparatuses generally turn into the sources of noises. Some of the vibrations become the electronic noises interfering with the intended operations of the apparatuses while some others are converted into undesirable sounds that make the users annoyed.
In order to weaken undesirable mechanical vibrations, the electronic devices are conventionally wrapped or padded with elastic materials, such as rubbers or corks, to absorb some of the vibrations and convert them into heat. However, such a traditional approach has gradually lost its advantages, as the trend of reducing size in electronic devices is ongoing. The smaller the electronic devices are, the more sensitive to any slight vibrations they become. Accordingly, there is a need to provide a more advantageous technology for reducing such vibrations effectively so as to fabricate more desirable electronic apparatuses.
SUMMARY OF THE INVENTION
The present invention provides an electronic apparatus including a housing, an electronic device generating vibrations during operations, and a vibration absorber. The vibration absorber, having a cavity and a plurality of deformation spaces, is positioned in the housing, wherein the cavity is inserted with the electronic device so as to reduce the vibrations and prevent the housing from the vibrations.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows an internal structure of an electronic apparatus in accordance with the present invention.
FIG. 2A shows a vibration absorber and a cooling fan before assembling in accordance with the present invention.
FIG. 2B shows a vibration absorber assembled with a cooling fan in accordance with the present invention.
FIG. 3 perspectively shows a vibration absorber in accordance with the present invention.
FIGS. 4A and 4B show a vibration absorber in front and rear views respectively in accordance with the present invention.
DETAILED DESCRIPTION
In accordance with the present invention, the electronic apparatus and the electronic device are respectively described and illustrated by way of a projector and a cooling fan, resulted from certain of the preferred embodiments. As shown in FIG. 1 , the projector 100 includes a housing 120 , a vibration absorber 160 positioned in the housing 120 , and a cooling fan 140 embedded into the vibration absorber 160 .
As shown in FIGS. 2A-2B , the vibration absorber 160 includes a cavity 161 formed for fitting the contour 141 of the cooling fan 140 inserted thereinto. The vibration absorber 160 is made of elastic materials such as silicon rubber, polyurethane, and poly vinyl chloride etc., in which the silicon rubber exhibiting hardness of greater than 35 Shore is preferred. However, because merely using the elastic materials for absorbing vibrations is insufficient as the above described, the vibration absorber 160 of the present invention additionally provides a plurality of deformation spaces 162 in order to reduce the vibrations effectively and prevent the housing 120 from them as well as keeping other devices, also connected with the housing 120 in the electronic apparatus, unaffected thereby. The vibration absorber 160 specifically includes a blocking device 163 formed on the bottom portion of the cavity 161 , used to avoid the cooling fan 140 from disengaging the vibration absorber 160 during operations. The blocking device 163 further includes an air outlet 168 for discharging air through the cooling fan 140 .
The plurality of deformation spaces 162 are particularly described as below. As shown in FIG. 3 , the vibration absorber 160 has a outer layer 164 , an inner layer 165 (i.e. the wall of the cavity 161 ), and a plurality of linking slices 166 , wherein each of the plurality of linking slices 166 is crossed to each other and connected with the outer layer 164 and the inner layer 165 , so as to create a plurality of deformation spaces 162 between the outer layer 164 and the inner layer 165 .
FIGS. 4A and 4B showing the vibration absorber 160 in a front and rear views respectively according to one embodiment of the present invention are intended to demonstrate that, each deformation space 162 is an open-ended channel, i.e. each opening of the deformation space 162 a in FIG. 4A has its corresponding opening of the same deformation space 162 b as indicated in FIG. 4B . Furthermore, the openings 162 a / 162 b are polygonal-shaped and distributed in the vibration absorber 160 to form a net configuration, thereby creating a firm structure for holding the electronic device (i.e. the cooling fan 140 ) as well as absorbing vibrations effectively.
The present invention has been described above with reference to preferred embodiments. However, those skilled in the art can understand that the scope of the present invention need not be limited to the disclosed preferred embodiments. On the contrary, it is intended to cover various modifications and equivalent arrangements within the scope defined in the following appended claims. The scope of the claims should be accorded the broadest interpretation so as to encompass all such modifications and equivalent arrangements.
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An optical access apparatus is provided. The optical access apparatus includes a mounting plate, characterized in that the mounting plate has a bent portion acting as a balance plate of the optical access apparatus.
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BACKGROUND OF THE INVENTION
[0001] A bed quilt 8 (see FIGS. 1 - 5 ) is commonly comprised of a mat of batting 10 or insulating fill material sandwiched between top and bottom fabric panels 11 t , 11 b that are stitched together by peripheral seams along the four edges (head seam 13 h, foot seam 13 f and two side seams 13 s ), and by pattern seams 14 across the panels (and batting) inwardly of the peripheral seams. Most quilts are rectangular in shape, having the side seams 13 s substantially parallel to one another and having the head and foot seams 13 h, 13 f substantially parallel to one another and substantially perpendicular to the side seams.
[0002] In forming the quilt, the panels 11 t , 11 b initially are laid with the outside faces against one another and are stitched together inside-out around three adjacent edge seams (see FIG. 3, typically the two side seams 13 s and the foot seam 13 f ). This defines a three-sided bag “B” having the fourth head edge 12 open. A fill machine 16 , commonly used to fill the bag, would have a tubular horn 15 elongated to almost the inside width of the open bag and a ram 17 sized to fit through the horn and completely into the bag. Two operators (not shown), standing on opposite ends of the horn would together fit the open bag onto the horn 15 , bunching up thereon the yet inside-out panels until the foot seam 13 f is aligned over an inlet opening of the horn. The ram 17 with batting 10 lying thereon would then be advanced against the stitched edge seam 13 f and through the horn, operable to unfurl the panels 11 t , 11 b through the horn and draw them right-side out and around the batting 10 . After the ram 17 is withdrawn, the now filled bag “B” is lying flat on the fill machine table 18 with the final or fourth edge 12 open toward and somewhat proximate the horn outlet opening.
[0003] The final or open fourth bag edge 12 would then have to be stitched closed along the seam 13 h. Heretofore, a skilled operator had to complete such stitching using a sewing machine, but this procedure has proved to be difficult and costly. For example, (1) the filled bag “B” had to be manually transferred to the sewing machine operator; who (2) then manually had to fold the separate end edges of the open bag panels inwardly along straight corners 20 as short flaps 21 , and (3) had to position the flaps flush against one another, with the flap corners lined up straight and even to define what many call a French Hemm flap configuration; but (4) the operator, starting at one side edge seam 13 s, would have to repeatedly fold and stitch only short lengths of the panel edges at a time, progressively folding additional lengths of the panel flaps 21 (possibly 5-10 inches at a time and just before being stitched at the sewing machine; and (5) all the while trying to keep the closure seam 13 h uniform and straight for yielding an acceptable guilt.
OBJECTS AND SUMMARY OF THE INVENTION
[0004] An object of this invention is to provide a machine and method for closing and stitching closed, in an in-folded flap configuration, the final open or fourth edge of a filled quilt bag or cover, virtually automatically once the bag fill machine operators have transferred the opened bag edge onto the machine.
[0005] A more specific object of this invention is to provide a machine and method for accurately forming an in-folded flap configuration or hemm simultaneously along the entire length of the final open bag edge, by: folding the in-folded flaps along only a short length of the open bag edge across and inwardly from each of the bag side seams, positioning the in-folded flaps over respective spaced separator members with the side seams overlying the separator members, and moving the separator members apart until the bag edges are drawn tight causing said folded flaps to be extended over the remaining intermediate portions of the bag edge, continuously between adjacent side seams of the bag.
[0006] A further object of this invention is to provide a machine and method for moving such folded but yet opened bag edge into operative association with an automatic sewing machine, and for moving the bag and sewing machine relative to one another along the final opened bag edges for first clearing away exposed fill or batting material and then for stitching the opened edges closed, all without operator assistance.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] [0007]FIG. 1 is a perspective view of a finished quilt:
[0008] [0008]FIG. 2 is a perspective view of a filled quilt bag or cover yet having its fourth edge open and unstitched;
[0009] [0009]FIG. 3 is a sectional view of stitched quilt bag panels when inside-out and before being filled with the batting;
[0010] [0010]FIGS. 4 and 5 are enlarged sectional views of the fourth edge of a filled quilt bag,
[0011] [0011]FIG. 4 showing the fourth edge folded in the French Hemm configuration, but unstitched; and
[0012] [0012]FIG. 5 showing the fourth edge stitched closed;
[0013] [0013]FIG. 6 is a sectional view of the fill machine horn with the inside-out stitched quilt panels bunched up thereon, and with the machine ram and a mat of fill batting thereon each positioned for movement against the panels and passage through the horn;
[0014] [0014]FIG. 7 is a side elevational view of the inventive machine operatively overlying the fill machine table and extending to be operatively proximate the sewing machine;
[0015] [0015]FIG. 8 is top view of the machine of FIG. 7;
[0016] [0016]FIGS. 9A and 9B are elevational views of the machine as seen from the right in FIG. 7, except without the fill machine table, and further with the machine being set in FIG. 9A to accommodate a large quilt and FIG. 9B to accommodate a smaller quilt;
[0017] [0017]FIG. 10 is an enlarged side elevational view of part of the machine illustrated in FIG. 7;
[0018] [0018]FIG. 11 is an elevational view of the left quilt bag gripping assembly, as seen generally from line 11 - 11 in FIG. 10, except showing the clamp arm opened;
[0019] [0019]FIG. 12A is a top view of the quilt bag gripping assembly, such as might be seen generally from line 12 - 12 in FIG. 10, showing the adjacent separator members positioned operatively parallel and the clamp closed;
[0020] [0020]FIG. 12B is a top view of the left side quilt bag gripping assembly, except showing only the small separator member in the operative position and the clamp opened;
[0021] [0021]FIGS. 13A and 13B are enlarged elevational views showing the guilt bag panel edges having in-folded flaps lying against and drawn tightly over the separator members, as in the operative positions of FIGS. 12A and 12B respectively;
[0022] [0022]FIG. 14A is an enlarged elevational view of part of the machine of FIG. 7, except having the transfer mechanism shifted to be in operative association with the sewing machine, and showing the guilt bag guide retracted from operative association with the quilt bag held on the transfer mechanism;
[0023] [0023]FIG. 14B is an elevational similar to FIG. 14A, except having the guilt bag guide shifted to be in operative association with the quilt bag held on the transfer mechanism;
[0024] [0024]FIG. 15 is an enlarged elevational view of the quilt bag guide of FIG. 14B, shown in operative association with the quilt bag illustrated in phantom; and
[0025] [0025]FIG. 16 is an enlarged elevational view of the quilt bag guide shown in operative association with the sewing machine, with the quilt bag illustrated in phantom.
DETAILED DESCRIPTION OF THE INVENTION
[0026] The illustrated machine 23 (see FIGS. 7, 8) has a frame 24 that supports and accommodates the different reciprocating movements of transfer mechanism 25 and automatic sewing machine 26 . Thus, frame beams 27 via bearing/guide means 28 , central beam 43 and linear actuator 48 provide for movement of the transfer mechanism 25 between a quilt bag Loading position (in FIGS. 7, 8, 10 ) overlying the fill machine table 18 (where a filled but open quilt bag “B” ready for closing would lay) and a stitching position operatively proximate the sewing machine 26 . Frame beams 29 support via bearing guide means 30 the sewing machine platform 31 for sewing machine movement for stitching the bag closing seam 13 h. The frame beams 27 , 29 lie transverse or even normal to one another, so that the transfer mechanism and sewing machine will move in like manner relative to one another.
[0027] The transfer mechanism 25 (see FIGS. 10, 11, 12 A, 12 B, 13 A, 13 B) includes a clamp and stretch assembly 32 comprised of spaced pairs of support arms 33 and separator members 34 , 35 ; spaced pairs of clamp ledges 36 and arms 37 closed by actuators 38 moving the clamp arms about axes 39 ; and telescoping cross bars 40 spanning the width of the assembly. The assembly 32 is carried near its opposite ends to the opposite ends of separate cross beams 41 (FIGS. 8, 10), that via bearing guide means 42 are supported by and can be telescoped relative to the central beam 43 . Gearmotors 45 , carried on central beam 43 and via output rotation of drive pinions 46 engaging racks 47 mounted on the respective beams 41 , can shift the separator members 34 , 35 to different lateral separations.
[0028] Panels 50 (FIG. 11) on the remote ends of respective lateral beams 41 support linear drive actuators 51 , which in turn via guides 52 support the assembly 32 to move between positions 32 - 1 (in solid) and 32 - 2 (in phantom) in FIG. 10. In position 32 - 2 (see FIG. 14A), the assembly 32 is close to the sewing machine 26 suited for stitching the quilt; but the small clearance between the assembly and overlying beams hinders the operators in reaching the separator members 34 , 35 for Loading the quilt bag thereon (as will be noted), However, with the assembly 32 in position 32 - 1 (and when overlying the table 18 , FIG. 7), the separator members 34 , 35 are laterally clear of the beams 41 yielding better accessibility for easy operator loading of the quilt bag onto the transfer mechanism 32 .
[0029] Each separator member 34 can be in the form of a cylindrical pin several inches long (or slightly longer than the width of the folded flap 21 ) and a small cross section of ¼ inch or less, the pin being fixed to and cantilevered from arm 33 to point away from sewing machine 26 . Each separator member 35 can also be a cylindrical pin (of related or shorter length than pin 34 ) but of larger cross section between ½ inch, and 1 and ½ inch. However, the pins 35 are pivoted inwardly adjacent the fixed pins 34 to swing around respective axes 54 disposed normal to a plane extended centrally through the spaced pins 35 . An actuator 55 powers each pin 35 between an operative orientation (FIG. 12A) generally parallel to the pin 34 and pointing away from the sewing machine 26 , and an inoperative orientation (see FIG. 12B) pointing transverse to the pin 34 and inwardly toward the other pin 35 . The fixed pins 34 extend substantially parallel to one another and normal to the beams 41 .
[0030] A power thruster 56 , having a drive rod 57 supporting the separator arm 33 , is further provided adjacent each end of the assembly 32 operable to move the separator pins 34 , 35 between the illustrated spacing from the edge clamps 36 , 37 (for quilt loading and sewing), and an inoperative position (not shown) where the pins are at a greater pin/clamp spacing so as to thereby axially withdraw the pins 34 from the yet clamped quilt bag “B”, at the end of the sewing cycle to be noted later herein.
[0031] The parallel pins 34 , 35 might be separated by perhaps 3-6 inches less than the inside of the final quilt bag opening, for easy but yet accurate operator bag loading on the pins. The two fill machine operators (not shown but acting as a team and standing on opposite sides of the table 18 ) could thus accurately fold along both the upper and lower panel corners 20 (see FIGS. 4, 5) in-folded flaps 21 extended between ½ and 1 inch in from the panel corners 20 (known to many as the French Hemm). The flaps 21 would extend across the intervening bag side seam 13 s and along both bag panel edges from the seam by only a few inches. The operators might then: orient the bag opening to open toward the sewing machine 26 (rotated one half turn from when on the table 18 ); pass the gripped folded bag edge over the cross bar 40 ; and position the opened and folded bag edges onto the nearby separator pins 34 , 35 , with the fold corners 20 against the arm 33 and with each side seam generally parallel to and overlying its pin members 34 , 35 (see FIG. 13A).
[0032] Each operator further can then make sure that the trailing bag side edge overlies the adjacent clamp ledge 36 , and when the bag is positioned accurately, can activate the clamp actuator 38 to swing the clamp arm 37 about axes 39 and against clamp ledge 36 to hold the quilt bag therebetween as positioned. Each clamp actuator 38 can be independently activated by each operator upon depressing a nearby clamp control element (not shown), or can be activated together but only after both operators have triggered both respective clamp control elements within a short duration of one another (such as within 2-5 seconds).
[0033] After the quilt bag “B” has been accurately located on the separator pins 34 , 35 and the clamps 36 , 37 have been closed to hold the bag sides, one or both of the gearmotors 45 can be activated to shift the pins 34 , 35 apart to a greater sewing separation. This will draw the final open bag edges tightly around both separator members 34 , 35 (see FIG. 13A) which effectively will hold the accurately in-folded flaps 21 thereon and will flip over the unsupported intermediate bag end edges between support on the large pins 35 to define accurately in-folded flaps extended completely across the span between these pins. The tightly drawn bag edges further will extend substantially straight across the span tangent to the pins 35 to define the bag opening 58 A (FIG. 13A). After the pins 34 , 35 have been separated as desired, the beams 41 , 43 can be locked in place such as by braking the gearmotors 45 , to keep this pin separation.
[0034] The stretching separation of separator pins 34 , 35 might be the same as or up to several inches more than the nominal full quilt width. However, as different quilt fabrics stretch differently, some experimentation might be needed for determining a preferred stretching separation for each construction, type, size of quilt bag to be stitched closed. Conventional means, such as linear encoders (not shown), can be associated with the separator pins to accurately control the gearmotors 45 to obtain any desired separation. Further, an alternative or supplemental separation control might be used, such as a force sensor (not shown) operatively associated with the powered separating gearmotor means 45 that would terminate the separation when a desired tensile force has been reached.
[0035] This method of folding the quilt flaps 21 between separating support pins 34 , 45 is fast and easy, and accurate to the end that the developed flaps should line up substantially opposite one another and the fold corners 20 should be straight, over the entire span between the pin supports.
[0036] With the beams 41 , 43 locked in place, the clamp and stretch assembly 32 , by drive actuator 51 , could be shifted from the loading position 32 - 1 to the stitching position 32 - 2 (FIG. 10) where the cross bar 40 underlies the central beam 43 . One or more power cylinders 59 are carried on the central beam 43 , and when actuated will shift respective ram carried clamps 60 against the underlying bar 38 , and the intermediate parts of the quilt bag therebetween. This would securely hold the stretched open bag end, with accurately the folded flaps 20 extended entirely across its unstitched edges, for transfer to the sewing machine.
[0037] The sewing machine 26 (FIGS. 14A, 14B, 16 ) can be conventional, having a base 63 (and underlying bobbin needle, not shown), an overlying sew head 65 and powered thread needle 66 . The open quilt edges to be stitched would ride over the base 63 and under a pressure foot (not shown), past the reciprocating needles. The illustrated arrangement provides for the quilt bag to be stationary and the sewing machine 26 via its supporting platform 31 to be moved laterally along frame beams 29 , powered by motor 68 (on the platform) and its driven pinion 69 engaging and rolling along rack 70 held on one of the beams. The arranged sewing machine base 63 will be aligned to be slightly below (by possibly ⅛ inch) the tangent plane spanning between the lower sides of the spaced separator pins 34 , 35 (FIG. 14A).
[0038] A quilt edge guide 72 (FIGS. 14A, 14B, 15 ) is also carried on the sewing machine platform 31 , spaced a small lateral distance (possibly several inches) upstream from or ahead of needle 66 (FIG. 16), referenced according to movement of the sewing machine during stitching. The guide 72 is carried by independently operated power actuators 73 , 75 , to be moved either generally toward and away from and/or transverse to the bag opening. Actuator 73 carried on the platform 31 thus powers a guided ram 74 and power actuator 75 carried thereon generally toward and away from the bag opening; and actuator 75 powers a guided ram 76 and guilt guide 72 carried thereon transverse to the elongation of the bag opening or to the top and bottom side tangent planes off of the separated support pins.
[0039] The quilt guide 72 includes a base 78 and three fingers 80 , 82 projected therefrom. The upper and lower fingers 80 project generally normal to the base 78 initially and then diverge apart like at 83 , and the intermediate finger 82 projects generally normal to the base evenly spaced between the fingers 80 . Thus, upper and lower channels 81 are defined between the spaced fingers 80 , 82 , the channels being sized to receive (somewhat snugly) the respective upper and lower folded bag edges that are to be stitched together. The guide fingers lie generally within a single plane that, when the guide is operatively mounted on the machine, extends generally normal to the elongated bag opening.
[0040] The fingers 80 , 82 are hollow, with base connections 83 for delivering via conventional lines (not shown) air under pressure to the finger interiors. The fingers 80 have side outlet openings 85 to direct air into the adjacent channels 81 angled about 40-50 degrees back toward the base 78 , and finger 82 has end outlet opening 86 to direct air forwardly away from the base, just beyond where the fingers 80 diverge. The fingers can be formed of rigid cylindrical tubing possibly between ¼ and ¾ inch outer diameters.
[0041] The air discharge jets from the upper and lower fingers 80 tend to bias the respective bag panels 11 t, 11 b into the channels 81 and hold them against the base, while the air discharge from the intermediate finger 82 is directed as jets against nearby batting 10 between the bag panels 11 t, 11 b to move such inwardly between the panels and clear of the baa edges, leaving the edges to be stitched together without any exposed batting that could for quality purposes require costly trimming to remove.
[0042] The sewing machine 23 could have a lateral start position, where: (1) the needle 66 and quilt guide 72 are between the spaced pair of separator pins 34 , 35 and closely adjacent one set of pins 34 , 35 , but adjacent the one set of pins 34 that will be on the opposite side of the sewing machine needle 66 from the quilt guide 72 ; (2) the quilt guide as shifted by actuator 75 will have its intermediate finger 82 aligned generally along a central plane through the large separator pins 35 , which central plane will be spaced above the sewing machine base 63 ; (3) the upper and lower diverging guide finger 80 will be projected forwardly beyond the front edge of the sewing machine base 63 and transversely above and below the respective stretched upper and lower quilt panels; and (4) the quilt guide as shifted by actuator 73 will have the guide channels 81 extended past the plane of needle movement during stitching.
[0043] Thus, as the transfer mechanism 25 (and stretched opened and folded quilt bag “B” held thereon) is moved by actuator 48 to the sewing position (FIGS. 14A, 14B), the intermediate guide finger 82 will fit quite accurately into the large bag opening 58 A while the outer fingers 80 overlap and direct the respective folded bag panels into the channels 81 so that the flap corners 20 can butt against the pin arms 33 . After the quilt guide 72 has vertical control of the bag via the bag panels being contained in the channels 81 , the large separator pins 35 will be shifted by actuator 55 to the inoperative positions (FIG. 12B). This provides open bag edge support (FIG. 13B) only on the smaller pins 34 , so that the upper and lower panel edges move closer together to reduce the bag opening 58 B size. The guide 72 will then be lowered (by actuator 75 ) to present the channels 81 even with or slightly below the base 63 , to draw the folded quilt bag edges to be stitched more tightly and/or evenly against the base for yielding more reliable stitching.
[0044] The sewing machine will traverse the quilt edges for stitching them, moving so that the quilt guide 72 will be ahead of the sewing needle 66 (Left to right in FIGS. 9A, 9B, and right to left in FIG. 16). To achieve accurate spacing of the stitched seam from or parallel to the panel edges, an optical scanner (not shown) having a receiver located in the base 63 and a sender in the sew head 65 can sense the moving bag edge and its spacing from the needle 66 or stitched seam, and respond to sensed excessive variances from a desired set distance (¼ inch for example) to active the actuator 48 and shift the sewing machine in a counter acting manner so as to maintain the desired seam/edge spacing.
[0045] During stitching, the initial sewing machine movement can be toward the adjacent side seam 13 s to back tack over several inches the bag edge up to close proximity (possibly within ⅛ inch) of the small support pin 34 (without striking the pin), whereupon the sewing machine movement can be reversed to stitch the closure seam in the direction toward the other support pin 34 until the seam is almost across the full width of the accurately folded bag opening. Just before the quilt guide 72 reaches the other pin 34 (perhaps yet 4-10 inches away), the guide actuator 73 can be activated to shift the guide 72 to its retracted position (FIG. 14A) clear of the path of the sewing machine so that seam stitching can continue up to an appropriate safe needle/pin gap (again possibly within ⅛ inch). The sewing machine movement can then be reversed to stitch a back tack at this opposite seam end. The seam thread can be trimmed as needed, and the sewing machine then can be moved back to the start position ready for stitching a subsequent quilt bag.
[0046] When the final edge seam (including back tacks at both ends) has been completed, the power thruster 56 will be activated to shift the support arm 33 and pins 34 axially away from the adjacent clamps 36 , 37 and 40 , 60 , for withdrawing the pins 34 from the yet clamped but now stitched quilt bag. The clamp actuators sequentially can be activated then to open the clamps 36 , 37 and 40 , 60 to release the quilt bag, for manual or automatic removal from the machine 23 , as will now be noted.
[0047] It will be appreciated that as the transfer mechanism 25 is initially moved from the table 18 to the sewing machine 26 (FIGS. 7, 8), the Lead portion of the quilt bag held thereon will be shifted right up to the sewing machine. On the other hand, only its mid portion will for sure also be moved over a frame beam 90 to a space between the frame beams 30 , 90 . If the beams 30 , 90 are spaced between 3-5 feet apart, means 91 can be provided between the beams 30 , 90 to support the quilt mid portion before, during and after seam stitching. Further, rotary product folders 92 , 95 can be mounted on the frame adjacent its opposite entry beam 90 and the sewing machine beam 30 , operable to fold the trailing and leading quilt bag ends inwardly toward and onto the quilt mid portion on the support 91 .
[0048] The folders 92 , 95 might respectively have shafts 93 , 96 and spaced fold arms 94 , 97 radially projected therefrom and underlying the respective trailing and leading quiet bag portions, and means (not shown) to support and rotate the shafts and arms. The folders further might extend to near side edges of the widest quilt bag to be stitched on the machine 23 . Thus, the trailing folder 92 can rotate its arms 94 counterclockwise (see FIG. 7) to fold the trailing quilt bag end onto the quilt bag mid portion already on the surface 91 ; and after the clamps have released the lead now stitched end of the quilt bag, the lead folder 95 can rotate its arms clockwise (see FIG. 7) to fold the stitched quilt end portion onto the mid and trailing quilt portions supported on the surface 91 . The surface 91 can be slightly lower than sewing machine base 63 , to ease the effort needed in folding the released quilt bag lead portion.
[0049] One preferred surface 91 can be a moveable belt of an automatic powered belt conveyor 98 suited for removing the stitched quilt bag away from the sewing machine. The conveyor might further operate to convey the stitched quilt bag directly to a subsequent handling station (not shown and which forms no part of this invention) that might be used as part of the quilt fabrication. The cleared sewing machine also will be ready for stitching a subsequent quilt.
[0050] Of great importance, the disclosed edge closure machine 23 stitches the final open edge of a quilt bag accurately and consistently; and without operator intervention after having the filled quilt bag loaded onto the machine's transfer mechanism initially. The illustrated and preferred embodiment has the closure machine paired with a fill machine, to be loaded by the same two operators generally used with the fill machine. However, its advantages would allow closure and stitching of filled but open quilt bag retrieved from a hopper of like bags and individually Loaded on the machine by one or more unskilled operators (not shown). Machines as disclosed herein have closed and stitched successive quilt bags on complete cycle times as fast as 25-40 seconds.
[0051] While specific structures have been disclosed, it is apparent that variations can be made therefrom, or the structures might even be eliminated completely, while yet having an operable and advantageous invention. For example, the clamp and stretch assembly 32 illustrated had transfer structures 51 for moving the assembly between two positions 32 - 1 and 32 - 2 ; but such structures and movement only provide for greater clearances for easing the efforts needed for the operators to load the quilt bag onto the separator pins 34 , 35 . However, the position 32 - 1 and its related structures could be eliminated entirely. The invention thus is not to be limited to its disclosure, but only by the scope of the following claim.
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Support members are mounted to move between two separations, respectively less than and greater than the open end of a two-panel cover otherwise seamed together around its edges. Flaps sized to define a desired closure hemm can be in-turned manually along short opposed portions of the panel ends and then positioned over the lesser spaced support members to mount the cover thereon. The support members when at the greater separation will tension the open panel edges and extend the flaps accurately in-folded between the support members. The support members can have a first size defining a large edge opening for receiving a nozzle suited for blowing unwanted materials from between the flaps, and a smaller size for minimally gapping the flaps. A sewing machine can then automatically stitch through the panels and hidden flaps, for closing the cover end edge. Clamps can grip spaced cover locations for added cover support.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is related to searching and retrieving electronic documents over a computer network and more specifically, to dynamically assembling electronic documents at retrieval, based on the document type most suitable for the user context.
2. Background Description
Normally, someone wishing to find information over the Internet uses a search engine to identify and retrieve relevant documents. Documents available over the Internet normally have a fixed document type (e.g. Download, Hints & Tips, White Paper, etc.) with static content layout. Specialized search engines may filter search results based on document type, filtering out all documents not matching the specified document type or types.
FIG. 1 illustrates a traditional document search and retrieval system 100 or search engine that may be used for such searches. In response to each search query, the search engine 100 returns documents of one preferred type only without returning other possibly more relevant documents. The system 100 includes a user interface 102 , a search unit 104 , a textual index 106 and a document storage system 108 . The document storage system 108 contains different types of static documents, e.g., Frequently Asked Questions (FAQ), Downloads and Authorized Program Analysis Reports (APAR). The textual index 106 contains a searchable index for documents in document storage system 108 . Each search query includes both search terms and preferred document type that are entered at user interface 102 and passed to search unit 104 . Search unit 104 searches textual index 106 to identify a hitlist, e.g., of FAQ documents, that contain specified search terms. Search unit 104 returns the document hitlist through user interface 102 . So, for example, listed FAQs are selected from document storage system 108 for viewing through user interface 102 . Two such examples of technical support search engines that include document type with a search query are support sites from Microsoft Corporation (support.microsoft.com/default.aspx?scid=fh;EN-US;sq1), where topic category must specify document type; and, from IBM Corporation (www-1.ibm.com/support/manager.wss?rs=0&rt=2), where the user directly specifies document type.
Unfortunately, very often this typical system 100 may not provide an answer/solution to the query, especially, when the correct answer is embedded in a document that does not match the requested document type/layout. In another example, to find downloadable video driver for product A, a prior art system may limit the search scope to ‘Download’ documents only. So, the search engine may overlook relevant information that appears in a Hints&Tips document instead for example. So, the search result is somewhat limited by a document layout or type that is normally once and forever determined by the document provider. Typically, unless the same document is stored in multiple formats, the searcher cannot choose content layout. So, typical state of the art search engines are restricted by the static nature of available documents. Thus, navigating through document storage to find relevant information often requires a level of familiarity with the document type schema. Document organization may hamper searching. Different content providers cannot choose suitable content and layout for particular local portals. So, users must live with whatever documents are stored and available.
These search constraints are especially troublesome in corporate technical support systems, typically a complex hierarchical schema of document types combined with a product taxonomy tree. Usually corporate-wide documents are standardized to provide a unified document view through the corporate technical support portal. These constraints make retrieving information from a corporate technical support system a challenging task especially if the document storage system contains heterogenous document collections.
Thus, there is a need for a way to select document presentation according to the needs of a particular user or presentation context.
SUMMARY OF THE INVENTION
It is a purpose of the invention to facilitate finding relevant information regardless of the format of documents containing the information;
It is another purpose of the invention to present such information in a selectable document type and/or layout that may not match the format of the original document containing the information;
It is yet another purpose of the invention to choose a most suitable document content layout.
The present invention is a document search and retrieval system and program product therefor. Search requests are provided to the system through a user interface. A document decomposer decomposes documents into individual document components. Document components and corresponding searchable indices for each are stored in a Component Library. A search unit searches stored document components responsive to search queries. A results validator compares document hitlists with a document type identified in a search query to select valid hitlists entries for a final hitlist. A document view assembly module collects identified document components and assembles them into a document for view at the user interface.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other objects, aspects, and advantages will be better understood from the following non limiting detailed description of preferred embodiments of the invention with reference to the drawings that include the following:
FIG. 1 shows a block diagram of a prior art document retrieval system;
FIG. 2 shows a block diagram of an example of a preferred embodiment of the present invention;
FIG. 3 shows an example of document decomposition and indexing schema according to a preferred embodiment wherein a Document Decomposer module extracts document components and stores them in the Component Library;
FIG. 4 shows an example of a document decomposition and indexing flow chart showing how the Document Decomposer module interacts with other modules;
FIG. 5 shows an example of a preferred embodiment document search schema, wherein different type documents are returned by the Search Engine for selection and viewing;
FIG. 6 shows an example of a preferred document search flow chart of how the Results Validator module interacts with other modules of the present invention;
FIG. 7 is an example of a document viewing schema, wherein the Document View Builder module retrieves document components from the Component Library module and assemble a document for view according to the selected context;
FIG. 8 shows an example of a preferred document viewing flow chart of how the Document View Builder interacts with other modules of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
According to a preferred embodiment of the present invention, content components are extracted from original documents and stored in a component library. When a query calls for information found in the content components, a context is selected in which retrieved information is viewed. Documents of the chosen type/layout are constituted on the fly from stored document components. More relevant documents may be identified and rendered in a selected context/layout.
FIG. 2 shows an example of a component based document search and retrieval system 110 according to a preferred embodiment of the invention. The system 110 includes an User Interface 112 , a Search Unit 114 , a Textual Index 116 , Document Storage 118 , a Component Library 120 , a Document Decomposer 122 , a Document View Builder 124 and a Result Validator 126 . The Document Storage 118 contains different types of documents, e.g., FAQs 128 , Downloads 130 and APARs 132 .
The Document Decomposer 122 distills individual components from each of the documents 128 , 130 , 130 and the components are stored in the Component Library 120 . For example, a typical FAQ 128 might include a Title, a Problem Statement, a Solution and, optionally a reference link to additional information. Further, these document components can be collected and assembled to form an FAQ document. Likewise, a Download document may include a Title, a Solution, an Attachment and a reference. Table 1 is an example illustrating typical document components for several document types. Typically, each of these components is tagged by a section subtitle in the original document. Each document type has its own set of sections according to predefined corporate templates. The Document Decomposer 122 locates each tagged component, extracts each located component and stores extracted components in the Component Library 120 . Then, the individual components are indexed in the Textual Index Unit 116 , making each indexed component available for full text search.
TABLE 1
Doc.Type
Title
Abstract
Problem
Solution
Attachment
Reference
FAQ
X
X
X
X
APAR
X
X
X
X
X
Hints
X
X
X
& Tips
Download
X
X
X
X
A search is initiated with a query that specifies both search terms and preferred document type passing through the User Interface 112 to Search Unit 114 . Search Unit 114 searches component indices in Textual Index 116 and retrieves a hitlist for specified search terms. Results Validator 126 checks the hitlist and identifies candidates that include all of the components needed to constitute a document in the selected format, e.g., FAQ format. The Results Validator 126 returns a list of remaining documents that can be constituted into the selected format. Each request also passes through User Interface 112 to Document View Assembly Module 124 which retrieves and assembles components into a document in the selected format. The assembled document is returned for viewing through User Interface 112 .
FIG. 3 illustrates document decomposition and indexing document collections 140 , 142 , 144 by Document Decomposer 122 . Different types of documents pass from collections 140 , 142 , 144 to Document Decomposer 122 . The Document Decomposer 118 locates and extracts document components/elements, according to the original document type model (e.g., Table 1). Extracted document components are stored in Component Library 120 . Then, the content of each of the document components is indexed in the Textual Index 122 for full text search.
FIG. 4 shows an example of a document decomposition and indexing flow chart 150 . The Document Storage System 116 passes a document 152 to Document Decomposer 122 . The Document Decomposer 122 extracts document components 154 and passes the extracted components to Component Library 120 . Document components are passed from Component Library 120 to Indexer 156 which creates an inverted Textual Index 158 of all words in each document component to enable full text search. The Indexer 156 associates the entries in this Textual Index 158 with documents that contain the components.
In addition to document components, the Component Library 120 contains a table of document type masks for every supported document type. Table 2 shows an example of a document type mask table for the above example of four identified document types. Each document type mask defines a set of components constituting a particular document type.
TABLE 2
Doc.Type
Title
Abstract
Problem
Solution
Attachment
Reference
FAQ
1
0
1
1
0
1
APAR
1
1
1
1
0
1
Hints
1
1
0
1
0
0
& Tips
Download
1
0
0
1
1
1
In another preferred embodiment of the present invention, a document search is constrained such that the search result hitlist includes only documents that can be rendered in the requested viewing context. So, for example, while search results may identify numerous documents in each of the document types, the search results hitlist would list only those documents that can be constitute a FAQ type layout, i.e., FAQ and APAR type documents.
FIG. 5 shows an example of this second preferred embodiment document search schema 160 . A Search Query 162 that specifies both query terms and a selected document type is submitted to Search Engine 164 . The Search Engine 164 uses the Textual Index 166 to find stored document components that contain the specified query terms. A hitlist of document hits of appropriate document types is extracted from Textual Index 166 as Search Results 168 . The Search Results 168 hitlist is passed to the Results Validator 170 which uses an appropriate document type mask to perform document selection, selecting documents that can be rendered in the selected context. The Results Validator 170 uses a requested document type mask from the Component Library 120 to filter documents (exclude) from the hitlist that could not be configured to match the requested document type. Results Validation Table 174 is an example of results validation output from Results Validator 170 . The Final Results 176 hitlist is a reduced hitlist that includes only documents with at least matching components necessary for requested document type.
FIG. 6 shows a flow chart of a document search 180 using the document schema 160 of FIG. 5 . A user submits a search query 182 to Search Engine 184 initiating the search. The Search Engine 184 uses the Textual Index 186 to produce a hitlist 188 of documents with components that match query terms. The Results Validator 190 checks document hits in the hitlist 188 against the requested document type mask from Component Library 120 . Only documents with at least components in the document type mask are output in a Final Hitlist 192 .
FIG. 7 shows an example of a preferred document viewing schema 200 . Once the search is completed, (i.e., in 176 and 192 of FIGS. 5 and 6 ), the user may select one of the listed documents to view the document content. The request is passed to a Document Retrieval Module 200 that retrieves requested document components from the Component Library 120 . One of the hits (e.g., an APAR document) in the Hitlist 202 is selected for viewing. The Document View Builder 204 , retrieves requested components from Component Library 120 and assembles the document components according to the requested document mask (FAQ mask) by applying the layout defined by the requested document type.
FIG. 8 shows an example of a document view construction flow chart 210 . The Document View Builder 218 assembles the document by including and omitting relevant components to match the requested document type. After selecting an entry from final hitlist 212 , the Document View Builder 214 retrieves components for the selected entry from the Component Library 216 . Then, the Document View Builder 214 assembles the components into a viewable document according to the selected format and outputs the assembled document over the user interface for viewing 218 .
Thus, search result documents are provided in a user selected document type based upon the user request. Documents of a requested type are assembled dynamically from a given content. The document with an answer/solution for the user's question/problem can be found, even if its static document type does not match the document type requested by the user. Advantageously, the number of available document types for a given content is supplemented from previously unavailable documents.
While the invention has been described in terms of preferred embodiments, those skilled in the art will recognize that the invention can be practiced with modification within the spirit and scope of the appended claims.
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A document search and retrieval system and program product therefor. Search requests are provided to the system through a user interface. A document decomposer decomposes documents into individual document components. Document components and corresponding searchable indices for each are stored in a Component Library. A search unit searches stored document components responsive to search queries. A results validator compares document hitlists with a document type identified in a search query to select valid hitlists entries for a final hitlist. A document view assembly module collects identified document components and assembles them into a document for view at the user interface.
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RELATED APPLICATION
This application is a continuation-in-part of Application Ser. No. 665,464, filed Mar. 6, 1991 entitled "A Method for Loading a Chemical Compound Within the Hollow Interior of Fibers" now abandoned.
1. Field of the Invention
The present invention relates generally to a method for loading a chemical compound within the hollow interior, cell walls and on the surfaces of the fibers of a fibrous material. More particularly, the present invention is directed to an improved process for the production of filler-containing paper pulp in which the filler is formed in situ while in proximity to the paper pulp and a substantial portion of the filler is disposed in the lumens and cell walls of the cellulose fibers of the paper pulp, to the paper pulp produced thereby and to papers produced from such pulp.
2. Background of the Invention
Paper is a material made from flexible cellulose fibers which, while very short (0.02-0.16 in. or 0.5-4 mm), are about 100 times as long as they are wide. These fibers have a strong attraction for water and for each other; when suspended in water they swell by absorption. When a suspension of a large number of such §fibers in water is filtered on a wire screen, the fibers adhere weakly to one another. When more water is removed from the mat formed on the screen by suction and by pressing, the sheet becomes stronger but is still relatively weak. When the sheet is dried, it becomes stronger, and paper is produced.
Any fibrous raw material such as wood, straw, bamboo, hemp, bagasse, sisal, flax, cotton, jute and ramie, can be used in paper manufacture. Separation of the fibers in such materials is called pulping, regardless of the extent of purification involved in the process. The separated fibers are called pulp, whether in suspension in water as a slurry or dewatered to any degree. Pulp from a pulping process which has been dewatered to an extent such that it is no longer a slurry and has been broken up into clumps which appear to have no free water is referred to as "dewatered crumb pulp". While dewatered crumb pulp appears to be particulate fragments, such pulp may contain up to about 95% by weight of water.
Wood is the major source of fiber for pulping because of its wide distribution and its high density compared with other plants. While any species of wood can be used, soft woods are preferred to hard woods because of their longer fibers and absence of vessels. Wood and most other fibrous material have cellulose as their main structural component, along with hemicellulose, lignin and a large number of substances collectively called resins or extractives.
Pulping may be carried out by any of several well known processes, such as mechanical pulping, kraft pulping and sulfite pulping. An essential property of paper for many end uses is its opacity. It is particularly important in papers for printing, where it is desirable that as little as possible of the print on the reverse side of a printed sheet or on a sheet below it be visible through the paper. For printing and other applications, paper must also have a certain degree of whiteness (or brightness as it is know in the paper industry). For many paper products, acceptable levels of these optical properties can be achieved from the pulp fibers alone. However, in other products, the inherent light-reflective powers of the fibers are insufficient to meet consumer demands. In such cases, the papermaker adds a filler to the papermaking furnish.
A filler consists of fine particles of an insoluble solid, usually of a mineral origin. By virtue of the high ratio of surface area to weight (and sometimes high refractive index), the particles confer high light-reflectance to the sheet and thereby increase both opacity and brightness. Enhancement of the optical properties of the paper produced therefrom is the principal object in adding fillers to the furnish although other advantages, such as improved smoothness, improved printability and improved durability, can be imparted to the paper.
The increasing use of alkaline conditions in the manufacture of printing and writing papers has made it technically feasible to incorporate high loadings of alkaline fillers, such as calcium carbonate. There is an economic incentive to increase this filler loading, because when paper is sold on a weight basis (or by the sheet), the cheaper filler material effectively substitutes for the more costly fiber. In Europe, where fiber is more expensive, printing and writing grade papers are commonly produced containing 30-50 percent calcium carbonate; whereas only 15-20 percent loading is typically used in the United States. At the higher levels of filler loading, in order to maintain other §desirable paper properties, like strength, it is necessary to use additional expensive chemical additives. In Europe, this added expense is justifiable due to the high cost of fiber. Lower fiber cost in the United States, however, makes the use of chemical additives in order to achieve higher filler substitution less cost effective. Yet, since calcium carbonate is about 20-25% of the cost of a pulp fiber, an economical way to increase the level of pulp substitution by filler remains desirable. However, filler addition does pose some problems.
One problem associated with filler addition is that the mechanical strength of the sheet is less than could be expected from the ratio of load-bearing fiber to non-load-bearing filler. The usual explanation for this is that some of the filler particles become trapped between fibers, thereby reducing the strength of the fiber-to-fiber bonds which are the primary source of paper strength.
A second problem associated with the addition of fillers is that a significant fraction of the small particles drain out with the water during sheet formation on the paper machine. The recovery and recycling of the particles from the drainage water, commonly known as the white water, poses a difficult problem for the papermaker. In seeking to reduce this problem, many researchers have examined the manner in which filler is retained by a sheet. It has become accepted that the main mechanism is co-flocculation, i.e., the adhesion of pigment particles to the fibers. As a result of this finding, major effort in filler technology has gone into increasing the adhesive forces. This work has lead to the development and use of a wide variety of soluble chemical additives known as retention aids. The oldest and the most widely-used of these is aluminum sulfate (Papermakers' alum), but in recent years a variety of proprietary polymers have been introduced. With all of these retention aids, however, retention is still far from complete. A further mechanism of retention is filtration of pigment particles by the paper web. This is relatively important with coarse fillers, but its effect is negligible with fine fillers.
U.S. Pat. No. 4,510,020 to Green, et al. describes a process whereby a particulate filler, such as titanium dioxide, whey or calcium carbonate, is loaded in the lumens of the cellulose fibers of paper pulp. In the method of the Green, et al. patent, the particulate filler is selectively loaded within the fiber lumens by agitating a suspension of pulp and filler until the fiber lumens become loaded with filler. The method requires the use of substantially more particulate filler than can be loaded within the lumens of the fiber. Accordingly, the method requires a step of separating the residual suspended filler from the loaded fibers by vigorously washing the pulp until substantially all of the filler on the external surfaces of the fibers is removed. Thus, the Green, et al. patent does not solve the problem referred to hereinabove wherein the filler must be recovered from the white water.
U.S. Pat. No. 2,583,548 to Craig describes a process for producing a pigmented cellulosic pulp by precipitating pigment in and on and around the fibers. According to the method of the Craig '548 patent, dry cellulosic fibers are added to a solution of calcium chloride. The suspension is mechanically worked so as to effect a gelatinization of the fibers. The proportions of the dry cellulosic stock to the calcium chloride solution can be varied, but in general, the amount of calcium chloride present in the dilute solution is several times the weight of the cellulose fibers which are treated therewith. A second reactant, such as sodium carbonate, is then added so as to effect the precipitation of fine solid particles of calcium carbonate in and on and around the fibers. The fibers are then washed to remove the soluble by-product, which in this case is sodium chloride. The pigmented fibers produced by the Craig '548 patent contain more pigment than cellulose and when used as a paper additive are combined with additional untreated paper pulp. The fibrous form of the pigmented additive provides good retention, but the process does have considerable limitations. The presence of filler on the fiber surfaces and the gelatinizing effect on the fibers are detrimental to paper strength.
A modification of the '548 Craig patent is disclosed in U.S. Pat. No. 2,599,091 to Craig. in the method of the Craig '091 patent, dry paper stock containing as high as 13% pulp solids is treated by the addition of solid calcium chloride to the stock. The solid calcium chloride brings about a profound modification of the cellulose fibers after a few minutes of agitation. The fibers become more or less gelatinous and transparent in appearance. After the treatment with calcium chloride, the stock is treated with a soluble carbonate salt in the form of a 10% solution, which is added in sufficient amount to react with the calcium chloride and precipitate an insoluble pigment of calcium carbonate. The resulting treated and pigmented stock is highly hydrated and has little strength or relatively much less strength than the untreated stock. The pigmented stock is then combined with untreated paper stock to provide a pigmented paper stock suitable for the preparation of paper.
U.S. Pat. No. 3,029,181 to Thomsen is a further modification of the in situ precipitation process of the Craig patents. In the method of the Thomsen patent, the fiber is first suspended in a 10% solution of calcium chloride. Thereafter, the fiber is pressed to a moisture content of 50% and is sprayed with a concentrated solution of ammonium carbonate in an amount sufficient to precipitate all the calcium as the carbonate. The fiber is then washed to remove ammonium chloride. The washed fiber is ready for the paper machine and will usually contain approximately 10% of loading material. The Thomsen patent indicates that the method disclosed therein coats the internal area with the loading material and increases the opacity of the cellulose fibers with such internal loading.
Japanese Patent Application 60-297382 to Hokuetsu Seishi describes a method for precipitating calcium carbonate in a slurry of pulp. In the method of the Hokuetsu patent, as set forth in the examples, calcium hydroxide is dispersed in a 1% slurry of beaten or unbeaten pulp. Carbon dioxide gas was then blown into the mixture of pulp slurry and calcium hydroxide to convert the calcium hydroxide to calcium carbonate.
While the Craig patents and the Thomsen patent disclose methods for the precipitation of pigment in the presence of fibers, each of the methods disclosed in these patents requires a washing step to remove the unwanted salt, i.e., sodium chloride or ammonium chloride. These methods also suffer from the aforementioned reduction in paper strength due to the gelatinizing effect on the fibers. The method of the Hokuetsu patent suffers from the fact that the calcium carbonate is precipitated in the aqueous phase of the slurry rather than a crumb pulp and is not substantially present in the lumen and cell walls of the pulp fiber.
Accordingly, it would be highly desirable to provide a method wherein a substantial amount of a filler can be dispersed within the lumens and cell walls of cellulose fibers by a simple method which is adapted to be used with existing papermaking machinery. It would also be highly desirable to provide a method for loading a chemical compound within the hollow interior and cell wall of the fibers of fibrous cellulose materials by a method which obviates the need for a subsequent washing step.
SUMMARY OF THE INVENTION
In a product aspect, the present invention relates to novel fibrous materials comprising a plurality of elongated fibers having a fiber wall surrounding a hollow interior and having a chemical compound loaded within the hollow interior, within the fiber walls of the fibers and on the surface of the fibers.
In process aspects, the present invention relates to a method for producing a chemical compound in situ while in proximity to the fibers of a fibrous material. In the method, a fibrous material is provided which consists of a plurality of elongated fibers having a fiber wall surrounding a hollow interior. The fibrous material has a moisture content such that the level of water ranges from 40-95% of the weight of the fibrous material and the water is positioned substantially within the hollow interior of the fibers and within the fiber walls of the fibers. A chemical is added to the fibrous material in a manner such that the chemical becomes associated with the water present in the fibrous material. The fibrous material is then contacted with a gas which is reactive with the chemical to form a water insoluble chemical compound. The method provides a fibrous material having a chemical compound loaded within the hollow interiors of the fibers, within the fiber walls of the fibers and on the surface of the fibers.
While various aspects of the present invention will be described with more particularity in respect to the loading of paper pulp, it should be understood that the method of the invention is amenable to use with other fibrous materials, which comprise a plurality of elongated fibers having a fiber wall surrounding a hollow interior and which are adapted to have a substantial amount of water dispersed in the hollow interior and fiber walls.
DESCRIPTION OF THE DRAWINGS
FIGS. 1-7 are plots of various parameters of paper handsheets prepared from cellulose loaded with calcium carbonate in accordance with the invention and compared with paper handsheets directly loaded on the surface with calcium carbonate in accordance with a conventional method.
DETAILED DESCRIPTION OF THE INVENTION
The structure of and physical properties of cellulosic fibers is an important aspect of the present invention. The most widely-used cellulosic fibers for papermaking are those derived from wood. As liberated by the pulping process, the majority of papermaking fibers appear as long hollow tubes, uniform in size for most of the length but tapered at each end. Along the length of the fiber, the fiber wall is perforated by small apertures (pits) which connect the central cavity (lumen) to the fiber exterior. It is well known that papermaking pulp can contain a high level of moisture within the cell wall and interior central cavity or lumen without appearing to be wet or without forming a slurry. An example of such pulp is referred to as "dewatered crumb pulp". The highest level of moisture that can be present in dewatered crumb pulp without providing free moisture on the surface of the pulp is dependent on the type of wood used to produce the pulp, the pulping process used to defiberize the wood and the dewatering method. The level of moisture for a particular pulp at which free water appears on the surface is referred to as the "free moisture level". At levels of moisture above the free moisture level, the pulp fibers become dispersed in the water and slurry is formed. Depending on the type of pulp, the free moisture level of the pulp can be from about 95% to about 90% of moisture, i.e., from about 5% to about 10% of pulp. All percentages used herein are by weight and all temperatures are in degrees Fahrenheit, unless otherwise indicated.
In accordance with the present invention, dewatered crumb pulp is utilized which contains less moisture than the free moisture level. Preferably, the dewatered crumb pulp contains from about 40% to about 95% of moisture, by weight, based on the total weight. In an important embodiment of the invention, it is preferred to use dewatered crumb pulp having from about 70% to about 15% of moisture, i.e., from about 85% to about 30% of cellulose fiber.
The process of the present invention for loading fibers is applicable to a wide range of papermaking fibers. The process can be carried out on pulps derived from many species of wood by any of the common pulping and bleaching procedures. The pulp can enter the process in a "never-dried" dewatered form or it may be reconstituted with water to a level of moisture within the indicated range from a dry state.
Cellulosic fibers of diverse natural origins may be used, including soft wood fibers, hard wood fibers, cotton fibers and fibers from bagasse, hemp and flax. The fibers may be prepared by chemical pulping, however, mechanically pulped fibers, such as ground wood, thermomechanical pulp and chemithermomechanical pulp can also be used. The fibers may have received some mechanical treatment, such as refining or beating prior to loading the chemical compound into the lumen. Synthetic fibers, such as hollow filament rayon, bearing accessible internal hollow structures can also be lumen-loaded by the process of the invention.
Further in accordance with the invention, calcium oxide (lime) or calcium hydroxide is mixed with dewatered crumb pulp having the desired level of moisture. In this connection, the calcium oxide can be added to the water used for reconstituting dried fibers prior to adding the water to the fibers. Upon adding the calcium oxide to a dewatered crumb pulp and simple mixing for a period of a few minutes, the calcium oxide (as a white powder) combines with the water to form calcium hydroxide within the mass of fibers in the pulp. Since both calcium oxide and calcium hydroxide are both relatively insoluble in water (1.2 and 1.6 grams per liter, respectively) and there is no substantial free surface moisture on the fibers, the mechanism whereby the calcium oxide is drawn into the water located in the hollow fiber interior and the fiber walls is not completely understood. Calcium oxide, however, reacts vigorously with water in an exothermic reaction to produce calcium hydroxide, enough for 100 grams of quicklime to heat 200 grams of water from 0° F. to boiling. While not wishing to be bound by any theory, it is believed that the calcium oxide reacts with water at the surface openings of the fiber to form calcium hydroxide and that the calcium hydroxide is drawn into the cell walls and hollow interior of the cellulose fibers by hydrostatic forces. For this reason, the highly reactive forms of calcium oxide (quicklime) are preferably used in the process of the invention. The less reactive forms, such as dolomitic limestone and dead burned limestone are less suitable.
The calcium oxide or calcium hydroxide may be added at any desired level up to about 50%, based on the weight of the dry cellulosic material. The lower limit for addition of the calcium oxide may be as low as desired, but is preferably not less than about 0.1%. Most preferably, the calcium oxide or calcium hydroxide is present at a level of from about 10% to about 40%, based on the weight of the dry cellulosic material. The carbon dioxide is added at a level sufficient to cause complete reaction of the chemical with the gas to form the water insoluble chemical compound. Excess gas can be used since no further reaction takes place. Since there is no extraneous chemical material formed, such as would be the case with precipitating a water-insoluble chemical compound with two water soluble salts, there is no need to wash the cellulosic material after treatment with carbon dioxide in accordance with the invention to load the fibers with the precipitated calcium carbonate. In the case of paper pulp, the paper pulp can be immediately transferred to a papermaking operation where it is formed into a slurry, refined and placed onto a Fourdrinier machine or other suitable papermaking apparatus. Alternatively, the paper pulp having the chemical compound loaded therein may be further dried and shipped as an item of commerce to a papermaking facility for subsequent usage.
It has been determined that the precipitation of calcium carbonate in cellulosic fibers containing from about 40% to about 85% of moisture (15% to 60% of fiber) and loaded with from about 10% to about 40% of calcium oxide or calcium hydroxide is easily effected in a pressurized container with low shear mixing. The carbon dioxide pressure in the container is preferably from about 5 psig to about 60 psig and the low shear mixing is preferably continued for a period of from about 1 minute to about 60 minutes.
It has also been determined that for fibers containing from about 95% to about 85% of moisture (5% to 15%) of fiber) and the same calcium oxide loading, that high shear treatment during contact with the carbon dioxide is required to cause complete precipitation of calcium carbonate. In this connection, any suitable high shear mixing device can be used. Preferably, the high shear treatment is sufficient to impart from about 10 to about 70 watt hours of energy per kilo of fiber, dry weight basis.
It has been determined that a simple way to provide contact of the carbon dioxide with the paper pulp under high shear treatment is by means of a pressurized refiner. The pressurized refiner is a well known piece of apparatus utilized in the papermaking industry and consists of a cylindrical hopper into which the paper pulp is loaded. The cylindrical hopper is gas tight and can be pressurized with a gas. A rotating shaft containing beater arms is disposed within the hopper to keep the paper pulp from matting. An auger screw is located beneath the hopper for conveying the paper pulp into the interior space between a set of matched discs. One of the discs is stationary whereas the opposing disk is driven by means of a motor. The discs are spaced apart by a distance sufficient to shred the pulp crumbs as the pulp passes between the stationary disk and the revolving disk. The discs may be provided with refining surfaces. The use of a "devil's tooth" plate, or fiberizing plate, has also been found to be suitable. Prior to forcing the pulp into contact with the rotating plate, the carbon dioxide is pumped into the sealed hopper to pressurized the hopper with carbon dioxide and remains in contact with the pulp while the paper pulp is stirred in the hopper and while the pulp is being transported by the auger through the refiner discs.
It has also been determined that it is not possible to effect the reaction between the calcium oxide or calcium hydroxide and the carbon dioxide by blowing the carbon dioxide through the mixture of dewatered crumb pulp and the calcium oxide or calcium hydroxide.
Through an investigation of handsheets prepared in accordance with the invention, it has been determined that about 50% of the precipitated calcium carbonate is retained by the pulp fibers. The remaining 50% is recovered as white water which can be used to fill paper on the papermaking machine in accordance with conventional surface filling processes. The retained calcium carbonate is distributed approximately equally in the lumen, within the cell walls of the cellulose fibers and on the surface of the cellulose fibers. A higher level of retention is attained by precipitation of calcium carbonate in a pressurized container with low shear than through use of the pressurized refiner. The quality of handsheets prepared from pulp wherein the precipitation is effected with the pressurized refiner is, however, superior.
The following example further illustrates various features of the invention, but is intended to in no way limit the scope of the invention as set forth in the appended claims.
Materials
Pulp--The pulps used were a softwood pulp mixture and a hardwood pulp mixture that were supplied by Consolidated Paper Company and refined further in a single disk refiner to pulp freenesses of 410 and 180 (CSF) for the softwood, and 395 and 290 (CSF) for the hardwood.
Calcium reactants--Calcium oxide used was a technical grade (Fisher Chemical Company) or a high reactivity Continental lime (Marblehead Lime Co.). Reagent grade calcium hydroxide (Aldrich Chemical) was also used. For the direct loading comparison, papermaker grade calcium carbonate (Pfizer) was used.
Equipment
Mixer--A bench-model 3-speed Hobart food mixer with a 20 quart stainless steel bowl and flat beater was used for mixing the calcium reactants with the pulp.
Refiner--A Sprout-Bauer pressurized disk refiner was used as both the reaction chamber and refiner for precipitating calcium carbonate and incorporating it into pulp fibers.
Filtering centrifuge--This 2-speed centrifuge is equipped with a perforated vessel lined with a canvas bag to filter a continuous flow of low consistency slurries.
Bauer-McNett Fiber Analyzer--An industry standard method for determining non-leachable filler retention.
Muffle furnace--A Thermodyne furnace was used for ashing samples.
Typical Refiner Run Procedure
Hobart--For each run, 1 kg pulp (based on dry weight of fiber) was blended in the Hobart mixer with varying amounts of calcium reactant and water required for a specific chemical load and consistency. The pulp was mixed for 15 minutes at low speed (approximately 110 rpm) to uniformly incorporate the calcium.
Refiner--The high consistency pulp was then loaded into the hopper of the refiner which was closed and sealed. Carbon dioxide was injected into the hopper to react with the calcium hydroxide. Carbon dioxide was held in the tank at 20 lbs. pressure for 15 minutes. During this interval, calcium carbonate was precipitated in the pulp fibers by the reaction of calcium oxide or calcium hydroxide with the carbon dioxide. The pulp is then refined in a carbon dioxide atmosphere at the desired plate gap and feed rate to provide intimate contact of the carbonate and fibers.
Direct loading--For comparisons, pulps were loaded directly with calcium carbonate without the aid of the pressurized refiner. Pulp for direct loading was fiberized in the British Disintegrator according to Tappi Standard T-205 for 60g/m2 handsheet preparation and poured into the doler tank. Varying amounts of calcium carbonate was added to the low consistency pulp slurry in the doler tank and stirred to assure uniform distribution prior to making handsheets.
Centrifuging--In order to avoid the high consistency mixing step using the Hobart mixer, pulps were sometimes loaded with calcium oxide or calcium hydroxide at low consistency and then dewatered. Pulp and the calcium reactant was stirred at 2% consistency with an air stirrer for 15 minutes. The pulp slurry was the fed into the filtering centrifuge to dewater the pulp to approximately 30% consistency. The pulp was removed from the centrifuge bag, shredded and loaded into the pressurized refiner for reaction with carbon dioxide.
TEST METHODS
Scanning Electron Microscopy (SEM)--SEM observations and X-ray microanalysis was carried out on transverse sections of pulp fibers and handsheets. Sections were hand-cut with a razor blade. The dry pulps and strips of handsheets (1 cm×0.3 cm) were cemented to aluminum stubs and sputter-coated with gold. Samples were photographed in a JEOL 840 SEM at an accelerating voltage of 20 kv.
SEM X-ray microanalysis--Samples were prepared as for SEM observation, but were adhered to carbon specimen stubs and coated with a conductive carbon layer. X-ray microanalysis was performed with a Tracor Northern T-2000/4000 energy-dispersive spectrometer in combination with the scanning electron microscope. The microanalysis spectra were recorded in an energy range of 15 keV.
The specimen preparation procedures for x-ray analysis make it necessary for controls to be employed if x-ray data are to be compared with any validity. The samples of pulp and handsheets were dried at the same time, under the same conditions. This eliminates variations arising from inconsistencies in procedures. Once a sample is dried, care was taken to keep it free of moisture. The samples were not exposed to room air and not stored in a desiccator with chemical desiccants for fear of elemental contamination. All x-ray data to be compared was obtained with the same specimen current for biological x-ray microanalysis.
Carbonate Test
Pulp and handsheet specimens were placed in 1% aqueous silver nitrate for 30 minutes, rinsed in §distilled water and placed in 5% aqueous sodium thiosulfate for 3 minutes and washed in tap water (Van Kossa's method for carbonates). Carbonate groups (calcium) stain black. Rapid spot tests were run on samples to confirm the presence of carbonates.
Pulp/Paper Tests
As each filled pulp sample was discharged from the refiner, a random sample was taken for the determination of freeness, pH and ash content. Ash content of the pulp was assessed by Tappi Method T-211. Handsheets (60g/m 2 ) were prepared from the pulp by standard Tappi Method T-205. Again, the ash content was determined on the handsheet, and the percent retention is reported as the percent filler in the handsheet based on the percent filler in the pulp (and subtracting the small blank of the pulp's original ash content). Percent retention, therefore, represents the filler retention that stays with the pulp during standard handsheet formation. Another sample of pulp from the refiner discharge was subjected to a thorough washing (20 minutes) with tap water in a chamber of a Bauer-McNett fiber fractionator and collected on a 200 mesh screen. The ash content was determined on this Bauer-McNett washed pulp sample, and is identified in the data tables as B/M ash%.
The handsheets were used for evaluation of §burst index and for the evaluation of optical properties. Burst index, as determined by Tappi Method T-403, is a convenient measure of strength and an accepted measure of fiber bonding. Densities of the handsheets were measured according to Tappi Method T-220 and appeared to correlate meaningfully with both freeness and burst index. Optical properties of brightness, opacity and scattering coefficient were determined on a Technidyne photometer. Spread sheets of all the test data obtained on the pulp and handsheets are attached in the appendix.
SEM
Initial loading experiments using CaO indicated that rhombohedral calcite crystals in the 1 to 3 micron size were attained, as evidenced by electron microscopy. Scanning electron microscopy of the cross-sections of pulp and handsheet fibers showed that calcium carbonate was precipitated as discrete angular particles, i.e., crystals. Crystalline aggregates can be seen in the lumen and on the surface. The distinctive spectrum of calcium is found within the cell-wall as well as on the fiber surface and in the cell lumen. This latter information indicates that a portion of the calcium ions can diffuse into the fiber wall as well. Calcium carbonate was confirmed to be in the lumen and on the surface of pulp and handsheet fibers.
Table 1 is a comparison of the burst and optical properties (at the same initial freeness) of refiner-run handsheets. The two numbers in parentheses, such as (15,20), indicate the pulp consistency and the calcium reactant loading, respectively. Also for comparison, are the burst and optical properties of handsheets in which the filler loading was obtained by direct addition during handsheet formation of papermaker's grade carbonate (Pfizer). The results in Table 1 are also presented in the FIGS. 1-7. If scattering coefficient, opacity or brightness are plotted versus burst index, FIGS. 1-7 points from the fiber loaded handsheets lie approximately on the same curves as the points from the direct-loaded handsheets. These plots indicate the expected inverse relationship between optical properties and strength; that is, as burst strength increases, the desirable optical properties decreases. The fact that both fiber loaded handsheets and direct loaded handsheets of the invention lie on the same curves means that for any given gain in optical properties, one should expect a comparable loss in strength properties regardless of how the filler is incorporated.
TABLE 1__________________________________________________________________________COMPARISON OF BURST AND OPTICAL PROPERTIESBETWEEN FIBER LOADED & DIRECT LOADED HANDSHEETS P. Scatt. Brightness Opacity Coeff. Density Burst Index Paper Ash B/W AshType (%) (%) (m2/Kg) (Kg · m3) (KPa · m2/g) (%) (%)__________________________________________________________________________CTRL-BL.HW (395) 87.7 78.5 47.7 717.7 3.14 0.24 --46% D.CaCO3 90.6 87.2 101.6 648.4 1.12 16.25 --36% D.CaCO3 90.3 86.2 93.0 651.6 1.26 12.35 0.35**27% D.CaCO3 89.6 84.6 79.6 671.7 1.65 8.80 0.3516% D.CaCO3 88.5 81.5 60.4 676.2 2.03 4.10 --12% D.CaCO3 88.1 81.5 58.2 687.2 2.23 3.02 --10% D.CaCO3 88.6 81.5 60.3 679.2 2.12 3.83 --5% D.CaCO3 87.8 79.5 53.5 696.0 2.57 1.74 --Run #214 (21,20) 89.0 82.2 64.1 722.6 1.70 9.82 4.19Run #233 (21,20) 88.8 82.5 63.9 750.8 1.92 10.48 5.34Run #243 (21,20) 88.7 82.2 62.6 741.1 1.86 9.38 3.80Run #245 (21,20) 88.7 82.4 64.0 738.5 1.81 9.51 3.30Run #275 (21,20) 88.6 82.2 63.1 737.1 1.78 9.16 3.34Run #265 (21,20) 88.7 83.0 66.7 727.2 1.71 10.17 3.77Run #213 (18,20) 88.8 82.2 64.3 736.3 1.80 10.04 3.59Run #217 (18,30) 90.0 84.5 78.9 719.2 1.27 15.39 5.22Run #211 (15,20) 88.8 82.7 65.1 712.6 2.10 10.58 3.54Run #218 (18,10) 87.8 79.8 53.2 720.7 2.34 5.11 2.69__________________________________________________________________________
FIG. 4 is a plot of burst index versus ash content. The direct loaded handsheets lie on a smooth curve; again demonstrating that as the ash content increases, the burst strength decreases. The points from the fiber-loaded handsheets are plotted in the same figure and all of the fiber-loaded handsheets lie considerably above the direct-loaded curve. This means that at comparable ash contents, the fiber-loaded §handsheets of the invention are considerably stronger. The converse also holds true, as seen in FIGS. 5-7, when optical properties are plotted versus ash content. At equal ash content, the direct-loaded handsheets exhibit better optical properties than the fiber-loaded handsheets of the invention.
Conclusions
It has been demonstrated that fiber loading with calcium carbonate can be accomplished by an in situ reaction between calcium oxide (or hydroxide) and carbon dioxide in high consistency dewatered crumb pulps. A pressurized Sprout-Bauer disk refiner adequately serves as both reaction chamber and as a means for obtaining a good dispersion of filler and fiber. SEM examination has revealed the presence of calcium carbonate crystals on both external fiber surfaces and within the cell lumen; and x-ray microprobe analysis indicates the presence of calcium within the cell wall. Optimum conditions for fiber loading using the pressurized refiner occur at pulp consistency of 18% for softwood pulp and 21% for hardwood pulp.
In some respects, handsheet properties prepared from fiber-loaded pulp outperformed direct loaded handsheets. When compared at equal filler content and equal freeness, the fiber-loaded handsheet exhibited greater bursting strength. This indicates that comparable burst strength can be obtained at higher ash content for handsheets made from fiber loaded pulp than handsheets made from direct loaded pulp. Also, at the same burst strengths, similar optical properties are obtained. This permits lower cost calcium carbonate to be substituted for higher cost fiber at no loss in burst or optical properties. This is a potential large saving in papermaking costs.
At equal ash contents, the poorer optical properties in comparison to the direct loaded sheets is partly understandable because the papermakers' carbonate was specifically designed in terms of crystal morphology and particle size to achieve maximum scattering power. In addition, filler in close contact with cell-wall material (as for example inside cell lumen) may inherently scatter less because the difference in refractive index between filler and cell-wall material is smaller than the difference in refractive index between filler and air.
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The present invention relates to a method for loading a chemical compound within the fibers of a fibrous material and to the fibrous materials produced by the method. In the method, a fibrous cellulose material is provided which consists of a plurality of elongated fibers having a fiber wall surrounding a hollow interior. The fibrous material has a moisture content such that the level of water ranges from 40-95% of the weight of the fibrous material and the water is positioned substantially within the hollow interior of the fibers and within the fiber walls of the fibers. A chemical is added to the fibrous material in a manner such that the chemical is disposed in the water present in the fibrous material. The fibrous material is then contacted with a gas which is reactive with the chemical to form a water insoluble chemical compound. The method provides a fibrous material having a chemical compound loaded within the hollow interiors and within the fiber walls of the plurality of fibers.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a holder for a drive piston of a setting tool.
2. Description of the Prior Art
European Publication EP-O 346275 B1 discloses an explosive powder charge-operated setting tool including a piston guide and a drive piston displaceable in the piston guide. The piston guide has radial openings facing the drive piston, and spring-biased braking balls engaging the drive piston. The spring, which applies a biasing force to the braking balls is formed as a ring spring for applying a radially acting, with respect to the piston, biasing force to the braking balls. The ring spring is provided on its inner profile with a bearing surface acting on the braking ball. The bearing surface is inclined to the piston at an acute angle that opens in a direction opposite a setting direction. In the ignition ready position of the drive piston, the braking balls engage the outer surface of the drive piston under the action of the ring spring. When the drive piston moves in the setting direction, it entrains the braking balls therewith. The braking balls expand the ring spring, which results in the bearing surface transmitting the radial biasing force to the braking balls in the direction toward the drive piston. The braking balls are pressed radially against the piston body by the ring spring. Even with a small displacement of the drive piston in a direction opposite the setting direction, the braking effect can be substantially reduced or eliminated, as the braking balls displace in the same direction as the drive piston, unloading the ring spring. After being unloaded, the spring washer does not press any more the braking balls against the piston body. Further, a possibility still remains that the drive piston would be displaced, before ignition or firing of the setting tool, in the setting direction as a result of, e.g., the setting tool being pressed too hard against a constructional component. The displacement in the return direction is effected due to cooperation of the spring washer with the braking balls.
U.S. Pat. No. 4,162,033 discloses a setting tool with a braking element that continuously applies a braking force to the drive piston.
An object of the present invention is to provide a piston holder having a simplified design and which would reliably retain the drive piston in its ignition-ready position in the absence of ignition.
SUMMARY OF THE INVENTION
This and other objects of the present invention, which will become apparent herein after, are achieved by providing a piston holder for a drive piston of a setting tool and including a support or a carrier for two expansion legs for frictionally receiving the drive piston therebetween, which carrier is fixedly secured in the setting tool.
The two expansion legs extend at an acute angle to each other and are resiliently deflectable relative to each other, forming together a resilient clamping device. The expansion legs overlap the drive piston in such a way that the inner edges of the two expansion legs apply pressure to approximately diametrically opposite circumferential sections of the drive piston. Advantageously, the two expansion legs lie in a plane that forms with the axial or drive-out direction of the drive piston an acute angle opening toward the front end of the setting tool.
When the drive piston moves in the setting, drive-out direction, i.e., toward the front end of the setting tool, the friction force, which is applied by the expansion legs to the drive piston or to its body, increases. With increase of the displacement path of the drive piston, a holding or braking force acting on the drive piston also increases due to the increase of the wedge action between the expansion legs and the drive piston. However, when the drive piston-displacing force exceeds a predetermined value, the expansion legs elastically expand, releasing the drive piston. In this way, the expansion legs act as a quasi overload protection means. Upon its release, the drive piston just slides through the guide channel and drives an object, e.g., a fastening element in, e.g., a constructional component. In this way, practically, there is obtained a speed-dependent friction coefficient that provides for reduction of friction at a high relative speed between the drive piston and the expansion legs. A total braking or a complete stop in this way is prevented.
The expansion legs do not hinder return movement of the drive piston when it returns to its initial, ignition-ready position after the completion of a drive-in or setting process, as the friction between the drive piston and the expansion legs is still very small.
Due to the prestress of the expansion legs relative to each other, a small pressure is constantly applied to the drive piston or its body. Thereby, the drive piston is reliably held in its ignition-ready position in the absence of ignition of the setting tool. If an undesirable displacement of the drive piston takes place as a result, e.g., of the setting tool being pressed too hard against a constructional component, the expansion legs would become loaded in the drive piston drive-out direction, whereby a restoring force is generated that provides for displacement of the drive piston into its initial position. The piston holder simultaneously provides for reduction of undesirable rebounds of the drive piston.
Generally, both expansion legs can be formed as separate parts securable on their carrier. However, according to an advantageous embodiment of the present invention, the expansion legs form legs of a V-shaped spring, forming parts of a one-piece element. Forming the expansion legs as the legs of a V-shaped spring facilitates their mounting and reduces manufacturing costs of the piston holder. The spring can be wound with its other end about a bolt secured in the carrier. This provides for preloading of the spring in the direction opposite the setting direction. Because of such preloading of the V-shaped spring, the expansion legs cannot rotate in the direction opposite the setting direction. For preventing the rotation of the expansion legs in the direction opposite the setting direction, also a suitable stop can be provided.
The novel features of the present invention, which are considered as characteristic for the invention, are set forth in the appended claims. The invention itself, however, both as to is construction and its mode of operation, together with additional advantages and objects thereof, will be best understood from the following detailed description of preferred embodiments when read with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The drawings show:
FIG. 1 a partially cross-sectional side view of a setting tool that can be equipped with a piston holder according to the present invention;
FIG. 2 a cross-sectional view of the setting tool shown in FIG. 1 in the region of the front end of the drive piston; and
FIG. 3 a partial axial cross-sectional view in the region of the front end of the drive piston.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A piston holder according to the present invention can be used with a setting tool a partially cross-sectional view of which a shown in FIG. 1 . The setting tool, which is shown in FIG. 1, is an explosive power charge-operated tool. However, the inventive piston holder can also be used in a setting tool driven upon ignition of an air-fuel mixture.
The setting tool, which is shown in FIG. 1, has a housing 1 with a handle 2 and a trigger 3 which, in the embodiment shown in FIG. 1, is provided in the handle. A stop socket 4 is screwed to the housing 1 at the housing end facing in the setting direction of the setting tool. A two-part piston guide 5 is displaceably arranged in the housing 1 . The piston guide 5 is formed of rear and front parts 6 and 7 , respectively. A drive piston 8 is arranged in the piston guide 5 . The drive piston 8 has its head 9 displaceable in the rear part 6 and its body 10 displaceable in the front part 7 . An inflow channel 12 for explosion gas of an explosive power charge opens into guide bore 11 of the part 6 at the rear end of the bore 11 . At its front end, the part 6 has breakthroughs 13 for releasing air, which is accumulated in front of the piston head 9 of the piston 8 in the piston drive-out or setting direction. The front end region of the rear part 6 concentrically overlaps the rear region of the front part 7 . The front part 7 extends beyond the stop socket 4 in the setting direction and forms a delivery tube. The rear end of the front part 7 can extend in form of a tubular projection into the guide bore 11 , forming a stop limiting the travel of the drive piston 8 .
The piston holder according to present invention can be located in a receiving region 14 which is formed in the connection region of the front and rear parts 6 , 7 .
A first embodiment of a piston holder according to the present invention is shown in FIGS. 2-3 which, as discussed, show radial and axial cross-sections of the front region of the setting tool shown in FIG. 1 .
The piston body 10 is guided in the guide channel 15 formed in the front part 7 of the piston guide 5 . At the rear end of the front part 7 , there is secured a bolt 16 that extends transverse to the axial direction 17 of the guide channel 15 . A leaf spring 18 is wound about the bolt 16 . An end 20 of the spring 18 , which faces in the drive piston drive-out direction 19 , setting direction, is supported at a shoulder 21 provided in the front part 7 . The other end of the leaf spring 18 , remote from the front end of the setting tool, passes in two expansion legs 22 , 23 that form with each other a V-shaped profile. The expansion legs 22 , 23 extend a short distance in the direction toward the rear end of the setting tool and then extend at an obtuse angle in a direction toward the piston body 10 and apply pressure with their respective inner edges to respective circumferential sections of the piston body 10 . The expansion legs 22 , 23 lie in a plane that forms an acute angle α with the drive-out direction of the drive piston 8 , opening toward the front end of the tool. The sections of the expansion legs 22 , 23 , which extend parallel to the axial direction 17 of the drive piston 8 , are received in a longitudinal groove 24 formed in the inner surface of the rear part 6 , and the sections of the expansion legs 22 , 23 , which extend toward the piston body 10 , extend through an opening 25 formed in the front part 7 . The spring 18 can also be so formed that after the spring 18 being wound about the bolt 16 , the expansion legs 22 , 23 are sidewise wound about the spring front end 20 .
Generally, the above-mentioned bolt 16 is not absolutely necessary. Rather, the spring 18 can be formed as a cantilevered spring. When the drive piston 8 with its body 10 is displaced in its drive-out direction, the expansion legs 22 , 23 , because of friction between the legs 22 , 23 and the piston body 10 , will be rotated, in FIG. 3, clockwise, with the front spring end 20 being supported against the inner surface of the rear part 6 . When no explosive force acts on the drive piston 8 , the spring 18 brings, with its expansion legs 22 , 23 , the drive piston 8 in its initial, ignition-ready position, as the expansion legs 22 , 23 would rotate counterclockwise, becoming loose.
However, when the drive piston 8 moves, upon application of the explosive force, further in its drive-out direction, the legs 22 , 23 elastically expand when the friction between the legs 22 , 23 and the piston body 10 , is overcome, releasing the drive piston 8 that now can slide through between the legs. The expansion legs 22 , 23 of the spring 18 do not hinder in any substantial manner the return movement of the drive piston 8 as the friction between the drive piston 8 and the legs 22 , 23 is substantially reduced.
Though the present invention was shown and described with references to the preferred embodiment, such is merely illustrative of the present invention and is not to be construed as a limitation thereof, and various modifications of the present invention will be apparent to those skilled in the art. It is, therefore not, intended that the present invention be limited to the disclosed embodiments or details thereof, and the present invention includes all variations and/or alternatives embodiments within the spirit and scope of the present invention as defined by the appended claims.
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A piston holder for a drive piston ( 8 ) of a setting tool and having a carrier ( 7 ) for two expansion legs ( 22, 23 ) for frictionally receiving the drive piston ( 8 ) therebetween, with the carrier ( 7 ) being fixedly secured in the setting tool.
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BACKGROUND OF THE INVENTION
This invention relates generally to the protection of wire ropes from corrosive conditions and more particularly to the sealing of wire ropes against corrosive environments by the use of plastic foam compositions.
Various expedients have in the past been used to bar the entrance of water and moisture into the interior of wire ropes and strands. Such expedients have included the use of heavy lubricants, external plastic coatings and the encapsulation of individual wires, strands or even an entire wire rope in solid plastic sheaths. Lubricants are soon lost from an otherwise unprotected strand or rope while external protective coatings are subject to wear and upon rupture at any point will admit moisture to the interior of the rope or strand. Solid encapsulation, on the other hand, seriously interferes with the flexibility of the rope or strand and is also difficult to attain.
U.S. Pat. Nos. 3,681,911 and 3,778,994 to D. V. Humphries and 3,800,522 to C. R. Hughes et al. as well as several other recently issued patents disclose a successful alleviation of many of these previous problems. In these disclosures a working wire rope or a single working strand is impregnated with a liquid plastic foam composition during fabrication and said liquid is then converted to a flexible foam by the application of heat. The foam material is adherent to the individual wires and because of its low overall density does not decrease the flexibility of the rope or strand. The exterior of the rope or strand may be covered with a thin layer of foam or with a layer of denser plastic or may more preferably be wiped clean, particularly in working ropes and strands, i.e. those which are used over sheaves and pulleys and the like or otherwise used in dynamic operations as opposed to static use such as guy lines and other types of permanent anchor lines. The bare wire surfaces resist abrasion and wear in these cases while the interior foam material between the wires, which preferably closely encloses all but the outer surfaces of the wires, prevents the access of water and moisture to the interior surfaces of the wires.
While these previous wire ropes and strands have been very successful, there are some applications in which it may not be desired to fully impregnate a wire rope with plastic. For example, in some installations it may be desired to make use of a permanently lubricated wire core or fiber core in a rope. Methods of completely or partially encapsulating a lubricant permanently in a wire rope core are disclosed to U.S. Pat. Nos. 3,705,489 to C. W. Smollinger, 3,824,777 to P. P. Riggs and 3,874,158 to F. Chiapetta et al. Where it is desired to use a natural or synthetic fiber core in a wire rope, it has often been found to be impractical to encapsulate all of the outer strands with a plastic foam and then heat cure the assembly all at one time because the heat of the foaming operation deleteriously affects the properties of the fiber core. Most experimental plastic foam impregnated wire ropes have, therefore, been made with the individual strands of the rope impregnated with plastic foam prior to stranding, or closing, of the individual strands together into a rope. In these experimental ropes the core of the rope has been a lubricated fiber core, but lubricated wire rope cores have also been used.
It is often desirable even in plastic foam filled ropes to prelubricate the surface of the strand with a heavy lubricant such as a heavy grease or asphalt composition which serves to protect the outer exposed surfaces of the wires from the environment prior to and during use and also serves during use to lubricate the surface of the rope. Frequently a reel of wire rope will be retained in very corrosive environmental conditions for long periods prior to and in between use. For example, a so-called shrimp rope for use on shrimp boats may remain on a reel in marine environments for several weeks or more prior to use and for shorter intermittent periods during use. While a plastic foam impregnated wire rope will be inherently quite corrosion resistant, as compared with an unimpregnated rope, portions of the outer wires will usually still be exposed and subject to corrosion which may tend to migrate even under the edges of the plastic as corrosion products such as rust lift the edges of the plastic. It has been found, therefore, that it is often desirable to apply the usual outer heavy lubrication ordinarily applied to conventional ropes under such conditions to the foam plastic impregnated ropes as well. Naturally it is desirable for such lubrication to remain on the surface of the rope as long as possible, both for lubrication during use and for corrosion protection.
BRIEF SUMMARY OF INVENTION
It has been unexpectedly found that where the outer strands of a wire rope are preimpregnated with plastic foam material and the strands then closed or stranded into a rope and the outer portions covered with a lubricant, that due to the excellent surface properties of the foam filled strand, the external lubricant is retained very significantly longer than a similar lubricant on a conventional wire rope. While the reason for such improved adhesion is not completely understood it has been observed that the surface of such ropes is uneven and of a porous nature with loose uneven fibers protruding from the surface, apparently due to a shredding and abrasion action upon the exterior of the plastic foam material adjacent to the surface of the strands during the closing of the strands into the rope. Small but definite pores or pockets can be detected in the surface of the foam plastic and just below the surface. It is theorized that the combined porous and fibrous character of the surface is effective to significantly increase the overall retention of a surface lubricant upon the rope.
It has also been unexpectedly found that the peculiar surface properties of the individual foam impregnated strands after closure into a rope serves very effectively to maintain a tight seal between adjacent outer strands of the wire rope, which seal will prevent loss of lubricant from a central fiber core or lubricated wire core of a rope having a lubricated central core. Such central core may comprise a lubricated fiber core, a lubricated wire strand core or an independent wire rope core, commonly referred to as an IWRC. While the exact reason for the excellent sealing between the outer strands is again not definitely known, it is believed that the rough, porous, fibrous character of the surface of the foam filled outer wire strands of the rope after closing about the core serves to hold lubricant securely between the strands and prevent escape of the internal lubricant from the core of the wire rope. The rough fibrous character of the surface together with the lubricant very effectively seals all large openings between the outer strands and seals the internal lubricant inside the rope.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal view of a rope made in accordance with the present invention showing the retentive surface before and after application of a surface lubricant.
FIG. 2 is a cross sectional of the rope shown in FIG. 1 at 2--2 in FIG. 1.
FIG. 2A is an enlarged view of a portion of FIG. 2 more clearly showing the characteristics of the surface of the foamed plastic after the closing operation.
FIG. 2B is a cross sectional of the rope shown in FIG. 1 at 2B--2B, after the application of a heavy lubricating grease or oil to the outside of the strand.
FIG. 3 is a schematic elevation of a manufacturing line for the making of the wire rope of the invention.
FIG. 4 is a cross sectional view of a modified rope made in accordance with the present invention.
FIG. 5 is a cross sectional view of a further embodiment of a rope in accordance with the invention.
FIG. 6 is a cross sectional view of a still further embodiment of a rope in accordance with the invention.
FIG. 7 is a cross sectional view of an additional embodiment of the rope of the invention.
FIG. 8 is a cross sectional view of a still further embodiment of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIGS. 1 and 2 there are shown an elevation and a cross section respectively of a wire rope 11 made in accordance with the present invention. This rope has a central fiber core 13 formed of a twisted strand of polypropylene fibers impregnated with a heavy lubricating oil 15. Other conventional fibers such as the traditional sisal fibers or else synthetic fibers other than polypropylene may also be used. Surrounding the fiber core are six outer wire strands 17 each comprised of nineteen wires twisted together into a strand and closed about the outside of the central fiber core 13. The outer strands 17 are impregnated with a plastic foam material 19. The outer wires 21 of the strands 17 are substantially bare and the surface of the wires protrude slightly through the plastic foam except for a number of fibers 23 which protrude from the surface from between and to some extent over the individual wires. Between the substantially bare wires the surface of the foamed plastic material has in addition to the protruding fibers 23, a number of variously dimensioned small pores 24 opening to the surface and sometimes partially interconnected below the surface. While the foamed plastic is, of course, inherently porous the pores in the surface tend to be larger than the normal foamed porosity. Between the individual outer strands these pores 24 and fibers 23 are compressed between the strands and impregnated with heavy lubricant derived from the lubricated central core.
FIG. 2A is an enlarged view of a portion of FIG. 2 in which the conformation of the foamed plastic 19 between the outer wires 21 of an individual strand 17 can be more clearly seen. A slight depression in the plastic surface 20 between wires is visible. Under the surface 20 are pores 24 opening to the surface and in some cases interconnected with each other. Uneven fibers, or shreds of plastic, 23 protrude from the surface of the foam plastic. Since the strands 17 are spirally wound the background shows a more or less even circumference of plastic surmounted with the fibers 23 about the entire circumference of the strand.
In FIG. 2B a heavy outer layer of lubricant 25 has been applied to the outer surfaces of the outer strands as both a lubricant and corrosion inhibiting medium. The individual outer fibers 23 of the strand extend into this outer layer and are believed to prevent such lubricant layer from being dislodged from the surface by mechanical means and expecially by exposure to sea water and the like. The pores 24 in the surface of the foamed plastic material are also filled with lubricant and serve as small protected reservoirs of lubricant. The lubricant layer is very effective in preventing premature corrosion of the exposed outer surfaces of the outer wires of the outer strands, which wires are not coated with foam or other plastic in order to provide a good wear surface for passage over sheaves and the like.
In FIG. 3 there is shown in schematic form an apparatus for making the rope shown in FIGS. 1, 2, 2A and 2B. A twisted wire strand is first made from a series of wires 31 held on a series of reels 33 all but one 33a of which are mounted on a rotatable flyer 35 driven by a motor 37. The individual wires 31 are passed from the rotating flyer during operation into a closing die 39 where the wires are closed into a twisted strand 40 which is then passed about a capstan 41 and onto a storage reel 61. Before passing into the closing die 39 the individual wires pass through a spray of a liquid foamable plastic composition which passes from a spray head 43 onto the wires 31. Excess foamable plastic falls into a reservoir 45 and is recirculated via pump 47 to the spray head 43. After passing through the closing die 39 and being formed into the twisted strand 40 the wires are exposed to heat in an induction furnace 58 where the foamable plastic material is foamed by the heat generated. This curing operation may be accomplished in line as shown or alternatively as a separate operation. After foaming the strand is passed through a rotating or stationary die, which will usually be a rubber or other elastomeric material die 53, which serves to wipe the outer surface of the strand so that only a very thin layer of densified plastic is left on the surface. The surface of the plastic material is still plastic and somewhat tacky in the elastomeric die 53 and although the plastic is below its heat distortion temperature it still exhibits poor tear strength. Consequently some shredding and tearing of the surface occurs which seems to accelerate and increase later shredding of the plastic surface when the individual strands are closed into a wire rope. The strand then passes through a weir type cooling trough 55 where the foamed plastic material is hardened and finally passes over the capstan 41 and onto the storage reel 61. All this is essentially as shown and claimed in the previous patents referred to above.
The plastic foam impregnated strand 59 on the reel 61 is next rewound on a series of bobbins 62 and mounted in a second flyer 63. A plastic fiber core strand 65 is taken from a reel 67 and passed down into a heavy oil bath 69 under a roller 71 and then up over guide rollers 73 through the flyer and into a closing die 75. The flyer 63 is rotated by a motor 77 and the wire strand 59 on the individual bobbins 62 is passed from the reels to the closing die 75 where it is closed about the lubricated central plastic core into a twisted wire rope which is drawn through a lubricating oil bath 79 to coat the outer surface of the strands and rope with lubricant and then over a capstan 81 and onto a storage reel 83. The rope on the reel 83 may be stored in the weather for long periods without corrosion of the outer wires of the strand.
In many cases the fiber core strand 65 will have been luricated when the individual fibers were stranded, woven or braided into a core strand. In such case the passage through the heavy oil or heated grease in bath 69 will serve to ensure thorough lubrication. However, in some cases the original lubrication of the core will be deemed sufficient and passage through the bath 69 may be dispensed with. The lubricant applied will be any suitable core or wire rope lubricant well know to those skilled in the art.
As the strands 59 are drawn through the closing die 75 the plastic on and at the surface of the strand is roughened and shredded until the surface of the strand appears to be coated or covered with a thin mat of plastic fibers. Pores are also opened in the surface as the surface is shredded and abraded. These fibers together with the rough surface characteristics including the pores in the plastic appear to be responsible for the very excellent retention of lubricant upon the surface of the wire rope and for very effective sealing between the individual strands which prevents the escape of internal lubrication from the interior of the strand to the surface of the strand.
It will be understood that while the normal closing operation by which the outer strands are stranded about the core strand will be effective to roughen and shred the surface of the plastic, that other special roughening operations could be used. Such operations might for example consist of passing the stranded rope through an external abrading device of various types or even reheating the plastic at the surface of the strands and passing the stranded rope through an elastomeric wiping die.
The plastic foam can be of any suitable composition such as vinyl plastic having an organic nitrogen compound such as azodiacarbonamide as a foaming agent. This plastic when heated above the decomposition temperature of the organic nitrogen compound decomposes into nitrogen and carbon dioxide and expands the plastic into a foam. Another suitable composition would be a foamable polyurethane consisting of a thermosetting elastomer filled with expandable plastic beads. When exposed to heat the plastic of the beads softens and an entrapped gas therein expands the plastic into a foam. The polyurethane elastomer matrix provides cross linking. Any other plastic composition which is flexible, tough and adherent to metal may be used with a foaming agent to coat the strand.
In FIG. 4 there is shown in cross section a further embodiment of the invention in which the outer strands 59 of the rope are closed about a lubricated wire core instead of the fiber core shown in FIGS. 2 and 2B.
In FIG. 5 there is shown an embodiment of the invention in cross section in which the lubricated core is an independent wire rope core, or IWRC. In both FIGS. 4 and 5 the rough surface of the outer strands serves very effectively to maintain the lubricant of the core within the core. As the lubricant is forced between the strands it becomes entangled in the rough fibrous surface of the strands and is prevented from escaping while the mixture of heavy lubricant and matted plastic fibers effectively prevents any substantial penetration of sufficient water into the core to remove any significant amount of lubricant even over long periods of immersion.
In FIG. 6 there is shown in cross section a still further embodiment of the invention in which the central core of the rope is a foam impregnated wire strand. The same excellent surface adhesion of lubricant is attained in this strand, but no lubricant is necessary in the core. However, if desired the outside of the core may be coated with a lubricant which will then be maintained inside the rope by the fibrous surface of the outer strands. It will be understood that the foam impregnated wire core may be either a twisted wire core or an independent wire rope core.
In FIGS. 7 and 8 there are shown further embodiments of the invention similar to the embodiment shown in FIG. 4 in which the core of the rope is a lubricated wire rope core in FIG. 7 or a lubricated synthetic or sisal core in FIG. 8. As in FIG. 5 the rough surface of the outer foam filled strands serves very effectively to maintain the lubricant of the core within the core. In both embodiments shown respectively in FIGS. 7 and 8 where is no outer lubrication applied to the outer strands so that only the portions of the outer strands which are adjacent to the lubricated cores are lubricated. It is sometimes desired under modern ecological conditions to have no lubricant upon the surface of a rope which is to be used directly in a body of water in order to avoid contamination of the water by small amounts of the lubricant. In such cases it is also, of course, desirable, if a lubricated core is to be used in the rope, not to have lubricant escape from the core either. It has been found that the construction shown in FIGS. 7 and 8 is quite effective in maintaining the lubricant within the rope. The lubricant is prevented from passing between the strands by the rough surface of opposing strands which interact or interengage intimately together to prevent passage of lubricant and substantially seal the lubricant within the strand.
By the formation of a wire rope in accordance with the invention there is provided a wire rope having exceptional retention of surface lubricant and in those cases where an internal lubricant is used, of internal lubricant. The rope is economical to make and durable in service.
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A corrosion resistant rope in which the individual strands are sealed with a plastic foam impregnant and which exhibits excellent retention of lubrication is made by preimpregnating the outer strands of the rope with plastic foam material prior to closing the strands into a wire rope. The final rope may then be surface lubricated to provide temporary and long term corrosion resistance and lubrication to exposed surface wires.
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FIELD OF THE INVENTION
This invention relates to a device and method for protecting plants from cold weather.
BACKGROUND OF THE INVENTION
Many plants, such as tomatoes, have growing seasons shortened by cold weather, thus lessening food production. These plants can be started or grown in greenhouses, but this is expensive.
Various types of outdoor plant heaters exist. Smudge pots burn oil to warm plants, such as citrus trees. However, the use of smudge pots is unsatisfactory. Hot air and combustion products rise rapidly from the level of the plants, especially if there is a wind, and soot is produced during combustion.
Other plant heaters spray warm water over plants, but this can lead to over-watering and requires a continuous water source. Still other heaters circulate warm ground water through a thermal barrier adjacent to a plant before spraying the water over the plant or directly onto the ground.
Still other plant heaters employ vented, transparent plastic covers to enclose plants, but have no active heating element, relying instead on unpredictable and intermittent sunshine, and do not warm the roots of the plant.
U.S. Pat. No. 4,137,667 teaches a method of protecting a plant from cold weather by interposing a water layer enclosed in transparent plastic between the plant and the outside atmosphere. However, the device does not include a heater to prevent the water from freezing, nor a means for heating the roots of the plant.
U.S. Pat. No. 5,575,109 teaches a plant protection device with a double-walled enclosure. However, the portion of the device extending above the ground is single-walled and there is no disclosure of heated fluid within the double-walled portion of the enclosure.
In summary, while other plant heaters exist, no one has developed a gardening device or method that warms a plant by surrounding it with a double-walled container full of fluid warmed by a heater, yet does not require a continuous water source.
The primary objective of this invention is to fulfill the above described need with a new gardening device consisting of a double-walled enclosure, adapted for filling with fluid, of a size sufficient to completely encircle a plant, fluid filling the double-walled enclosure and a heater operatively connected to a wall of the enclosure for heating the fluid within the double-walled enclosure.
A further object of the present invention is the provision of a method for keeping a plant warm.
These and other objects, features and/or advantages of the present invention will become apparent from the specification and claims.
SUMMARY OF THE INVENTION
The foregoing objects may be achieved by a device comprising a double-walled enclosure, adapted for filling with fluid, of a size sufficient to encircle a plant, fluid filling the double-walled enclosure and a heater operatively connected to the wall of the enclosure.
According to another feature of the invention, the device includes an elongated heating member extending from above ground to a determined depth below ground, and a second heater connected to and causing heating of the elongated heating member.
According to another feature of the invention, the device includes a vented lid removably mounted to the top of the double-walled enclosure.
According to another feature of the invention, the device includes a trellis removably mounted to the double-walled enclosure for supporting a plant growing above the double-walled enclosure.
According to another feature of the invention, the device includes a cover surrounding the trellis.
According to another feature of the invention, the device includes a fluid circulation pump for circulating fluid within the double-walled enclosure.
The method of the present invention comprises positioning a double-walled enclosure around a plant and adjustably heating the fluid to maintain the plant above a critical temperature.
According to another feature of the invention, the method includes positioning a heating member underground near the roots of the plant, and applying heat to the heating member.
According to another feature of the invention, the method includes positioning a vented lid on top of the enclosure.
According to another feature of the invention, the method includes positioning a trellis on top of the enclosure.
According to another feature of the invention, the method includes positioning a cover around or over the trellis.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view of a gardening device.
FIG. 2 is an exploded view of the gardening device.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1 and 2, 10 designates a gardening device.
A double-walled enclosure 12 includes an outer wall 14 , an inner wall 16 , a top wall 18 and a bottom wall 20 . The double walled enclosure 12 may be made of any suitable material such as plastic. The walls define an annular space 22 . The walls may be opaque, translucent or, preferably, transparent. The annular space is filled with fluid 24 through a fill hole 26 that is sealed with a cap 28 . The fluid 24 may be water, but aqueous solutions and other fluids may be used.
Pockets 30 attach to the outer wall 14 and include receptacles 31 which removably receive and support vertical members 32 of the trellis 34 . The trellis 34 may be made of any suitable material such as plastic, wood or metal. Horizontal members 36 of the trellis 34 connect the vertical members 32 . While the trellis 34 is shown to be cylindrical, it may also lie in a single plane or be square, or any other enclosed shape that forms a cage for containing the plant being grown. A plastic cover 38 is cylindrical in shape and fits around the trellis 34 and is fastened with fasteners 40 . The plastic cover 38 may be opaque, translucent or, preferably, transparent. The fasteners 40 may be hook and loop fasteners.
A first heater 42 and circulation pump 44 attach to the outer wall 14 . The first heater 42 may be an electric heater. Heater 42 is shown with a heating element inside annular space 22 , but it is also possible to place the heater totally outside the outer wall 14 . Furthermore, the heater 42 may be placed inside the inner wall 16 . When placed inside inner wall 16 it may be either totally inside inner wall 16 or it may have a heating element positioned inside annular space 22 . The circulation pump 44 may be an electric circulation pump. A removable, vented lid 46 attaches to the top wall 18 . The vented lid 46 may be made out of any suitable material such as plastic and may be opaque or, preferably, transparent.
Stakes 48 may optionally be attached to the bottom wall 20 for fastening the enclosure to the ground 50 . The stakes 48 may be made of any suitable material such as plastic, wood or metal. The top of a plant 52 sits inside the cylindrical space defined by the inner wall 16 . The roots of the plant 54 sit beneath the ground 50 under the top of the plant 52 .
A second heater 56 attaches to the outer wall 14 . The second heater 56 may be an electrical heater. Attached to the second heater 56 is an elongated heating member 58 buried in the ground 50 near the roots of the plant 54 . It is possible to eliminate second heater 56 and instead mount heating member on outer wall 14 or inner wall 16 in such a manner that it conducts heat from the heated water through the walls 16 or 14 to heat the soil beneath roots 54 .
A gardener can employ the gardening device 10 early in a growing season to get a head start on a garden. After planting a seed or plant outdoors, the gardener can encircle the seed or plant with the double-walled enclosure 12 . The stakes 48 anchor the double-walled enclosure 12 to the ground. The gardener can then fill the double-walled enclosure 12 , through the fill hole 26 , with water, an aqueous solution or other fluid 24 and cap the fill hole with the cap 28 . The gardener can heat the fluid 24 by adjusting the first heater 42 that is operatively connected to the double-walled enclosure 12 . The heated fluid 24 , in turn, warms the plant. The gardening device 10 optionally includes the circulation pump 44 to circulate the warmed fluid from the first heater 42 to all through the annular space 22 .
Once the double-walled enclosure 12 is around the plant, such as a tomato plant, the gardener can optionally pile dirt inside the enclosure around the stem of the plant to root up the stem. Optionally, the garden device 10 includes the second heater 56 connected to and causing heating of the elongated heating member 58 . The gardener can bury the elongated heating member 58 in the ground 50 to warm the roots of the plant 54 .
The drawings show the double walled structure 12 resting on the upper surface of the soil 50 , but it is also possible to excavate soil 50 and bury the lower end of double walled structure several inches in the soil 50 . This will further stabilize device 10 and will also impart heat to the top several inches of soil 50 .
The gardening device optionally includes the vented lid 46 removably mounted to the top of the double-walled enclosure 12 . The vented lid 46 helps to retain heat around the plant, yet allows some air-circulation. Once the plant has grown sufficiently, the gardener can remove the vented lid 46 from the top of the double-walled enclosure and, optionally, mount the trellis 34 into the receptacles 31 to support the plant in growing above the double-walled enclosure 12 .
The double-walled enclosure 12 and vented lid 46 are both preferably transparent to let the sun shine in onto the plant.
Late in the growing season, the gardener can turn on the first heater 42 and/or second heater 56 again and wrap the trellis 34 with the plastic cover 38 . The gardener can even warm adjacent plants by placing a tarp over the entire gardening device 10 and adjacent plants. The warmth from the first heater 42 and/or second heater 56 is then distributed to all plants under the tarp.
The gardener may reuse the gardening device 10 from one growing season to the next.
In the drawing and specification, there has been set forth a preferred embodiment of the invention, and although specific terms are employed, these are used in a generic and descriptive sense only and not for purposes of limitation. Changes in the form and the proportion of parts as well as in the substitution of equivalents are contemplated as circumstances may suggest or render expedient without departing from the spirit or scope of the invention as further defined in the following claims.
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A device and method are disclosed for protecting plants from cold weather damage. A transparent, fluid-filled enclosure encircles a plant above the ground. A heater warms the fluid, which in turn warms the plant.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Patent Application No. 60/434,902, filed Dec. 19, 2002, herein incorporated by reference in its entirety for all purposes.
FIELD OF THE INVENTION
[0002] This invention is directed to indazole compounds that mediate and/or inhibit hyperproliferative disorders, such as cancer and ophthalmic diseases, and the activity of certain protein kinases, and to pharmaceutical compositions containing such compounds. The invention is also directed to the therapeutic or prophylactic use of such compounds and compositions, and to methods of treating hyperproliferative disorders, such as ophthalmic diseases and cancer as well as other disease states associated with unwanted angiogenesis and/or cellular proliferation, by administering effective amounts of such compounds.
BACKGROUND OF THE INVENTION
[0003] Hyperproliferative disorders and several diseases and conditions of the posterior segment of the eye threaten vision. Age related macular degeneration (ARMD or AMD), choroidal neovascularization (CNV), retinopathies (e.g., diabetic retinopathy, vitreoretinopathy, retinopathy of prematurity), retinitis (e.g., cytomegalovirus (CMV) retinitis), uveitis, macular edema, and glaucoma are several examples.
[0004] Age related macular degeneration (ARMD or AMD) is the leading cause of blindness in the elderly. ARMD attacks the center of vision and blurs it, making reading, driving, and other detailed tasks difficult or impossible. About 200,000 new cases of ARMD occur each year in the United States alone. Current estimates reveal that approximately forty percent of the population over age 75, and approximately twenty percent of the population over age 60, suffer from some degree of macular degeneration. “Wet” ARMD is the type of ARMD that most often causes blindness. In wet ARMD, newly formed choroidal blood vessels (choroidal neovascularization (CNV)) leak fluid and cause progressive damage to the retina. In the particular case of CNV in ARMD, two main methods of treatment are currently being developed, (a) photocoagulation and (b) the use of angiogenesis inhibitors.
[0005] However, photocoagulation can be harmful to the retina and is impractical when the CNV is in proximity of the fovea. Furthermore, photocoagulation often results in recurrent CNV over time.
[0006] Angiogenesis is the mechanism by which new capillaries are formed from existing vessels. When required, the vascular system has the potential to generate new capillary networks in order to maintain the proper functioning of tissues and organs. In the adult, however, angiogenesis is fairly limited, occurring only in the process of wound healing and neovascularization of the endometrium during menstruation. See Merenmies et al., Cell Growth & Differentiation, 8, 3-10 (1997). On the other hand, unwanted angiogenesis is a hallmark of several diseases, such as retinopathies, psoriasis, rheumatoid arthritis, age-related related macular degeneration (AMD), and cancer (solid tumors). Folkman, Nature Med., 1, 27-31 (1995). Protein kinases which have been shown to be involved in the angiogenic process include three members of the growth factor receptor tyrosine kinase family: VEGF-R2 (vascular endothelial growth factor receptor 2, also known as KDR (kinase insert domain receptor) and as FLK-1); FGF-R (fibroblast growth factor receptor); and TEK (also known as Tie-2).
[0007] Oral administration of anti-angiogenic compounds is also being tested as a systemic treatment for ARMD. However, due to drug-specific metabolic restrictions, systemic administration usually provides sub-therapeutic drug levels to the eye. Therefore, to achieve effective intraocular drug concentrations, either an unacceptably high dose or repetitive conventional doses are required. Various implants have also been developed for delivery of anti-angiogenic compounds locally to the eye. Examples of such implants are disclosed in U.S. Pat. No. 5,824,072 to Wong, U.S. Pat. No. 5,476,511 to Gwon et al., and U.S. Pat. No. 5,773,019 to Ashton et al., each of which is herein incorporated by reference in their entireties for all purposes.
[0008] The compounds of the present invention are improved anti-angiogenic agents that can be used alone or in combination.
SUMMARY OF INVENTION
[0009] The present invention provides compounds having the following structures:
or a pharmaceutically acceptable salt or pharmaceutically acceptable solvate thereof.
[0010] In another embodiment, the present invention relates to a compound represented by the formula
or a pharmaceutically acceptable salt or a pharmaceutically acceptable solvate thereof.
[0011] In another embodiment, the present invention relates to 6-(2-Prop-2-ynylcarbamoyl-phenylamino)-1H-indazole-3-carboxylic acid methylamide.
[0012] In another embodiment, the present invention relates to 2-{3-[2-(5-Ethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-prop-2-ynyl-benzamide.
[0013] In another embodiment, the present invention relates to N-Cyclopropyl-2-{3-[(E)-2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0014] In another embodiment, the present invention relates to N-Methoxy-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0015] In another embodiment, the present invention relates to N-Allyloxy-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0016] In another embodiment, the present invention relates to N-Isopropoxy-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0017] In another embodiment, the present invention relates to N-Cyclopropyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0018] In another embodiment, the present invention relates to 1-Methyl-1H-pyrrole-2-carboxylic acid.
[0019] In another embodiment, the present invention relates to N′-(1-{2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-phenyl}-methanoyl)-hydrazide.
[0020] In another embodiment, the present invention relates to N-Benzyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0021] In another embodiment, the present invention relates to N-(2-Methoxy-benzyl)-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0022] In another embodiment, the present invention relates to N-Furan-2-ylmethyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0023] In another embodiment, the present invention relates to N-Cyclobutyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0024] In another embodiment, the present invention relates to N-(2-Methyl-allyl)-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0025] In another embodiment, the present invention relates to N-Prop-2-ynyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0026] In another embodiment, the present invention relates to 2-{3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(4-hydroxy-but-2-ynyl)-benzamide.
[0027] In another embodiment, the present invention relates to N-(prop-2-ynyl)-2-{3-[(E)-2-(2,4-dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0028] In another embodiment, the present invention relates to 2-{3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(2-methyl-allyl)-benzamide.
[0029] In another embodiment, the present invention relates to N-(3-Cycloprop-2-ynyl)-2-{3-[(E)-2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0030] In another embodiment, the present invention relates to Acetic acid 4-(2-{3-[(E)-2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzoylamino)-but-2-ynyl ester.
[0031] In another embodiment, the present invention relates to 2-{3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(4-hydroxy-but-2-ynyl)-nicotinamide.
[0032] In another embodiment, the present invention relates to N-(3-Cyclopropyl-prop-2-ynyl)-2-{3-[(E)-2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-nicotinamide.
[0033] In another embodiment, the present invention relates to 2-{3-[(E)-2-(4-Methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-prop-2-ynyl-benzamide.
[0034] In another embodiment, the present invention relates to N-(2-Methyl-allyl)-2-{[(E)-2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0035] In another embodiment, the present invention relates to N-(3-Cycloprop-2-ynyl)-2-{3-[(E)-2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0036] In another embodiment, the present invention relates to 2-{3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-pyridin-2-ylmethyl-benzamide.
[0037] In another embodiment, the present invention relates to 2-{3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-pyridin-4-ylmethyl-benzamide.
[0038] In another embodiment, the present invention relates to N-(6-Methyl-pyridin-2-ylmethyl)-2-{3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0039] In another embodiment, the present invention relates to N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-{3-[(E)-2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0040] In another embodiment, the present invention relates to N-(1-Methyl-1H-benzoimidazol-2-ylmethyl)-2-{3-[(E)2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0041] In another embodiment, the present invention relates to N-(1-Methyl-1H-imidazol-2-ylmethyl)-2-{3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide.
[0042] In another embodiment, the present invention relates to 2-{3-[(E)-2-(4-Methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(4-hydroxy-but-2-ynyl)-benzamide.
[0043] In another embodiment, the present invention relates to N-(3-Cyclopropyl-prop-2-ynyl)-2-[3-(pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzamide.
[0044] In another embodiment, the present invention relates to N-(4-Hydroxy-but-2-ynyl)-2-[3-(pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzamide.
[0045] In another embodiment, the present invention relates to N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-[3-(pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzamide.
[0046] In another embodiment, the present invention relates to N-Prop-2-ynyl-2-[3-(pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzamide.
[0047] In another embodiment, the present invention relates to N-(4-Hydroxy-but-2-ynyl)-2-[3-(2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0048] In another embodiment, the present invention relates to N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-[3-(2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide.
[0049] The compounds of the present invention may have asymmetric carbon atoms. The carbon-carbon bonds of the compounds of the present invention may be depicted herein using a solid line ( ), a solid wedge or a dotted wedge The use of a solid line to depict bonds to asymmetric carbon atoms is meant to indicate that all possible stereoisomers at that carbon atom are included. The use of either a solid or dotted wedge to depict bonds to asymmetric carbon atoms is meant to indicate that only the stereoisomer shown is meant to be included. It is possible that compounds of the invention may contain more than one asymmetric carbon atom. In those compounds, the use of a solid line to depict bonds to asymmetric carbon atoms is meant to indicate that all possible stereoisomers are meant to be included. The use of a solid line to depict bonds to one or more asymmetric carbon atoms in a compound of the invention and the use of a solid or dotted wedge to depict bonds to other asymmetric carbon atoms in the same compound is meant to indicate that a mixture of diastereomers is present. Solutions of individual stereoisomeric compounds of the present invention may rotate plane-polarized light. The use of either a “(+)” or “(−)” symbol in the name of a compound of the invention indicates that a solution of a particular stereoisomer rotates plane-polarized light in the (+) or (−) direction, as measured using techniques known to those of ordinary skill in the art.
[0050] The inventive compounds of the present invention relate to a method of modulating and/or inhibiting the kinase activity of VEGF-R, FGF-R, a CDK complex, CHK1, LCK, TEK, FAK, and/or phosphorylase kinase by administering a compound of the present invention, or a pharmaceutically acceptable salt or pharmaceutically acceptable solvate thereof. Preferred compounds of the present invention may have selective kinase activity—i.e., they possess significant activity against one or more specific kinases while possessing less or minimal activity against one or more different kinases.
[0051] The inventive compounds of the present invention are useful for treating hyperproliferative disorders, such as ophthalmic diseases and cancer, and mediating the activity of protein kinases. More particularly, the compounds are useful as anti-angiogenesis agents and as agents for modulating and/or inhibiting the activity of protein kinases, thus providing treatments for ophthalmic diseases and cancer or other diseases associated with cellular proliferation mediated by protein kinases.
[0052] The inventive compounds of the present invention relate to pharmaceutical compositions, each comprising an effective amount of an agent selected from compounds of the present invention and pharmaceutically acceptable salts or pharmaceutically acceptable solvates thereof; and a pharmaceutically acceptable carrier or vehicle for such agent. The invention further provides methods of treating ophthalmic diseases/conditions and cancer as well as other disease states associated with unwanted angiogenesis and/or cellular proliferation, comprising administering effective amounts of such an agent to a patient in need of such treatment.
[0053] The inventive compounds of the present invention are useful for treating ophthalmic diseases, for example, age related macular degeneration (ARMD or AMD), retrolental fibroblasia, choroidal neovascularization (CNV), corneal neovascularization, retinopathies (e.g., diabetic retinopathy, vitreoretinopathy, retinopathy of prematurity), retinitis (e.g., cytomegalovirus (CMV) retinitis), uveitis, macular edema, and glaucoma.
[0054] Thus, within one aspect of the present invention methods are provided for treating neovascular diseases of the eye such as corneal neovascularization (including corneal graft neovascularization), comprising the step of administering to a patient a therapeutically effective amount of an anti-angiogenic composition to the cornea. A wide variety of disorders can result in corneal neovascularization, including for example, corneal infections (e.g., trachoma, herpes simplex keratitis, leishmaniasis and onchocerciasis), immunological processes (e.g., graft rejection and Stevens-Johnson's syndrome), alkali burns, trauma, inflammation (of any cause), toxic and nutritional deficiency states, and as a complication of wearing contact lenses.
[0055] Anti-angiogenic factors and compositions of the present invention are useful by blocking the stimulatory effects of angiogenesis promoters, reducing or inhibiting abnormal cell growth, reducing endothelial cell division, decreasing endothelial cell migration, and impairing the activity of the proteolytic enzymes secreted by the endothelium.
[0056] In a specific embodiment of any of the inventive methods described herein, the abnormal cell growth is cancer, including, but not limited to, lung cancer, bone cancer, pancreatic cancer, skin cancer, cancer of the head or neck, cutaneous or intraocular melanoma, uterine cancer, ovarian cancer, rectal cancer, cancer of the anal region, stomach cancer, colon cancer, breast cancer, uterine cancer, carcinoma of the fallopian tubes, carcinoma of the endometrium, carcinoma of the cervix, carcinoma of the vagina, carcinoma of the vulva, Hodgkin's Disease, cancer of the esophagus, cancer of the small intestine, cancer of the endocrine system, cancer of the thyroid gland, cancer of the parathyroid gland, cancer of the adrenal gland, sarcoma of soft tissue, cancer of the urethra, cancer of the penis, prostate cancer, chronic or acute leukemia, lymphocytic lymphomas, cancer of the bladder, cancer of the kidney or ureter, renal cell carcinoma, carcinoma of the renal pelvis, neoplasms of the central nervous system (CNS), primary CNS lymphoma, spinal axis tumors, brain stem glioma, pituitary adenoma, or a combination of one or more of the foregoing cancers. In another embodiment of said method, said abnormal cell growth is a benign proliferative disease, including, but not limited to, psoriasis, benign prostatic hypertrophy or restinosis.
[0057] In a particular aspect of this embodiment, the cancer is selected from gastrointestinal stromal tumors, renal cell carcinoma, breast cancer, colorectal cancer, non-small cell lung cancer, neuroendocrine tumors, thyroid cancer, small cell lung cancer, mastocytosis, glioma, sarcoma, acute myeloid leukemia, prostate cancer, lymphoma, and combinations thereof.
[0058] In further specific embodiments of any of the inventive methods described herein, the method further comprises administering to the mammal an amount of one or more substances selected from anti-tumor agents, anti-angiogenesis agents, signal transduction inhibitors, and antiproliferative agents, which amounts are together effective in treating said abnormal cell growth. Such substances include those disclosed in PCT publication nos. WO 00/38715, WO 00/38716, WO 00/38717, WO 00/38718, WO 00/38719, WO 00/38730, WO 00/38665, WO 00/37107 and WO 00/38786, the disclosures of which are incorporated herein by reference in their entireties for all purposes.
[0059] Examples of anti-tumor agents include mitotic inhibitors, for example vinca alkaloid derivatives such as vinblastine vinorelbine, vindescine and vincristine; colchines allochochine, halichondrine, N-benzoyltrimethyl-methyl ether colchicinic acid, dolastatin 10, maystansine, rhizoxine, taxanes such as taxol (paclitaxel), docetaxel (Taxotere), 2′-N-[3-(dimethylamino)propyl]glutaramate (taxol derivative), thiocholchicine, trityl cysteine, teniposide, methotrexate, azathioprine, fluorouricil, cytocine arabinoside, 2′2′-difluorodeoxycytidine (gemcitabine), adriamycin and mitamycin. Alkylating agents, for example cis-platin, carboplatin oxiplatin, iproplatin, Ethyl ester of N-acetyl-DL-sarcosyl-L-leucine (Asaley or Asalex), 1,4-cyclohexadiene-1,4-dicarbamic acid, 2,5 -bis(1-azirdinyl)-3,6-dioxo-, diethyl ester (diaziquone), 1,4-bis(methanesulfonyloxy)butane (bisulfan or leucosulfan) chlorozotocin, clomesone, cyanomorpholinodoxorubicin, cyclodisone, dianhydroglactitol, fluorodopan, hepsulfam, mitomycin C, hycantheonemitomycin C, mitozolamide, 1-(2-chloroethyl)-4-(3-chloropropyl)-piperazine dihydrochloride, piperazinedione, pipobroman, porfiromycin, spirohydantoin mustard, teroxirone, tetraplatin, thiotepa, triethylenemelamine, uracil nitrogen mustard, bis(3-mesyloxypropyl)amine hydrochloride, mitomycin, nitrosoureas agents such as cyclohexyl-chloroethyinitrosourea, methylcyclohexyl-chloroethylnitrosourea 1-(2-chloroethyl)-3-(2,6-dioxo-3-piperidyl)-1-nitroso-urea, bis(2-chloroethyl)nitrosourea, procarbazine, dacarbazine, nitrogen mustard-related compounds such as mechloroethamine, cyclophosphamide, ifosamide, melphalan, chlorambucil, estramustine sodium phosphate, strptozoin, and temozolamide. DNA anti-metabolites, for example 5-fluorouracil, cytosine arabinoside, hydroxyurea, 2-[(3hydroxy-2-pyrinodinyl)methylene]-hydrazinecarbothioamide, deoxyfluorouridine, 5-hydroxy-2-formylpyridine thiosemicarbazone, alpha-2′-deoxy-6-thioguanosine, aphidicolin glycinate, 5-azadeoxycytidine, beta-thioguanine deoxyriboside, cyclocytidine, guanazole, inosine glycodialdehyde, macbecin II, pyrazolimidazole, cladribine, pentostatin, thioguanine, mercaptopurine, bleomycin, 2-chlorodeoxyadenosine, inhibitors of thymidylate synthase such as raltitrexed and pemetrexed disodium, clofarabine, floxuridine and fludarabine. DNA/RNA antimetabolites, for example, L-alanosine, 5-azacytidine, acivicin, aminopterin and derivatives thereof such as N-[2-chloro-5-[[(2,4-diamino-5-methyl-6-quinazolinyl)methyl]amino]benzoyl]-L-aspartic acid, N-[4-[[(2,4-diamino-5-ethyl-6-quinazolinyl)methyl]amino]benzoyl]-L-aspartic acid, N-[2-chloro-4-[[(2,4-diaminopteridinyl)methyl]amino]benzoyl]-L-aspartic acid, soluble Baker's antifol, dichloroallyl lawsone, brequinar, ftoraf, dihydro-5-azacytidine, methotrexate, N-(phosphonoacetyl)-L-aspartic acid tetrasodium salt, pyrazofuran, trimetrexate, plicamycin, actinomycin D, cryptophycin, and analogs such as cryptophycin-52 or, for example, one of the preferred anti-metabolites disclosed in European Patent Application No. 239362 such as N -(5-[ N -(3,4-dihydro-2-methyl-4-oxoquinazolin-6-ylmethyl)- N -methylamino]-2-thenoyl)-L-glutamic acid; growth factor inhibitors; cell cycle inhibitors; intercalating antibiotics, for example adriamycin and bleomycin; proteins, for example interferon; and anti-hormones, for example anti-estrogens such as Nolvadex™ (tamoxifen) or, for example anti-androgens such as Casodex™ (4′-cyano-3-(4-fluorophenylsulphonyl)-2-hydroxy-2-methyl-3′-(trifluoromethyl)propionanilide). Such conjoint treatment may be achieved by way of the simultaneous, sequential or separate dosing of the individual components of the treatment.
[0060] Anti-angiogenesis agents include MMP-2 (matrix-metalloprotienase 2) inhibitors, MMP-9 (matrix-metalloprotienase 9) inhibitors, and COX-Il (cyclooxygenase II) inhibitors. Examples of useful COX-II inhibitors include CELEBREX™ (alecoxib), valdecoxib, and rofecoxib. Examples of useful matrix metalloproteinase inhibitors are described in WO 96/33172 (published Oct. 24, 1996), WO 96/27583 (published Mar. 7, 1996), European Patent Application No. 97304971.1 (filed Jul. 8, 1997), European Patent Application No. 99308617.2 (filed Oct. 29, 1999), WO 98/07697 (published Feb. 26, 1998), WO 98/03516 (published Jan. 29, 1998), WO 98/34918 (published Aug. 13, 1998), WO 98/34915 (published Aug. 13, 1998), WO 98/33768 (published Aug. 6, 1998), WO 98/30566 (published Jul. 16, 1998), European Patent Publication 606,046 (published Jul. 13, 1994), European Patent Publication 931,788 (published Jul. 28, 1999), WO 90/05719 (published May 331, 1990), WO 99/52910 (published Oct. 21, 1999), WO 99/52889 (published Oct. 21, 1999), WO 99/29667 (published Jun. 17, 1999), PCT International Application No. PCT/IB98/01113 (filed Jul. 21, 1998), European Patent Application No. 99302232.1 (filed Mar. 25, 1999), Great Britain patent application number 9912961.1 (filed Jun. 3, 1999), U.S. Provisional Application No. 60/148,464 (filed Aug. 12, 1999), U.S. Pat. No. 5,863,949 (issued Jan. 26, 1999), U.S. Pat. No. 5,861,510 (issued Jan. 19, 1999), and European Patent Publication 780,386 (published Jun. 25, 1997), all of which are herein incorporated by reference in their entirety. Preferred MMP-2 and MMP-9 inhibitors are those that have little or no activity inhibiting MMP-1. More preferred, are those that selectively inhibit MMP-2 and/or MMP-9 relative to the other matrix-metalloproteinases (i.e. MMP-1, MMP-3, MMP-4, MMP-5, MMP-6, MMP-7, MMP-8, MMP-10, MMP-11, MMP-12, and MMP-13).
[0061] Examples of MMP inhibitors include AG-3340, RO 32-3555, RS 13-0830, and the compounds recited in the following list:
[0062] 3-[[4-(4-fluoro-phenoxy)-benzenesulfonyl]-(1-hydroxycarbamoyl-cyclopentyl)-amino]-propionic acid; 3-exo-3-[4-(4-fluoro-phenoxy)-benzenesulfonylamino]-8-oxa-bicyclo[3.2.1]octane-3-carboxylic acid hydroxyamide; (2R, 3R) 1-[4-(2-chloro-4-fluoro-benzyloxy)-benzenesulfonyl]-3-hydroxy-3-methyl-piperidine-2-carboxylic acid hydroxyamide; 4-[4-(4-fluoro-phenoxy)-benzenesulfonylamino]-tetrahydro-pyran-4-carboxylic acid hydroxyamide; 3-[[4-(4-fluoro-phenoxy)-benzenesulfonyl]-(1-hydroxycarbamoyl-cyclobutyl)-amino]-propionic acid;
[0063] 4-[4-(4-chloro-phenoxy)-benzenesulfonylamino]-tetrahydro-pyran-4-carboxylic acid hydroxyamide; 3-[4-(4-chloro-phenoxy)-benzenesulfonylamino]-tetrahydro-pyran-3-carboxylic acid hydroxyamide; (2R, 3R) 1-[4-(4-fluoro-2-methyl-benzyloxy)-benzenesulfonyl]-3-hydroxy-3-methyl-piperidine-2-carboxylic acid hydroxyamide; 3-[[4-(4-fluoro-phenoxy)-benzenesulfonyl]-(1-hydroxycarbamoyl-1-methyl-ethyl)-amino]-propionic acid; 3-[[4-(4-fluoro-phenoxy)-benzenesulfonyl]-(4-hydroxycarbamoyl-tetrahydro-pyran-4-yl)-amino]-propionic acid;
[0064] 3-exo-3-[4-(4-chloro-phenoxy)-benzenesulfonylamino]-8-oxa-bicyclo[3.2.1]octane-3-carboxylic acid hydroxyamide; 3-endo-3-[4-(4-fluoro-phenoxy)-benzenesulfonylamino]-8-oxa-bicyclo[3.2.1]octane-3-carboxylic acid hydroxyamide; and 3-[4-(4-fluoro-phenoxy)-benzenesulfonylamino]-tetrahydro-furan-3-carboxylic acid hydroxyamide;
[0065] and pharmaceutically acceptable salts, solvates and prodrugs of said compounds.
[0066] Examples of signal transduction inhibitors include agents that can inhibit EGFR (epidermal growth factor receptor) responses, such as EGFR antibodies, EGF antibodies, and molecules that are EGFR inhibitors; VEGF (vascular endothelial growth factor) inhibitors; and erbB2 receptor inhibitors, such as organic molecules or antibodies that bind to the erbB2 receptor, for example, HERCEPTIN™ (Genentech, Inc. of South San Francisco, Calif., USA).
[0067] EGFR inhibitors are described in, for example in WO 95/19970 (published Jul. 27, 1995), WO 98/14451 (published Apr. 9, 1998), WO 98/02434 (published Jan. 22, 1998), and U.S. Pat. No. 5,747,498 (issued May 5, 1998). EGFR-inhibiting agents include, but are not limited to, the monoclonal antibodies C225 and anti-EGFR 22Mab (ImClone Systems Incorporated of New York, N.Y., USA), the compounds ZD-1839 (AstraZeneca), BIBX-1382 (Boehringer Ingelheim), MDX-447 (Medarex Inc. of Annandale, N.J., USA), and OLX-103 (Merck & Co. of Whitehouse Station, N.J., USA), VRCTC-310 (Ventech Research) and EGF fusion toxin (Seragen Inc. of Hopkinton, Mass.).
[0068] VEGF inhibitors, for example SU-5416 and SU-6668 (Sugen Inc. of South San Francisco, Calif., USA), can also be combined or co-administered with the composition. VEGF inhibitors are described in, for example in WO 99/24440 (published May 20, 1999), PCT International Application PCT/IB99/00797 (filed May 3, 1999), in WO 95/21613 (published Aug. 17, 1995), WO 99/61422 (published Dec. 2, 1999), U.S. Pat. No. 5,834,504 (issued Nov. 10, 1998), WO 98/50356 (published Nov. 12, 1998), U.S. Pat. No. 5,883,113 (issued Mar. 16, 1999), U.S. Pat. No. 6,534,524, issued Mar. 18, 2003, U.S. Pat. No. 6,531,491, issued Mar. 11, 2003, U.S. Pat. No. 5,886,020 (issued Mar. 23, 1999), U.S. Pat. No. 5,792,783 (issued Aug. 11, 1998), WO 99/10349 (published Mar. 4, 1999), WO 97/32856 (published Sep. 12, 1997), WO 97/22596 (published Jun. 26, 1997), WO 98/54093 (published Dec. 3, 1998), WO 98/02438 (published Jan. 22, 1998), WO 99/16755 (published Apr. 8, 1999), and WO 98/02437 (published Jan. 22, 1998), all of which are herein incorporated by reference in their entirety. Other examples of some specific VEGF inhibitors are IM862 (Cytran Inc. of Kirkland, Wash., USA); anti-VEGF monoclonal antibody bevacizumab (Genentech, Inc. of South San Francisco, Calif.); and angiozyme, a synthetic ribozyme from Ribozyme (Boulder, Colo.) and Chiron (Emeryville, Calif.).
[0069] ErbB2 receptor inhibitors, such as GW-282974 (Glaxo Wellcome plc), and the monoclonal antibodies AR-209 (Aronex Pharmaceuticals Inc. of The Woodlands, Tex., USA) and 2B-1 (Chiron), may be administered in combination with the composition. Such erbB2 inhibitors include those described in WO 98/02434 (published Jan. 22, 1998), WO 99/35146 (published Jul. 15, 1999), WO 99/35132 (published Jul. 15, 1999), WO 98/02437 (published Jan. 22, 1998), WO 97/13760 (published Apr. 17, 1997), WO 95/19970 (published Jul. 27, 1995), U.S. Pat. No. 5,587,458 (issued Dec. 24, 1996), and U.S. Pat. No. 5,877,305 (issued Mar. 2, 1999), each of which is herein incorporated by reference in its entirety. ErbB2 receptor inhibitors useful in the present invention are also described in U.S. Provisional Application No. 60/117,341, filed Jan. 27, 1999, and in U.S. Provisional Application No. 60/117,346, filed Jan. 27, 1999, both of which are herein incorporated by reference in their entirety.
[0070] Other antiproliferative agents that may be used include inhibitors of the enzyme farnesyl protein transferase and inhibitors of the receptor tyrosine kinase PDGFr, including the compounds disclosed and claimed in the following U.S. patent applications: Ser. No. 09/221946 (filed Dec. 28, 1998); Ser. No. 09/454058 (filed Dec. 2, 1999); Ser. No. 09/501163 (filed Feb. 9, 2000); Ser. No. 09/539930 (filed Mar. 31, 2000); Ser. No. 09/202796 (filed May 22, 1997); Ser. No. 09/384339 (filed Aug. 26, 1999); and Ser. No. 09/383755 (filed Aug. 26, 1999); and the compounds disclosed and claimed in the following U.S. provisional patent applications: 60/168207 (filed Nov. 30, 1999); 60/170119 (filed Dec. 10, 1999); 60/177718 (filed Jan. 21, 2000); 60/168217 (filed Nov. 30, 1999), and 60/200834 (filed May 1, 2000). Each of the foregoing patent applications and provisional patent applications is herein incorporated by reference in their entirety.
[0071] The composition may also be used with other agents useful in treating abnormal cell growth or cancer, including, but not limited to, agents capable of enhancing antitumor immune responses, such as CTLA4 (cytotoxic lymphocite antigen 4) antibodies, and other agents capable of blocking CTLA4; and anti-proliferative agents such as other farnesyl protein transferase inhibitors. Specific CTLA4 antibodies that can be used in the present invention include those described in U.S. Provisional Application 60/113,647 (filed Dec. 23, 1998) which is herein incorporated by reference in its entirety.
[0072] Specific examples of combination therapy can be found in PCT Publication No. WO 03/015608 and U.S. Provisional Patent Application No. 60/426,386, filed Nov. 15, 2002, the disclosures of which are incorporated herein by reference in their entireties.
DETAILED DESCRIPTION OF INVENTION
Definitions
[0073] “Abnormal cell growth”, as used herein, unless otherwise indicated, refers to cell growth that is independent of normal regulatory mechanisms (e.g., loss of contact inhibition). This includes the abnormal growth of: (1) tumor cells (tumors) that proliferate by expressing a mutated tyrosine kinase or overexpression of a receptor tyrosine kinase; (2) benign and malignant cells of other proliferative diseases in which aberrant tyrosine kinase activation occurs; and (4) any tumors that proliferate by receptor tyrosine kinases.
[0074] The term “treating”, as used herein, unless otherwise indicated, means reversing, alleviating, inhibiting the progress of, or preventing the disorder or condition to which such term applies, or one or more symptoms of such disorder or condition. The term “treatment”, as used herein, unless otherwise indicated, refers to the act of treating as “treating” is defined immediately above.
[0075] The phrase “pharmaceutically acceptable salt(s)”, as used herein, unless otherwise indicated, includes salts of acidic or basic groups which may be present in a compound. Compounds that are basic in nature are capable of forming a wide variety of salts with various inorganic and organic acids. The acids that may be used to prepare pharmaceutically acceptable acid addition salts of such basic compounds are those that form non-toxic acid addition salts, i.e., salts containing pharmacologically acceptable anions, such as the acetate, benzenesulfonate, benzoate, bicarbonate, bisulfate, bitartrate, borate, bromide, calcium edetate, camsylate, carbonate, chloride, clavulanate, citrate, dihydrochloride, edetate, edislyate, estolate, esylate, ethylsuccinate, fumarate, gluceptate, gluconate, glutamate, glycollylarsanilate, hexylresorcinate, hydrabamine, hydrobromide, hydrochloride, iodide, isothionate, lactate, lactobionate, laurate, malate, maleate, mandelate, mesylate, methylsulfate, mucate, napsylate, nitrate, oleate, oxalate, pamoate (embonate), palmitate, pantothenate, phospate/diphosphate, polygalacturonate, salicylate, stearate, subacetate, succinate, tannate, tartrate, teoclate, tosylate, triethiodode, and valerate salts.
[0076] The term “tolyl” represents CH 3 C 6 H 5 —.
[0077] “DMF” represents dimethyl formamide.
[0078] “DIEA” represents di-isopropyl ethyl amine.
[0079] “Me” represents methyl or CH 3 —.
[0080] “Et” represents ethyl or CH 3 CH 2 —.
[0081] “OAc” represents “—O—C(O)—CH 3 ”.
[0082] “R-BINAP” represents (R)-(+)-2,2′-Bis(diphenylphosphiono)-1,1′-binaphthyl).
[0083] “Pd” represents palladium.
[0084] “Dba” represents dibenzanthracene.
[0085] “THF” represents tetrahydrofuran.
[0086] “TBDM” represents Dimethyl-tert-butyl silyl
[0087] “HATU” represents O-(7-Azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate.
[0088] “Ts” represents tosyl.
[0089] “Ph” represents phenyl.
[0090] “THP” represents tetrahydropyran.
[0091] “TFA” represents trifluoroacetic acid.
[0092] “TES” represents triethylsilane.
[0093] “MTBE” represents tert butyl methyl ether.
[0094] “DBU” represents 1,8-Diazabicyclo[5.4.0]Undec-7-ene.
[0095] “DPPA” represents Diphenylphosphorylazide.
[0096] “DIBAL” represents Di-isobutyl aluminum hydride.
[0097] “IBX” represents 1-Hydroxy-1-oxo-benzo[d][1,2]iodoxol-3-one.
[0098] The term “h” or hr” represents hour(s).
[0099] The term “mg” represents milligrams.
[0100] The term “g” represents grams.
[0101] The term “μL” represents microliter.
[0102] The term “mL” represents milliliter.
[0103] The term “L” represents liter.
[0104] The term “mmol” represents millimole.
[0105] The term “M” represents molar.
[0106] The term “min” or “mins” represents minute(s).
[0107] The term “conc” represents “concentrated”.
[0108] The term “Ar” represents aryl.
[0109] The terms “comprising” and “including” are used in an open, non-limiting sense.
[0110] The inventive agents may be prepared using the reaction routes and synthesis schemes as described below, employing the techniques available in the art using starting materials that are readily available.
[0111] In one general synthetic process, compounds of Formula I are prepared according to the following reaction Scheme 1:
[0112] 6-Nitroindazole (compound V) is treated with iodine and base, e.g., NaOH, in an aqueous/organic mixture, preferably with dioxane. The mixture is acidified and the product isolated by filtration. To the resulting 3-iodo-6-nitroindazole in dichloromethane-50% aqueous KOH at 0° C. is added a protecting group (“Pg”) reagent (wherein X=halo), preferably trimethylsilylethoxymethyl chloride (SEM-Cl), and a phase transfer catalyst, e.g., tetrabutylammonium bromide (TBABr). After 1-4 hours, the two phases are diluted, the organics are separated, dried with sodium sulfate, filtered and concentrated. The crude product is purified by silica gel chromatography to give compounds of formula VI. Treatment of compounds of formula VI in a suitable organic solvent with a suitable R 1 -organometallic reagent, preferably an R 1 -boronic acid, in the presence of aqueous base, e.g., sodium carbonate, and a suitable catalyst, preferably Pd(PPh 3 ) 4 gives, after extractive work-up and silica gel chromatography, compounds of formula VII. The R 1 substituent may be exchanged within compounds of formula VII or later intermediates throughout this scheme by oxidative cleavage (e.g., ozonolysis) followed by additions to the resulting aldehyde functionality with Wittig or condensation transformations (typified in Example 42(a-e)). Treatment of compounds of formula VII with a reducing agent, preferably SnCl 2 , provides, after conventional aqueous work up and purification, compounds of formula VII. For the series of derivatives where Y═NH or N-lower alkyl, compounds of formula VIII may be treated with aryl or heteroaryl chlorides, bromides, iodides or triflates in the presence of a base, preferably Cs 2 CO 3 , and catalyst, preferably Pd-BINAP, (and where Y=N-lower alkyl, with a subsequent alkylation step) to provide compounds of formula X. To produce other Y linkages, sodium nitrite is added to compounds of formula VIII under chilled standard aqueous acidic conditions followed by the addition of potassium iodide and gentle warming. Standard work-up and purification produces iodide compounds of formula IX.
[0113] Treatment of compounds of formula IX with an organometallic reagent, e.g., butyllithium, promotes lithium halogen exchange. This intermediate is then reacted with an R 2 electrophile, e.g., a carbonyl or triflate, through the possible mediation of additional metals and catalysts, preferably zinc chloride and Pd(PPh 3 ) 4 to provide compounds of formula X. Alternatively, compounds of formula IX may be treated with an organometallic reagent such as an organoboronic acid in the presence of a catalyst, e.g., Pd(PPh 3 ) 4 , under a carbon monoxide atmosphere to give compounds of formula X. Alternatively, for derivatives where Y═NH or S, compounds of formula IX may be treated with appropriate amines or thiols in the presence of base, preferably Cs 2 CO 3 or K 3 PO 4 and a catalyst, preferably Pd-BINAP or Pd-(bis-cyclohexyl)biphenylphosphine to provide compounds of formula X. Conventional functional group interchanges, such as oxidations, reductions, alkylations, acylations, condensations, and deprotections may then be employed to further derivatize this series giving final compounds of Formula I.
[0114] The inventive compounds of Formula I may also be prepared according general procedure shown in the following Scheme 2:
[0115] 6-lodoindazole (XI) is treated with iodine and base, e.g., NaOH, in an aqueous/organic mixture, preferably with dioxane. The mixture is acidified and the product XII is isolated by filtration. To the resulting 3,6di-iodoindazole in dichloromethane-50% aqueous KOH at 0° C. is added a protecting group reagent, preferably SEM-Cl, and a phase transfer catalyst, e.g., TBABr. The two phases are diluted, the organics separated, dried with sodium sulfate, filtered and concentrated. The crude product is purified by silica gel chromatography to give compounds of the formula XIII. Treatment of compounds of formula XII in a suitable organic solvent with a suitable R 2 -organometallic reagent, e.g., R 2 —ZnCl or boron R 2 -boron reagent and a suitable catalyst, preferably Pd(PPh 3 ) 4 gives, after extractive work-up and silica gel chromatography, compounds of formula XIV. Treatment of compounds of formula XIV in a suitable organic solvent with a suitable R 1 -organometallic reagent (e.g., boron R 1 -boron reagent or R 1 —ZnCl), in the presence of aqueous base, sodium carbonate, and a suitable catalyst, preferably Pd(PPh 3 ) 4 gives, after extractive work-up and silica gel chromatography, compounds of formula XV. Conventional functional group interchanges, such as oxidations, reductions, alkylations, acylations, condensations and deprotections may then be employed to further derivatize this series giving final compounds of Formula I.
[0116] Alternatively, compounds of Formula I where R 2 is a substituted or unsubstituted Y—Ar, where Y is O or S may be prepared according to the following general Scheme 3:
[0117] A stirred acetone solution of 3-chloro-cyclohex-2-enone (XV), H—R 2 , and anhydrous potassium carbonate is refluxed for 15-24 hours, cooled, and filtered. Concentrating and chromatographing the filtrate on silica gel gives 3-R 2 -cyclohex-2-enone (XVI).
[0118] The ketones of formula XVI may be reacted with a suitable base (M-B), preferably lithium bis(trimethylsily)amide, and reacted with R 1 —CO—X (where X=halogen), which after standard acid work up and purification provides compounds of the formula XVII. This product, in HOAc/EtOH, combined with hydrazine monohydrate, is heated at a suitable temperature for an appropriate time period, preferably at 60-80° C. for 24 hours. After cooling, the mixture is poured into saturated sodium bicarbonate solution, extracted with an organic solvent, concentrated, and purified on silica gel to give compounds of formula XVIII. Compounds of formula XVIII may be oxidized using a variety of known methods, such as catalyst or heat, to give compounds of the Formula I.
[0119] An alternative process for synthesizing the compounds of the present invention follows:
wherein the conditions of the steps a) through i) are as follows:
a) NaNO 2 , Br 2 , HBr, 0° C. to −5° C., 4 hours; 48% yield; b) Pd(OCH 3 ) 2 , Pd(O-tolyl) 3 , DIEA, DMF, H 2 O, degassed, microwave, 110° C., 1 hr; 68% yield; c) Iron powder, saturated aqueous NH 4 OH, CH 3 CH 2 OH, 45° C., 3 hours; 72% yield; d) Methyl-2-bromobenzoate, R-BINAP, Pd 2 (dba) 3 , Cs 2 CO 3 , toluene, degassed, 110° C., overnight (18 hours); 74% yield;
[0124] e) KOH in CH 3 OH:THF:H 2 O (3:1:1) 70° C., 2-3 hours; quantitative;
f) TBDMS, HATU, NEt 3 , DMF, room temperature for 2 hours; 80% yield; g) TsOH (12% TsOH in acetic acid), EtOH (10% aqueous), 2 hours; 44% yield; h) Tributylvinyltin, Pd(PPh 3 ) 4 , 2,6-Di-t-butyl-4-methylphenol, toluene, degassed, 105° C., overnight (18 hours); 31% yield; i) Pd(OAc) 2 , Pd(o-tolyl) 3 , DIEA, DMF, degassed, 100° C., overnight (18 hours); approximately 70% yield.
[0129] Reagents used in the above synthetic pathways may be commercially available, for example, from Aldrich.
[0130] Other compounds of the present invention may be prepared in manners analogous to the general procedures described above or the detailed procedures described in the examples herein. The affinity of the compounds of the invention for a receptor may be enhanced by providing multiple copies of the ligand in close proximity, preferably using a scaffolding provided by a carrier moiety. It has been shown that provision of such multiple valence compounds with optimal spacing between the moieties dramatically improves binding to a receptor. See, e.g., Lee et al., Biochem, 23, 4255 (1984). The multivalency and spacing can be controlled by selection of a suitable carrier moiety or linker units. Such moieties include molecular supports which contain a multiplicity of functional groups that can be reacted with functional groups associated with the compounds of the invention. Of course, a variety of carriers can be used, including proteins such as bovine serum albumin (BSA) or HAS (human albumin from serum). a multiplicity of peptides including, for example, pentapeptides, decapeptides, pentadecapeptides, and the like. The peptides or proteins can contain the desired number of amino acid residues having free amino groups in their side chains; however, other functional groups, such as sulfhydryl groups or hydroxyl groups, can also be used to obtain stable linkages.
[0131] It is understood that while an inventive compounds may exhibit the phenomenon of tautomerism, the formula drawings within this specification expressly depict only one of the possible tautomeric forms. It is therefore to be understood that within the invention the formulae are intended to represent any tautomeric form of the depicted compound and is not to be limited merely to a specific tautomeric form depicted by the formula drawings.
[0132] Diastereomeric mixtures can be separated into their individual diastereomers on the basis of their physical chemical differences by methods known to those skilled in the art, for example, by chromatography or fractional crystallization. Enantiomers can be separated by converting the enantiomeric mixtures into a diastereomeric mixture by reaction with an appropriate optically active compound (e.g., alcohol), separating the diastereomers and converting (e.g., hydrolyzing) the individual diastereomers to the corresponding pure enantiomers. All such isomers, including diastereomeric mixtures and pure enantiomers are considered as part of the invention.
[0133] Alternatively, individual stereoisomeric compounds of the present invention may be prepared in enantiomerically enriched form by asymmetric synthesis. Asymmetric synthesis may be performed using techniques known to those of skill in the art, such as the use of asymmetric starting materials that are commercially available or readily prepared using methods known to those of ordinary skill in the art, the use of asymmetric auxiliaries that may be removed at the completion of the synthesis, or the resolution of intermediate compounds using enzymatic methods. The choice of such a method will depend on factors that include, but are not limited to, the availability of starting materials, the relative efficiency of a method, and whether such methods are useful for the compounds of the invention containing particular functional groups. Such choices are within the knowledge of one of ordinary skill in the art.
[0134] When the compounds of the present invention contain asymmetric carbon atoms, the derivative salts, prodrugs and solvates may exist as single stereoisomers, racemates, and/or mixtures of enantiomers and/or diastereomers. All such single stereoisomers, racemates, and mixtures thereof are intended to be within the scope of the present invention.
[0135] As generally understood by those skilled in the art, an optically pure compound having one chiral center is one that consists essentially of one of the two possible enantiomers (i.e., is enantiomerically pure), and an optically pure compound having more than one chiral center is one that is both diastereomerically pure and enantiomerically pure. Preferably, the compounds of the present invention are used in a form that is at least 90% optically pure, that is, a form that contains at least 90% of a single isomer (80% enantiomeric excess (“e.e.”) or diastereomeric excess (“d.e.”)), more preferably at least 95% (90% e.e. or d.e.), even more preferably at least 97.5% (95% e.e. or d.e.), and most preferably at least 99% (98% e.e. or d.e.).
[0136] Additionally, the formulas are intended to cover solvated as well as unsolvated forms of the identified structures. For example, the present invention includes compounds of the indicated structure in both hydrated and non-hydrated forms. Other examples of solvates include the structures in combination with isopropanol, ethanol, methanol, DMSO, ethyl acetate, acetic acid, or ethanolamine.
[0137] If the inventive compound is a base, the desired pharmaceutically acceptable salt may be prepared by any suitable method available in the art, for example, treatment of the free base with an inorganic acid, such as hydrochloric acid, hydrobromic acid, sulfuric acid, nitric acid, phosphoric acid and the like, or with an organic acid, such as acetic acid, maleic acid, succinic acid, mandelic acid, fumaric acid, malonic acid, pyruvic acid, oxalic acid, glycolic acid, salicylic acid, a pyranosidyl acid, such as glucuronic acid or galacturonic acid, an alpha-hydroxy acid, such as citric acid or tartaric acid, an amino acid, such as aspartic acid or glutamic acid, an aromatic acid, such as benzoic acid or cinnamic acid, a sulfonic acid, such as p-toluenesulfonic acid or ethanesulfonic acid, or the like.
[0138] If the inventive compound is an acid, the desired pharmaceutically acceptable salt may be prepared by any suitable method, for example, treatment of the free acid with an inorganic or organic base, such as an amine (primary, secondary or tertiary), an alkali metal hydroxide or alkaline earth metal hydroxide, or the like. Illustrative examples of suitable salts include organic salts derived from amino acids, such as glycine and arginine, ammonia, primary, secondary, and tertiary amines, and cyclic amines, such as piperidine, morpholine and piperazine, and inorganic salts derived from sodium, calcium, potassium, magnesium, manganese, iron, copper, zinc, aluminum and lithium.
[0139] In the case of agents that are solids, it is understood by those skilled in the art that the inventive compounds and salts may exist in different crystal or polymorphic forms, all of which are intended to be within the scope of the present invention and specified formulas.
[0140] Therapeutically effective amounts of the agents of the invention may be used to treat diseases mediated by modulation or regulation of protein kinases. An “effective amount” is intended to mean that amount of an agent that, when administered to a mammal in need of such treatment, is sufficient to effect treatment for a disease mediated by the activity of one or more protein kinases, such as tryosine kinases. Thus, e.g., a therapeutically effective amount of a compound of the present invention, salt, solvate, active metabolite or prodrug thereof is a quantity sufficient to modulate, regulate, or inhibit the activity of one or more protein kinases such that a disease condition which is mediated by that activity is reduced or alleviated.
[0141] The amount of a given agent that will correspond to such an amount will vary depending upon factors such as the particular compound, disease condition and its severity, the identity (e.g., weight) of the mammal in need of treatment, but can nevertheless be routinely determined by one skilled in the art. “Treating” is intended to mean at least the mitigation of a disease condition in a mammal, such as a human, that is affected, at least in part, by the activity of one or more protein kinases, such as tyrosine kinases, and includes: preventing the disease condition from occurring in a mammal, particularly when the mammal is found to be predisposed to having the disease condition but has not yet been diagnosed as having it; modulating and/or inhibiting the disease condition; and/or alleviating the disease condition.
[0142] Compounds that potently regulate, modulate, or inhibit the protein kinase activity associated with receptors vascular endothelial growth factor (VEGF), fibrobalst growth factor (FGF), cyclin dependent kinase (CDK) complexes, Tie-2 kinase (TEK), CHK1, Lymphocyte specific kinase (LCK), Focal Adhesion Kinase (FAK), and phosphorylase kinase among others, and which inhibit angiogenesis and/or cellular profileration is desirable and is one preferred embodiment of the present invention. The present invention is further directed to methods of modulating or inhibiting protein kinase activity, for example in mammalian tissue, by administering an inventive agent. The activity of the inventive compounds as modulators of protein kinase activity, such as the activity of kinases, may be measured by any of the methods available to those skilled in the art, including in vivo and/or in vitro assays. Examples of suitable assays for activity measurements include those described in Parast C. et al., BioChemistry, 37, 16788-16801 (1998); Jeffrey et al., Nature, 376, 313-320 (1995); WIPO International Publication No. WO 97/34876; and WIPO International Publication No. WO 96/14843. These properties may be assessed, for example, by using one or more of the biological testing procedures set out in the examples below.
[0143] The active agents of the invention may be formulated into pharmaceutical compositions as described below. Pharmaceutical compositions of the present invention comprise an effective modulating, regulating, or inhibiting amount of a compound of the present invention and an inert, pharmaceutically acceptable carrier or diluent. In one embodiment of the pharmaceutical compositions, efficacious levels of the inventive agents are provided so as to provide therapeutic benefits involving modulation of protein kinases. By “efficacious levels” is meant levels in which the effects of protein kinases are, at a minimum, regulated. These compositions are prepared in unit-dosage form appropriate for the mode of administration, e.g., parenteral or oral administration.
[0144] An inventive agent is administered in conventional dosage form prepared by combining a therapeutically effective amount of an agent (e.g., a compound of the present invention) as an active ingredient with appropriate pharmaceutical carriers or diluents according to conventional procedures. These procedures may involve mixing, granulating and compressing or dissolving the ingredients as appropriate to the desired preparation.
[0145] The pharmaceutical carrier employed may be either a solid or liquid. Exemplary of solid carriers are lactose, sucrose, talc, gelatin, agar, pectin, acacia, magnesium stearate, stearic acid and the like. Exemplary of liquid carriers are syrup, peanut oil, olive oil, water and the like. Similarly, the carrier or diluent may include time-delay or time-release material known in the art, such as glyceryl monostearate or glyceryl distearate alone or with a wax, ethylcellulose, hydroxypropylmethylcellulose, methylmethacrylate and the like.
[0146] A variety of pharmaceutical forms can be employed. Thus, if a solid carrier is used, the preparation can be tableted, placed in a hard gelatin capsule in powder or pellet form or in the form of a troche or lozenge. The amount of solid carrier may vary, but generally will be from about 25 mg to about 1 g. If a liquid carrier is used, the preparation will be in the form of syrup, emulsion, drop, soft gelatin capsule, sterile injectable solution or suspension in an ampoule or vial or non-aqueous liquid suspension.
[0147] To obtain a stable water-soluble dose form, a pharmaceutically acceptable salt of an inventive agent is dissolved in an aqueous solution of an organic or inorganic acid, such as 0.3M solution of succinic acid or citric acid. If a soluble salt form is not available, the agent may be dissolved in a suitable cosolvent or combinations of cosolvents. Examples of suitable cosolvents include, but are not limited to, alcohol, propylene glycol, polyethylene glycol 300, polysorbate 80, gylcerin and the like in concentrations ranging from 0-60% of the total volume. In an exemplary embodiment, a compound of Formula I is dissolved in DMSO and diluted with water. The composition may also be in the form of a solution of a salt form of the active ingredient in an appropriate aqueous vehicle such as water or isotonic saline or dextrose solution.
[0148] It will be appreciated that the actual dosages of the agents used in the compositions of this invention will vary according to the particular complex being used, the particular composition formulated, the mode of administration and the particular site, host and disease being treated. Optimal dosages for a given set of conditions can be ascertained by those skilled in the art using conventional dosage-determination tests in view of the experimental data for an agent. For oral administration, an exemplary daily dose generally employed is from about 0.001 to about 1000 mg/kg of body weight, more preferably from about 0.001 to about 50 mg/kg body weight, with courses of treatment repeated at appropriate intervals. Administration of prodrugs are typically dosed at weight levels which are chemically equivalent to the weight levels of the fully active form.
[0149] The compositions of the invention may be manufactured in manners generally known for preparing pharmaceutical compositions, e.g., using conventional techniques such as mixing, dissolving, granulating, dragee-making, levigating, emulsifying, encapsulating, entrapping or lyophilizing. Pharmaceutical compositions may be formulated in a conventional manner using one or more physiologically acceptable carriers, which may be selected from excipients and auxiliaries that facilitate processing of the active compounds into preparations which can be used pharmaceutically.
[0150] Proper formulation is dependent upon the route of administration chosen. For injection, the agents of the invention may be formulated into aqueous solutions, preferably in physiologically compatible buffers such as Hanks's solution, Ringer's solution, or physiological saline buffer. For transmucosal administration, penetrants appropriate to the barrier to be permeated are used in the formulation. Such penetrants are generally known in the art.
[0151] For oral administration, the compounds can be formulated readily by combining the active compounds with pharmaceutically acceptable carriers known in the art. Such carriers enable the compounds of the invention to be formulated as tablets, pills, dragees, capsules, liquids, gels, syrups, slurries, suspensions and the like, for oral ingestion by a patient to be treated. Pharmaceutical preparations for oral use can be obtained using a solid excipient in admixture with the active ingredient (agent), optionally grinding the resulting mixture, and processing the mixture of granules after adding suitable auxiliaries, if desired, to obtain tablets or dragee cores. Suitable excipients include: fillers such as sugars, including lactose, sucrose, mannitol, or sorbitol; and cellulose preparations, for example, maize starch, wheat starch, rice starch, potato starch, gelatin, gum, methyl cellulose, hydroxypropylmethyl-cellulose, sodium carboxymethylcellulose, or polyvinylpyrrolidone (PVP). If desired, disintegrating agents may be added, such as crosslinked polyvinyl pyrrolidone, agar, or alginic acid or a salt thereof such as sodium alginate.
[0152] Dragee cores are provided with suitable coatings. For this purpose, concentrated sugar solutions may be used, which may optionally contain gum arabic, polyvinyl pyrrolidone, Carbopol gel, polyethylene glycol, and/or titanium dioxide, lacquer solutions, and suitable organic solvents or solvent mixtures. Dyestuffs or pigments may be added to the tablets or dragee coatings for identification or to characterize different combinations of active agents.
[0153] Pharmaceutical preparations which can be used orally include push-fit capsules made of gelatin, as well as soft, sealed capsules made of gelatin and a plasticizer, such as glycerol or sorbitol. The push-fit capsules can contain the active ingredients in admixture with fillers such as lactose, binders such as starches, and/or lubricants such as talc or magnesium stearate, and, optionally, stabilizers. In soft capsules, the active agents may be dissolved or suspended in suitable liquids, such as fatty oils, liquid paraffin, or liquid polyethylene glycols. In addition, stabilizers may be added. All formulations for oral administration should be in dosages suitable for such administration. For buccal administration, the compositions may take the form of tablets or lozenges formulated in conventional manner.
[0154] For administration intranasally or by inhalation, the compounds for use according to the present invention are conveniently delivered in the form of an aerosol spray presentation from pressurized packs or a nebuliser, with the use of a suitable propellant, e.g., dichlorodifluoromethane, trichlorofluoromethane, dichlorotetrafluoroethane, carbon dioxide or other suitable gas. In the case of a pressurized aerosol the dosage unit may be determined by providing a valve to deliver a metered amount. Capsules and cartridges of gelatin for use in an inhaler or insufflator and the like may be formulated containing a powder mix of the compound and a suitable powder base such as lactose or starch.
[0155] The compounds may be formulated for parenteral administration by injection, e.g., by bolus injection or continuous infusion. Formulations for injection may be presented in unit-dosage form, e.g., in ampoules or in multi-dose containers, with an added preservative. The compositions may take such forms as suspensions, solutions or emulsions in oily or aqueous vehicles, and may contain formulatory agents such as suspending, stabilizing and/or dispersing agents.
[0156] Pharmaceutical formulations for parenteral administration include aqueous solutions of the active compounds in water-soluble form. Additionally, suspensions of the active agents may be prepared as appropriate oily injection suspensions. Suitable lipophilic solvents or vehicles include fatty oils such as sesame oil, or synthetic fatty acid esters, such as ethyl oleate or triglycerides, or liposomes. Aqueous injection suspensions may contain substances which increase the viscosity of the suspension, such as sodium carboxymethyl cellulose, sorbitol, or dextran. Optionally, the suspension may also contain suitable stabilizers or agents which increase the solubility of the compounds to allow for the preparation of highly concentrated solutions.
[0157] For administration to the eye, a compound of the present invention is delivered in a pharmaceutically acceptable ophthalmic vehicle such that the compound is maintained in contact with the ocular surface for a sufficient time period to allow the compound to penetrate the cornea and/or sclera and internal regions of the eye, including, for example, the anterior chamber, posterior chamber, vitreous body, aqueous humor, vitreous humor, cornea, iris/cilary, lens, choroid/retina and sclera. The pharmaceutically acceptable ophthalmic vehicle may be an ointment, vegetable oil, or an encapsulating material. A compound of the invention may also be injected directly into the vitreous humor or aqueous humor.
[0158] Further, a compound may be also be administered by well known, acceptable methods, such as subtebnon and/or subconjunctival injections. The sclera and Tenon's capsule define the exterior surface of the globe of the eye. For treatment of ARMD, CNV, retinopathies, retinitis, uveitis, cystoid macular edema (CME), glaucoma, and other diseases or conditions of the posterior segment of the eye, it is preferable to dispose a depot of a specific quantity of an ophthalmically acceptable pharmaceutically active agent directly on the outer surface of the sclera and below Tenon's capsule. In addition, in cases of ARMD and CME it is most preferable to dispose the depot directly on the outer surface of the sclera, below Tenon's capsule, and generally above the macula.
[0159] Alternatively, the active ingredient may be in powder form for constitution with a suitable vehicle, e.g., sterile pyrogen-free water, before use. The compounds may also be formulated in rectal compositions such as suppositories or retention enemas, e.g, containing conventional suppository bases such as cocoa butter or other glycerides.
[0160] In addition to the formulations described above, the compounds may also be formulated as a depot preparation. Such long-acting formulations may be administered by implantation (for example, subcutaneously or intramuscularly) intramuscular injection or by the above mentioned subtenon or intravitreal injection.
[0161] Within particular embodiments of the invention, the compounds may be prepared for topical administration in saline (combined with any of the preservatives and antimicrobial agents commonly used in ocular preparations), and administered in eyedrop form. The anti-angiogenic factor solution or suspension may be prepared in its pure form and administered several times daily. Alternatively, anti-angiogenic compositions, prepared as described above, may also be administered directly to the cornea.
[0162] Within alternative embodiments, the composition is prepared with a muco-adhesive polymer which binds to cornea. Thus, for example, the compounds may be formulated with suitable polymeric or hydrophobic materials (for example, as an emulsion in an acceptable oil) or ion-exchange resins, or as sparingly soluble derivatives, for example, as a sparingly soluble salt. Within further embodiments, the anti-angiogenic factors or anti-angiogenic compositions may be utilized as an adjunct to conventional steroid therapy.
[0163] A pharmaceutical carrier for hydrophobic compounds is a cosolvent system comprising benzyl alcohol, a nonpolar surfactant, a water-miscible organic polymer, and an aqueous phase. The cosolvent system may be a VPD co-solvent system. VPD is a solution of 3% w/v benzyl alcohol, 8% w/v of the nonpolar surfactant polysorbate 80, and 65% w/v polyethylene glycol 300, made up to volume in absolute ethanol. The VPD co-solvent system (VPD:5W) contains VPD diluted 1:1 with a 5% dextrose in water solution. This co-solvent system dissolves hydrophobic compounds well, and itself produces low toxicity upon systemic administration. The proportions of a co-solvent system may be varied considerably without destroying its solubility and toxicity characteristics. Furthermore, the identity of the co-solvent components may be varied: for example, other low-toxicity nonpolar surfactants may be used instead of polysorbate 80; the fraction size of polyethylene glycol may be varied; other biocompatible polymers may replace polyethylene glycol, e.g. polyvinyl pyrrolidone; and other sugars or polysaccharides may be substituted for dextrose.
[0164] Alternatively, other delivery systems for hydrophobic pharmaceutical compounds may be employed. Liposomes and emulsions are known examples of delivery vehicles or carriers for hydrophobic drugs. Certain organic solvents such as dimethylsulfoxide also may be employed, although usually at the cost of greater toxicity. Additionally, the compounds may be delivered using a sustained-release system, such as semipermeable matrices of solid hydrophobic polymers containing the therapeutic agent. Various sustained-release materials have been established and are known by those skilled in the art. Sustained-release capsules may, depending on their chemical nature, release the compounds for a few weeks up to over 100 days. Depending on the chemical nature and the biological stability of the therapeutic reagent, additional strategies for protein stabilization may be employed.
[0165] The pharmaceutical compositions also may comprise suitable solid- or gel-phase carriers or excipients. Examples of such carriers or excipients include calcium carbonate, calcium phosphate, sugars, starches, cellulose derivatives, gelatin, and polymers such as polyethylene glycols.
[0166] Some of the compounds of the invention may be provided as salts with pharmaceutically compatible counter ions. Pharmaceutically compatible salts may be formed with many acids, including hydrochloric, sulfuric, acetic, lactic, tartaric, malic, succinic, etc. Salts tend to be more soluble in aqueous or other protonic solvents than are the corresponding free-base forms.
[0167] The preparation of the compounds of the present invention is described in detail in the following examples, but the artisan will recognize that the chemical reactions described may be readily adapted to prepare a number of other protein kinase inhibitors of the invention. For example, the synthesis of non-exemplified compounds according to the invention may be successfully performed by modifications apparent to those skilled in the art, e.g., by appropriately protecting interfering groups, by changing to other suitable reagents known in the art, or by making routine modifications of reaction conditions. Alternatively, other reactions disclosed herein or known in the art will be recognized as having applicability for preparing other compounds of the invention.
EXAMPLES
[0168] In the examples described below, unless otherwise indicated all temperatures are set forth in degrees Celsius and all parts and percentages are by weight. Reagents were purchased from commercial suppliers such as Aldrich Chemical Company or Lancaster Synthesis Ltd. and were used without further purification unless otherwise indicated. Tetrahydrofuran (THF), N,N-dimethylformamide (DMF), dichloromethane, toluene, and dioxane were purchased from Aldrich in Sure seal bottles and used as received. All solvents were purified using standard methods readily known to those skilled in the art, unless otherwise indicated.
[0169] The reactions set forth below were done generally under a positive pressure of argon or nitrogen or with a drying tube, at ambient temperature (unless otherwise stated), in anhydrous solvents, and the reaction flasks were fitted with rubber septa for the introduction of substrates and reagents via syringe. Glassware was oven dried and/or heat dried. Analytical thin layer chromatography (TLC) was performed on glass-backed silica gel 60 F 254 plates Analtech (0.25 mm) and eluted with the appropriate solvent ratios (v/v), and are denoted where appropriate. The reactions were assayed by TLC and terminated as judged by the consumption of starting material.
[0170] Visualization of the TLC plates was done with a p-anisaldehyde spray reagent or phosphomolybdic acid reagent (Aldrich Chemical 20 wt % in ethanol) and activated with heat. Work-ups were typically done by doubling the reaction volume with the reaction solvent or extraction solvent and then washing with the indicated aqueous solutions using 25% by volume of the extraction volume unless otherwise indicated. Product solutions were dried over anhydrous Na 2 SO 4 prior to filtration and evaporation of the solvents under reduced pressure on a rotary evaporator and noted as solvents removed in vacuo. Flash column chromatography (Still et al., J. Org. Chem., 43, 2923 (1978)) was done using Baker grade flash silica gel (47-61 μm) and a silica gel: crude material ratio of about 20:1 to 50:1 unless otherwise stated. Hydrogenolysis was done at the pressure indicated in the examples or at ambient pressure.
[0171] 1 H-NMR spectra were recorded on a Bruker instrument operating at 300 MHz and 13 C-NMR spectra were recorded operating at 75 MHz. NMR spectra were obtained as CDCl 3 solutions (reported in ppm), using chloroform as the reference standard (7.25 ppm and 77.00 ppm) or CD 3 OD (3.4 and 4.8 ppm and 49.3 ppm), or internally tetramethylsilane (0.00 ppm) when appropriate. Other NMR solvents were used as needed. When peak multiplicities are reported, the following abbreviations are used: s (singlet), d (doublet), t (triplet), m (multiplet), br (broadened), dd (doublet of doublets), dt (doublet of triplets). Coupling constants, when given, are reported in Hertz (Hz).
[0172] Infrared (IR) spectra were recorded on a Perkin-Elmer FT-IR Spectrometer as neat oils, as KBr pellets, or as CDCl 3 solutions, and when given are reported in wave numbers (cm −1 ). The mass spectra were obtained using LSIMS or electrospray. All melting points (mp) are uncorrected.
Example 1(a)
2-(4-Chloro-2-nitro-phenyl)-malonic acid dimethyl ester
[0173]
[0174] To a stirred slurry of NaH (36.0 g, 1500 mmol) in NMP (1.0 L) was added dimethyl malonate (137.4 mL, 1200 mmol) drop wise. The reaction was cooled as needed to keep the internal temperature below 30 degrees Celsius. After gas evolution ceased, 2,4-dichloronitrobenzene (192 g, 1000 mmol) was added to the reaction. It was carefully heated to 65 degrees Celsius until the reaction was complete as determined by HPLC. The reaction was cooled to room temperature, and then poured over 500 mL ice mixed with 150 mL conc. HCl. The pH of the aqueous layer was adjusted to neutral using 1 N NaOH. The solids were removed by filtering through a coarse fritted filter, and rinsed with water (3 L). The yellow solids were allowed to dry overnight. Yield 261.5 g, 91%.
Example 1(b)
(4-Chloro-2-nitro-phenyl)-acetic acid methyl ester
[0175]
[0176] A solution of 2-(4-Chloro-2-nitro-phenyl)-malonic acid dimethyl ester (195 g, 679.4 mmol) in water (100 mL) and NMP (1000 mL) was heated to reflux for 3.5 hours. The solvent was removed by rotary evaporation to an oil. The oil was dissolved in EtOAc, and then washed with water (5×300 mL). The aqueous layer was then extracted with EtOAc (4×300 mL). The organic was washed with water. The organic layers were combined and dried over MgSO 4 . After removing the solids by filtration, the solvent was evaporated to yield the desired product as a orange/brown solid (160.0 g, 95%).
Example 1(c)
(2-Acetylamino-4-chloro-phenyl)-acetic acid methyl ester
[0177]
[0178] An argon filled flask was charged with (4-Chloro-2-nitro-phenyl)-acetic acid methyl ester (40 g, 175 mmol), 10% Pd/C (2.5 g), acetic anhydride (64 mL, 677 mmol), water (9 mL) and acetic acid (150 mL). The flask was vacuum flushed with hydrogen gas at 30 PSI and shook vigorously. After 2 hours, more 10% Pd/C (2 g) was added, and the reaction was complete after a total of 4 hours reaction time. The 10% Pd/C was removed by filtration, and the solvent was removed by rotary evaporation.
Example 1(d)
6-Chloro-1H-indazole-3-carboxylic acid methyl ester
[0179]
[0180] To a solution of (2-Acetylamino-4-chloro-phenyl)-acetic acid methyl ester (32.0 g, 133 mmol) in acetic acid (200 mL) stirred at 90 degree Celsius was added tert-butyl nitrite (20.5 mL, 172.3 mmol) over 1 hour. The reaction was poured into water (1.4 L) and the solids were recovered by filtration. The yellow precipitate was dissolved in EtOAc, then washed with saturated NaCl. The organic was dried over MgSO 4 , filtered, and concentrated to a solid. The solids were triturated with hexanes and filtered to afford the desired material (21.63 g, 77%).
Example 1(e)
6-Chloro-1-(tetrahydro-pyran-2-yl)-1H-indazole-3-carboxylic acid methyl ester
[0181]
[0182] To a slurry of 6-Chloro-1H-indazole-3-carboxylic acid methyl ester (8.3 g, 39.5 mmol) in MeCN (200 mL) was added 3,4-Dihydro-2H-pyran (5.4 mL, 59.3 mmol) and p-toluenesulfonic acid (237 mg, 1.25 mmol). After letting the reaction stir for 10 minutes, saturated NaHCO 3 (1 mL) was added and the solvent was removed by rotary evaporation to a volume of 100 mL. The mixture was diluted with EtOAc and washed with water (50 mL) and then with saturated NaCl (50 mL). The organic layer was then dried over Na 2 SO 4 After the solids were removed by filtration, the organic layer was concentrated to an oil by rotary evaporation. The product was precipitated from the oil using hexanes to yield the desired product (7.667 g, 66% yield).
Example 1(f)
6-(2-Methoxycarbonyl-phenylamino)-1-(tetrahydro-pyran-2-yl)-1H-indazole-3-carboxylic acid methyl ester
[0183]
[0184] To a solution of 6-Chloro-1H-indazole-3-carboxylic acid methyl ester (2.94 g, 10.0 mmol) in 1,2-dimethoxyethane (30 mL) was added K 3 PO 4 (5.32 g, 25.0 mmol), tris(dibenzylideneacetone)dipalladium (459 mg, 0.05 mmol), 2-(dicyclohexylphosphino) biphenyl (701 mg, 2.0 mmol), and methyl anthranilate (2.59 mL, 20.0 mmol). The solution was vacuum flushed with argon three times before being heated to 80 degrees Celsius for 18 hours. The reaction was cooled to room temperature and the solids were removed by filtration. After washing the solids with ethyl acetate, the solvent was removed by rotary evaporation. The residual oil was chromatographed (150 g silica gel, 10-30% EtOAc/Hex) to yield 1.23 g (51%) of the desired product.
Example 1(g)
6-(2-Methoxycarbonyl-phenylamino)-1-(tetrahydro-pyran-2-yl)-1H-indazole-3-carboxylic acid
[0185]
[0186] To a solution of 6-(2-Methoxycarbonyl-phenylamino)-1-(tetrahydro-pyran-2-yl)-1H-indazole-3-carboxylic acid methyl ester (2.05 g, 5 mmol) in methanol (18 mL) and tetrahydrofuran (8 mL), was added a solution of sodium hydroxide (0.30 g, 7.5 mmol) in water (2.7 mL). The reaction was stirred at room temperature for 3 hours and was then neutralized with 1 N HCl to a pH of 1. The mixture was diluted with EtOAc (25 mL) and water (25 mL). After separating the layers, the aqueous layer was washed with CH 2 Cl 2 (3×25 mL). The combined organic extracts were washed with saturated NaCl (100 mL) and then dried over Na 2 SO 4 . The solids were filtered and the liquid was concentrated to an oil. The product was crystallized from EtOAc and Hexanes to yield the desired product (1.616 g, 82%).
Example 1(h)
2-[3-Methylcarbamoyl-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester
[0187]
[0188] To a solution of 6-(2-Methoxycarbonyl-phenylamino)-1-(tetrahydro-pyran-2-yl)-1H-indazole-3-carboxylic acid (0.50 g, 1.27 mmol) in DMF was added triethylamine (0.42 mL, 3.04 mmol), methylamine (1.9 mL, 3.81 mmol), and HATU (0.578 g, 1.52 mmol). The reaction was stirred for 3 hours and then concentrated by rotary evaporation. The crude oil was chromatographed (50 g silica gel, 25-50% EtOAc/hexanes) to yield the desired product (214 mg, 42%).
Example 1(i)
2-[3-Methylcarbamoyl-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid
[0189]
[0190] To a solution of 2-[3-Methylcarbamoyl-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester (0.20 g, 0.49 mmol) in methanol (1.4 mL) and tetrahydrofuran (0.6 mL) was added a solution of sodium hydroxide (59 mg, 1.47 mmol) in water (0.3 mL). The reaction was heated to 60 degrees Celsius for 1 hour and then was cooled to room temperature. The pH was adjusted with 2 N HCl to a pH of 2. EtOAc (30 mL) and water (30 mL) was added and the layers were separated. The aqueous was extracted with EtOAc (3×20 mL) and the organic layers were combined. After washing with water (15 mL), the organic layer was dried over Na 2 SO 4 . The solids were filtered away, and the organic was evaporated to yield a yellow solid (193 mg, 100%).
Example 1(j)
6-(2-Prop-2-ynylcarbamoyl-phenylamino)-1-(tetrahydro-pyran-2-yl)-1H-indazole-3-carboxylic acid methylamide
[0191]
[0192] To a solution of 2-[3-Methylcarbamoyl-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid (150 mg, 0.381 mmol) in DMF (3.6 mL) was added propargylamine (0.052 mL, 0.761 mmol), triethylamine(TEA) (0.264 mL, 1.90 mmol), and HATU (217 mg, 0.571 mmol). The reaction was stirred for 4 hours, and then diluted with EtOAc (30 mL) and water (30 mL). The layers were separated, and the aqueous was extracted with EtOAc (2×20 mL). The combined organics were washed with saturated NaCl (15 mL) and then dried over Na 2 SO 4 . The solids were removed by filtration, and the liquid was concentrated by rotary evaporation to a yellow oil (164 mg, 100%).
Example 1(k)
6-(2-Prop-2-ynylcarbamoyl-phenylamino)-1H-indazole-3-carboxylic acid methylamide
[0193]
[0194] Dissolved 6-(2-Prop-2-ynylcarbamoyl-phenylamino)-1-(tetrahydro-pyran-2-yl)-1H-indazole-3-carboxylic acid methylamide (30 mg) in 1.5 mL of a 90:10:1 mixture of CH 2 Cl 2 :Trifluoroacetate TFA:triethyl silane and heat to reflux for 2 hours. Diluted the solution with toluene (40 mL) and concentrate by rotary evaporation to an oil. Dissolved the oil in DMF (1 mL), and filter using a 0.2-micron syringe filter. Used prep-HPLC to isolate the desired compound (12 mg, 50%). 1 H NMR (CDCl 3 -d) δ 9.96 (1H, s), 9.49 (1H, s), 8.28 (1H, d, J=8.85 Hz), 7.47 (1H, m), 7.34 (1H, m), 7.22 (1H, m), 7.15 (1H, dd, J1=8.76 Hz, J2=1.79 Hz), 6.99 (1H, m), 6.86 (1H, t, J=6.97 Hz), 6.31 (1H, m), 4.23 (2H, dd, J=5.18 Hz, J2=2.54 Hz), 3.49 (3H, s), 2.29 (s, 1H).
[0195] Anal. Calcd. For C 19 H 17 N 5 O 2 .1.0 MeOH.0.1 TFA: C, 62.08; H, 5.44; N, 17.92. Found: C, 61.78; H, 5.45; N, 18.04.
Example 2(a)
[6-Chloro-1-(tetrahydro-pyran-2-yl)-1H-indazol-3-yl]-methanol
[0196]
[0197] To a solution of 6-Chloro-1H-indazole-3-carboxylic acid methyl ester (2.94 g, 10.0 mmol) in dry CH 2 Cl 2 (50 mL) cooled to −78 degrees Celsius was added DIBAL-H (3.56 mL, 20.0 mmol) slowly. After the addition was complete, the reaction was allowed to warm to room temperature, where HPLC showed that there was a remaining 10% starting material. Extra DIBAL-H (0.35 mL) was then added and stirred for 10 minutes. The reaction was diluted with EtOAc (1000 mL) and washed with 1 N HCl (2×100 mL). It was further washed with 1 N NaHCO 3 (100 mL), and then with saturated NaCl (100 mL). The organic was dried over Mg SO 4 , filtered, and then concentrated to a white solid (2.65 g, 99.5%).
Example 2(b)
6-Chloro-1-(tetrahydro-pyran-2-yl)-1H-indazole-3-carbaldehyde
[0198]
[0199] A solution of [6-Chloro-1-(tetrahydro-pyran-2-yl)-1H-indazol-3-yl]-methanol (1.75 g, 6.58 mmol), IBX (2.76 g, 9.87 mmol) and DMSO (27 mL) was stirred overnight. The reaction was diluted in EtOAc and water. The layers were separated, and the aqueous was extracted with EtOAc (3×100 mL). The organics were combined and washed with saturated NaCl (100 mL). The organic was dried over MgSO 4 , filtered, and then concentrated to a solid. The solid was dissolved in CH 2 Cl 2 , and filtered. The organic was evaporated to yield the desired product (1.707 g, 92%).
Example 2(c)
1-(6-Chloro-1H-indazol-3-yl)-2-(5-ethyl-pyridin-2-yl)-ethanol
[0200]
[0201] To a stirred solution of 4-ethyl-2-methylpyridine (0.458 g, 3.79 mmol) in THF (4 mL) at −50 degrees Celsius, add butyl lithium (1.5 mL, 2.5 M, 3.79 mmol) slowly and stir for 10 minutes. To the reaction, slowly add a solution of 6-Chloro-1H-indazole-3-carbaldehyde (0.5 g, 1.89 mmol) in THF (4 mL). After stirring for 10 minutes, the reaction was quenched with 1 N citric acid (10 mL). The mixture was diluted with EtOAc (50 mL), water (20 mL), and saturated NaCl (10 mL). The layers were separated, and the aqueous was extracted with EtOAc (3×15 mL). The organics were combined and washed with saturated NaCl (20 mL). After drying the organic layer over Na 2 SO 4 , the solids were removed by filtration and the liquid was concentrated to an oil by rotary evaporation. Chromatography (40 g silica gel, 60-100% EtOAc/hex) yields the desired product (142 mg, 32%) and recovered 6-Chloro-1H-indazole-3-carbaldehyde (348 mg).
Example 2(d)
6-Chloro-3-[2-(5-ethyl-pyridin-2-yl)-vinyl]-1H-indazole
[0202]
[0203] To a stirred solution of 1-(6-Chloro-1H-indazol-3-yl)-2-(5-ethyl-pyridin-2-yl)-ethanol (232 mg, 0.60 mmol) in CH 2 Cl 2 was added TEA (0.25 mL, 1.81 mmol) and mesyl chloride (0.070 mL, 0.90 mmol). The reaction was stirred for 30 minutes, and then DBU (2 mL) was added. The reaction was refluxed for 18 hours and then quenched with 40 mL of 1 N citric acid. The layers were separated, and the aqueous was extracted with 20 mL CH 2 Cl 2 . The combined organics were dried over Na 2 SO 4 , filtered, and concentrated by rotary evaporation. Purification by chromatography (12 g silica gel, 50-70% EtOAc/hexanes) yielded the desired compound (135 mg, 71%).
Example 2(e)
2-{3-[2-(5-Ethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzoic acid methyl ester
[0204]
[0205] 1,2-Dimethoxymethane (2 mL) was added to 6-Chloro-3-[2-(5-ethyl-pyridin-2-yl)-vinyl]-1H-indazole (130 mg, 0.354 mmol), tris(dibenzylideneacetone)dipalladium (16 mg, 0.018 mmol), -(dicyclohexylphosphino)biphenyl (25 mg, 0.071 mmol), K 3 PO 4 (0.188 g, 0.885 mmol), and methyl anthranilate (0.092 mL, 0.71 mmol). The reaction was vacuum flushed with argon (4×) and then heated to 80 degrees Celsius for 19 hours. The reaction was diluted with EtOAc (20 mL) and filtered through a silica gel plug. After washing with EtOAc (50 mL), the solvent was removed by rotary evaporation. The crude oil was purified by chromatography (40 g silica gel, 30-40% EtOAc/hexanes) to yield the desired product (54 mg, 32%).
Example 2(f)
2-{3-[2-(5-Ethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzoic acid
[0206]
[0207] To a solution of 2-{3-[2-(5-Ethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzoic acid methyl ester (50 mg, 0.104 mmol) in methanol (0.42 mL) and THF (0.10 mL) was added a solution of sodium hydroxide (12 mg, 0.311 mmol) in water (0.05 mL). The solution was heated to 60 degrees Celsius for 3.5 hours and then neutralized with saturated NH 4 Cl. The reaction was diluted with water (20 mL), and then extracted with EtOAc (2×20 mL). The combined extracts were first dried over Na 2 SO 4 , and then the solids were removed by filtration. The desired product (48.7 mg, 100%) was recovered after rotary evaporation to remove the solvents.
Example 2(g)
2-{3-[2-(5-Ethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-prop-2-ynyl-benzamide
[0208]
[0209] To 2-{3-[2-(5-Ethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzoic acid (49 mg, 0.105 mmol) was added 2 mL of a 90:10:1 mixture of CH 2 Cl 2 :TFA:TES. The reaction was stirred at reflux for 1 hour, and then diluted with toluene (20 mL). The solvent was removed by rotary evaporation to yield a thick oil. The oil was dissolved in DMF (1 mL) and to this solution was added TEA (0.072 mL, 0.52 mmol), propargyl amine (0.014 mL, 0.208 mmol), and HATU (59 mg, 0.156 mmol). The reaction was stirred for 3 hours, and then purified by preparatory HPLC to yield the desired product (29 mg, 66%). 1 H NMR (CDCL 3 -d): δ 9.83 (1H, s), 8.63 (2H, s), 8.04 (2H, m), 7.68 (2H, s), 7.47 (1H, m), 7.32 (1H, d, J=1.51 Hz), 7.10 (1H, dd, J1=8.67 Hz, J2=1.88 Hz), 6.93 (1H, m), 6.07 (2H, dd, J1=5.09 Hz, J2=2.26 Hz), 3.15 (1H, t, J=2.35 Hz), 2.97 (2H, s), 2.74 (1H, s), 2.29 (1H, s), 1.27 (3H, J=7.44 Hz)
[0210] Anal. Calcd. for C 26 H 23 N 5 O.0.3 H 2 O.1.2 TFA: C, 60.51; H, 4.43; N, 12.42. Found: C, 60.38; H, 4.73; N, 12.44.
Example 2(h)
N-Cyclopropyl-2-{3-[(E)-2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide
[0211]
[0212] The title compound was prepared analogously to 2-{3-[2-(5-Ethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-prop-2-ynyl-benzamide described above, substituting 2,4-dimethyl-pyridine for 4-ethyl-2-methyl-pyridine in the step where 1-(6-Chloro-1H-indazol-3-yl)-2-(5-ethyl-pyridin-2-yl)-ethanol was prepared, and substituting cyclopropyl amine in place of propargyl amine in the final step of the sequence. 1 H NMR (DMSO-d 6 ): δ 9.85 (1H, s), 8.56 (2H, m), 8.20 (3H, m), 7.53 (5H, m), 7.35 (1H, s), 7.2 (1H, d, J=6.5 Hz), 7.0 (1H, s), 2.83 (1H, m), 0.70 (2H, m), 0.56 (2H, m). ESIMS (M+H + ): 410.3.
Example 3(a)
N-Methoxy-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0213]
[0214] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), O-methyl-hydroxylamine hydrochloride (15 mg, 0.17 mmol), triethylamine(58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 21.6 mg (67%) of the title compound as a yellow solid. 1 H NMR (DMSO-d 6 ): δ 9.23 (1H, s), 8.71 (1H, d, J=2.2), 8.05 (4H, m), 7.51 (5H, m), 7.25 (1H, s), 7.10 (1H, d, J=7.7 Hz), 6.91 (1H, m), 5.98 (1H, m), 4.31 (1H, d, J=14.3), 7.20 (1H, d, J=7.3),4.42 (2H, d, J=3.2). ESIMS (M+H + ): 412.1.
Example 3(b)
N-Allyloxy-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0215]
[0216] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), O-allyl-hydroxylamine hydrochloride (18.3 mg, 0.17 mmol), triethylamine(58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 25.5 mg (74%) of the title compound as a yellow solid. 1 H NMR (DMSO-d 6 ): δ 9.28 (1H, s), 8.67 (2H, d, J=3.4), 8.05 (4H, m), 7.48 (5H, m), 7.23 (1H, s), 7.04 (1H, d, J=7.6 Hz), 6.91 (1H, m), 3.69 (3H, s). ESIMS (M+H + ): 386.1.
Example 3(c)
N-lsopropoxy-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0217]
[0218] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), O-isopropyl-hydroxylamine hydrochloride (18.7 mg, 0.17 mmol), triethylamine(58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 17.4 mg (50%) of the title compound as a yellow solid. 1 H NMR (DMSO-d 6 ): δ 9.23 (1H, s), 8.69 (H, d, J=2.1), 8.03 (4H, m), 7.50 (5H, m), 7.23 (1H, s), 7.04 (1H, d, J=6.7 Hz), 6.92 (1H, m), 5.98 (1H, m), 4.13 (1H, m), 1.29 (6H, d, J=8.1). ESIMS (M+H + ): 414.1.
Example 3(d)
N-Cyclopropyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0219]
[0220] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), cyclopropyl amine (11.6 μL, 0.17 mmol), triethylamine (58 μl, 0.25 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 11.7 mg (35%) of the title compound as a yellow solid. 1 H NMR (DMSO-d 6 ): δ 9.81 (1H, s), 8.68 (1H, d, J=1.7), 8.51 (1H, s), 8.01 (4H, m), 7.50 (5H, m), 7.24 (1H, s), 7.03 (1H, d, J=5.3), 6.89 (1H, t, J=4.2), 2.84 (1H, m), 0.72 (2H, m), 0.56 (2H, m). ESIMS (M+H + ): 396.1.
Example 3(f)
1-Methyl-1H-pyrrole-2-carboxylic acid N′-(1-{2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-phenyl}-methanoyl)-hydrazide
[0221]
[0222] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), 1-methyl-1H-pyrrole-2-carboxylic acid hydrazide (23.3 mg, 0.17 mmol), triethylamine(58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 16.1 mg (40%) of the title compound as a yellow solid. 1 H NMR (DMSO-d 6 ): δ 10.39 (1H, s), 10.00 (1H, s), 9.52 (1H, s), 8.67 (1H, d, J=2.4), 8.07 (4H, m), 7.77 (1H, d, J=5.2), 7.51 (4H, m), 7.32 (1H, s), 7.09 (1H, d, J=6.3), 6.98 (3H, m), 6.13 (1H, m), 3.87 (3H, s), ESIMS (M+H + ): 478.1.
Example 3(g)
N-Benzyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0223]
[0224] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), benzylamine (18.2 μL, 0.17 mmol), triethylamine (58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 45.2 mg (76%) of the title compound as a TFA salt (1.5 H 2 O, 2.1 TFA, effective MW=711.98). 1 H NMR (DMSO-d 6 ): δ 9.86 (1H, s), 9.14 (1H, t, J=5.4), 8.73 (1H, d, J=4.8), 8.29 (4H, m), 7.56 (1H, d, J=7.0), 7.74 (2H, m), 7.89 (2H, m), 7.31 (5H, m), 7.16 (1H, d, J=7.8), 6.93 (1H, t, J=7.3), 4.46 (2H, d, J=6.1), ESIMS (M+H + ): 446.5.
Example 3(h)
N-(2-Methoxy-benzyl)-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0225]
[0226] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), o-methoxybenzylamine (21.8 μL, 0.17 mmol), triethylamine (58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 46 mg (81%) of the title compound as a TFA salt (1.5 H 2 O, 1.5 TFA, effective MW=673.59). 1 H NMR (DMSO-d 6 ): δ 9.83 (1H, s), 9.03 (1H, t, J=3.4), 8.70 (1H, d, J=3.7), 8.08 (4H, m), 7.82 (1H, d, J=7.4), 7.49 (4H, m), 7.21 (3H, m), 6.96 (4H, m), 4.48 (2H, d, J=6.3). ESIMS (M+H + ): 476.1.
Example 3(i)
N-Furan-2-ylmethyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0227]
[0228] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), C-furan-2-yl-methylamine (19 μL, 0.17 mmol), triethylamine (58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 45 mg (85%) of the title compound as a TFA salt (1.5 H 2 O, 1.5 TFA, effective MW=633.52). 1 H NMR (DMSO-d 6 ): δ 9.82(1H, s), 9.05 (1H, t, J=2.6), 8.73 (1H, d, J=3.7), 8.13 (4H, m), 7.73 (1H, d, J=6.8), 7.57 (2H, m), 7.26 (1H, s), 7.03 (1H, d, J=7.5), 6.40 (1H, m), 6.28 (1H, m), 4.48 (2H, d, J=6.5). ESIMS (M+H + ): 436.1.
Example 3(j)
N-Cyclobutyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0229]
[0230] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), cyclobutylamine (18.2 μL, 0.17 mmol), triethylamine (58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 43.2 mg (92%) of the title compound as a TFA salt (1.5 H 2 O, 1.1 TFA, effective MW=561.92). 1 H NMR (DMSO-d 6 ): δ 9.78 (1H, s), 8.72 (2H, m), 8.13 (4H, m), 7.70 (1H, d, J=7.1), 7.58 (2H, m), 7.41 (2H, m), 7.27 (1H, s), 6.89 (1H, t, J=4.2), 2.84 (1H, m), 0.72 (2H, m), 0.56 (2H, m). ESIMS (M+H + ): 396.1.
Example 3(k)
N-(2-Methyl-allyl)-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0231]
[0232] A solution of 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoic acid (50.0 mg, 0.084 mmol), 2-methyl-allylamine (16.4 μL, 0.17 mmol), triethylamine (58 μl, 0.42 mmol), dissolved in DMF (0.8 mL), was treated with HATU (48 mg, 0.13 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 45 mg (91%) of the title compound as a TFA salt (1.6 H 2 O, 1.3 TFA, effective MW=586.53). 1 H NMR (DMSO-d 6 ): δ 9.78 (1H, s), 8.72 (2H, m), 8.13 (4H, m), 7.70 (1H, d, J=7.1), 7.58 (2H, m), 7.41 (2H, m), 7.27 (1H, s), 7.06 (1H, d, J=7.1), 6.91 (1H, t, J=7.5), 4.42 (1H, m), 2.22 (2H, m), 2.08 (2H, m), 1.68 (2H, m). ESIMS (M+H + ): 410.1.
Example 3(l)
6-Nitro-3-pyridin-2-ylethynyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazole
[0233]
[0234] A mixture of 3-Iodo-6-nitro-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazole (838 mg, 2.0 mmol), 2-ethynyl-pyridine (242 μL, 2.4 mmol), and triethylamine (6.0 mL), were degassed and flushed with argon, then treated with CuI (8 mg, 0.042 mmol), and Pd(PPh 3 ) 2 Cl 2 (16 mg, 0.023 mmol). The resulting mixture was stirred overnight at room temperature, at which time HPLC indicated all starting material had been consumed. The mixture was purified by stripping of volatiles under high vacuum, then passing through a plug of silica eluted with ethyl acetate. The resulting product was used in the next step without further purification. ESIMS (M+H + ): 395.1.
Example 3(m)
3-Pyridin-2-ylethynyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamine
[0235]
[0236] A mixture of 6-Nitro-3-pyridin-2-ylethynyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazole (2 mmol), SnCl 2 (1.37 g, 6.0 mmol), water (0.5 mL), and MeOH (10 mL), were stirred in a 60 deg C. oil bath for 30 min at which time HPLC indicated complete reduction. The resulting mixture was stripped of methanol, suspended in EtOAc (50 mL) and diluted with 1M NaOH (18 mL). The resulting emulsion was gently extracted EtOAc (10×25 ml). The combined organics were extracted with 1M Na 2 CO 3 , brine, dried over MgSO 4 , concentrated and filtered through a pad of silica eluted with EtOAc. The yield of crude product for two steps was 701 mg, 96% mass recovery. ESIMS (M+H + ): 365.1.
Example 3(n)
2-[3-Pyridin-2-ylethynyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid methyl ester
[0237]
[0238] A mixture of 3-Pyridin-2-ylethynyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamine (560 mg, 1.54 mmol), 2-bromomethylbenzoate (647.5 μL, 4.61 mmol), biphenyl-2-yl-dicyclohexyl-phosphane (107.8 mg, 0.308 mmol), Pd 2 (dba) 3 (70.5 mg, 0.0768 mmol), K 3 PO 4 (816 mg, 3.844 mmol), and dimethoxyethane (1.7 ml), were vacuum flushed with nitrogen, then heated in an oil bath at 70 degrees C. for 24 h. The black mixture was diluted with methylene chloride, and filtered, concentrated, and chromatographed (20% to 40% ethylacetate/hexanes). Yield of yellow/orange oil was 260 mg, 35% for three steps.
Example 3(o)
2-[3-Pyridin-2-ylethynyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid
[0239]
[0240] 2-[3-Pyridin-2-ylethynyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid methyl ester (253 mg, 0.517 mmol), was added to a solution of NaOH (62 mg, 1.55 mmol), dissolved in THF (1.0 mL), MeOH (2.25 mL), and water (0.5 mL). The reaction was stirred at room temperature for 1 h, at which time HPLC indicated that all starting material had been consumed. The reaction was neutralized with 1N HCL, extracted with ethylacetate, which was then washed with brine and dried with MgSO 4 . After concentrating under vacuum, 249 mg of yellow solid was obtained (99% mass recovery). This material was used without further purification. ESIMS (M−H − ): 483.0.
Example 3(p)
2-[3-Pyridin-2-ylethynyl-1H-indazol-6-ylamino]-benzoic acid
[0241]
[0242] A solution of 2-[3-Pyridin-2-ylethynyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid (231 mg, 0.477), 1M tetrabutylammonium fluoride in THF (3.8 mL, 3.816 mmol), and ethylenediamine (127 μL, 1.908 mmol), were stirred in an oil bath at 80 deg C. for 6 h. The reaction was quenched with acetic acid (218 μL, 3.816 mmol), diluted with water, and extracted with EtOAc (10×50 mL). The combined organics were washed with brine and dried over MgSO 4 . After concentrating a solid forms which was triturated with CH 2 Cl 2 , giving the product as a yellow powder (124 mg, 73%). ESIMS (M−H − ): 353.0.
Example 3(q)
N-Prop-2-ynyl-2-[3-((E)-2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0243]
[0244] A solution of 2-(3-Pyridin-2-ylethynyl-1H-indazol-6-ylamino)-benzoic acid (41 mg, 0.117 mmol), propargylamine (24 μL, 0.35 mmol), triethylamine (81 μl, 0.58 mmol), dissolved in DMF (0.5 mL), was treated with HATU (89 mg, 0.233 mmol). The mixture was stirred overnight, then purified by reverse phase HPLC yielding 27 mg (59%) of the title compound as a yellow solid. 1 H NMR (DMSO-d 6 ): δ 9.78 (1H, s), 8.99 (1H, m), 8.61 (1H, d, J=2.1), 7.88 (1H, s), 7.72 (3H, m), 7.43 (4H, m), 7.29 (1H, s), 7.04 (1H, d, J=7.3), 6.91 (1H, t, J=5.2), 4.04 (2H, s), 3.04 (1H, s). ESIMS (M+H + ): 392.1.
Example 4(a)
2-Bromo-4,6-dimethyl-pyridine
[0245]
[0246] A solution of 48% HBr (aq) (Aldrich, 65 mL, 1.2 mol, 10 eq) was cooled to −5° C. and treated with 4,6-dimethyl-pyridin-2-ylamine (Aldrich, 15.0 g, 0.12 mol. 1.0 eq). The thick white salt mixture was stirred with a mechanical stirrer while bromine (Aldrich, 19.7 mL, 0.38 mol, 3.1 eq) was added dropwise. The resultant red mixture was treated with an aqueous solution (32 mL H 2 O) of NaNO 2 (Aldrich, 22.1 g, 0.32 mol, 2.6 eq) over one hour. The temperature was maintained below 5° C. during the nitrite addition, and then gradually warmed to 20° C. over 2 hours. The reaction mixture was adjusted to pH 14 with NaOH (aq), and extracted with MTBE. The organic extracts were washed with water, brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The crude product (29 g of a red oil) was purified by flash chromatography (silica, 350 g) and eluted with 2-7% ethyl acetate-cyclohexane, which gave an orange oil (11.0 g, 48%). 1 H NMR (DMSO-d 6 , 300 MHz) δ 7.30 (1H, s), 7.13 (1H, s), 2.39 (3H, s), 2.26 (3H, s). 13 C NMR (DMSO-d 6 , 75 MHz) δ 159.4, 151.3, 140.9, 125.7, 124.0, 23.7, 20.3. ESI m/z 186/188 (M+H) + .
Example 4(b)
3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-6-nitro-1-(tetrahydro-pyran-2-yl)-1H-indazole
[0247]
[0248] A suspension of 2-bromo-4,6-dimethylpyridine (2.42 g, 13 mmol), 3-vinyl-6-nitro-1-(tetrahydro-pyran-2-yl)-1H-indazole (2.37 g, 8.67 mmol), palladium acetate (0.145 g, 0.65 mmol), tri-ortho-tolylphosphine (0.791 g, 2.6 mmol), and diisopropylethylamine (2.4 mL, 13.8 mmol) in aqueous DMF (85%, 34.5 mL) was degassed with Argon bubbling for 5 minutes followed by sonication for 5 minutes before heating in microwave apparatus (300 watts, 10% power) at 110° C. for 40 minutes. After cooling, the mixture was dropped into cold water. The resulting yellow ppt was collected by filtration. The solids were dissolved in ethyl acetate, dried (sodium sulfate), and concentrated under reduced pressure. The residue was purified on silica gel using a gradient of 0 to 20% ethyl acetate in a mixture of chloroform and hexanes (1:1) as eluent. Product from chromatography was triturated with MTBE/hexanes to obtain clean product as yellow solid. Mother liquor was repurified in a similar fashion on silica gel followed by trituration to obtain product in a 68% yield. 1 H NMR (CDCl 3 ): δ 8.54 (1H, s), 8.15 (1H, d, J=9.4 Hz), 8.08 (1H, dd, J=9.04, 1.9 Hz), 7.87 (1H, d, J=16.6 Hz), 7.55 (1H, d, J=16.6 Hz), 7.14 (1H, s), 6.90 (1H, s), 5.82 (1H, dd, J=9.0, 3.0 Hz), 4.08-4.01 (1H, m), 3.84-3.76 (1H, m), 2.56 (3H, s), 2.62-2.54 (1H, m), 2.34 (3H, s), 2.24-2.10 (2H, m), 1.88-1.68 (3H, m).
Example 5
3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamine
[0249]
[0250] A suspension of 3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-6-nitro-1-(tetrahydro-pyran-2-yl)-1H-indazole (4.22 g, 11.16 mmol), iron powder (2.71 g, 48.51 mmol) and sat. aq. NH 4 Cl (25 ml) in 25 ml of ethanol was heated at 45° C. for 18 hr. The reaction was cooled and filtered through filter paper washing with methanol. The solvents were removed under reduced pressure and the aqueous layer was extracted with EtOAc (2×). The combined organic layers were washed with brine, dried (MgSO 4 ) and concentrated under reduced pressure to give 4.02 g (quantitative) of a rust colored solid and was used without further purification.
[0251] 1 H NMR (DMSO-d6) δ 7.79 (1H, s), 7.74 (1H, d, J=16.4 Hz), 7.35 (1H, d, J=16.4 Hz), 7.29 (1H, s), 6.96 (1H, s), 6.63 (2H, m), 5.57 (1H, dd, J=2.4, 9.5 Hz), 5.44 (2H, broad s), 3.88 (1H, m), 3.67 (1H, m), 2.45 (3H, s), 2.37 (1H, m), 2.29 (3H, s), 1.99 (2H, m), 1.73 (1H, m), 1.57 (2H, m).
Example 6
2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester
[0252]
[0253] A stirred suspension of 3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamine (870 mg, 2.5 mmol), 2-Bromo-benzoic acid methyl ester (0.44 ml, 3.12 mmol), R-BINAP (78 mg, 0.125 mmol), Pd 2 (dba) 3 (29 mg, 0.03 mmol) and Cesium Carbonate (1.22 g, 3.75 mmol) in toluene (6 ml) was degassed and heated at 100° C. for 18 hr. The reaction mixture was cooled, poured into sat. NaHCO 3 and extracted with EtOAc (2×). The combined organic layers were washed with brine, dried (MgSO 4 ) and concentrated under reduced pressure. The residue was flash chromatographed on silica gel eluting a gradient of 5-10% EtOAc in CH 2 Cl 2 to give 964 mg (80%) of a yellow foam.
[0254] 1 H NMR (DMSO-d 6 ) δ 9.49 (1H, s), 8.13 (1H, d, J=8.7 Hz), 7.94 (1H, dd, J=1.5, 8.0 Hz), 7.85 (1H, d, J=16.4 Hz), 7.58 (1H, d, J=1.5 Hz), 7.48 (1H, d, J=16.4 Hz), 7.47 (1H, m), 7.37 (1H, d, J=7.7 Hz), 7.34 (1H, s), 7.19 (1H, dd, J=1.7, 8.7 Hz), 6.99 (1H, s), 6.89 (1H, t, J=8.1 Hz), 5.83 (1H, d, J=7.2 Hz), 3.88 (3H, s), 3.75 (1H, m), 2.48 (3H, s), 2.41 (2H, m), 2.31 (3H, s), 2.02 (2H, m), 1.75 (1H, m), 1.59 (2H, m). Anal. Calcd for C 29 H 30 N 4 O 3 .0.15 EtOAc: C, 71.71; H, 6.34; N, 11.30. Found: C, 71.60; H, 6.14; N, 11.37.
Example 7
2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid
[0255]
[0256] To a stirred solution of 2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester (1.98 g, 4.11 mmol) in THF:MeOH (12 ml, 3:1) was added Potassium hydroxide (1.15 g, 20.5 mmol) dissolved in H 2 O (3 ml). The reaction was heated at 70° C. for 2 hr, cooled, concentrated under reduced pressure to about 5 ml and diluted with more water. The solution was neutralized with 2N HCl and the precipitate was collected by filtration and washed with water to give 2.00 g (quantitative) of a bright yellow solid. 1 H NMR (DSMO-d 6 ) δ 13.12 (1H, broad s), 9.82 (1H, s), 8.13 (1H, d, J=8.7 Hz), 7.95 (1H, dd, J=1.5, 8.0 Hz), 7.89 (1H, d, J=16.4 Hz), 7.60 (1H, s), 7.50 (1H, d, J=16.4 Hz), 7.46 (1H, d, J=6.9 Hz), 7.37 (1H, d, J=7.7 Hz), 7.20 (1H, d, J=8.7 Hz), 7.06 (1H, s), 6.86 (1H, t, J=6.9 Hz), 5.85 (1H, d, J=7.3 Hz), 3.82 (2H, m), 2.50 (3H, s, obscured by dmso), 2.48 (2H, m), 2.34 (3H, s), 2.03 (2H, m), 1.76 (1H, m), 1.59 (2H, m). Anal. Calcd for C 28 H 28 N 4 O 3 .0.5 KOH: C, 67.72; H, 5.79; N, 11.28. Found: C, 67.65; H, 5.88; N, 11.07.
Example 8
2-{3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzoic acid p-toluene sulfonate
[0257]
A mixture of 2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid (2 mmol) and p-toluene sufonic acid (10 mmol) in aqueous methanol (90%, 20 mL) was stirred at 70 C for 18 hr. After cooling, the resulting thick yellow slurry was filtered and the solids washed with methanol to give 2-{3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzoic acid as the tosylate salt in 85% yield as a pale yellow solid. 1 H NMR (DMSO-d 6 ): δ 13.43 (1H, s), 9.78 (1H, s), 8.24-8.19 (2H, m), 8.09 (1H, d, J=9.04 Hz), 7.95 (1H, dd, J=7.9, 1.1 Hz), 7.62-7.55 (2H, m), 7.49-7.38 (5H, m), 7.20 (1H, dd, J=9.0, 1.9 Hz), 7.09 (2H, d, J=8.3 Hz), 6.86 (1H, dt, J=7.9, 1.1 Hz), 2.67 (3H, s), 2.54 (3H, s), 2.27 (3H, s).
Example 9
N-[4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide
[0258]
[0259] Prepared in a similar manner to that described for Example 33(a) step (v), in U.S. Pat. No. 6,531,491, issued Mar. 11, 2003, herein incorporated by reference in its entirety for all purposes, except using 4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynylamine and 2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid. 1 H NMR (DMSO-d 6 ) δ 9.56 (1H, s), 9.01 (1H, t, J=5.7 Hz), 8.06 (1H, d, J=8.7 Hz), 7.81 (1H, d, J=16.4 Hz), 7.66 (1H, d, J=7.5 Hz), 7.41 (4H, m), 7.32 (1H, s), 7.09 (1H, dd, J=1.8, 8.7 Hz), 6.98 (1H, s), 6.89 (1H, t, J=8.0 Hz), 5.79 (1H, dd, J=2.4, 9.2 Hz), 4.28 (2H, s), 4.09 (2H, m), 3.86(1H, m), 3.72 (1H, m), 2.46 (3H, s), 2.42 (1H, m), 2.30 (3H, s), 2.08 (2H, m), 1.74 (1H, m), 1.57 (2H, m), 0.80 (9H, s), 0.03 (6H, s). Anal. Calcd for C 38 H 47 N 5 O 3 Si.0.7 H 2 O: C, 68.89; H, 7.36; N, 10.57. Found: C, 68.99; H, 7.36; N, 10.21.
Example 10
2-{3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(4-hydroxy-but-2-ynyl)-benzamide
[0260]
[0261] A stirred solution of N-[4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide (737 mg, 1.13 mmol) and p-Toluene-sulfonic acid (8.2 ml, 12% in HOAC) was heated at 70° C. for 2 hr. The reaction was cooled, and cautiously poured into sat. NaHCO 3 and extracted with EtOAc (2×). The combined organic layers were washed with brine (2×), dried (MgSO 4 ) and concentrated under reduced pressure. The residue was flash chromatographed on silica gel eluting CH 2 Cl 2 :EtOAc: MeOH (1:1:0.1) to give 225 mg (44%) of a white solid. 1 H NMR (DMSO-d 6 ) δ 12.91 (1H, s), 9.84 (s, 1H), 9.01 (1H, t, J=5.3 Hz), 8.07 (1H, d, J=8.7 Hz), 7.84 (1H, d, J=16.4 Hz), 7.70 (1H, d, J=7.2 Hz), 7.43 (3H, m), 7.31 (1H, s), 7.26 (1H, s), 7.02 (1H, dd, J=1.6, 8.7 Hz), 6.97 (1H, s), 6.89 (1H, t, J=6.7 Hz), 5.12 (1H, t, J=5.8 Hz), 4.10 (2H, d, J=5.3 Hz), 4.07 (2H, d, J=5.8 Hz), 2.47 (3H, s), 2.31 (3H, s).
[0262] Anal. Calcd for C 27 H 25 N 5 O 2 .1.1 H 2 O: C, 68.80; H, 5.82; N, 14.86. Found: C, 68.72; H, 5.81 N, 14.65.
Example 11
4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynylamine
[0263]
[0264] To an ice cold, stirred solution of the known 4-(tert-Butyl-dimethyl-silanyloxy)-but-2-yn-1-ol (3.14 g, 15.7 mmol) in THF (50 ml) was added DBU (2.6 ml, 17.4 mmol) and DPPA (3.8 ml, 17.6 mmol). The solution was warmed to room temperature and stirred under an inert atmosphere overnight. The reaction was poured into sat. NaHCO 3 and the layers separated. The aqueous layer was re-extracted with EtOAc (2×) and the combined organic layers were dried (Na 2 SO 4 ), and concentrated under vacuum. Triphenylphosphine (4.61 g, 17.6 mmol) was added to this crude azide dissolved in THF (50 ml), followed by addition of H 2 O (0.44 ml). The resultant solution was stirred overnight at room temperature, concentrated under reduced pressure and the residue was slurried in a 1:1 mixture of Et 2 O/pet ether. The solids were removed and the filtrate was concentrated and purified by flash chromatography on silica gel eluting CH 2 Cl 2 /MeOH (19:1) to give an amber oil. 1 H NMR (CDCl 3 ) δ 4.19 (2H, t, J=1.9 Hz), 3.33 (2H, t, J=1.9 Hz), 0.79 (9H, s), 0.00 (6H, s).
Example 12
2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-N-prop-2-ynyl-benzamide
[0265]
[0266] Prepared in a similar manner to that described for Example 6 above, except using 2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid and propargyl amine. 1 H NMR (DMSO-d 6 ) δ 9.87 (1H, s), 9.04 (1H, t, J=5.8 Hz), 8.08 (1H, d, J=8.7 Hz), 7.83 (1H, d, J=16.4 Hz), 7.69 (1H, d, J=7.5 Hz), 7.44 (4H, m), 7.34 (1H, s), 7.12 (1H, dd, J=1.7, 8.7 Hz), 6.99 (1H, s), 6.91 (1H, t, J=5.8 Hz), 5.81 (1H, dd, J=2.4, 9.2 Hz), 4.07 (2H, dd, J=2.5, 5.7 Hz), 3.88 (1H, m), 3.74 (1H, m), 3.12 (1H, t, J=2.5 Hz), 2.48 (3H, s), 2.43 (1H, m), 2.31 (3H, s), 2.01 (2H, m), 1.74 (1H, m), 1.58 (2H, m).
[0267] Anal. Calcd for C 31 H 31 N 5 O 2 .1.1 H 2 O.0.3 TBME: C, 70.73; H, 6.72; N, 12.69. Found: C, 70.56; H, 6.45; N, 12.49.
Example 13
N-(prop-2-ynyl)-2-{3-[(E)-2-(2,4-dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide
[0268]
[0269] Prepared in a similar manner to that described for Example 7 except using N-(3-Cyclopropyl-prop-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide instead of N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ): δ 12.90 (1H, s), 9.78 (1H, s), 9.01 (1H, t, J=5.3 Hz), 8.06 (1H, d, J=8.3 Hz), 7.84 (1H, d, J=16.2 Hz), 7.68 (1H, dd, J=7.9, 1.1 Hz), 7.45-7.36 (3H, m), 7.30 (1H, s), 7.25 (1H, d, J=1.5 Hz), 7.01 (1H, dd, J=8.7, 1.9 Hz), 6.96 (1H, s), 6.88 (1H, dt, J=6.8, 1.9 Hz), 4.04 (2H, dd, J=5.6, 2.6 Hz), 3.11 (1H, t, J=2.6 Hz), 2.46 (3H, s), 2.29 (3H, s).
Example 14
2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-N-(2-methyl-allyl)-benzamide
[0270]
[0271] Prepared in a similar manner to that described for Example 6 above, except using 2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid and 2-Methyl-allylamine. 1 H NMR (DMSO-d 6 ) δ 9.87 (1H, s), 8.82 (1H, t, J=5.8 Hz), 8.07 (1H, d, J=8.7 Hz), 7.82 (1H, d, J=16.4 Hz), 7.74 (1H, d, J=7.3 Hz), 7.43 (4H, m), 7.33 (1H, s), 7.10 (1H, d, J=8.7 Hz), 6.99 (1H, s), 6.92 (1H, t, J=7.8 Hz), 5.80 (1H, dd, J=2.2, 9.2 Hz), 4.83 (2H, d, J=11.8 Hz), 3.83 (4H,m), 2.47 (3H, s), 2.44 (1H, m), 2.31 (3H, s), 2.00 (2H, m), 1.75 (1H, m), 1.73 (3H, s), 1.58 (2H, m).
[0272] Anal. Calcd for C 32 H 35 N 5 O 2 .1.09 H 2 O: C, 71.00; H, 6.92; N, 12.94. Found: C, 71.40; H, 6.89; N, 12.54.
Example 15
2-{3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(2-methyl-allyl)-benzamide
[0273]
[0274] Prepared in a similar manner to that described for Example 7 except using N-(2-Methyl-allyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide instead of N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ) δ 12.89 (1H, s), 9.75 (1H, s), 8.79 (1H, t, J=5.6 Hz), 8.05 (1H, d, J=8.7 Hz), 7.85 (1H, d, J=16.2 Hz), 7.74 (1H, d, J=7.9 Hz), 7.45-7.33 (4H, m), 7.23 (1H, d, J=1.5 Hz), 7.00-6.97 (2H, m), 6.90 (1H, dt, J=7.9, 1.1 Hz), 4.81 (2H, d, J=11.3 Hz), 3.81 (2H, d, J=5.6 Hz), 2.47 (3H, s), 2.30 (3H, s), 1.71 (3H, s).
Example 16(a)
Cyclopropyl-prop-2-yn-1-ol
[0275]
[0276] To a round bottom flask containing 70 mL anhydrous THF cooled in −10° C. ice bath was added 65.6 mL 1.6M BuLi in hexanes (105 mmol). 5-Chloro-pent-1-yne (5.13 g, 50 mmol) was introduced slowly while maintaining temperature at −10 to 0° C. The mixture was stirred at 0° C. for two hours under argon. Paraformaldehyde (3 g, 100 mmol) was added as a solid. The mixture was warmed up slowly to room temperature and stirred overnight under argon. The next day, water was added and c.a. 50 mL 1 N aqueous HCl was added. The mixture was extracted with ethyl acetate and the combined organic layers was washed with brine, dried over Na 2 SO 4 , filtered and concentrated. The crude product was purified by column eluting with 20% Et 2 O in hexanes to give 3 g 3-cyclopropyl-prop-2-yn-1-ol as an oil (62% yield). 1 H NMR (CDCl 3 ) δ 4.22 (dd, 2H, J=6.04, 2.01 Hz), 1.46 (t, 1H, J=6.04 Hz), 1.26 (m, 1H), 0.77 (m, 2H), 0.70 (m, 2H).
Example 16(b)
3-Cyclopropyl-prop-2-ynylazide
[0277]
[0278] 3-Cyclopropyl-prop-2-yn-1-ol (3.28 g, 34.1 mmol) was dissolved in 40 mL toluene, DPPA (11.26 g, 40.9 mmol) was added, followed with DBU (6.24 g, 40.9 mmol) while maintaining temperature with a water bath. The mixture was stirred at room temperature for one hour and was diluted with 100 mL hexane and 15 mL CH 2 Cl 2 . The mixture was washed with water four times and once with brine, dried over Na 2 SO 4 , filtered and concentrated under rotovap with cold water bath to remove most of organic solvent leaving some toluene (product volatile). The residual oil was used for the next step.
[0279] 1 H NMR (CDCl 3 ) δ 3.85 (s, 2H), 1.26 (m, 1H), 0.80 (m, 2H), 0.72 (m, 2H).
Example 16(c)
3-Cyclopropyl-prop-2-ynylamine
[0280]
[0281] 3-Cyclopropyl-prop-2-ynylazide (c.a. 34 mmol) was dissolved in 100 mL THF, 1 mL water was added, followed with addition of PPh 3 (13.37 g, 51 mmol) as a solid while maintaining temperature with a water bath. The mixture was stirred at room temperature for one hour. 150 mL 1N aqueous HCl was added to the mixture. The mixture was washed with methylene chloride three times. The aqueous layer was basified with 5 N NaOH to pH 10˜12. The mixture was extracted with ethyl acetate. The aqueous layer was checked with TLC staining to monitor progress of extraction of amine to the organic phase. The combined organic layer was dried over Na 2 SO 4 , filtered, and concentrated to give 1.62 g desired product (product volatile, contains residual EtOAc solvent) (50% yield for two steps). 1 H NMR (CDCl 3 ) δ 3.37 (d, 2H, J=2 Hz), 1.22 (m, 1H), 0.74 (m, 2H), 0.65 (m, 2H).
Example 17
N-(3-Cyclopropyl-prop-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide
[0282]
Was prepared in a similar manner to that described for Example 6 above, except using 2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid E and 3-Cyclopropyl-prop-2-ynylamine. 1 H NMR (CDCl 3 ): δ 9.51 (1H, s), 7.97 (1H, d, J=8.7 Hz), 7.81 (1H, d, J=16.6 Hz), 7.51-7.42 (3H, m), 7.34-7.29 (2H, m), 7.16 (1H, s), 7.11 (1H, dd, J=9.0, 1.9 Hz), 6.85 (1H, s), 6.81 (1H, dt, J=7.2, 1.1 Hz), 6.23 (1H, t, J=7.2 Hz), 5.61 (1H, dd, J=9.0, 2.6 Hz), 4.17 (2H, dd, J=5.3, 2.3 Hz), 4.07-4.00 (1H, m), 3.75-3.66 (1H, m), 2.63-2.50 (1H, m), 2.54 (3H, s), 2.32 (3H, s), 2.20-2.02 (2H, m), 1.79-1.62 (3H, m), 1.29-1.19 (1H, m), 0.77-0.67 (4H, m).
Example 18
N-(3-Cycloprop-2-ynyl)-2-{3-[(E)-2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide
[0283]
[0284] Prepared in a similar manner to that described for Example 7 above, except using 2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-N-prop-2-ynyl-benzamide instead of N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ): δ 12.90 (1H, s), 9.79 (1H, s), 8.91 (1H, t, J=5.6 Hz), 8.06 (1H, d, J=8.7 Hz), 7.83 (1H, d, J=16.2 Hz), 7.68 (1H, dd, J=7.9, 1.1 Hz), 7.49-7.38 (3H, m), 7.29 (1H, s), 7.25 (1H, d, J=1.9 Hz), 6.99 (1H, dd, J=9.0, 2.3 Hz), 6.96 (1H, s), 6.88 (1H, dt, J=7.9, 1.5 Hz), 4.00 (2H, dd, J=5.6, 1.9 Hz), 2.46 (3H, s), 2.29 (3H, s), 1.31-1.23 (1H, m), 0.75-0.70 (2H, m), 0.57-0.52 (2H, m).
Example 19(a)
2-Butyne-1,4-diol, monoacetate
[0285]
[0286] To a solution of butyne-1,4-diol (5 g, 58 mmol) in dry THF at room temperature (RT) was added portion-wise sodium hydride (60% dispersion in oil, 2.32 g, 58 mmol). After 4.3 hr, acetyl chloride (4.12 mL, 58 mmol) was added. After stirring at RT for 22 hr, the mixture was concentrated under reduced pressure. The residue was concentrated twice from toluene before purification on silica gel using ethyl acetate/dichloromethane (1:3) as eluent to give 2-Butyne-1,4-diol, monoacetate as an oil in 49% yield. 1 H NMR (DMSO-d 6 ) δ 5.23 (1H, bs), 4.70 (2H, t, J=1.8 Hz), 4.09 (2H, s), 2.03 (3H, s).
Example 19(b)
Acetic acid 4-amino-but-2-ynyl ester
[0287]
[0288] Prepared in a similar manner as described in Example 8 except 2-Butyne-1,4-diol monoacetate was used instead of 4-(tert-Butyl-dimethyl-silanyloxy)-but-2-yn-1-ol. 1 H NMR (DMSO-d 6 ) δ 4.77 (2H, s), 4.20 (2H, s), 2.04 (3H, s).
Example 20
Acetic acid 4-(2-{3-[(E)-2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzoylamino)-but-2-ynyl ester
[0289]
[0290] Prepared in a similar manner to that described for Example 6 above, except using 2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl] 1H-indazol-6-ylamino]-benzoic acid p-toluene sulfonate and Acetic acid 4-amino-but-2-ynyl ester. 1 H NMR (CD 3 CN): δ 11.00 (1H, bs), 9.59 (1H, s), 7.99 (1H, d, J=8.6 Hz), 7.86 (1H, d, J=16.4 Hz), 7.58 (1H, d, J=7.8 Hz), 7.49-7.37 (4H, m). 7.32 (1H,s), 7.21 (1H, s), 7.06 (1H, dd, J=8.8, 1.8 Hz), 6.96 (1H, s), 6.90 (1H, t, J=7.8 Hz), 4.63 (2H, s), 4.16 (2H, d, J=5.6 Hz), 2.49 (3H, s), 2.32 (3H, s), 2.01 (3H, s).
Example 21
2-[3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinic acid methyl ester
[0291]
[0292] Prepared in a similar manner to that described for Example 3 above except using 2-Bromo-nicotinic acid methyl ester instead of 2-bromo-benzoic acid methyl ester. 1 H NMR (DMSO-d 6 ): δ 10.36 (1H, s), 8.50 (1H, dd, J=4.7, 1.9 Hz), 8.36 (1H, d, J=1.4 Hz), 8.30 (1H, dd, J=7.8, 2.0 Hz), 8.08 (1H, d, J=8.8 Hz), 7.83 (1H, d, J=16.4 Hz), 7.48 (1H, d, J=7.5 Hz), 7.44 (1H, s), 7.33 (1H, s), 6.98-6.93 (2H, m), 5.80 (1H, d, J=7.0 Hz), 2.93 (3H, s), 3.93-3.90 (1H, m), 3.80-3.75 (1H, m), 2.46 (3H, s), 2.30 (3H, s), 2.10-1.97 (2H, m), 1.89-1.60 (3H, m).
Example 22
2-[3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinic acid
[0293]
[0294] Prepared in a similar manner to that described for Example 4 except using 2-[3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinic acid methyl ester instead of 2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester. 1 H NMR (DMSO-d 6 ): δ 10.73 (1H, s), 8.49 (1H, d, J=1.9 Hz), 8.45 (1H, s), 8.31 (1H, dd, J=7.7, 1.8 Hz), 8.16-7.97 (3H, m), 7.70 (1H, d, J=16.4 Hz), 7.50 (1H, d, J=8.6 Hz), 7.37 (1 (1H, dd, J=7.7, 4.8 Hz), 5.87 (1H, d, J=8.4 Hz), 3.95-3.90 (1H, m), 3.79-3.70 (1H, m), 2.63 (3H, s), 2.47 (3H, s), 2.07-1.99 (2H, m), 1.81-1.62 (3H, m).
Example 23
2-{3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(4-hydroxy-but-2-ynyl)-nicotinamide
[0295]
[0296] A crude mixture of N-(4-Hydroxy-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinamide and N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinamide was prepared from 2-[3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinic acid and 4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynylamine in a similar fashion to that described for Example 6 above and subsequently converted to 2-{3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(4-hydroxy-but-2-ynyl)-nicotinamide in a similar fashion to that described for Example 7 except using a mixture of N-(4-Hydroxy-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinamide and N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinamide instead of N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ): δ 12.99 (1H, s), 11.21 (1H, s), 9.26 (1H, t, J=5.3 Hz), 8.50 (1H, d, J=1.9 Hz), 8.41 (1H, dd, J=4.9, 1.9 Hz), 8.16 (1H, dd, J=8.3, 1.9 Hz), 8.04 (1H, d, J=9.0 Hz), 7.85 (1H, d, J=16.6 Hz), 7.42 (1H, d, J=16.6 Hz), 7.31 (1H,s), 7.06 (1H, dd, J=8.7, 1.5 Hz), 6.96 (1H, s), 6.93 (1H, dd, J=7.5, 4.9 Hz), 5.14 (1H, t, J=5.6 Hz), 4.16 (2H, d, J=5.6 Hz), 4.08 (2H, d, J=7.2 Hz), 2.46 (3H, s), 2.30 (3H, s).
Example 24
2-{3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-nicotinic acid p-toluene sulfonate
[0297]
[0298] Prepared in a similar manner to that described for Example 5 except using 2-[3-[(E)-2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-nicotinic acid instead of 2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid.
[0299] 1 H NMR (DMSO-d 6 ): δ 13.49 (1H, s), 10.80 (1H, s), 8.63 (1H, d, J=1.5 Hz), 8.49 (1H, dd, J=4.8, 1.9 Hz), 8.31 (1H, dd, J=7.7, 1.9 Hz), 8.24-8.19 (2H, m), 8.06 (1H, d, J=8.8 Hz), 7.60-7.55 (2H, m), 7.46 (2H, d, J=8.1 Hz), 7.22 (1H, dd, J=8.8, 1.7 Hz), 7.09 (2H, d, J=7.9 Hz), 6.95 (1H, dd, J=7.7, 4.7 Hz), 2.66 (3H, s), 2.54 (3H, s), 2.27 (3H, s).
Example 25
N-(3-Cyclopropyl-prop-2-ynyl)-2-{3-[(E)-2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-nicotinamide
[0300]
[0301] Prepared in a similar manner to that described for Example 6 above, except using 2-{3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-nicotinic acid p-toluene sulfonate and 3-Cyclopropyl-prop-2-ynylamine. 1 H NMR (DMSO-d 6 ): δ 13.01 (1H, s), 11.20 (1H, s), 9.19 (1H, bt), 8.51 (1H, s), 8.40 (1H, d, J=4.9 Hz), 8.15 (1H, d, J=7.5 Hz), 8.05 (1H, d, J=8.7 Hz), 7.83 (1H, d, J=16.4 Hz), 7.42 (1H, d, J=16.4 Hz), 7.31 (1H, s), 7.05 (1H, d, J=8.3 Hz), 6.96 (1H, s), 6.92 (1H, dd, J=7.5, 4.9 Hz), 4.06 (2H, d, J=4.14 Hz), 2.46 (3H, s), 2.29 (3H, s), 1.33-1.28 (1H, m), 0.77-0.72 (2H, m), 0.60-0.55 (2H, m).
Example 26
4-Methyl-2-vinyl-pyridine
[0302]
[0303] A yellow mixture of 2-bromo-4-methyl-pyridine (Aldrich, 5.2 g, 30.5 mmol, 1.0 eq), 2,6-di-tert-butyl-4-methyl-phenol (Aldrich, 67 mg, 0.3 mmol, 1 mol %), tributyl-vinyl-stannane (Aldrich, 26.8 mL, 91.5 mmol, 3.0 eq) and tetrakis(triphenylphosphine) palladium (0) (Strem, 1.8 g, 1.5 mmol, 5 mol %) in toluene (100 mL) was degassed and purged with argon. An amber solution was obtained after the mixture was warmed to 100° C. The reaction mixture was quenched after 18 hours by the addition of 1.0 M HCl. The acidic extract was washed with ether, adjusted to pH 9 with solid sodium bicarbonate, and extracted with ethyl acetate. The organic extracts were washed with brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The crude product (3.7 g of a brown oil) was purified by flash chromatography (silica) and eluted with 0-5% ethyl acetate-dichloromethane, which gave a clear oil (1.9 g, 53%). 1 H NMR (DMSO-d 6 , 300 MHz) δ 8.39 (1H, d, J=4.9 Hz), 7.33 (1H, s), 7.10 (1H, dd, J=5.0, 0.8 Hz), 6.77 (1H, dd, 17.5, 10.8 Hz), 6.20 (1H, dd, J=17.5, 1.7 Hz), 5.44 (1H, dd, J=10.8, 1.8 Hz), 2.31 (3H, s). ESIMS m/z 120 (M+H) + .
Example 27
3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-6-nitro-1-(tetrahydro-pyran-2-yl)-1H-indazole
[0304]
[0305] A suspension of 4-Methyl-2-vinyl-pyridine (Example 23) (1.9 g, 15.97 mmol), 6-Nitro-1-(tetrahydro-pyran-2-yl)-3-vinyl-1H-indazole (4.96 g, 13.3 mmol), Pd(OAc) 2 (149 mg, 0.66 mmol), P(o-tolyl) 3 , and DIEA(3.5 ml, 19.96 mmol) in degassed DMF (50 ml) was heated under argon at 100° C. for 18 hr. The reaction mixture was cooled and the solids removed by filtration washing with EtOAc. The filtrate was diluted with EtOAc and washed with brine (2×), dried (MgSO 4 ) and concentrated under reduced pressure. The residue was chromatographed on silica gel eluting Hexanes:EtOAc (3:1) to give 3.40 g (70%) of a bright yellow solid.
[0306] 1 H NMR (CDCl 3 ) δ 8.56 (1H, s), 8.50 (1H, d, J=5.0 Hz), 8.11 (2H, m), 7.89 (1H, d, J=16.3 Hz), 7.61 (1H, s), 7.03 (1H, d, J=4.3 Hz), 5.83 (1H, dd, J=2.6, 9.0 Hz), 4.06 (1H, m), 3.82 (1H, m), 2.58 (1H, m), 2.39 (3H, s), 2.18 (2H, m), 1.78 (3H, m). Anal. Calcd for C 20 H 20 N 4 O 3 : C, 65.92; H, 5.53; N, 15.38. Found: C, 65.80; H, 5.52; N, 15.15.
Example 28
3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamine
[0307]
[0308] Prepared in a similar manner to that described for Example 2 except using [2-(4-Methyl-pyridin-2-yl)-vinyl]-6-nitro-1-(tetrahydro-pyran-2-yl)-1H-indazole (Example 24) instead of 3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-6-nitro-1-(tetrahydro-pyran-2-yl)-1H-indazole. 1 H NMR (DMSO-d 6 ): δ 8.43 (1H, d, J=4.8 Hz), 7.79-7.73 (2H, m), 7.50 (1H, s), 7.39 (1H, d, J=16.4 Hz), 7.09 (1H, d, J=4.8 Hz), 6.64-6.62 (2H, m), 5.57 (1H, dd, J=9.8, 2.5 Hz), 5.48 (2H, bs), 3.92-3.85 (1H, m), 3.72-3.64 (1H, m), 2.43-2.34 (1H, m), 2.33 (3H, s), 2.07-2.00 (1H, m), 1.96-1.90 (1H, m), 1.79-1.66 (1H, m), 1.60-1.53 (2H, m).
Example 29
2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester
[0309]
[0310] Prepared in a similar manner to that described for Example 3 except using 3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamine instead of 3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamine. 1 H NMR (DMSO-d 6 ): δ 9.48 (1H, s), 8.45 (1H, d, J=4.9 Hz), 8.13 (1H, d, J=8.7 Hz), 7.93 (1H, dd, J=8.3, 1.9 Hz), 7.86 (1H, d, J=16.2 Hz), 7.58 (1H, d, J=1.9 Hz), 7.54-7.44 (3H, m), 7.36 (1H, d, J=7.5 Hz), 7.18 (1H, dd, J=8.7, 1.9 Hz), 7.11 (1H, d, J=4.9 Hz), 6.87 (1H, t, J=8.3 Hz), 5.83 (1H, dd, J=9.4, 2.3 Hz), 3.87 (3H, 1H), 3.93-3.84 (1H, m), 3.77-3.69 (1H, m), 2.46-2.37 (1H, m), 2.34 (3H, s), 2.10-1.94 (2H, m), 1.81-1.53 (3H, m).
Example 30
2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid
[0311]
[0312] Prepared in a similar manner to that described for Example 4 above except that 2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester was used instead of 2-[3-[2-(4,6-Dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid methyl ester (Example 3). 1 H NMR (DMSO-d 6 ) δ 13.17 (1H, broad s), 9.83 (1H, s), 8.51 (1H, d, J=5.2 Hz), 8.14 (1H, d, J=8.7 Hz), 7.95 (1H, d, J=16.4 Hz), 7.94 (dd, 1H, J=1.5, 8.0 Hz), 7.73 (1H, s), 7.60 (1H, d, J=1.5 Hz), 7.59 (1H, s), 7.54 (1H, s), 7.46 (1H, m), 7.37 (1H, d, J=7.6 Hz), 7.23 (2H, m), 6.86 (1H, t, J=6.9 Hz), 5.87 (1H, d, J=7.6 Hz), 3.90 (1H, m), 3.76 (1H,m), 2.45 (1H,m), 2.41 (3H, s), 2.03 (2H, m), 1.77 (1H, m), 1.59 (2H, m).
Example 31
2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-N-prop-2-ynyl-benzamide
[0313]
[0314] Prepared in a similar manner to that described for Example 6 above, except using propargyl amine and 2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid. 1 H NMR (DMSO-d 6 ) δ 9.87 (1H, s), 9.03 (1H, t, J=5.5 Hz), 8.46 (1H, d, J=4.9 Hz), 8.08 (1H, d, J=8.7 Hz), 7.86 (1H, d, J=16.4 Hz), 7.69 (1H, d, J=7.3 Hz), 7.53 (1H, s), 7.44 (4H, m), 7.13 (2H, m), 6.91 (1H, t, J=7.9 Hz), 5.81 (1H, dd, J=2.2, 9.6 Hz), 4.07 (2H, dd, J=2.5, 5.5 Hz), 3.89 (1H,m), 3.75 (1H, m), 3.12 (1H, t, J=2.5 Hz), 2.42 (1H, m), 2.36 (3H, s), 2.00 (2H, m), 1.75 (1H, m), 1.58 (2H, m).
[0315] Anal. Calcd for C 30 H 29 N 5 O 2 .0.25 TBME: C, 73.07; H, 6.28; N, 13.64. Found: C, 72.95; H, 6.30; N, 13.64.
Example 32
2-{3-[(E)-2-(4-Methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-prop-2-ynyl-benzamide
[0316]
[0317] Prepared in a similar manner to that described for Example 7 except that 2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-N-prop-2-ynyl-benzamide was used instead of N-[4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ) δ 12.93,s), 9.79 (1H, s), 9.02 (1H, t, J=5.4 Hz), 8.45 (1H, d, J=4.9 Hz), 8.08 (1H, d, J=8.7 Hz), 7.88 (1H, d, J=16.4 Hz), 7.69 (1H, d, J=7.7 Hz), 7.45 (4H, m). 7.27 (1H, s),), 7.10 (1H, d, J=4.9 Hz), 7.03 (1H, d, J=8.8 Hz), 6.90 (1H, t, J=7.9 Hz), 4.06 (2H, dd, J=2.4, 5.4 Hz), 3.12 (1H, t, J=2.4 Hz), 2.35 (3H, s).
[0318] Anal. Calcd for C 25 H 21 N 5 O.0.35 CH 2 Cl 2 : C, 69.64; H, 5.00; N, 16.02. Found: C, 69.65; H, 5.15; N, 15.80.
Example 33
N-(2-Methyl-allyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide
[0319]
[0320] Prepared in a similar manner to that described for Example 6 above, except using 2-Methyl-allylamine and 2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid. 1 H NMR (DMSO-d 6 ) δ 9.86 (1H, s), 8.81 (1H, t, J=5.5 Hz), 8.46 (1H, d, J=4.9 Hz), 8.07 (1H, d, J=8.9 Hz), 7.86 (1H, d, J=16.4 Hz), 7.75 (1H, d, J=7.7 Hz), 7.54 (1H, s), 7.50 (1H, d, J=16.4 Hz), 7.43 (3H, m), 7.11 (2H, m), 6.92 (1H, t, J=8.1 Hz), 5.81 (1H, dd, J=2.5, 9.8 Hz), 4.83 (2H, d, J=11.5 Hz), 3.81 (4H, m), 2.41 (1H, m), 2.35 (3H, s), 2.00 (2H, m), 1.76 (1H, m), 1.73 (3H, s), 1.58 (2H, m). Anal. Calcd for C 31 H 33 N 5 O 2 . 0.80 TBME: C, 72.71; H, 7.43; N, 12.11. Found: C, 72.43; H, 7.57; N, 12.02.
Example 34
N-(2-Methyl-allyl)-2-{[(E)-2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-ylamino}-benzamide
[0321]
[0322] Prepared in a similar manner to that described for Example 7 except that N-(2-Methyl-allyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide was used instead of N-[4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ) δ 12.90 (1H, s), 9.76 (1H, s), 8.80 (1H, t, J=5.5 Hz), 8.45 (1H, d, J=5.1 Hz), 8.07 (1H, d, J=8.9 Hz), 7.88 (1H, d, J=16.4 Hz), 7.75 (1H, d, J=7.9 Hz), 7.51 (1H, s), 7.48 (1H, d, J=16.4 Hz), 7.43 (2H, m), 7.24 (1H, s), 7.10 (1H, d, J=4.9 Hz), 7.00 (1H, dd, J=1.9, 8.9 Hz), 6.91 (1H, t, J=8.1 Hz), 4.82 (2H, d, J=11.3 Hz), 3.83 (2H, d, J=5.8 Hz), 2.35 (3H, s), 1.73 (3H, s).
[0323] Anal. Calcd for C 26 H 25 N 5 O.0.20 H 2 O: C, 73.11; H, 5.99; N, 16.40. Found: C, 73.13; H, 6.03; N, 16.13.
Example 35
N-(3-Cyclopropyl-prop-2-ynyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide
[0324]
[0325] Prepared in a similar manner to that described for Example 6 above, except using 2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid and 3-Cyclopropyl-prop-2-ynylamine. 1 H NMR (DMSO-d 6 ): δ 9.88 (1H, bs), 8.93 (1H, bt), 8.46 (1H, d, J=4.9 Hz), 8.08 (1H, d, J=8.7 Hz), 7.85 (1H, d, J=16.4 Hz), 7.69 (1H, d, J=7.6 Hz), 7.54-7.40 (5H, m), 7.14-7.11 (2H, m), 6.90 (1H, t, J=6.1 Hz), 5.81 (1H, d, J=7.5 Hz), 4.02 (2H, d, J=3.6 Hz), 3.95-3.85 (1H, m), 3.79-3.72 (1H, m), 2.49-2.35 (1H, m), 2.35 (3H, s), 2.15-2.01 (2H, m), 1.87-1.55 (3H, m), 1.30-1.25 (1H, m), 0.77-0.70 (2H, m), 0.59-0.54 (2H, m).
Example 36
N-(3-Cycloprop-2-ynyl)-2-{3-[(E)-2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide
[0326]
[0327] Prepared in a similar manner to that described for Example 7 above except using N-(3-cycloprop-2-ynyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide instead of N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ): δ 12.91 (1H, s), 9.79 (1H, s), 8.91 (1H, t, J=5.6 Hz), 8.44 (1H, d, J=4.9 Hz), 8.06 (1H, d, J=8.7 Hz), 7.87 (1H, d, J=16.6 Hz), 7.67 (1H, dd, J=7.9, 1.5 Hz), 7.50-7.35 (4H, m), 7.24 (1H, d, J=1.9 Hz), 7.09 (1H, d, J=4.9 Hz), 7.00 (1H, dd, J=8.7, 1.5 Hz), 6.88 (1H, dt, J=4.1, 1.5 Hz), 4.00 (2H, dd, J=5.3, 1.9 Hz), 2.34 (3H, s), 1.31-1.23 (1H, m), 0.75-0.69 (2H, m), 0.56-0.52 (2H, m).
Example 37
2-{3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-pyridin-2-ylmethyl-benzamide
[0328]
[0329] Prepared in a similar manner to that described for Example 6 and Example 7 above except using 2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid and C-Pyridin-2-yl-methylamine. 1 H NMR (DMSO-d 6 , 300 MHz) δ 12.91 (1H, s), 9.77 (1H, s), 9.19 (1H, t, J=5.8 Hz), 8.50 (1H, d, J=4.1 Hz), 8.45 (1H, d, J=5.0 Hz), 8.06 (1H, d, J=8.8 Hz), 7.88 (1H, d, J=16.4 Hz), 7.82-7.70 (2H, m), 7.51-7.25 (7H, m), 7.10 (1H, d, J=4.6 Hz), 6.98 (1H, dd, J=8.8, 1.8 Hz), 6.96-6.91 (1H, m), 4.58 (2H, d, J=5.9 Hz), 2.35 (3H, s). ESIMS m/z 461 (M+H) + . Anal. Calcd. for C 28 H 24 N 6 O×0.3 MTBE: C, 72.71; H, 5.77; N, 17.25. Found: C, 72.38; H, 5.80; N, 16.88.
Example 38
2-{3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-pyridin-4-ylmethyl-benzamide
[0330]
[0331] Prepared in a similar manner to that described for Examples 6 and 7 above except using 2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid and C-Pyridin-4-yl-methylamine.
[0332] 1 H NMR (DMSO-d 6 , 300 MHz) δ 12.90 (1H, s), 9.73 (1H, s), 9.21 (1H, t, J=5.9 Hz), 8.49-8.44 (3H, m), 8.06 (1H, d, J=8.7 Hz), 7.88 (1H, d, J=16.4 Hz), 7.81 (1H, d, J=7.5 Hz), 7.51-7.40 (4H, m), 7.31 (2H, d, J=5.9 Hz), 7.24 (1H, s), 7.11 (1H, d, J=4.4 Hz), 7.00 (1H, dd, J=8.7, 1.7 Hz), 6.97-6.92 (1H, m), 4.50 (2H, d, J=5.9 Hz), 2.35 (3H, s). ESIMS m/z 461 (M+H) + .
[0333] Anal. Calcd. for C 28 H 24 N 6 O×0.4 H 2 O×0.7 MTBE: C, 71.36; H, 6.45; N, 15.85. Found: C, 71.27; H, 6.29; N, 15.53.
Example 39
N-(6-Methyl-pyridin-2-ylmethyl)-2-{3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide
[0334]
[0335] Prepared in a similar manner to that described for Examples 6 and 7 above except using 2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid and C-(6-Methyl-pyridin-2-yl)-methylamine.
[0336] 1 H NMR (DMSO-d 6 , 300 MHz) δ 12.92 (1H, s), 9.76 (1H, s), 9.20 (1H, t, J=5.8 Hz), 8.44 (1H, d, J=4.9 Hz), 8.05 (1H, d, J=8.6 Hz), 7.86 (1H, d, J=16.4 Hz), 7.81 (1H, d, J=7.7 Hz), 7.59 (1H, t, J=7.7 Hz), 7.49-7.37 (4H, m), 7.23 (1H, s), 7.11-7.08 (3H, m), 6.99 (1H, dd, J=8.7, 1.6 Hz), 6.95-6.90 (1H, m), 4.51 (2H, d, J=5.9 Hz), 2.42 (3H, s), 2.33 (3H, s), ESIMS m/z 475 (M+H) + . Anal. Calcd. for C 29 H 26 N 6 O×0.4 DCM: C, 68.98; H, 5.29; N, 16.39. Found: C, 68.84; H, 5.42; N, 16.20.
Example 40
N-(2,6-Dimethyl-2H-pyrazol-3-ylmethyl)-2-[(E)-3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide
[0337]
[0338] Prepared in a similar manner to that described for Example 6 above, except using 2-{3-[2-(4-methyl-pyridin-2-yl-vinyl)-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid and C-(2,5-Dimethyl-2H-pyrazol-3-yl)-methylamine. 1 H NMR (DMSO-d 6 ) δ 9.81(1H, s), 9.05 (1H, bt), 8.46 8.7 Hz), 7.85 (1H, d, J=16.4 Hz), 7.71 (1H, d, J=7.5 Hz), 7.54-7.40 (5H, m), 7.11-7.09 (2H, m), 6.91 (1H, t, J=6.9 Hz), 5.94 (1H, s), 5.80 (1H, d, J=7.3 Hz), 4.45 (2H, d, J=5.5 Hz), 3.93-3.85 (1H, m), 3.78-3.69 (1H, m), 3.73 (3H,s), 2.45-2.35 (1H, m), 2.35 (3H, s), 2.07 (3H, s), 2.06-1.95 (2H, m), 1.85-1.53 (m, 3H).
Example 41
N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-{3-[(E)-2-(4-methyl-pyridin-2-yl-vinyl]-1H-indazol-6-ylamino}-benzamide
[0339]
[0340] Prepared in a similar manner to that described for Example 7 except using N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-[(E)-3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide instead of N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ) δ 12.90 (1H, s), 9.70 (1H, s), 9.03 (1H, t, J=6.0 Hz), 8.44 (1H, d, J=4.9 Hz), 8.06 (1H, d, J=9.0 Hz), 7.87 (1H, d, J=16.2 Hz), 7.70 (1H, d, J=7.5 Hz), 7.50-7.38 (4H, m), 7.22 (1H, s), 7.1 (1H, d, J=5.6 Hz), 6.99 (1H, dd, J=8.7, 1.5 Hz), 6.90 (1H, dt, J=7.9, 1.9 Hz), 5.91 (1H, s), 4.43 (2H, d, J=5.6 Hz), 3.72 (3H, s), 2.34 (3H, s), 2.05 (3H, s).
Example 42
1-Methyl-1H-benzoimidazole-2-carbaldehyde oxime
[0341]
[0342] To a stirred suspension of 1-Methyl-1H-benzoimidazole-2-carbaldehyde (980 mg, 6.61 mmol) in H 2 O (10 ml) was added a solution of Sodium Acetate (3.25 g, 39.68 mmol) and Hydroxylamine hydrochloride (1.38 g, 19.84 mmol) in 10 ml of H 2 O. The reaction was stirred at rt for 2 hr and the thick precipitate was collected by filtration, washed with water and dried under vacuum to give 1.02 g (94%) of a white solid. 1 H NMR (DMSO-d 6 ) δ 12.06 (1H, s), 8.28 (1H, s), 7.65 (1H, d, J=7.5 Hz), 7.60 (1H, d, J=6.8 Hz), 7.32 (1H, t, J=7.2 Hz), 7.23 (1H, t, J=6.8 Hz), 4.00 (3H, s).
[0343] Anal. Calcd for C 9 H 9 N 3 O: C, 61.70; H, 5.18; N, 23.99. Found: C, 61.80; H, 5.23; N, 23.98.
Example 43
C-(1-Methyl-1H-benzoimidazol-2-yl)-methylamine dihydrochloride
[0344]
[0345] A Parr pressure bottle was charged with 1-Methyl-1H-benzoimidazole-2-carbaldehyde oxime (267 mg, 1.6 mmol), 10% Palladium on Carbon (75 mg), concentrated HCl (2 drops) and EtOH (25 ml). The reaction mixture was shaken under 45 psi H 2 for 2 hr before the catalyst was removed by filtration. The filtrate was concentrated under reduced pressure and the residue was triturated with Et 2 O to give 340 mg (90%) of a white solid as the dihydrochloride salt and was used without further purification. 1 H NMR (DMSO-d 6 ): δ 8.87 (2H, broad s), 7.72 (2H, m), 7.38 (2H, m), 4.50 (2H, s), 3.89 (3H, s).
Example 44
N-(1-Methyl-1H-benzoimidazol-2-ylmethyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide
[0346]
[0347] Prepared in a similar manner to that described for Example 6 above, except using C-(1-Methyl-1H-benzoimidazol-2-yl)-methylamine hydrochloride N and 2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid. 1 H NMR (DMSO-d 6 ) δ 9.82 (1H, s), 9.20 (1H, t, J=5.3 Hz), 8.46 (1H, d, J=4.9 Hz), 8.07 (1H, d, J=8.9 Hz), 7.85 (1H, d, J=16.4 Hz), 7.74 (1H, d, J=7.3 Hz), 7.58 (1H, d, J=7.2 Hz), 7.50 (6H, m), 7.19 (4H, m), 6.92 (1H, t, J=8.1 Hz), 5.78 (1H, dd, J=2.5, 9.5 Hz), 4.79 (2H, d, J=5.5 Hz), 3.89 (1H,m), 3.83 (3H, s), 3.71 (1H, m), 2.41 (1H, m), 2.35 (3H, s), 2.00 (2H, m), 1.74 (1H, m), 1.57 (2H, m).
[0348] Anal. Calcd for C 36 H 35 N 7 O 2 .0.65 Hexanes: C, 73.31; H, 6.80; N, 15.00. Found: C, 72.92, H, 6.90; N, 14.71.
Example 45
N-(1-Methyl-1H-benzoimidazol-2-ylmethyl)-2-{3-[(E)2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide
[0349]
[0350] Prepared in a similar manner to that described for Example 7 except that N-(1-Methyl-1H-benzoimidazol-2-ylmethyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide was used instead of N-[4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ) δ 12.93 (1H, s), 9.73 (1H, s), 9.19 (1H, t, J=5.3 Hz), 8.45 (1H, d, J=4.9 Hz), 8.06 (1H, d, J=8.5 Hz), 7.88 (1H, d, J=16.4 Hz), 7.74 (1H, d, J=7.9 Hz), 7.60-7.36 (6H, m), 7.29-7.14 (3H, m), 7.10 (1H, d, J=4.7 Hz), 7.04 (1H, dd, J=1.8, 8.9 Hz), 6.91 (1H, t, J=7.3 Hz), 4.79 (2H, d, J=5.3 Hz), 3.83 (3H, s), 2.35 (3H, s).
[0351] Anal. Calcd for C 31 H 27 N 7 O.1.80H 2 O.0.40CH 2 Cl 2 : C, 65.02; H, 5.46; N, 16.91. Found C, 64.97; H, 5.82; N, 17.09.
Example 46
1-Methyl-1H-imidazole-2-carbaldehyde oxime
[0352]
[0353] Prepared in a similar manner to that described for Example 39 except that 1-Methyl-1H-imidazole-2-carbaldehyde was used instead of 1-Methyl-1H-benzoimidazole-2-carbaldehyde.
[0354] 1 H NMR (DMSO-d 6 ): δ 11.50 (1H, s), 8.05 (1H, s), 7.28 (1H, s), 6.95 (1H, s), 3.80 (3H, s),
[0355] Anal. Calcd for C 5 H 7 N 3 O: C, 47.99; H, 5.64; N, 33.58. Found: C, 48.22; H, 5.58; N, 33.45.
Example 47
C-(1-Methyl-1H-imidazol-2-yl)-methylamine dihydrochloride
[0356]
[0357] Prepared in a similar manner to that described for Example 40 except that 1-Methyl-1H-imidazole-2-carbaldehyde oxime was used instead of 1-Methyl-1H-benzoimidazole-2-carbaldehyde oxime. 1 H NMR (DMSO-d 6 ): δ 7.45 (1H, s), 7.29 (1H, s), 4.25 (21H, s), 3.79 (3H, s).
Example 48
N-(1-Methyl-1H-imidazol-2-ylmethyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide
[0358]
[0359] Prepared in a similar manner to that described for Example 6 above except using C-(1-Methyl-1H-imidazol-2-yl)-methylamine hydrochloride and 2-[3-[2-(4-Methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid. 1 H NMR (DMSO-d 6 ) δ 9.83 (1H, S 9.03 (1H, t, J=5.5 Hz), 8.45 (1H, d, J=4.7 Hz), 8.09 (1H, d, J=8.5 Hz), 7.85 (1H, d, J=16.5 Hz), 8.67 (1H, d, J=7.3 Hz), 7.53-7.39 (4H, m), 7.11 (3H, m), 6.90 (1H, d, J=6.9 Hz), 6.86 (1H, s), 5.79 (1H, d, J=8.9 Hz), 5.75 (1H, s), 4.54 (1H, d, J=5.5 Hz), 3.85-3.70 (2H, m), 3.66 (3H, s), 2.35 (3H, s), 2.10 (2H, m), 1.70 (2H, m), 1.60 (3H, m). Anal. Calcd for C 32 H 33 N 7 O 2 .0.8 CH 2 Cl 2 : C, 63.99; H, 5.672; N, 15.93. Found: C, 63.95; H, 5.72; N, 16.01.
Example 49
N-(1-Methyl-1H-imidazol-2-ylmethyl)-2-{3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-benzamide
[0360]
[0361] Prepared in a similar manner to that described for Example 7 except that N-(1-Methyl-1H-imidazol-2-ylmethyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide was used instead of N-[4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ) δ 12.89 (1H, s 9.72 (1H, s 8.99 (1H, t, J=5.6 Hz), 8.44 (1H, d, J=4.9 Hz), 8.05 (1H, d, J=8.7 Hz), 7.86 (1H, d, J=16.4 Hz), 7.66 (1H, d, J=6.7 Hz), 7.49-7.36 (4H, m), 7.24 (1H, m), 7.09 (2H, d, J=8.1 Hz), 7.02 (1H, d, J=8.8 Hz), 6.88 (1H, t, J=6.9 Hz), 6.81 (1H, s), 4.52 (2H, d, J=5.5 Hz), 3.29 (3H, s), 2.34 (3H, s). Anal. Calcd for C 27 H 25 N 7 O.0.35CH 2 Cl 2 : C, 66.59; H, 5.25; N, 19.88. Found: C, 66.48; H, 5.65; N, 19.56.
Example 50
N-(4-Hydroxy-but-2-ynyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide
[0362]
[0363] Prepared in a similar manner to that described for Example 6 except using 2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzoic acid and 4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynylamine. 1 H NMR (CDCl 3 ): δ 9.48 (H, s), 8.46 (1H, d, J=5.3 Hz), 7.92 (1H, d, J=9.0 Hz), 7.83 (1H, d, J=16.2 Hz), 7.52 (1H, d, J=16.6 Hz), 7.46-7.41 (2H, m), 7.34-7.31 (3H, m), 7.12 (1H, dd, J=8.7, 1.9 Hz), 6.99 (1H, d, J=4.9 Hz), 6.81 (1H, t, J=6.8 Hz), 6.40 (1H, t, J=4.9 Hz), 5.62 (1H, dd, J=9.4, 3.0 Hz), 4.28-4.23 (4H, m), 4.08-4.01 (1H, m), 3.76-3.67 (1H, m), 2.63-2.49 (1H, m), 2.38 (3H, s), 2.22-2.06 (2H, m), 1.80-1.60 (3H, m).
Example 51
2-{3-[(E)-2-(4-Methyl-pyridin-2-yl)-vinyl]-1H-indazol-6-ylamino}-N-(4-hydroxy-but-2-ynyl)-benzamide
[0364]
[0365] Prepared in a similar manner to that described for Example 7 except using a mixture of N-(4-Hydroxy-but-2-ynyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide and N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4-methyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide instead of N-[4-(tert-butyl-dimethyl-silanyloxy)-but-2-ynyl)-2-[3-[2-(4,6-dimethyl-pyridin-2-yl)-vinyl]-1-(tetrahydro-pyran-2-yl)-1H-indazol-6-ylamino]-benzamide. 1 H NMR (DMSO-d 6 ): δ 12.92 (1H, s), 9.83 (1H, s), 9.00 (1H, t, J=5.3 Hz), 8.44 (1H, d, J=4.9 Hz), 8.06 (1H, d, J=9.0 Hz), 7.87 (1H, d, J=16.6 Hz), 7.68 (1H, d, J=7.9 Hz), 7.50-7.38 (4H, m), 7.26 (1H, s), 7.09 (1H, d, J=5.3 Hz), 7.01 (1H, dd, J=8.7, 1.5 Hz), 6.88 (1H,dt, J=6.8, 1.5 Hz), 5.11 (1H, t, J=3.0 Hz), 4.10-4.04 (4H, m), 2.34 (3H, s).
Example 52
2-[3-(Pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid methyl ester
[0366]
[0367] Prepared in a similar manner to that described for Examples 2 and 3 above except starting with 6-Nitro-3-styryl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazole instead of 6-Iodo-3-styryl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazole.
[0368] This material was taken on as a crude mixture of product and 2-Amino-benzoic acid methyl ester in the next step.
Example 53
2-[3-(Pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid
[0369]
[0370] Isolated as a byproduct from reaction of N-[4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-(pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzamide and TBAF using a procedure similar to Example 11 in U.S. Pat. No. 6,534,524, issued Mar. 18, 2003, hereby incorporated in its entirety for all purposes. 1 H NMR (DMSO-d 6 ) δ 13.19 (1H, broad s 10.00 (1H, s, 9.13 (1H, s), 8.37 (1H, d, J=8.7 Hz), 8.06 (1H, d, J=7.5 Hz), 7.75 (1H, s), 7.64 (2H, t, J=2.3 Hz), 7.54 (2H, m), 7.35 (1H, dd, J=1.9. 8.7 Hz), 6.99 (1H, m), 6.33 (2H, t, J=2.3 Hz), 5.89 (2H, s), 3.68 (2H, t, J=8.1 Hz), 0.94 (2H, t, J=8.1 Hz), 0.00 (9H, s).
Example 54
N-(3-Cyclopropyl-prop-2-ynyl)-2-[3-(pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzamide
[0371]
[0372] Prepared in a similar manner to that described for Example 6 above, except using 2-[3-(Pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid and 3-Cyclopropyl-prop-2-ynylamine. ‘ H NMR (DMSO-d 6 ) δ 9.93 (1H, s 8.99 (1H,s), 8.95 (1H, d, J=5.6 Hz), 8.20 (1H, d, J=8.9 Hz), 7.68 (1H, d, J=8.1 Hz), 7.51 (4H, m), 7.37 (1H, t, J=6.8 Hz), 7.14 (1H, d, J=9.0 Hz), 6.91 (1H, t, J=7.5 Hz), 6.21 (2H, t, J=2.3 Hz), 5.74 (2H, s), 4.00 (2H, dd, J=2.0, 5.6 Hz), 3.55 (2H, t, J=7.9 Hz), 1.26 (1H, m), 0.82 (2H, t, J=7.9 Hz), 0.72 (2H, m) 0.54 (2H, m), −0.12 (9H, s).
Example 55
N-(3-Cyclopropyl-prop-2-ynyl)-2-[3-(pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzamide
[0373]
[0374] Prepared in a similar manner to that described for Example 11 in U.S. Pat. No. 6,534,524, issued Mar. 18, 2003, herein incorporated by reference in its entirety for all purposes, except that N-(3-Cyclopropyl-prop-2-ynyl)-2-[3-(pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzamide was used instead of N-methyl-N-{3-styryl-1-[2-trimethyl-silanyl)-ethoxymethyl]-1H-indazol-6-yl}-benzene-1,3-diamine.
[0375] 1 H NMR (DMSO-d 6 ) δ 13.29 (1H, s), 9.83 (1H, s 8.98 (1H, s), 8.95 (1H, t, J=5.5 Hz), 8.19 (1H, d, J=8.9 Hz), 7.68 (1H, d, J=7.5 Hz), 7.52 (2H, t, J=2.3 Hz), 7.43 (2H, m), 7.29 (1H, s), 7.07 (1H, dd, J=1.9, 8.7 Hz), 6.91 (1H, t, J=7.4 Hz), 6.21 (2H, t, J=2.3 Hz), 4.01 (2H, dd, J=1.7, 5.5 Hz), 1.27 (1H, m), 0.73 (2H, m), 0.55 (2H, m). Anal. Calcd for C 25 H 22 N 6 O.0.05Hexanes.0.30 H 2 O: C, 70.31; H, 5.43; N, 19.45. Found: C, 70.63; H, 5.38; N, 19.18.
Example 56
N-[4-tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzamide
[0376]
[0377] Prepared in a similar manner to that described for Example 6 above except using 2-[3-(Pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid and 4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynylamine. 1 H NMR (DMSO-d 6 ) δ 10.04 (1H, s 9.16 (1H, t, J=5.3 Hz), 9.10 (1H,s), 8.31 (1H, d, J=8.7 Hz), 7.78 (1H, d, J=7.9 Hz), 7.67 (4H, m), 7.49 (1H, t, J=8.5 Hz), 7.24 (1H, dd, J=1.7, 8.7 Hz), 7.03 (1H, t, J=7.4 Hz), 6.33 (2H, t, J=2.3 Hz), 5.85 (2H, s), 4.83 (2H, s), 4.19 (2H, d, J=5.5 Hz), 3.66 (2H, t, J=7.9 Hz), 0.94 (2H, m), 0.89 (9H, s), 0.13 (6H, s), 0.00 (9H, s).
Example 57
N-(4-Hydroxy-but-2-ynyl)-2-[3-(pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzamide
[0378]
[0379] Prepared in a similar manner to that described for Example 11, in U.S. Pat. No. 6,534,524, issued Mar. 18, 2003, herein incorporated by reference in its entirety for all purposes, except that N-[4-(tert-Butyl-dimethyl-silanyloxy)-but-2-ynyl]-2-[3-(pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzamide was used instead of N-methyl-N-{3-styryl-1-[2-trimethyl-silanyl)-ethoxymethyl]-1H-indazol-6-yl}-benzene-1,3-diamine. 1 H NMR (DMSO-d 6 ) δ 13.30 (1H, s), 9.87 (1H, s 9.04 (1H, t, J=5.3 Hz), 8.99 (1H, s), 8.19 (1H, d, J=8.5 Hz), 7.70 (1H, d, J=7.3 Hz), 7.46 (4H, m), 7.31 (1H, s), 7.08 (1H, dd, J=1.7, 8.7 Hz), 6.91 (1H, t, J=7.3 Hz), 6.21 (2H, t, J=2.1 Hz), 5.14 (1H, t, J=5.8 Hz), 4.10 (2H, d, J=5.5 Hz), 4.06 (2H, d, J=5.8 Hz). Anal. Calcd for C 23 H 20 N 6 O 2 .0.35Hexanes.0.20 H 2 O: C, 67.45; H, 5.86; N, 18.81. Found: C, 67.70; H, 5.73; N, 18.56.
Example 58
2,5-Dimethyl-2H-pyrazole-3-carbonitrile
[0380]
[0381] 2,5-Dimethyl-2H-pyrazole-3-carbonitrile was prepared from ethyl 1,3-dimethylpyrazole-5-carboxlate according to procedures published for 1-methyl-pyrazol-5-carbonitrile by Castellanos, Maria and Montserrat, Llinas; JCS Perkins Trans I (1985) 1209-1215. 1 H NMR (CDCl 3 ) δ 6.52 (1H, s), 3.96 (3H, s), 2.27 (3H, s).
Example 59
C-(2,5-Dimethyl-2H-pyrazol-3-yl)-methylamine
[0382]
[0383] A suspension of 2,5-Dimethyl-2H-pyrazole-3-carbonitrile (654 mg, 5.4 mmol) and 10% palladium on carbon (200 mg) in ethanol (15 mL) was shaken in a Parr hydrogenation apparatus under 45 psi H 2 for 17 hr. The mixture was filtered through celite and the filtrate was concentrated under reduced pressure to give 608 mg of an oil which was used without any further purification. 1 H NMR (CDCl 3 ) δ 5.91 (1H, s), 3.81, 3.73 (2H,2s), 3.75 (3H, s), 2.21 (3H, s),
Example 60
N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-[3-(pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzamide
[0384]
[0385] Prepared in a similar manner to that described for Example 6 above except using 2-[3-(Pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid and C-(2,5-Dimethyl-2H-pyrazol-3-yl)-methylamine. 1 H NMR (CDCl 3 ) δ 9.56 (1H, s), 8.68 (1H, s), 8.30 (1H, d, J=8.7 Hz), 7.49 (1H, d, J=8.3 Hz), 7.43 (1H, dd, J=7.9, 1.5 Hz), 7.36-7.31 (2H, m), 7.23 (2H, t, J=2.6 Hz), 7.17 (1H, dd, J=8.7, 1.9 Hz), 6.83 (1H, t, J=7.2 Hz), 6.32 (1H, bt), 6.29 (2H, t, J=2.3 Hz), 6.01 (1H, s), 5.67 (2H, s), 4.61 (2H, d, J=5.6 Hz), 3.60 (3H, s), 3.58 (2H, t, J=8.3 Hz), 2.22 (3H, s), 0.90 (2H, t, J=8.7 Hz), 0.06 (9H, s).
Example 61
N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-[3-(pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzamide
[0386]
[0387] Prepared in a similar manner to that described for Example 11 in U.S. Pat. No. 6,534,524, issued Mar. 18, 2003, herein incorporated by reference in its entirety for all purposes, except that N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-[3-(pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzamide was used instead of N-methyl-N-{3-styryl-1-[2-trimethyl-silanyl)-ethoxymethyl]-1H-indazol-6-yl}-benzene-1,3-diamine.
[0388] 1 H NMR (DMSO-d 6 ) δ 13.27 (1H, s), 9.72 (1H, s), 9.05 (1H, t, J=5.3 Hz), 8.97 (1H, s), 8.16 (1H, d, J=8.7 Hz), 7.68 (1H, dd, J=8.3, 1.9 Hz), 7.50 (2H, t, J=2.6 Hz), 7.46-7.38 (2H, m), 7.25 (1H, s), 7.05 (1H, dd, J=8.7, 1.9 Hz), 6.91 (1H, t, J=6.80 Hz), 6.20 (2H, t, J=2.3 Hz), 5.91 (1H, s), 4.43 (2H, d, J=5.6 Hz), 3.71 (3H, s), 2.04 (3H, s).
Example 62
2-[3-(Pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzoic acid
[0389]
[0390] Prepared in a similar manner to that described for Example 11 in U.S. Pat. No. 6,534,524, issued Mar. 18, 2003, herein incorporated by reference in its entirety for all purposes, except using 2-[3-(Pyrrol-1-yliminomethyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-6-ylamino]-benzoic acid instead of N-methyl-N-{3-styryl-1-[2-trimethyl-silanyl)-ethoxymethyl]-1H-indazol-6-yl}-benzene-1,3-diamine. 1 H NMR (DMSO-d 6 ) δ 13.12 (1H, s), 12.70 (1H, s), 8.94 (1H, s), 8.10 (1H, d, J=8.7 Hz), 7.91 (1H, dd, J=1.7, 7.7 Hz), 7.50 (2H, t, J=2.3 Hz), 7.36 (1H, d, J=7.9 Hz), 7.27 (1H, d, J=1.5 Hz), 7.16 (1H, t, J=7.5 Hz), 6.94 (1H, dd, J=1.7, 8.7 Hz), 6.68 (1H, t, J=7.5 Hz), 6.19 (2H, t, J=2.3 Hz).
Example 63
N-Prop-2-ynyl-2-[3-(pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzamide
[0391]
[0392] Prepared in a similar manner to that described for Example 6 above, except using 2-[3-(Pyrrol-1-yliminomethyl)-1H-indazol-6-ylamino]-benzoic acid and propargylamine. 1 H NMR (DMSO-d 6 ) δ 13.30 (1H, s), 9.82 (1H, s), 9.04 (1H, t, J=5.6 Hz), 8.98 (1H, s) 8.19 (1H, d, J=8.6 Hz), 7.69 (1H, d, J=7.9 Hz), 7.45 (4H, m), 7.31 (1H, s), 7.08 (1H, d, J=8.6 Hz), 6.91 (1H, t, J=7.6 Hz), 6.21 (2H, s), 4.05 (2H, s), 3.13 (1H, s). Anal. Calcd for C 22 H 18 N 6 O.0.40H 2 O.0.05 Hexanes: C, 67.97; H, 5.01; N, 21.33. Found: C, 67.91; H, 4.78; N, 21.00.
Example 64
N-(4-Hydroxy-but-2-ynyl)-2-[3-(2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0393]
[0394] Prepared in a similar manner to that described for Example 6 above, except using tetrabutyl ammonium 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoate and 4-Amino-but-2-yn-1-ol. 1 H NMR (DMSO-d 6 ): δ 12.95 (1H, s), 9.84 (1H, s), 9.02 (1H, t, J=5.6 Hz), 8.59 (1H, d, J=4.9 Hz), 8.08 (1H, d, J=8.7 Hz), 7.90 (1H, d, J=16.2 Hz), 7.80 (1H, t, J=7.2 Hz), 7.70-7.64 (2H, m), 7.51 (1H, d, J=16.2 Hz), 7.45-7.36 (2H, m), 7.27-7.24 (2H, m), 7.02 (1H, d, J=9.0 Hz), 6.88 (1H, t, J=7.2 Hz), 5.13 (1H, t, J=5.6 Hz), 4.10-4.04 (4H, m).
Example 65
N-(2,5-Dimethyl-2H-pyrazol-3-ylmethyl)-2-[3-(2-pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzamide
[0395]
[0396] Prepared in a similar manner to that described for Example 6 above, except using tetrabutyl ammonimum 2-[3-(2-Pyridin-2-yl-vinyl)-1H-indazol-6-ylamino]-benzoate and C-(2,5-Dimethyl-2H-pyrazol-3-yl)-methylamine. 1 H NMR (DMSO-d 6 ) δ 12.93 (1H, s), 9.70 (1H, s), 9.04 (1H,bt), 8.58 (1H, d, J=4.0 Hz), 8.07 (1H, d, J=8.8 Hz), 7.88 (1H, d, J=16.4 Hz), 7.79 (1H, t, J=8.6 Hz), 7.71-7.64 (2H, m), 7.50 (1H, d, J=16.4 Hz), 7.44-7.39 (2H, m), 7.28-7.23 (2H, m), 7.00 (1H, d, J=8.8 Hz), 6.90 (1H, t, J=8.0 Hz), 5.91 (1H, s), 4.43 (2H, d, J=5.5 Hz), 3.71 (3H, s), 2.04 (3H, s).
[0397] The exemplary compounds described above may be tested for their activity using the tests described below.
[0000] Biological Testing; Ensyme Assays
[0398] The stimulation of cell proliferation by growth factors such as VEFG, FGF, and others is dependent upon their induction of autophosphorylation of each of their respective receptor's tyrosine kinases. Therefore, the ability of a protein kinase inhibitor to block autophosphorylation can be measured by inhibition of the peptide substrates. To measure the protein kinase inhibition activity of the compounds, the following constructs were devised.
[0399] VEGF-R2 Construct for Assay: This construct determines the ability of a test compound to inhibit tyrosine kinase activity. A construct (VEGF-R2Δ50) of the cytosolic domain of human vascular endothelial growth factor receptor 2 (VEGF-R2) lacking the 50 central residues of the 68 residues of the kinase insert domain was expressed in a baculovirus/insect cell system. Of the 1356 residues of full-length VEGF-R2, VEGF-R2Δ50 contains residues 806-939 and 990-1171, and also one point mutation (E990V) within the kinase insert domain relative to wild-type VEGF-R2. Autophosphorylation of the purified construct was performed by incubation of the enzyme at a concentration of 4 μM in the presence of 3 mM ATP and 40 mM MgCl 2 in 100 mM HEPES, pH 7.5, containing 5% glycerol and 5 mM DTT, at 4° C. for 2 h. After autophosphorylation, this construct has been shown to possess catalytic activity essentially equivalent to the wild-type autophosphorylated kinase domain construct. See Parast et al., Biochemistry, 37, 16788-16801 (1998).
[0400] FGF-R1 Construct for Assay: The intracellular kinase domain of human FGF-R1 was expressed using the baculovirus vector expression system starting from the endogenous methionine residue 456 to glutamate 766, according to the residue numbering system of Mohammadi et al., Mol. Cell. Biol., 16, 977-989 (1996). In addition, the construct also has the following 3 amino acid substitutions: L457V, C488A, and C584S.
[0401] LCK Construct for Assay: The LCK tyrosine kinase was expressed in insect cells as an N-terminal deletion starting from amino acid residue 223 to the end of the protein at residue 509, with the following two amino acid substitutions at the N-terminus: P233M and C224D.
[0000] VEGF-R2 Assay
[0402] Coupled Spectrophotometric (FLVK-P) Assay
[0403] The production of ADP from ATP that accompanies phosphoryl transfer was coupled to oxidation of NADH using phosphoenolpyruvate (PEP) and a system having pyruvate kinase (PK) and lactic dehydrogenase (LDH). The oxidation of NADH was monitored by following the decrease of absorbance at 340 nm (e 340 =6.22 cm −1 mM −1 ) using a Beckman DU 650 spectrophotometer. Assay conditions for phosphorylated VEGF-R2Δ50 (indicated as FLVK-P in the tables below) were the following: 1 mM PEP; 250 μM NADH; 50 units of LDH/mL; 20 units of PK/mL; 5 mM DTT; 5.1 mM poly(E 4 Y 1 ); 1 mM ATP; and 25 mM MgCl 2 in 200 mM HEPES, pH 7.5. Assay conditions for unphosphorylated VEGF-R2Δ50 (indicated as FLVK in the tables) were the following: 1 mM PEP; 250 μM NADH; 50 units of LDH/mL; 20 units of PK/mL; 5 mM DTT; 20 mM poly(E 4 Y 1 ); 3 mM ATP; and 60 mM MgCl 2 and 2 mM MnCl 2 in 200 mM HEPES, pH 7.5. Assays were initiated with 5 to 40 nM of enzyme. K i values were determined by measuring enzyme activity in the presence of varying concentrations of test compounds. The data were analyzed using Enzyme Kinetic and Kaleidagraph software.
[0000] ELISA Assay
[0404] Formation of phosphogastrin was monitored using biotinylated gastrin peptide (1-17) as substrate. Biotinylated phosphogastrin was immobilized using streptavidin coated 96-well microtiter plates followed by detection using anti-phosphotyrosine-antibody conjugated to horseradish peroxidase. The activity of horseradish peroxidase was monitored using 2,2′-azino-di-[3-ethylbenzathiazoline sulfonate(6)] diammonium salt (ABTS). Typical assay solutions contained: 2 μM biotinylated gastrin peptide; 5 mM DTT; 20 μM ATP; 26 mM MgCl 2 ; and 2 mM MnCl 2 in 200 mM HEPES, pH 7.5. The assay was initiated with 0.8 nM of phosphorylated VEGF-R2Δ50. Horseradish peroxidase activity was assayed using ABTS, 10 mM. The horseradish peroxidase reaction was quenched by addition of acid (H 2 SO 4 ), followed by absorbance reading at 405 nm. K i values were determined by measuring enzyme activity in the presence of varying concentrations of test compounds. The data were analyzed using Enzyme Kinetic and Kaleidagraph software.
[0000] Fibroblast Growth Factor (FGF-R) Assay
[0405] The spectrophotometric assay was carried out as described above for VEGF-R2, except for the following changes in concentration: FGF-R=50 nM, ATP=2 mM, and poly(E4Y1)=15 mM.
[0000] Lymphocyte-Specific Protein-Tyrosine Kinase (LCK) Assay
[0406] The spectrophotometric assay was carried out as described above for VEGF-R2, except for the following changes in concentration: LCK=60 nM, MgCl 2 =0 mM, poly(E4Y1)=20 mM.
[0000] Focal Adhesion Kinase (FAK) Assay
[0407] FAK High Throughput Screening (HTS) utilizes the fluorescence polarization assay provided by LJL Biosystems. The kinase reaction contained: 100 mM Hepes pH 7.5, 10 mM MgCl 2 , 1 mM DTT, 1 mM ATP, and 1 mg/ml poly Glu-Tyr (4:1). The reaction is initiated by the addition of 5 nM FAKcd409. The reaction is terminated by the addition of EDTA followed by addition of fluor-labelled peptide and anti-phosphotyrosine antibody, both provided by LJL Biosystems. Inhibition results are read on a Analyst (LJL) detector.
[0000] TIE-2 Spectrophotometric Assay
[0408] The kinase-catalyzed production of ADP from ATP that accompanies phosphoryl transfer to the random copolymer poly(Glu 4 Tyr) was coupled to the oxidation of NADH through the activities of pyruvate kinase (PK) and lactate dehydrogenase (LDH). NADH conversion to NAD + was monitored by the decrease in absorbance at 340 nm (ε=6.22 cm −1 mM −1 ) using a Beckman DU650 spectrophotometer. Typical reaction solutions contained 1 mM phosphoenolpyruvate, 0.24 mM NADH, 40 mM MgCl 2 , 5 mM DTT, 2.9 mg/mL poly(Glu 4 Tyr), 0.5 mM ATP, 15 units/mL PK, 15 units/mL LDH in 100 mM HEPES, pH 7.5. Assays were initiated with the addition of 4 to 12 nM phosphorylated Tie-2 (aa 775-1122). Percent inhibition was determined in triplicate at a 1 μM level of inhibitor.
[0000] TIE-2 DELFIA Assay
[0409] Formation of phosphotyrosine was monitored using biotinylated p34cdc2 (aa6-20=KVEKIGEGTYGWYK) peptide as substrate. Biotinylated peptide was immobilized using NeutrAvidin™ coated 96-well microtiter plates followed by detection using anti-phosphotyrosine-antibody (PY20) conjugated to europium N1 chelate. Typical assay solutions contained: 1 μM biotinylated p34cdc2 peptide, 150 μM ATP, 5 mM MgCl 2 , 1 mM DTT, 0.01% BSA, 5% glycerol, 2% DMSO, 25 mM HEPES pH 7.5. The assay was initiated in the NeutrAvidin plate with 50 nM of TIE2 intracellular domain. The kinase reaction was terminated with 50 mM EDTA. Plates were then washed, and europium antibody added. After incubation, they were again washed, and DELFIA™ Enhancement Solution added. Plates were read at standard Europium time-resolved settings (ex 340 nm, em 615 nm, delay 400 μsec, window 400 μsec). Percent inhibition was calculated with reference to intraplate wells which had added DMSO rather than compound in DMSO, with background subtracted from both experimental and control with reference to an intraplate well which had EDTA added prior to addition of enzyme.
[0000] HUVEC Proliferation Assay
[0410] This assay determines the ability of a test compound to inhibit the growth factor-stimulated proliferation of human umbilical vein endothelial cells (“HUVEC”). HUVEC cells (passage 3-4, Clonetics, Corp.) were thawed into EGM2 culture medium (Clonetics Corp) in T75 flasks. Fresh EGM2 medium was added to the flasks 24 hours later. Four or five days later, cells were exposed to another culture medium (F12K medium supplemented with 10% fetal bovine serum (FBS), 60 μg/mL endothelial cell growth supplement (ECGS), and 0.1 mg/mL heparin). Exponentially-growing HUVEC cells were used in experiments thereafter. Ten to twelve thousand HUVEC cells were plated in 96-well dishes in 100 μl of rich, culture medium (described above). The cells were allowed to attach for 24 hours in this medium. The medium was then removed by aspiration and 105 μl of starvation media (F12K+1% FBS) was added to each well. After 24 hours, 15 μl of test agent dissolved in 1% DMSO in starvation medium or this vehicle alone was added into each treatment well; the final DMSO concentration was 0.1%. One hour later, 30 μl of VEGF (30 ng/mL) in starvation media was added to all wells except those containing untreated controls; the final VEGF concentration was 6 ng/mL. Cellular proliferation was quantified 72 hours later by MTT dye reduction, at which time cells were exposed for 4 hours MTT (Promega Corp.). Dye reduction was stopped by addition of a stop solution (Promega Corp.) and absorbance at 595 λ was determined on a 96-well spectrophotometer plate reader.
[0411] IC 50 values were calculated by curve-fitting the response of A 595 to various concentrations of the test agent; typically, seven concentrations separated by 0.5 log were employed, with triplicate wells at each concentration. For screening compound library plates, one or two concentrations (one well per concentration) were employed, and the % inhibition was calculated by the following formula:
% inhibition=(control−test)+(control−starvation)
where
[0412] control=A 595 when VEGF is present without test agent
[0413] test=A 595 when VEGF is present with test agent
[0414] starvation=A 595 when VEGF and test agent are both absent.
[0000] Mouse PK Assay
[0415] The pharmacokinetics (e.g., absorption and elimination) of drugs in mice were analyzed using the following experiment. Test compounds were formulated as a solution or suspension in a 30:70 (PEG 400: acidified H 2 O) vehicle or as a suspension in 0.5% CMC. This was administered orally (p.o.) and intraperitoneally (i.p.) at variable doses to two distinct groups (n=4) of B6 female mice. Blood samples were collected via an orbital bleed at time points: 0 hour (pre-dose), 0.5 h, 1.0 h, 2.0 h, and 4.0 h, and 7.0 h post dose. Plasma was obtained from each sample by centrifugation at 2500 rpm for 5 min. Test compound was extracted from the plasma by an organic protein precipitation method. For each time bleed 50 μL of plasma was combined with 1.0 mL of acetonitrile, vortexed for 2 min. and then spun at 4000 rpm for 15 min. to precipitate the protein and extract out the test compound. Next, the acetonitrile supernatant (the extract containing test compound) was poured into new test tubes and evaporated on a hot plate (25° C.) under a steam of N 2 gas. To each tube containing the dried test compound extract 125 μL of mobile phase (60:40, 0.025 M NH 4 H 2 PO 4 +2.5 mL/L TEA:acetonitrile) was added. The test compound was resuspended in the mobile phase by vortexing and more protein was removed by centrifugation at 4000 rpm for 5 min. Each sample was poured into an HPLC vial for test compound analysis on an Hewlett Packard 1100 series HPLC with UV detection. From each sample, 95 μL was injected onto a Phenomenex-Prodigy reverse phase C-18, 150×3.2 mm column and eluted with a 45-50% acetonitrile gradient run over 10 min. Test-compound plasma concentrations (μg/mL) were determined by a comparison to standard curve (peak area vs. conc. μg/mL) using known concentrations of test compound extracted from plasma samples in the manner described above. Along with the standards and unknowns, three groups (n=4) of quality controls (0.25 μg/mL, 1.5 μg/mL, and 7.5 μg/mL) were run to insure the consistency of the analysis. The standard curve had an R2>0.99 and the quality controls were all within 10% of their expected values. The quantitated test samples were plotted for visual display using Kalidagraph software and their pharmacokinetic parameters were determined using WIN NONLIN software. Example 1(a) provided the following results: 0.69 (Mouse pK, AUC, ip, μg-h/ml); 0.33 (Mouse pK, AUC, po, μg-h/ml).
[0000] KDR (VEGFR2) Phosphorvlation in PAE-KDR Cells Assay
[0416] This assay determines the ability of a test compound to inhibit the autophosphorylation of KDR in porcine aorta endothelial (PAE)-KDR cells. PAE cells that overexpress human KDR were used in this assay. The cells were cultured in Ham's F12 media supplemented with 10% fetal bovine serum (FBS) and 400 ug/mL G418. Thirty thousands cells were seeded into each well of a 96-well plate in 75 μL of growth media and allowed to attach for 6 hours at 37° C. Cells were then exposed to the starvation media (Ham's F12 media supplemented with 0.1% FBS) for 16 hours. After the starvation period was over, 10 μL of test agent in 5% DMSO in starvation media were added to the test wells and 10 μL of the vehicle (5% DMSO in starvation media) were added into the control wells. The final DMSO concentration in each well was 0.5%. Plates were incubated at 37 μC for 1 hour and the cells were then stimulated with 500 ng/ml VEGF (commercially available from R & D System) in the presence of 2 mM Na 3 VO 4 for 8 minutes. The cells were washed once with 1 mm Na 3 VO 4 in HBSS and lysed by adding 50 μL per well of lysis buffer. One hundred μL of dilution buffer were then added to each well and the diluted cell lysate was transferred to a 96-well goat ant-rabbit coated plate (commercially available from Pierce) which was pre-coated with Rabbit anti Human Anti-flk-1 C-20 antibody (commercially available from Santa Cruz). The plates were incubated at room temperature for 2 hours and washed seven times with 1% Tween 20 in PBS. HRP-PY20 (commercially available from Santa Cruz) was diluted and added to the plate for a 30-minute incubation. Plates were then washed again and TMB peroxidase substrate (commercially available from Kirkegaard & Perry) was added for a 10-minute incubation. One hundred μL of 0.09 N H 2 SO 4 was added to each well of the 96-well plates to stop the reaction. Phosphorylation status was assessed by spectrophotometer reading at 450 nm. IC 50 values were calculated by curve fitting using a four-parameter analysis.
[0000] PAE-PDGFRβ Phosphorylation in PAE-PDGFR Cells Assay
[0417] This assay determines the ability of a test compound to inhibit the autophosphorylation of PDGFRβ in porcine aorta endothelial (PAE)-PDGFRβ cells. PAE cells that overexpress human PDGFRβ were used in this assay. The cells were cultured in Ham's F12 media supplemented with 10% fetal bovine serum (FBS) and 400 ug/ml G418. Twenty thousands cells were seeded in each well of a 96-well plate in 50 μL of growth media and allowed to attach for 6 hours at 37° C. Cells were then exposed to the starvation media (Ham's F12 media supplemented with 0.1% FBS) for 16 hours. After the starvation period was over, 10 μL of test agent in 5% DMSO in starvation media were added to the test wells and 10 μL of the vehicle (5% DMSO in starvation media) were added into the control wells. The final DMSO concentration in each well was 0.5%. Plates were incubated at 37° C. for 1 hour and the cells were then stimulated with 1 μg/mL PDGF-BB (R & D System) in the presence of 2 mM Na 3 VO 4 for 8 minutes. The cells were washed once with 1 mm Na 3 VO 4 in HBSS and lysed by adding 50 μL per well of lysis buffer. One hundred μL of dilution buffer were then added to each well and the diluted cell lysate was transferred to a 96-well goat ant-rabbit coated plate (Pierce), which was pre-coated with Rabbit anti Human PDGFRβ antibody (Santa Cruz). The plates were incubated at room temperature for 2 hours and washed seven times with 1% Tween 20 in PBS. HRP-PY20 (Santa Cruz) was diluted and added to the plate for a 30-minute incubation. Plates were then washed again and TMB peroxidase substrate (Kirkegaard & Perry) was added for a 10-minute incubation. One hundred μL of 0.09 N H 2 SO 4 was added into each well of the 96-well plate to stop the reaction. Phosphorylation status was assessed by spectrophotometer reading at 450 nm. IC 50 values were calculated by curve fitting using a four-parameter analysis.
[0000] Human Liver Microsome (HLM) Assay
[0418] Compound metabolism in human liver microsomes was measured by LC-MS analytical assay procedures as follows. First, human liver microsomes (HLM) were thawed and diluted to 5 mg/mL with cold 100 mM potassium phosphate (KPO4) buffer. Appropriate amounts of KPO4 buffer, NADPH-regenerating solution (containing B-NADP, glucose-6-phosphate, glucose-6-phosphate dehydrogenase, and MgCl 2 ), and HLM were preincubated in 13×100 mm glass tubes at 37 C for 10 min. (3 tubes per test compound-triplicate). Test compound (5 □M final) was added to each tube to initiate reaction and was mixed by gentle vortexing, followed by incubation at 37° C. At t=0, 2 h, a 250-μL sample was removed from each incubation tube to separate 12×75 mm glass tubes containing 1 mL ice-cold acetonitrile with 0.05 μM reserpine. Samples were centrifuged at 4000 rpm for 20 min. to precipitate proteins and salt (Beckman Allegra 6KR, S/N ALK98D06, #634). Supernatant was transferred to new 12×75 mm glass tubes and evaporated by Speed-Vac centrifugal vacuum evaporator. Samples were reconstituted in 200 μL 0.1% formic acid/acetonitrile (90/10) and vortexed vigorously to dissolve. The samples were then transferred to separate polypropylene microcentrifuge tubes and centrifuged at 14000×g for 10 min. (Fisher Micro 14, S/N M0017580). For each replicate (#1-3) at each timepoint (0 and 2 h), an aliquot sample of each test compound was combined into a single HPLC vial insert (6 total samples) for LC-MS analysis, which is described below.
[0419] The combined compound samples were injected into the LC-MS system, composed of a Hewlett-Packard HP1100 diode array HPLC and a Micromass Quattro II triple quadruple mass spectrometer operating in positive electrospray SIR mode (programmed to scan specifically for the molecular ion of each test compound. Each test compound peak was integrated at each timepoint. For each compound, peak area at each timepoint (n=3) was averaged, and this mean peak area at 2 h was divided by the average peak area at time 0 hour to obtain the percent test compound remaining at 2 h.
[0420] The results of the testing of the compounds using various assays are summarized in the table below, where a notation of “% @” indicates the percent inhibition at the stated concentration, “*” values represent Ki (nM) or % inhibition at a compound concentration of 1 μM for * or 50 nM for **, unless otherwise indicated. “NT” indicates no significant inhibition or not tested.
TABLE 1 FLVK Ki % LckP* FGF-P HUVEC + % PAE PDGFR PAE KDR bFGFHuvec Example inh @ 50 % inhibit % inhibit HUVEC albumin remaining autophos IC50 nM IC50 # nM FLVK-P** @1 μM @1 μM IC50 (nM) IC50 (nM) (HLM) IC50 (nM) AVG (nM)AVG 3(a) 98 NT 30 99 12.7 NT NT NT NT NT 3(b) 98 NT 27 96 5.7 NT 84@2 h NT NT NT 3(c) 91 NT 9 83 0.43 9.2 46@0.5 h NT NT NT 3(d) 89 NT 11 80 0.4 7.5 68@2 h 3.5 NT 147 3(f) 95 NT 41 60 NT >100 NT NT NT NT 3(g) 95 NT 28 72 1.1 NT 72@0.5 h NT NT NT 3(h) 96 NT 37 85 1.6 NT 75@0.5 h 0.63 NT NT 3(i) 88 NT 22 45 0.2 NT NT 1.9 NT 1000 3(j) 80 NT 17 43 1.7 NT 65@0.5 h 4.7 NT NT 3(k) 74 NT 19 36 0.8 NT 75@0.5 h 5 NT 1000 3(q) 47 NT 7 31 5 NT 82@0.5 h 5.2 NT NT 2(h) 84 NT NT 75 1.6 NT 74@0.5 h 2.8 NT 70 1(k) 27 NT NT 12 >10 NT NT NT NT NT 2(g) 83 NT NT 79 0.71 NT 85@0.5 h 10.5 NT 173 64 94 NT NT 39 0.15 NT 66@0.5 h 5.5 NT 1250 65 3.11 nM NT NT NT 3.4 NT 86@0.5 h 5.8 NT NT 61 65 NT NT 14 6.5 NT NT NT NT 662 41 45 NT NT 11 6.4 NT NT NT NT 3775 51 82 NT NT 52 NT NT NT NT NT NT 15 64 NT NT 29 1.5 NT NT 12.3 NT 1613 36 95 0.3 nM NT 69 1.67 NT NT NT 1.62 935 13 80 NT NT 63 NT NT NT 6 NT NT 18 94 NT NT 59% NT NT NT NT NT 1882 20 91 NT NT 35% 0.084 NT NT NT NT NT 37 90 NT NT 45 NT NT NT NT 0.76 NT 38 75 NT NT NT NT 0.68 NT 2 NT NT 39 96 NT NT 76% NT NT NT 4.7 NT NT 32 78 NT NT 70% 0.61 NT 97@0.5 h 0.5 NT NT 55 97 NT NT 67% 0.2 NT NT 3.7 NT NT 57 91 NT NT 52% <1.8 NT NT 1.3 NT NT 63 85 NT NT 63% 0.1 NT NT 2.4 NT NT 34 72 NT NT NT NT NT NT 4.5 NT NT 10 76 6.07 NT 38, 197 nM 0.67 NT 80@0.5 h 21 NT NT 45 28 NT NT 24 NT NT NT NT NT NT 49 11 NT NT 36 NT NT NT NT NT NT 23 23 NT NT 56 NT NT NT 40 NT NT 25 64 NT NT 13 3 NT NT NT NT NT
In Vivo Assay of Retinal Vascular Development in Neonatal Rats
[0421] The development of the retinal vascular in rats occurs from postnatal day 1 to postnatal day 14 (P1-P14). This process is dependent on the activity of VEGF (J. Stone, et al, J. Neurosci., 15, 4738 (1995)). Previous work has demonstrated that VEGF also acts as a survival factor for the vessels of the retina during early vascular development (Alon, et. al, Nat. Med., 1, 1024 (1995)). To assess the ability of specific compounds to inhibit the activity of VEGF in vivo, compounds were formulated in an appropriate vehicle, usually 50% polyethylene glycol, average molecular weight 400 daltons, and 50% solution of 300 mM sucrose in deionized water. Typically, two microliters (2 μl) of the drug solution was injected into the midvitreous of the eye of rat pups on postnatal day 8 or 9. Six days after the intravitreal injection, the animals were sacrificed and the retinas dissected free from the remaining ocular tissue. The isolated retinas were then subjected to a histochemical staining protocol that stains endothelial cells specifically (Lutty and McLeod, Arch. Ophthalmol., 110, 267 (1992)), revealing the extent of vascularization within the tissue sample. The individual retinas are then flat-mount onto glass slides and examined to determine the extent of vascularization. Effective compounds inhibit the further development of the retinal vasculature and induce a regression of all but the largest vessels within the retina. The amount of vessel regression was used to assess the relative potency of the compounds after in vivo administration. Vessel regression is graded on subjective scale of one to three pluses, with one plus being detectable regression judged to be approximately 25 percent or less, two pluses being judged to be approximately 25-75% regression and three pluses give to retinas with near total regression (approximately 75% or greater).
[0422] For more quantitative analysis of regression, images of ADPase-stained, flat-mounted retinas were captured with a digital camera attached to a dissecting microscope. Retinal images were then imported into an image analysis software (Image Pro Plus 4.0, Media Cybernetics, Silver Spring, Md.). The software was employed to determine the percentage of the area of the retina that contained stained vessels. This value for the experimental eye was compared to that measured for the vehicle injected, contralateral eye from the same animal. The reduction in the vascular area seen in the eye that received compound as compared to the vehicle-injected eye was then expressed as the “percent regression” for that sample. Percent regression values were averaged for groups of 5-8 animals.
[0423] In samples in which observation through the microscope indicated near total regression, a percent regression value of 65-70% was routinely measured. This was due to stain deposits within folds of retina, folds that were induced by the vehicle used for drug injection. The image analysis software interpreted these stain-containing folds as vessels. No attempt was made to correct for these folds since they varied from eye to eye. Thus, it should be noted that the percent regression values reported result from a conservative measurement that accurately rank orders compounds, but underestimates their absolute potency.
[0000] In Vivo Assay of Retinal Vascular Development in Neonatal Rat Model of Retinopathy of Prematurity
[0424] A second model of VEGF dependent retinal neovascularization was employed to evaluate the activities of this series of compounds. In this model (Penn et. al, Invest. Ophthalmol. Vis. Sci., 36, 2063, (1995)), rats pups (n=16) with their mother are placed in a computer controlled chamber that regulates the concentration of oxygen. The animals are exposed for 24 hours to a concentration of 50% oxygen followed by 24 hours at a concentration of 10% oxygen. This alternating cycle of hyperoxia followed by hypoxia is repeated 7 times after which the animals are removed to room air (P14). Compounds are administered via intravitreal injection upon removal to room air and the animals are sacrificed 6 days later (P20). The isolated retinas are then isolated, stained mounted and analyzed as detail above in the development model. The effectiveness was also graded as is described for the development model.
[0425] The exemplary compounds described above may be formulated into pharmaceutical compositions according to the following general examples.
Example A
Parenteral Composition
[0426] To prepare a parenteral pharmaceutical composition suitable for administration by injection, 100 mg of a water-soluble salt of a compound of Formula I is dissolved in dimethylsulfoxide and then mixed with 10 mL of 0.9% sterile saline. The mixture is incorporated into a dosage unit form suitable for administration by injection.
Example B
Oral Composition
[0427] To prepare a pharmaceutical composition for oral delivery, 100 mg of a compound of Formula I is mixed with 750 mg of lactose. The mixture is incorporated into an oral dosage unit for, such as a hard gelatin capsule, which is suitable for oral administration.
Example C
Intraocular Composition
[0428] To prepare a sustained-release pharmaceutical composition for intraocular delivery, a compound of Formula I is suspended in a neutral, isotonic solution of hyaluronic acid (1.5% conc.) in phosphate buffer (pH 7.4) to form a 1% suspension.
[0429] It is to be understood that the foregoing description is exemplary and explanatory in nature, and is intended to illustrate the invention and its preferred embodiments. Through routine experimentation, the artisan will recognize apparent modifications and variations that may be made without departing from the spirit of the invention. Thus, the invention is intended to be defined not by the above description, but by the following claims and their equivalents.
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Indazole compounds that modulate and/or inhibit the ophthalmic diseases and the activity of certain protein kinases are described. These compounds and pharmaceutical compositions containing them are capable of mediating tyrosine kinase signal transduction and thereby modulate and/or inhibit unwanted cell proliferation. The invention is also directed to the therapeutic or prophylactic use of pharmaceutical compositions containing such compounds, and to methods of treating ophthalmic diseases and cancer and other disease states associated with unwanted angiogenesis and/or cellular proliferation, such as diabetic retinopathy, neovascular glaucoma, rheumatoid arthritis, and psoriasis, by administering effective amounts of such compounds.
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RELATED APPLICATION
This application is a continuation application of U.S. patent application Ser. No. 11/490,820, filed Jul. 21, 2006, which claims the benefit of U.S. Provisional Application No. 60/701,685, filed Jul. 22, 2005, the entire contents of which are hereby incorporated by reference.
BACKGROUND
Fully enclosed dispensing cartons having dispensing openings at a top portion of the carton are known. A conventional dispensing carton is typically formed from a unitary paperboard blank having a pattern of tear lines that define a dispensing section of the carton. When the dispensing section is torn away from the carton, containers held within the carton can be removed. Such dispensing sections, however, are difficult to remove because of the stiffness of the paperboard material, which may cause difficulty in gripping the dispensing flap for tearing at the tear lines. The cartons also tend to tear at locations other than along the tear lines defining the dispensing section.
SUMMARY
According to a first embodiment, a carton comprises a first side panel, a top panel, a second side panel, a bottom panel, an exiting end panel, an end panel, and a dispenser section defined at least in part by a dispenser pattern extending at least through the top panel. The dispenser pattern includes a deformation pattern that facilitates gripping of the dispenser section and tearing of the carton along the dispenser pattern during opening of the dispenser.
Other aspects, features, and details of embodiments of the present invention can be more completely understood by reference to the following detailed description of preferred embodiments, taken in conjunction with the drawings figures and from the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
According to common practice, the various features of the drawings discussed below are not necessarily drawn to scale. Dimensions of various features and elements in the drawings may be expanded or reduced to more clearly illustrate the embodiments of the invention.
FIG. 1 is a plan view of a blank used to form a carton having a dispenser according to a first embodiment of the invention.
FIG. 2 is a perspective view of the carton blank in a partially erected state.
FIG. 3 is an end view of the carton blank in a partially erected state.
FIG. 4 is a perspective view of the carton according to the first embodiment of the invention.
FIG. 5 is an end view of the exiting end of the carton.
FIG. 6 is a partial left side view of the carton.
FIG. 7 is a partial right side view of the carton.
FIG. 8 is a top plan view of the carton.
FIGS. 9-12 illustrate the carton dispenser being opened.
FIG. 13 is a perspective view of the carton with the dispenser opened.
DETAILED DESCRIPTION
The present invention generally relates to dispensers for cartons having a deformation pattern that allow the dispenser to be easily and reliably opened. The present invention can be used, for example, in cartons that contain articles or other products such as, for example, food and beverages. The articles can also include beverage containers such as, for example, cans, bottles, PET containers, or other containers such as those used in packaging foodstuffs. For the purposes of illustration and not for the purpose of limiting the scope of the present invention, the following detailed description describes generally cylindrical beverage containers as disposed within the carton embodiments. In this specification, the relative terms “lower,” “bottom,” “upper” and “top” indicate orientations determined in relation to fully erected cartons. For purposes of the description presented herein, the term “line of disruption” can be used to generally refer to cuts, creases, cut-space lines, cut-creases, tear lines, scores, cut-scores, cuts interspersed with nicks, and combinations of these features. A “breachable” line of disruption is a line of disruption that is intended to be breached during ordinary use of the carton. An example of a breachable line of disruption is a tear line.
FIG. 1 is a plan view of a first, underside or interior side 5 of a blank 8 used to form a carton 150 (illustrated in FIG. 4 ) according to a first embodiment of the invention. The first side 5 of the blank 8 will be disposed in the interior of the erected carton 150 . The blank 8 comprises a first side panel 10 foldably connected to a top panel 30 at a first transverse fold line 32 , a second side panel 70 foldably connected to the top panel 30 at a second transverse fold line 72 , and a bottom panel 90 foldably connected to the second side panel 70 at a third transverse fold line 92 . An adhesive flap 40 can be foldably connected to the first side panel 10 at a fourth transverse fold line 42 . The blank 8 may include a slotted handle 120 in the top panel 30 , or at one or more other locations in the blank.
The first side panel 10 is foldably connected to a first side flap 12 and a first side exiting end flap 14 . The top panel 30 is foldably connected to a top flap 32 and a top exiting end flap 34 . The second side panel 70 is foldably connected to a second side flap 72 and a second side exiting end flap 74 . The bottom panel 90 is foldably connected to a bottom flap 92 and a bottom exiting end flap 94 . When the carton 150 is erected, the end flaps 12 , 32 , 72 , 92 close one end of the carton 150 , and the exiting end flaps 14 , 34 , 74 , 94 close an exiting end of the carton 150 . The end flaps 12 , 32 , 72 , 92 extend along a first marginal area of the blank 8 , and may be foldably connected at a first longitudinal fold line 60 that extends along the length of the blank 8 . The exiting end flaps 14 , 34 , 74 , 94 extend along a second marginal area of the blank 8 , and may be foldably connected at a second longitudinal fold line 62 that extends along the length of the blank 8 . The longitudinal fold lines 60 , 62 may be, for example, straight or substantially straight fold lines, or may be offset at one or more locations to account for, for example, blank thickness.
According to one aspect of the invention, the carton blank 8 includes a dispenser pattern 100 that defines a dispenser 110 in the erected carton 150 (illustrated in FIG. 4 ). The dispenser pattern 100 includes a tear line pattern 102 and a deformation pattern 80 .
The tear line pattern 102 extends across the panels 10 , 30 , 70 and the exiting end flaps 14 , 74 , 94 . The perimeter of the tear line pattern 102 is defined by first and second side tear lines 22 , 24 and a top tear line 26 . The first side tear line 22 includes an oblique section 23 that extends obliquely from a side edge of the first side exiting end flap 14 . The first side tear line 22 then turns to extend transversely across the longitudinal fold line 62 and into the first side panel 10 . The first side tear line 22 divides the first side exiting end flap 14 into a first tear away section 16 and a first retainer section 18 . The second side tear line 24 includes an oblique section 25 that extends obliquely from a side edge of the second side exiting end flap 74 . The second side tear line 24 then turns to extend transversely across the longitudinal fold line 62 and into the second side panel 70 . The second side tear line 24 divides the second side exiting end flap 74 into a second tear away section 76 and a second retainer section 78 . The top tear line 26 extends between the first and second side tear lines 22 , 24 and may designed to be torn continuously with the first and second side tear lines 22 , 24 . The top tear line 26 extends across the first and second side panels 10 , 70 and across the top panel 30 . A center portion of the top tear line 26 includes a generally v-shaped access portion. The tear lines 22 , 24 , 26 can form a generally continuous breachable line of disruption such as a tear line, or, one or more interruptions can be included in and between the tear lines. The tear line pattern 102 also comprises spaced oblique tear lines 96 , 98 in the bottom exiting end flap 94 . The tear line pattern 102 defines a removable dispenser section 50 in the erected carton 150 .
According to one aspect of the invention, the deformation pattern 80 is a pattern of lines of disruption in the blank 8 that allows the dispenser section 50 to deform during opening of the carton 150 . Deformation of the dispenser section 50 allows a user to more easily grasp the dispenser section 50 , and also facilitates reliable tearing along the tear line pattern 102 during opening of the dispenser 110 . The deformation pattern 80 includes first and second v-shaped edge deformation lines 52 , 53 first and second curved, access deformation lines 54 , 56 , and first and second oblique top deformation lines 58 .
A first v-shaped, edge deformation line 52 , 53 extends along each end of the top tear line 26 . The first v-shaped edge deformation line 52 , 53 extends obliquely through the first side panel 10 , from the juncture of the tear lines 22 , 26 , to the transverse fold line 32 . At the transverse fold line 32 , the first edge deformation line 52 , 53 extends obliquely through the top panel 30 towards the first access deformation line 54 . Similarly, the second v-shaped edge deformation line 52 , 53 extends obliquely through the second side panel 70 , from the juncture of the tear lines 24 , 26 , to the transverse fold line 72 . At the fold line 72 , the second v-shaped edge deformation line 52 , 53 extends obliquely through the top panel 30 towards the first access deformation line 54 .
The first and second access deformation lines 54 , 56 are disposed in the dispenser section 50 with their concave faces opposing the generally v-shaped central portion of the top tear line 26 . The first access deformation line 54 may extend across substantially all of the width of the top panel 30 , and may extend adjacent to the top tear line 26 at each end of the deformation line 54 . The first curved access deformation line 54 may be, for example, arcuate in shape, with the concave portion of the arc opposing the concave section of the top tear line 26 . The second curved access deformation line 56 may extend across at least about one third of the width of the top panel 30 , and may extend adjacent to the top tear line 26 at each end of the deformation line 56 . The second access deformation line 56 may be, for example, arcuate in shape, with the concave portion of the arc opposing the concave section of the top tear line 26 . The access deformation lines 54 , 56 are illustrated as generally arcuate, although other shapes are possible. For example, the access lines 54 , 56 may have a v-shape.
First and second oblique top deformation lines 58 extend from at or adjacent to respective corners of the dispenser section 50 , and converge toward one another as they approach the first access deformation line 54 . The first and second oblique top deformation lines 58 can intersect with or extend to points adjacent to the first curved deformation line 54 .
The top panel 30 can have a width W 1 that generally corresponds to a height of a container C to be held within the carton 150 . The first and second retainer sections 18 , 78 can each have a height H 1 selected to retain a container or containers C within the carton 150 , as discussed in further detail below. The side panels 10 , 70 have a height H 2 that generally corresponds to the height of the carton 150 . Erection of the carton 150 is discussed below with reference to FIGS. 2-4 .
FIG. 2 is a perspective view of an erection step of the carton 150 . The carton 150 is erected by gluing the adhesive flap 40 (shown in FIG. 1 ) to the bottom panel 90 so that the first side panel 10 , the top panel 30 , the second side panel 70 , and the bottom panel 90 may be opened into a generally tubular form or sleeve, as shown in FIG. 2 . The back end of the tubular sleeve is closed by folding the end flaps 32 , 92 across the open back end of the tubular form, folding the side end flap 12 over the flaps 32 , 92 and adhering the flaps together, and then folding the side end flap 72 over the flaps 12 , 32 , 92 and adhering the flap 72 thereto. Similarly, referring to FIG. 3 , the exiting end of the tubular sleeve is closed by folding the exiting end flaps 34 , 94 across the open exiting end of the tubular form, folding the side exiting end flap 14 over the flaps 34 , 94 and adhering the flaps together, and then folding the side exiting end flap 74 over the flaps 14 , 34 , 94 and adhering the flap 74 thereto. FIG. 3 illustrates the exiting end flaps 14 , 34 , 74 , 94 being closed over containers C loaded inside the tubular sleeve. The containers C may be loaded into the sleeve in a conventional manner before one or both ends of the tubular form are closed. In the exemplary embodiment, the carton 150 encloses twelve 12-ounce beverage containers C. The containers C are arranged in the carton 150 in a 2×6×1 configuration.
FIG. 4 is a perspective view of the carton 150 constructed from the blank illustrated in FIG. 1 . The carton 150 is parallelepipedal in shape. In the erected carton 150 , the end flaps 12 , 32 , 72 , 92 form a first end panel 130 and the exiting end flaps 14 , 34 , 74 , 94 form an exiting end panel 140 . The dispenser 110 extends across the side panels 10 , 70 , the top panel 30 , and the exiting end panel 140 , and comprises the removable dispenser section 50 . In FIG. 4 , the 2×6×1 arrangement of containers C is indicated by hidden lines.
FIG. 5 is an end view of the carton 150 . As shown in FIG. 5 , the first and second side tear lines 22 , 24 of the dispenser 110 can be separated by a width W 2 at the tops of the retainer sections 16 , 76 , and may converge to a width W 3 at or adjacent to the bottom of the exiting end panel 140 . The width W 2 may be selected to optimize the ease of removal of containers C from the carton 150 once the dispenser 110 is opened. The retainer sections 16 , 76 may extend to uppermost points having a height H 1 that is shorter than a height H 2 of the carton 150 . The height H 1 may be selected, for example, to retain an uppermost row or layer of containers C within the carton once the dispenser 110 is opened, as is discussed in further detail below.
FIGS. 6 and 7 are side views of the carton 150 , and illustrate the depth D 1 to which the first and second side tear lines 22 , 24 extend into the first and second side panels 10 , 70 , respectively. FIG. 8 is a top view of the carton 150 . As shown in FIG. 8 , the first and second oblique top deformation lines 58 extend from respective upper corners of the dispenser section 50 and may connect to or extend adjacent to the first, curved access deformation line 54 of the deformation pattern 80 .
FIG. 9 is a perspective view of the dispenser 110 being opened. Opening may be begun by pressing downwardly on the top panel 30 between the top tear line 26 of the tear line pattern 102 and the first curved deformation line 54 of the deformation pattern 80 so that the top panel 30 tears along the top tear line 26 . At this stage, gripping of the dispenser section 50 and tearing along the top tear line 26 is facilitated by deformation of the top panel 30 at the first and second curved access deformation lines 54 , 56 of the deformation pattern 80 . The upper edges of the carton 150 may also begin to flex inwardly at the first and second v-shaped edge deformation lines 52 . The first and second curved access deformation lines 54 , 56 allow the dispenser section 50 to flex inwardly to facilitate access to the dispenser section 50 during tearing.
Referring to FIGS. 10 and 11 , the tear line pattern 102 is further torn long the first and second side tear lines 22 , 24 (see also FIGS. 6 and 7 ), which extend down the first and second side panels 10 , 70 , respectively. Referring also to FIG. 1 , a center portion of the bottom exiting end panel 94 disposed between the tear lines 96 , 98 may be adhered to the tear away sections 16 , 76 , and is removed during opening of the dispenser 110 . During opening of the dispenser 110 , gripping of the dispenser section 50 and tearing along the tear line pattern 102 is facilitated by further deformation of the top panel 30 at the deformation lines 54 , 56 , 58 , and inward deformation of the upper edges of the carton 150 at the v-shaped deformation lines 52 , 53 .
FIG. 12 is a perspective view of the carton 150 with the dispenser 110 opened, leaving a dispenser opening 105 . With the dispenser section 50 removed, the container C in the top or uppermost row or layer adjacent to the dispenser opening can be easily accessed and removed from the carton 150 . Also, the dispenser opening 105 may extend downward in the exiting end panel 140 such that containers C in the lower row are also accessible by hand.
FIG. 13 is an end view of the carton 150 illustrating the exiting end panel 140 after opening the dispenser 100 . As shown in FIG. 13 , the containers C may be generally cylindrical in shape and may have a height H C and a diameter D C . The height H 1 of the retainer sections 18 , 78 may be selected to retain the container in the uppermost row of containers. For example, the height H 1 can be in the range of about 110-200% of the container diameter D C . In other embodiments, the height H 1 can be in the range of about 130-180% of the container diameter D C . The upper width W 2 may be between about 30-90% of the height H C of the containers C or the carton width W 1 (shown in the FIG. 1 ). In other embodiments, the width W 2 is between about 40-70% of the height H C or the carton width W 1 . The lower width W 3 may be between about 10-70% of the height H C of the containers C or the carton width W 1 . In other embodiments, the width W 3 is between about 30-50% of the height H C or the carton width W 1 . In general, the widths W 2 and W 3 between the retainer sections 18 , 78 are selected to be large enough so that a user can insert a finger into the dispenser opening 105 and pull a container C upwardly and out through the dispenser opening 105 .
EXAMPLE 1
A carton as illustrated in FIGS. 4-13 accommodated twelve 12-ounce cans. The cans were arranged in a 2×6×1 arrangement, as shown in FIG. 4 . The curved access deformation lines 54 , 56 were generally circular arcs comprised of cut-crease lines, with the cuts extending through the blank (i.e., 100% cuts). The deformation lines 52 , 53 , 58 were crease lines.
For purposes of illustration, the present invention is generally disclosed in the context of paperboard cartons or packages sized and dimensioned to contain generally cylindrical beverage containers in a two-row configuration with multiple columns of beverage containers included in each row. Other types of containers, however, can be accommodated within a carton according to the present invention. The dimensions of the blank may also be altered, for example, to accommodate various container forms.
The blank 8 can be, for example, formed from coated paperboard and similar materials. For example, the interior and/or exterior sides of the blank can be coated with a clay coating. The clay coating may then be printed over with product, advertising, price coding, and other information or images. The blank may then be coated with a varnish to protect any information printed on the blank. The blank may also be coated with, for example, a moisture barrier row, on either or both sides of the blank. In accordance with the above-described embodiments, the blank may be constructed of paperboard of a caliper such that it is heavier and more rigid than ordinary paper. The blank can also be constructed of other materials, such as cardboard, or any other material having properties suitable for enabling a dispenser to function as described above. The blank can also be laminated to or coated with one or more sheet-like materials at selected panels or panel sections.
In accordance with the exemplary embodiments, a fold line can be any substantially linear, although not necessarily straight, form of weakening that facilitates folding therealong. More specifically, but not for the purpose of narrowing the scope of the present invention, fold lines include: a score line, such as lines formed with a blunt scoring knife, or the like, which creates a crushed portion in the material along the desired line of weakness; a cut that extends partially into a material along the desired line of weakness, and/or a series of cuts that extend partially into and/or completely through the material along the desired line of weakness; and various combinations of these features.
A tear line can be any substantially linear, although not necessarily straight, breachable line of disruption that facilitates tearing therealong. Specifically, but not for the purpose of narrowing the scope of the present invention, tear lines include: a cut that extends partially into the material along the desired line of weakness, and/or a series of cuts that extend partially into and/or completely through the material along the desired line of weakness, or various combinations of these features. As a more specific example, one type of tear line is a series of cuts that extend completely through the material, with adjacent cuts being spaced apart slightly so that small somewhat bridge-like pieces of the material (e.g., ‘nicks’) are defined between adjacent cuts. The nicks are broken during tearing along the tear line. Such a tear line that includes nicks can also be referred to as a cut line, since the nicks typically are a relatively small in relation to the cuts.
The term “line” as used herein includes not only straight lines, but also other types of lines such as curved, curvilinear or angularly displaced lines.
The above embodiments may be described as having one or panels adhered together by glue. The term “glue” is intended to encompass all manner of adhesives commonly used to secure paperboard carton panels in place.
In the present specification, a “panel” or “flap” need not be flat or otherwise planar. A “panel” or “flap” can, for example, comprise a plurality of interconnected generally flat or planar sections.
The foregoing description of the invention illustrates and describes the present invention. Additionally, the disclosure shows and describes only selected embodiments of the invention, but it is to be understood that the invention is capable of use in various other combinations, modifications, and environments and is capable of changes or modifications within the scope of the inventive concept as expressed herein, commensurate with the above teachings, and/or within the skill or knowledge of the relevant art.
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A dispensing carton includes a dispenser section having a deformation pattern provided therein. The deformation pattern facilitates removal of the dispenser section during opening of the carton.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to an exhaust gas turbine that is driven by exhaust gas emitted from an engine, more specifically, the present invention relates to an exhaust gas turbine equipped with an exhaust gas control valve, i.e. a waste gate valve, for closing and opening an exhaust gas bypass passage so that the exhaust gas emitted from an engine bypasses the exhaust gas turbine and flows into an exhaust gas outlet passage.
[0003] 2. Background of the Invention
[0004] In an exhaust gas turbocharger of a relatively smaller size class, the exhaust gas turbine therein that is driven by the exhaust gas emitted from the engine is provided with a waste gate valve for closing and opening the exhaust gas bypass passage through which the exhaust gas emitted from the engine toward the exhaust gas turbine bypasses the exhaust gas turbine and flows into an exhaust gas (waste gas) outlet passage; in a case where the flow rate of the exhaust gas toward the turbine becomes excessive, the waste gate is relatively opened so that a part of the exhaust gas toward the turbine bypasses the turbine and flows into the exhaust gas outlet passage; and, the flow rate through the turbine is controlled so as to be kept at an pertinent flow rate level. Thus, the engine boost pressure during the higher load side operation is enhanced by relatively closing the waste gate valve that is relatively opened during the lower load side operation where the exhaust gas flow rate is surplus. It is noted that the term “relatively open” or “relatively close” means that the valve is not of an on-off type.
[0005] FIGS. 3(A) and 3(B) show the structure of the waste gate valve (the exhaust gas flow rate control valve) as well as the structure around the waste gate valve in the exhaust gas turbine of the exhaust gas turbocharger; FIG. 3(A) shows a longitudinal section as to the drive part of the waste gate valve; FIG. 3(B) shows the A-A cross section in FIG. 3(A) .
[0006] The exhaust gas turbine 100 shown in FIGS. 3(A) and 3(B) comprises: a turbine casing 1 in which a turbine 2 (detail not shown) is provided; a waste gate valve 3 through which the exhaust gas that is supplied from the engine (not shown) toward the turbine 2 is diverged in an exhaust gas passage 6 to bypass the turbine 2 , and flows into an exhaust gas (waste gas) outlet passage 5 a , through an exhaust gas bypass passage 5 . In addition, the numeral 4 denotes an exhaust gas inlet flange (of the turbine casing 1 ) by which the waste gate valve is fitted to the engine or a pertinent component relating to the engine.
[0007] A valve body 3 a of the waste gate valve 3 opens and closes the exhaust gas bypass passage 5 with reciprocating movements or hinge-like movements; in closing the exhaust gas bypass passage 5 , the valve body 3 a sit on a valve seat 5 b that is formed on the outer side surface of the turbine casing 1 around the exhaust gas bypass passage 5 ; in opening exhaust gas bypass passage 5 , the valve body 3 a leaves the valve seat 5 b so that a part of the exhaust gas (the bypassing exhaust gas) flows from the exhaust gas passage 6 into the exhaust gas (waste gas) outlet passage 5 a along the curved arrow direction as depicted in FIG. 3(B) .
[0008] A support axis (shaft) 8 of a L-shape is fastened to the valve body 3 a of the waste gate valve 3 , at an end part 8 b of the support axis (shaft) 8 , by means of a rivet (coupling) 8 c . The support axis (shaft) 8 is rotation-freely (swing-freely) fitted in a bush 7 that is fixed to the turbine casing 1 (or, in a guide hole that is provided in the turbine casing 1 ).
[0009] An arm 9 is fixed to a shaft end part of the support axis (shaft) 8 , by means of a caulking device 9 a or the like. The arm 9 is provided with a connecting part 13 via which the support axis (shaft) 8 is connected to an actuator (not shown) therefor. Thus, according to the swing movements of the connecting part 13 , the support axis (shaft) 8 is rotated or swung around an axis 8 a thereof; further, via the rotation (rotational swing) movements of the support axis (shaft) 8 , the valve body 3 a of the waste gate valve sits on or leaves the valve seat 5 b , namely the valve body opens or closes the exhaust gas bypass passage 5 .
[0010] In the patent reference 1 (JP1995-10434), a technology is disclosed regarding a method for firmly locking a swing arm 6 as well as a swing lever 7 of the waste gate valve; whereby, a spring-biased lock lever 10 interlocks the swing lever 7 (and the swing arm 6 ) in a manner that a cam surface of the lock lever 10 comes in contact with a cam surface of an end part of the swing lever 7 , and presses the latter cam surface along the contact tangential direction so that the former cam surface interlocks the latter cam surface when the waste gate valve is closed and a control rod 8 is placed at a retired position. Thus, the patent reference 1 provides a technology whereby the valve body of the waste gate valve is firmly fixed to a predetermined valve-closing position.
[0011] It is noted that the numerals as to the structure components in this paragraph are the numerals that are used in the reference 1, not in the attached drawings of this application.
[0012] As shown in FIGS. 3(A) and 3(B) , through the waste gate valve 3 , the exhaust gas that is supplied from the engine toward the exhaust gas turbine 2 is diverged in the exhaust gas passage 6 which is located upstream of the turbine 2 ; a part of the exhaust gas before the turbine 2 bypasses the turbine 2 , and flows into the exhaust gas (waste gas) outlet passage 5 a , through the through an exhaust gas bypass passage 5 .
[0013] Further, according to the swing movements of the connecting part 13 via which the support axis (shaft) 8 is connected to the actuator therefor, the support axis (shaft) 8 is rotated (swung) around an axis 8 a thereof; thus, via the rotation (rotational swing) movements of the support axis (shaft) 8 , the valve body 3 a of the waste gate valve sits on or leaves the valve seat 5 b , namely the valve body opens or closes the exhaust gas bypass passage 5 .
[0014] The bearing area between the bush 7 and the support axis (shaft) 8 that are exposed to the exhaust gas of high temperature is of an oil free type as it is difficult to provide the bearing area with a lubrication condition; thus, the running surfaces as to the bush 7 and the support axis (shaft) 8 of the waste gate valve 3 is prone to wear down in response to the frequency of use (or the operating hours) thereof.
[0015] In addition to the non-lubrication condition, or in response to the trend of the nowadays boost increasing, the levels of the waste gate valve vibration along the X-arrow direction as shown in FIG. 3(B) the vibration which is caused by the engine vibration or the exhaust gas flow pulsation become greater and greater; thus, it becomes a prerequisite to restrain the wear around the bearing area between the bush 7 and the support axis (shaft) 8 , in consideration of not only the valve closed condition but also over the whole operating conditions.
[0016] As a matter of fact, in the conventional technology of the patent reference 1 (JP1995-10434), the valve body of the waste gate valve is firmly pressed and maintained to a predetermined location in a case where the valve is closed; however, the valve body is not firmly maintained at an expected location in a case where the valve is half-opened. In other words, the vibration reduction effect as to the waste gate valve cannot exceed the desired level, in the case where the valve is half-opened.
DISCLOSURE OF THE INVENTION
[0017] In view of the above described subjects in the conventional technology, the present invention aims at providing an exhaust gas turbine equipped with an exhaust gas control valve (a waste gate valve) comprising: a support axis (shaft) that controls the movement of the valve body of the exhaust gas control valve; a bush (or a guide hole in the turbine casing of the exhaust gas turbine) in which the support axis (shaft) is rotation-freely or swing-freely fitted; wherein, the wear of the fitting clearance area (between the support axis shaft and the bush hole (or the casing hole) can be reduced over the whole operating range as to the exhaust gas control valve.
[0018] In order to reach the goal of the invention, the present invention discloses an exhaust gas turbine driven by exhaust gas emitted from an engine and being equipped with an exhaust gas control valve for closing and opening an exhaust gas bypass passage through which the exhaust gas emitted from an engine bypasses the exhaust gas turbine and flows into an exhaust waste gas outlet passage, the exhaust gas control valve comprising:
[0019] a support axis shaft for supporting a valve body for controlling the opening of the exhaust gas bypass passage, the support axis shaft being rotation-freely or swing-freely supported in a turbine casing of the turbine;
[0020] an arm for rotating or swinging the support axis shaft around an axis of the support axis shaft by reciprocating rotational movements or swing movements that are transferred from a drive source to the arm via a connecting part provided to the arm at an end part of the arm; and
[0021] a weight equipped at an arm end part opposite to where the connecting part is provided, with respect to the axis of the support axis shaft.
[0022] Regarding the above-described invention, the preferable embodiments are:
[0023] (1) the exhaust gas turbine equipped with an exhaust gas control valve according to the above disclosure, a valve body center of the exhaust gas control valve is located at a predetermined distance apart from the connecting part via which the running gears or moving parts of the exhaust gas control valve are operated, in the direction of the axis of the support axis shaft; and, the center of gravity of the weight in the direction of the axis is placed at a position between the connecting part and the valve body center;
[0024] (2) the exhaust gas turbine equipped with an exhaust gas control valve according to the above disclosure, wherein the middle part of the arm is fixed to the support axis shaft, the weight is equipped at the arm end part opposite to the other arm end part at which the connecting part is placed and transfers the operation movements from the drive source to the moving parts of the waste gate valve, further wherein, the weight is fastened to the arm by means at least one self-locking nut and a bolt.
[0025] Another preferable embodiment is the exhaust gas turbine equipped with an exhaust gas control valve according to the above disclosure or the above preferable embodiment (2), wherein the arm and the weight are formed as a single piece made by casting or forging, and the middle part of the arm is fixed to the support axis shaft.
[0026] According to the present invention as described above, the exhaust gas control valve (the waste gate valve) comprising:
[0027] the support axis shaft for supporting the valve body for controlling the opening of the exhaust gas bypass passage, the support axis shaft being rotation-freely or swing-freely supported in the turbine casing of the turbine;
[0028] the arm for rotating or swinging the support axis shaft around the axis of the support axis shaft by reciprocating rotational movements or swing movements that are transferred from a drive source to the arm via the connecting part provided to the arm at the end part of the arm; and
[0029] the weight equipped at the arm end part opposite to where the connecting part is provided, with respect to the axis of the support axis shaft.
[0030] More concretely, the valve body center of the exhaust gas control valve is located at the predetermined distance apart from the connecting part via which the running gears or moving parts of the exhaust gas control valve are operated, in the direction of the axis of the support axis shaft; and, the center of gravity of the weight in the direction of the axis is placed at a position between the connecting part and the valve body center.
[0031] Further concretely, the middle part of the arm is fixed to the support axis shaft, the weight is equipped at the arm end part opposite to the other arm end part at which the connecting part is placed and transfers the operation movements from the drive source to the moving parts of the waste gate valve, further wherein, the weight is fastened to the arm by means at least one self-locking nut and a bolt.
[0032] In addition, as a matter of great import, the weight is equipped at an (arm) end part counter to the (arm) connecting part with regard to the axis of the support axis shaft.
[0033] Therefore, the inertia mass (the moment of inertia) around the axis 8 as to the running gear parts of the waste gate valve is increased due to the provided weight, in contrast to the conventional way; thus the swing vibration of the valve body around the axis of the support axis shaft due to the pressure pulsation in the exhaust gas emitted from the engine can be restrained.
[0034] Moreover, due to the increased moment of inertia as to the moving parts of the exhaust gas control valve thereby the increased moment of inertia is attributable to the provided weight that is equipped at the end part counter to the connecting part via which the moving parts of the exhaust gas control valve are operated as per the movements of drive source, the angular velocity change as to the swing movement of the arm and the support axis shaft in response to the engine exhaust gas pressure pulsation can be smooth; thus, the relative movement between the bush (or a hole in the turbine casing to place the support axis shaft) and the support axis shaft connected to the valve body can be also smooth. In this way, the vibration levels of the exhaust gas control valve can be reduced over the whole operation zone of the valve body (, besides, in the middle operation zone of the valve body or under the closed condition thereof).
[0035] Further, in this embodiment, the center of the exhaust gas control valve (namely, the center of the valve body) is located at a predetermined distance S from the connecting part via which moving parts of the exhaust gas control valve are operated as per the movements of drive source, in the direction of the axis of the support axis shaft (cf. claim 2 ). As for the position of the provided weight in the direction along the axis of the support axis shaft, the center of gravity of the provided weight is placed between the connecting part and the valve body center. Thanks to the balance between the mass around the provided weight and the mass around the connecting part, the center of the gravity as to the moving parts gets closer to the axis of the support axis shaft; thus, the tilting moment (or pitching moment) induced by the engine vibration the moment which works the support axis shaft can be reduced. In addition, the provided weight is firmly fastened to the arm by use of the self-locking nut and the bolt therefor; thus, there is no apprehension that the provided weight comes off.
[0036] Further, according to the present invention, the arm and the provided weight are formed as a single-piece construction made by casting or forging; the middle part of the arm is fitted to the support axis shaft; thus, this embodiment brings effective results, as is the case with the former embodiment; in addition, since the arm and the provided weight are formed as a single-piece construction made by casting or forging, the number of components as well as the assembly cost can be reduced; further, there is no apprehension that the provided weight comes off, thanks to the single piece configuration; thus, the reliability of the exhaust gas control valve can be enhanced. Moreover, the single piece configuration made by casting or forging can be designed with an enhanced degree of freedom in shape; therefore, the narrow space around the engine can be effectively used.
BRIEF DESCRIPTION OF THE DRAWINGS
[0037] FIG. 1(A) shows the structure of the waste gate valve (the exhaust gas flow rate control valve) as well as the structure around the waste gate valve in the exhaust gas turbine of the exhaust gas turbocharger, according to the first embodiment of the present invention;
[0038] FIG. 1(B) shows a view as to the Z-arrow in FIG. 1(A) ;
[0039] FIG. 2(A) shows the structure of the waste gate valve (the exhaust gas flow rate control valve) as well as the structure around the waste gate valve in the exhaust gas turbine of the exhaust gas turbocharger, according to the second embodiment of the present invention;
[0040] FIG. 2(B) shows a view as to the Y-arrow in FIG. 1(A) ;
[0041] FIG. 3(A) shows the structure of the waste gate valve (the exhaust gas flow rate control valve) as well as the structure around the waste gate valve in the exhaust gas turbine of the exhaust gas turbocharger, according to the conventional technology;
[0042] FIG. 3(B) shows the A-A cross-section in FIG. 3(A) .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0043] Hereafter, the present invention will be described in detail with reference to the embodiments shown in the figures. However, the dimensions, materials, shape, the relative placement and so on of a component described in these embodiments shall not be construed as limiting the scope of the invention thereto, unless especially specific mention is made.
First Embodiment
[0044] FIG. 1(A) shows the structure of the waste gate valve (the exhaust gas flow rate control valve) as well as the structure around the waste gate valve in the exhaust gas turbine of the exhaust gas turbocharger, according to the first embodiment of the present invention; FIG. 1(B) shows a view as to the Z-arrow in FIG. 1(A) .
[0045] The exhaust gas turbine 100 shown in FIGS. 1(A) and 1(B) comprises a turbine casing 1 in which a turbine 2 (details not shown) is provided with a waste gate valve 3 . The waste gate valve 3 , as shown in FIG. 3(A) and FIG. 3(B) , is for diverging the exhaust gas emitted from the engine (not shown) to the turbine 2 via an exhaust gas passage 6 , in the exhaust gas passage 6 located upstream of the turbine 2 so that the diverged exhaust gas bypasses the turbine 2 and flows to an exhaust gas outlet passage 5 a via an exhaust gas bypass passage 5 . In addition, the numeral 4 denotes an exhaust gas inlet flange.
[0046] As is the case with FIGS. 3(A) and 3(B) , a valve body 3 a of the waste gate valve 3 opens and closes the exhaust gas bypass passage 5 by reciprocating movements or hinge-like movements. When the exhaust gas bypass passage 5 is in an opening condition apart of the exhaust gas flows into the exhaust gas outlet passage 5 a from the exhaust gas passage 6 along the arrow (the curved arrow) direction as depicted in FIG. 3(B) .
[0047] A support axis (shaft) 8 of a L-shape is fastened to the valve body 3 a of the waste gate valve 3 at an end part 8 b of the support axis (shaft) 8 by means of a rivet (coupling) 8 c . The support axis (shaft) 8 is rotation-freely or swing-freely fitted in a bush 7 that is fixed to the turbine casing 1 .
[0048] An arm 9 is fixed to a shaft end part of the support axis (shaft) 8 , by means of a caulking device 9 a or the like. The arm 9 is provided with a connecting part 13 through which the support axis (shaft) 8 is connected to an actuator (not shown) therefor.
[0049] Thus far, the configuration of the first embodiment is the same as that depicted in FIGS. 3(A) and 3(B) . In this embodiment, a weight 10 is provided to an end part of the arm 9 opposite to the position where the connecting part 13 is attached, with respect to the location where the axis 8 a intersects with the arm 9 .
[0050] In the waste gate valve 3 as shown in FIGS. 1(A) and 1(B) , the weight 10 is fastened to the arm (the extended arm) 9 at an end part 10 s thereof, by means of a bolt 12 and a self-locking nut 11 ; thereby, the end part 10 s is on the opposite side of the connecting part 13 position, with respect to the location where the axis 8 a of the support axis shaft 8 intersects with the arm 9 .
[0051] As shown in FIG. 1(A) , a center of the waste gate valve 3 is located at a position, a valve body center 3 c , which is a predetermined distance S away from the position of the connecting part 13 , thereby, the position of the weight 10 is between the connecting part 13 and the valve body center 3 c.
[0052] Thus, in response to the reciprocating movements or swing movements as to the connecting part 13 the movements which are brought by the actuator, the support axis (shaft) 8 is rotated (with reciprocating rotational movements) around the axis 8 a so that the valve body 3 a sits on the valve seat 5 b or leaves the seat, namely, the waste gate valve 3 closes or opens. Regarding the reciprocating rotational movements, the inertia mass (the moment of inertia) of the waste gate valve 3 has been increased by the weight 10 , in contrast to the conventional way ( FIGS. 3(A) and 3(B) ).
[0053] In this first embodiment as described above, the waste gate valve 3 comprises the support axis shaft 8 for driving the valve body 3 a that is rotation-freely supported by the bush 7 , and controls the opening (the degree of openings) as to the exhaust gas bypass passage 5 , the extended arm for rotating the support axis shaft 8 around the axis 8 a by the reciprocating movements or swing movements as to the arm 9 , and the weight 10 equipped at an end part 10 s opposite to the connecting part 13 with respect to the axis 8 a of the support axis shaft 8 , the arm 9 being operated so as to rotate with the reciprocating movements or swing movements by an actuator via the connecting part 13 .
[0054] Further, the center of the waste gate valve 3 is located at a predetermined distance S from the connecting part 13 . As for the position of the center of gravity as to the weight 10 in the direction along the axis 8 a , the weight 10 is placed between the connecting part 13 and the valve body center 3 c . In addition, the arm 9 is fixed to the support axis (shaft) 8 by means of a caulking device 9 a at the middle position of the arm 9 . The arm 9 is provided with the connecting part 13 via which the support axis (shaft) 8 is connected to the actuator (not shown). The arm 9 is fitted with the weight 10 at another end part 10 s of the arm 9 , thereby the end part 10 s is located at a position opposite to the connection part 13 with respect to the caulking position (the middle position of the arm 9 ), the weight 10 being fitted to the arm by means of the bolt and the self-locking nut 11 .
[0055] According to the above-described configuration as per the first embodiment, the running gear parts (the support axis shaft, the valve body and the extended arm) of the waste gate valve are equipped with the weight 10 that is placed at an end part of the extended arm, the end part located at the opposite side of the arm where the connecting part 13 is provided that performs reciprocating movements or swing movements around the middle part of the extended arm, namely, around the axis 8 a of the support axis shaft 8 . Therefore, the inertia mass (the moment of inertia) around the axis 8 as to the running gear parts of the waste gate valve is increased due to the weight 10 , in contrast to the conventional way; thus the swing vibration of the valve body 3 a around the axis 8 due to the pressure pulsation in the exhaust gas emitted from the engine can be restrained.
[0056] Moreover, in the above embodiment, due to the increased moment of inertia as to the running gears thereby the increased moment of inertia is attributable to the weight 10 that is equipped at the end part opposite to the connecting part 13 , the angular velocity change as to the swing movement of the arm 9 and the support axis shaft 8 in response to the pressure pulsation can be smooth. Thus, the relative movement of the bush 7 and the support axis shaft 8 connected to the valve body 3 a can be also smooth. In this way, the vibration levels of the waste gate valve 3 can be reduced over the whole operation zone of the valve body 3 a ; besides, in the opening levels as to the middle operation zone of the waste gate valve or under the closed condition thereof.
[0057] Further, in this embodiment, the center of the waste gate valve 3 (namely, the center 3 c of the valve body 3 a ) is located at a predetermined distance S from the connecting part 13 via which the running gears (moving parts) of the waste gate valve are operated, in relation to the direction of the axis of the support axis shaft. As for the position of the weight 10 in the direction along the axis 8 a , the center of gravity of the weight 10 is placed between the connecting part 13 and the valve body center 3 c . Thanks to the balance between the mass around the weight 10 and the mass around the connecting part 13 , the center of the gravity as to the running gears gets closer to the axis 8 a of the support axis (shaft) 8 ; thus, the tilting moment induced by the engine vibration the moment which works the support axis (shaft) 8 can be reduced. In addition, the weight 10 is firmly fastened to the arm 9 by use of the self-locking nut 11 and the bolt 12 therefor; thus, there is no apprehension that the weight comes off.
Second Embodiment
[0058] FIG. 2(A) shows the structure of the waste gate valve (the exhaust gas flow rate control valve) as well as the structure around the waste gate valve in the exhaust gas turbine of the exhaust gas turbocharger, according to the second embodiment of the present invention; FIG. 2(B) shows a view as to the Y-arrow in FIG. 1(A) .
[0059] In this second embodiment as shown in FIG. 2(A) , the arm 10 a and the weight 10 are formed as a single-piece construction made by casting or forging. The middle part of the arm 10 a is fitted to the support axis (shaft)) 8 by means of the caulking device 9 a . Other configuration or component arrangement is the same as that of the first embodiment; the common symbols or numerals are used for the common components in the first and the second embodiments
[0060] The second embodiment brings effective results, as is the case with the first embodiment. In addition, since the arm 10 a and the weight 10 are formed as a single-piece construction made by casting or forging metal, the number of components as well as the assembly cost can be reduced. Further, there is no apprehension that the weight comes off due to the single niece configuration. Thus, the reliability of the waste gate valve can be enhanced. Moreover, the single piece configuration made of casting or forging metal can be designed with an enhanced degree of freedom in shape, therefore, the narrow space around the engine can be effectively used.
INDUSTRIAL APPLICABILITY
[0061] The present invention can provide an exhaust gas turbine equipped with an exhaust gas control valve (a waste gate valve) comprising: a support axis (shaft)) that controls the movement of the valve body of the exhaust gas control valve; a bush (or a guide hole in the turbine casing of the exhaust gas turbine) in which the support axis (shaft) is rotation-freely or swing-freely fitted; wherein, the wear of the fitting clearance area (between the support axis shaft and the guide hole (or the casing hole) can be reduced over the whole operating range as to the exhaust gas control valve.
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Provided is an exhaust turbine equipped with an exhaust control valve (waste gate valve) which can reduce wear of the contact surfaces between the shaft and the bushing or the turbine casing that support the moving components of the valve in the entire operating range of the exhaust control valve. The exhaust turbine is equipped with the exhaust control valve for opening/closing an exhaust bypass passage which extends from an exhaust passage leading the exhaust turbine being driven by exhaust gas output from an engine to an exhaust outlet passage while bypassing the exhaust turbine, wherein the exhaust control valve comprises a shaft which is supported rotation-freely by a bushing or a turbine casing and supports a valve element for controlling the opening of the exhaust bypass passage, an arm equipped with a connecting part with a drive source and turning the shaft about the axis thereof by the reciprocating motion of the connecting part produced by the drive source, and a weight attached to an end on the side opposite to the connecting part with the drive source with respect to the axis of the shaft.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method of compressing gas in a compressor station for a gas pipe line, particularly in permanent frost areas. The method includes compressing the gas delivered in the pipeline with an entry pressure in a compression procedure to a higher pressure, subsequently cooling the gas by a heat exchange and again feeding the gas for the further transportation to the pipeline with a lower exit temperature, particularly an exit temperature of at most 0° C., and with an increased exit pressure as compared to the entry pressure.
The present invention also relates to an arrangement for carrying out the method.
2. Description of the Related Art
Natural gas is transported today in very large quantities frequently over distances of several thousand kilometers in large gas pipelines to the centers of consumption. For example, such long-distance gas pipelines may have a diameter of 56 inches and may be operated with gas pressures of 75 bar or even up to 100 bar, in order to achieve a transportation capacity which is as large as possible. Because of the unavoidable pressure loss along the gas pipelines, the compressor stations must be provided at certain intervals for increasing the gas pressure back to the nominal pressure. As a rule, the compressors used for this purpose, usually turbo compressors, are driven by gas turbines which use a portion of the transported natural gas as fuel. A very large portion of the known natural gas reserves are located in so-called permanent frost areas, i.e., in areas in which the ground thaws during the summer months only to a depth of about 80 to 100 cm and remains otherwise permanently frozen. The gas pipelines are usually placed at a depth in the ground where permanent frost prevails. Since the soil frequently becomes very soft in the thawed state, it must be ensured that the gas pipeline does not result in thawing of the ground because the pipeline would otherwise at least at certain locations sink lower and lead to mechanical stresses in the pipe wall which may lead to pipe ruptures. Heating of the soil is a possibility because the compression of the gas in the compressor inevitably also results in a temperature increase. Therefore, the gas compressed to nominal pressure is conventionally cooled before being returned into the pipeline, wherein a maximum temperature of approximately 0° C. must be maintained. If possible, a temperature of - 5° C. is desirable.
Because of the low outside temperatures substantially below 0° C., the required cooling poses no problems during the winter months and can be easily carried out by gas/air coolers. However, during the transition periods and particularly in the summer months, during which maximum day temperatures of 15° to 20° C. are possible, the gas coolers are inevitably no longer sufficient. For this reason, special re-cooling plants with separate cooling cycle, i.e., refrigerating or cooling machines in which propane in particular is used as a cooling agent, are used in such compressor stations during the warm weather periods.
The use of re-cooling plants of the conventional type poses several problems. The re-cooling plants are very expensive and constitute a large portion of the total investment for a compressor station. In addition, there is the fact that the plant is completely unused during the major portion of a year, i.e., for eight months. In addition, there is a safety problem with respect to possible leakages because the propane as cooling agent is not only easily flammable, but is also heavier than air and, therefore, has a reduced volatility, so that the explosion risk is substantially increased.
SUMMARY OF THE INVENTION
Therefore, it is the primary object of the present invention to propose a method of the above-described type and an arrangement for carrying out the method in which the required investments and operation risk are substantially reduced.
In accordance with the present invention, the method of the above-described type includes the steps of compressing the gas at least during individual intervals to a substantially higher pressure (excess pressure) than the desired exit pressure, cooling the compressed gas by the heat exchange to a temperature above the exit temperature, and obtaining the further cooling to the desired exit temperature by expanding the gas from the excess pressure to the desired exit pressure.
A compressor station for a gas pipeline for carrying out the above-described method includes at least one compressor for compressing gas, at least one heat exchanger for cooling compressed gas, additionally valve-controlled pipelines for connecting the compressor and the heat exchanger to one another and to the gas pipeline, as well as control units for controlling the compressor and the valves. In accordance with the present invention, an electronic control is provided which operates in such a way that at least one compressor carries out a compression of the gas to an excess pressure which is substantially above the desired exit pressure. In addition, an expanding unit is provided for expanding the compressed gas, wherein the electronic control is operated in such a way that the expansion takes place until the desired exit pressure is reached.
The present invention starts from the fact that it is known to carry out the compression of a gas supplied at an entry pressure below the nominal pressure (rated pressure of the gas pipeline) to an increased pressure, wherein the compression can be carried out in a single stage or in multiple stages in compressors which are connected in series. Between the compressor stages and particularly after the last compressor stage, cooling by heat exchange takes place (usually air/gas heat exchange), in order to reach the required lower exit temperature of at most 0° C., preferably -5° C., for the re-entry of the compressed gas into the gas pipeline.
During the warmer period of the year, in which the use of re-cooling units was necessary in the past for ensuring the required exit temperature, the present invention provides for a different type of cooling. The present invention utilizes the known physical effect according to which a compressed gas is inevitably cooled when expanded to a lower pressure, either by throttling or with the simultaneous performance of work. In order to ensure the required exit pressure or nominal pressure at the exit of the compressor station, the present invention provides that the gas to be transported is compressed to an excess pressure which is substantially above the exit pressure, for example, 10 to 50 bar above the exit pressure, to carry out at the end of the single-stage or multiple-stage compression a cooling by heat exchange, particularly by air/gas heat exchange, and subsequently to expand the compressed gas to the desired exit pressure. The excess pressure is selected in such a way that, taking into consideration the extent by which the gas compressed to excess pressure can be cooled by heat exchange, cooling during expansion is sufficient for obtaining a temperature reduction at least to the desired exit temperature of the gas for the re-entry into the gas pipeline or transportation. These parameters can be easily computed with the aid of the existing limiting or boundary conditions.
The expansion can be carried out in a simple manner, for example, by means of a valve. However, a more significant cooling effect can be achieved if the compressed gas additionally performs work during the expansion, as this is possible in an expansion turbine. This embodiment of the invention is particularly recommended for the operation during the summer months, and this embodiment provides the additional advantage that the recovered mechanical energy can be utilized for providing a portion of the drive energy for the compression of the gas to the intended excess pressure.
A particularly advantageous embodiment of the present invention provides that the compression to the excess pressure is carried out in a total of three stages, wherein a predominant portion of the compression takes place in two successive primary., compression stages which are equipped with machines which produce approximately the same pressure ratio. This provides the advantage that the compressors of the primary compression stages may be essentially of the same construction. Only the compressor housing of the subsequent compressor or compressors must be dimensioned for a higher pressure than the housing of the compressor or compressors of the first primary compression stage. Between the two primary compression stages, the gas heated in the first primary compression stage is cooled preferably by air/gas heat exchange. When the compressed gas leaves the second primary compression stage, the gas has not yet reached the desired excess pressure. The desired excess pressure is reached in an additional compression stage which includes a booster compressor. Subsequently, the gas is again cooled, preferably by means of an air/gas heat exchange. An expansion with simultaneous performance of work is then carried out in an expansion turbine. The latter is coupled, for example, mechanically to the booster compressor of the additional compression stage and is the sole drive means for the booster compressor, so that a significant portion of the total drive energy required for producing the excess pressure can be recovered and is not lost.
The above-described manner of carrying out the method in two primary compression stages with compressors having approximately the same pressure ratio provides the significant advantage that the compressors used in the stages can be completely exchanged for one another, as long as they are operated with the maximum permissible pressure of the first primary compression stage.
The possibility of exchanging the compressors is of particular interest because the requirements with respect to the rate of flow through the pipeline, i.e., the required nominal pressure in the pipeline, on the one hand, and the environmental conditions for cooling by heat exchange, on the other hand, are subject to substantial changes during the course of the year. During the cold season, during which the cooling can be ensured without problems by heat exchange alone, the pressure achievable with one primary compression stage (i.e. single-stage) is already sufficient, so that cooling by expansion from an even higher excess pressure becomes superfluous. On the other hand, during the warmer season, the insufficient cooling by heat exchange means that the amount of gas required is usually lower, for example, 10 to 15% lower, than in the cold season, so that it is possible to operate with a pipeline pressure which is lower as compared during the winter season. Consequently, the actually required excess pressure can be selected lower, and, in order to still achieve the required temperature level, the expansion can be carried out instead to a nominal pressure which is lower than the nominal pressure during the cold season. Because of these conditions, not only the operation in the warm season can be carried out inexpensively and with a comparatively small quantity of energy; there are also advantages with respect to the operation during the cold season because the compressors of the second primary compression stage can be operated parallel with the compressors of the first primary compression stage, i.e., under the same pressure conditions. For this purpose, the connecting pipelines to the inlets and outlets of the compressors are switched to parallel operation by means of a suitable valve control. Since several compressors of the same type already operate in parallel in each primary compression stage, and since all compressors never have to be used even during peak load periods, in addition to already existing stand-by machines, additional compressors are available which can be used as needed during breakdowns or when maintenance has to be performed. As compared to the prior art in which special re-cooling units are used which can only be used efficiently during the warm season, i.e., in summer operation, the present invention provides an altogether better possibility of using the principal units of the compressor stations throughout the entire year.
The various features of novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of the disclosure. For a better understanding of the invention, its operating advantages, and specific objects attained by its use, reference should be had to the drawing and descriptive matter in which there are illustrated and described a preferred embodiment of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawing:
FIG. 1 is a schematic diagram showing an embodiment of a compressor station according to the present invention during summer operation; and
FIG. 2 shows the compressor station of FIG. 1 during winter operation.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIGS. 1 and 2 of the drawing, those connecting pipelines through which the gas flows during the respective type of operation are shown in thick lines and the pipelines which are closed off by valves are shown in thin lines. In the illustrated embodiment, the gas pipeline has two parallel line strands 1a, 1b. The pressure in the pipeline which may have dropped at the entry into the compressor station to, for example, 50 bar, is to be raised again to reach a nominal pressure of, for example, 75 or 100 bar, at the exit of the compressor station. The gas pipeline 1a, 1b initially leads into a purifying unit 2a and 2b, respectively, which may be constructed as cyclone separators with or without filters and serve to separate undesirable impurities, such as moisture, dust, etc. from the gas. Subsequently, the gas is conducted into the first primary compression stage with the compressors 3a and 3b which are driven by gas turbines 4a and 4b, respectively. The fuel for driving the gas turbines 4a and 4b is removed from the gas line 1a or 1b, respectively, in a manner not illustrated in detail. The compression taking place in the compressors 3a and 3b increases the temperature of the gas. This temperature is again reduced by a subsequently arranged heat exchanger 5a, 5b which is preferably constructed as an air/gas heat exchanger.
The gas cannot yet be returned to the pipeline 1a, 1b because cooling by the heat exchange cannot be carried out to a temperature which is low enough. This is because the external temperatures of the air are too high during the summer operation and, consequently, the temperatures of the cooling agent are too high. Since the valves V 4a and V 4b , in the gas pipeline 1a, 1b are closed, the compressed gas flows into the connecting pipeline L 2a , L 2b and is conducted into a second primary compression stage with the compressor 6. For this purpose, the connecting pipelines L 2a and L 2b lead into a common supply line (line L 3 ) of the compressor 6. This line L 3 can also be connected directly to the purifying units 2a, 2b through the connecting pipelines L 1a and L 1b . However, during summer operation, these connections are locked by the valves V 11 and V 1a , V 1b . The compressor 6 is driven by a gas turbine 6 which, as is the case in the gas turbines 4a, 4b of the first primary compression stage, removes a portion of the gas from the gas pipeline 1a or 1b to be used as fuel. Immediately following the compressor 6, the line L 3 branches and leads to an additional compression stage with compressors 8a, 8b (booster compressors) which are connected in parallel and raise the pressure of the gas to a previously determined excess pressure. Following the additional compressors 8a, 8b, the compressed gas which has been heated as a result is again conducted to a heat exchanger 10 (preferably air/gas heat exchanger) for cooling the gas to a temperature corresponding to the ambient temperature. The line L 3 can also be switched in such a way that a direct connection between the compressor 6 and the heat exchanger 10 is obtained. However, in the case of summer operation shown in FIG. 1, this direct connection is locked by a valve V 5 . After leaving the heat exchanger 10, the line L 3 branches into supply pipelines L 4a and L 4a which lead to expansion turbines 9a and 9b. In the expansion turbines 9a and 9b, the gas is expanded from the excess pressure to the nominal pressure of the pipeline 1a, 1b while simultaneously performing work.
As a result, the gas is cooled to such an extent that it can be returned behind the closed valves V 4a and V 4b at the required nominal pressure and the desired nominal temperature to the pipeline 1a and 1b. In the illustrated embodiment, the expansion turbines 9a and 9b are coupled to the additional compressors 8a and 8b, and they meet the drive energy demand of these compressors. The heat exchanger 10, as is the case in the heat exchangers 5a, 5b, is constructed as a gas/air cooler, can also be connected directly through the pipelines L 5a and L 5b to the two pipeline strands 1a, 1b. However, during summer operation, this connection is closed by the valves V 3 and V 2a , and V 2b .
With respect to the actuation of the individual valves and the control of the compressors and the turbines, the entire compressor station is controlled by an electronic control system, not illustrated in FIGS. 1 and 2.
In accordance with a useful feature of the present invention, the compressor station would not be constructed in the manner schematically illustrated in FIG. 1 for simplicity stake. Rather, instead of single compressors, each of the two primary compression stages would have several compressors connected in parallel. For example, each pipeline strand 1a, 1b would have in the first primary compression stage three primary compressors 3a and 3b with a stand-by machine, i.e., altogether 2×(3+1) primary compressors 3a, 3b (in a 56 inch double gas line at 75 bar operating pressure with 16 MW units and at 100 bar operating pressure with 25 MW units), wherein corresponding gas turbines 4a, 4b are provided as drive units. A smaller number of primary compressors 6 (connected in parallel) is sufficient in the second primary compression stage because the pressure increase effected up to then also results in a corresponding volume reduction of the compressed gas. For example, in view of the above-mentioned equipment of the first primary compression stage, it would be useful to have four primary compressors 6 and an additional stand-by machine, i.e., altogether five compressors 6.
Instead of the expansion turbines 9a, 9b, it is also possible to use simple throttling devices for pressure reduction. However, this would mean that the temperature decrease of the gas resulting from the pressure reduction would be substantially less, i.e., for obtaining the same final temperature, under otherwise the same conditions the excess pressure would have to be even higher. In addition, no drive energy could be recovered and, therefore, the specific energy consumption of the compressor station would be accordingly higher. Therefore, the use of expansion turbines is preferred. However, if the expansion turbines are not used, it is apparent that the excess pressure can be produced in the transition phase only in two stages. As is the case in the three-stage compression using two primary compression stages and an additional compression stage, it is preferred to provide compressors 3a, 3b and 6 which have approximately the same pressure ratio in order to make it possible to use compressors which are as much as possible of the same construction.
When the outside temperatures (winter operation) are sufficiently low, cooling of the gas by pressure expansion is no longer necessary. As FIG. 2 shows, the present invention provides that during the cold season the compressor station is operated differently by switching the valves to essentially obtain a parallel operation of the compressors. The valves V 1a , V 1b , V 2a , V 2b , V 3 , V 4a , V 4b , V 5 , are all open and, in order to simplify FIG. 2, are not shown in FIG. 2.
After flowing through the heat exchangers 5a, 5b the gas compressed in the primary compressors 3a, 3b to the nominal pressure of, for example, 75 bar or 100 bar, can already be supplied at a temperature of below 0° C. to the gas pipeline 1a, 1b.The compressors 3a, 3b can produce the required throughput quantity together with additional units of the compressor 6 because the latter, contrary to the summer operation, can produce a portion of the required flow rate since they are connected in parallel. For this purpose, the gas having a low entry pressure reaches through the pipelines L 1a , L 1b , L 3 the compressor or compressors 6 in which the gas is compressed in one compression step to the required nominal pressure. The additional compressors 8a, 8b are switched off during winter operation by closing the valves V 7a , V 7b , V 8a , V 8b . As is the case in the primary compressors 3a, 3b, the compressed, heated gas is initially conducted for cooling to the required exit temperature into the heat exchanger 10 and is then returned through the lines 5a, 5b into the gas pipeline 1a, 1b. The connecting pipelines L 2a , L 2b and L 4a , L 4b are closed by the valves V 6a , V 6b , V 12a , V 12b and V 9a , V 9b , V 10a , V 10b which are not illustrated in FIG. 1. For example, during normal winter operation, 2×3 compressors 3a, 3b of the first primary compression stage and two parallel compressors of the second primary compression stage may be in continuous operation. In addition, a stand-by machine is available at each pipeline strand 1a, 1b and even three stand-by machines are available in the parallel second primary compression stage. These stand-by machines can be put into operation in case of interruptions or for the purposes of maintenance without reducing the throughput quantity. The above-described configuration is particularly useful for double-strand long-distance pipelines having a diameter of 56 inches and operated at a pressure of 100 bar with the use of 25 MW turbine sets or at 75 bar with the use of 16 MW turbine sets.
The effectiveness of the method according to the present invention under the conditions of summer operation (about three to four months of the year) becomes clear from the following example which is described with respect to the configuration of the arrangement shown in FIG. 1.
It is assumed that natural gas enters the purifying units 2a, 2b at the pipeline beginning at a production source from a separation plant with a temperature of approximately 15° C. and a pressure of approximately 50 bar. The nominal entry temperature into the pipeline 1a, 1b for further transportation is at most 0° C. The required pipeline pressure results as a function of the required throughput quantity. When the natural gas is compressed in the primary compressors 3a3b, it is heated to approximately 60° to 80° C. (corresponding to the pressure ratio in the compressor) and is then cooled to 25° C. in the air/gas heat exchangers 5a, 5b. The heat exchangers 5a, 5b and the pipelines within the compressor station result in a pressure loss of about 2 bar. A further compression in the subsequent primary compressor 6 produces an intermediate pressure, which causes the temperature of the natural gas to increase to approximately 50° to 60° C. The subsequent additional compressors 8a, 8b increase the pressure further to the desired final pressure or excess pressure which causes a temperature rise to about 80° C. Immediately subsequently, the compressed gas is again cooled in the heat exchanger 10 to a temperature of about 25° C. and the gas is then expanded in the expansion turbines 8a, 8b to the pipeline pressure, for example, 75 bar. As a result, the compressed natural gas has a temperature of approximately -5° C. to ±O° C. when entering the gas pipeline. The respective expansion pressure is determined by the ambient temperature and the throughput quantity through the line.
Because of the recovery of drive energy in the expansion turbines, the quantity of energy required for such a compressor station is not higher than in a comparable compressor station using conventional re-cooling technology on the basis of a closed propane cooling cycle. The important aspect is the fact that the investment required for a plant according to the present invention is substantially lower, approximately by 40 to 45 % percent than for a plant utilizing conventional re-cooling technology. This not only results in an increase of the availability of the overall plant, but also in a reduction of the risk of accidents due to the fact that re-cooling units are not present.
The invention is not limited by the embodiments described above which are presented as examples only but can be modified in various ways within the scope of protection defined by the appended patent claims.
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A method and an arrangement for compressing gas in a compressor station for a gas pipeline, especially in areas of permanent frost, wherein the gas is supplied in the gas pipeline to the compressor station at an entry pressure and the gas is returned to the pipeline for further transportation in the pipeline at a desired exit temperature and at an exit pressure which is higher than the entry pressure. The gas is initially compressed at least during individual time intervals to an excess pressure which is substantially higher than the desired exit pressure. The compressed gas is then cooled by heat exchange to a temperature above the desired exit temperature. Finally, the gas is further cooled to the desired exit temperature by expanding the gas from the excess pressure to the exit pressure.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to office furniture systems and more particularly to a hinged panel forming a part of the office furniture system. In one of its aspects, the invention relates to a hinged panel which is capable of being supported in an open position by a support stand which extends from the hinged panel to a lower panel or support surface forming part of the wall panel structure.
2. Description of the Related Art
Office furniture systems such as that disclosed in Kelley, U.S. Pat. No. 4,685,255 typically utilize a number of wall panel structures having communication and power wiring disposed therein for purposes of providing power and telecommunications hookups at individual work stations within the overall office furniture system. It is well known in the art that easy access to these telecommunication and power cables is needed for maintenance purposes once the office furniture system is put in use.
An easy method of providing access to such telecommunication and power cables is to position the cables or wires behind a hinged panel (e.g., at waistline level) which is capable of being raised for gaining access to the wiring or cabling disposed behind the hinged panel. Such hinged panels are often placed a few feet above the floor for providing easy access to telecommunications and electrical cabling at a convenient height. For example, the Kelley patent discloses a movable panel (FIG. 5) having a hooked clip which engages a slot in the panel support structure and a spring clip which engages a retainer spring mounted to the wall support structure. The hooked clip is positioned near a bottom portion of the panel and the spring clip is positioned at an upper portion of the panel. The Kelley patent also discloses a wire management panel positioned near the bottom of the wall panel structure. This panel is shown in FIG. 4 of the Kelley patent and comprises a hinged cover 82 having an inwardly directed flange 86 and a downwardly-extending projection 86a which is snap-fit with a retainer 92 for holding the hinged cover 82 in place.
Tenser et al., U.S. Pat. No. 4,535,577 discloses a wire management panel mounted to a steel frame of a wall panel support structure by clips extending downwardly beneath a lower portion of the panel, and by clips extending upwardly from an upper portion of the panel. The clips fit behind frame portions of the steel support structure. A sealing lip 32 extends between a lower portion of the wire management panel and the upper portion of a decorative panel disposed below the wire management panel. The sealing lip 32 provides a flexible closure, wherein a wire can pass between the wire management panel and the lower decorative wall panel. The Tenser et al. patent also discloses in FIGS. 8 and 10 a hinge 253 for securing the decorative panel 252 to an upper support member 254.
Propst et al., U.S. Pat. No. 4,372,629 discloses a hingedly mounted wire cover 22 (FIG. 3) for a desk which includes a wire brush 40 having a plurality of bristles extending from the cover to the desk to permit wires to pass therethrough.
It is known to provide a panel hinged to a frame in a modular wall system wherein the hinges include springs to bias the panel to a closed position. However, it has become apparent that there is a need to occasionally hold a wire management cover panel (sometimes called a "tile") in an open position to facilitate access to the wire management system. Hinged panels of the prior art must be held open manually to gain such access. With this need in mind, the present inventor has discovered that such a hinged panel can be provided with structure to enable the panel to be retained in an open position without manually holding it.
SUMMARY OF THE INVENTION
According to the invention, a panel is provided for covering a wire raceway in a modular wall structure. The panel comprises a surface having a first edge, a second edge, and opposite side edges extending between the first and second edges. A hinge is mounted on the surface adjacent the first edge for hingedly mounting the panel to the wall structure. Thus, the panel is moveable between a closed position where the surface encloses the wire raceway, and an open position where the wire raceway is exposed. The panel also includes a support member pivotably mounted to the surface for movement between a retained position and an engaging position. The support member has a pedestal which is adapted to engage the wall structure to maintain the panel in the open position when the support member is in the engaging position.
Preferably, the support member is pivotably mounted to a bracket disposed on the surface of the panel away from the first edge. The support member comprises an elongated shaft having an arm extending at a predetermined angle from the shaft. The bracket has a shackle which is disposed at the same angle relative to the second edge. The arm is received in the shackle so that when it is pivoted to the retained position, the shaft is substantially parallel to the second edge.
In one aspect of the invention, the pedestal has an indentation. In another aspect of the invention, the panel comprises a retaining clip on the surface which is adapted to receive and maintain the support member in the retaining position.
Preferably, the panel includes a stop to limit movement of the support member beyond the engaging position. Preferably, the stop is a pin extending from the support member and adapted to abut the surface when the support member is in the engaging position.
In another aspect of the invention, an improvement is provided in a panel for covering a wire raceway in the partition of a modular office divider system. The wire raceway typically extends horizontally between the edges of the partition and the panel is typically pivotally mounted to the partition for movement between a closed position enclosing the wire raceway and an open position exposing the wire raceway. The improvement comprises a prop mounted to the panel with the prop being adapted to maintain the panel in the open position. Preferably, the prop comprises a support member pivotably mounted to the panel for movement between a retained position and an engaging position. The support member has a pedestal adapted to engage the partition to maintain the panel in the open position when the support member is in the engaging position.
Typically, the panel is mounted to the partition by means of a hinge. Preferably, the hinge comprises a mounting plate which is securely fixed to the partition. An L-shaped member extends perpendicularly from the mounting plate and the L-shaped member has a first aperture. A clip is provided which has two spaced legs and a web connecting the legs. The web has nonparallel sides, and the legs extend substantially perpendicularly from the nonparallel sides. One of the legs is securely mounted to a flange on the panel, and the other of the legs is securely mounted to an adjacent surface of the panel. The web has a second aperture. In this construction of the hinge, the first aperture and the second aperture are in registry, and a pin extends through the first and second apertures so that the panel can be pivoted relative to the partition about the pin.
In yet another aspect of the invention, a bearing is disposed between the L-shaped member and the web of the hinge. Preferably, the bearing is a polymer washer. Also, in a preferred embodiment, the pin comprises a plastic expandable bolt which is elastically deformed.
It will thus be seen that the present invention meets the existing need for providing a structure to maintain a hinged panel on a partition in an office furniture system having electrical wire management capability in an open position for easy access to the wire management components.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be described with reference to the drawings in which:
FIG. 1 is a perspective view of a hinged panel used in connection with a wall panel structure, wherein the hinged panel is supported in an open position;
FIG. 2 is a perspective view of a back surface of the hinged panel of FIG. 1;
FIG. 3 is an enlarged, exploded, perspective view of a hinge assembly which forms a part of the hinged panel;
FIG. 4 is an enlarged, exploded, perspective view of a support stand assembly which forms a part of the hinged panel; and
FIG. 5 is a sectional view taken along lines 5--5 of FIG. 1.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
It is well known in the prior art that a hinged panel can be used as part of a wall panel structure in an office furniture system especially to cover wire raceways, thereby providing easy access to telecommunication and power components. However, a hinged panel 12 of the present invention enjoys an advantage over the prior art hinged panels because it includes a novel hinge 50 and a support stand assembly 30 acting as a pedestal for holding the panel 12 in an open position. In the following description of the preferred embodiments, the hinged panel will be described with reference to a wall panel structure. However, the invention is understood to have a somewhat broader application, since it can be used in connection with other structures within an office furniture system. For example, the hinged panel 12 could be used with a desk and could be mounted so that when closed, the hinged panel 12 would be flush with a top surface of the desk.
Referring to FIG. 1, an office furniture system 10 comprises decorative wall panels 11 (which can be modular) with the hinged panel 12 placed between the panels 11. The hinged panel 12 is generally rectangular and has a top 14, two sides 16 and a bottom 18. Mounted to each side 16 are long and slender wipers 24 which have a flexible construction. The wipers 24 are preferably formed of a thermosetting rubber. Mounted to the bottom 18 of the hinged panel 12 is a brush 26 having bristles 28. The hinged panel 12 includes two openings 22 which permit access to electrical components when the hinged panel is in a closed position. For example, electrical outlets (not shown) can be disposed in a wire management channel 23 in position to be aligned with the openings 22 when the hinged panel 12 is in the closed position in a manner disclosed by U.S. Pat. No. 4,685,255 to Kelley which is incorporated herein by reference. Thus, electrical plugs can be inserted into the electrical outlets by a user of the office furniture system 10 even when the hinged panel 12 is in the closed position. The hinged panel 12 further comprises the support stand assembly 30 which is used to support the hinged panel 12 in the open position when one needs to gain access to the wire management channel 23.
Referring to FIG. 2, a back surface 48 of the hinged panel 12 has two hinges 50 mounted near the wipers 24 and adjacent the top 14 of the hinged panel 12. The structure of the hinge 50 is explained in further detail below. Also mounted on the back surface 48 of the hinged panel 12 is the support stand assembly 30. The support stand assembly 30 will also be described in further detail below.
Referring to FIG. 3, the hinge 50 comprises a mounting plate 52 and a clip 54. The mounting plate 52 comprises a planar leaf 56 having a generally rectangular shape and having two holes 58 disposed therein. The holes 58 are adapted to receive fasteners 60 to secure the mounting plate 52 to a vertical support member 63 (see FIG. 5) which forms the support structure for the wall panel. Preferably, the fasteners 60 comprise conventional self-tapping screws. Alternatively, the fasteners 60 can include bolts received in holes of the wall panel support structure. Nuts can be placed on the opposite side of the wall support structure and can threadably receive the bolts. Further, as shown in FIG. 5, one or both fasteners 60 can comprise a spacer 65 adapted to receive a long screw or bolt 67. The spacer 65 acts as a stop for the hinged panel 12 when the panel is in the closed position. In such position, the backup of the panel will contact the head of the bolt 67, thus maintaining a front surface of the panel even with the adjacent panels 11.
Referring again to FIG. 3, the mounting plate 52 further includes an L-shaped member 64 extending perpendicularly from an edge 62 of the mounting plate 52. The L-shaped member 64 includes a short leg 66 integral with a long leg 68, the legs 66, 68 forming the L-shape of the L-shaped member 64. At an opposing end of the long leg 68 (opposite the short leg 66), the long leg 68 ends in a round 70. The long leg 68 has an aperture 72 disposed therein adjacent the round 70.
The clip 54 includes two rectangular leg members 80 and a trapezoidal-shaped member 82 integrally mounted to both rectangular leg members 80. Referring to FIG. 5, one rectangular leg member 80 is mounted to a flange 144 of the hinged panel 12, and one rectangular leg member 80 is mounted to a segment 146 of the hinged panel 12. Further, the rectangular leg members 80 are mounted on the back surface 48 of the hinged panel 12 near the top 14. Preferably, the rectangular leg members 80 are spot welded to the hinged panel 12.
Referring again to FIG. 3, the trapezoidal-shaped member 82 includes an aperture 88. A pin 90 is used to mount the mounting plate 52 to the clip 54. The pin 90 is received through aligned apertures 72, 88, with a bearing member 76 disposed between the L-shaped member 64 and the clip 54. The bearing member 76 is preferably a washer formed of a polymer material to facilitate pivotable movement of the clip 54 relative to the mounting plate 52. The pin 90 can be a bolt with a nut threaded onto the end thereof. However, the pin 90 preferably comprises a plastic, expandable bolt which anchors itself so that once inserted through the apertures 72, 88, the mounting plate 52 cannot be separated from the clip 54 without destroying the pin 90.
The support stand assembly 30, as shown in detail in FIG. 4, comprises a swivel bracket 102, a support stand 118 and a conventional U-shaped clip 104. The swivel bracket 102 comprises a rectangular portion 106 and a rectangular portion 108 that has a triangular cut-out. Because the rectangular portion 108 includes a triangular cut-out, a beveled edge 110 is thereby formed. The beveled edge 110 preferably extends in a direction 29° away from the horizontal edge of the rectangular portion 108. A shackle 112 is disposed between the rectangular portions 106, 108 and is integral with the rectangular portions 106, 108, thus forming a unitary structure for the swivel bracket 102.
The support stand 118 preferably comprises a long cylindrical shaft, which can be either hollow or solid. The support stand 118 includes a long, straight leg 119 having an arm 116 mounted at one end thereof. The arm 116 has a pin 114 mounted to it which extends in a substantially perpendicular direction away from the arm 116. The opposite end of the leg 119 includes a pedestal 120 having an indentation 122 therein. The arm 116 of the support stand 118 is rotatably mounted within the shackle 112 of the swivel bracket 102. The support stand 118 can be rotated roughly 90° so that the pedestal 120 of the support stand 118 extends away from the back surface 48 of the hinged panel 12 and the leg 119 is perpendicular to the back surface 48.
Referring to FIG. 5, the support stand 118 can only be rotated roughly 90° because the pin 114 acts as a stop and abuts the back surface 48 of the hinged panel 12 after the support stand 118 has been rotated roughly 90°. As shown in FIGS. 2 and 4, the leg 119 of the support stand 118 can be retained within the U-shaped clip 104. The support stand 118 preferably is formed of a ten gauge steel wire material.
Referring to FIG. 5, the brush 26 includes a brush holder 130. The brush holder 130 has the same cross-sectional shape as a chair. In other words, the brush holder 130 includes a seat 132 and a back 134 mounted to the seat 132 and extending away from the seat 132 in a perpendicular direction. The brush holder 130 also includes two legs 136 mounted to the seat 132 and also extending in a direction perpendicular to the plane of the seat 132 but extending in an opposite direction and away from the back 134. The legs 136 include flanges 138 which extend inwardly toward each other. Thus, the seat 132, the legs 136 and the flanges 138 of the brush holder 130 form a U-shaped channel 140 which is adapted to receive the bristles 28 of the brush 26. The brush 26 further includes double sided adhesive tape 142 to mount the brush holder 130 to the hinged panel 12 near the bottom 18.
FIG. 5 also illustrates the shape of the top 14 of the hinged panel 12. As can easily be seen, the top 14 includes the flange 144 which extends rearwardly (away from the top surface 46 of the hinged panel 12) in a direction perpendicular to the segment 146 of the hinged panel 12.
In operation, the hinged panel 12 according to the present invention can rest in two positions, the open position as shown in FIG. 1 or the closed position (not shown) wherein the top surface 46 (FIG. of the hinged panel 12 is generally flush with surfaces 15 (FIG. 1) of the decorative wall panels 11. If one desires to gain access to telecommunications cabling or electrical cabling in the wire management channel 23, the hinged panel 12 can be manually opened so that the bottom 18 of the hinged panel 12 moves away from the decorative wall panel 11 disposed below the hinged panel 12. Such movement of the hinged panel 12 takes place because the clip 54 rotates relative to the mounting plate 52 about a longitudinal axis of the bolt 90.
Once the hinged panel 12 is manually opened, the support stand 118 can be manually released from the U-shaped clip 104, the support stand 118 rotated about 90° so that the pedestal 120 of the support stand 118 is adjacent an upper and outermost ledge 34 of the decorative wall panel 11 disposed below the hinged panel 12. The support stand 118 should be positioned so that the indentation 122 of the support stand 118 rests against the ledge 34 of the decorative wall panel 11 disposed below the hinged panel 12.
The hinged panel 12 can be lowered to a closed position by slightly raising the bottom 18 of the hinged panel 12 and then rotating the pedestal 120 of the support stand 118 back to its original position adjacent the back surface 48 of the hinged panel 12 and placing the leg 119 of the support stand 118 within the U-shaped clip 104. The hinged panel 12 can then be manually lowered to its closed position.
When the hinged panel 12 is in its closed position, the bristles 28 preferably extend to a point such that they are flush with a top surface 32 (FIG. 1) of the decorative wall panel 11 disposed below the hinged panel 12. Electrical wiring or telecommunications cabling can extend from the wire management channel 23, through the bristles 28 of the brush 26, and outside of the wall panel structure. For example, as shown in FIG. 1, a telephone 150 can be placed on a desk 152 such that a telephone cord 154 attached to the telephone 150 can extend through the bristles 28 of the brush 26 and into the wire management channel 23.
The wipers 24 of the hinged panel 12 conceal wiring or cabling which passes from one wall panel structure to an adjacent wall panel structure. Typically, the wiper of the first wall panel structure will slightly overlap the wiper of the adjacent wall panel structure so that any wiring or cabling which passes from one wall panel structure to the adjacent wall panel structure cannot be seen.
The hinged panel 12 according to the present invention is preferably used as a wire management panel to conceal and provide ready access to telecommunications cabling, electrical wiring, or electrical receptacles in the wire management channel 23. The hinged panel 12 of the present invention is advantageous because it can be supported in the open position by the support stand 118 when one needs to gain access to the wire management channel 23.
Reasonable variation and modification are possible within the spirit of the foregoing specification and drawings without departing from the scope of the invention. For example, the hinged panel 12 need not include openings 22 for electrical outlets, and the hinged panel 12 could include more than two openings 22 for electrical outlets or for other purposes. Furthermore, the support stand 118 need not be shaped exactly as shown in the accompanying drawings since it is clearly contemplated that other support stands could be used which would accomplish the same function of the support stand 118 in substantially the same manner.
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A panel (12) is mounted to a partition (10) by a hinge (50). The panel (12) includes a support member (118) which is pivotably mounted to a bracket (102) on the panel (12). The support member (118) includes a pedestal (120) which is adapted to engage the partition (10) to hold the panel (12) in an open position.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part of U.S. patent application Ser. No. 08/070,949 filed Jun. 4, 1993 for Guide System for Vertically Moveable Flexible Door.
This application is also related to U.S. patent application Ser. No. 07/919,035 filed Jul. 24, 1992 for Closure Assembly for Structural Members now U.S. Pat. No. 5,351,742 issued Oct. 4, 1994, which is a continuation-in-part of U.S. patent application Ser. No. 07/729,696 filed Jul. 15, 1991 for Closure Assembly for Structural Members now U.S. Pat. No. 5,163,495 issued Nov. 17, 1992 which is a division of U.S. application Ser. No. 07/535,101 filed Jun. 8, 1990, now U.S. Pat. No. 5,131,450 issued Jul. 21, 1992.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention generally relates to a damage minimizing closure door that is moved vertically between open and closed positions in which the door is flexible and a guide assembly is mounted on the side edges of the doorway for receiving and guiding the side edges of the flexible door during vertical movement. The flexible door or curtain and the guide assembly include unique features which enable the side edges of the curtain to separate from the guide assembly upon being impacted by an externally applied force, such as by a vehicle, without damaging the curtain or guide assembly and also enabling the side edges of the curtain to be easily reinserted into the guide assembly.
2. Description of the Prior Art
Vertically disposed doors which move between open and closed positions are well known as are such doors or curtains constructed of flexible material with guide assemblies along the side edges of the opening receiving, retaining and guiding the side edges of the curtain. My U.S. Pat. Nos. 5,131,450 issued Jul. 21, 1992 and 5,163,495 issued Nov. 17, 1992 and my copending U.S. applications Ser. Nos. 08/070,949 and 07/919,035 disclose this type of door.
As indicated in the above patents and applications when a flexible door or curtain is used as a vertically movable door, it is necessary to provide a guide structure along the side edges thereof for retaining the side edges in a slot-like structure during vertical movement of the flexible door or curtain. Also, it is desirable to provide a structure which enables the side edges of the flexible curtain to separate from the guide structure in the event the flexible curtain is subjected to an excessive impact force such as a vehicle striking the door but withstand wind or air pressure without disengagement from the guide structure. However, the prior art does not disclose a structure equivalent to the unique features of the present invention which guides the side edges of the flexible curtain, enables the side edges to separate from the guide structure upon excessive impact force and enables the side edges of the curtain to be easily reinserted into the guide structures thereby avoiding damage to the flexible curtain in the event of excessive impact forces engaging the flexible curtain.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a vertically opening and closing flexible door or curtain provided with a guide structure along the side edges of the door opening with cooperating structure on the side edges of the flexible curtain and on the guide structure to facilitate vertical movement of the flexible curtain, provide a single or double windlock at the side edges of the flexible curtain and enable the side edges of the flexible curtain to be disengaged from the guide structure in the event of excessive impact force on the flexible curtain and enable the side edges of the flexible curtain to be quickly and easily reinserted into the guide structure after disengagement therefrom.
Another object of the invention is to provide a guide system as defined in the preceding object in which the side edges of the flexible curtain are provided with a single or double windlock in the form of a lateral projection or projections which engage with a windbar or windbars on the guide structure in which the windbar or windbars are constructed to enable separation from the guide structure which enables the curtain to disengage from the guide structure when the curtain receives excessive impact force.
A further object of the invention is to provide a guide system for a flexible curtain which includes a guide channel having a pair of spaced, generally parallel flanges with one or both flanges including a windbar releasably mounted thereon and associated with a windlock or windlocks on the edge of the flexible curtain to enable separation of the curtain from the guide channel without damage to the curtain or the guide channel in the event of an excessive impact force coming into contact with the curtain.
Still another object of the invention is to provide a damage minimizing, low maintenance door which may include a roll up door mounted on a barrel or drum across the upper end of a doorway or in the form of a vertical lift door in which the door moves vertically completely above the upper edge of a doorway with various mechanisms being provided to facilitate movement of the door or flexible curtain between open and closed positions.
A still further object of the invention is to provide a guide system in accordance with the preceding objects in which the guide structure is provided with guides such as rollers or outwardly flared flanges forming a bell shaped guide at the top of the guide structure, weather stripping when required along each guide structure and across the top of the door opening and a bottom bar connected to the flexible curtain to provide an effective closure door for an opening with the closure door being either a roll up door or a full vertical lift door and the windlocks being one or two substantially continuous narrow strips along each side edge of the curtain.
An additional object of the invention is to provide a bottom bar which evenly distributes the weight of the bottom bar across the width of the curtain by the use of a strip attached adjacent the bottom edge of the curtain on which the bottom bar retainer sits and is retained thereby reducing the amount of bolts needed to distribute said weight.
A still further object of the invention is to provide a damage minimizing door which uses a power spring (clock type) as a counter balance to assist a motor or any other mode of operation chosen to raise the flexible curtain out of the opening.
These together with other objects and advantages which will become subsequently apparent reside in the details of construction and operation as more fully hereinafter described and claimed, reference being had to the accompanying drawings forming a part hereof, wherein like numerals refer to like parts throughout.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an elevational view of a roll up type vertically moving door illustrating the guide structure along each side of the flexible door or curtain.
FIG. 2 is a sectional view taken substantially along section line 2--2 on FIG. 1 illustrating the specific structural details of the roller type guide at the upper end of the guide structure.
FIG. 3, is a sectional view taken along section line 3--3 on FIG. 1 illustrating guide rollers at the top edge of the guide structure.
FIG. 4 is a sectional view taken along section line 4--4 on FIG. 1 illustrating the specific structure of the guide structure and edge of the curtain.
FIG. 4A is an enlarged sectional view of a portion of FIG. 4.
FIG. 5 is a sectional view taken along section line 5--5 on FIG. 1 illustrating the bottom bar construction connected to the bottom end of the flexible curtain.
FIG. 6 is an elevational view illustrating a full lift vertical door.
FIG. 7 is a top plan view thereof.
FIG. 8 is a sectional view taken along section line 8--8 on FIG. 6 illustrating the counterweight structure.
FIG. 9 is an elevational view illustrating a spiral spring assisted door which can be manually operated.
FIG. 10 is an elevational view, with portions in section, of the spring and its housing.
FIG. 11 is a sectional view taken along section line 11--11 on FIG. 10 illustrating details of the spring assembly.
FIG. 12 is a fragmental perspective view illustrating another embodiment of the guide and curtain.
FIG. 13 is a sectional view, on an enlarged scale, illustrating structural details of FIG. 12.
FIG. 14 is a perspective view of the segmental windlock.
FIG. 15 is an elevational view of the upper end of the guide structure illustrating a bell shaped guide.
FIG. 16 is a sectional view taken along section line 16--16 on FIG. 15 illustrating additional details.
FIG. 17 is an enlarged sectional view, similar to FIG. 4A, illustrating another embodiment of the invention in which double windlocks and windbars are provided.
FIG. 18 is a fragmental sectional view of the structure of FIG. 17 wound onto a drum and providing an interlocking relation between the windlocks.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIGS. 1-5 disclose one embodiment of the invention generally designated by reference numeral 10 which includes a flexible door or curtain 12 having sufficient length and width characteristics to form a closure for a doorway or opening 14 in a wall 16 of a building structure. The door 10 includes a roll up drum generally designated by reference numeral 18 oriented at the top of the opening 14, a guide structure generally designated by reference numeral 20 along each side edge of the opening 14 and receiving and guiding the side edges of the curtain 12 and the bottom of the curtain 12 is provided with a bottom bar generally designated by reference numeral 22.
The structural details of the guide structure 20 is illustrated in FIG. 4 and includes an elongated, rigid support member 24 in the form of an angle or other structural member having a flange 26 secured to the wall 16 by any suitable fastening structures 28. The support member 24 also includes an outwardly extending flange 30 perpendicular to the flange 26 which supports a continuous inwardly facing guide member 32 with the guide member facing the doorway or opening 14 and including an inner flange 34 and an outer flange 36 generally parallel thereto with the flanges being connected at one end by a bight portion 38 that is secured to the flange 30 by a plurality of fasteners 40 in the form of bolts or the like which extend through an opening in the flange 30 and into a threaded opening 42 in the bight portion 38 of the member 32 with the flanges 34 and 36 being spaced apart to provide a groove or channel 44 which receives a side edge of the curtain 12.
As illustrated in FIG. 4, the side edge of the curtain 12 is provided with a strip 46 bonded to one surface of the side edge thereof with the strip being relatively narrow in width and also narrow in thickness with the thickness of the strip 46 being generally the same thickness as the curtain 12 although this relationship may vary. The side edge of the curtain and the strip 46 thereon serves as a windlock when associated with the guide member 32 as set forth hereinafter. The end edge of the flange 36 has an elongated retaining strip or windbar 48 mounted thereon with the windbar being constructed of plastic material and including a recess 50 in the surface thereof which faces the end edge of the flange 36 with the recess 50 being generally cylindrical in configuration but opening toward the flange 36 for snap mounting engagement with a projection or lip 52 on the end edge of the flange 36 with the lip 52 being of corresponding generally cylindrical shape for snap engagement with the recess 50 in the windbar 48. As illustrated, the windbar or strip 48 includes an inner flange portion 54 positioned interiorly of the flange 36 and projecting into the space 44 to abuttingly engage and retain the strip 46 and thus the edge of the curtain 12 within the channel shaped space 44. The construction of the windbar or strip 48 provides a low coefficient of friction with the curtain 12 and edge strip 46 and will effectively guide and retain the side edge of the curtain in the channel shaped space in the guide member 32. When the curtain 12 is in closed position and is impacted with an excessive force such as when a vehicle strikes the curtain, the lateral outward force exerted on the side edge of the curtain is resisted by the inner edge of the flange 54 on the strip 48 abutting the edge of the strip 46 until the lateral force overcomes the resilient snap mounting engagement between the recess 50 and the strip 48 and the projection 52 on the flange 36 is overcome at which time the strip 48 separates from the flange 36 and the side edge of the curtain 12 can separate from the guide member 32 with no damage or minimal damage to the curtain and guide structure.
This structure enables the side edge of the curtain 12 to be reinserted into the channel shaped space 44 and the resilient plastic strip 48 reattached to the projection 52 on the flange 36 by merely pressing the strip back into place by snapping the recess 48 onto the projection 52.
As illustrated in FIGS. 4 and 4A, the inner flange 34 is sometimes provided with a longitudinal spacer strip 56 which engages the surface of the curtain 12 in opposed relation to a portion of the strip 46 with the spacer strip 56 cooperating to insure engagement of the strip 46 against the windbar 48 to provide a windlock for the curtain 12 between the curtain 12 and the guide member 32. The spacer strip 56 is used when a thinner than normal curtain 12 is used to close the doorway. When a standard thickness curtain is used, the spacer strip 56 is not required. The strip 56 is replaceable by the use of a projection 58 on the surface of the strip 56 remote from the curtain 12 received in a recess 60 in the inner surface of the flange 34. The strip 56 is also constructed of plastic material while the guide member 32 is constructed of metal such as aluminum or other rigid material. The flange 34 is also provided with a weather stripping member 62 extending along the inner surface of the flange 32 and secured thereto by fastener 64 with the outer end of the weather stripping 62 including a brush member 66 engaging the surface of the curtain 12 inwardly of the guide member 32 and windbar 48 as illustrated in FIG. 4 to further provide a sealing relationship between the curtain 12 and the guide structure 20.
FIGS. 2 and 3 illustrate further structural details of the door 10 including a cylindrical drum 68 having one end of the curtain 12 attached thereto and wound thereon during rotation of the drum 68 which is supported by shaft structure 70 journaled in enlarged support plates 72 attached to the upper ends of flanges 30 on the support structure 24 by the use of bolt type fasteners 74 extending through slot opening 76 in the plate 72 to enable some adjustment of the position of the drum 68.
The upper end of the guide structure 20 includes a pair of guide rollers 78 and 80 spaced from each other and rotatably supported on elongated fastener bolts 82 and internal spacer sleeves 84 and 86. The roller 78 includes a cylindrical external surface and the roller 80 includes a generally cylindrical external surface but which includes a radially outwardly offset end portion 88 which receives the strip 46 on the edge of the curtain 12 with the radially offset end portion 86 defining an abutment edge 89 engaging and guiding the inner edge of the strip 46 as illustrated in FIG. 3 during movement between the rollers 78 and 80 which are idler rollers with the external surfaces thereof being generally in alignment with the channel shaped recess 44 between the flanges 34 and 36 on the guide member 32 as illustrated in FIG. 2 thus guiding movement of the curtain 12 when it is being wound onto or off of the drum 68 thus guiding the curtain in relation to the guide structure 20 and specifically guiding the strip 46 into the channel shaped space 44. A weather stripping member 90 is mounted on a bracket 92 connected to the wall 16 above the doorway opening 14 and includes a weather seal brush 94 in engagement with the surface of the curtain 12 which faces the wall 16 which, together with the weather seal brushes 66 forms a complete seal along the top and side edges of the flexible curtain when the flexible curtain is in lowered or closed position.
FIG. 5 illustrates the construction of the bottom bar 22 which is a rigid structure connected to the lower end of the curtain 12 and terminates about an inch from the guide structure 20. The bottom bar 22 includes a pair of identical rigid members 95 and 96 each of which includes an indentation 97 in the inner surface. The indentation 97 includes a lip 98 which extends downwardly to engage an upturned lip 99 on a mounting strip 100. The mounting strips 100 carries and evenly distributes the weight of the bottom bar 22 across the width of the curtain 12 to keep the curtain taut and assist the downward travel of the curtain in the guide system along the side edges. The upturned lip 99 on each mounting strip 100 receives the downturned lip 98 and helps to retain the bottom bar 22 on the strips 100 which are secured to the curtain 12 such as by welding or sewing. Bolts 101 retain the bottom bar members 95, 96 on the mounting strips 100 and curtain 12 by clamping the members to the strips and curtain. The lower bottom portion of each of the members 95 and 96 is provided with a continuous cavity 102 extending therethrough capable of receiving one or more elongated weight members 103 in the form of elongated rods, cables or the like to vary the total weight of the bottom bar. The bottom edges of the members 95 and 96 have downwardly facing T-shaped grooves 104 receiving correspondingly shaped projection on a hollow, generally semicircular seal member 106 which sealingly engages the bottom surface or floor surface forming the bottom of the door opening 14 thus forming a seal for the bottom edge of the flexible curtain 12 where it engages the floor or bottom surface of the opening and the weight of the bottom bar will retain the flexible curtain 12 in a taut, straight line condition when the bottom bar 22 is spaced from the bottom surface 108 of the opening 14.
FIGS. 6-8 disclose a vertical lift door generally designated by reference numeral 110 and which includes a flexible door or curtain 112 guided by guide structures 114 which are the same in construction as the guide structures 20 in FIGS. 1-5 except that the guide structures 114 extend a vertical distance above the doorway 116 to enable the flexible curtain 112 to move vertically upwardly in a straight line condition until the bottom bar 118 is positioned in line with or above the doorway 116. The upper end of the guide structures 114 have a cable pulley or sheave 120 supported by a bracket structure 122 on the wall 124 with a cable 126 entrained over the pulley 120 with one end of the cable 126 extending downwardly along the outside of the upper portion of the guide structure 114 and being attached to a cable bracket 128 mounted on the upper edge of the flexible curtain 112. The other end of the cable 126 extends downwardly in spaced relation to the upper portion of the guide structure 114 and has a counterweight 130 attached thereto with the counterweight being vertically movably mounted in a vertically disposed guide tube 132 secured to the guide structure and wall structure in a manner to enable the counterweights 130 to balance or partially balance the weight of the flexible curtain or door to facilitate manual vertical movement of the flexible curtain 112 between open and close positions.
FIGS. 9-11 illustrate a manually operated roll up door 140 including a flexible curtain 141 and guide structures 142 and a bottom bar 143 which are the same as the structure illustrated in FIGS. 1-5 except that the drum or barrel 144 across the upper end of the door opening can be manually operated by a hand chain drive 145 at one end thereof or by a motor 146, gear box 147 and drive sprocket and roller chain 148 at the same end to drive shaft 149 which supports drum 144. An emergency release pull chain 150 enables the motor 146 or chain drive 145 to operate the shaft 149 and drum 144. If a hand chain operation is selected as the primary mode of operation, the motor 146, gear box 147 and chain drive 145 will be omitted. At the other end of the drum 144, a counterbalancing spring mechanism 151 which includes a spiral power spring 156 received in a housing or frame 154 with one end of the spring 156 connected to the housing or frame 154 and the other end connected to shaft 149. The spring housing 154 is supported from a mounting plate 152 attached to guide structure 142. The plate 152 includes lateral angle clips 153, preferably welded thereto, which support the hollow housing 154 by adjusting bolts 155 which interconnect the angle clips 153 on the plate 152 and angle clips 157 fastened around the outside circumference of the housing 154. A spiral power spring 156 is positioned in housing 154 with the outer end of the spring being secured to the housing 154 and the inner convolution secured to an end of the shaft 149 by a keyed casting 158. The barrel 144 and shaft 149 are supported by bearings 160 in plates 152. The spring counterbalance mechanism 151 supports and assists the manual movement of the flexible curtain 141 between open and closed positions thereby reducing the force necessary to open and close the door or curtain. The spring mechanism may be easily replaced to reduce maintenance costs and other types of springs typically used in the industry, such as a torsion spring enclosed in a barrel, can be used as a counterbalancing spring.
FIGS. 12-16 illustrate a modified guide structure 20 in which the flanges 34' and 36' flare away from each other and the bight portion of the channel shaped member 32' is omitted or separated from the flanges 34' and 36' thus enabling the flanges to be flared upwardly and outwardly to form a bell shaped upper end to the guide structure illustrated.
An optional structure for retaining the side edges of the door curtain in relation to the guide structure is illustrated in which the curtain is designated by reference numeral 161 having attached to the side edges thereof a segmental flexible, bendable and resilient windlock in the form of spaced angled tabs 162 attached to curtain 161 by fasteners 163 in a manner to enable the curtain to be wound onto a drum or barrel at the upper end. The guide structure includes flanges 164 and 166 defining a guide channel with the flange 166 being detachable by a bolt and nut arrangement 168. The flange 164 is provided with a stationary windbar or projection 170 which engages the curtain 161. As illustrated in FIGS. 13 and 14, the segmental tabs 162 are flexible and bendable and provided with memory or resilient characteristics sufficient to enable the tabs 162 to bend to a substantially straight condition in alignment with the curtain 161 to enable the curtain 161 to be separated from the guide structure by moving past the windbar 170. In this embodiment of the invention, the windlock formed by tabs 162 and side edge of the curtain 161 is reinserted into the guide structure by removing the nut and bolt fasteners 168.
FIGS. 17 and 18 illustrate an embodiment of the invention which includes a guide structure generally designated by reference numeral 180 supported by a bracket structure 182 attached to a wall 184 in the same manner as the embodiment of the invention illustrated in FIG. 4. The guide structure 180 includes a guide channel 186 including spaced, generally parallel vertical flanges 188 and 190 which are interconnected at one end by a bight portion 192. The bight portion 192 is secured to the supporting bracket 182 by fastening bolts or cap screws 194. The flanges 188 and 190 may be constructed as an extrusion of metal, plastic or the like and the flanges are spaced apart to receive a flexible door or curtain 196 with the side edge of the curtain 196 received between the flanges 188 and 190.
The side edge of the curtain 196 is provided with a strip 198 on the outer surface thereof and a strip 200 on the inner surface thereof which form double windlocks. As illustrated in FIGS. 17 and 18, the strips 198 and 200 are not aligned with each other with the strip 198 on the outer surface being spaced laterally inwardly from the edge of the curtain 196 slightly greater than the width of the strip 200 which is on the inner surface of the curtain 196 and which has its outer edge generally aligned with the side edge of the curtain 196.
The outer flange 190 has a longer lateral extent as compared to the inner flange 188 with each of the flanges including an inwardly offset end portion 206 terminating in a partially cylindrical end edge 208 for snap engagement with a windbar 210 in the form of a generally channel shaped member having an internal recess 212 for snap engagement with the edge 208 of the channels 188 and 190. As illustrated, the inner edge of each of the windbars projects inwardly from the flanges 188 and 190 and engage opposite surfaces of the curtain 196 in slightly staggered relation. Thus, the inner edge of the inner flange of each of the windbars is in the path of movement of the windlocks 198 and 200 when the edge of the curtain 196 is moved out of the guide channel with the snap engagement of the windbars 210 enabling the windbars 210 to be pulled off of the flanges 188 and 190 when the curtain is subjected to an excessive force such as an impact from a vehicle or the like. This structure operates in a manner similar to that illustrated in FIGS. 4 and 4A except that a double windlock is provided on the curtain 196 by the strips 198 and 200 and a double windbar is provided on the guide channel 186 by the windbars 210. As illustrated in FIG. 17, the partially cylindrical end edge 208 and the windbars 210 have a positioning projection and recess to orient the windbars in proper position which is also provided by the outer flange of the windbars including an inclined edge which engages the inclined surface of the offset portion 206 of the flanges. The staggered relation of the windbars enables sequential separation of the windbars from the flanges as the curtain moves outwardly from the flanges.
FIG. 18 illustrates the curtain wound on a drum 216 supported by a shaft 218 in which the stagger relationship of the windlocks or strips 198 and 200 provide an interlocking effect on the end portion of the convolutions of the curtain 196 when it is wound onto the drum thus maintaining the end edges of the convolutions of the curtain 196 in radial alignment when being wound on or unwound from the drum. This interlocking effect provides for proper orientation of the curtain as it is wound onto the drum or unwound from the drum with the relationship of the windlocks and flanges of the guide channel maintaining proper position of the side edges of the curtain during vertical movement with the windbars maintaining the windlocks within the guide channels to resist the forces of wind or air pressure differentials without separating the windbars. When the curtain is impacted such as by a vehicle or the like by an excessive force, the windlock strips 198 and 200 will pull the windbars 210 off of the edges of the flanges 188 and 190 thereby releasing the curtain before damage occurs. This also enables the curtain to be reassembled by inserting the side edge between the flanges 188 and 190 and reinstalling the windbars by snapping engagement with the partially cylindrical edges 208 of the flanges.
The foregoing is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described, and, accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention.
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A damage minimizing closure door that is moved vertically between open and closed positions in which the door is a flexible curtain and a guide assembly is mounted on the side edges of the doorway for receiving and guiding the side edges of the flexible door during vertical movement. A counterbalancing power spring is associated with the door to assist in raising and lowering the curtain. The flexible door or curtain and the guide assembly include unique features which enable the side edges of the curtain to move vertically in the guide assembly, resist wind forces and air pressure differentials when the door is closed or moving vertically and to separate from the guide assembly upon being impacted by an externally applied force, such as by a vehicle, with little if any damage occurring to the curtain or guide assembly.
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RELATED APPLICATION
This is a continuation application of International Patent Application PCT/EP01/08147, filed Jul. 14, 2001, designating the United States, and published in German as WO 02/08291 A2, which claims priority to German application number 100 34 607, filed Jul. 20, 2000.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is concerned, in a general manner, with stimulating cells and in particular with selectively activating receptors on the cell surface.
2. Description of the Related Art
It is well known that extracellular signals are transmitted through the plasma membrane by way of receptor proteins which are able to convert the extracellular binding of ligands into an intracellular biochemical event. In this way, cell surface receptors activate intracellular signal pathways which lead to different sites in the cell and induce particular events at these sites.
All cell surface receptors are transmembrane proteins or protein complexes which establish a connection between the inside and the outside of the cell. Many receptors undergo a defined change in the protein conformation when their respective ligand is bound. In the case of some receptor types, this change in conformation leads to an ion channel being opened while, in the case of other receptors, the change in conformation leads to the cytoplasmic region of the receptor being affected in such a way that it can associate with intracellular signal proteins and signal enzymes and activate these proteins and enzymes.
A crucial effect of ligands being bound to receptors is frequently that of multimerizing or crosslinking the receptor and thereby activating the intracellular signal cascade. Such a crosslinking of surface receptors can either be effected by the physiological ligands of the receptors or, for example, be effected in vitro using appropriate crosslinking antibodies.
For example, it has been demonstrated, in the case of lymphocytes, that, while it is not possible to stimulate specific antigen receptors as a result of binding F(ab′) fragments, which possess only one binding site, the receptors form clusters, and the cells are activated, as the result of binding (Fab′) 2 antibody fragments, i.e. fragments possessing two binding sites. However, a stronger reaction is achieved if lymphocytes are stimulated by intact antibodies which are bound to cells which carry receptors for the immunoglobulin Fc moiety. In other words, activation takes place when receptors are efficiently crosslinked by being bound to many identical antibody molecules which are provided by other cells which possess Fc receptors for the constant regions of the intact antibodies. The receptors are efficiently crosslinked by the antibodies which are immobilized in this way.
In vitro, such a crosslinking can, on the one hand, be achieved by the constant regions of antibodies which are bound to the receptors being crosslinked by way of protein A or by way of other antibodies which bind specifically to the constant regions of the antibodies which are bound to the receptors.
For example, it is known that the members of the TNF (tumor necrosis factor) family act as trimers and that the ligand induced trimerization of their receptors is the critical event in initiating signal transmission.
Dhein et al., INDUCTION OF APOPTOSIS BY MONOCLONAL ANTIBODY ANTI-APO-1 CLASS SWITCH VARIANTS IS DEPENDENT ON CROSS-LINKING OF APO-1 CELL SURFACE ANTIGENS”, the Journal of Immunology, volume 149, 1992, pages 3166-3173 report that efficient crosslinking of the APO-1 cell surface antigen leads to the induction of apoptosis. They show that, while apoptosis is induced in SKW6.4 cells when anti-APO-1 F(ab′) 2 fragments which are crosslinked by way of a sheep anti-mouse antibody bind to the APO-1 receptor, the binding of the F(ab′) 2 fragments on their own is insufficient to achieve this. The authors conclude from these results that the bivalency of the antibody, which thus possesses two binding sites for the APO-1 cell surface antigen, is insufficient for inducing apoptosis and that, on the contrary, efficient crosslinking of the APO-1 cell surface antigen is necessary in order to achieve this.
The sequence of the APO-1 antigen, and a monoclonal antibody directed against the APO-1 antigen are described in U.S. Pat. No. 5,891,434. This patent specification mentions that the anti-APO-1 antibodies can be used for treating tumors which the APO-1 antigen, with it furthermore being possible to induce apoptosis in different types of cells.
However, it is known that many cells in the body carry the APO 1 cell surface antigen, which means that administering an anti-APO-1 antibody to a tumor patient would lead not only to an attack on the tumor cells but also, in addition to this, to an attack on other, healthy and perhaps even essential cells which also carry the APO-1 surface antigen.
Against this background, the use of the known anti-APO-1 antibodies for treating tumor patients, for example, is only suitable under certain circumstances.
The TRAIL (TNF-related apoptosis-inducing ligand) receptors R1 and R2 represent another type of death receptor which is activated by crosslinking; see Griffith et al., “Functional Analysis of TRAIL Receptors using Monoclonal Antibodies”, The Journal of Immunology, volume 162, 1999, pages 2597-2605. The authors report that, while all the anti-TRAIL-R2 antibodies, and two of the anti-TRAIL-R1 antibodies, were unable to induce any lysis, or only able to induce minimal lysis, of TRAIL-sensitive melanoma cells when they were added to the cells in solution, these antibodies exhibited an increase in their lytic ability when they were immobilized on a culture plate such that they were able to ensure that the TRAIL-R1 and TRAIL-R2 death receptors were crosslinked.
Antibodies against the death receptors TRAIL-R1 and TRAIL-R2 also act nonspecifically on TRAIL-sensitive cells, which means that they are only of slight therapeutic value.
In addition to this, it is known that what are termed bispecific antibodies, i.e. antibodies which possess a specificity for a tumor-associated antigen and a specificity for a surface antigen on defensive cells of the immune system, such as macrophages, T-lymphocytes or natural killer cells, which cells are activated by way of this binding, can be employed in cancer immunotherapy for directing the activity of the defensive cells toward the particular target cells.
In a general manner, bispecific antibodies are antibodies which are able to bind two different epitopes and are monovalent for each epitope. They are prepared by oxidizing monovalent F(ab′) fragments to give an F(ab′) 2 fragment, by fusing two hybridoma cell lines to give hybrid hybridoma or quadroma cells, or recombinantly.
Jung et al., “Target cell-induced T cell activation with bi- and trispecific antibody fragments”, Eur. J. Immunol., volume 21, 1991, pages 2431-2435 describe the preparation of bispecific F(ab) hybrid fragments which are monovalent for each antigen. The reader is referred to this publication for further references to the preparation of bispecific antibodies.
The authors demonstrate that bispecific antibodies or fragments can be used to effect a target cell induced activation of T cells, by the antibodies on the one hand binding to the target antigen on the target cell and, on the other hand, binding to the CD3 and/or CD28 receptor on the T cell.
Segal et al., “Bispecific antibodies in cancer therapy”, Current Opinion in Immunology, volume 11, 1999, pages 558-562 also describe the use of bispecific antibodies for directing an effector cell to a target cell which it would not otherwise recognize. For this purpose, the bispecific antibodies bind to a surface molecule on the target cell and to a surface receptor on the effector cell.
Roosnek et al., “T cell activation by a bispecific anti-CD3/anti-major histocompatibility complex class I antibody”, Eur. J. Immunol., volume 20, 1990, pages 1393-1396 showed that a bispecific antibody which possessed specificity both for MHC and for CD3, both of which were expressed on T cells, was able to induce efficient proliferation of T cells whereas a mixture of the two original antibodies was unable to do this. The authors hypothesize that this synergistic effect is due to the anchoring of the T cell receptor/CD3 complex in the membrane being disturbed. In this connection, they make the assumption that the T cell receptor is unable to distinguish whether it is anchored to an antigen-presenting cell (APC) or to surface molecules within its own membrane. They therefore speculate that the T cell receptor/CD3 complex, which in vivo is triggered by antigens on another cell, reacts to changes in its mobility within the membrane.
However, the mechanism of this T cell receptor activation, which is restricted to certain T cell subpopulations, has remained unclear. The prior art has thus far assumed that this is a T cell receptor-specific effect which is probably due to the fact that, in addition to the T cell receptor, a coreceptor such as CD4 or CD8 is stimulated, with this coreceptor also generating a signal on stimulation, see Emmrich et al., Eur. J. Immunol., 18, 645 (1988).
SUMMARY OF THE INVENTION
In view of the above, an object underlying the present application is to provide a reagent which, in a general manner, restricts the stimulation of cell surface receptors to particular target cells.
According to the invention, this object is achieved by means of a multispecific reagent which possesses at least one first binding site for a cell surface receptor which requires multimeric ligand binding in order to be stimulated, and at least one second binding site for a target antigen, with the cell surface receptor and the target antigen being expressed on the same cell. The first binding site at its own does not stimulate/the cell surface receptor, to achieve this, the second binding site has to be bound to the target antigen. By this, only such cells are selectively killed which express both, the cell surface receptor and the target antigen.
The object underlying the invention is fully achieved in this way.
Thus, the inventor of the present application has perceived that cell surface receptors which require multimeric stimulation do not imperatively have to be crosslinked by way of immobilized antibodies or, for example, antibodies which are bound by protein A or are bound to other antibodies, and that, instead, bispecific antibodies, for example, are able, in a general manner, to induce a target antigen-restricted stimulation of the cell surface receptor.
In this way, it is possible to use the target antigen to select a particular cell type and to activate the corresponding cell surface receptor on this cell type. Consequently, of the two binding sites possessed by the reagent, one is responsible for the function, namely the cell surface receptor, while the other is responsible for the specificity, namely the target antigen restriction.
According to the inventor's findings, the cell surface receptors are also, and particularly, efficiently crosslinked when the two antigens are expressed on the same cell. This result is surprising insofar as it was not clear from the prior art in what way bispecific antibodies were able to ensure a crosslinking between a function receptor and a target receptor which was sufficient to trigger the function receptor even when the two receptors were expressed on the same cell.
From a variety of his own experiments, the inventor of the present application has deduced that it is possible, in this bispecific manner, to use various target antigens, which may also, but do not have to, have a signal function, to stimulate, for example, the death receptor APO-1 or antigen-presenting cells (APCs) by way of stimulating CD40 (another member of the TNF receptor family). This was not to be expected on the basis of the studies carried out by Roosnek et al. loc. cit. And Emmrich et al. loc. cit. but, instead, required extensive experimental verification.
In view of the above, the present invention according to a further object relates to a method for treating cells in which method the novel reagent is used to bring about a target antigen-restricted stimulation of the cell surface receptor.
Thus, a further object is a method for treating cells, each cell expressing a target antigen and a death receptor, comprising the step of contacting said cells with a bispecific reagent having at least a first binding site for said death receptor and a second binding site for said target antigen, said first binding site being selected such that it stimulates the death receptor only when the second binding site has bound to the target antigen, thereby bringing about a target antigen-restricted stimulation of the death receptors of said cells.
Using this method, it is now possible, for example, to stimulate death receptors on particular target cells in order, in this way, to selectively kill cancer cells or else to, within the content of an immunosuppression, bring about the apoptotic death of activated T cells which are expressing death receptors.
Cells only expressing the death receptor but not the target antigen are not killed by the novel reagent.
The novel reagent can also be used in a pharmaceutical composition together with a pharmaceutically acceptable excipient since, according to the invention, the restriction by way of the target antigen avoids the lack of specificity which is particularly harmful when using antibodies directed against death receptors.
The methods which can be used for selecting pharmaceutically acceptable excipients, formulations, etc., are described, for example, in the patent U.S. Pat. No. 5,891,434, which was mentioned at the outset and whose disclosure is hereby made part of the subject matter of the present application.
Preference is given, in a general manner, to the novel reagent being selected from the group: multispecific, preferably bispecific antibodies or their antigen-binding fragment F(ab′) 2 ; and a receptor ligand which is preferably prepared recombinantly.
The essential requirement which the novel multispecific reagent has to fulfil is that of providing two binding sites, namely one for antigen, a cell surface receptor and another one for a target antigen, with the receptor and the antigen being expressed on the same cell, and the first binding site for said cell surface receptor not stimulating said cell surface receptor at its own.
This can be brought about by specific antibodies or other antigen-binding fragments, using bispecific antibodies, trispecific antibodies or other multispecific antibodies or their antigen-binding fragments, or else by using an appropriate receptor ligand which is preferably prepared recombinantly.
The recombinant DNA technique makes it possible to synthesize different bispecific antibodies, namely tandem antibodies and diabodies. In the case of tandem antibodies, the gene fragments for two scFvs (single-chain antigen-binding proteins) are linked by way of a linker sequence and synthesized as one peptide. In the case of diabodies, two scFvs, which frequently tend to dimerize such that the variable region of the one light chain does not bind to the variable region of “its” heavy chain but, instead, to that of the second scFv molecule, without the regions being covalently linked, are expressed in one cell. In this way, it is possible to produce bispecific diabodies in which the DNA sequences for the variable regions of the light chains of the two scFv molecules to be combined are exchanged for each other in the expression vectors. After they have been synthesized, the variable regions of the antigen-specific light and heavy chains bind to each other and a recombinant antibody molecule possessing two different specificities is formed.
The fusion of different binding domains to the scFvs makes it possible to create a broad spectrum of possibilities for combining two scFvs to generate bispecific antibodies.
In a general manner, however, it can be emphasized that it is possible to use, as a reagent, any substance which binds selectively to several cell surface receptors on one cell, which means that the invention is not restricted to bispecific antibodies and bispecific receptor ligands.
In this connection, preference is given to the target antigen also being a cell surface receptor which requires multimeric ligand binding in order to be stimulated.
In this connection, it is advantageous if the target antigen is itself an activatable cell surface receptor such that the two cell surface receptors are activated and restricted simultaneously. In this way, it is possible, for example, to achieve a synergistic effect, as a result of the simultaneous stimulation of two cell surface receptors, on the cell which has thus been selected.
Preference is furthermore given to the surface receptor being selected from the group: death receptors, such as APO-1, TRAIL-R1 and TRAIL-R2; and receptors, such as CD40, which activate antigen-presenting cells (APCs).
This enumeration of the cell surface receptors is solely by way of example; the invention also includes other functional receptors which, by way of multimeric stimulation, elicit selected functions in the target cells.
Preference is furthermore given to the target antigen being selected from the group: tumor cell-specific cell surface antigen, T cell-specific cell surface antigen, CD markers generally, and cell-specific markers.
This enumeration is also solely by way of example; the invention encompasses the restriction of the multispecific reagent by any target antigens which are specific for a particular target cell.
CD markers, which characterize the different subpopulations of the leukocytes, for example, or their different development or differentiation stages, are particularly suitable for this purpose. However, the continually growing list of CD antigens also encompasses molecules which are to be found on other cell types, for example endothelial cells, nerve cells or fibroblasts; see, in this regard, Lexikon der Biologie [Encyclopedia of Biology], Spektrum Akademischer Verlag GmbH, Heidelberg, 1999, volume III, pages 323-329.
The multispecific reagent of the invention can in this way be employed universally by the function, which is stimulated by the first binding site, of the cell surface receptor being restricted by way of the target antigen.
When the cell surface receptor in the method for treating cells is a death receptor, it is then possible to induce target antigen-restricted apoptosis. This method can, for example, be employed in the immunotherapy of cancer.
Thus, when the target antigen in the new method is specifically expressed on tumor cells, it is only tumor cells which are selectively killed whereas other cells in the body which also contain the activatable cell surface receptor are not damaged since they lack the target antigen.
When, on the other hand, the target antigen is expressed specifically on T cells, it is then possible to selectively destroy the T cells which are expressing death receptors. This is advantageous, for example, in the context of immunosuppression in association with an organ transplantation.
When the target antigen is expressed specifically on antigen presenting cells, these APCs can be selectively stimulated if, in addition to the binding site for the target antigen, the multispecific reagent at least possesses a binding site for CD40.
In summary, it can be emphasized that it has for the first time become possible, as a result of the invention, to restrict the activation of particular cell surface receptors to particular target cells by using a reagent which possesses at least two binding sites, i.e. one for a cell surface receptor which is to be stimulated and a further one for a target antigen on the same cell, with this target antigen specifying the target cell.
Other advantages ensue from the description and the attached drawings.
It will of course be understood that the abovementioned features, and the features which are still to be explained below, can be used not only in the combinations which have in each case been specified but also in other combinations, or on their own, without departing from the scope of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the invention are depicted in the drawing and are described in more detail in the subsequent description.
FIG. 1 shows, in diagrammatic form, the binding of bispecific antibodies to two different antigens on the same cell: A) in a bicellular manner, or B) in a monocellular manner. 10 —target cell; 11 —cell surface; 12 —cell surface receptor; 14 —target antigen; 15 —bispecific antibody; 16 —Fab fragment of the bispecific antibody possessing a binding site for the target antigen 14 ; 17 —Fab fragment possessing a binding site for the cell surface receptor 12 ; 18 —Fc fragment.
FIG. 2 shows the selective killing of SKW6.4 cells after incubating for 16 hours with a bispecific antibody fragment having a specificity for CD20 and APO-1 whereas Jurkat cells are not killed.
FIG. 3 shows the selective killing of SKW6.4 cells and Jurkat cells by bispecific antibodies possessing specificity for APO-1 and different target antigens.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Example 1
Binding Bispecific Antibodies to Target Cells
FIG. 1 depicts target cells 10 on each of whose surfaces 11 a cell surface receptor 12 and a target antigen 14 are expressed.
A bispecific antibody 15 , whose Fab fragment 16 possesses a binding site for the target antigen 14 and whose Fab fragment 17 possesses a binding site for the cell surface receptor 12 binds to the target cells 10 . The Fc fragment is not involved either in the binding or in a crosslinking, for which reason it was possible to use antibody fragments lacking an Fc moiety in the experiments described below. The bispecific antibody 15 , which recognizes the two antigens 12 and 14 , binds to both antigens on the same cell.
The cell surface receptors 12 on the target cells 10 are only stimulated when the Fab fragment 16 is simultaneously able to bind to a target antigen 14 .
On the other hand, the possibility of the bispecific antibody 15 linking two target cells 10 with each other in a bicellular manner, as shown in FIG. 1A , cannot be ruled out. This means that, while, within one cell type, in which each cell 10 possesses the two antigens 12 and 14 , the bispecific antibody 15 can either bind unicellularly, as in FIG. 1B , or bicellularly, as in FIG. 1A , it leads, in either case, to the target antigen restricted stimulation of the cell surface receptor 12 which is present on the same cell as the target antigen 14 .
Various death receptors, such as APO-1, TRAIL-R1 or TRAIL-R2, can serve as cell surface receptor 12 while any cell surface antigens which can be used to achieve restricted stimulation of the cell surface receptor 12 can be employed as target antigen 14 .
In other words, the cell surface receptor 12 is only stimulated on those target cells 10 which either carry a target antigen 14 or which, in the case of bicellular binding, are located in the immediate vicinity of such a target cell 10 .
This general principle is now described below using the target antigen-restricted stimulation of the death receptor APO-1 as an example.
Example 2
Cell Lines Employed
The cell lines employed are SKW6.4 cells and Jurkat cells. SKW6.4 cells (ATCC: TIB 215) are derived from B-lymphocytes and express CD95 (APO-1) and are apoptosis-sensitive.
Jurkat cells (ATCC: TIB 152) are derived from T-lymphocytes and also express CD95 and are apoptosis-sensitive.
Both the cell lines are incubated in RPMI 1640 medium which is supplemented with 10 mM glutamate, 100 U/ml of penicillin, 100 μg/ml of streptomycin and 10% heat-inactivated fetal bovine serum (Sigma, Deisenhofen, Germany).
The APO-1 receptor (CD 95), which is expressed on both cell lines, was selected as the cell surface receptor while the CD markers CD2, CD5, CD19, CD20, CD28 and CD40 were selected as target antigens.
CD95 antibodies can be purchased from Santa Cruz Biotechnology, Santa Cruz, Calif. Monoclonal antibodies which are directed against the 6 target antigens employed can be obtained, for example, from Biotrend Chemikalien GmbH, Eupener Straβe 157, Cologne.
In order to check the expression of APO-1 and the 6 target antigens, SKW6.4 and Jurkat cells were incubated, after having been incubated with the corresponding antibodies (10 μg/ml), with FITC-labeled antibodies directed against mouse IgG (Dako, Hamburg, Germany). The FACS analysis was carried out using a FACS Calibur and the CelQuest software (Becton Dickinson, San Jose Calif.).
It was found that both cell lines express APO-1 while CD20 and CD40 and, somewhat more weakly, CD19 are expressed on SKW6.4 and CD28 and, more weakly, CD2 and CDS are expressed on Jurkat cells.
Example 3
Preparing Bispecific Antibody Fragments
Bispecific antibody fragments were prepared by selectively reducing and reoxidizing disulfide bridges in the joint region; see, for example, Jung et al. loc. cit. The reaction conditions which were used were selected such that the formation of homodimers was prevented and it was possible to hybridize the modified original Fab fragments almost completely.
For the subsequent experiments, the IgG2a variant of the APO-1 antibody was hybridized with antibodies which are directed against the antigens CD19, CD20 and CD40 on SKW6.4 cells and against the antigens CD2, CDS and CD28 on Jurkat cells.
In the figures, the bispecific antibody fragments which were prepared in this way are identified by their two specificities, which are separated from each other by an X.
Example 4
Determining the Target Antigen-Restricted Induction of Apoptosis
In the experiments which were carried out, the aim was to test whether the bispecific antibody fragments were only able to stimulate the APO-1 receptor on those target cells which were also expressing the relevant target antigen for which the bispecific antibody also possessed a binding site.
This effect was determined on the basis of the rate at which the target cells were destroyed, with the target cells (SKW6.4 and Jurkat) being incubated, for this purpose, in triplicate in 96-well plates (1×10 5 /well) with 1 μg of the relevant antibody construct/mL.
After 16 hours of incubation, the viability of the remaining cells was determined using the tetrazolium salt WST-1 (Boehringer, Mannheim, Germany), which is transformed by mitochondrial enzymes and in the process forms a dark-red formazan.
The optical density was measured using an ELISA laser (Spektra-Max 340, Molecular Devices, Sunnyville, Calif.), and the percentage of cells which have been killed, with the optical density being OD x , was calculated in accordance with the following formula:
(1−OD x /OD max )×100,
where OD max is the optical density which is produced by tumor cells in the absence of antibodies.
In some experiments, the percentage was determined using a chromium release test. For this purpose, target cells were incubated with 51 Cr-labeled sodium chromate (80 μCi/ml, one hour), then washed thoroughly and sown in triplicate in 96-well plates. After incubating with the antibodies for 16 hours, the indicated activity was counted and the percentage of killed cells was calculated as follows:
cpm/cpm max ×100,
where cpm max is the radioactivity released by target cells which have been treated with a detergent.
The percentages of killed target cells which were measured using the two different methods were to a large extent in correspondence.
Example 5
Results
FIG. 2 shows that while bispecific antibody fragments having a specificity for APO-1 and CD20 (APO-1-2a×CD20) were able to kill CD20-positive SKW6.4 cells efficiently, this was not the case with the CD20-negative Jurkat cells. That both cell lines are sensitive to APO-1-mediated cell death follows from the fact that they are both killed by the antibody 7C11, which is an agonistic IgM antibody (Immunotech, Marseilles, France) which induces apoptosis.
Mixtures of the two original antibodies, which were employed either as intact antibodies or as Fab fragments, were unable to induce any apoptosis even in SKW6.4 cells.
In addition to this, coincubating the bispecific antibody fragment APO-1-2a×CD20 with the APO-1-2a antibody resulted in the lysis mediated by the bispecific antibody fragment being blocked.
It can be seen from FIG. 3 , in which the FACS numbers on the right provide information about the expression of the relevant target antigen on the cells, that the quantity of target antigen which is expressed on the target cells is essentially responsible for the extent of the destruction of the target cells.
Significant lysis of Jurkat cells was only achieved by the APO 1-2a×CD28 construct.
APO-1-2a×CD2 only brought about marginal destruction of Jurkat cells, with APO-1-2a×CD5 in fact being completely ineffective with these cells. On the other hand, APO-1-2a×CD20 and APO-1-2a×CD40 were very efficient, bringing about virtually 100% destruction of SRW6.4 cells.
APO-1-2a×CD19 and APO-1-2a×CD28 were less effective on SKW6.4 cells and Jurkat cells, respectively.
On the basis of these results, it can be stated that apoptosis was only induced in cells which were expressing the appropriate target antigen in addition to the APO-1 receptor.
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A multispecific reagent has at least one first binding site for a cell surface receptor which requires multimeric ligand binding to be stimulated. The reagent possesses a second binding site for a target antigen which is expressed on the same cell as the cell surface receptor.
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PRIORITY CLAIM
[0001] The present application is a National Phase entry of PCT Application No. PCT/EP2012/062075, filed Jun. 22, 2012, which claims priority from French Patent Application No. 11 55513, filed Jun. 22, 2011, said applications being hereby incorporated by reference herein in their entirety.
FIELD OF THE INVENTION
[0002] The field of this invention is that of exploration and exploitation of oil reservoirs. More precisely, this invention relates to the development of nanoparticles which can be used as tracers in order to follow the movement of fluids injected into an oil reservoir.
[0003] The injected fluids diffuse through a solid geological medium which constitutes the oil reservoir, thus making it possible to study this latter by following the path of the injected fluids. The objective is in particular to monitor the flows between the injection well(s) and the production well(s) and/or to evaluate the volumes of oil in reserve and water in the reservoir and ultimately to optimize oil exploration and exploitation.
BACKGROUND OF THE INVENTION
[0004] In the exploitation of an oil reservoir it is well known that most often no more than half, or even less, of the oil originally present in the reservoir is extracted. The recovery by the primary means, that is to say the use of the extraction energy resulting from gases or liquids present underground under the effect of a certain pressure in the reservoir only makes it possible to extract small percentages of the total oil present in the reservoir. In order to complete this primary recovery, a secondary recovery is performed: it consists of implementing what is known as production by “water drive” or “water flooding”, i.e. by injecting water into a well (injection well) at a location of the reservoir in such a way as to drive the oil in the reservoir out of the underground area through at least one other well referred to as the “production well”.
[0005] In order to be aware of the behavior of the injection water, it is known to add tracers to it which are easily detectable in the liquid. These tracers make it possible to track the injection water. The measurement of the quantity of tracer at the level of the production well makes it possible to know the volume and the distribution of the injection fluid in the formation. Furthermore, the tracer/oil interaction can enable determination of the proportion of liquids in the deposit constituted by the oil reservoir. This is one of the most important parameters which can be determined by the use of such tracing fluids, since this parameter makes it possible, on the one hand, to adjust the water injection program and, on the other hand, to evaluate the quantity of oil still to be produced. As soon as the fluid containing the tracer has been detected at the production well(s), the study method enabling the analysis, control and optimized recovery of oil makes it necessary for the concentration of tracer in the fluid produced at the outlet to be measured continuously or intermittently, in such a way that tracer concentration curves can be plotted as a function of time or as a function of the volume of fluid produced.
[0006] The tracers in the injection water for oil reservoirs also enable detection of aberrations in the flow rates caused by of pressure differentials in the reservoir which are caused by factors other than the injection of water and which impair the performance.
[0007] The specification of tracers which can be used in these injection waters for optimization of the recovery of oil comprises the following details:
economical; compatible with the fluids naturally present in the reservoir, and with oil-bearing rock itself and also with the fluids injected into the reservoir, namely the injection liquids (waters); easy qualitative and quantitative detection of the tracer regardless of the materials present in the fluid at the outlet of the production well. For example, an aqueous solution of sodium chloride cannot be used as tracer because the majority of oil fields contain sea water and therefore sodium chloride in substantial quantities, so that the detection of chloride of NaCl used as tracer would be particularly difficult; surreptitious tracer, that is to say it cannot be easily absorbed in the solid medium through which it passes or eliminated from the tracing fluid, since in the analytical technique used, the tracer concentration in the fluids produced at the outlet is determined and compared with the concentration of fluids injected in the injection well(s); resistance of the tracer to bacterial contamination, to the high temperatures and high pressures existing in the oil reservoirs; offers the possibility of the tracer interacting or not with the environment of the reservoir, namely the geological media which may or may not be oil-bearing; access for a large number of different tracers and coding for possible simultaneous detections (several injection wells) or chronologically successive tracing tests.
[0015] With regard to the prior art relating to such tracers for injection waters (tracing fluid) enabling surveying of the oil reservoirs by diffusion between an injection well and a production well, reference may be made to the U.S. Pat. No. 4,231,426 B1 and U.S. Pat. No. 4,299,709 B1 which disclose aqueous tracer fluids comprising from 0.01 to 10% by weight of a nitrate salt associated with a bactericidal agent chosen from among the aromatic compounds (benzene, toluene, xylene).
[0016] Canadian Patent Application CA 2 674 127 A1 relates to a method which uses a natural isotope of carbon 13 for the identification of early breakthrough of the injection waters into the oil well.
[0017] Moreover, there are about ten families of appropriate molecules currently validated as tracer for injection waters in oil reservoirs. These families of molecules are for example fluorinated benzoic acids or naphthalenesulphonic acids.
[0018] The known tracer molecules which are used have a specific chemical/radioactive signature. These known tracers can be detected with great sensitivity but nevertheless have three major drawbacks:
quantification thereof requires a process which is quite complex and expensive, and can only be carried out in a specialist center, often remote from the production sites; These molecules are not very numerous and do not enable multi-labelling or repeated labelling to be effected; some of these known markers are destined to disappear because of their negative impact on the environment.
[0022] Moreover, the site of “Institute for Energy Technology” (IFE) has put online a PowerPoint presentation entitled SIP 2007-2009 “ New functional tracers based on nanotechnology and radiotracer generators Department for Reservoir and Exploration Technology ” (last modification dated 7 Mar. 2011). In particular, this document suggests the use of surface-modified nanoparticles as tracer for monitoring flows in oil reservoirs and oil wells and in studies of processes. This presentation describes functionalized tracer nanoparticles comprising a core based on Gd 2 O 3 and a surface coating based on siloxane functionalised with additional molecules. It is also suggested that the rare earth core and/or the additional molecules can emit luminous signals by fluorescence or radioactive signals.
[0023] In a quite different field, the French Patent Application FR 28 67 180 A1 describes hybrid nanoparticles comprising, on the one hand, a core consisting of a rare earth oxide, possibly doped with a rare earth or an actinide or a mixture of rare earths and actinide and, on the other hand, a coating around this core, the said coating consisting predominantly of polysiloxane functionalised by at least one biological ligand grafted by covalent bond. The core may be based on Gd 2 O 3 doped with Tb 3+ or by uranium and the coating of polysiloxane can be obtained by causing an aminopropyltriethoxysilane, a tetraethylsilicate and triethylamine to react. These nanoparticles are used as probes for the detection, the monitoring and the quantification of biological systems.
[0024] French Patent Application FR 29 22 106 A1 derives from the same technical field and relates to the use of these nanoparticles as radiosensitizing agents in order to increase the effectiveness of radiotherapy. These nanoparticles have a size between 10 and 50 nanometers.
SUMMARY OF THE INVENTION
[0025] In this context the object of the present invention is to address at least one of the following objectives:
to propose a novel method of studying a solid medium, for example an oil reservoir, by diffusion of a liquid through said solid medium, which is simple to implement and economical; to remedy the drawbacks of tracers for injection waters of oil reservoirs according to the prior art; to provide a tracer which perfectly follows the injection waters in their diffusion (percolation) through the solid media constituted by the oil reservoirs, without interacting with the geological underground area through which it passes (neither attraction nor repulsion); to provide a tracer for injection waters of oil reservoirs of which the interactions (attraction-repulsion) in the relation to the geological medium through which it percolates can be monitored intentionally; to provide a novel surreptitious tracer for injection waters of oil reservoirs; to provide a novel tracer for injection waters of oil reservoirs having a sensitivity and/or facility for detection substantially improved relative to the tracers known until now; to provide a novel tracer for injection waters for oil reservoirs having several easily detectable signals in order to produce multi-detection and multiply the analyses over the course of time or space; to provide a novel and co-compatible tracer for injection waters of oil reservoirs; to provide a novel tracer for injection waters of oil reservoirs which is physically, chemically and biologically stable in the geological solid media constituted by the oil reservoirs; to provide a novel liquid, in particular novel injection waters, of oil reservoirs which can be used in particular in a process for studying a solid medium, for example an oil reservoir by diffusion of said liquid through said solid medium; to provide a novel process for synthesis for such tracers which is simple and economical to implement.
[0037] These objectives, amongst others, are achieved by the invention which relates in the first place to nanoparticles for use in the study of an oil reservoir, said nanoparticles being characterized in that they comprise:
a core consisting of a noble metal or an alloy of noble metals, a matrix comprising (i) polysiloxanes and (ii) an organometallic fluorophore bound covalently to the polysiloxanes, said matrix being functionalized on its surface in order to form silane bonds Si—R, wherein preferably at least 50%, preferably at least 75% of said radicals —R consist of neutral or charged hydrophilic compounds, preferably from amongst polyethers or polyols, or mixtures thereof.
[0040] The invention relates secondly to a method of preparation of a colloidal solution of nanoparticles which can be used for the study of an oil reservoir, said method comprising the following steps:
i. a noble metal core is synthesized and is coated with a matrix of polysiloxane prefunctionalized with hydrophilic silanes, within a reverse microemeulsion, ii. an aqueous colloidal solution of nanoparticles is extracted by decantation after destabilization of the microemulsion, for example in a water/alcohol mixture, iii. the nanoparticles are heated to at least 50° C., for example approximately 80° C.
[0044] Thirdly, the invention relates to an injection liquid for the study of an oil reservoir, comprising nanoparticles as defined above, or a colloidal solution of nanoparticles capable of being obtained by the method as defined above.
[0045] The invention also concerns the use of these nanoparticles as tracers in injection waters of an oil reservoir, which are intended for the study of said reservoir by diffusion therethrough, for the purpose in particular of controlling the flows between an injection well and a production well and/or evaluating the volumes of oil in reserve in the reservoir.
BRIEF DESCRIPTION OF THE DRAWINGS
[0046] FIG. 1 shows the time-resolved emission spectrum (delay 0.1 ms, acquisition time 5 ms) of the nanoparticles containing Eu DTPA and fluorescein excited to 395 nm and the time-resolved excitation spectrum (delay 0.1 ms, acquisition time 5 ms) of these same nanoparticles with an emission fixed at 615 nm
[0047] FIG. 2 shows the time-resolved emission spectrum (delay 0.1 ms, acquisition time 5 ms) of the nanoparticles containing Eu DTPA and fluorescein excited to 615 nm and the time-resolved excitation spectrum (delay 0.1 ms, acquisition time 5 ms) of these same nanoparticles with an emission fixed at 395 nm
[0048] FIG. 3 a shows the the time-resolved excitation spectrum (delay 0.1 ms, acquisition time 5 ms) of the particles containing the nanoparticles containing Tb and derivatives of pyridine with an emission fixed at 545 nm
[0049] FIG. 3 b shows the the time-resolved emission spectrum (delay 0.1 ms, acquisition time 5 ms) of the particles containing the nanoparticles containing Tb and derivatives of pyridine excited to 246 nm
[0050] FIG. 4 shows comparative permeation curves between a reference tracer (grey) and the nanoparticles (black) according to the method of preparation 4. In the X axes, the flow volume In the Y axes, the absorption or the fluorescence, standardized to the initial values.
[0051] After 180 mL, a solution of degassed sea water without tracers is injected.
DETAILED DESCRIPTION OF THE INVENTION
[0052] The Nanoparticles
[0053] The nanoparticles according to the invention are intended for use in the study of an oil reservoir, said nanoparticles being characterized in that they comprise:
a core consisting essentially of a noble metal or an alloy of noble metals, a matrix comprising (i) polysiloxanes and (ii) an organometallic fluorophore bound covalently to the polysiloxanes, said matrix being functionalised on its surface in order to form silane bonds Si—R, wherein preferably at least 50%, preferably at least 75% of said radicals —R consist of neutral or charged hydrophilic compounds, preferably from amongst polyethers or polyols, or mixtures thereof.
[0056] The nanoparticles according to the invention are detectable, that is to say that it is possible to identify their presence or absence in the medium above a certain concentration and that it is even possible to quantify the concentration thereof when they are present in the medium.
[0057] These nanoparticles are capable of forming a stable colloidal suspension in a saline medium which does not settle very much. For example, this suspension does not exhibit precipitation or agglomeration over time, e.g. after 6 months at ambient temperature.
[0058] The core of nanoparticles makes it possible to structure the nanoparticle. According to the present invention the core consists essentially of a noble metal, for example gold, silver or platinum, and/or an alloy of noble metals. In a preferred embodiment the core essentially consists of particles of gold.
[0059] In fact it has been found, surprisingly, that the nanoparticles obtained according to the invention are more dense and of more regular structure than those carried out with other materials for the choice of the core. Furthermore, in certain cases gold has an antenna effect which then makes it possible advantageously to amplify the fluorescent signal emitted by the organometallic fluorophore of the matrix during detection.
[0060] Gold, with other noble metals such as Ag, Pd, Pt, Ir, or Rh, is also detectable by the ICP detection method (or plasma torch spectrometry) and can be used as internal reference for the detection of nanoparticles and any degradation thereof.
[0061] Finally, gold has the advantage that it is also detectable by plasmon absorption enabling the detection and the quantification of nanoparticles at very low concentrations, for example at the level of the single particle, in particular after dispersion of a given volume on a substrate. A particle can be detected in 10 μL at least, preferably 100 μL.
[0062] The gold particles forming the core of nanoparticles have a size of at least 3 nm, preferably between 5 nm and 15 nm.
[0063] The matrix forms a layer coating the core of noble metals of the nanoparticle. It makes it possible to encapsulate the detectable molecules for the detection and/or the quantification of nanoparticles.
[0064] The matrix of nanoparticles according to the invention comprises polysiloxanes and at least one organometallic fluorophore bound covalently to the polysiloxanes. In a specific embodiment, said matrix consists essentially of polysiloxane, functionalised on the exterior surface of the nanoparticles and encapsulating organometallic fluorophores.
[0065] The matrix/core assembly forms nanoparticles having a mean diameter preferably between 20 nm and 100 nm, for example between 20 nm and 50 nm. In an advantageous embodiment the nanoparticles according to the invention have a polydispersity index of less than 0.5, preferably less than 0.3, or less than 0.2, preferably less than 0.1.
[0066] The size distribution of the nanoparticles is for example measured with the aid of a commercial granulometer such as a Malvern Zetasizer Nano-S granulometer based on PCS (Photon Correlation Spectroscopy). This distribution is characterized by a mean diameter and a polydispersity index.
[0067] Within the meaning of the invention, “mean diameter” is understood to mean the harmonic mean of the diameters of the particles. The polydispersity index makes reference to the width of the size distribution deriving from the analysis of the cumulants. These two characteristics are described in the Standard ISO 13321:1996.
[0068] If applicable, the matrix may comprise other materials, chosen from within the group consisting of silicas, aluminas, zircons, aluminates, aluminophosphates, metal oxides or also metals (example: Fe, Cu, Ni, Co . . . ) passivated on the surface by a layer of the oxidized metal or another oxide and mixtures and alloys thereof.
[0069] An essential function of the matrix is to maintain the organometallic fluorophores in the nanoparticles and in particular to protect them from attacks from the external environment.
[0070] The organometallic fluorophores make it possible to produce one or more detectable signals per nanoparticle. The organometallic fluorophores used in the nanoparticles according to the invention are preferably chosen in such a way as to produce a fluorescent signal which is stable in time and which is not significantly influenced by the physico-chemical conditions of the environment through which they pass (for example temperatures, pH, ionic compositions, solvents, redox conditions . . . )
[0071] The organometallic fluorophores contained in the matrix of the nanoparticles are chosen from among vanadates or rare earth oxides, or mixtures thereof. In a specific embodiment they are chosen from among lanthanides, alloys thereof and mixtures thereof, bound to complexing molecules.
[0072] In a preferred embodiment the organometallic fluorophores are detectable by time-resolved fluorescence. Then lanthanides bound to complexing molecules are particularly preferred.
[0073] The metals of the lanthanide series comprise elements with atomic numbers from 57 (lanthanum) to 71 (lutetium). For example, the lanthanides will be chosen from within the group consisting of: Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm and Yb and mixtures and/or alloys thereof, bound to complexing molecules.
[0074] “Complexing molecules” or “chelating agent” are understood to mean any molecule capable of forming with a metallic agent a complex comprising at least two co-ordination bonds.
[0075] In a preferred embodiment, a complexing agent having a co-ordinance of at least 6, for example at least 8, and a dissociation constant of the complex pKd, greater than 10 and preferably greater than 15, with a lanthanide
[0076] Within the meaning of the invention, the “dissociation constant pKd” is understood to mean the measurement of the equilibrium between the ions complexed by the ligands and the free ligand dissociated in the solvent. Precisely, it is not so much the base 10 logarithm of the product of dissociation (−log(Kd)), defined as the equilibrium constant of the reaction which expresses the passage from the complexed state to the ionic state.
[0077] Such complexing agents are preferably polydentate chelating molecules chosen from amongst the families of molecules of the polyamine type, carboxylic polyacids and those having a high number of potential co-ordination sites preferably greater than 6, such as certain macrocycles.
[0078] In a more preferred embodiment, DOTA or 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid of the following formula will be chosen:
[0000]
[0000] or one of the derivatives thereof
[0079] The matrix may also contain, in addition to the complexing agent, a cyclic agent, for example grafted to the polysiloxanes.
[0080] A “cyclic agent” is understood to be an organic molecule, having at least one aromatic ring or heterocyclic ring, preferably chosen from amongst benzene, pyridine or derivatives thereof and capable of amplifying the fluorescent signal emitted by the organometallic fluorophore, for example a complexing agent bound to lanthanide. These cyclic agents, which are of interest if they are characterized by a high absorbance, are used in particular to amplify the fluorescent signal emitted by the organometallic fluorophores (antenna effect by transfer of the excitation of the agent to the fluorophore).
[0081] The cyclic agent can be grafted covalently either directly to the polysiloxanes of the matrix or to the organometallic fluorophore.
[0082] In a specific embodiment, the organometallic fluorophores consisting of a lanthanide with a complexing agent are grafted covalently to the polysiloxanes via an amide function.
[0083] The matrix of the nanoparticles according to the invention is functionalised on its surface. The functionalization of the matrix comprises the formation of silane bonds Si—R, wherein preferably at least 50%, preferably at least 75% of said radicals —R consist of neutral or charged hydrophilic compounds, preferably from amongst polyethers or polyols, or mixtures thereof.
[0084] In a preferred embodiment the functionalization of the nanoparticles is carried out in such a way that the zeta potential of the nanoparticles measured at a pH of 6.5 is less than +10 mV.
[0085] Within the meaning of the invention, the term “zeta potential” refers to the electrokinetic potential in the colloidal systems. This is the electrical potential of the double surface layer or also the difference in potential between the solvent and the layer of liquid attached to the particle. The zeta potential can be measured with the same apparatus as that used in order to measure the size distribution as described in the article “zeta potential of colloids in Water”, ASTM Standard D 4187-82, American Society for Testing and Materials, 1985.
[0086] The objective of functionalization is in particular to obtain good colloidal stability in a saline medium, for example a critical salt concentration of at least 50 g/L, even at least 100 g/L. It also has the function of modulating the water/rock interactions of the nanoparticle (minimizing adsorption thereof on the rock for example), even of modulating (for example minimizing) the water/oil interactions.
[0087] Such interactions can be measured during an experiment of permeation on a core as described in the examples below. According to a preferred embodiment, the nanoparticles according to the invention exhibit a minimal adsorption with this type of test.
[0088] The radicals —R covalently grafted on the basis of silane bonds Si—R may comprise:
i. charged hydrophilic groups, preferably hydrophilic organic compounds, molar masses below 5000 g/mol and more preferably below 450 g/mol, preferably chosen from among the organic groups including at least one of the following functions: alcohol, carboxylic acid, amine, amide, ester, ether oxide, sulphonate, phosphonate and phosphinate, and a combination of these functions, ii. neutral hydrophilic groups, preferably chosen from among sulphonate derivatives, alcohols, for example sugars or polyols, more preferably a polyalkylene glycol or a polyol, even more preferably a polyethylene glycol, Diethylene Triamine PentaAcetic acid (DTPA), dithiolated DTPA (DTDTPA), a gluconamide or a succinic acid, and mixtures of these neutral hydrophilic groups, iii. if appropriate, hydrophobic groups, for example chosen from among molecules containing alkyl or fluorinated chains.
[0092] According to one embodiment of the invention, at least 50%, preferably at least 75%, of the radicals —R of the silanes Si—R on the surface consist of neutral hydrophilic radicals, for example chosen from among polyols, for example gluconamide, or polyethers, for example polyethylene glycol, or mixtures thereof.
[0093] Advantageously, the —R radicals of the silane bonds are present on the surface in a proportion of at least one radical —R per 10 nm 2 of surface, for example at least one radical —R per 1 nm 2 , and preferably at least between 1 and 10 radicals —R per nm 2 .
[0094] The surface functionalization is effected by condensation of silanes on the surface of the matrix. It is also possible to add polysilanes (such as diethylene-di(trimethoxy)silane) during the condensation in order to passivate the surface of the coating and to ensure good adhesion thereof
Method for Preparation of a Colloidal Suspension of Nanoparticles
[0095] The invention relates to a method for preparation of a colloidal suspension of nanoparticles which can be used as tracer for the study of an oil reservoir.
[0096] The method according to the invention comprises the following steps:
a noble metal core is synthesized and is coated with a matrix of polysiloxane prefunctionalized with hydrophilic silanes, within a reverse microemeulsion, an aqueous colloidal solution of nanoparticles is extracted by decantation after destabilization of the microemulsion, for example in a water/alcohol mixture, for example water/isopropanol, the nanoparticles are heated to at least 50° C., for example approximately 80° C.
[0100] More precisely, according to the method according to the invention the core and the matrix are synthesised in reverse microemeulsion. It is possible, if applicable, to pre-coat the nanoparticles at this stage with a hydrophilic silane.
[0101] The microemulsion is then destabilized, for example with a water/alcohol mixture such as water/isopropanol, in such a way as to extract the nanoparticles in the form of a stable colloidal aqueous solution (i.e. which is not precipitated). Furthermore, the solution extracted by decantation can be washed for example by tangential filtration. Thus in an advantageous embodiment of the method according to the invention the nanoparticles are never in a dry phase.
[0102] The method without a dry solid phase would make it possible to obtain nanoparticles of more homogeneous size, and therefore with a lower polydispersity index.
[0103] Another particularly advantageous step of the method according to the invention is the step of heating, to at least 50° C., for example at least 60° C., at least 70° C., for example to 80° C., for a sufficient time to enable densification of the coating layer, for example at least 30 minutes, preferably at least 1 hour. The step of heating makes it possible to increase the stability of particles, in particular in time, by limiting the agglomeration phenomena. This would also make it possible to densify the coating and to reduce the number of free silanol groups on the surface and more generally in the coating layer. Thus the adhesion and the stability of the coating layer are improved and would also enable additional protection of the fluorophores contained in the matrix.
[0104] Therefore the method according to the invention makes it possible to obtain colloidal solutions with nanoparticles having advantageous properties and distinct from the prior art, in particular with a smaller mean diameter, for example less than 50 nm and a low polydispersity index, for example less than 0.3, even less than 0.1, and with a very low reactivity with the external environment (surreptitious tracer), as can be demonstrated with the aid of the permeation test described in the example.
[0105] The invention also relates to a colloidal solution of nanoparticles which can be obtained according to the method of the invention described above.
[0106] Even more preferably, the nanoparticles are prepared as claimed in the method above and have the advantageous structural characteristics as defined above. In particular, the nanoparticles obtained by the above method comprise a core of noble metal, for example of gold, and a matrix comprising polysiloxanes including an organometallic fluorophore, for example a complexing agent bound to a lanthanide.
Methodology
[0107] The nanoparticles according to the invention are particularly useful as tracers in injection waters of an oil reservoir, which are intended for the study of said reservoir by diffusion therethrough, for the purpose in particular of monitoring the flows between an injection well and a production well and/or evaluating the volumes of oil in reserve in the reservoir.
[0108] Before the analysis of the liquid which has diffused, said liquid is concentrated, preferably by filtration or dialysis, and, even more preferably, by tangential filtration and preferably by use of a membrane with cut-off thresholds below 300 kDa (kilo Dalton).
[0109] Preferably, it will be desirable to detect at least two types of signals emitted by the nanoparticles:
a first signal capable of being emitted by the organometallic fluorophores and measured by fluorescence. and a second signal capable of being emitted by the noble metal (such as gold, silver, platinum and mixtures and/or alloys thereof), and measured by chemical analysis and/or by ICP; said noble metal constituting the core of the nanoparticle.
[0113] In a preferred embodiment, in order to measure the quantity of nanoparticles in the liquid which has diffused, detection is carried out by time-resolved fluorescence (in order to detect the organometallic fluorophores) and/or by ICP (for the detection of the noble metal in the core of the nanoparticles).
[0114] The method of detection by time-resolved fluorescence is for example described in the article “ultrasensitive bioanalytical assays using time resolved fluorescence detection”, Phnrmac. Thu. Vol. 66, pp. 207-335, 21995. The method of detection by ICP is for example described in “application of laser ICP-MS in environmental analysis”, Fresenieus date of Analytical Chemistry, 355: 900-903 (1996).
[0115] Detection by time-resolved fluorescence, i.e. activated with a time lag after excitation (i.e. several microseconds) makes it possible to eliminate a large part of the intrinsic luminescence in the solid medium studied and to measure only the intrinsic luminescence relative to the tracing nanoparticle.
Injection Liquid (Water) for the Study of a Solid Medium, Namely i.e. an Oil Reservoir
[0116] According to another aspect, the invention relates to a liquid for injection in an oil reservoir, characterized in that it comprises a tracer based on nanoparticles according to the invention as defined above.
[0117] Advantageously, this liquid comprises water and the nanoparticles as defined above.
[0118] The injection waters may comprise, in addition to the nanoparticles, the following elements: surfactants, small hydrophilic polymers, polyalcohols (for example diethylene glycol), salts and other molecules conventionally used in oil injection.
Examples
[0119] Method of Preparation 1. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Fluorophores Derived from Fluorescein and Europium Complexes (DTPA)
[0120] 200 mg of diethylenetriaminepentaacetic acid bisanhydride (DTPABA), 0.130 mL of APTES and 0.0065 mL of triethylamine are introduced with 4 mL of DMSO (dimethyl sulfoxide) into a 10 mL bottle and stirred vigorously. After 24 hours, 200 mg of EuCl 3 ,6H 2 O are added. After i48 hours the complexing is sufficient; the following steps are then carried out: 20 mg of FITC (fluorescein isothiocyanate) are introduced with 0.5 mL of APTES ((3-aminopropyl)triethoxysilane) into a 2.5 mL bottle and stirred vigorously. Homogenization is carried out for 30 minutes at ambient temperature.
[0121] 36 mL of Triton X-100 (surfactant), 36 mL of n-hexanol (co-surfactant), 150 mL of cyclohexane (oil) and 21 mL of aqueous solution containing 9 mL of HAuCl 3H 2 O at 16.7 mM, 9 mL of MES (sodium 2-mercaptoethanesulphonate) at 32.8 mM and 3 mL of NaBH 4 at 412 mM are introduced into a 500 mL flask and stirred vigorously. After 5 minutes, 0.400 mL of solution containing fluorescein is added into the microemulsion with 1 mL of the solution containing the europium complex. Then 0.200 mL of APTES and 1.5 mL of TEOS (tetraethyl orthosolicate) are also added to the microemulsion.
[0122] The polymerization reaction of the silica is completed by the addition of 0.800 mL of NH 4 OH after 10 minutes. The microemulsion is stirred for 24 hours at ambient temperature.
[0123] Next, 190 μL of silane gluconamide (N-(3-triethoxysilylpropyl)gluconamide at 50% in ethanol is added to the microemulsion and stirred at ambient temperature.
[0124] After 24 hours, 190 μL of silane gluconamide are again added to the solution and stirring is continued at ambient temperature.
[0125] After 24 hours, the microemulsion is destabilized in an ampoule for decanting by addition of a mixture of 250 mL of distilled water and 250 mL of isopropanol. The solution is left to decant for 15 minutes and the lower phase containing the particles is recovered.
[0126] The recovered colloidal solution is then placed in a tangential filtration system VIVASPIN® at 300 kDa then centrifuged at 4000 r.p.m. until a purification rate greater than 500 is obtained.
[0127] The solution thus obtained is then filtered at 0.2 μm and diluted by 5 in DEG (diethyleneglycol).
[0128] Method of Preparation 2. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Fluorophores Derived from Fluorescein and Europium Complexes (DOTA).
[0129] The synthesis is similar to that described in the method of preparation 1 with the difference that the 200 mg of diethylenetriaminepentaacetic acid bisanhydride are replaced by 256 mg of 1,4,7,10-tetraazacyclododecane-1,4,5,10-tetraacetic glutaric anhydride (DOTAGA). The rest of the synthesis is identical.
[0130] Method of Preparation 3. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Molecules Containing an Aromatic Ring which are Derived from Pyridine (Antenna) and Terbium Complexes.
[0131] 85 mg de 2-pyridinethioamide (antenna), 70 mg de NHS (N-hydroxysuccinimide) and 230 mg of EDC (ethyl(dimethylaminopropyl)carbodiimide) are introduced with 2 mL of DMSO (dimethyl sulfoxide) into a 2.5 mL bottle and stirred vigorously. After 30 minutes, 140 μL of APTES are added and the mixture is left for 5 hours.
[0132] Next, 1 batch of freeze-dried terbium oxide nanoparticles (diameter 5 nm) purchased from Nano-H SAS are re-dispersed in 2 mL of distilled water in a 2.5 mL bottle.
[0133] 36 mL of Triton X-100 (surfactant), 36 mL of n-hexanol (co-surfactant), 150 mL of cyclohexane (oil) and 21 mL of aqueous solution containing 9 mL of HAuCl 4 3H2O at 16.7 mM, 9 mL of MES (sodium 2-mercaptoethanesulphonate) at 32.8 mM and 3 mL of NaBH 4 at 412 mM are introduced into a 500 mL flask and stirred vigorously. After 5 minutes, 0.600 mL of solution containing the antennas is added into the microemulsion with 2 mL of the solution containing the terbium particles. Then 0.550 mL of APTES and 1.5 mL of TEOS (tetraethyl orthosolicate) are also added to the microemulsion.
[0134] The polymerization reaction of the silica is completed by the addition of 0.800 mL of NH 4 OH after 10 minutes. The microemulsion is stirred for 24 hours at ambient temperature.
[0135] The functionalization with the silane-gluconamide and the treatment of the microemulsion are as described for the method of preparation 1.
[0136] Method of Preparation 4. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Molecules Containing an Aromatic Ring which are Derived from Fluorescein and Particles Containing Europium Complexes.
[0137] 20 mg of FITC (fluorescein isothiocyanate) are introduced with 0.5 mL of APTES ((3-aminopropyl)triethoxysilane) into a 2.5 mL bottle and stirred vigorously. Homogenization is carried out for 30 minutes at ambient temperature.
[0138] 1 batch of freeze-dried SRP-europium nanoparticles (diameter 5 nm-20 micromoles equivalent europium—Small Rigid Platform polysiloxane-DOTA(Eu)) (Nano-H SAS, France) are re-dispersed in 1.5 mL of distilled water in a 2.5 mL bottle.
[0139] 36 mL of Triton X-100 (surfactant), 36 mL of n-hexanol (co-surfactant), 150 mL of cyclohexane (oil) and 21 mL of aqueous solution containing 9 mL of HAuCl 4 3H2O at 16.7 mM, 9 mL of MES (sodium 2-mercaptoethanesulphonate) at 32.8 mM and 3 mL of NaBH4 at 412 mM are introduced into a 500 mL flask and stirred vigorously. After 5 minutes, 0.400 mL of solution containing fluorescein is added into the microemulsion with 1.5 mL of the solution containing the europium particles. Following this, 0.200 mL of APTES and 1.5 mL of TEOS (tetraethyl orthosolicate) are also added to the microemulsion.
[0140] The polymerization reaction of the silica is completed by the addition of 0.800 mL of NH4OH after 10 minutes. The microemulsion is stirred for 24 hours at ambient temperature.
[0141] The functionalization with the silane-gluconamide and the treatment of the microemulsion are as described for the method of preparation 1.
[0142] Method of Preparation 5a. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Molecules Containing an Aromatic Ring of Pyridine and Particles Containing Europium Complexes.
[0143] The synthesis is similar to that described in the method of preparation 1 with the difference of the functionalization effected in the microemulsion. The second addition of 190 mL of silane-gluconamide is replaced by an addition of 450 mg of silane (N-triethoxysilylpropyl)-O-polyethylene oxide urethane) corresponding to a theoretical quantity of 2 silanes per nm 2 of surface.
[0144] Method of Preparation 5b. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Molecules Containing an Aromatic Ring of Pyridine and Particles Containing Europium Complexes.
[0145] The synthesis is similar to that described in the method of preparation 1 with the difference of the functionalization effected in the microemulsion. The second addition of 190 mL of silane-gluconamide is replaced by an addition of 340 μL of silane ([hydroxy(polyethylenoxy)propyl]triethoxysilane) at 50% in ethanol, corresponding to theoretical quantity of 2 silanes per nm 2 of surface.
[0146] Method of Preparation 5c. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Molecules Containing an Aromatic Ring of Pyridine and Particles Containing Europium Complexes.
[0147] The synthesis is similar to that described in the method of preparation 1 with the difference of the functionalization effected in the microemulsion. The second addition of 190 mL of silane-gluconamide is replaced by an addition of 185 μL of silane (N-(trimethoxysilylpropyl)ethylenediaminetriacetic acid) at 45% in water, corresponding to a theoretical quantity of 2 silanes per nm 2 of surface.
[0148] Method of Preparation 5d. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Molecules Containing an Aromatic Ring of Pyridine and Particles Containing Europium Complexes.
[0149] The synthesis is similar to that described in the method of preparation 1 with the difference of the functionalization effected in the microemulsion. The second addition of 190 mL of silane-gluconamide is replaced by an addition of 60 μL of silane (3-thiocyanatopropyltriethoxysilane), which corresponds to a theoretical quantity of 2 silanes per nm 2 of surface.
[0150] Method of Preparation 5e. Preparation of a Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Molecules Containing an Aromatic Ring of Pyridine and Particles Containing Europium Complexes.
[0151] The synthesis is similar to that described in the method of preparation 1 with the difference of the functionalization effected in the microemulsion. The second addition of 190 mL of silane-gluconamide is replaced by an addition of 60 μL of silane (3-isocyanatopropyltriethoxysilane), which corresponds to a theoretical quantity of 2 silanes per nm 2 of surface.
[0152] Method of Preparation 6a.
[0153] The solution obtained according to the method of preparation 4 is post-functionalised by a silane (N-(2-aminoethyl)-3-aminopropyltriethoxysilane). In a 15 mL bottle 20 μL of silane is diluted in 10 mL of DEG. In a 15 mL bottle 10 μL of the dilute solution of silane (corresponding to a theoretical quantity of 0.1 molecule of silane per nm 2 of surface of a particle) is added to 10 mL of the solution obtained according to the method of preparation 4, and the solution obtained is stirred at 40° C. for 48 hours.
[0154] Method of Preparation 6b.
[0155] The solution obtained according to the method of preparation 4 is post-functionalised by a silane (3-(triethoxysilyl)propylsuccinic anhydride). In a 15 mL bottle 20 μL of silane is diluted in 10 mL of DEG. In a 15 mL bottle 10 μL of the dilute solution of silane (corresponding to a theoretical quantity of 0.1 molecule of silane per nm 2 of surface of a particle) is added to 10 mL of the solution obtained according to the method of preparation 4, and the solution obtained is stirred at 40° C. for 48 hours.
[0156] Method of Preparation 6c.
[0157] The solution obtained according to Example 4 is post-functionalised by a silane (O-(propargyloxy)-N-(triethoxysilylpropyl)urethane). In a 15 mL bottle 24 μL of silane is diluted in 10 mL of DEG. In a 15 mL bottle 10 μL of the dilute solution of silane (corresponding to a theoretical quantity of 0.1 molecule of silane per nm 2 of surface of a particle) is added to 10 mL of the solution obtained in Example 4, and the solution obtained is stirred at 40° C. for 48 hours.
[0158] Method of Preparation 7. Colloidal Solution of Nanoparticles with a Core of Gold and a Silica Matrix Encapsulating Organic Molecules Containing an Aromatic Ring which are Derived from Pyridine and Europium Complexes (DTPA).
[0159] 140 mg de antennas (2,2′:6′,2″-terpyridine), 70 mg de NHS (N-hydroxysuccinimide) and 230 mg of EDC (ethyl(dimethylaminopropyl)carbodiimide) are introduced with 2 mL of DMSO (dimethyl sulfoxide) into a 2.5 mL bottle and stirred vigorously. After 30 minutes, 140 μL of APTES are added.
[0160] 200 mg of diethylene triamine pentaacetic acid (DTPA), 0.130 mL of APTES and 0.065 mL of triethylamine are introduced with 4 mL of DMSO (dimethyl sulfoxide) into a 10 mL bottle and stirred vigorously. After 24 hours, 200 mg of EuCl 3 ,6H 2 O are added. After 48 hours the complexing is sufficient. 36 mL of Triton X-100 (surfactant), 36 mL of n-hexanol (co-surfactant), 150 mL of cyclohexane (oil) and 21 mL of aqueous solution containing 9 mL of HAuCl 4 3H2 2 O at 16.7 mM, 9 mL of MES (sodium 2-mercaptoethanesulphonate) at 32.8 mM and 3 mL of NaBH 4 at 412 mM are introduced into a 500 mL flask and stirred vigorously. After 5 minutes, 0.400 mL of solution containing fluorescein is added into the microemulsion with 1 mL of the solution containing the europium complex. Next, 0.200 mL of APTES and 1.5 mL of TEOS (tetraethyl orthosolicate) are also added to the microemulsion.
[0161] The polymerization reaction of the silica is completed by the addition of 0.800 mL of NH 4 OH after 10 minutes. The microemulsion is stirred for 24 hours at ambient temperature.
[0162] Next, 190 μL of silane gluconamide (N-(3-triethoxysilylpropyl)gluconamide at 50% in ethanol is added to the microemulsion and stirred at ambient temperature.
[0163] After 24 hours, 190 μL of silane gluconamide are again added to the solution and stirring is continued at ambient temperature.
[0164] After 24 hours, the microemulsion is destabilized in an ampoule for decanting by addition of a mixture of 250 mL of distilled water and 250 mL of isopropanol. The solution is left to decant for 15 minutes and the lower phase containing the particles is recovered.
[0165] The recovered colloidal solution is then placed in a filtration system VIVASPIN® at 300 kDa then centrifuged at 4000 r.p.m. until purification rate above 500 is obtained.
[0166] The solution thus obtained is then filtered at 0.2 μm and diluted by 5 in DEG (diethyleneglycol).
[0167] The solution obtained is then post-functionalised with 3.72 μl of silane (N-(triethyoxysilylpropyl)-O-polyethylene oxide urethane) (corresponding to a theoretical quantity of 0.1 molecule of silane per nm2 of particle) at 40° C. and stirred for 48 hours.
[0168] Results
[0169] Mean diameter and polydispersity of nanoparticles as claimed in the methods of preparation 1 to 5 (examples 1 to 5).
[0170] Colloidal solutions of nanoparticles were prepared according to the methods of preparation 1 to 5 (Examples 1 to 5 respectively).
[0171] The following table gives the mean diameter and the polydispersity index of nanoparticles as obtained according to Examples 1 to 5.
[0000]
Examples
Mean diameter
Polydispersity
Example 1
50 nm
0.091
Example 2
62 nm
0.057
Example 3
37 nm
0.060
Example 4
41 nm
0.055
Example 5a
46 nm
0.050
Example 5b
44 nm
0.109
Example 5c
55 nm
0.083
Example 5d
53 nm
0.081
Example 5e
70 nm
0.109
[0172] FIGS. 1 , 2 and 3 exhibit the excitation and emission spectra with a time lag of 0.1 ms for Examples 1 to 3 respectively. These data show that the nanoparticles exhibit a good property of time-resolved fluorescence.
[0173] Comparison of Properties of the Nanoparticles Before and after the Step of Heating
[0174] For Examples 6a to 6c, nanoparticles were prepared according to the methods of preparation 6a to 6c.
[0175] The following table shows the mean diameter, the polydispersity and the zeta potential of the nanoparticles before and after the step of heating, wherein the step of heating consists of heating the solution of nanoparticles after the post-functionalization at 80° C. for 1 hour and then cooling it at ambient temperature.
[0000]
Values before heating
Values after heating
Mean diameter
Mean diameter
Polydispersity
Polydispersity
Examples
Zeta potential
Zeta potential
Example 1
50 nm
51 nm
0.091
0.075
n/d
n/d
Example 3
37 nm
39 nm
0.060
0.077
n/d
n/d
Example 4
41 nm
47 nm
0.055
0.026
n/d
n/d
Example 6a
35 nm
35 nm
0.053
0.066
3.69 mV measured at pH
5.15 mV measured at pH
6.2
6.5
Example 6b
35 nm
34 nm
0.034
0.116
13.0 mV measured at pH
−22.2 mV measured at pH
6.2
6.5
Example 6c
33 nm
38 nm
0.077
0.035
13.7 mV measured at pH
−25.0 mV measured at pH
6.2
6.5
[0176] Test of Permeation
[0177] We describe here the manufacture of a cartridge enabling a fluid to percolate through a cylindrical core of porous rock in the longitudinal direction, without loss of fluid through the side thereof and the permeation of particles.
[0178] The equipment used is composed of the core, two plugs of the same diameter specially machined to enable the screwing of connectors, transparent PVC tube, a PTFE template, Araldite glue and a tube of commercial silicone sealant.
[0179] Insert one of the two plugs in the template, fix it with the silicone, then leave to dry for 30 minutes. Prepare the Araldite glue in an aluminum cup, then place the core on the plug and glue it, leave to dry for several minutes. Do the same for the top plug. Cutting out PVC tube to the corresponding length, put the silicone on the base of the tube then turn it over on the template. Put the whole thing into the oven at 50° C. for ½ hour.
[0180] Determine the volume of epoxy resin taking account of the phenomenon of imbibition in the rock (volume equivalent to 0.4 cm diameter of the column) The epoxy resin is composed of 70% of a resin base (Epon 828—Miller-Stephenson Chemical Company, Inc) and 30% of a hardener (Versamid 125—Miller-Stephenson Chemical Company, Inc). In a single-use plastic beaker, mix the resin with the hardener for 10 minutes, then place the mixture at 50° C. for 40 to 50 minutes until a transparent fluid mixture is obtained. Pour the mixture slowly along the PVC tube, then leave at ambient temperature for two hours. Then place the whole thing at 70° C. for two hours. Leave to cool at ambient temperature.
[0181] A synthetic sea water solution is composed of mineral water (containing 35 ppm of dissolved SiO 2 ) in which the following salts are dissolved:
[0000]
Salts
Concentration (g/l)
NaCl
24.80
KCl
0.79
MgCl 2
5.25
CaCl 2
1.19
NaHCO 3
0.10
Na 2 SO 4
4.16
[0182] A known quantity of potassium iodide is added to this solution—the iodide ion having an ideal tracer behavior for the permeation tests—in such a way as to have a concentration of 1 g/L in KI. The whole mixture is degassed by active stirring in a vacuum for 5 to 10 minutes.
[0183] Concentrated suspensions of nanoparticles in water or in diethylene glycol (DEG) are available, according to the preceding examples. A known quantity of these suspension is diluted in the preceding solution at a volume of 300 to 500 mL in such a way it has a concentration of particles between 0.1 and 10 mg/L. The suspension is left to be stirred gently for 10 minutes, then filtered on a membrane of 0.2 nm.
[0184] The assembly is composed of a double syringe pump which makes it possible to fix a flow rate of between 1 and 1000 mL per hour, typically between 20 and 100 mL per hour. This directs a fluid towards a cartridge containing the porous rock. The fluid percolates through this latter, the pressure differential on either side of the rock is tracked by a sensor. Finally, the fluid is directed towards a fraction collector.
[0185] In the case of a permeation of particles, the fluid used is a dilute suspension of particles and KI. In the case of washing of the rock or a test of desorption of particles after permeation, the fluid injected is degassed sea water without tracers.
[0186] In these fractions, on the one hand the UV absorption is measured at λ=254 nm of the fluid. This is very low when the fluid does not contain any iodide, and becomes substantial in the presence thereof. Therefore the UV absorption makes it possible to track the permeation of the ideal tracer. On the other hand, the fluorescence of the fractions is measured in conditions which make it possible to detect the fluorophore(s) present in the particles. Therefore this technique makes it possible to track the permeation of the particles.
[0187] The rock has the following characteristics:
Type: Bentheimer
[0188] Nature of the material: sandstone, with clays (<5%).
Dimensions: 5 cm in diameter; 12.5 cm in length
Permeability: 800 mD approximately
Porosity: 20%
[0189] Particles used, prepared according to Example 4.
[0190] The flow rate imposed by the pump is 60 mL/hour. The fractions collected at the rock outlet have a volume of 5 mL.
[0191] FIG. 4 shows a permeation curve of nanoparticles prepared according to the method of preparation 4 (comprising a step of heating to 80° C. for 1 hour) by comparison with the control KI (ideal tracer). The results of permeation show that the nanoparticles according to the invention can be easily used as tracers in injection waters. In fact a very good correlation is observed between the fluorescent nanoparticulate tracers and the ideal tracer taken as a reference (KI). In particular, a rate of passage of nanoparticles greater than 99% is obtained with a mean deviation with respect to the ideal tracer of less than 10%. As far as the inventors know, such results had not been obtained with nanoparticles having fluorophores detectable by time-resolved fluorescence, prepared by the methods according to the prior art.
[0192] The embodiments above are intended to be illustrative and not limiting. Additional embodiments may be within the claims. Although the present invention has been described with reference to particular embodiments, workers skilled in the art will recognize that changes may be made in form and detail without departing from the spirit and scope of the invention.
[0193] Various modifications to the invention may be apparent to one of skill in the art upon reading this disclosure. For example, persons of ordinary skill in the relevant art will recognize that the various features described for the different embodiments of the invention can be suitably combined, un-combined, and re-combined with other features, alone, or in different combinations, within the spirit of the invention. Likewise, the various features described above should all be regarded as example embodiments, rather than limitations to the scope or spirit of the invention. Therefore, the above is not contemplated to limit the scope of the present invention.
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This invention relates to the development of nanoparticles, which can be used as tracers, in order to track the movement of fluids injected into an oil reservoir. The injected fluids diffuse through a solid geological medium which constitutes the oil reservoir, thus making it possible to study this latter by following the path of the injected fluids. The objective is in particular to monitor the flows between the injection well(s) and the production well(s) and/or to evaluate the volumes of oil in reserve and water in the reservoir and ultimately to optimize oil exploration and exploitation.
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BACKGROUND AND SUMMARY OF THE INVENTION
This invention relates to polyester fibers having high boiling water shrinkage, i.e., at least 40%, yarns made therefrom, and a method of producing the high shrinkage polyester fibers.
Polyester fibers have been prepared for commercial use for more than thirty years, and are produced in large quantities. Most commercial polyester comprises poly(ethylene terephthalates).
The term "fiber" as used herein includes fibers of extreme or indefinite length (i.e., filaments) and fibers of short length (i.e., staple). The term "yarn", as used herein, means a continuous strand of fibers.
Because fibers produced from polyester have a number of outstanding characteristics: excellent dimensional stability and sturdiness, a high degree of crease resistance, good bulk elasticity, and warm handle, the fibers made from polyester have found a wide variety of applications, especially in the textile field.
Polyester fibers are normally produced having a reduced final shrinkage. However, in certain applications, it is desirable for the polyester fibers to have a high shrinkage. For instance, since polyester fibers tend to have a "crushing problem", or, in other words, when an object of sufficient weight is placed on a fabric comprising polyester fibers, the contour of the object tends to remain on the fabric after the object is removed. This problem is particularly acute for fabrics made from polyester fibers which are used for automotive upholstery. In this application, the weight of an object, such as a person, produces a profile of the object after the weight of the object has been removed. This result affects the aesthetic qualities of the product containing the polyester fibers. Therefore, there is a need in the art to provide polyester fibers which overcome or at least mitigate this problem.
In addition, it is sometimes desirable to blend polyester fibers having low shrinkage with polyester fibers having high shrinkage to produce a resulting product in which bulk is developed along with a soft handle.
Procedures have been utilized in the past to produce high shrinkage polyester fibers. Problems associated with these procedures are that, many times, strength or uniform dyeability or combinations of these properties are adversely effected in producing the high shrinkage polyester fibers.
Thus, the combined objective of polyester fibers having high shrinkage, uniform dyeability, good light stability, and good strength becomes somewhat irreconcilable in many of the processes for producing polyester fibers.
The present invention produces high shrinkage polyester fibers and yarns made therefrom which have an improved combination of properties, i.e., good strength and uniform dyeability and a method of producing the high shrinkage polyester fibers having the improved combination of properties, i.e., one which involves less sacrifice of one or more individual properties to improve the other.
It has been unexpectedly discovered that yarn comprising poly(ethylene terephthalate) fibers having the above-described combination of properties can be prepared from a partially oriented feeder yarn comprising poly(ethylene terephthalate) fibers having a birefringence (Δn) of at least 0.0175 by drawing the feeder yarn at a draw ratio in the range of from about 1.98 to about 2.10 and at ambient temperature (20°-25° C.).
The poly(ethylene terephthalate) filaments produced are characterized by a boiling water shrinkage of at least 40%, low crystallization, usually 15 to about 20 percent, a tenacity of 4.0 to 5.0 grams per denier, a long-period spacing (LPS) of greater than 225 Å. Preferably, the filaments have an average crystal size in the range of from about 25 to about 30 Å as measured in the direction of the fiber axis (105).
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partial schematic of the apparatus and process suitable for preparing the feeder yarn of the invention.
FIG. 2 is a partial schematic of an apparatus and process suitable for the drawing process of the invention.
FIG. 3 represents a graph showing the boiling water shrinkage of resulting polyester yarn produced by drawing feeder yarns at various draw ratios and ambient temperature.
FIG. 4 represents graph showing the tenacity of resulting polyester yarns produced by drawing feeder yarn at various draw ratios and ambient temperature.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
By the term poly(ethylene terephthalate), it is meant a linear polyester in which at least about 85% of the recurring structural units are ethylene terephthalate units of the following formula: ##STR1##
Preferably the linear polyester contains at least ninety percent (90%) recurring structural units of ethylene terephthalate. In a particularly preferred embodiment of the process, the polyester is substantially all poly(ethylene terephthalate). Up to 15 mol percent of other copolymerizable ester units other than poly(ethylene terephthalate) can also be present as long as their effect does not appreciably decrease the light stability and dye lightfastness of the resulting filaments.
The yarn comprising poly(ethylene terephthalate) fibers having the improved combination of properties can be produced by drawing a feeder yarn comprising polyester fibers having a birefringence (Δn) of at least 0.0175 at a draw ratio in the range of from about 1.98 to about 2.10 and at ambient temperature.
Preferably, the drawing of the feeder yarn is carried out at a draw ratio in the range of from about 1.98 to about 2.05 and, more preferably, about 2.02.
Any suitable procedure can be utilized to prepare the feeder yarn used in the invention. A preferred procedure comprises the following steps:
(a) extrude molten poly(ethylene terephthalate) having an intrinsic viscosity in the range of from about 0.40 to about 0.8, and preferably 0.64, through a spinneret to form one or more fibers;
(b) quench said fibers, preferably to a temperature not exceeding 40° C. higher than the glass transition of the poly(ethylene terephthalate);
(c) optionally, apply to said fibers of step (b) a lubricating finish in an amount in the range of 0.1 to about 1.0 weight percent based on the weight of the yarn; and,
(d) take up said quenched fibers of step (b) or (c) at a take-up speed sufficient to partially orient the fibers in an amount sufficient to achieve a birefringence (Δn) in said fibers of at least 0.0175, and preferably at least 0.020, which generally is a speed in the range of from about 2,200 meters/minute to about 3,000 meters/minute and, more preferably, 2,700 meters/minute to 2,800 meters/minute.
The yarns comprising poly(ethylene terephthalate) fibers can be processed into fabrics which are used in applications that desire high shrinkage polyester fibers having the improved combination of properties, i.e., upholstery for automobiles.
Various characteristics and measurements are utilized throughout the application. These characteristics and measurements are grouped here for convenience, although most are standard.
Density measurements are obtained by means of a density gradient column.
Percent crystallinity of the filaments is obtained from the following formula: ##EQU1## where ρ= sample density ρa= amorphous density of polyester
ρc= crystalline polyester density
Long-period spacing is obtained by small-angle x-ray scattering (SAXS) patterns made by known photographic procedures. X-radiation of a known wavelength, e.g., CuK a radiation having a wavelength of 1.5418 Å, is passed through a parallel bundle of filaments in a direction perpendicular to the filament axis, and the diffraction pattern is recorded on photographic film.
Birefringence (Δn) is obtained in the following manner:
Sodium D rays (wavelength 589 millimicrons) are used as a light source, and the filaments are disposed in a diagonal position. The birefringence (Δn) of the specimen is computed from the following equation: ##EQU2## when n is the interference fringe due to the degree of orientation of the polymer molecular chain; r is the retardation obtained by measuring the orientation not developing into the interference fringe by means of a Berek's compensator; α is the diameter of the filament; and λ is the wavelength of the sodium D rays.
The crystal size (L) is a value obtained in accordance with the following (P. Scherrer's) equation, which represents the size of a crystal in a direction approximately at right angles to the fiber axis: ##EQU3## wherein B is a (010) diffraction peak width in radian unit when the diffraction intensity is (It+Iam)/2, in which It is a diffraction intensity at (010) peak position, and Iam is a meridional X-ray diffraction intensity at a Bragg's reflection angle of 2θ=17.7°;
b is 0.00204 radian;
K is 0.94; and,
λ is 1.542 Å
The term "shrinkage of the fibers in boiling water" is defined as "percent decrease in length of material when exposed to elevated temperatures for a period of time and under 0.05 g.p.d. tension". In the present invention, the percent thermal shrinkage is measured in a boiling water bath of 100° C. for a period of 30 minutes. The shrinkage of the fiber is determined in accordance with the following formula: ##EQU4## wherein L 1 is original length of fiber; and,
L 2 is length of fiber after treatment.
Throughout the present specification and claims, the intrinsic viscosity of the polyester melt is given as a measure for the mean molecular weight, which is determined by standard procedures wherein the concentration of the measuring solution amounts to 0.5 g./100 ml., the solvent is a 60 percent by weight phenol/40 percent by weight tetrachloroethane mixture, and the measuring temperature is 25° C.
The tenacity or breaking strength in grams per denier (UTS) is defined by ASTM Standards, Part 24, American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pa., page 33 (1965) as "the maximum resultant internal force that resists rupture in a tension test." or "breaking load or force, expressed in units of weight required to break or rupture a specimen in a tensile test made according to specified standard procedure."
The photocell test value is obtained by first knitting yarn into a hoseleg using a Lawson Hemphill 54 gauge Fiber Analysis Knitter. The hoseleg is then dyed in a bath containing 1.2% by weight, based on fabric weight, of color index blue disperse 27 and 1.5% by weight of palegal MB-SF leveling agent. The bath is raised to 130° C. over a 45 minute period and held at 130° C. for 30 minutes. After drying, the hoseleg is placed on a flat surface and folded double. The measuring head of a Photovolt Model 670 Reflection Meter is placed on the hoseleg. A reflectance value is determined. A control sample is used to calibrate the reflection meter at 50. Reflection values below 50 indicate darker dyeing.
The apparatus and process are represented schematically in FIG. 1 and FIG. 2. With respect to FIG. 1, a method of preparing feeder yarn having a birefringence (Δn) of at least 0.0175 is illustrated. The method comprises first supplying a chip hopper 1 with chips comprising poly(ethylene terephthalate) 2. The hopper 1 in turn supplies an extruder 3 with the chips 2. An additive pump 4 is also illustrated whereby various liquid additives such as pigments or heat stabilizers can be added, if desired, to the chip stream which is entering the extruder 3. Once the chips exit the extruder as a molten stream 5, the stream is pumped through a conduit 6 which contains a plurality of static mixers 7. Once through the static mixers 7, the mix stream enters the spinneret 8 and is extruded into a plurality of molten streams 9 which are solidified in a quench chamber 10. The quench chamber is generally an elongated chimney of conventional length, preferably 60 to 80 inches, which has a gaseous atmosphere below the glass transition temperature of the molten polyester. The solidified fibers 11 next pass over an applicator 12 whereby the fibers are lubricated. Lubricants suitable for such use are known to those skilled in the art and include mineral oil, butyl stearate, alkoxylated alcohols, and phosphates or cationic antistatic compositions. The fibers next travel around a first (upstream) powered godet 13 and then around a second (downstream) godet 14, following which the yarn 11 is interlaced by an interlacer 15. Lastly, the filaments are wound into a bobbin 16. The fibers at this point are generally referred to as feeder yarn.
The speed at which the spun fibers are wound must be in the range of from about 2,200 to about 3,000 meters per minute and, preferably, about 2,750 meters per minute.
Referring to FIG. 2, the feeder yarn is fed continuously from package 17 by feed roll 18 by means of guides 19 and 20. The yarn is taken up and drawn by means of a godet 21 at a draw ratio in the range of from about 1.98 to about 2.10 and ambient temperature, i.e., 20°-25° C. At this point, the yarn is ready to be wound on a pirn (not shown).
Preferably, the feeder yarn is drawn at a draw ratio in the range of from about 1.98 to about 2.05 and, more preferably, the feeder yarn is drawn at a draw ratio of about 2.02.
The yarn produced in accordance with the invention has a denier per filament of 3 to 20. Total denier of the yarns produced in accordance with the present invention preferably range from about 40 to about 200 denier and, more preferably, from about 70 to about 150 denier.
The invention is further exemplified by the examples below, which are presented to illustrate certain specific embodiments of the invention, but are not intended to be construed so as to be restrictive of the scope and spirit thereof.
EXAMPLE I
Feeder yarn comprising polyethylene terephthalate were prepared under the following spinning and winding conditions set forth in Table I
TABLE I______________________________________Polymer PET PET PETLuster SD SD SDIntrinsic Viscosity 0.641 0.641 0.641Fiber Cross Section Round Round RoundFilament Count 24 24 32Spinning Temperature, °C. 292 292 295Pump Yield, g/min 41.7 43.8 43.0Winding Speed 2,200 2,725 2,725______________________________________
The feeder yarns thus produced had the characteristics set forth in Table II below.
TABLE II______________________________________ Elon- Denier Finish Tenacity gation Evenness (% onYarn Denier (g/denier) (%) (% Range) yarn) Δn______________________________________A 171 1.98 245 2.1 0.58 0.0219B 142 2.23 190 2.0 0.71 0.0313C 142 2.39 197 4.0 1.14 0.0304______________________________________
EXAMPLE II
The feeder yarn designated as C in Table II was then drawn at a draw ratio of 2.05 at ambient temperature. Various characteristics of this yarn were measured and reported in Table III.
TABLE III______________________________________Denier 71Boiling Water Shrinkage, % 40Tenacity, grams/denier 4.65Elongation, % 30Density, grams/cc 1.3569Denier Evenness, % Range 3.4Crystallinity, % 18.5X-Ray AnalysisCrystal Size in 105 Direction 26.5Long Period Spacing, Å >225Photocell Dye Value 41Birefringence 0.1444Glass Transition Temperature, °C. 72Melting Temperature, °C. 261______________________________________
These results in Table III demonstrate the good strength and good dyeability of the high shringage polyester fibers of the invention. Normally, polyester yarn having a boiling water shrinkage of at least 40% has low strength and poor uniformity.
EXAMPLE III
A feeder yarn prepared with a winding speed of 2,725 meters/minute and having a resulting birefringence (Δn) of 0.0304, denier of 142 and comprising 32 filaments which were semi-dull and had a round cross section was drawn at various draw ratios. The resulting yarn was measured for tenacity and boiling water shrinkage. These results are shown in FIGS. 3 and 4.
As shown in FIGS. 3 and 4, the processing of feeder yarn having a birefringence (Δn) greater than 0.0175, i.e., 0.0304, in accordance with the present invention produced a yarn having a boilig water shrinkage greater than 40% and good strength (tenacity).
Although certain preferred embodiments of the invention have been described for illustrative purposes, it will be appreciated that various modifications and innovations of the procedures and compositions recited herein may be affected without departure from the basic principles which underlie the invention. Changes of this type are therefore deemed to lie within the spirit and scope of the invention except as may be necessarily limited by the amended claims or reasonable equivalents thereof.
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High shrinkage polyester fibers having good strength and uniform dyeability are disclosed, along with a method of producing the high shrinkage polyester fibers, by drawing a feeder yarn having a birefringence (Δn) of at least 0.0175 at ambient temperature and carefully controlled draw ratios.
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BACKGROUND OF THE INVENTION
This invention relates to the electrical coupling of a touch-sensitive piezoelectric transducer to a voltage-responsive electric control circuit, and more particularly to a circuit for performing the coupling function in a reliable manner, despite the high impedance of the piezoelectric transducer output. The circuit is adapted for use with a keyless access system in which access to a locked area is obtained by the operation of a series of numbered or lettered buttons in a predetermined sequence.
A number of patents has been allowed for such access systems, among which is Haygood et al, U.S. Pat. No. 4,205,325 which discloses a sophisticated system wherein an operator selectively enters a five digit number into a keyboard on the door of a vehicle in order to gain access, open windows or trunk, etc. The keyboard has an individual switch for each key, and closure of the switch is achieved by pressing the associated key so that the operation is analagous to the selective depressing of a series of old fashioned push buttons.
Other patents relating to access systems are Ligman et al, U.S. Pat. No. 4,206,491 and Kompanek, U.S. Pat. No. 4,190,785. Patents relating to touch sensitive piezoelectric transducers and their manufacture are Kompanek U.S. Pat. No. 4,193,010 and Kompanek U.S. Pat. No. 4,056,654.
SUMMARY OF THE INVENTION
A piezoelectric sensor is used to detect the manual actuation of a touch button. The electric signal given off by the piezoelectric sensor is used to control electronic circuitry which, in turn, controls mechanical equipment, such as the bolt of a door lock. Since the output of the piezoelectric sensor is at an exceedingly high impedance level (of the order of the impedance level of ambient static electricity on a dry day) it is difficult to couple the signals from the piezoelectric sensor to electronic circuitry.
In the instant invention the piezoelectric sensor is coupled to an adjacent CMOS (complementary metal oxide-silicon field effect transistor), which normally has an enormous input impedance. Thus, there is a good impedance match, as is required for transfer of signals from the sensor to the CMOS. The CMOS is protected against excessive voltage input (which would destroy the thin insulating layer of the gate structure) by clamps which limit the maximum swing of the input signal to the range defined by the positive and negative sides of the transistor bias supply, +V DD and -V SS , respectively. In the disclosed embodiment these voltages are +5 and zero, respectively. Normally the voltage swing caused by manual actuation of the piezoelectric sensor can be much larger, but no harm is done by clipping the larger signal, for the limited input swing is more than ample to swing the binary output signal of the CMOS between high and low.
The piezoelectric sensor produces the desired output when it is stressed by a manual touch. However, the piezoelectric sensor also produces an undesired pyroelectric signal whose magnitude is roughly as large as the piezoelectric signal. The pyroelectric signal is caused by ambient temperature changes. Thus, the CMOS circuitry may respond improperly or not at all to the piezoelectric signal, which may be swamped by the unpredictable pryoelectric signal. The pyroelectric signal can also remain high for long periods of time.
In order to distinguish between the two kinds of signals, use is made of the fact that the piezoelectric signals, caused by the stress of manual touching, vary much more rapidly than the pyroelectric signal changes, caused by thermal changes.
This is done by periodically and briefly shorting together the positive and negative sides of the CMOS bias supply, so that the output of the piezoelectric sensor is briefly clamped to zero volts. Thus, the circuit is periodically restored to a zero voltage reference state, without the use of a shunting resistor on the output of the piezoelectric sensor.
The periodic shorting of the bias supply does not interfere with sensing of piezoelectric signals because a normal manual touch will cause increasing stress during several cycles of the shorting. On the other hand, the build up of a pyroelectric signal within one cycle is insufficient in magnitude to swamp the piezoelectric signal resulting from manual touching of the sensor.
THE DRAWINGS
FIG. 1 is a schematic diagram showing a piezoelectric sensor coupled to a CMOS which is powered by a pulsed bias supply; and
FIG. 2 is a group of aligned graphs showing conditions at different times in the circuit of the invention.
DETAILED DESCRIPTION
Apparatus according to the invention includes a touch-sensitive piezoelectric sensor 10, represented by the conventional symbol for a piezoelectric device. The actual construction of such a sensor may be as disclosed in the patent to Kompanek, U.S. Pat. No. 4,190,785. In any event, the sensor has a piezoelectric element 11 which, when stressed by touching of the touch pads of the sensor, will develop a direct voltage between its upper and lower surfaces by electric charge transfer within the body of the piezoelectric element 11. The voltage, by capacitive coupling, appears as a voltage between the electrodes 12 and 14. Since this voltage is the result of a charge transfer, and since the amount of the charge is directly proportional to the stress and therefore limited, it follows that this voltage has no power behind it, and cannot drive a continuing current. This voltage must therefore be sensed by equipment which draws no significant current from the piezoelectric sensor 10.
The piezoelectric sensor 10 produces the piezoelectric voltage instantaneously and in direct proportion to the pressure of an operator's finger on the pressure pad, since electric output is directly proportional to stress. When an operator operates the pressure pad rapidly, in the manner of a typist, the finger pressure will increase monotonically for a period of, perhaps, twenty-five milliseconds, level off during perhaps another twenty-five milliseconds, and then taper off to zero during perhaps another twenty-five milliseconds. In the operation of the circuit described below, the fact that the minimum rise time of the piezoelectric voltage is, roughly, in the range of twenty-five milliseconds, is significant.
Besides the piezoelectric signal, the sensor 10 also produces a pyroelectric signal having a magnitude comparable to that of the piezoelectric signal. The pyroelectric signal is produced instantaneously with a change of temperature, but temperature can change only slowly. For example, there is considerable thermal resistance between an operator's fingertip and the piezoelectric element 11, since there conventionally is a pressure pad and other items such as a waterproof membrane and a protective structural barrier between. Thus, a warm fingertip will cause only a slow temperature rise. A change of temperature caused by a large source of heat, such as the sun shining on the automobile, also causes a relatively slow temperature rise of the piezoelectric element 11, which is partly protected against rapid temperature changes by the thermal inertia of its mounting housing. In the operation of the circuit described below, the fact that the minimum rise time of the pyroelectric voltage is perhaps a second or so, also is significant.
The electrical output at electrode 14 is referenced to ground and the resulting single ended electrical output from electrode 12 is connected to the input terminal 21 of CMOS (complementary metal-oxide-silicon field effect push-pull amplifier) 20, which is also referenced to ground at its negative bias supply terminal 22. Positive bias is applied to positive bias terminal 23.
The CMOS 20 may be of any several commercial types, such as the 4009, 4010, or 4069, manufactured by RCA, Motorola, and others. These amplifiers have incorporated into the semiconductor chip in which they are formed excess-voltage protective means on both the input and output sides of the amplifier. The excessive voltage protective means on the input side are formed by clamping diodes 24, 25, and 26 and resistor 27 Diode 24 and diode 25, in conjunction with resistor 27, prevent the input signal, applied to the two field-effect transistors 30 and 31, from going significantly more positive than the positive voltage V DD at positive bias terminal 23. Diode 26, in conjunction with resistor 27, prevents the voltage from going significantly more negative than the grounded reference voltage V SS at negative bias terminal 22. The internally grounded capacitor 28, in conjunction with resistor 27, prevents the application of any over voltage from high voltage spikes, such as those from nearby discharges of static electricity. Thus, the field effect transistors 30 and 31 are protected against having their oxide barrier pierced by excessive input voltage.
If the input voltage at terminal 21 has a magnitude in the range between the voltages of bias supply terminals 22 and 23, the diodes 24, 25, and 26 will not conduct. Accordingly, the electrode 12 of the piezoelectric sensor 10 is connected to gates 32 and 33 of field effect transistors 30 and 31 by a circuit which has no shunt resistive loading and negligible shunt capacitive loading, since the CMOS 20 is adjacent to the piezoelectric sensor 10. Thus, any voltage developed by piezoelectric sensor 10 is applied to the gates 32 and 33 with substantially no loss. Under this condition, the enormous output impedance of the piezoelectric sensor 10 is well matched to the enormous input impedance of gates 32 and 33, in parallel.
If, on the other hand, the input voltage at terminal 21 is at a level beyond the range delimited by the voltages of bias supply terminals 22 and 23, the voltage clamping diodes 24 and 25 or 26 conduct and the input impedance at 21 is low.
The output terminal 40 may be connected to logic circuits, not shown, which can be used for any selected one of a wide variety of uses. For example, the output may be used to lock or unlock a door or ignition circuit. The logic circuits should be compatible with the CMOS 20, so CMOS logic curcuits are preferred.
Bias voltage is applied to terminal 23 from a +5 volt source terminal 50 by way of two resistors, 51 and 52. The junction 53 between resistors 51 and 52 is connected to the collector of grounded emitter NPN transistor 54. The base of transistor 54 is driven by a differentiated square wave signal. This is obtained from a square wave signal 55, having a repetition rate of about 125 pulses per second, applied to terminal 56. The square wave is differentiated by capacitor 57 and resistor 58, having a time constant of a few microseconds, to produce the pulse train or wave 59 having alternate positive and negative spikes.
When the base of NPN transistor 54 is pulsed highly positive by the positive pulses of the wave 59, transistor 54 conducts heavily and pulls down the potential of junction 53 substantially to ground potential for a period of about a microsecond, after which the lessening amplitude of the short positive spikes of wave 59 no longer are effective to keep NPN transistor 54 in a conductive state. When the base of transistor 54 is at ground potential or when it is pulsed negatively the transistor 54 also is not conductive. Thus, about every 8 milliseconds the CMOS 20 is deprived of bias between terminals 23 and 22 for a period of about 1 microsecond. During that brief period, any voltage supplied to input terminal 21 by electrode 12 will be shorted to ground.
The operation of the system of FIG. 1 is best understood by reference to the six aligned time graphs of FIG. 2. Graph A shows the variation in contact pressure in newtons of a conventional quick finger stroke on a touch pad. During an attack phase lasting 32 milliseconds the force on the touch pad increases. During a dwell phase of 32 milliseconds the force is constant. During a release phase of 32 milliseconds the force decreases. While this representation may be rather crude, it does not differ grossly from reality, and the assumptions of the representation simplify the explanation.
The solid line of graph B shows the resulting piezoelectric voltage generated by operation of the sensor 12. For purposes of explanation the voltage is represented as increasing positively during the attack phase, so that the circuit is activated on the attack phase. (If the leads from electrodes 12 and 14 were reversed, the piezoelectric voltage would be negative during the attack phase, and the circuit would not be activated until the release phase, when the piezoelectric voltage would, under that condition, be positive). The piezoelectric voltage graph B is similar to the force graph A, since piezoelectric voltage is directly proportional to stress.
The dotted line labeled pyroelectric in graph B will be discussed below.
Graph C shows the CMOS bias voltage at terminal 23. The bias is essentially continuous and constant at +5 volts, but is interrupted every 8 milliseconds for a brief moment, shown greatly exaggerated in the time dimension, of about one microsecond in duration. Thus, the duty ratio of the bias supply is 7999 to 1.
When the bias supply at bias terminal 23 is interrupted for the brief period of about one microsecond, any positive voltage present at the gates 32 and 33 is shorted to ground through clamping diodes 24 and 25. Such voltage may be caused by a charge transfer within the piezoelectric element 11, and when the short is removed, by reenergization of the positive bias terminal 23, the voltage does not restore itself. Consequently, as shown by graph D, the voltage at the input terminal 21 stays at zero when the piezoelectric sensor has no output, and it is held clamped at zero during those moments of the attack phase when the bias supply at bias terminal 23 is zero. However, throughout the attack phase the piezoelectric element 11 is being increasingly stressed, and continues to produce further charge transfer in accordance with the stress, resulting in a voltage build up at the rate of 10 volts every 32 milliseconds (see graph B), resulting in a steeply rising triangular wave, as shown by the slanted voltage rises of graph D. When the rise reaches +5 volts, it causes the clamping diodes 24 and 25 to conduct, and the triangular wave is truncated at +5 volts, as shown in graph D.
During the dwell phase no further charge transfer occurs within piezoelectric element 11, and the clamped sensor voltage of graph D therefore stays at zero voltage.
During the release phase, the piezoelectric sensor 10 has a tendency to output a negative signal because of the descending open-circuit sensor voltage of graph B and because of the intermittent clamping to zero voltage. However, the voltage at the gates 32 and 33 cannot go negative because of the action of clamping diode 26.
The particular CMOS amplifier 20 illustrated in FIG. 1 has a configuration which makes it an inverter. Thus, the clamped sensor voltage wave of graph D appears as an inverted output wave, as shown by graph E. Before being used by the logic circuits controlled by the piezoelectric sensor 10, the inverted wave would be subjected to low pass filtering, producing the final output voltage wave shown in graph F. The wave form shown in graph F has a shape which is satisfactory for controlling logic circuits.
When a piezoelectric element, such as 11, is directly connected to an amplifier without any shunt loading, the amplifier will respond to both the piezoelectric and pyroelectric signals from the piezoelectric element. The piezoelectric and pyroelectric signals can be of comparable magnitude. However, the piezoelectric signal is proportional to stress, which can change rapidly, as, for example, during the attack phase. The pyroelectric signal, on the other hand, is proportional to change of temperature, which normally occurs much more slowly. Thus, in graph B, a possible pyroelectric signal is shown in dotted lines which slannts negatively at a gentle slope. It is apparent that, when the slowly changing pyroelectric signal is added to the more rapidly changing piezoelectric signal, the shape of graph D will not be appreciably altered. The rapidly changing signal swamps the effects of the slowly changing signal because of the intermittent action of the clamping diodes, which restores both signals back to a zero reference level.
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The high impedance output of a touch-sensitive piezoelectric sensor is coupled directly to the high impedance input of a CMOS (complementary metal oxide silicon field effect transistor pair). The CMOS is protected on its input side by clamps which restrict the voltage swing applied to the gates to within the range defined by the positive and negative CMOS bias supply (+V DD and -V SS ). The sensor produces voltages of approximately equal magnitude in response to slow acting temperature changes and quicker acting manual touching. In order to distinguish piezoelectric from pyroelectric signals, the CMOS bias is periodically and briefly shorted, to ensure a brief return-to-zero of the sensor output, thereby effectively suppressing the slow acting pyroelectric signal without interfering with sensing of quick acting piezoelectric signals.
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This is a continuation-in-part application of my impending Ser. No. 478,284 filed on June 11, 1974, and now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to the particleboard art generally with particular reference to a product that is pressed and molded in a single operation to form a panel-like building component containing integral support members.
(2) Description of Prior Art
In conventional wood-frame building construction, framing members (studs, joists, or rafters), are covered with lumber, or wide flat panels, to form walls, roofs, and floors. For example, sheathing, often in the form of plywood panels is applied to the exterior surface of the vertical framing support members, or studs, in conventional wall construction. Currently, such sheathing and studding are distinct, separable components.
At a time when factory production line techniques for producing house components are becoming a reality, and lumber quantity and quality are declining, a more economical product, which incorporates the desirable characteristics of both sheathing and framing members, is highly desirable. The invention incorporates these characteristics. In addition, lower grade or previously unusable wood in the form of forest residues can be used in producing the invention as opposed to the higher grade of wood used to make the separate plywood and framing members of conventional frame construction.
The process used to manufacture the product essentially follows the flat-pressed particleboard process with the exception that caul plates and platens having the desired shape are used. Forming the shape, which incorporates walls at steep angles to the horizontal plane, does not necessarily depend on the material "flow" essential to closed mold operations, but is dependent on the interaction between material type, initial mat formation, and proper die configuration to hold, shape, and form the product. German Patent No. 2,035,953 describes methods of producing articles with steep sidewalls such as are essential to form the framing portion of our product.
The inventors are unaware of any press-molded cellulosic replacement for conventional roof, wall, or floor components which incorporates both framing and sheathing members into one integral unit.
SUMMARY OF THE INVENTION
The invention disclosed is a building component of cellulosic particles and adhesive binder that is press-molded in a single operation to form a panel with integral support or framing members. The particleboardlike product may be formed in standard press equipment except that the press must be modified by the substitution of dies for regular flat platens. As will be disclosed, the cellulosic particles and adhesive binder are felted into a mat on a caul plate having a shape similar to the lower die or platen. The mat and caul plate are then inserted between the heated upper and lower shaped platens whereupon the press is closed and the mat is pressed and molded to the predetermined configuration.
The lower die basically has a flat horizontal surface indented with a plurality of parallel troughlike depressions running its length. Each depression generally has steeply inclined sidewalls and a more or less flat bottom. The sidewalls themselves may be grooved (i.e., having a series of steps running the length of the die) or smooth. The depth and width of the depressions, angle of sidewall inclination, and the surface configuration of sidewalls is determined by the exact requirements of the desired product and type of material to be pressed.
The upper platen serves as the male portion of the die and has the same general configuration, in reverse, as the lower portion, i.e., a basically flat surface with a plurality of parallel ridgelike projections corresponding to the depressions mentioned. These projections in the upper die are not necessarily, and most unlikely to be, exact reverse images of the depressions in the lower die. The projections may be grooved or smooth. Like the lower die, the width and depth of the projections, angle of inclination of the sidewalls, and surface configuration of the projection walls is determined by the requirements of the final products and characteristics of the material to be pressed. When positioned prior to pressing, it is important that the projections in the upper die be directly alined with the lower die depressions to obtain a symmetrical product.
This depression and projection combination in the dies serve to channelize the final panel product at regular intervals. We have therefore termed these regular combinations of depressions and projections as channels.
It is this resulting series of channels which give the panel the strength and support of conventional 2 by 4 stud-and-sheathing construction. As such, the between-channel spacing may be a standard 16 or 24 inches or varied to meet structural requirements.
The material type used is, to a certain extent, determined by the shape of the channel. Deep channels with steep sidewalls, for example, are best formed using a material with a low bulk density, such as fiber or planer shavings or a combination of material types having low bulk density such as a flake and fiber mix.
The type and amount of binder employed, additives, presstime, temperature, and mat moisture control are all matters of choice for a skilled operator within the ranges utilized for standard particle- or fiber-board manufacture.
The inventive product, after removal from the press, has assumed the die configuration, i.e., a panel having smooth, flat sections interrupted at regular intervals with channels. Between the flat sections on one side of the panel are parallel, evenly spaced projections, each of which is made up of paired sidewalls which are inclined toward one another, but which culminate in a flat bottom parallel to the flat sections previously mentioned. Accordingly, an object of this invention is a product designed to absorb loads such as wind, snow, or other forms of stress; and transfer the load directly to the ground or to other members in contact with the ground, e.g., the lower plate. This eliminates the need for framing as required by the prior art as those products absorbed loads and transmitted those loads to the frame. Also, a panel having smooth, flat sections on both sides interrupted by a plurality of parallel evenly spaced projections differs from the prior art characterized by a wavelike pattern. These structural differences determine the use to which the respective products may be put. On the opposite side of the panel is found the inverse design, i.e., parallel and evenly spaced depressions between the flat sections. These projections and depressions, in effect, form the channels mentioned and such channels give the panel strength and serve as support members. In the manufacture of standard 4- by 8-foot wall sections, for example, a plurality of evenly spaced depressions will run parallel to the 8-foot length on the outer, or sheathing side. Evenly spaced on the reverse or inner side are a plurality of correspondingly located flat-top ridgelike projections running the product's length. When the product is so used as a wall section, the panel is fitted with a top and bottom plate (normally constructed of 2- by 4-inch lumber routed out on the 4-inch face with a pattern to match the panel) along both of its 4-foot edges, and exterior siding is applied to the outer or sheathing side. Interior wall material, such as rock lath, paneling, or gypsum board is then nailed to the flat tops of the projecting support members, on the inner side, much the same as application over 2- by 4-inch studs in the more conventional mode of construction.
Accordingly, an object of the invention is a press-molded panel that combines the previous dual components of sheathing and framing support members. A further object of the invention is the provision of a readily made panel that substantially reduces material handling costs while decreasing setup or installation time at a construction site. Another object of the invention is an integral multipurpose panel product that serves as sheathing and framing for wall, roof, and flooring applications. A final objective is the provision of a panel which is simply and economically molded from residue cellulosic material to thereby aid in conserving our timber resources.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-sectional view of the panel being pressed and molded by the dies.
FIG. 2 is a perspective view of the panel after its emergence from the press.
FIG. 3 is a perspective view of the panel being used as a wall section.
FIG. 4 is a detailed view of a portion of the panel being fitted to a plate when the panel serves as a wall section.
FIG. 5 is a perspective view of the panel being utilized as a floor section.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
When press-molding a panel having channels with rather steep sidewalls, selection of the raw material is somewhat critical because different die configurations may dictate necessary changes in material types. Material "flow" is essentially absent and the form is achieved, without adverse tearing of the mat or detrimental density differences within the panel, by selecting and using the proper combination of material type, die configuration, and mat preparation.
Fibrous "furnishes" having a low bulk density of from 2 to 3 pounds per cubic foot (pcf) work very well in our preferred die configuration. These are described as individual wood fibers 0.5 to 9.5 millimeters in length or groups of fibers in bundles. Panels have been made, however, from planer shavings (bulk density from 3 to 5 pcf), having thickness from 0.005 to 0.050 inch, widths of 0.1 to 1 inch and lengths from 0.5 to 3 inches. Panels have also been made from flakes or splinters, within the same dimension range as described above for planer shavings but having bulk densities from 5 to 7 pcf. The difference between planer shavings, flakes, and splinters arises from their method of preparation. Planer shavings are smooth cut and usually of varying thickness throughout the length of the shaving and tend to curve. This provides for a relatively low bulk density. Flakes are smooth cut, but have a constant thickness throughout their length. Splinters have rough surfaces and, therefore, vary in thickness throughout the length.
Because the described material does not flow when molding, the transformation of the matted material to the proper locations in the die is in part determined by the bulk density of the material. Bulk density is determined by the size and form of the particles. That material which has a low bulk density creates a thick loose mat if the proper mat configuration is created, and the dies are shaped correctly. The press upon closure will force the material into the proper locations. With low bulk density material, the adjustment in material location begins while the press is relatively far open and continues while the mat stays relatively loose. In pressing a high bulk density material the mat has only a short time and small distance to be acted on by the press forces prior to reaching final dimension and since the mat is relatively tight, resists forces to a greater degree than a low bulk density mat. The size of particle also determines the strength of the final product. The longer particles have more chance to overlap and become bonded to several other particles than short particles. Thin particles raise the compression ratio, create better bonding conditions, and result in stronger boards. Particles over 0.050 inch thick do not conform well to molding forces and give relatively lower strengths. Larger particles generally have higher bulk density properties. This is not always the case as described previously for planer shavings where because of the curl the shavings have a relatively low bulk density. In any event, the selection of proper material for the manufacture of a "no flow" molded structural member becomes a tradeoff between materials having low bulk density and low strength and those having a high strength but a high bulk density. Particle size selection will vary therefore with the die configuration and product strength requirements and may be a combination of sizes and types as described in a previous section.
The cellulosic material is prepared in a manner consistent with that employed in manufacturing regular particleboard. The material is first dried and then sprayed, coated, or mixed with a suitable adhesive binding usually a synthetic thermosetting resin, amounting to from 3 to 8 percent of the ovendry (O.D.) weight of the raw fibrous material. Suitable binders such as urea-formaldehyde, phenolformaldehyde, resorcinol, melamine, urethane, or isocyanate may be used. Other substances may be added at this stage such as waxes to improve weathering characteristics or borates to increase fire resistance.
The prepared material is then spread to form a mat on the caul plate. With a material having a low bulk density, prepressing the material in the caul plate troughs promotes a more uniform wall density.
Again, when certain raw fibrous material types are used, panel formation is aided by depositing ridges of material on the top of the mat parallel to and directly above the edges of the troughs. This provides sufficient material to obtain uniform density in the sidewalls.
The amount of the material used in mat formation is dependent on the final desired density and thickness of the panel.
Following prepressing of the felted mat, if this be desirable, the caul and mat are inserted into the lower section of the die which serves as the bottom platen of the hot press. The top platen has the shape of the top die. Referring now to the drawings, FIG. 1 shows panel 11 in a cross-sectional view during the press-molding operation. Upper die 12 has a projecting portion 13 which runs the length of the die. It is noted the sidewalls 14 of projection 13 are smooth as the inventors prefer, but they may also be stepped as sidewalls 17 of lower die 15 are. Caul plate 16, of course, has the same configuration as the surface of lower die 15. Sidewalls 17 in combination with flat bottom 18 create a trough in lower die 15. It is noted that projection 13 need not be an exact mirror image of the trough. A skilled operator may find a preference for the stepped sidewalls 17 of lower die 15 since such steps tend to hold the raw material and prevent its being pushed or slipping into the lower part of the trough during pressing. This is particularly true if the lower die has quite steeply inclined sidewalls and less so if the angle of incline is small. The trough extends the length of die 15 and it is noted that the upper and lower dies, 12 and 15 respectively, must be constructed such that the projection 13 of the upper die 12 and the trough of the lower die 15 are directly alined. Although only one projection of the upper die and one trough of the lower die are depicted, the dies in actual use would have a plurality of such alined projections and troughs. These projections and troughs form the support member sections of panel 11, and may be placed at 16-, 24-inch, or other intervals depending on the design criteria of the final use.
Returning now to the pressing operation, after insertion of the caul and mat into the press, the press is closed and the mat pressed and cured to final shape. Presstime, pressure, moisture content, and all the variables associated with mat formation and pressing are subject to the variations encountered in producing flat particleboard and as such may be altered by a skilled operator to ensure the best panel formation.
Product handling and end-use requirements will dictate actual manufacturing techniques such as press size, type, and mat felting methods. For example, when the panel is to be used as a wall section where the height of the panel (distance parallel to the channels) is essentially 8 feet, the panel might conceivably be produced on an 8-foot-wide continuoustype press wherein the channels run across the width of the press. If the panel is to become a floor or roof component, where spans greater than 8 feet are common, it may be desirable to manufacture the panel in a 4-foot-wide by 24-foot or longer press whereas the channels would run parallel to the press length.
After emergence from the press, the panel is cooled and trimmed in preparation for its use as a structural building component.
Referring again to the drawings, FIG. 2 shows the invented panel 11 after removal from the press and cooling. Panel 11 has a number of flat sections 19 separated by channels 20. Channels 20 are parallel to one another and each channel is equidistant from its next adjoining channel. Each channel 20 consists of a pair of sidewalls 21 which are inclined toward one another but culminate in a flat bottom 22, which is parallel with the flat sections 19 described above. As a way of showing the alternatives available, it is noted in FIG. 2 that the surface of the sidewalls 21 are smooth on the projecting side of the channel and stepped on the depressed side. This is the reverse of that depicted in FIG. 1. The "depth" of each channel, i.e., the distance between flat section 19 and flat bottom 22, being measured perpendicular to each, is a matter of choice with the operator and would roughly correspond to the depth of the conventional support member replaced by channels 20, such as a 2 by 4 stud. For descriptive purposes, the side of panel 11 where the channels 20 project will be termed the interior side of the panel since the support members for wall and roof applications would normally be on the interior side of the frame building. The opposite side will be termed the exterior side of panel 11 because exterior materials will be applied to that side in normal building construction. The exterior side of panel 11 is depicted in FIG. 2. The shape of panel 11 further facilitates later shipment to construction sites because a plurality of panels is easily nestled together to create a high density package.
FIG. 3 is a more complete view of the invention utilized in forming a wall section. The wall could be formed from a single panel 11 cut out and framed to form the windows. The wall may also be built by using the invention to construct smaller individual sections, i.e., wall 11, window header 11 feet and window base 11 inches and fastening these sections together. When used as a wall, the integral support members or channels are stressed as a column in compression and the whole panel is subjected to racking-type forces. As demanded by the application, panel 11 may be constructed with increased density through the channel section to better resist the compressive force.
FIG. 4 shows plate 23 routed to fit the invention, and more specifically the flat sections 19, and the sidewalls 21, and flat bottom 22 of channel 20. Plate 23 is used in conjunction with panel 11 when wall sections are being formed. The design of plate 23 allows its use as either a top or bottom plate.
FIG. 5 shows panel 11 being used as a floor section. The channels 20 and flat sections 19 of panel 11 in effect incorporate the joists and subfloor, respectively, into a single integral unit. Channels 20 are seated in joist header 24 and underlayment (not depicted) will be applied over panel 11. Unlike the columnar stress as a wall section, when panel 11 serves as a floor section the support members or channels 20 must withstand the forces associated with a beam stressed in bending. The stiffness of the floor may be altered (and thereby its maximum design span) by changing the channel 20 design and/or increasing the stiffness of the channel 20 portion. The latter goal is accomplished by densification, use of longer flakes, and/or alining the flakes. With the process and materials used in constructing panel 11, any of the above alternatives is possible.
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A wood-base building component of cellulosic particles and/or fibers and adhesive binder is, in a single pressing operation, molded into an integral product of sheathing and support members for use in constructing wood-frame buildings. The dies utilized during press-molding form a flat panel containing a plurality of evenly spaced channels that serve as support members to replace conventional framing such as studs, joists, and rafters. The integral product may serve as roof, wall, or flooring components in the usual wood-frame building applications.
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This is a continuation of application Ser. No. 08/258,556, filed on Jun. 10, 1994, now U.S. Pat. No. 5,476,111.
FIELD OF THE INVENTION
The present invention relates generally to the field of manufacturing ophthamalic lenses, especially molded, hydrophilic contact lenses, and more specifically, to a high speed automated method and apparatus for demolding and hydrating the lenses after polymerization.
DESCRIPTION OF THE PRIOR ART
The molding of hydrophilic contact lenses is disclosed in U.S. Pat. No. 4,495,313 to Larsen, U.S. Pat. No. 4,565,348 to Larsen, U.S. Pat. No. 4,640,489 to Larsen et al., U.S. Pat. No. 4,680,336 to Larsen et al., U.S. Pat. No. 4,889,664 to Larsen et al., and U.S. Pat. No. 5,039,459 to Larsen et al., all of which are assigned to the assignee of the present invention. This prior art discloses a contact lens production process wherein each lens is formed by sandwiching a monomer or a monomer mixture between a front curve (lower) mold section and a back curve (upper) mold section, carried in a 2×4 mold array. The monomer is polymerized, thus forming a lens, which is then removed from the mold sections and further treated in a hydration bath and packaged for consumer use. During polymerization, particularly of the hydrogels, the lens tends to shrink. To reduce shrinkage, the monomer is polymerized in the presence of an inert diluent like boric acid ester as described in the above patents, which fills up the spaces in the hydrogel lens during polymerization. The diluent is subsequently exchanged for water during the hydration process.
The prior art process of exchanging the diluent for water and hydrating the lens has been very time consuming. The two part molds are opened and the lenses are assembled in large groups and placed in a leaching tank for several hours. The leach tank includes heated water, small amounts of surfactants and salts. When the lenses are inserted in the leach tank they immediately expand in the presence of water and release from the mold in which they were molded. The boric acid ester diluent hydrolizes into glycerol and boric acid leaving the water behind in the matrix of the lens to thus exchange diluent for water to hydrate the lens.
Salts and a pH buffer are used in the water so that the water placed in a lens has an osmolality and pH substantially similar to that of human tears so that the lens will not irritate the eye when it is inserted by the user. If the polymer from which the lens is made has ionic characteristics, the buffer neutralizes any ionic species in the lens. That neutralization causes temporary destabilization of the dimensions of the lens and requires an extended period of time to complete.
The lenses are then transferred to a rinse tank where removal of diluent and surfactant continues for another extended period of time. The lenses are then transferred to a large equilibration tank filled with heated water and salts for completion of diluent and surfactant removal and equilibration of the lens for several more hours. The equilibration step entails completion of the neutralization of any ionic species in the polymer from which the lens is made. The lens is then removed from the equilibration tank and rinsed in clean saline and transferred for inspection and packaging.
U.S. Pat. Nos. 5,080,839 and 5,094,609 disclose respectively a process for hydrating soft contact lenses and a chamber for hydrating contact lenses which represent a substantial improvement over the foregoing prior art process. These patents teach the use of a unique chamber formed of a male and female member which forms a hydration cavity which permits the hydration of the lens without permitting it to invert or roll over. Fluid flow is introduced into the cavity about the lens from each side to extract leachable material from the lens. The process significantly reduces the amount of leaching fluid that is used and the amount of time that is needed for hydration, washing and extraction. The apparatus disclosed in these patents enabled placement on a frame suitable for automated handling. The process significantly reduced the through-put time by hydrating the lens and releasing the lens from the mold cavity with deionized water and a small amount of surfactant without any salts, so that the time consuming ionic neutralization of the polymer from which the lens blank is made does not occur during the hydration process. When deionized water is used, the final step of the process is to introduce buffered saline solution into the final package with the lens and then sealing the lens within the package so that final lens equilibration (ionic neutralization, final hydration and final lens dimensioning) is accomplished in the package at room temperature or during sterilization.
As taught in these prior art references, the use of deionized water is an important step in this process because it allows the time consuming ionic neutralization to be done essentially outside the hydration process after the lens has been packaged and sealed.
While the chamber and process described in the foregoing patents enabled automated handling of the lens during hydration, suitable automated equipment to handle these chambers at high production rates and implement this process in a fully automated apparatus was not readily available or taught by the prior art.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide an automated process and apparatus that will enable high production rates in the hydration process disclosed in U.S. Pat. No. 5,080,839. It is a further object of the present invention to provide a high speed robotic apparatus to facilitate the handling and manipulation of lens molds having a molded hydrophilic contact lens therein and the chambers described in U.S. Pat. No. 5,094,069 in a high through-put, high production rate automated apparatus.
It is an object of the present invention to provide an automated means for hydrating a molded hydrophilic contact lens wherein a first robotic assembly removes a plurality of contact lens molds from a production line carrier, wherein each of the lens molds has a contact lens adhered thereto. The first robotic assembly assembles the molds with a lens transfer means to form a first hydration carrier, and then hands the first hydration carrier to a second robotic assembly which immerses the first hydration carrier in a hydration bath to hydrate the lens and to release the lens from the lens mold. During transit through the hydration bath, the lens is transferred from the mold to the lens transfer means. After a predetermined period of time, the second robotic assembly removes the first hydration carrier from the hydration bath and hands the carrier off to a third robotic assembly which removes the molds from the lens transfer means, flushes the lenses carried on the lens transfer means and then transports the lens transfer means and lenses to a second hydration carrier to form a second hydration carrier for the extraction/flushing/hydration of the lens in subsequent processing stations. The second hydration carrier is then transported through a plurality of flushing stations wherein fresh deionized water is introduced into the hydration chambers at each hydration station to flush leachable substances from the hydration chamber. During transit travel between flushing stations, the residual fluid in the hydration chamber extracts impurities from the contact lens through mass transfer exchange. At each flushing station, fresh deionized water is introduced into the hydration chamber to remove previously extracted impurities and the products of hydrolysis. Finally, a final robotic assembly separates lens transfer means from the hydration base, to provide fully hydrated lenses in a concave lens holding means ready for inspection and packaging.
It is an object of the present invention to provide a method and apparatus for the high speed robotic handling of soft, wet and slippery contact lenses, primarily through fluid flow devices, which transport the lens and move it from carrier to carrier without physically damaging the lens, losing the lens, or allowing it to invert or roll over.
It is also an object of the present invention to provide a method for handling the lenses which will minimize the formation of air bubbles which might otherwise impair subsequent handling of the lens in a fluid transfer media.
It is further an object of the present invention to provide a robotic handling device that will quickly and efficiently secure a large number of discreet individual molds having a molded contact lens therein, and then eject said discreet mold parts after said lens has been released and transferred to a lens carrier. It is further an object of the present invention to provide a high speed robotic device for handling a plurality of contact lenses which secures the contact lenses to the lens carrier elements with surface tension, and releases the lenses from the carrier elements via fluid flow of air or water.
It is another object of the present invention to provide a device for transporting a plurality of first hydration carriers through a hydration bath from a first pick and place robotic assembly to a second pick and place robotic assembly which removes the first hydration carrier from the hydration bath.
It is another object of the present invention to provide an automated control means for sequencing and coordinating each of the robotic assemblies used in the transfer of lenses from the production line pallet, through hydration and extraction stations, and finally to an inspection carrier.
While the invention is described with particular reference to molded contact lenses wherein the lens is molded between a first and second mold half, it is understood that the hydrating apparatus is equally suitable for the hydration of lenses formed by lathe cutting wherein the hydrogel is maintained in a dry state while the desired optical surfaces are cut and polished. Further, the process may be used with spin cast lenses which subject a liquid monomer to a centrifugal force in a mold which has the same shape as the desired optical surface of the lens.
It is an object of the present invention to provide an automated process and apparatus for hydrating contact lenses where the volume of solution used to release and hydrate the lens is significantly reduced, and to significantly reduce the quantity of chemicals used in the hydration process.
It is another object of the present invention to provide a high speed automated apparatus and method to remove leachable substances with water, alcohol, or other organic solvents, or a mixture thereof, thus flushing unreacted monomers, catalysts and/or partially reacted comonomers, diluents or other impurities from a hydrophilic contact lens.
Finally, it is an object of the present invention to provide a high speed automated method and apparatus for hydrating contact lenses formed in an automated production line as more fully described in Application Serial No. 08/258,654, of W. A. Martin, et al. entitled "Consolidated Contact Lens Molding", the disclosure of which is incorporated herein by reference thereto.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing objects and advantages of the present invention for an automated method and apparatus for hydrating soft contact lenses may be more readily understood by one skilled in the art with reference being had to the following detailed description of the preferred embodiments, taken in conjunction with the accompanied drawings, wherein like elements are designated by identical reference numerals throughout the several views, and in which:
FIG. 1 is a top plan view of the apparatus of the present invention illustrating in block form the arrangement and relative location of each of the robotic handling devices of the present invention.
FIG. 2 is a schematic illustration of the relative motion imparted by each of the robotic handling devices as the lenses are transported through the hydration apparatus of the present invention.
FIG. 3 is an elevation view of the apparatus illustrated in FIG. 1 illustrating in block form and schematic form the principle components of the present invention.
FIG. 4 is a planar view of the top chamber plate which is utilized as a lens transfer device in the present invention.
FIG. 5 is an end view of the top chamber plate illustrated in FIG. 4.
FIG. 6 is a partially cross-sectioned side or elevation view of a hydration base carrier utilized in the present invention.
FIG. 7 is a top or plan view of the hydration base carrier illustrated in FIG. 6.
FIG. 8 is a top plan view of a production line pallet which may be used to provide contact lens molds and lenses from the automated production line to the present invention.
FIG. 9 is a partially cross-sectioned elevation view of a single lens transport means of the first hydration carrier, formed by the top chamber plate of FIGS. 4 and 5 with a contact lens mold and contact lens secured thereto for transport through a hydration bath.
FIG. 10 is a partially cross-sectioned and elevation or side view of a single lens transport means of the second hydration carrier formed when the top chamber plate of FIGS. 4 and 5 is combined with the hydration base carrier of FIGS. 6 and 7.
FIG. 11 is a partially cross-sectioned side view of the hydration tank of the present invention illustrating in elevation, a walking beam mechanism which transports the first hydration carrier through the hydration tank of the present invention.
FIG. 12 is a top plan view of the hydration tank illustrated in FIG. 11 as viewed from section line F--F in FIG. 11.
FIG. 13 is a cross-sectioned end view taken along section line A-A' of FIG. 11.
FIG. 14 is a sectional view taken along section line B-B' of FIG. 11.
FIG. 15 is an elevation and diagrammatic view of a first pick and place robotic assembly used in the present invention.
FIG. 16 is a top plan view of the first robotic pick and place unit illustrated in FIG. 15.
FIG. 17(a) is an end view of the first robotic pick and place unit illustrated in FIGS. 15 and 16 at an initial home position.
FIG. 17(b) is an elevational end view of the first robotic pick and place unit illustrated in FIGS. 15 and 16 immediately prior to the assembly of the top chamber plate and a plurality of contact lens molds.
FIG. 17(c) is a diagrammatic elevation or end view of the first robotic pick and place assembly at its hand-off position.
FIG. 18 is a elevation side view of a second robotic assembly of the present invention having first and second pick and place units.
FIG. 18(a) is a diagrammatic illustration of the movement of the first pick and place unit of the second robotic assembly illustrated in FIG. 18.
FIG. 18(b) is a diagrammatic illustration of the movements of a second pick and place unit of the second robotic assembly illustrated in FIG. 18.
FIG. 19 is a partially cross-sectioned elevation and diagrammatic end view of the second robotic assembly illustrated in FIG. 18.
FIG. 20 is a top plan view of a third robotic assembly used in the present invention.
FIG. 21 is an elevation side view of the third robotic assembly illustrated in FIG. 20.
FIG. 22 is an elevational end view of the third robotic assembly illustrated in FIGS. 20 and 21.
FIG. 23 is a diagrammatic illustration of the movement of the third robotic assembly illustrated in FIGS. 20-22.
FIG. 24 is an elevation end view of a lens flushing station utilized in the present invention.
FIG. 25 is a side elevation view of the lens flushing station illustrated in FIG. 24.
FIG. 26 is an end elevation view of an indexing or alignment guide utilized in the present invention.
FIG. 27 is a side elevation view of the indexing or alignment guide illustrated in FIG. 26.
FIG. 28 is a partially cross-sectioned elevation view of a flushing manifold utilized in the flushing station of FIGS. 24 and 25.
FIG. 29(a) is a diagrammatic planar view of level 1 of the manifold illustrated in FIG. 28.
FIG. 29(b) is a diagrammatic plan view of level 2 of the manifold illustrated in FIG. 28.
FIG. 29(c) is a diagrammatic plan view of level 3 of the manifold illustrated in FIG. 28.
FIG. 29(d) is a diagrammatic plan view of level 4 of the manifold illustrated in FIG. 28.
FIG. 30 is a planar view of the manifold illustrated in FIGS. 28 and 29 illustrating diagrammatically the innerconnections between manifold levels.
FIG. 31 is a side elevation view in cross-section of level 1 of the manifold illustrated in FIGS. 29(a) and 28.
FIG. 31(a) is an enlarged cross-sectional view of a portion of FIG. 31.
FIG. 32 is a partially cross-sectioned elevation end view of a hydration extraction station utilized in the present invention.
FIG. 33 is a side elevation view of the hydration extraction station of FIG. 32.
FIG. 34 is a diagrammatic plan view of a manifold utilized in the hydration extraction station of FIG. 32.
FIG. 35 is a partially cross-sectioned view of the manifold illustrated in FIG. 34.
FIG. 35(a) is an enlarged cross-sectional view of a portion of FIG. 35.
FIG. 36 is a cross-sectional end view of one layer of the manifold illustrated in FIGS. 34 and 35.
FIG. 37 is an elevation side view of the separation station utilized in the present invention.
FIG. 38 is a cross-sectioned elevation end view of the separation station illustrated in FIG. 37.
FIG. 39 is a cross-sectioned top planar view of the separation station illustrated in FIGS. 37 and 38.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is an automated method and apparatus for hydrating soft contact lenses, especially molded hydrophilic contact lenses manufactured in two-part molds in the presence of a diluent and then polymerized in the presence of a catalyst with ultraviolet light. After the polymerization process is completed, the two halves of the mold are separated or demolded with the contact lens preferentially adhered to the front curve mold half, as more fully described in Application Ser. No. 08/258,654, of W. A. Martin et al. entitled "Consolidated Contact Lens Molding". While the invention described herein is preferentially utilized in combination with the automated production line disclosed therein, it is understood that the present invention is equally suitable for the hydration of lenses formed by lathe cutting wherein the hydrogel is maintained in a dry state while the desired optical surfaces are cut and polished, or with contact lenses formed by the spin cast method wherein a liquid monomer is subjected to centrifugal force in a mold which has the same shape as the desired optical surface of the lens.
The present invention is particularly suited to the hydration of hydrophilic contact lenses formed from monomer and monomer mixtures which include copolymers based on 2-hydroxyethyl methacrylate ("HEMA") and one or more comonomers such as 2-hydroxyethyl acrylate, methyl acrylate, methyl methacrylate, vinyl pyrrolidone, N-vinyl acrylamide, hydroxypropyl methacrylate, isobutyl methacrylate, styrene, ethoxyethyl methacrylate, methoxy triethyleneglycol methacrylate, glycidyl methacrylate, diacetone acrylamide, vinyl acetate, acrylamide, hydroxytrimethylene acrylate, methoxyethyl methacrylate, acrylic acid, methacryl acid, glyceryl methacrylate, and dimethylamino ethyl acrylate.
Preferred polymerizable compositions are disclosed in U.S. Pat. No. 4,495,313 to Larsen, U.S. Pat. No. 5,039,459 to Larsen et al. and U.S. Pat. No. 4,680,336 to Larsen et al., which include anhydrous mixtures of a polymerizable hydrophilic hydroxy ester of acrylic acid or methacrylic acid and a polyhydric alcohol, and a water displaceable ester of boric acid and a polyhydroxyl compound having preferably at least 3 hydroxyl groups. Polymerization of such compositions, followed by displacement of the boric acid ester with water, yields a hydrophilic contact lens.
The polymerizable compositions preferably contain a small amount of a cross-linking agent, usually from 0.05 to 2% and most frequently from 0.05 to 1.0%, of a diester or triester. Examples of representative cross linking agents include: ethylene glycol diacrylate, ethylene glycol dimethacrylate, 1,2-butylene dimethacrylate, 1,3-butylene dimethacrylate, 1,4-butylene dimethacrylate, propylene glycol diacrylate, propylene glycol dimethacrylate, diethylglycol dimethacrylate, dipropylene glycol dimethacrylate, diethylene glycol diacrylate, dipropylene glycol diacrylate, glycerine trimethacrylate, trimethylol propane triacrylate, trimethylol propane trimethacrylate, and the like. Typical cross-linking agents usually, but not necessarily, have at least two ethylenically unsaturated double bonds.
The polymerizable compositions generally also include a catalyst, usually from about 0.05 to 1% of a free radical catalyst. Typical examples of such catalysts include lauroyl peroxide, benzoyl peroxide, isopropyl percarbonate, azobisisobutyronitrile and known redox systems such as the ammonium persulfate-sodium metabisulfite combination and the like. Irradiation by ultraviolet light, electron beam or a radioactive source may also be employed to catalyze the polymerization reaction, optionally with the addition of a polymerization initiator. Representative initiators include camphorquinone, ethyl-4-(N,N-dimethylamino)benzoate, and 4-(2-hydroxyethoxy)phenyl-2-hydroxyl-2-propyl ketone.
Polymerization of the monomer or monomer mixture in the mold assembly is preferably carried out by exposing the composition to polymerization initiating conditions. The preferred technique is to include in the composition, initiators which work upon exposure to ultraviolet radiation; and exposing the composition to ultraviolet radiation of an intensity and duration effective to initiate polymerization and to allow it to proceed. For this reason, the mold halves are preferably transparent to ultraviolet radiation. After the precure step, the monomer is again exposed to ultraviolet radiation in a cure step in which the polymerization is permitted to proceed to completion. The required duration of the remainder of the reaction can readily be ascertained experimentally for any polymerizable composition.
After the lens has been polymerized, it is demolded in preparation for the hydration process. The hydration process of the present invention is used to hydrolyze the diluent used in the monomer or monomer mixture and then extract or leach from the lens the products of hydrolysis, together with unreacted or partially reacted monomer or inhibitors, surfactants from the lens. In the hydration step, a plurality of lenses, still adhered to the mold in which they were formed, are immersed in a deionized water bath having a small amount of surfactant therein. The hydration bath hydrolizes the boric acid ester used as a diluent in the lens into glycerol and boric acid which is then exchanged by the physical phenomenon of mass transfer by the concentration gradient of the products of hydrolysis between the contact lens and the fluid in the hydration tank.
Simultaneously, the lens, in the presence of deionized water and surfactant, swells, creating a shear force with respect to the mold in which the lens was formed thereby separating the contact lens from the mold. After the contact lens and mold have been separated, they are removed from the hydration bath, the mold is discarded, and the lens is placed in a hydration chamber in a manner similar to that described in U.S. Pat. No. 5,094,609. While the lens is in the hydration chamber, deionized water is introduced through the chamber to periodically flush the chamber and permit extraction of impurities from the contact lens. As the extraction continues, the concentration gradient between the lens and each batch of fresh deionized water diminishes, and it is therefore useful to provide a residence time between each of the extraction stations. In the preferred embodiment of the invention, extraction is carried out in a series of discreet steps where fresh deionized water is introduced into the hydration cavity for approximately 2 seconds, while the residence time for leaching or mass transfer exchange continues for approximately 72 seconds between each extraction or washing station. After 6 such step-wise extraction steps, the products of hydrolysis, monomers and surfactants have been reduced below detectable levels.
In the process for the present invention, the wet contact lens is transferred by a variety of techniques, including gravity, surface tension, and fluids that are introduced through specialized lens transfer elements to transfer the lens from convex to concave lens holding surfaces, or vice versa. In the present invention, both air and water are utilized as suitable fluids. This avoids direct mechanical handling of the lens as it is transferred from chamber to chamber thereby minimizing physical damage to the lens.
SUMMARY OF OPERATION
FIGS. 1, 2 and 3 illustrate diagrammatically and in block form the preferred embodiment of the automated means for hydrating a mold and hydrophilic contact lens of the present invention. As illustrated in FIG. 1 an automated production line having an output conveyor 11 supplies a plurality of pallets 12 to a hydration transfer mechanism 13 which transfers four pallets at a time from the production line conveyor 11 to a first pick and place robotic assembly 40.
While any suitable pallet arrangement would be satisfactory, the invention is described with respect to hydration carriers that handle thirty-two lenses at once, taken from four separate production pallets simultaneously. This arrangement achieves a suitable compromise between a desirable batch size and convenient robotic handling, although it is understood that a variety of pallet configurations and lens arrangements would be suitable, depending on the output rate and configuration of the contact lens production line.
The first robotic assembly 40 has a plurality of motions generally illustrated in box 40(a) of FIG. 2 including a first up and down motion in the Z axis with respect to FIG. 1 which picks a top assembly plate (illustrated in FIG. 4) from a return conveyor 41 and lifts it from the conveyor for transport in the direction of A' on arrow A-A' to an assembly position 40(b).
For the purposes of explanation, the term X axis will refer to the horizontal axis of the Figure under discussion, the Y axis will refer to the vertical axis of the Figure under discussion, and the Z axis will be perpendicular to the plane of the Figure under discussion.
At the assembly position 40(b), the top chamber plate is again reciprocated downwardly in the Z axis with respect to FIG. 1 to engage a plurality of contact lens molds carried in pallets 12, wherein each of the molds has a molded contact lens therein. The first robotic assembly 40 and the top chamber plate then secure each of the individual molds with clips as will hereinafter be more fully described with respect to FIGS. 4, 5, 8 and 9 and then reciprocates both the plate and the molds upwardly in the Z axis for clearance. After achieving the desired clearance, the robotic assembly rotates the top chamber plate and molds 135° to an angle approximately 45° from the vertical for hand-off to the second robotic assembly. The top chamber plate 15 of FIGS. 4 and 5 and the associated contact lens molds 9 secured thereto form a first hydration carrier for the lenses to be hydrated.
As illustrated in FIGS. 1 and 3, a second robotic assembly including a first pick and place robot 60 and a second pick and place robot 70 are arranged on either end of a hydration tank 20. The first pick and place unit 60 takes the first hydration carrier from the first robotic assembly 40 and moves it upwardly in the Z axis (the Y axis in FIG. 3) at a 45° angle to clear the side of tank 20, and then reciprocates along the X axis in the direction of arrow B-B', from B to B' as illustrated in FIG. 1. The motions of pick and place unit 60 are illustrated in box 60(a) of FIG. 2. After the first pick and place unit 60 has reached the desired insertion point over hydration tank 20, the first hydration assembly is inserted into the tank at a 45° angle from the Z axis in FIG. 1 (the Y axis in FIG. 3) and released onto a walking beam assembly 50. Walking beam assembly 50 translates the first hydration carrier along the length of the hydration tank 20 with a gentle up and down motion in the Z axis of FIG. 1 as illustrated in the summary box 50(a) of FIG. 2. When it has reached the end of hydration tank 20, the second pick and place robot 70 reciprocates downwardly to engage the hydration carrier within the hydration bath and draw it upwardly at a 45° angle out of the hydration bath and then reciprocate in the X axis as indicated by the arrow C-C' in the direction of C to C' as more fully illustrated in the summary box 70(a) of FIG. 2. The second pick and place unit 70, carries the first hydration chamber to a fixed reference point where it is engaged by a third robotic assembly 80.
The motions of the third robotic assembly 80 are complex, and are summarized in box 80(a) of FIG. 2. In its first motion, the third robotic assembly secures the first hydration carrier and backs it away from the reference point and the second pick and place unit 70. The first hydration carrier is then rotated approximately 90° downwardly and the mold halves are ejected by ejector pins as will be hereinafter more fully described with respect to FIGS. 20-23. After removal of the mold halves at position 80(a), the top chamber plate and the contact lenses are reciprocated in the direction of arrow of D-D' in the direction of D to D' to rest under a flushing station 90. The flushing station 90 then descends to the top chamber plate and the contact lenses to flush the lenses prior to the next processing step. Contemporaneously therewith, the hydration base (illustrated in FIGS. 6 and 7) is extracted from the return conveyor 41 by means of an indexing assembly 100 and placed on a conveyor transport path at the position indicated by 80(b). After flushing, the third robotic assembly drains the flush water by tipping the top chamber plate, and then moves to a position above the hydration base. The third robotic assembly 80(a) then makes a third translation in the direction of arrow D-D' in the direction of D' to a point directly above position 80(b) and rotates 180°. When it has reached this position, it then descends downwardly in the Z axis of FIG. 1 to assemble the top chamber plate, and the contact lenses supported thereon, with the second hydration carrier at position 80(b). After assembly, the second hydration carriers are transported along transport path 101 through a plurality of extraction stations 110 by means of the indexing assembly 100.
Return assembly 150 includes an arm 151 which is suspended over return conveyor 41 at a height that will allow the top chamber plate to pass thereunder, and be transported to the first robotic assembly 40. The hydration base units, as illustrated in FIGS. 6 and 7, are higher, and will engage arm 150 and be held there. The hydration base is transferred from the return conveyor by pusher arm 151 to the index conveyor path 101 at position 80(b).
After the hydration base and top chamber plate have been assembled to form the second hydration carrier, index drive 100 pushes the carrier the distance of one carrier width in the direction of D' in arrow D-D'. When the next hydration base is received, the next second hydration carriers is formed and indexed down the index conveyor path 101. In this matter a row of second hydration carrier is formed on conveyor path 101, wherein each of the second hydration carriers are sequentially indexed, one carrier width at a time, to pass through each of the extraction stations 110, and thereby arrive at the separation station 120, following completion of hydration.
Each of the extraction stations 110 flushes the hydration chambers of the second hydration carrier and provides fresh deionized water for leaching exchange of the by-products of hydrolysis.
At the end of the automated apparatus, a fourth robotic assembly at separation station 120 separates top chamber plate 15 from the hydration base and returns it to the return conveyor 41 where it is conveyed back to the first robotic assembly 40. After separation, the hydration base is transported to position 120(a) by index drive 100 wherein the lenses are transferred for inspection and packaging by a fifth robotic assembly 160. After the lenses are removed, a pusher arm mechanism 170 returns the second hydration carrier to the return conveyor belt 41 with push arm 171 where it is recycled to the return assembly 150.
The top chamber plate 15 used to transfer the contact lenses from point to point is illustrated in FIGS. 4 and 5. The top chamber plate 15 is equipped with a frame 15(f) and a plurality of carrier elements 16 secured thereto. As illustrated in FIGS. 4 and 5, a total of 32 carrier elements are mounted on each transport plate enabling the transport plate to receive 32 contact lens molds from four separate pallets of the type illustrated in FIG. 8. Each of the carrier elements 16 includes a convex lens attachment surface 17 and a pair of clips 18(a), 18(b) which extend beyond a circumferential wall 19 having a plurality of openings 21 formed therein. While two clips are illustrated, three or four clips could be used if desired. In the preferred embodiment, these clips are formed of a liquid crystalline polymer. Each of the convex lens attachment surfaces includes a port 22 which may be used to introduce a fluid between the convex lens attachment surface and a contact lens carried thereon in order to release or flush the lens. The top chamber plate also includes eight openings 23 which provide an opening or entry path for ejector pins which will be used to remove the molds after the contact lens has been transferred from the lens mold to the convex lens attachment surface. Transport frame 15(f) also includes four fluid conduit openings 24 which will be subsequently used in connection with the second hydration carrier to provide fluid flow through top chamber plate to the hydration base unit 860, illustrated in FIGS. 6 and 7. The transport frame 15(f), illustrated in FIGS. 4 and 5, also includes first and second support tabs 15(a),15(b) which are used by the walking beam assembly 50 to transport the first hydration carrier through the hydration bath. The transport frame 15(f) also includes a pair of registration openings 15(c) that are used to register and secure the first hydration carrier to the pick and place units of the second robotic assembly.
The top chamber plate illustrated in FIGS. 4 and 5, when coupled with a plurality of lens molds as illustrated in FIG. 9, forms a first hydration carrier 22 to be utilized by the apparatus of the present invention for hydrating the contact lens secured therein.
As illustrated in FIG. 9, the carrier elements 16 are secured to the transport frame 15(f) by means of a boss 25 formed on the body of the carrier element 16. The fluid port 22 extends through the carrier element from the convex lens attachment surface 17 to a fluid opening 26 defined in transport frame 15(f). When the top chamber plate is combines with the hydration base, as illustrated in FIG. 10, a fluid opening 26 is used to mate with a fluid discharge nozzle formed on an extraction manifold as will be hereinafter subsequently described. The contact lens mold 9 having a contact lens 8, which was molded therein includes an annular flange member 9(a) which is gripped by clips 18(a),18(b) to secure the lens mold to carrier element 16.
As illustrated in FIGS. 1 and 8, the contact lens molds 9 are transported to the hydration apparatus by means of a pallet carrier 12 which includes eight cavities 14 for receiving the concave body of front curve mold half 9. Extending radially outward on each side of cavity 14 are recesses 14(a),14(b) which provide clearance for the clip members 18(a),18(b) when the top chamber plate is lowered into engagement with the pallet 12 and molds halves 9. As will be hereinafter explained in more detail, the pallet carrier 13 transports four of the pallets 12 to a transfer position wherein the top chamber plate illustrated in FIGS. 4 and 5 is lowered into engagement with the pallets and molds to transfer the molds to the top chamber plate by means of clips 18(a),18(b). After the clips 18(a),18(b) have engaged mold half 9, the mold chamber plate and molds 9 are lifted upwardly and inverted for transfer to the hydration tank by the first robotic assembly 40.
FIRST ROBOTIC ASSEMBLY
The first robotic assembly 40 is more fully illustrated in FIGS. 15-17(c) wherein FIG. 15 is an elevation end view. FIG. 16 is a plan view and FIGS. 17(a)-(c) are elevation side views. The first robotic assembly includes a rotating transport head 415 which is illustrated in a first position in solid lines in FIGS. 15 and 16 and in a second position in dotted lines in FIGS. 15 and 16. In the first position, the first robotic assembly picks up a top chamber plate from conveyor 41 by means of a plurality of suction cups 413 and a reciprocal rotating platform 414 which reciprocates along a vertical axis on guide pins 405,406 by means of a pneumatic drive cylinder 407. The operation of the first robotic assembly is controlled by a PLC control means indicated schematically as 155 in FIG. 1. As the top chamber plates are returned along conveyor 41, they first encounter fixed guides 421,422 which guide them into a fixed reference surface. A sensor mechanism 424 then triggers a pneumatic cylinder 425 and a pusher arm 426 which urges the top chamber plate into engagement with a second fixed reference 427, thereby assuring the first robotic assembly of precise positioning of the top chamber plate prior to pickup.
After the top chamber plate 15 has been securely positioned, pneumatic cylinder 407 is actuated, and the reciprocal platform 414 begins its downward descent until the suction cup members 413 engage the top chamber plate. Suction cup grippers 413 are connected to a vacuum line to provide a positive vacuum grip. After the top chamber plate has been securely engaged, pneumatic cylinder 407 is reversed, and the top chamber plate is lifted free of conveyor 41 and movable carriage 412 is then translated by means of guide rail 410 and rollers 411 to the assembly position 40(a) for pick up of the contact lens molds as illustrated in FIG. 17(b). The carriage member 412 is reciprocated along guide rail 410 by a rodless cylinder drive mechanism 418 which reciprocates the carriage 412 to translate the rotating carriage 415 to the position over pick up point 40(a) as illustrated in FIG. 17(b). Drive cylinder 407 is then actuated again and the reciprocal rotating carriage 414 is driven downwardly so that the clip members 18(a),18(b) on each of the carrier elements engages the outer annular flange 9(a) of the front curve mold as previously described with respect to FIG. 9. After engagement, pneumatic cylinder 407 is reversed, and the rotating reciprocal carriage 414 is lifted, thereby lifting each of the front curve mold halves from the production line pallets 12 and the transfer carrier 13. Once clearance is achieved, drive motor 416 is actuated which rotates the rotating platforms 414,415 as illustrated in FIG. 17(c) through 135° of arc. When the rotating head 415 has completed its rotational travel, first hydration assembly 22, including a top chamber plate 15 and molds 9 is now in position for pick up by the second robotic assembly. Motor 416 is fixably attached to reciprocating carriage 412 and rotates the rotatable platforms 414,415 by means of shaft 419 and bearing members 420, illustrated schematically in FIG. 16.
THE SECOND ROBOTIC ASSEMBLY
The second robotic assembly includes a pair of pick and place units 60,70 positioned on either end of the hydration tank, and a walking beam assembly 50 for moving each of the first hydration carriers through the hydration tank. The walking beam assembly is illustrated in FIGS. 11-14, while the first and second pick and place units 60,70 are illustrated in FIGS. 18-19.
As illustrated in FIG. 11, the hydration tank 20 provides for complete and full immersion of the first hydration carrier in a deionized water solution, wherein the solution contains a small amount of surfactant, typically on the order of 0.01% to 5% by volume. Suitable surfactants include the family of polymeric surfactants, in this instance, preferably a polyethylene oxide sorbitan mono-oleate, commercially sold under the trade name "Tween 80". This solution differs substantially from the hydration solution used in the prior art processes typified in U.S. Pat. No. 4,495,313 to Larsen inasmuch as the time consuming ionic neutralization of the polymer from which the lens blank may be made does not have to occur during the hydration process. When deionized water is used in the hydration process, a buffered saline solution is added to the final packaging of the lens so that final lens equilibrium (ionic neutralization, final hydration and final lens dimensioning) is accomplished in the package at room temperature or during the sterilization process. That neutralization creates temporary destabilization of the dimensions of the lens, and requires an extended period of time to complete, which results in a undesirably large batch operation when placed in an automated production line having a serial molding input and serial package output.
The first hydration carriers, with enclosed contact lenses, as illustrated in FIGS. 4 and 9, are inserted into hydration tank 20 by a first pick and place robotic unit 60 illustrated in FIGS. 18-19. The first pick and place unit 60 and the second pick and place unit 70 are substantially similar in their end view and a single end view, illustrated in FIG. 19, is provided for the description of both pick and place units 60 and 70. The relative motions of the two pick and place units 60,70 are somewhat different, and are diagrammatically illustrated in FIGS. 18(a) and 18(b). As illustrated in FIG. 18(a), the first pick and place unit 60 starts its cycle of operation at the pick point wherein it receives the first hydration carrier in a hand-off from the first robotic assembly, at the position illustrated in FIGS. 3 and 17(c).
Referring to FIG. 19, a first pair 601,602 and second pair 603,604 of gripping fingers engage the upper diagonal edge of the top chamber plate with a pair of registration pins 605,606 engaging the openings 15(c) in the top chamber plate as illustrated in FIG. 4. Registration pins 605,606 simultaneously maintain precise registration with respect to the positioning of the first hydration carrier, while ensuring that the first hydration chamber does not slip out of the gripping fingers during transit. Gripping fingers 601-604 are actuated by means of rotary shafts 607,608 which extend outwardly to a pair of actuating fingers 609,610 and 611,612. The actuating fingers 609-612 are opened and closed by pneumatic cylinders 613,614 mounted on the upper actuating fingers 609,611. Thus, as the cylinder 613 is actuated, the actuating fingers 609,610 open and close, rotating shaft 607, and thereby opening and closing the engaging fingers 601,602. Likewise, engaging fingers 603,604 are actuated by pneumatic cylinder 614 through the motion of actuating fingers 611,612 and rotating shaft 608.
The gripping fingers and actuating fingers are carried on a first horizontal beam member 615 which is cantilevered out from a reciprocating frame member 616 and is secured to a reciprocating guide rail 617. Guide rail 617 is fixed for reciprocal movement between first and second pairs of guide rollers, two of which are illustrated in FIG. 19 at 618 and 620. The reciprocating frame member 616 and reciprocating guide 617 are fixed for reciprocation at a 45° angle by means of the bracket 621 which aligns the rollers 618-620 and supports them via a cross beam 622 to a set of reciprocating rollers 624. The entire reciprocal assembly, including fingers 601-604, cantilevered beam 615, reciprocating beam 616 and guide 617 thus reciprocate in both the Z axis of FIG. 19 (the X axis of FIG. 18) and along a diagonal axis, as best seen in FIG. 18. The reciprocating frame 616 also includes an L shaped lower member 616(a) which has mounted thereon a screw nut assembly 684 which may be driven up and down rotating screw 685 by means of drive motor 686. As drive motor 686 rotates in a clockwise direction, the screw rod 685 rotates thereby driving the screw nut 684 and reciprocating frame 616,616(a) upward (at a 45° angle as seen in FIG. 18). Counterclockwise rotation of motor 686 will drive the screw member 684 and the reciprocating frame 616,616(a) downwardly to the lower most portion of rotating screw rod 685, illustrated in dotted lines in FIG. 19.
Reciprocating frame 616 is held at an angled orientation by means of two pairs of guide rollers mounted on either side of reciprocating guide 617, two of which are illustrated as 618 and 620 in FIG. 19. Guide rollers 618,620 are secured to frame 621 and travel on a second reciprocal carrier 622 which will be hereinafter described with respect to FIG. 18.
FIG. 18(a) describes the relative motion of the gripping fingers 601-604 and the first hydration carrier, beginning with the pick point where the first hydration carrier is received from the first robotic assembly. After the first hydration carrier is secured by means of gripping fingers 601-604 and pins 605,606, the first pick and place unit 60 moves to the left in the direction of arrow A to provide clearance between the first hydration carrier and the first robotic assembly 40. After clearance is secured, the first hydration carrier is reciprocated upwardly in the direction of arrow C at a 45° angle until it has been lifted to a distance sufficient to clear the edge of hydration tank 20. After vertical clearance is secured, the pick and place unit 60 carries the first hydration carrier to the tank entry point in the direction indicated by the arrow B as carriage 622 traverses guide rail 630. When the pick and place unit 60 has reached the hydration tank entry point, motor 686 is actuated to lower support frame 615 downwardly in a direction indicated by arrow D until the first hydration carrier reaches the level of the hydration solution in tank 20. Upon reaching the solution level, motor 686 is slowed and the entry into the hydration tank continues at a rate not exceeding 40 mm per second. It has been found that if the rate of entry into the tank exceeds 40 mm per second, bubbles of air can be trapped in the hydration chamber formed between the first carrier element 17 and the contact lens mold 9 which may subsequently interfere with the transfer of the lens 8 from the mold 9 to the first convex lens carrier 17. Subsequent handling of the lens by the lens transfer means and convex carrier element 17 is via surface tension and gravity while immersed and air bubbles trapped between the lens and the convex carrier element 17 will impair the lens handling ability of the transfer means.
After reaching the end of its downward reciprocal travel, the first hydration carrier is placed in tank 20 as illustrated in FIG. 19, and released by the gripping fingers 601-604. The reciprocal frame 616 is then backed or withdrawn from the tank in the direction opposite to arrow D, and the pick and place unit 60 is reciprocated in a direction opposite arrow B to a home position. When the pick and place unit 60 has reached the home position, the drive motor 686 may be actuated to begin a second cycle of operation, wherein the pick and place unit 60, and horizontal frame member 615 begin a downward descent to the pick point or handoff point between the first robotic assembly and the pick and place unit 60.
The first hydration carrier travels through the hydration tank 20 on two pairs of walking beams as will be hereinafter described with respect to FIGS. 11-14. As illustrated in FIG. 11, a first pair stationary walking beams is illustrated as a single beam 201 which is fixably mounted within the hydration tank with a series of notches 202 formed therein allowing its upper periphery for engaging the tabs 15(b) formed on the top carrier plate as illustrated in FIG. 4. The first hydration carrier 22 is also supported along edge 15(g) by a pair of lower support rails 203,204 as illustrated in FIG. 13. When the hydration carrier 22 is transported through the hydration tank 20, it is also supported by a pair of upper walking beams, one of which is illustrated at 210, which also has a plurality of notches 212 along their upper peripheries for engaging tab members 15(a) of the top chamber plate 15 and first hydration carrier 22. The upper walking beams 210 reciprocate vertically and horizontally with a first upward movement as illustrated by arrow A in FIG. 11 followed by a horizontal traverse as indicated by arrow B followed by a second vertical downward reciprocation indicated by arrow C, and a return stroke in the horizontal axis as indicated by the arrow D. The first hydration carrier is inserted into the tank before the upper walking beams 210 traverse their lower horizontal traverse, between arrow C and arrow A. This enables the upper walking beams 210 to enter space 15(e) between the upper and lower support tabs 15(a),15(b). When the upper walking beams 210 have reached their furthest travel in the X axis in the director of arrow D, it begins its upward travel in the direction of arrow A, wherein notches 212(a) engage the first hydration carrier and lift it from the insertion point where it was deposited by pick and place unit 60. As the first hydration carrier 22 is lifted upwardly by walking beams 210, the lower most tab 15(b) is lifted clear of the stationary walking beams 201. The upper walking beams 212 then traverse in the direction of arrow B carrying the first hydration carrier 22 with it for one horizontal step. Upper walking beams 212 are then lowered in the direction of arrow C thereby dropping the first hydration carrier 22 so that the lower most tab 15(b) will come to rest in the notches 202 of the stationary walking beam 201. While the first hydration carrier 22 is thus supported, the upper walking beams 210 continue their downward descent until completely free and are then reciprocates backwardly in the direction of arrow D to the initial start point. In this manner, the first hydration carrier 22 is advanced in a step by step manner to the opposite end of hydration tank 20.
The reciprocal movement of the upper walking beams 212 is provided by means of two traveling yokes 221,222 which are suspended from a traveling support beam 223. Support beam 223 is mounted for vertical reciprocal movement on guide tubes 238 as illustrated in FIG. 14. The support beam 223 is lifted in the vertical dimension by means of drive cylinder 224 and a rotating over center mechanism 225 which is journaled for rotation about pivot axis 236. The over center mechanism 226 is supported by a movable carriage 227 which travels along guide tubes 228,229 by means of a rotating screw mechanism 230. Rotating screw 230 is driven by a reversible motor and a reduction transmission 231 through belt drive 232. As drive motor 231 is rotated in a first direction, the drive screw 230 advances carriage 227 in the direction of arrow B of FIG. 11, thereby moving carriage 227, support shaft 226, the over center mechanism 225, the drive cylinder 224, and the cross beam 223 which supports the upper walking beams 210 and each of the hydration carriers 22 resting thereon.
The horizontal beam 223 is also fixed for vertical reciprocation on guide tubes 238 which are fixably attached to the traveling carriage 227. Guide tubes 238 thereby restrain horizontal motion in the X axis of FIGS. 13 and 14 and translate all of the pivotable motion of the over center mechanism 225 into a vertical lifting moment.
The over center mechanism 225 which lifts support beam 223 and the upper walking beam 210 is driven by drive cylinder 224 to rotate a first link 235 about pivot axis 236. About pivot axis 236, are fixed two bell cranks 237, on to which are mounted two shafts with rollers 226. Link 235 then reciprocates for a first moment along the axis of the arrow F as illustrated in FIG. 13 until roller 226 reaches carriage 227 as indicated by stop point axis G in FIG. 13. Drive cylinder 224 continues to expand, thereby causing rotation of crank 237, which results in an upward movement of crank arms 237 and pivot axis 236, thereby lifting the entire assembly as illustrated in FIG. 14. While the assembly is thus lifted, drive motor 231 is then actuated to advance traveling carriage 227 along guides 228,229 by means of the rotating screw 230. When the upper walking beam has reached the end of its transit in the horizontal axis, then drive cylinder 224 is relaxed, thereby allowing the short crank arms 237, link 235 and the cross beam 223 to return to their original position, and the walking beam 210 to reach its lower most limit of travel.
The transit time in hydration tank 20 is to some extent dependent upon the temperature of the hydration bath. For a deionized water hydration bath with a 0.05% surfactant, the desired residence time for a HEMA soft contact lens varies from 3 to 10 minutes at temperatures of 55° C. to 90° C. In the preferred embodiment, a 5 minute residence time has been found advantageous when the hydration bath temperature is maintained at 70° C. ±5°. At the end of the 5 minute period, the first hydration carrier 22 has traveled the length of hydration tank to the lift tank exit point indicated as 22(b) in FIG. 11. The hydration tank 20 may be covered with an insulating cover 250 having a pair of opening slots 251,252 which provide entrance and egress for the first hydration carriers 22, as carried by pick and place units 60,70 respectively.
It is noted that during the transit in the hydration tank, the contact lens 8 hydrates and swells, thereby breaking free of the front curve mold half 9. Since the top chamber plate 15 and the front curve mold halves have been inverted by the first robotic assembly 40, prior to placement in the tank, the lens is subjected to gravity as soon as it breaks free of mold half 9.
While subsequent agitation of the first hydration carrier may move the lens about in the defined hydration chamber, the lens will settle on the convex lens transfer surface 17 as the first hydration carrier is lifted free of the hydration bath by pick and place robotic unit 70.
The second pick and place unit 70 withdraws the first hydration carrier 22 from the hydration tank 20 by descending downwardly at a 45° angle as illustrated in FIG. 18(b) to reach the pick point. In doing so, the gripping fingers 601-604 traverse through opening 252 in the tank cover and engage the openings 15(c) in the top chamber plate 15 with pins 605,606. The fingers are then clamped together by means of pneumatic cylinders 613,614, and a rotary motor similar to 686 is actuated to drive the second pick and place unit 70 upwardly along threaded rod 685(b) along the diagonal axis illustrated in FIG. 18(b). While the hydration carrier is immersed in the hydration tank, the upward movement is limited to 24 cm/sec. After the first hydration carrier 22 has cleared the hydration bath, the upward movement is accelerated, until it reaches the vertical limit of travel as indicated in FIGS. 18 and 19. Pick and place unit 70 is then reciprocated in the travel direction indicated in FIG. 18(b) until it reaches the hand-off point for the third robotic assembly, and begins a short downward stroke to place the first hydration carrier 22 on a fixed reference bar 830 as illustrated in FIG. 21. After reaching the reference bar, the gripping fingers 601-604 are opened, and the pins 605,606 withdrawn, to allow the hydration carrier to rest at a fixed reference point for hand-off to the third robotic assembly as will be hereinafter discussed in detail. After hand-off, the second pick and place unit 70 is then reciprocated back upwardly to its upward moment of travel by rotation of the screw thread 685(b) and the entire assembly is then reciprocated back along the return path to its initial starting point. At the initial starting point, the second pick and place unit 70 may begin its downward descent into the hydration tank 20 to pick up another first hydration carrier.
The movements of pick and place unit 60, walking beams 210,212 and the pick and place unit 70 are coordinated by a PLC control means 155 to ensure an orderly sequence of hydration for first hydration carriers 22 as they are placed into and lifted out of the hydration tank.
The pick and place units 60 and 70 are mounted for reciprocal travel in the horizontal axis of FIG. 18 on a fixed track 630 by means of carriages 622 and 642. Carriage 622 is supported by four grooved rollers 624 while carriage 642 is supported by four grooved rollers 644. The carriage member 642 is reciprocated in the horizontal axis by means of pneumatic drive cylinder 645 and piston rod 646 which is fixably attached to carriage 642 by means of bracket 647. The first pick and place unit 60 is carried by carriage 622 along the horizontal axis and is reciprocated by means of pneumatic cylinder 650 and piston rod 651, from reference point 652 to reference point 653, as indicated by the dotted lines in FIG. 18.
A second short stroke hydraulic cylinder 654 is connected between the carriage member 624 and piston rod 651 and provides the short clearance bump of the pick and place unit 60 away from the first robotic assembly 40 prior to insertion.
THIRD ROBOTIC ASSEMBLY
The third robotic assembly of the present invention receives the first hydration carrier from the second robotic assembly, removes the lens molds, flushes the contact lenses that are now retained by the convex lens carrier elements of the top chamber, plate and then matches the top chamber plate with a hydration base to form a second hydration carrier. The movements of the third robotic assembly are complex, and summarized in FIG. 23. The third robotic assembly itself is summarized in FIGS. 20-22, the hydration base with which it interacts is summarized in FIGS. 6, 7 and 10 and the stations with which it interacts are depicted in FIGS. 24-31.
As noted previously, each of the lenses have been transferred by gravity, through the hydration solution, and are now supported on the convex lens engagement surfaces 17 of each of the carrier elements 16.
The operation of the third robotic assembly will be summarized with respect to FIG. 23 wherein the third robotic assembly receives a top chamber plate, contact lenses and front curves at step 1 after the second pick and place unit 70 has deposited the top chamber plate, lenses and front curve mold halves (the first hydration assembly) on a reference bar 830 for registration purposes. A reciprocal gripping head with a plurality of vacuum grippers is reciprocated into engagement with the first hydration carrier and the third robotic assembly then backs away from the reference bar and the second pick and place unit for clearance purposes. After clearance is achieved, the first hydration assembly is rotated approximately 90° counterclockwise and the reciprocating head is actuated to draw the front curve mold halves into engagement with fixed ejector rods mounted on the third robotic assembly. This causes the front curve mold halves to be ejected and removed from the top chamber plate leaving the contact lenses carried on the convex surface of the lens carrier 16 via surface tension. After ejection of the front curve mold halves, the rotating assembly of the third robotic assembly is rotated approximately 150°, or approximately 15° over center to the position schematically illustrated at position 5 in FIG. 23. The carrier is then reciprocated along the horizontal axis to a flushing station and paused, wherein the flushing station reciprocates downwardly to the top chamber plate while the contact lenses remain secured to the convex surface of the lens carrier means via surface tension. The lenses are flushed, partially to cool the lenses from the temperature of the hydration bath, partially to flush away any residual aqueous solution remaining on the lenses from the hydration bath and partially to ensure adequate hydration of the lens while in an atmospheric environment. The flush station is then reciprocated upwardly, and the third robotic assembly then rotates approximately 45° to drain the top chamber plate and lenses of any remaining flushing solution from the flushing station. After a suitable drain period, the rotating assembly is then reciprocated along the X axis to the final handoff position, illustrated at step 8 in FIG. 23, where it is rotated approximately 165° to a vertical position, and a reciprocating head is then reciprocated downwardly from step 8 to step 9 of FIG. 23 to engage the top chamber plate with a hydration base, and thereby form the second hydration carrier of the present invention. Following the hand-off of the top chamber plate, the rotating assembly is rotated back 135° to approximately 45° off vertical, and the entire assembly is then reciprocated along the X axis back to the assembly start point where it is indexed to receive another first hydration assembly.
As illustrated in FIG. 22, the rotating assembly includes a first rotating platform 801 and a reciprocating rotating platform 802, which is reciprocated with respect to the first rotating platform 801 along guide tubes 803,804 via pneumatic drive cylinder 805. Secured to the first rotating platform 801 are eight ejector rods 806, four of which are visible in FIG. 22. Mounted to the reciprocating rotating plate 802 are eight vacuum grippers 807 which are adapted to engage and grip the back or smooth side 15(d) of the top chamber plate 15 illustrated in FIG. 4. The first rotating platform 801 is mounted for rotation about shaft 810, and is rotated by means of motor 811 and drive belt 812. Shaft 810 is journaled for rotation within housing 813 which also serves as a reciprocal carriage for the rotating portion of the third robotic assembly.
Carriage member 813 is mounted for reciprocal travel on a horizontal rail 814 by means of four slotted rollers 815, two of which are visible in FIGS. 21 and 22, and four of which are visible in FIG. 20. Carriage 813 reciprocates along track 814 from a pick position, illustrated in solid lines in FIG. 20 to a hand-off position, illustrated in dotted lines in FIG. 20. The carriage 813 and rotating assembly are reciprocally driven by means of a screw thread 820 which engages a screw follower 821 mounted on carriage 813. Screw thread 820 is rotated by means of drive motor 822 to draw the rotatable carriage to the hand-off position when rotating in a clockwise direction, and to return the rotating carriage to the pick position when rotating in the counterclockwise direction.
As illustrated in FIG. 21, the rotatable reciprocating platform 802 having vacuum grippers 807 mounted thereon has been positioned substantially adjacent a first hydration assembly 22 that is resting on a registration bar 830 and supported by fingers 602,604 of pick and place unit 70. The reciprocal rotatable platform 802 is advanced into contact with the first hydration assembly to ensure that each of the extraction rods 806 is in alignment with one of the apertures 23 formed in the top chamber plate 15 of the first hydration carrier. Two of the apertures 23 formed in the top chamber plate 15 may be used for registration purposes, by fitting the reciprocating platform 802 with tapered pins for engaging apertures 23. After the first hydration carrier 22 has been secured to the vacuum gripping means 807, the second pick and place unit 70 reciprocates upwardly out of the way, and then back to its home position as previously described. The rotating assembly is then moved along the horizontal X axis in the direction of the arrow A for a short distance to clear registration bar 830.
Once clearance is achieved, rotating assembly 813 is rotated approximately 90° in a counterclockwise direction to place the front curve mold halves over the collection tray 831. The reciprocating and rotating platform 802 is then reciprocated to the position illustrated in FIG. 22, which drives the extraction rods 806 through the openings 23 into the top chamber plate, to thereby engage a plurality of triangular tabs formed on one of the front curve mold halves, as illustrated by tab 9(b) in FIG. 8. The front curve mold halves 9 are thereby freed from the clips 18(a),18(b) which secured the front curve mold half to the top chamber plate 15. During the rotation of the rotating assembly 813, and the movement of the rotating and reciprocating plate 802, a contact lens is retained on the convex lens holding surface 17 by virtue of surface tension. After the front curve mold halves 9 have been ejected into the collection tray 831, the reciprocating and rotating platform 802 and the top chamber plate 15 are rotated clockwise approximately 150°, and the movable carriage 813 is then reciprocated to a second position in the direction of arrow A in FIG. 21, to bring the top chamber plate, and the contact lenses secured thereto, into alignment with the flushing station 90 illustrated in FIG. 21.
Flushing station 90 includes a reciprocal flushing head 901, and a flushing manifold 902, which reciprocate on a pair of guide tubes 903,904 by means of a pneumatic cylinder 905. The flushing head 901 is fixably secured to a pair of reciprocal collars 906,907 which reciprocate along guide tubes 903,904. The source of flushing fluid, preferably deionized water, is supplied to conduit 910 for flushing the exterior concave surface of the contact lens secured to the lens carrier surface 17 of the top chamber plate 15. As will be hereinafter explained with respect to the flushing station and the manifold of FIGS. 28-31, a separate stream of flushing fluid is provided for each contact lens to cool the lens from the approximate 70° C. temperature of the hydration bath, and to remove any residual aqueous solution remaining on the lens from the hydration bath. This flushing step is also desirable to maintain complete hydration of the lens prior to the transfer of the lens to the second hydration carrier. After a short flushing cycle of 0.5 to 5 seconds, the flushing station 901 and flushing manifold 902 is reciprocated upwardly, and the rotatable carrier is then rotated approximately 30° in a counterclockwise direction to drain the top chamber plate and lenses of flushing fluid. The reciprocal carriage 813 is then advanced again in the X axis in the direction of arrow A to center line 840 of the hand-off position. Upon arrival at the hand-off position, the rotatable carriage 813 and the rotatable and reciprocal plate member 802 are rotated in a counterclockwise direction approximately 165° to position the top chamber plate, and the contact lenses adhered thereto, directly above the hydration base member 860 which has been positioned therebelow by indexing mechanism 100. The reciprocal rotatable carriage 802 is then reciprocated downwardly to engage the top chamber plate 15 with the hydration base member 860 to form the second hydration carrier and the hydration chamber as illustrated in FIG. 10. FIG. 10 illustrates a single lens transfer means, and a single concave lens holding means in partial cross-section. After the transfer of the top chamber plate to the hydration base member 860, the vacuum cups 807 are released, and the reciprocal rotatable platform 802 is raised to the position illustrated in FIG. 22, wherein the rotating assembly is rotated back approximately 135° in a clockwise direction and the carriage 821 is returned along the horizontal axis in a direction opposite to arrow A to place the third robotic assembly at the initial home position.
The hydration base member 860 is more fully described and illustrated with respect to FIGS. 6, 7 and 10 which illustrates a multilevel carrier having a plurality of concave lens holding means 861 mounted thereon. Each of the concave lens holding means 861 includes a central fluid port 862 for introducing a fluid between the concave lens holding means and a contact lens contained therein. As will be hereinafter described, this fluid may be air or water. Each of the fluid ports 862 is connected via a plurality of fluid passageways which extend through each layer of the manifold to four upwardly extending fluid coupling members 863, one of which is illustrated in cross-section in FIG. 6. Fluid introduced through these fluid coupling ports 863 travels through the coupling to four V-shaped conduits 864 defined in plate layer 865 to feed a series of crossover manifolds 866. Crossover manifolds 866 are defined in manifold layer 867 and feed directly to the fluid ports 862 defined in each of the concave lens holding means 861. In between each row of concave lens holding means 861 is a drain trough 870 which extends outwardly to an outer collection channel 871 which extends around the periphery of the hydration base to drain liquid flowing from the hydration chambers to be defined by the concave lens holding means 861 into a sump 872 for collection as will be hereinafter later described.
The hydration base illustrated in FIGS. 6 and 7 is combined with the top chamber plate 15 to form the second hydration carrier 23, having a plurality of hydration chambers therein. In the embodiment illustrated with the top chamber plate of 4 and 5 and the hydration base of FIGS. 6 and 7, thirty-two separate hydration chambers are formed between the convex lens transfer surface 17 and each of the concave lens holding means 861. When the top chamber plate 15 is lowered into engagement with the hydration base 860, the clips 18(a), 18(b) spring outwardly to engage the outer wall 861(a) of the concave lens holding means. The outer circumferential wall 19 of the carrier element 16 is received within a stepped recess 861(b) defined by the concave lens holding means 861. A plurality of openings 21 formed in the circumferential wall 19 provide a plurality of fluid discharge openings for fluid introduced through fluid port 862 for the concave lens holding means, and port 22 of the convex lens holding means 17. Thus, fluid may be introduced into the hydration chamber from either side of contact lens during flushing of the hydration chamber, and will remain in the concave lens holding means 861 after flushing by virtue of a fluid equilibrium which is established at the upper periphery 861(c) of the concave lens holding means. This residual fluid is used for extraction.
The registration bar for the hand-off between the pick and place unit 70 and the third robotic assembly is further illustrated in FIGS. 26 and 27 wherein registration bar 830 has mounted thereon an adjustably fixed stop member 840 which provides a fixed reference point along the X axis of FIG. 26. On the opposite end of reference bar 830, is a pneumatic cylinder 841 having a piston member 842 which is actuated after the first hydration chamber 22 has been placed on the reference bar 830 as illustrated in FIG. 27. After placement, pneumatic cylinder 841 is actuated, thereby urging piston 842 into engagement with the first hydration carrier 22 and moving it against the fixed reference stop 840. The reference bar 830 is secured to the hydration station of the present invention by means of vertical supports 842,843. The upper portion of the hydration carrier is held in position by the fingers of the second pick and place unit 70. In this manner, the first hydration carrier 22 is precisely positioned and registered for hand-off to the third robotic assembly to ensure that the extraction rods 806 will be in alignment with the openings 23 defined in the top chamber plate 15 of the first hydration carrier 22.
The flushing station 90 of the present invention is further illustrated in FIGS. 24 and 25 wherein the reciprocal flushing head 901 is mounted on collars 906,907 for reciprocation along vertical guide tubes 903,904 by virtue of pneumatic cylinder 905. The vertical guide tubes 903,904 are mounted on a stationary frame member 915 secured to the hydration apparatus. A flushing liquid is supplied by a conduit 916 to port 910 and the flow of fluid therethrough is sequenced by a solenoid operated pinch valve 917 in response to the control system 155 for the hydration apparatus. A catch basin 831 is provided for receiving the discarded front curve lens molds after ejection by ejector rods 806. A pneumatic drive cylinder 845 is used to drive a sweep mechanism 846 across the catch basin 831 to thereby move the discarded front curve lens molds into opening 846 where they are removed for regrinding and recycling. A water makeup line 847 may also be provided with a pinch valve 848 to supply makeup deionized water to the hydration tank through conduit 849. A positive displacement pump also meters a small amount of surfactant into the hydration tank with each water makeup, in order to maintain the surfactant concentration at 125 to 500 ppm with respect to the deionized water.
The flushing manifold 902 is more particularly illustrated and described in FIGS. 28-31 in which FIG. 28 represents a partially cross-sectioned elevation view of the flushing manifold, FIGS. 29(a)-29(d) represent each of the various levels of the manifold and FIG. 30 represents diagrammatically the overall arrangement of the manifold passageways. FIG. 31 is a cross-sectioned elevation view of manifold level 1, and FIG. 31(a) is an enlarged cross-section of a portion of FIG. 31.
As illustrated in FIGS. 28 and 29(a)-(d), manifold 902 is formed from four discreet layers or levels 912, 913, 914 and 915. The manifold is secured together by a plurality of screws, one of which is illustrated at 916, which extend through a plurality of commonly aligned openings 917 for a threaded engagement with level 1 manifold 915. As illustrated in FIGS. 29 and 30, thirty-seven such screw fasteners are used, two rows of which have been referenced with reference numeral 917. As illustrated in FIG. 30, flushing fluid enters from fluid line 916 into the fluid port 910 and is distributed by channels 918,919 that are milled or cast into the under surface of the top level 912 to be distributed to four distribution points 920-923. From distribution points 920-923, the fluid travels through plate 913 or manifold level 3 by virtue of holes drilled in plate 913 at 920(a)-923(a) to a second set of milled or cast channels 924-927 which provide distribution to eight vertical bores 928 drilled through plate 914 or manifold level 2. The fluid then flows to eight cross manifolds 929 that are milled or cast on the upper surface of plate 915 to thirty-two vertical bores 930 which terminate in nozzles 931 as illustrated in FIGS. 31 and 31(a).
While the exact configuration of vertical bores and milled channels may vary from manifold to manifold, the principles of construction for each of the manifolds used in the flushing station, the extraction station, and the separation station are substantially the same as set forth in FIGS. 29(a)-(d). The purpose of this configuration is to ensure a very precise even distribution of flow from one supply line to a plurality of receiving points.
In particular, the extraction station manifold illustrated in FIGS. 34-36 utilizes a similar method of construction with one additional layer of functionality. The extraction manifold in FIGS. 34-36 includes two distinct sets of fluid passageways, one to feed a plurality of discharge nozzles as illustrated in FIG. 35(a), and a second to feed a series of pass through nipples which supply a flushing flow to the hydration base as will be hereinafter described. As illustrated in FIG. 34, a central port 935 receives a flow of deionized water and diverts it into two primary manifolds 936,937. Manifold 937 is milled in the under side of plate 938 and channels the fluid flow to four distribution points 939 where the fluid passes downwardly through vertical bores in plate 940 to be distributed along channels 940(a) formed in the lower or under surface of plate 940. Each of these channels terminate in a vertical distribution port 941 which is drilled into plate 942. The output of the flow through bore 941 is then diverted by means of cross channel manifolds 943 that are milled or cast into the upper surface of plate 944. Plate 944 has formed thereon two separate types of discharge orifices. In the embodiments as illustrated in FIGS. 34-36, thirty-two separate discharge nozzles 945 provide a flow of deionized water to each of the hydration chambers formed in the second hydration means through the openings 26 formed in the top chamber plate 15. Simultaneously, a second flow of fluid flows through distribution manifold 936 to four vertical discharge ports 946 and passes through each of the manifold plates 940-944 to terminate in a hydration base nozzle 947 as illustrated in FIG. 35(a). Each of these discharge nozzles engages the upstanding fluid couplings 863 which extend upwardly from the hydration base through the openings 24 defined in a top chamber plate to enable fluid to be supplied directly to ports 862 formed in each of the concave lens holding means 861.
The extraction station illustrated in FIGS. 32 and 33 receives the second hydration carrier formed from a combination of the hydration base 860 and the top chamber plate 15 which form a plurality of hydration chambers therebetween as previously described and illustration in FIG. 10. Each of the second hydration carriers are indexed in a step wise manner down indexing conveyor path 101 by index drive 100. A plurality of extraction stations 110 are arranged on the path to receive the second hydration carriers, and periodically flush and exchange the deionized water therein to continue to leach the byproducts of hydration from the contact lenses 8 carried therein.
Each of the extraction stations 110 includes a stationary platform 111 supported on first and second columns 112,113 which serve as a support for pneumatic cylinder 114 and as reciprocating guides for collars 115,116 and a reciprocating platform 117 attached thereto. Reciprocating platform 117 includes a discharge nozzle 118 that supplies deionized water to the extraction station through flexible conduit 950, as regulated by the solenoid operated pinch valve 951 and control means 150. The deionized water is distributed by manifold 950 to the first and second water distribution systems as previously described with respect to FIGS. 34-36. A first distribution system provides thirty-two discharge outlets 945 which engage cavities 26 formed in the upper surface of top chamber plate 15 to provide a flow of fluid through port 22 of each of the convex lens carrier surfaces. Likewise, a second flow of fluid is supplied through nipples 947 to the upwardly extending couplings 863 to provide a flow of flushing fluid through the hydration base member manifold passageways and into ports 862 of each of the concave lens holding means 861.
As the second hydration carrier is indexed into position below the extraction station 110, the reciprocating platform 117 is lowered by pneumatic cylinder 114 to cause each of the fluid delivery ports 945,947 to engage the respective openings 26 in the top chamber plate 15 and the fluid supply nipple 863 of the hydration base. Simultaneously, an extraction nozzle 119 is lowered into sump 872 to extract the hydration fluid as it flows from the hydration chamber through the circumferential wall passageways 21 and into the collection troughs 870,871. Extraction nozzle 119 evacuates the fluid through suction line 121 which is also opened and closed by a solenoid operated pinch valve 122 by the hydration control circuitry 150.
While prior art hydration baths required 120 to 180 minutes to achieve satisfactory results, it has been found that a 5 to 10 minute cycle of cycled flushes and leaching will produce a lens with no detectable contaminants therein. In the preferred embodiment, a flush cycle of 24 seconds (with 1 to 2 seconds of actual flushing in the cycle) is provided for each extraction station 110, and the extraction stations are spaced from one another a distance corresponding to the width of three of the hydration base members 860. Thus, step wise indexing of the hydration base members results in a 1 to 2 second flush (in the 24 second dwell or flush period) and a 72 second leach cycle to provide maximum exchange of leachable materials from the lens. This cycle is repeated six times for a total of slightly more than 7 minutes, the total time for travel through the apparatus of the present invention, including the hydration tank time is approximately 15 minutes.
THE SEPARATION STATION
The separation station 120 in the present invention is illustrated in FIGS. 37-39 wherein FIG. 38 represents a cross-section elevation end view, FIG. 37 represents a elevation side view of the traveling head of a fourth robotic assembly and FIG. 39 represents a sectional plan view of the assembly.
As illustrated in FIG. 8, the separation station 120 spans conveyor 101, and the second hydration carriers 23 as they arrive on conveyor track 101. FIG. 39 illustrates a single second hydration carrier 23, but it is understood that in operation, the hydration carriers abut one another as they traverse conveyor track 101. The separation station includes a fixed stationary tower 125 which is supported by columns 126,127 which have mounted thereon a vertically reciprocal carrier 128 which reciprocates on glide bearings, two of which are illustrated at 129. Reciprocating carrier 128 provides a support for a cantilevered beam 130, a guide track 131 and a housing member 132. Mounted for reciprocation on guide track 131 is a fourth robotic assembly including a reciprocal separation head 133 which traverses track 131 on four grooved rollers 134. The reciprocating separation station 133 reciprocates horizontally from a position over conveyor track 101 to the position illustrated in FIG. 38, in order to remove the top chamber plate 15 from the second hydration carrier and deposit it on a return conveyor 41. The reciprocating separation head 133 also reciprocates vertically with respect to conveyor surface 101 and 41 as carriage 128 is reciprocated up and down the guide tubes 126,127 by drive motor 135 which rotates a screw thread 136 to drive a screw follower 137 up and down the threaded rod 136, depending upon the direction of rotation of motor 135. The reciprocating carriage 128 is spring mounted to screw follower 137 by means of bellville washers 138 which act as springs when head 133 is in contact with the top chamber plate 15. A rodless cylinder 145, parallel to beam 130 and spaced therefrom, is used to drive the reciprocating separation head 133 along track 131 from a position directly over conveyor track 101 to the position over return conveyor 41, as illustrated in FIG. 38.
A vacuum line 139 is connected to eight separate vacuum cups 140 which extend through manifold 147 and engage the top chamber plate 15 in order to separate it from the hydration base 860. The vacuum is supplied by a pneumatic ejector while pressurized deionized water is supplied to manifold 147.
In operation, the pneumatic rodless cylinder 145 reciprocates the reciprocating separation head 133 to a position directly over conveyor track 101, and the reciprocating head is lowered into engagement with the second hydration carrier 23 by drive motor 135 and rotating screw 136. As the vacuum cups 140 engage the top chamber plate 15 of the second hydration carrier 23, a vacuum is drawn in the vacuum cups 140, thereby positively engaging the top chamber plate.
Simultaneously, deionized water is supplied to manifold 147, which in turn supplies pressurized water through each of the nozzles 141, through each of the upper openings 26 on the top chamber plate, through the ports 22 and into the hydration chamber formed between the top chamber plate and the hydration base. This supply of deionized water ensures that the contact lens is transferred to the concave lens holding means. The drive motor 135 is reversed, while deionized water is still flowing through ports 22, to lift the reciprocating separation head 133 and the top chamber plate 15. The top chamber plate is lifted, and the carriage reciprocated along the cantilever beam to the position illustrated in FIG. 38, wherein drive motor 135 is again reversed to drop the top chamber plate towards return conveyor 41. The vacuum line is then closed and the vacuum cups release the top chamber plate to conveyor 41 for return to the first robotic assembly 40.
After separation, the hydration base member 860, having a contact lens in each of the concave lens retaining means 861, is reciprocated along path 101 as illustrated in FIG. 1 to the hand-off position 120(a) wherein the individual contact lenses are removed by a robotic transfer device 160. After the lenses are removed, a pneumatic cylinder 170 is actuated to drive push arm 171 into engagement with the hydration base member 860 and return it to the return conveyor 41. Return conveyor 41 conveys the hydration base member back to indexing mechanism 100 and arm 150 which pulls the hydration base member from the return conveyor belt 41 as hereinbefore previously described.
While the invention has been particularly shown and described with respect to the preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing and other changes in form and details made therein without departing from the spirit and scope of the invention, which is limited only by the scope of the following claims.
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An automated method for high speed production rates in the hydration of soft contact lenses. The method includes the use of robotic transfer equipment to transfer contact lens molds containing contact lenses to and from a hydration station and a flushing station.
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This application claims the benefit of U.S. Provisional Application No. 60/654,283, filed Feb. 18, 2005, entitled F IFTH W HEEL S ENSOR A SSEMBLY , which is hereby incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
The present invention is directed to an electronic system for monitoring the coupling of a trailer to a trailer hitch assembly that is mounted on a truck chassis, and in particular is directed to an electronic system that indicates whether the trailer is properly coupled to the trailer hitch assembly by discriminating between components of the trailer, components of the hitch assembly and foreign materials.
Electronic coupling control systems for a vehicle trailer hitch assembly are described in each of U.S. Pat. No. 5,861,802, entitled “F IFTH W HEEL H ITCH C OUPLING C ONTROL S YSTEM ” to Hungerink et al. and U.S. Pat. Nos. 6,285,278 and 6,452,485, each entitled “E LECTRONIC S YSTEM FOR M ONITORING A F IFTH W HEEL H ITCH ,” to Schutt et al. U.S. Pat. Nos. 5,861,802; 6,285,278 and 6,452,485 are each assigned to the assignee of the present invention and are hereby incorporated by reference in their entirety. Each of these patents disclose an electronic coupling control system that includes a trailer sensor for sensing when a trailer is located proximate the hitch assembly, a kingpin sensor for sensing the presence of a trailer kingpin in a hitch plate throat, and a lock sensor for sensing when the locking mechanism is locked in a secured position. These patents further disclose an indicator located within the vehicle for providing trailer hitch assembly coupling status information to a driver of a vehicle. A control circuit is coupled to the trailer sensor, the kingpin sensor, the lock sensor and the indicator. The sensors are utilized by the control circuit to inform a driver when a trailer is in close proximity to the trailer hitch assembly, when the trailer kingpin is positioned in the hitch throat and when the locking mechanism is in a locked position. The electronic coupling control system is also capable of performing various self-diagnostic routines to ensure proper operation of the system when the vehicle ignition is turned on.
Heretofore, systems like those described above typically incorporate contact-type sensors susceptible to degradation from the stringent environment within which these sensors are utilized, including degradation from normal use, extreme use such as experienced during some coupling operations, and the inclusion of foreign solids within the environment, such as grease, water and ice each laden with ferromagnetic materials. These ferromagnetic materials as laden within the grease, etc., can be the cause of “false-positive” readings as conveyed to the operator, or readings that falsely indicate proper alignment of the kingpin with respect to the throat of the hitch plate. Improper alignment of the kingpin with the throat of the hitch plate may potentially result in dropping a trailer from the associated vehicle either at a shipping dock, or potentially on a public roadway, with significant damage to the associated equipment and surrounding property, and further personal injury or worse.
An electronic system for monitoring the receiving of a kingpin of a trailer within a throat of a hitch plate is desired that accurately and reliably differentiates between the kingpin and foreign materials, thereby eliminating “false-positive” readings of proper alignment to the operator of an associated vehicle.
SUMMARY OF THE INVENTION
One aspect of the present invention is to provide an electronic system for monitoring a trailer hitch assembly having a hitch plate and a throat for receiving a kingpin of a trailer and a locking mechanism for locking the kingpin within the throat, the electronic system determining whether the trailer hitch assembly is properly coupled to the trailer and comprising a first magnet creating a first magnetic flux, and a first Hall-effect sensor for sensing the position of the kingpin of the trailer relative to the throat of the hitch plate by measuring the first magnetic flux. The electronic system further comprises a control circuit operably coupled with the first Hall-effect sensor and determining whether the first magnetic flux indicates a proper location of the kingpin of the trailer relative to the throat of the hitch plate.
Another aspect of the present invention is to provide a hitching system that comprises a trailer hitch assembly having a hitch plate with a throat for receiving a kingpin of a trailer and a locking mechanism for locking the kingpin in the throat. The hitching system also includes a first magnet creating a first magnetic flux, and a first Hall-effect sensor for sensing the position of the kingpin of the trailer relative to the throat of the hitch plate by measuring the first magnetic flux. The hitching system further includes a control circuit operably coupled with the first Hall-effect sensor and determining whether the first magnetic flux indicates a proper location of the kingpin of the trailer relative to the throat of the hitch plate.
A further aspect of the present invention is to provide an electronic system for monitoring a trailer hitch assembly having a hitch plate with a throat for receiving a kingpin of a trailer and a locking mechanism for locking the kingpin in the throat, wherein the electronic system determines whether the trailer hitch assembly is properly coupled to the trailer. The electronic system comprises a non-contact proximity sensor for sensing the position of a kingpin of a trailer relative to a throat of a hitch plate, a control circuit operably coupled with the proximity sensor and determining whether a kingpin of the trailer is properly located relative to a throat of a hitch plate, and a display device operably coupled to the control circuit and displaying coupling status to an operator of a vehicle.
Yet another aspect of the present invention is to provide a hitching system that comprises a trailer hitch assembly having a hitch plate with a throat for receiving a kingpin of a trailer and a locking mechanism for locking the kingpin within the throat, and a non-contact proximity sensor for sensing the position of a kingpin of a trailer relative to the throat of the hitch plate. The hitching system further comprises a control circuit operably coupled with the proximity sensor and determining whether a kingpin of a trailer is properly located within the throat of the hitch plate, and a display device operably coupled to the control circuit and displaying coupling status to an operator of a vehicle.
The present inventive electronic system for monitoring the kingpin of a trailer within a throat of a hitch plate accurately and reliably differentiates between the kingpin and foreign materials, thereby eliminating “false-positive” readings of proper alignment to the operator of an associated vehicle, and increases the safety associated therewith. The system further reduces manufacturing costs, increases system reliability, is more durable, is capable of a long operating life and is particularly well adapted for the proposed use.
These and other features, advantages and objects of the present invention will be further understood and appreciated by those skilled in the art by reference to the following specification, claims, and appended drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a truck/tractor including an electronic system embodying the present invention for monitoring a trailer hitch assembly;
FIG. 2 is a bottom view of the trailer hitch assembly;
FIG. 3 is a side view of the trailer hitch assembly;
FIG. 4 is a partial cross-section side view of a the trailer hitch assembly;
FIG. 5 is a perspective view of an output device;
FIG. 6A is a schematic view of a first embodiment of the sensor assembly, wherein the sensor assembly is at a zero-state;
FIG. 6B is a schematic view of the first embodiment of the sensor assembly, wherein the sensor assembly indicates the location of a kingpin within the throat of an associated hitch plate;
FIG. 6C is a schematic view of the first embodiment of the sensor assembly, wherein a ferromagnetic material is positioned within the throat of the hitch plate;
FIG. 7 is an electrical schematic of the first embodiment of the sensor assembly;
FIG. 8 is a theoretical plot of sensor output versus flux intensity;
FIG. 9A is a schematic view of a second embodiment of the sensor assembly, wherein the second embodiment of the sensor assembly is at a zero-state;
FIG. 9B is a schematic view of the second embodiment of the sensor assembly, wherein the second embodiment of the sensor assembly indicates the location of the kingpin within the throat of the hitch plate;
FIG. 10 is an electrical schematic of the electrical circuit of the second embodiment of the sensor assembly;
FIG. 11A is a schematic view of a third embodiment of the sensor assembly, wherein the third embodiment of the sensor assembly is at a zero-state;
FIG. 11B is a schematic view of the third embodiment of the sensor assembly, wherein the sensor assembly indicates the location of a component different than the kingpin in close proximity to the sensor assembly;
FIG. 11C is a schematic view of the third embodiment of the sensor assembly, wherein the sensor assembly indicates the location of a kingpin within the throat of the hitch plate;
FIG. 12 is an electrical schematic of the electrical circuit of the third embodiment of the sensor assembly;
FIG. 13A a schematic view of a fourth embodiment of the sensor assembly, wherein a Hall-effect type sensor and a biased magnet are positioned across a portion of the throat of the hitch plate from one another;
FIG. 13B is a schematic view of the fourth embodiment of the sensor assembly, wherein the a kingpin is positioned within the throat of the hitch plate;
FIG. 14 is an electrical schematic of the electrical circuit of the fourth embodiment of the sensor assembly;
FIG. 15A is a schematic view of a fifth embodiment of the sensor assembly, wherein the sensor assembly is at a zero-state;
FIG. 15B is a schematic view of the fifth embodiment of the sensor assembly, wherein the sensor assembly indicates the location of a component different than the kingpin;
FIG. 15C is a schematic view of the fifth embodiment of the sensor assembly, wherein the sensor assembly indicates the location of the kingpin within the throat of the hitch plate;
FIG. 16 is an electrical schematic of the electrical circuit of the fifth embodiment of the sensor assembly; and
FIG. 17 is a schematic view of an electrical circuit of a sixth embodiment of the sensor assembly that includes an inductive proximity sensor.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
For purposes of description herein, the terms “upper,” “lower,” “right,” “left,” “rear,” “front,” “vertical,” “horizontal,” and derivatives thereof shall relate to the invention as oriented in FIG. 1 . However, it is to be understood that the invention may assume various alternative orientations and step sequences, except where expressly specified to the contrary. It is also to be understood that the specific devices and processes illustrated in the attached drawings, and described in the following specification are exemplary embodiments of the inventive concepts defined in the appended claims. Hence, specific dimensions and other physical characteristics relating to the embodiments disclosed herein are not to be considered as limiting, unless the claims expressly state otherwise.
The reference numeral 10 ( FIGS. 1-3 ) generally designates an electronic monitoring and sensing system incorporated within a truck/tractor 12 which includes a trailer hitch assembly having a base 16 securely mounted to a chassis 18 , a trailer hitch plate 20 pivotally mounted on the base 16 on a transverse axis, and a locking mechanism 22 for locking a conventional trailer kingpin in place. The electronic system 10 preferably includes a non-contact kingpin sensor assembly 24 mounted to the hitch assembly 14 , a tilt sensor assembly 25 , a lock sensor 27 , and an output device 26 mounted in the cab of the tractor 12 . The tilt sensor assembly 25 and the lock sensor assembly 27 are described in U.S. Pat. Nos. 5,861,802; 6,285,278; and 6,452,485. The sensor assemblies 24 , 25 , 27 are coupled to the output device 26 by a multi-conductor cable 28 . In a preferred embodiment, the non-contact kingpin proximity sensor 24 includes an inductive-type sensor, however, other proximity sensors may be utilized, including Hall-effect type sensors, and the like, as discussed below.
In the illustrated example, the sensor assembly 24 is mounted to the hitch plate 20 near the throat 30 formed in the hitch plate 20 , into which a trailer kingpin 32 is positioned and locked. FIG. 4 provides an upside-down side view and partial cross section illustrating the location of the trailer kingpin 32 when properly disposed within the throat 30 . As constructed, the sensor assembly 24 outputs a detection signal when the kingpin 32 is disposed within the throat 30 . The calibration of the sensor assembly 24 prevents it from indicating that the kingpin 32 is present when a misaligned coupling occurs, which prevents the locking mechanism 22 from securing the kingpin 32 (i.e., the trailer) to the hitch plate assembly 14 , or further from providing “false-positives” or untrue readings of a proper coupling, as discussed below. The locking mechanism 22 of the hitch plate assembly 14 is biased by a compression spring to automatically lock-in and secure the trailer kingpin 32 as soon as the trailer kingpin 32 enters the hitch throat 30 . Those of ordinary skill in the art will appreciate that the present invention may be used in connection with any type of locking mechanism. It should further be noted that the present invention may be applied to tractor hitch assemblies having other constructions and is not limited to particular mounting locations as shown for the embodiments of the sensor assembly 24 described herein.
FIG. 5 illustrates an exemplary output device 26 . A multiple conductor cable 28 couples the sensor assembly 24 to the output device 26 . The internal components (i.e., the control circuitry) of the output device 26 are further shown and described in U.S. Pat. No. 6,285,278, which is incorporated by reference herein in its entirety. The output device 26 includes a display panel 34 for providing coupling status information to the driver/operator of the tractor 12 . In a preferred embodiment, the display panel 34 includes an “unlocked” icon 36 , a “locked” icon 38 , a “fifth wheel” icon 40 and seven-segment display 42 . In the embodiment, the display 42 provides an error code indicating possible sources of a coupling malfunction, again as further described in U.S. Pat. No. 6,285,278. Preferably, a red light diode (LED) is provided behind the “unlocked” icon 36 . Further, a yellow, a red, and green LED are provided behind the “fifth wheel” icon 40 and a green LED is provided behind the “lock” icon 38 . One of ordinary skill in the art will appreciate that the individual LEDs could be replaced by an LED array capable of providing multiple colors. While output device 26 as shown only indicates visual indicators, one of ordinary skill in the art will readily appreciate that and audio output may be provided. For example, by adding a speaker and appropriate voice processing circuitry, the output device 26 may provide voice output to instruct a driver as to possible causes of a coupling malfunction. Additionally, a warning buzzer may be activated in addition to, or as an alternative, providing an unlocked icon 36 .
In a first embodiment, the sensor assembly 24 ( FIG. 6A ) includes an analog Hall-type sensor 44 with an integrated circuit, a biasing magnet 46 having a magnetic axis 47 and producing a magnetic flux 48 , and a threshold adjustment and a switching circuit 50 . The Hall-effect sensor 44 is sensitive to magnetic flux in a direction perpendicular to the larger dimension thereof. As best illustrated in FIG. 6A , the biasing magnet 46 provides a base or zero level flux 48 when the kingpin 32 is not properly located within the throat 30 . The strength of the bias magnet 46 and the dynamic range of the Hall device within the sensor 44 determine the effective range of the sensor 44 . As illustrated in FIG. 6B , with the kingpin 32 moved in a direction as illustrated and represented by directional arrow 52 and positioned proximate the sensor assembly 24 , the flux 48 of the magnet 46 as read by the Hall sensor 44 is greater in strength due to the proximity of the ferromagnetic material comprising the kingpin 32 . A positive signal is then generated indicating proper location of the kingpin 32 within the throat 30 of the hitch plate 20 . As illustrated in FIG. 6C , a foreign material, such as grease, water, ice, and the like containing shavings or particles of a ferromagnetic material, commonly referred to as swarf, does not provide an adequate amount of flux 48 , per proper calibration of the adjustment and switching circuit 50 , in order to indicate a positive and proper location of the kingpin 32 within the throat 30 .
A schematic view of the sensor assembly 24 is illustrated in FIG. 7 and includes a power supply 54 and a ground 56 each coupled to the Hall sensor 44 , and the switching circuit 50 . The switching circuit 50 includes a comparator circuit 58 , a hysteresis feedback loop 60 , an analog or digital potentiometer 62 for adjusting the threshold sensitivity of the sensor assembly 24 , and a signal conditioner 64 for conditioning the output signal 66 for the desired switching. A theoretical plot of the sensor output for optimizing the switching is illustrated in FIG. 8 , wherein output is plotted versus the flux intensity.
The reference numeral 24 a ( FIG. 9A ) generally designates another embodiment of the present invention, having a first Hall effect sensor 68 , a second Hall sensor 70 , a third Hall sensor 72 , a first bias magnet 74 having a magnetic axis 73 and creating a first magnetic flux 75 , a second bias magnet 76 having a magnetic axis 79 and creating a second magnetic flux 77 , and a switching circuit 78 . Each Hall sensor 68 , 70 , 72 is sensitive to the magnetic flux in a direction perpendicular to the larger dimension thereof. In the illustrated example, the first Hall sensor 68 is sensitive to the flux flowing between the magnets 74 , 76 and along the magnetic axis 73 , 79 thereof, while the second Hall sensor 70 and the third Hall sensor 72 are sensitive to magnetic fields that are perpendicular to the magnetic axis 73 , 79 of the magnets 74 , 76 . As illustrated in FIG. 9B , the flux 75 , 77 created by the magnets 74 , 76 is drawn off through the second Hall sensor 70 and third Hall sensor 72 by a proper positioning of kingpin 32 within the throat 30 .
A schematic of the sensor assembly 24 a is shown in FIG. 10 , wherein the sensor assembly 24 a includes a power supply 80 operably coupled to each of the Hall sensors 68 , 70 , 72 , and ground lines 82 for the same, and the switching circuit 78 . In the illustrated example, the switching circuit 78 includes a threshold adjustment circuit 84 , a first to second Hall sensor comparator 86 , a first to third Hall sensor comparator 88 , a window and comparator 90 to compare the differences between the outputs of the comparators 86 , 88 , and an output signal conditioner 92 providing an output signal 94 .
The reference numeral 24 b ( FIG. 11A ) represents another embodiment of the sensor assembly. In the illustrated example, the sensor assembly 24 b includes a first Hall sensor 96 , a second Hall sensor 98 oriented perpendicularly to the first Hall sensor 96 , a bias magnet 100 having a magnetic axis 101 and creating a magnetic flux 103 , and a thresholding and switching circuit 102 . As illustrated, the Hall sensors 96 , 98 are oriented such that the first Hall sensor 96 is sensitive to flux along the magnetic axis 101 , while the second Hall sensor 98 is sensitive to flux perpendicular to the magnet axis 101 , thereby making the sensor assembly 24 b more sensitive to monitoring objects located along the magnetic axis 101 of the magnet, as well as perpendicular thereto. For example, as illustrated in FIG. 11B , the sensor assembly 24 b may be calibrated to take into account magnetic flux as caused by components of the hitch assembly 14 , such as hitch plate 20 . In this arrangement, the second Hall sensor 98 is sensitive to flux 104 flowing in a perpendicular direction to the magnetic axis 101 , which is used to precisely adjust the sensitivity of the overall sensor assembly 24 b . As illustrated in FIG. 11C , proper placement of the kingpin 32 within the throat 30 causes an increase in the flux 106 flowing through the first Hall sensor 96 , which is compared to the steady state reading developed from the orientation as illustrated in FIG. 11B .
FIG. 12 illustrates the circuitry of the sensor assembly 24 b and includes a power supply 105 and a ground 106 to each of the first Hall sensor 96 and the second Hall sensor 98 , and the switching circuit 102 . The switching circuit 102 includes a comparator 108 for comparing the outputs of the first Hall sensor 96 and the second Hall sensor 98 , a feedback loop 110 , and an output signal conditioner 112 producing an output signal 114 .
The reference numeral 24 c ( FIG. 13A ) represents yet another alternative embodiment of the sensor assembly that includes a Hall switch 116 and a bias magnet 118 having a magnetic axis 121 and creating a magnetic flux 122 . In the illustrated example, the Hall switch 116 is mounted on one side of a horseshoe-shaped member 120 preferably constructed of a soft iron or other highly permeable material, thereby attracting magnetic flux on account of low magnetic resistance thereof. The magnet 118 is mounted to an opposite side of the member 120 and is positioned so as to direct the flux 122 created thereby in the direction of the Hall switch 116 . Due to the spacing across the ends of the member 120 , a relative small amount of the flux 122 is encountered by the Hall switch 116 when the kingpin 32 is not present within the throat 30 . As illustrated in FIG. 13B , the flux 122 is increased with the presence of the kingpin 32 within the throat 30 . It should be noted that in the illustrated example of the sensor assembly 24 C the build up or addition of swarf material 52 within the throat 30 and about the kingpin 32 actually assists in the trip of the Hall switch 116 by filling any air gaps located between the kingpin 32 and the side edges of the throat 30 . It should further be noted that the arrangement of the sensor assembly 24 c has the advantage of not requiring an analog output to properly function.
FIG. 14 is a schematic view of the sensor assembly 24 c that includes the Hall switch 116 having a power supply 124 and a ground 126 , and a switching circuit 128 . The switching circuit 128 includes a comparator 130 , a feedback loop 132 , a threshold adjustment circuit 134 and an output signal conditioner 136 providing an output signal 138 .
The reference numeral 24 d ( FIG. 15A ) represents another embodiment of the sensor assembly. The sensor assembly 24 d includes a first Hall-effect sensor 140 , a bias magnet 142 having a magnetic axis 143 creating a flux 146 , and a switching circuit 144 . In the illustrated example, the first Hall sensor 140 is oriented perpendicularly to and is offset from the axis of the magnet 142 . As best illustrated in FIG. 15A , the flux 146 flows generally along the axis of the magnet 142 . As illustrated in FIG. 15B , the flux 146 is pulled perpendicularly to the axis of the magnet 142 towards a component of the trailer hitch assembly 14 , such as the hitch plate 20 , thereby allowing for adjustment and fine tuning of the overall sensor assembly 24 d and allowing the adjustments thereof to take into account the presence of components other than the kingpin 32 . The sensor assembly 24 d further includes a pair of shields each containing an amount of ferromagnetic material that aids in directing the flux 146 about the sides of the sensor 24 d , thereby creating or acting as a shield to any other external medal components or swarf in the monitored area. As best illustrated in FIG. 13C , a larger amount of the flux 146 is directed along the axis of the magnet 142 and toward the kingpin 32 away from the Hall sensor 140 when the kingpin 32 is properly located within the throat 30 . As illustrated, the sensor assembly 24 d allows the setting of a trip point to incorporate a threshold to ignore detrimental amounts of swarf causing a “false-positive” reading of the sensor assembly 24 d.
FIG. 16 is a schematic view of the sensor assembly 24 d including a power supply 150 and a ground 152 to the Hall sensor 140 , and the switching circuit 144 . The switching circuit 144 includes a comparator 154 , a feedback loop 156 , a threshold circuit 158 and an output signal conditioner 160 providing an output signal 162 .
The electronic monitoring system 10 preferably includes an induction proximity sensor 164 ( FIG. 17 ) in place of the Hall-effect sensor arrangements as disclosed herein. As is known in the art, inductive proximity sensors function by sensing a change to the properties of a related inductor. The properties of the inductor will change if a ferrous or conductive material is placed within a space-sensing region within the inductors magnetic field that may extend outwardly of the inductor. Typically, inductor sensors utilize an oscillating (AC) signal within the inductor to sense inductor property changes, with the frequency of the oscillations changing the importance of the various properties of the inductor. As illustrated, the inductor sensor of the induction proximity sensor 164 senses the amount of loss on the inductor when a ferromagnetic material is in close proximity thereto. In the present example, the operating frequency of the inductive proximity sensor is preferably less than 50 kHz, 20 kHz nominal, thereby reducing false-positives as caused by ferromagnetic material laden swarf. A specific advantage of the induction proximity sensor 164 is the elimination of a bias magnet as required with Hall-effect and reed switch sensors.
FIG. 17 is a schematic view of the inductive proximity sensor 164 that comprises a tank circuit 166 including a sense coil 168 and a series combination of a pair of capacitors 170 . The oscillation frequency of the tank circuit 166 is preferably less than or equal to 50 kHz (20 kHz nominal). The tank circuit 166 forms part of a Colpitts oscillator circuit 172 that includes a capacitor 174 , resistors, 176 , 178 , 180 , 182 , 184 , 186 , a capacitor 188 , and a transistor 190 . The transistor 190 provides feedback energy needed to maintain the oscillation of the tank circuit 166 . The resistors 176 , 178 , 180 and the series combination of the resistors 182 , 184 , 186 set the DC operating point of the transistor 190 . The capacitor 188 is utilized to AC-bypass the resistor 186 to increase the AC gain of the transistor 190 independent of the DC bias. The components of the oscillator circuit minimize the amount of feedback required to maintain the oscillation. In the present example, losses induced by a conductive object proximate the sense coil 168 causes the oscillator to decrease in amplitude. Preferably, the resistor 184 is utilized to compensate for temperature-dependent circuit losses, and mainly the resistance of the copper winding utilized within the sense coil 168 . A transistor 192 and a resistor 194 provide a buffered output of the Colpitts oscillator 172 . A capacitor 196 blocks the DC level present at the emitter of the transistor 192 . A first diode 198 provides a new ground-based DC level, and a second diode 200 half-wave rectifies the AC output of the oscillator. A capacitor 202 and a resistor 204 filter the rectified AC to obtain a DC level proportional to the amplitude of the oscillator, that is compared to a DC level derived from a resistor 210 and a resistor 212 . A comparator 214 and a resistor 216 perform the comparison function and generate an output signal 218 for the inductive proximity sensor 164 .
In the foregoing description, it will be readily appreciated by those skilled in the art that modifications may be made to the invention without departing from the concepts disclosed herein. Such modifications are to be considered as included in the following claims, unless these claims by their language expressly state otherwise.
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An electronic system that monitors a trailer hitch assembly having a plate hitch with a throat for receiving a kingpin of a trailer and a locking mechanism for locking the kingpin within the throat. The electronic system determines whether the trailer hitch assemblies is properly coupled to the trailer, and comprises a first magnet creating a first magnetic flux, and a first Hall-effect sensor for sensing the position of the kingpin of the trailer relative to the throat of the hitch plate by measuring the first magnetic flux. The system further comprises a control circuit operably coupled with the first Hall-effect sensor in determining whether the first magnetic flux indicates a proper location of the kingpin of the trailer relative to the throat of the hitch plate. The electronic system discriminates between the kingpin and foreign materials, thereby assuring proper locking of the locking mechanism.
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This is a continuation of application Ser. No. 07/862,657, filed Apr. 1, 1992 abandoned, which is incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
The present invention relates to novel compounds having potent activity as histamine H 3 -receptor ("H 3 ") antagonists, and methods of using such compounds.
BACKGROUND OF THE INVENTION
Dementias tend to be characterized by cognitive disorders and often by depression. A particularly devastating dementia is Alzheimer's disease (AD). AD affects more than 30% of humans over 80 years of age, and as such, represents one of the most important health problems in developed countries (Evans et al., J.A.M.A. 262: 2551-2556 (1989); Katzman and Saitoh, FASEB J. 280: 278-286 (1991)). This neurodegenerative disorder of unknown etiology is clinically characterized by gradual impairment of cognitive function. The large buildup of intracytoplasmic neurofibrillary tangles and neurite plaques observed histopathologically in AD plausibly leads to degeneration of affected nerve cells. At least one study showed decreases in histamine and histidine levels in frontal, temporal and occipital cortices and in the caudate nucleus of brains from AD patients examined post mortem (Mazurkiewics and Wsonwah, Can. J. Physiol. Pharmacol., 67:75-78 (1989)).
Histamine is a chemical messenger involved in various complex biological actions. It is widely distributed in the plant and animal kingdoms. In mammals, including man, it occurs mainly in an inactive bound form in most body tissues. When released, histamine interacts with specific macromolecular receptors on the cell surface or within a target cell to elicit changes in many different bodily functions. Histamine (4(2-aminoethyl) imidazole) is a base. Its chemical structure is: ##STR1##
Histamine receptor pharmacology has revealed three subtypes of receptors which mediate (or are associated with) the activity of histamine. These receptors are most commonly referred to as H 1 , H 2 , and H 3 . The most recently discovered of these receptors is the H 3 histamine receptor. Early studies suggested the presence of another histamine receptor when it was demonstrated that histamine inhibits its own synthesis and release in brain slices by a negative feedback process operating at the level of histaminergic nerve-endings (see, for example, Arrang, J.M. et al. Nature 302:832-837 (1983)). More recently, the H 3 receptor has been shown to function as a pre-synaptic autoreceptor inhibiting histamine synthesis and histamine release from neurons, especially in the central nervous system (Arrang, et al. Nature 327:117-123 (1987)). The presence of H 3 receptors in peripheral tissues has also been reported and here too they appear to be involved with the nervous system. Thus, histamine depresses sympathetic neurotransmission in the guinea pig mesenteric artery by interacting with H 3 receptors on the perivascular nerve terminals (Ishikawa and Sperelakis, Nature 327:158 (1987)). This important observation suggests that histamine may control the release of other neurotransmitters (Tamura et al., Neuroscience 25:171 (1988)). Inhibitory histamine H 3 receptors also exist in the guinea pig ileum where their role appears to be to modify the magnitude of histamine contraction, rather than affecting histamine release (Trzeciakowski, J. Pharmacol. Exp. Therapy 243:847 (1987)). Particularly intriguing is the discovery of H 3 receptors in the lung (Arrang et al. supra (1987)). The presence of histamine H 3 receptors in the lung raises the question of whether they control histamine release in anaphylaxis and whether they may be manipulated to provide therapy in asthma. Indeed it has been suggested that H 3 receptors may have a modulating role on excitatory neurotransmission in airways. Generally, however, H 3 receptor inhibition tends to increase histamine activity, with potentially detrimental effects. Thus, it is desirable to avoid introducing H 3 receptor antagonists that act on peripheral tissues.
Histamine H 3 receptor activation was found to inhibit acetylcholine release in a guinea pig ileum model (Poli et al., Agents and Actions 33: 167-169). Selective H 3 -receptor blockers reversed the histamine-induced inhibitory effect. Histamine also decreased serotonin release; this effect was reversed with an H 3 -antagonist, and was suggested to operate via the histamine H 3 -receptors (Schlicker et al., Naunyn-Schmiedaberg's Arch. Pharmacal. 337:588-590 (1988). Activation of H 3 -receptors was found to inhibit excitatory presynaptic potentials (Arrang et al., J. Neurochem. 51:105 (1988)).
One reported highly specific competitive antagonist of histamine H 3 receptors is thioperamide (Arrang et al., supra (1987)). Although thioperamide is a very potent antagonist in vitro (K i =4.3 nmol/L), relatively high doses are required in vivo to inhibit histamine release from the brain in rats (Ganellin et al., Collect. Czech. Chem. Commun. 56:2448-2455 (1991)). Ganellin et al. suggests that this most probably results from poor penetration through the blood-brain-barrier by this peramide, although the pharmacokinetic properties of thioperamide may also play a role. Moreover, the thiourea functionality found in thioperamide may result in higher intrinsic toxicity of thioperamide.
Thiourea-containing drugs are known to be associated with undesirable side effects in clinical use. For example, with thiourea-containing drug molecules that are used to treat hyperthyroidism, agranulocytosis is known to be a serious, and occasionally fatal, toxic effect in clinical use (see, e.g., Brimblecombe et al. Gastroenterology 74:339-346 (1978)). The thiourea-containing histamine H 2 -receptor antagonist metiamide caused a low incidence of granulocytopenia in peptic ulcer patients and was withdrawn from clinical use (Forrest et al., Lancet 1: 392-393 (1975)). In high dose, repeated dose toxicological studies in dogs, incidences of agranulocytosis were seen at 162 mg/kg/day (Brimblecombe et al., "Toxiology of Metiamide," International Symposium on Histamine H 21 --Receptor Antogonists, Wood and Simpkins, Smith Kline & French, pp. 53-72 (1973)). A proportion of dogs (<10%) died acutely with pulmonary edema and pleural effusion. The metiamide isostere cimetidine, in which the thiourea group was replaced by an alternative group (cyanoguanidine), did not cause granulocytopenia, or any other side effects in animal toxicity studies or in clinical usage by multimillions of patients, indicating that the toxicological problems with metiamide could be attributed to the presence of the thiourea group (Brimblecomb et al., supra). It is likely that the thiourea functionality, with its association with toxiological phenomena and its likelihood of inducing undesirable side effects, could limit the clinical development of thioperamide.
Although some predictions have been made concerning the ability of molecules to pass through the blood brain barrier, these predictions are at best speculative. The rate and extent of entry of a compound into the brain are generally considered to be determined primarily by partition coefficient, ionization constant(s) and molecular size. No single partition solvent system has emerged as a universally applicable model for brain penetration, although the octanol water system has received particular attention, and Hansch and coworkers have suggested that a partition coefficient in this system of about 100 is optimal for entry into the central nervous system (CNS) (Glave and Hansch, J. Pharm. Sci., 61:589 (1972); Hansch et al., J. Pharm. Sci., 76:663 (1987)). Comparisons between known H 2 antagonists, however, suggest that there is no such simple relationship between their brain penetration and octanol water partition coefficients (Young t al., J. Med. Chem. 31:656 (1988)). The comparison of the ability of histamine H 2 receptor antagonists to cross the blood brain barrier suggests that brain penetration may increase with decreasing over-all hydrogen binding ability of a compound (Young et al., supra). However, optimizing H 2 receptor antagonists to improve brain penetration reduced antagonist potency (Young et al., supra). Thus it is fundamentally difficult to optimize both blood brain barrier permeability and function of a compound.
It is therefore an object of the present invention to provide novel potent histamine H 3 -receptor antagonists that are better able to penetrate the blood-brain-barrier than previously reported compounds.
Further it is an object of the present invention to provide novel potent histamine H 3 -receptor antagonists that have reduced toxicity compared to other known H 3 antagonists.
Another object of the present invention is to provide histamine H 3 -receptor antagonists that will act selectively on the brain and have limited activity on H 3 receptors in peripheral tissues.
It is yet another object of the present invention to provide a novel class of histamine H 3 -receptor antagonists.
SUMMARY OF THE INVENTION
The present invention provides novel compounds having activity as histamine H 3 -receptor antagonists. In a preferred aspect, the compounds of the invention exhibit ready penetration of the blood-brain-barrier and reduced toxicity. The novel compounds of this invention include compounds of the formula: ##STR2## wherein D is CH 2 or CH 2 -CH 2 , Z represents S or O, preferably O, x is 0 or 1, n is an integer from 0 to 6, R 1 represents preferably hydrogen, or a hydrolyzable group, but can be a lower alkyl or aryl group, and R 2 represents a linear chain, branched chain or carbocyclic group or aryl group of up to about 20 carbon atoms, and salts thereof. If R 2 is tert-butyl, cyclohexyl, or dicyclohexylmethyl, x or n must not be 0. If R 2 is adamantane, the sum of x and n must be greater than 1. The various alkyl or aryl groups can have functional group substituents.
It has been discovered that amide or carbamate functional groups can be used to join alkyl or aryl substituents to the piperidyl nitrogen of 4(4-piperidyl)-1H-imidazole groups. Other cyclic imides, particularly pyrrolidyl or cycloheptamidyl (C 6 H 11 N) can be substituted for piperidine. In a preferred aspect, the compounds of the invention are surprisingly effective at transport across the blood brain barrier, thus limiting their effects primarily to cerebral histamine H 3 -receptors, and are also less toxic than histamine H 3 -receptor antagonists based on a thiourea functional group.
In addition, the present invention encompasses a pharmaceutical composition comprising a compound of the invention, and a method of using a compound or pharmaceutical composition of the inspection in an animal, particularly in a human, to treat Alzheimer's disease and other dementias by ameliorating the cognitive defects and neurodegenerative effects associated therewith. The histamine H 3 -receptor antagonists of the invention have additional therapeutic uses where increased arousal and attention is desired.
DESCRIPTION OF THE FIGURES
FIG. 1. Binding of N.sup.α -methylhistamine to rat cortical homogenate. Open box: total bound; x'ed box: specific binding; closed box: non-specific binding.
FIG. 2. Binding of 3 H-labeled N.sup.α -methylhistamine to the cortical homogenate of thioperamide injected rats.
FIG. 3. Binding of 3 H-labeled N.sup.α -methylhistamine to the cortical homogenate of compound 1 injected rats.
FIG. 4. The effect of α-methylhistamine on sleeping one hour after injection.
FIG. 5. The effect (dose-response) of thioperamide on sleep induced by R(-)-α-methylhistamine (30 mg/kg).
FIG. 6. The effect (dose-response) of compound 1 on sleep induced by R(-)-α-methylhistamine (25 mg/kg).
DETAILED DESCRIPTION OF THE INVENTION
The compounds of the present invention are compounds of the general formula. ##STR3## wherein D is C H 2 or C H 2 -C H 2 , Z represents sulfur (S) or oxygen (O), preferably O, x is 0 or 1, n is an integer from 0 to 6, R 1 represents hydrogen, an in vivo hydrolizable group, a lower alkyl group, a lower cyclic alkyl group, or a lower aryl group, and R 2 represents a substituted or unsubstituted linear chain or branched chain alkyl group of up to about 20 carbon atoms, a substituted or unsubstituted carbocyclic group of up to about 20 carbon atoms including mono and bicylic moieties, and a substituted or an unsubstituted aryl group of up to about 20 carbon atoms, or any combination of above-mentioned groups, or salts thereof. In a specific embodiment, R 2 can represent a disubstituted methyl, such as but not limited to dicyclohexyl methyl (--CH(C 6 H 11 ) 2 ), diphenyl methyl (--CH(C 6 H 5 ) 2 ), and the like. If R 2 is tert-butyl, cyclohexyl, or dicyclohexylmethyl, x or n must not be 0. If R 2 is adamantane, the sum of x and n must be greater than 1.
In a preferred embodiment, R 1 is hydrogen. It is also contemplated that R 1 can be a hydrolyzable leaving group, such as an acyl or carbamyl, including where R 1 =--CZ(O) x (CH 2 ) n R 2 , as in I above. It is well known that N-acylimidazoles are hydrolytically labile, and R 1 may be selected such that it yields the parent imidazole compound in vivo at an optimal rate. Such hydrolysis will yield the compound with hydrogen as R 1 . Thus, the contemplated compounds of the invention with a hydrolyzable substituent at R 1 are functionally equivalent to the preferred embodiment, i.e., where R 1 is hydrogen. R 1 can also be a lower linear chain, branched chain, or cyclic alkyl, or a lower aryl. The term "lower" as applied to the alkyl or aryl substituents at R 1 indicates the presence of up to seven carbon atoms. In specific embodiments infra, R 1 is methyl, benzyl, methylcyclohexane, N-cyclohexylformamide, benzaldehyde, and t-butylaldehyde.
In yet a further embodiment, the nitrogen atom at position 3 of the imidazole ring can be substituted with a lower alkyl or aryl group, or with a hydrolyzable leaving group.
In a preferred embodiment, D is CH 2 -CH 2 , resulting in a piperidine ring structure. However, it is contemplated that D can be CH 2 , yielding a pyrrolidine ring structure. In yet another embodiment, D can be (CH 2 ) 3 , yielding a cycloheptimide (seven membered heterocycle with one nitrogen). While orientation of the imidazole group distal to the N of the piperidine is preferred, the invention contemplates the imidazole at the 2 or 3 position on the piperidine (or the 2 position of pyrrolidine, or the 2 and 3 position of the cycloheptimide ring). These alternate embodiments can be used instead of the piperidyl embodiment with the imidazole group located at the 4 position, although the piperidyl embodiment is preferred.
Although the present invention is not limited to any mechanistic theory, it is believed that the blood brain barrier is permeable to the compounds of the present invention in part because of the subtle decrease in polarity afforded by an amide or carbamate bond linking the (-(0) x (CH 2 ) n R) moiety (e.g., a hydrophobic tail) to the 4(4-piperidyl)-1H-imidazole (or 4(3-pyrrolidyl)-1H-imidazole) structure. With slightly less polarity and hydrogen-bonding capability than urea or thiourea, the amide or carbamate functionality can more efficiently traverse the blood brain barrier. Moreover, the dipole of the amide or carbamate is distal to the hydrophobic tail, more proximal to the imidazole (which is a fairly polar group), and thus tends to effect greater amphiphilicty in the molecule. That the compounds of the invention retain amphiphilic character is important for solubility in aqueous solution. Solubility in aqueous solution is desirable for a compound to be used therapeutically in an animal particularly in a human. That such a subtle difference, use of an amide or carbamate functionality, should perceptably alter blood brain barrier permeability may be considered to be surprising since it is not generally appreciated.
In preferred embodiments, a bulky hydrocarbon R 2 group is chosen so that the net hydrophilicity of the H 3 -receptor antagonist is increased, and the steric effects of a bulky substituent at R 2 are decreased, by increasing the number of methylenes in a straight chain alkyl group (i.e., in Formula I, n>1). In a specific embodiment, a tetramethylene bound to the amide or carbamate group is used. Preferably a cyclic alkyl or aryl group is linked to the amide or carbamate via the straight chain alkyl group. In a specific embodiment, tetramethylene cyclohexane (cyclohexylbutyl) is bound to an amide. Although specific hydrophobic alkyl and aryl groups have been mentioned, one of ordinary skill in the art will recognize that there are many possible hydrophobic groups for use in the compounds of the invention. These fall within the scope of the instant invention.
Thus, R 2 can be one or more bulky substituent groups. As stated above, in a preferred aspect of the invention, the bulky substituents are removed from the amide or carbanate group on the piperidyl-imidazole by increasing n. In one embodiment, R 2 is CHR 3 R 4 , in which n is 3 or 4 and R 3 and are cyclohexyl, phenyl, or the like. R 3 and R 4 can be the same group or different groups. In another embodiment, R 2 is decalin or adamantane or the like. If R 2 is adamantane, preferably n is greater than 1, but the sum of x and n must be greater than 1.
As used herein, the phrase linear chain or branched chained alkyl groups of up to about 20 carbon atoms means any substituted or unsubstituted acyclic carbon-containing compounds, including alkanes, alkenes and alkynes. Examples of alkyl groups include lower alkyl, for example, methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl or tert-butyl; upper alkyl, for example, octyl, nonyl, decyl, and the like; and lower alkylene, for example, ethylene, propylene, propyldiene, butylene, butyldiene, and the like. The ordinary skilled artisan is familiar with numerous linear and branched alkyl groups, which are with the scope of the present invention.
In addition, such alkyl group may also contain various substituents in which one or more hydrogen atoms has been replaced by a functional group. Functional groups include but are not limited to hydroxyl, amino, carboxyl, amide, esther, ether, and halogen (fluorine, chlorine, bromine and iodine), to mention but a few.
As used herein, substituted and unsubstituted carbocyclic groups of up to about 20 carbon atoms means cyclic carbon-containing compounds, including but not limited to cyclopentyl, cyclohexyl, cycloheptyl, admantyl, and the like. Such cyclic groups may also contain various substituents in which one or more hydrogen atoms has been replaced by a functional group. Such functional groups include those described above, and lower alkyl groups as described above. The cyclic groups of the invention may further comprise a heteroatom. For example, in a specific embodiment, R 2 is cyclohexanol.
As used herein, substituted and unsubstituted aryl groups means a hydrocarbon ring bearing a system of conjugated double bonds, usually comprising six or more even number of π (pi) electrons. Examples of aryl groups include, but are not limited to, phenyl, naphthyl, anisyl, toluyl, xylenyl and the like. According to the present invention, aryl also includes heteroaryl groups, e.g., pyrimidine or thiophene. These aryl groups may also be substituted with any number of a variety of functional groups. In addition to the functional groups described above in connection with substituted alkyl groups and carbocylic groups, functional groups on the aryl groups can be nitro groups.
As mentioned above, R 2 can also represent any combination of alkyl, carbocyclic or aryl groups, for example, 1-cyclohexylpropyl, benzyl cyclohexylmethyl, 2-cyclohexylpropyl, 2,2-methylcyclohexylpropyl, 2,2-methylphenylpropyl, 2,2-methylphenylbutyl.
In a specific embodiment, R 2 represents cyclohexane, and n=4 (cyclohexylvaleroyl). In another specific embodiment, R 2 represents cinnamoyl.
Particularly preferred are compounds of the formula: ##STR4## wherein x is 0 or 1, n is an integer from 0 to 6, more preferably n=3-6, and most preferably n=4, and R is as defined for R 2 above. Examples of preferred alkyl groups for R include but are not limited to cyclopentyl, cyclohexyl, admantane methylene, dicyclohexyl methyl, decanyl and t-butyryl and the like. Examples of preferred aryl and substituted aryl groups include but are not limited to phenyl, aryl cyclohexyl methyl and the like.
SYNTHESIS OF THE COMPOUNDS
The compounds of the present invention can be synthesized by many routes. It is well known in the art of organic synthesis that many different synthetic protocols can be used to prepare a given compound. Different routes can involve more or less expensive reagents, easier or more difficult separation or purification procedures, straightforward or cumbersome scale-up, and higher or lower yield. The skilled synthetic organic chemist knows well how to balance the competing characteristics of synthetic strategies. Thus the compounds of the present invention are not limited by the choice of synthetic strategy, and any synthetic strategy that yields the compounds described above can be used.
As shown in the Examples, infra, two general procedures can be used to prepare the instant compounds. Both involve condensation of an activated (electrophilic) carbonyl with the nucleophilic piperidyl nitrogen of 4-(4-piperidyl)-1H-imidazole.
The first procedure involves preparing the acid chloride derivative or acid anhydride of a carbonyl, i.e., activating the carbonyl. This activated carbonyl is added in molar excess to the piperidyl-imidazole in the presence of a molar excess of an unreactive base, for example, but not limited to, dicyclohexyl amine.
The second procedure is to condense the piperidyl-imidazole with a slight molar excess of a dicarbonate, again in the presence of an unreactive base, for example and not by way of limitation, triethylamine. This method can be used especially in the preparation of carbamate compounds.
A preferred synthesis of the 4-(4-piperidyl)-1H-imidazole is also provided. Commercially available 4-acetyl pyridine (Aldrich Chemical Co.) is converted into the key intermediate 4-(4-pyridyl)-1H-imidazole by bromination with hydrogen bromide in acetic acid (Barlin, et al., Aust. J. Chem. 42:735 (1989)) to yield the bromacetyl pyridine in high yield. Reaction of bromoacetyl pyridine with formamide at 110° C. affords the substituted imidazole in high yield. The reaction is usually performed without the addition of any solvent. The pyridyl moiety is reduced by catalytic hydrogenation using 5-10% Rhodium on carbon in acidified water at a pressure of 20-55 atmospheres to yield 4-(4-piperidyl)-1H-imidazole. This synthesis is disclosed more fully in application Ser. No. 07/862,658, now U.S. Pat. No. 5,380,858, filed by the instant inventors of even data herewith, entitled "PROCESS FOR THE PREPARATION OF INTERMEDIATES USEFUL FOR THE SYNTHESIS OF HISTAMINE RECEPTOR ANTOGONISTS," which is specifically incorporated herein by reference in its entirety.
Solvents for use in the synthesis of the compounds of the invention are well known in the art. The solvent must be non-reactive, and the starting materials and base must be soluble in the solvent. Preferably, an aprotic organic solvent of medium to high polarity is used. For example, acetonitrile, can be used. Under appropriate conditions, in the synthesis of carbamates of the invention, an alcohol, e.g., methanol, can be used.
The electrophilic carbonyl group, which contains the R 2 moiety, can be obtained from commercial sources, or it may be prepared synthetically. In specific examples, infra, the carbonyl is obtained commercially. Activation of carbonyls is well known. The acid chloride can be prepared by reacting the carboxylic acid with sulfonyl chloride. Alternatively, the acid chloride may be available commercially. In specific embodiments, infra, acid chlorides we obtained from commercial sources (Aldrich Chemical). Similarly, the acid anhydride can be prepared conveniently by reaction of a salt of the carboxylic acid with the acid chloride. In another embodiment, the acid anhydride can be obtained commercially. In a specific embodiment, infra, the acid anhydride was obtained from Aldrich Chemical. Dicarbonates for use in the invention are available commercially, e.g., from Aldrich Chemical.
BIOLOGICAL ACTIVITY
The compounds of the present invention are biologically active in assays for histamine H 3 -receptor antagonist activity, as well as in a radioligand binding assay in rat brain membranes (e.g., Table I, infra). The binding assay procedure used and its standardization with known H 3 -receptor antagonists is shown in the examples infra.
Further biological studies can demonstrate that the histamine H 3 -receptor antagonists of this invention reverse the soporific effects of the histamine H 3 -receptor agonist, R(-)-alphamethylhistamine in mice when both drugs are administered peripherally (infra). In a specific embodiment, the compound designated No. 2016 reverses the soporific effect of R(-)-alphamethylhistamine.
The data in the Examples, infra, support the view that antagonists of histamine H 3 -receptors of the invention are useful regulators of the sleep-wakefulness cycle with potentially useful cognitive and behavioral effects in mammals including humans.
In vivo studies can be used to show effectiveness of a compound of the invention to cross the blood-brain barrier, as shown in the examples, infra. The data support the view that drugs of the present invention penetrate the blood brain barrier and are able to exert beneficial central actions in mammals when these drugs are administered to the peripheral circulation.
THERAPY
The histamine H 3 -receptor antagonists of the invention can be provided therapeutically for the treatment of a subject suffering from a cognitive disorder or an attention or arousal deficit, according to the present invention. One of ordinary skill in the art would readily determine a therapeutically effective dose of an H 3 receptor antagonist of the invention based on routine pharmacological testing and standard dosage testing. In one aspect of the present invention, the compounds can be administered in doses of about 0.01 to about 200 mg/kg, more preferably 1 to 100 mg/kg, and even more preferably 30 to 100 mg/kg. In a specific embodiment, greater than about 20 mg/kg of a compound of the invention was effective to reduce the soporific effect of (R)α-methylhistamine. Included in the routine pharmacological testing are toxicity studies to determine an upper limit dose. Such toxicity studies can include LD 50 studies in mice, and 15 day toxicity studies in mammals.
The histamine H 3 -receptor antagonists of the invention are believed to increase the release of cerebral histamine, acetylcholine and serotonin. These compounds can lead to increased arousal and attention. They can also be of benefit in the treatment of cognitive disorders.
Therapy with a compound of the invention is indicated to treat dementia, as either a primary or an adjunct therapy. The compounds of the invention have clinical utility in the treatment of dementia disorders in general. In a preferred embodiment, a compound of the invention can be used in the treatment for Alzheimer's disease. The compounds can also be used to treat presenile and senile dementia, Huntington's chorea, tardive dyskinesia, hyperkinesia, mania, Tourette syndrome and Parkinson's disease, to name but a few. Other specific indications include the treatment of narcolepsy and hyperactivity in children. In another embodiment, the compounds of the invention can be used in the treatment of certain psychoses, for example forms of depression or schizophrenia.
The compounds of the invention can be used to arouse victims of comas induced by stroke, drugs or alcohol. In another embodiment, the compounds of the invention can be used to increase wakefulness, where this effect is desired. For example, the compounds of the invention, which are preferentially targeted to H 3 receptors in the brain, can be used to counteract the soporific effect of some antihistamines without negating the therapeutic effects of the antihistamines on peripheral tissue, e.g., lung. Thus allergy patients can relieve some of the side effects of antihistamine therapy. Similarly, the compounds of the invention can be used to reverse overdose of barbituates and other drugs.
The effective dose of a compound of the invention, and the appropriate treatment regime can vary with the indication and patient condition, e.g., the treatment of a dementia or the treatment of tiredness may require different doses and regemens. These parameters are readily addressed by one of ordinary skill in the art and can be determined by routine experimentation.
A therapeutic compound of the invention may also contain an appropriate pharmaceutically acceptable carrier or excipient, diluent or adjuvant, i.e., the compound can be prepared as a pharmaceutical composition. Such pharmaceutical carriers can be sterile liquids, such as water and oils, including those of petroleum, animal, vegetable or synthetic origin, such as peanut oil, soybean oil, mineral oil, sesame oil and the like. Water is a preferred carrier when the pharmaceutical composition is administered intravenously. Saline solutions and aqueous dextrose and glycerol solutions can also be employed as liquid carriers, particularly for injectable solutions. Suitable pharmaceutical excipients include starch, glucose, lactose, sucrose, gelatin, malt, rice, flour, chalk, silica gel, magnesium carbonate, magnesium stearate, sodium stearate, glycerol monostearate, talc, sodium chloride, dried skim milk, glycerol, propylene, glycol, water, ethanol and the like. These compositions can take the form of solutions, suspensions, tablets, pills, capsules, powders, sustained-release formulations and the like. Suitable pharmaceutical carriers are described in "Remington's Pharmaceutical Sciences" by E. W. Martin. Such compositions will contain an effective therapeutic amount of the active compound together with a suitable amount of carrier so as to provide the form for proper administration to the patient. While intravenous injection is a very effective form of administration, other modes can be employed, including but not limited to intraventricular, intramuscular, intraperitoneal, intra-arteriolar, and subcutaneous injection, and oral, nasal and parenteral administration.
The therapeutic agents of the instant invention may be used for the treatment of animals, and more preferably, mammals, including humans, as well as mammals such as dogs, cats, horses, cows, pigs, guinea pigs, mice and rats.
In another embodiment, the therapeutic compound can be delivered in a vesicle, in particular a liposome (see Langer, Science 249:1527-1533 (1990); Treat et al., in Liposomes in the Therapy of Infectious Disease and Cancer, Lopez-Berestein and Fidler (eds.), Liss, New York, pp. 353-365 (1989); Lopez-Berestein, ibid., pp. 317-327; see generally ibid.)
In yet another embodiment, the therapeutic compound can be delivered in a controlled release system. In one embodiment, a pump may be used (see Langer, supra; Sefton, CRC Crit. Ref. Biomed. Eng. 14:201 (1987); Buchwald et al., Surgery 88:507 (1980); Saudek et al., N. Engl. J. Med. 321-574 (1989)). In another embodiment, polymeric materials can be used (see Medical Applications of Controlled Release, Langer and Wise (eds.), CRC Pres., Boca Raton, Fla. (1974); Controlled Drug Bioavailability, Drug Product Design and Performance, Smolen and Ball (eds.), Wiley, New York (1984); Ranger and Peppas, J. Macromol. Sci. Rev. Macromol. Chem. 23:61 (1983); see also Levy et al., Science 228:190 (1985); During et al., Ann. Neurol. 25:351 (1989); Howard et al., J. Neurosurg. 71:105 (1989)). In yet another embodiment, a controlled release system can be placed in proximity of the therapeutic target, i.e., the brain, thus requiring only a fraction of the systemic dose (see, e.g., Goodson, in Medical Applications of Controlled Release, supra, vol. 2, pp. 115-138 (1984)).
Other controlled release systems are discussed in the review by Langer (Science 249:1527-1533 (1990)).
EXAMPLES
A series of compounds were prepared and tested for their histamine H 3 receptor antagonist activity. The results are summarized in Table 1. The antagonist activity of the compounds was detected by observing inhibition of ( 3 H)-N-(alpha)methylhistamine activity on rat brain membranes.
SYNTHESIS OF THE COMPOUNDS
The amide and carbamate compounds of Table 1 were synthesized from 4-(4-piperidyl)-1H-imidazole by two general procedures:
Procedure A: 4-(4-piperidyl)-1H-imidazole and the appropriate acid chloride were conjugated using dicyclohexylamine as base according to the following scheme: ##STR5##
Procedure B: 4-(4-piperidyl)-1H-imidazole and the corresponding acid anhydride were conjugated using triethylamine as base according to the following scheme: ##STR6##
PREPARATION OF 4-(1-CYCLOHEXYLVALEROYL-4-PIPERIDYL) 1H-IMIDAZOLE (COMPOUND 1)
To a mixture of 755 mg (5.00 mmol) 4-(4-piperidyl)-1-H-imidazole and 942 mg (5.20 mmol) of dicyclohexylamine in 10 ml anhydrous acetonitrile at 25° C. was slowly added 1.06 g (5.20 mmol) cyclohexanevaleroyl chloride in 2 ml of dichloromethane over a period of 10 min with stirring; then the reaction mixture was heated at 60° C. for 1.5 h. After cooling to ambient temperature, the solid side product that was obtained (dicyclohexylammonium chloride) was filtered off and the filtrate was concentrated in vacuo to remove acetonitrile. The resulting crude oil was crystallized with methanol: anhydrous diethyl ether to give 1.085 mg of analytically pure product as a yellow powder. Yield: 68% M.P.: 159° C.; MS: m/e=317(M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.65 (s, 1H), 6.75 (s, 1H); cyclohexylbutyl: δ2.20 (m, 8H), 1.20 (m, 11H); piperidyl: 4.65 (d, 2H), 3.95 (d, 2H), 3.10 (d, 2H), 2.84 (m, 1H), 2.20 (m, 2H).
Compounds No. 3, 4, 5, 6, 7, 8, 9, 10, 11 and 12 in Table I were synthesized in similar manner, i.e., by condensation of the acid chloride with 4(4-piperidyl) 1-H-imidazole in the presence of dicyclohexylcarbodiimide. Purified product was obtained by preparative TLC Silica Gel GF. 60 (2000 Microns) and the solvent of recrystallization was methanol:anhydrous ether (20:80).
Compound No. 3, yield: 70%; oil; MS m/e 275 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.60 and 6.75 (s, 1H); piperidine H: complex, δ4.65 (d, 2H), 3.90 (d, 2H), 3.10 (m, 3H), 2.10 (m, 2H); cyclohexyl acetyl H: δ1.50 (m, 11H), 2.80 (m, 2H).
Compound No. 4, yield: 67%; oil; MS: m/e 267 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.50 and 6.60 (s, 1H); piperidine H: complex, δ3.90 (d, 2H), 2.80 (m, 3H), 2.55 (m, 2H), 1.80 (m, 2H); phenyl acetyl H: δ7.10 (m, 5H), 1.50 (m, 2H).
Compound No. 5, yield: 71%; oil; MS: m/e 297 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.80 and 6.70 (s, 1H); piperidine H: complex, δ4.60 (d, 2H), 3.80 (d, 2H), 3.10 (m, 3H), 1.80 (d, 2H); phenyl propyl H: δ7.20 (m, 5H), 2,65 (m, 2H), 235 (m, 2H), 2.10 (m, 2H).
Compound No. 6, yield: 74%; oil; MS: m/e 289 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.70 and 6.80 (s, 1H); piperidine H: complex, δ4.60 (d, 2H), 3.85 (d, 2H), 3.10 (m, 3H), 1.90 (m, 2H); cyclohexyl ethyl H: δ1.10 (m, 11H), 2.00 (br, 2H), 2.20 (m, 2H).
Compound No. 7, yield: 75%; oil; MS: m/e 283 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.60 and 6.70 (s, 1H); piperidine H: complex, δ4.60 (d, 2H), 3.90 (d, 2H), 3.10 (m, 3H), 1.80 (m, 2H); phenyl ethyl H: δ7.30 (m, 5H,) 2.10 (br, 2H), 1.50 (m, 2H).
Compound No. 8, yield: 69%; M.P.: 151° C.; MS: m/e 327 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.65 and 6.80 (s, 1H); piperidine H: complex, δ4.70 (d, 2H), 4.50 (d, 2H), 3.60 (m, 1H), 2.80 (m, 2H), 2.10 (m, 2H); adamantyl acetyl H: δ1.80 (m, 12H), 3.10 (m, 2H), 4.05 (m, 1H).
Compound No. 9, yield: 62%; M.P.: 148° C. (decomposed); MS: m/e 357 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.60 and 6.85 (s, 1H); piperidine H: complex, δ4.50 (d, 2H), 4.05 (m, 3H), 3.40 (d, 2H), 2.10 (m, 2H); dicyclohexyl acetyl H: δ1.50 (m, 22H), 2.50 (m, 1H).
Compound No. 10, yield: 64%; oil; MS: m/e 281 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.75 and 6.60 (s, 1H); piperidine H: complex, δ4.70 (d, 2H), 4.20 (m, 3H), 2.80 (m, 2H), 2.10 (d, 2H); phenyl vinyl H: δ7.40 (m, 5H), 6.50 (m, 2H).
Compound No. 11, yield: 62%; oil; MS m/e 351 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.50 and 6.40 (s, 1H); piperidine H: complex, δ4.60 (d, 2H) 4.10 (m, 3H), 2.80 (d, 2H), 1.80 (m, 2H); phenyl cyclohexyl acetyl H: δ7.20 (m, 5H), 1.80 (m, 11H), 3.70 (m, 1H).
Compound No. 12, yield: 72%; M.P.: 136° C.; MS:m/e 304 (M+); 1 H NMR (CDCl 3 ): imidazole H: δ7.70 and 6.80 (s, 1H); piperidine H: complex, δ4.60 (d, 2H), 4.00 (m, 2H), 3.60 (m, 3H), 1.88 (m, 2H); cyclohexyl propyl H; complex, δ1.20 (m, 17H).
PREPARATION OF 4-(t-BUTOXY CARBONYL-4-PIPERIDYL) 1H-IMIDAZOLE (COMPOUND 2)
To a suspension of 224 mg (1.00 mmol) of 4-(4-piperidyl)-1H-imidazole dihydrochloride in 10 ml of methanol was added 202 mg (2.00 mmol) of triethylamine (the suspension turned to a clear solution) followed by dropwise addition of 218 mg (1.00 mmol) of di-t-butyl dicarbonate in 5 ml methanol over a period of 10 min. The reaction mixture was stirred at 25° C. for 6 h, at the end of which the volatile materials were removed in vacuo. The oily residue was partitioned between 50 ml chloroform and 25 ml water. The organic layer was washed with 50 ml brine solution, then dried over anhydrous sodium sulfate. After filtration and removal of solvent, a pale yellow oil was obtained. The oil was treated with a mixture of methanol: petroleum ether (10:90). The resulting mixture was agitated vigorously with a glass rod until a solid appeared. After filtration and drying, the desired product was obtained as a white power. Yield: 65%; M.P.: 198° C.; MS: m/e 251 (M + ); 1 H NMR (CDCl 3 ): imidazole H: δ7.60 (s, 1H) and 6.60 (s, 1H); piperidine H: δ4.20 (d, 2H), 2.80 (m, 4H), 2.20 (d, 2H), 1.60 (m, 1H), t-BOC H: 1.45 (s, 9H).
Compounds No. 13 and 14 in Table I were synthesized in similar manner. The pure product was obtained by preparative TCL Silica GEL GF, 60 (2000 microns), and the solvent of recrystallization was methanol:anhydrous ether (20:80).
Compound No. 13, yield: 78%; M.P.: 180° C.; MS: m/e 255 (M+); 1 H NMR (DMSOd 6 ): imidazole H: δ7.95 and 6.80 (s, 1H), NH: δ7.80 and 6.60 (d, 1H); piperidine H: complex, δ4.50 (d, 2H), 3.60 (m, 3H), 3.10 (m, 1H), 2.75 (m, 2H); phenyl H: δ7.40 (m, 5H); MA: (C,H,N,): 70.36%, 6.71%, 16.30%.
Compound No. 14, yield: 72%; M.P.: 185° C.; 1 H NMR (CDCl 3 ); imidazole H: δ7.60 and 6.80 (s, 1H); piperidine H: complex, δ4.50 (d, 2H), 3.00 (m, 3H), 2.05 (d, 2H), 1.60 (m, 2H); t-butyl H: δ1.10 (s, 9H).
PREPARATION OF 4(-4-PIPERIDYL)-1H-IMIDAZOLE
In a preferred embodiment, 4(4-piperidyl)-1H-imidazole for use in the synthesis of the H 3 -receptors antagonists is prepared according to the following method.
Bromination of 4-acetyl piperidine (Aldrich) in hydrogen bromide/acetic acid was performed as described (Barlin et al., Aust. J. Chem 42:735 (1989)).
A mixture of 11.23g (4.00 mmol) of bromoacetyl pyridine and 3.98 ml (10.0 mmol) formamide were fused together at 110° C. with stirring for 4 h. The crude reaction mixture was then concentrated on the rotary evaporator to remove volatile matter. The residue was dissolved in 50 ml methanol, and to this solution was added 100 ml anhydrous dimethyl ether slowly with stirring, which led to the formation of a brown precipitate. After stirring for another 0.5 h, the precipitate was filtered, washed with 50 ml anhydrous ether and dried. This solid residue was dissolved in 20 ml water and the aqueous solution was basified to pH 9 with sodium carbonate. To this solution was added 150 ml absolute ethanol slowly with stirring till a solid formed, which was filtered off. The filtrate was heated to boiling, then treated with activated carbon and filtered. The filtrate was concentrated on rotary evaporator to dryness. Yield: 3.36g 58%; M.P.: 152° C. (decomposed); MS: m/e 145 (M+), 1 H NMR (D 2 O): imidazole H: δ7.80 (s, 1H) and 7.20 (s, 1H); pyridyl H: 8.10 (d, 2H), 7.17 (d, 2H). The pyridyl moiety was reduced by catalytic hydrogenation using 5-10% rhodium on carbon in acidified water at 20-55 atmospheres as described (Schunack, Archiv. Pharma. 306:934 (1973)).
ANTAGONIST ACTIVITY IN VITRO
The various compounds were tested for the ability to bind to the histamine H 3 receptor. A binding assay in a rat brain membrane preparation, based on inhibition of binding of [ 3 H]-N-alpha-methylhistamine using excess unlabeled alpha-methylhistamine to account for nonspecifc binding, was developed. Total, specific and nonspecific binding of [3H]-N-alphamethylhistamine to brain membranes is shown in FIG. 1. The K d value was 0.19 nM in this preparation and the nonspecific binding was less than 20% of the total binding at the Kd value. The compounds thioperamide (Arrang et al., Nature 327:117-123 (1987)) and burimamide (Black et al., Nature 236:385-390 (1972)) were tested as controls for this assay. The results are shown in Table I.
TABLE I__________________________________________________________________________4-Piperidyl (imidazole) Compounds andTheir Activities on Rat Brain Membranes.(.sup.3 HN.sup.α -methylhistamine as Radioligand)__________________________________________________________________________Cmpd XNo. R.sub.1 (CO(O).sub.x (CH.sub.2).sub.n R) IC.sub.50 (nm) M.P.__________________________________________________________________________Thioperamide H 4.0 ± 0.6 170° C. n = 4 Burimamide 156 ± 57 1 H ##STR7## 23 ± 6 n = 3 159° 3 H ##STR8## 19 ± 12 n = 3 Oil 4 H ##STR9## 1400 ± 437 n = 3 Oil 5 H ##STR10## 262 ± 9 N = 3 Oil 6 H ##STR11## 34 ± 1.4 n = 3 Oil 7 H ##STR12## 34.1 ± 3.6 n = 3 Oil12 H ##STR13## 41.4 ± 9 n = 3 136° C.13 H ##STR14## 151 ± 44 n = 4 180° C.41 H ##STR15## inactive n = 2(1 μM) 192° C.42 CH.sub.3 ##STR16## inactive n = 2(1 μM) Oil43 X ##STR17## inactive n = 3 99° C.44 X ##STR18## inactive n = 2 81° C.45 X ##STR19## inactive n = 2 79° C.46 PhCH.sub.2 ##STR20## inactive n = 2 62° C.47 H ##STR21## 231 n = 1 185° C.48 H ##STR22## inactive n = 2 168° C.__________________________________________________________________________Cmpd.No. Structure IC.sub.50 (Nm) M.P.__________________________________________________________________________50 ##STR23## inactive n = 2(μM) 148.5°-150.5° C. ##STR24## 243.5 ± 1.9 n = 2 198° C.14 ##STR25## inactive n = 2 185° C.8 ##STR26## inactive n = 2 151° C.9 ##STR27## inactive n = 2 148° C.10 ##STR28## 570 ± 172 n = 3 Oil11 ##STR29## 260 ± 38 n = 2 Oil51 ##STR30## 115° C.__________________________________________________________________________
DISCUSSION
The results in Table I show that the compounds of the invention are effective for binding to the histamine H 3 -receptor. Interestingly, cyanoguanidine derivatives (e.g., compounds 47, 48 and 50) were ineffective at binding to the H 3 -receptor. This result is in contrast to earlier observations about H 2 -receptor antagonists. With H 2 -receptor antagonists, cyanoguanidine and thiourea-containing derivatives (cimetidine and metiamide, respectively) were found to be bioisosteres, i.e., functionally substantially equivalent (Brimblecombe et al., Gastroenterology 74:339-347 (1978)).
PHARMACOLOGICAL EVALUATION IN THE CNS
A representative compound, 1, was tested in vivo for (1) the ability to penetrate the blood brain barrier; and (2) the effect of behavior in mice.
PENETRATION OF THE BLOOD-BRAIN BARRIER
Blood-brain barrier penetration in rats was assessed by an ex vivo binding procedure. Young adult male Long-Evans rats were injected i.p. with saline or H 3 antagonists in saline. At various times after injection animals were sacrificed, the cortex was removed, homogenized in 50 mM Na/K-phosphate buffer, pH 7.4, and the binding of 1 nM [ 3 H]-N.sup.α -methylhistamine was measured using 400 μg protein of the homogenate. Nonspecific binding was accounted for by the inclusion of excess thioperamide in some samples. Under these conditions, the binding was approximately 90% specific.
As shown in FIG. 2, thioperamide at doses of 2, 5, and 10 mg/kg, when measured 15 min after injection, decreased the binding of [ 3 H]-Nα-methylhistamine to H 3 receptors in the cortex. This means that the thioperamide at these doses and after this time was able to penetrate the blood-brain barrier. FIG. 3 shows that compound 1 also penetrates the blood-brain barrier one hour after injections of doses of 50 and 70 mg/kg. Taking into account the difference in affinity comparing thioperamide (4.0 nM) and compound 1 (23 nM), these data suggest that compound 1 penetrates the blood-brain barrier at least as well as thioperamide.
BEHAVIORAL EFFECTS IN MICE
The overall strategy to show central nervous system antagonist activity was to challenge effects of the agonist (R)α-methylhistamine. Therefore, the first objective was to establish a dose response curve for behavioral effects of (R)α-methylhistamine. Male albino CF-1 mice weighing 20-30 g were used. Saline or (R)α-methylhistamine in saline was injected i.p. in a volume ≦0.4 ml. Animals were observed for various behaviors three times for 10 seconds during each 10 minute interval for a total of 2 hours. Animals were scored for the presence (1) or absence (0) of the behavior and the results were reported as the accumulated score for a 30 minute period (maximum score=9). As shown in FIG. 4, (R)α-methylhistamine produced a dose-dependent (range of 15 to 35 mg/kg) increase in sleeping one hour after injection. The effect was also evident at 30 minutes after injection.
To assess the effects of antagonists, they were administered with the (R)α-methylhistamine in saline. FIG. 5 shows that thioperamide was able to inhibit the soporific effect of 30 mg/kg of (R)α-methylhistamine. With thioperamide alone (i.e., in the absence of the α-methylhistamine H 3 receptor agonist), animals were very active, exhibiting normal behaviors. FIG. 6 shows that compound 1 inhibited the soporific effect of 25 mg/kg (R)α-methylhistamine.
DISCUSSION
The results of the in vitro (see section 6, supra) and in vivo activity assays show that a compound of the invention is useful for increasing histamine activity in the brain.
In the foregoing in vivo assays, thioperamide was used as a positive control. The results indicate that compound 1 is effective as an H 3 -receptor antagonist. Direct comparison of the two compounds is not available from the data, however, since the experimental protocols used to test each were not identical.
It is noteworthy that in all testing to date, no toxicity of the 1 compound has been observed, even at high doses.
SPECIFICITY OF COMPOUND 1
The selecitivity of action of compound 1 for histamine H 3 -receptors was determined in a NOVASCREEN™ receptor selectivity study. At concentrations of 10 -5 M, no significant binding to adenosine, excitory or inhibitory amino acid, dopamine, serotonin, or a broad range of petidergic receptors, or to ion channel proteins, peptide factor or second messenger systems was observed. The binding study results are shown in Table II.
TABLE II______________________________________NOVASCREEN ™ RECEPTOR SELECTIVITY ASSAY Initial Percent Inhibition Refer- (Average;Receptor/ Reference ence N = 2)Selectivity Compound K.sub.i (nM) 10.sup.-5 M______________________________________AdenosineAdenosine NECA 120.00 -3.0Amino AcidsEcitatoryQuisqualate Quisqualic Acid 11.80 -1.8Kainate Kainic Acid DME 24.93 42.1MK-801 MK801 4.30 -8.6NMDA NMDA 359.00 -4.5PCP PCP 62.30 9.7Glycine Glycine 300.00 1.8InhibitoryGlycine Strychinine Nitrate 33.50 17.4GABA.sub.A GABA 2.80 0.6GABA.sub.B GABA 176.00 0.0Benzodiazephine Clonazepam 3.40 2.7Biogenic AminesDopamine 1 Butaclamol 37.30 6.4Dopamine 2 Spiperone 0.08 3.5Serotonin 1 Serotonin 4.60 -3.6Serotonin 2 Serotonin 531.00 10.5PeptidesAngiotensin Angiotensin II 0.20 6.5Arg-Vasopressin V.sub.1 arg-Vasopressin 4.90 10.1Bombesin Tyr4-Bombesin 0.55 -5.5CCK Central CCK 0.13 18.6CCK Peripheral CCK 0.02 6.9Substance K Neurokinin A 2.75 29.2Substance P Substance P 0.08 20.0NPY Neuropeptide Y 0.50 -8.7Neurotensin Neurotensin 1.23 -10.5Somatostatin Somatostatin 0.03 4.1VIP VIP 1.53 17.1Channel ProteinsCalcium w-Conotoxin 0.01 1.9Calcium Nifedipine 1.60 8.1Chloride TBPS 112.40 -3.4Potassium Apamin 0.05 7.7Peptide FactorsANF (rat) ANP 0.15 0.1EGF EGF 0.24 18.1NGF NGF 0.80 17.1Second MessengerSystems Forskolin 29.40 2.1Adenylate CyclaseForskolinProtein Kinase CPhorbol Ester PDBU 16.50 0.9Inositol Triphosphate IP3 12.50 9.2______________________________________ Values are expressed as the percent inhibition of specific binding and represent the average of duplicate tubes at each of the concentrations tested. Bolded values represent inhibition of fifty percent or greater.
The present invention is not to be limited in scope by the specific embodiments described herein. Indeed, various modifications of the invention in addition to those described herein will become apparent to those skilled in the art from the foregoing description and accompanying figures. Such modifications are intended to fall within the scope of the appended claims.
Various publications are cited herein, the disclosures of which are incorporated by reference in their entireties.
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The present invention provides novel compounds having activity as histamine H 3 -receptor antagonists. The novel compounds include 4-imidazolyl-N-substituted pyrrolidines, piperidines, and cycloheptimides. The preferred compounds are 4-imidazolyl-N-(cycloalkyl/aryl-alkyl-carbonyl) piperidines such as 4-(1-cyclohexylvaleryol-4-piperidyl)-1H-imidazole.
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CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application is a continuation of application Ser. No. 09/700,037, filed Jul. 2, 2001, which is the National Stage of International Application No. PCT/US99/12128, filed Jun. 1, 1999, which claims the benefit of Provisional Application No. 60/087,524, filed Jun. 1, 1998, the disclosures of which are hereby incorporated by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to classification of plant embryos for determination of suitability for germination or other treatments. In particular, it is concerned with selection of conifer somatic embryos most likely to be successfully germinated and to produce normal plants.
BACKGROUND
[0003] Reproduction of selected plant varieties by tissue culture has been a commercial success for many years. The technique has enabled mass production of genetically identical selected ornamental plants, agricultural plants and forest species. The woody plants in this last group have perhaps posed the greatest challenges. Some success with conifers was achieved in the 1970s using organogenesis techniques wherein a bud, or other organ, was placed on a culture medium where it was ultimately replicated many times. The newly generated buds were placed on a different medium that induced root development. From there, the buds having roots were planted in soil.
[0004] While conifer organogenesis was a breakthrough, costs were high due to the large amount of handling needed. There was also some concern about possible genetic modification. It was a decade later before somatic embryogenesis achieved a sufficient success rate so as to become the predominant approach to conifer tissue culture. With somatic embryogenesis, an explant, usually a seed or seed embryo, is placed on an initiation medium where it multiplies into a multitude of genetically identical immature embryos. These can be held in culture for long periods and multiplied to bulk up a particularly desirable clone. Ultimately, the immature embryos are placed on a development or maturation medium where they grow into somatic analogs of mature seed embryos. These embryos are then individually selected and placed on a germination medium for further development. Alternatively, the embryos may be used in manufactured seeds.
[0005] There is now a large body of general technical literature and a growing body of patent literature on embryogenesis of plants. Examples of procedures for conifer tissue culture are found in U.S. Pat. Nos. 5,036,007 and 5,236,841 to Gupta et al.; U.S. Pat. No. 5,183,757 to Roberts; U.S. Pat. No. 5,464,769 to Attree et al.; and U.S. Pat. No. 5,563,061 to Gupta.
[0006] One of the more labor intensive and subjective steps in the embryogenesis procedure is the selection from the maturation medium of individual embryos suitable for germination. The embryos may be present in a number of stages of maturity and development. Those that are most likely to successfully germinate into normal plants are preferentially selected using a number of visually evaluated screening criteria. Morphological features such as axial symmetry, cotyledon development, surface texture, color, and others are examined and applied as a pass/fail test before the embryos are passed on for germination. This is a skilled yet tedious job that is time consuming and expensive. Further, it poses a major production bottleneck when the ultimate desired output will be in the millions of plants.
[0007] It has been proposed to use some form of instrumental image analysis for embryo selection to replace the visual evaluation described above. For examples, refer to Cheng, Z. and P. P. Ling, “Machine Vision Techniques for Somatic Coffee Embryo Morphological Feature Extraction,” Trans. Amer. Soc. Agri. Eng. 37:1663-1669 (1994), or Chi, C.M., C. Zhang, E. J. Staba, T. J. Cooke, and W-S. Hu, “An Advanced Inage Analysis System for Evaluation of Somatic Embryo Development,” Biotech. and Bioeng. 50:65-72 (1996). All of these methods require considerable pre-judgment of which morphological features are important and the development of mathematical methods to extract this information from the images. Relatively little of the information from the image has actually been used.
[0008] The problem of how to best use image analysis to automate the selection of somatic embryos after they had been separated from residual tissue, singulated, and imaged in color from multiple positions has not been successfully addressed. Various methods are known for extracting size and shape information from scanned images. As one example, Moghaddam et al., U.S. Pat. No. 5,710,833, describes a method useful for recognition of any multifeatured entity such as a human face. Sclaroff et al., U.S. Pat. No. 5,590,261, describes a method that can be used for object recognition purposes.
[0009] Where embryos are concerned, a further problem using scanning technology is that morphology differs between clones within a given species. The differences between acceptable and rejected embryos can be very subtle, varying by clone. Hence, the choice of selection criteria for machine use tends to be subjective, difficult to specify mathematically, and may be clone specific.
[0010] The development of high speed computers and new spectroscopic hardware has led to the development of new instruments which have the capability to rapidly acquire spectra on large numbers of samples. However, the acquisition of vast amounts of spectral data from a sample necessitates the development of similarly powerful data analysis tools to uncover subtle relationships between the collected spectra and the chemical properties of the sample. One such data analysis methodology, commonly known as chemometrics, applies multivariate statistical techniques to complex chemical systems in order to facilitate the discovery of the relationship between the absorption, transmittance or reflectance spectral data acquired from a sample and some specified property of the sample that is subject to independent measurement. The end result of multivariate analysis is the development of a predictive classification model that allows new samples of unknown properties to be rapidly and accurately classified according to a specified property based upon the acquired spectral data. For example, multivariate analysis techniques such as: principal component analysis (PCA) and a principal component-based method, projection to latent structures (PLS), have been used to explore the multivariate information in previous applications of near-infrared (NIR) spectroscopy to the pulp and paper industry to develop classification models for paper quality. See, for example, U.S. Pat. Nos. 5,638,284, 5,680,320, 5,680,321, and 5,842,150.
SUMMARY
[0011] The present invention is based on classification of plant embryos by the application of classification algorithms to digitized images and absorption, transmittance, or reflectance spectra of the embryos. The methods are generally applicable and emphasize the importance of acquiring and using as much image and absorption, transmittance, or reflectance spectral information as possible, based on objective criteria. One goal has been automated classification and selection of embryos most suitable for further culture and rejection of those seen as less suitable. The technique is capable of utilizing more complex imaging technology; e.g., multi-viewpoint images and images in color or from non-visible portions of the electromagnetic spectrum.
[0012] In one aspect of the present invention, a method for classifying plant embryos according to embryo quality is provided. The method first develops a classification model by acquiring raw digital image data of reference samples of plant embryos of known embryo quality. Optionally, the raw digital image data is preprocessed using one or more preprocessing algorithms to reduce the amount of raw image data yet retain substantially all of the image data that contains geometric and color information regarding the embryo or embryo organ. An example of such an optional preprocessing technique involves removing image data that is not derived from the plant embryo or plant embryo organ. Another optional preprocessing step results in the calculation of metrics which emphasize image features that are particularly important in embryo quality classification. Data analysis is performed on the raw digital image data, or on the preprocessed image data depending upon which method is followed, using one or more classification algorithms to develop a classification model for classifying plant embryos by embryo quality. During this data analysis one or more of the classification algorithms utilizes raw digital image data representative of more than just the embryo perimeter, or the preprocessed image data to develop the classification model. The embryo quality of the reference samples is determined by reference to such qualities as morphological comparison to normal zygotic plant embryos, determination of the reference embryo's conversion potential, resistance to pathogens, drought resistance and the like. Raw digital image data of plant embryos of unknown embryo quality is then acquired using the same methods as performed on the reference samples. The acquired raw digital image data is then analyzed using classification algorithms used to develop the classification model in order to classify the quality of the plant embryo of unknown quality. A more robust method is obtained by acquiring raw digital image data of multiple views of the embryo, such as end-on views of the embryo and/or longitudinal views.
[0013] In another aspect of the present invention plant quality is classified by developing a single metric classification model by acquiring raw digital image data of reference samples of whole plant embryos or any portion thereof from plant embryos of known embryo quality. A metric value is calculated from the acquired raw digital image data of each embryo of known quality. The metric values are divided into two sets of metric values based upon the known embryo quality. A Lorenz curve is calculated from each set of metric values. A threshold value is determined from a point on the Lorenz curve which serves as a single metric classification model to classify plant embryos by embryo quality. Raw image data is acquired from a whole plant embryo or any portion thereof from a plant embryo of unknown quality. The single metric classification model developed from embryos of know quality is applied to the raw image data acquired from plant embryos of unknown quality in order to classify the quality of the unknown plant embryo. Single metric classification models can optionally be combined using one or more classification algorithms to develop more robust classification models for classifying plant embryos by embryo quality.
[0014] In another embodiment of the present invention, plant embryo quality is classified by collecting absorption, transmittance or reflectance spectral raw data from plant embryos or portions thereof and processing the data using classification algorithms. The inventive method first requires that a classification model be developed by acquiring absorption, transmittance or reflectance spectral raw data of reference samples of plant embryos or portions thereof whose embryo quality is known. In one alternative embodiment, prior to making the classification model, the spectral raw data in whole or in specific parts is preprocessed to among other things, reduce noise and adjust for drift and diffuse light scatter. The classification model is then made by performing a data analysis using classification algorithms on the preprocessed spectral raw data. Absorption, transmittance or reflectance spectral raw data is then acquired from a plant embryo of unknown embryo quality. The spectral raw data collected from the embryo of unknown quality is either applied directly to the embryo quality classification model or preprocessed to reduce noise and adjust for drift and diffuse light scatter and then the preprocessed spectral data is applied to the classification model depending upon which method was used to make the classification model in use. In either case, the application of the unknown spectral data to the classification model allows classification of the quality of the plant embryo of unknown plant embryo quality.
DESCRIPTION OF THE DRAWINGS
[0015] The foregoing aspects and many of the attendant advantages of this invention will become more readily appreciated as the same becomes better understood by reference to the following detailed description, when taken in conjunction with the accompanying drawings, wherein:
[0016] FIG. 1 shows a diagrammatic representation of a tree embryo 8 . The circled areas represent the embryo regions representative of the three embryo organs known as cotyledon 10 , hypocotyl 12 , and radicle 14 .
[0017] FIG. 2A displays a scoreplot obtained from principal component analysis of spectral data collected from Douglas-fir zygotic embryos of three different developmental stages and a set of Douglas-fir somatic embryos (genotype 1 ). The units on the principal component (PC) axes are universal standard deviations for the set.
[0018] FIG. 2B shows the loadings spectra for each PC depicted in FIG. 2A . Each curve shows the relative contribution that each wavelength makes in accounting for the variance depicted along the scoreplot axes in FIG. 2A .
[0019] FIG. 3A displays a scoreplot obtained from principal component analysis of spectral data collected from loblolly pine zygotic embryos of two different developmental stages and two sets of somatic embryos (genotypes 5 and 7 ). The units on the PC axes are universal standard deviations for the set, and the crossover of zero axes is the average behavior of all the embryos.
[0020] FIG. 3B shows the loadings spectra for each PC depicted in FIG. 3A . Each curve shows the relative contribution that each wavelength makes in accounting for the variance depicted along the scoreplot axes in FIG. 3A .
[0021] FIG. 4A displays a scoreplot obtained from principal component analysis of spectral data collected from Douglas-fir somatic embryos at the cotyledonary stage (genotype 2 ) that have “good” and “poor” embryo morphology. The units on the PC axes are universal standard deviations for the set.
[0022] FIG. 4B shows the loadings spectra for each PC depicted in FIG. 4A . Each curve shows the relative contribution that each wavelength makes in accounting for the variance depicted along the scoreplot axes in FIG. B.
[0023] FIG. 5A displays a scoreplot obtained from principal component analysis of spectral data collected from loblolly pine somatic embryos (genotype 5 ) at the cotyledonary stage that have “good” and “poor” embryo morphology. The units on the PC axes are universal standard deviations for the set.
[0024] FIG. 5B shows the loadings spectra for each PC depicted in FIG. 5A . Each curve shows the relative contribution that each wavelength makes in accounting for the variance depicted along the scoreplot axes in FIG. 5A .
[0025] FIG. 6A displays a scoreplot obtained from principal component analysis of spectral data collected from Douglas-fir somatic embryos (genotype 3 ). The scanned somatic embryos were of two different developmental stages, the cotyledon stage and “dome” or “just cotyledon” stage. The units on the PC axes are universal standard deviations for the set.
[0026] FIG. 6B shows the loadings spectra for each PC depicted in FIG. 6A . Each curve shows the relative contribution that each wavelength makes in accounting for the variance depicted along the scoreplot axes in FIG. 6A .
[0027] FIG. 7A displays a scoreplot obtained from principal component analysis of spectral data collected from Douglas-fir somatic embryos (genotypes 3 and 4 ). A set of somatic embryos from each genotype were either subjected to a cold treatment (which improves germination) or received no cold treatment (Control). The units on the PC axes are universal standard deviations for the set.
[0028] FIG. 7B shows the loadings spectra for each PC depicted in FIG. 7A . Each curve shows the relative contribution that each wavelength makes in accounting for the variance depicted along the scoreplot axes in FIG. 7A .
[0029] FIG. 8A displays a scoreplot obtained from principal component analysis of spectral data collected from loblolly pine somatic embryos (genotypes 5 and 7 ) at the cotyledonary stage. A set of somatic embryos from each genotype were either subjected to a cold treatment (which improves germination) or received no cold treatment (Control). The units on the PC axes are universal standard deviations for the set.
[0030] FIG. 8B shows the loadings spectra for each PC depicted in FIG. 8A . Each curve shows the relative contribution that each wavelength makes in accounting for the variance depicted along the scoreplot axes in FIG. 8A .
DETAILED DESCRIPTION
[0031] The inventive methods are used to classify any type of plant embryos, such as, for example, zygotic and somatic embryos, by any embryo quality that is amenable to characterization. For example, embryo quality can be defined using morphological criteria such as axial symmetry, cotyledon development, surface texture and color. As used herein “zygotic morphology” refers to morphological criteria, such as axial symmetry, cotyledon development, surface texture and color that are characteristic of a normal zygotic plant embryo. Alternatively, embryos can be classified using developmental or functional criteria, such as embryo germination and subsequent plant growth and development, often collectively referred to in the literature as “conversion.” As used herein “conversion potential” refers to the capacity of a somatic embryo to germinate and/or survive and grow in soil, preceded or not by desiccation or cold treatment of the embryo. In addition, “plant embryo quality” refers to other plant characteristics such as resistance to pathogens, drought resistance, heat and cold resistance, salt tolerance, preference for light quality, suitability for long term storage of somatic embryos or any other plant quality susceptible to quantification.
[0032] Embryos from all plant species can be adapted to the inventive methods. The methods have particular application to agricultural plant species where large numbers of somatic embryos are used to propagate desirable genotypes such as with forest tree species. In particular, the methods can be used to classify somatic embryos from conifer tree family Pinaceae, particularly from the genera: Pseudotsuga and Pinus. A diagrammatic drawing of a Pseudotsuga tree embryo 8 is presented in FIG. 1 in which the general locations of the three embryo organs, cotyledon 10 , hypocotyl 12 , and radicle 14 are indicated.
[0033] In one embodiment of the present invention images of plant embryos or plant embryo organs are acquired in a digital form by scanning one or more views of the embryos or organs from multiple positions using known technology, such as electronic camera containing a charge couple devise (CCD) linked to a digital storage devise. A classification model for plant embryo quality is then developed by performing a data analysis on the digital image data using one or more classification algorithms. Examples of such classification algorithms include, but are not limited to, principal components analysis (see, for example, Jackson, J. E., A User's Guide to Principal Components, John Wiley and Sons, New York (1991); Jolliffe, I. T., Principal Components Analysis, Springer-Verlag, N.Y. (1986); Wold, S., “Pattern Recognition by Means of Disjoint Principal Components Models,” Pattern Recognition 8:127-139 (1976); and Watanapongse, P. and H. H. Szu, “Application of Principal Wavelet Component in Pattern Classification,” Proceedings of SPIE, Wavelet Applications V, H. H. Szu, Editor, vol. 3391, pp. 194-205 (1998)), Artificial Neural Networks (Mitchell, Tom M., Machine Learning, WCB/McGraw-Hill pp. 112-115, (1997)), Bayesian Classifiers (Mitchell at 174-176), Probably Approximately Correct (PAC) Learning (Mitchell at 203-220), Radial Basis Functions which includes the statistical technique of fitting mixture distribution models to data (Mitchell, pp. 238-240), and Nearest-Neighbor Methods (Mitchell at 231-236). In addition to the aforementioned classification algorithms, a new classification algorithm is provided in the present invention to classify plant embryos based upon the Lorenz curve. For a brief introduction to Lorenz curves, see Johnson, S. and N. L. Kotz, Eds. Encyclopedia of Statistical Sciences, John Wiley, vol. 5, pp. 156-161 (1985).
[0034] It is also well known in the art of data analysis that several different algorithms besides Principal Component Analysis (PCA) can be used to develop and use classification models. More specifically, the following statistical techniques can also be adapted to the present invention: Partial Least Squares Regression, Principal Components Regression (PCR), Multiple Linear Regression Analysis (MLR), Discriminant Analysis, Canonical Correlation Analysis, Multivariate Multiple Regression, Classification Analysis, Regression Tree Analysis which includes Classification Analysis by Regression Trees (CART™, Salford Systems, San Diego, Calif.), and Logistic and Probit Regression. See U.S. Pat. No. 5,842,150 and (Mitchell, Tom M., Machine Learning, WCB/McGraw-Hill pp. 112-115, 238-240 (1997)).
[0035] The classification model is deduced from a “training” data set of multiple images of plant embryos or plant embryo organs acquired from embryos having known embryo quality. Embryos providing the training set images are classified as acceptable or unacceptable based on biological fact data such as morphological similarity to normal zygotic embryos or proven ability to germinate or convert to plants. The inventive methods are generally adaptable to any plant quality that is susceptible to quantification. Unclassified embryos are classified as acceptable or not based on how close images of the unclassified embryos fit to the classification model developed from the training set groups.
[0036] As used herein the term “classification algorithm” refers to any sequence of mathematical or statistical calculations, formulae, functions, models or transforms of image or spectral data from embryos used for the purpose of classifying embryos according to embryo quality. A classification algorithm can have just one step or many. In addition, classification algorithms of the present invention can be constructed by combining intermediate classification models or single metric classification models through the use of mathematical algorithms such as the Bayes optimal classifier, neural networks or the Lorenz curve. Except for the single metric classification models, the image classification models of the present invention are derived from a data analysis of more than just embryo perimeter image data acquired from plant embryos or embryo organs during the training sessions that lead to the identification of an embryo quality classification model. That is, the classification models of the present invention, except for the single metric classification models, are developed using at least one classification algorithm which considers more of the acquired raw digital image data than required to define the perimeter of the embryo. Thus, the classification algorithms perform a data analyses that results in the development of a classification model from the image or spectral data without any subjective assumptions being made regarding which data features are important for embryo quality classification.
[0037] As used herein “embryo perimeter” means the pixels in raw digital image data or preprocessed digital image data which define the outer perimeter of an imaged embryo.
[0038] Optionally, the raw digital image data can be preprocessed using preprocessing algorithms. As used hereafter the term “preprocessing algorithm” refers to any sequence of mathematical or statistical calculations, formulae, functions, models or transforms of image or spectral data from embryos used for the purpose of manipulating image or spectral data in order to: 1) remove image or spectral data that is derived from non-embryo sources, i.e., background light scatter or other noise sources; 2) reduce the size of the digital data file that is used to represent the acquired image or spectra of the embryo while retaining substantially all of the data that represents informational features such as geometric embryo shape and surface texture, color, and light absorption, transmittance or reflectance, of the acquired image or spectra; and 3) calculate metrics from the acquired raw image or spectral data and from values obtained during other preprocessing steps, in order to identify and emphasize embryo data that is useful in development of an embryo quality classification model.
[0039] For example, U.S. Pat. No. 5,842,150 discloses that NIR spectral data can be preprocessed prior to multivariate analysis using the Kubelka-Munk transformation, the Multiplicative Scatter Correction (MSC), e.g., up to the fourth order derivatives, the Fourier transformation or by using the Standard Normal Variate transformation, all of which can be used to reduce noise and adjust for drift and diffuse light scatter.
[0040] Alternatively, the amount of digital data required to represent an acquired image or spectrum of an embryo can be reduced using preprocessing algorithms such as wavelet decomposition. See, for example, Chui, C. K., An Introduction to Wavelets, Academic Press, San Diego (1992); Kaiser, Gerald, A Friendly Guide to Wavelets, Birkhauser, Boston; and Strang, G. and T. Nguyen, Wavelets and Filter Banks Wellesley-Cambridge Press, Wellesley, Mass. Wavelet decomposition has been used extensively for reducing the amount of data in an image and for extracting and describing features from biological data. For example, wavelet techniques have been used to reduce the size of fingerprint image files to minimize computer storage requirements. A biological example is the development of a method for diagnosing obstructive sleep apnea from the wavelet decomposition of heart beat data. Wavelets enable rearrangement of the information in a picture of an embryo into size and feature categories. For example, size and shape data may be separated from texture. The results of a wavelet decomposition or functions thereof are then used as inputs to the classification algorithms described above. A variety of other interpolation methods can be used to similarly reduce the amount of data in an image or spectral data file, such as, calculation of adjacent averages, Spline methods (see, for example, C. de Boor, A Practical Guide to Splines, Springer-Verlag, (1978)), Kriging methods (see, for example, Noel A. C. Cressie, Statistics for Spatial Data, John Wiley, 1993)) and other interpolation methods which are commonly available in software packages that handle images and matrices.
[0041] Other preprocessing algorithms can be used to process data collected from an embryo in order to obtain the most robust correlation of the acquired data to embryo quality. For example, in Example 1 several statistical values were calculated to recapture some of the data information that was lost when a wavelet decomposition was used to reduce the size of the image. The recaptured information represented in the metrics allowed the development of a classification model that was better at predicting embryo quality than a model developed from principal component analysis of image data that was preprocessed using wavelet methods. As used hereinafter “metrics” refers to any scalar statistical value that captures geometric, color, or spectral features which contains information about the embryos, such as central and non-central moments, function of the spectral energy at specific wavelengths or any function of one or more of these statistics. In image processing language sets of metrics are also known as feature vectors. In addition, metrics can be derived from external considerations, such as embryo processing costs, embryo processing time, and the complexity of an assembly line sorting embryos by quality.
[0042] In another embodiment of the present invention embryo regions are scanned and spectral data is acquired regarding absorption, transmittance or reflectance of electromagnetic radiation (hereinafter referred to as light) at multiple discrete wavelengths ranging from 180 nm to 4000 nm. Differences in spectral data collected from embryos of high quality (for example, high conversion potential or high morphological similarity to normal zygotic embryos) versus those of low quality are presumed to reflect differences in chemical composition that are related to embryo quality. Numerous studies assert that embryo quality is related to gross chemical composition of the embryo or its parts, especially the amounts of water and storage compounds (proteins, lipids, and carbohydrates). Some examples include: Chanprame, S., T. M. Kuo, and J. M. Widholm, “Soluble Carbohydrate Content of Soybean [ Gycine max (L.) Merr.] Somatic and Zygotic Embryos During Development,” In Vitro Cell Dev. Biol - Plant. 34:64-68 (1998); Dodeman, V. L., M. Le Guilloux, G. Ducreux, and D. de Vienne, “Somatic and Zygotic Embryos of Daucus carota L. Display Different Protein Patterns Until Conversion to Plants,” Plant Cell Physiol. 39:1104-1110 (1998); Morcillo, F., F. Aberlenc-Bertossi, S. Hamon, and Y. Duval, “Accumulation of Storage Protein and 7S Globulins During Zygotic and Somatic Embryo Development in Elaeis Guineensis,” Plant Physiol. Biochem. 36:509-514 (1998); and Obendorf, R. L., A. M. Dickerman, T. M. Pflum, M. A. Kacalanos, and M. E. Smith, “Drying Rate Alters Soluble Carbohydrates, Desiccation Tolerance, and Subsequent Seedling Growth of Soybean ( Glycine mac L. Merrill) Zygotic Embryos During In Vitro Maturation,” Plant Sci. 132:1-12 (1998).
[0043] Spectrometric analysis of embryos can be performed using a data collection setup that includes a light source, a microscope, a light sensor, and a data processor. Preferably, each embryo region undergoes multiple light scans in order to obtain a representative average spectrum. In addition, it is useful that the data processor include a built-in calibration program which is run periodically throughout the data collection phase to recalibrate the internal baseline to correct for dark current, and to recalibrate against the standard white background material upon which the embryo sits.
[0044] Preferably, the light sensor has a measuring interval of at the most 10 nm, preferably 2 nm, and most preferably 1 nm or less. The detection of light is performed in the ultraviolet, visible, and near infrared (including Raman spectroscopy) wavelength range of 180 nm to 4000 nm. This can be accomplished by the use of a scanning instrument, a diode array instrument, a Fourier transform instrument or any other similar equipment, known to the person of skill in the art.
[0045] The classification of embryos according to quality (as defined above) by the spectrometric measurements comprises two main steps. The first is the development of a classification model, involving the substeps of development of training and cross validating sets. Spectral data is acquired from embryos or embryo regions of known embryo quality, optionally a preprocessing of the acquired spectral data is performed, and then a data analysis is performed using one or more classification algorithms to develop a classification model for embryo quality. The second main step is the acquisition of spectrometric data from an embryo whose quality is unknown, optionally performing preprocessing of the acquired spectral data, followed by data analysis of the acquired spectral data using the classification model developed in the first main step.
[0046] Model training sets consist of a large number of absorption, transmittance or reflectance spectra acquired from embryos that have a known high or low quality. The training sets are used in the classification algorithms to develop a classification model. As previously noted, a variety of preprocessing algorithms are available that can be used to first reduce noise and adjust for base line drift. However, for some data sets it may not be necessary to preprocess the data to reduce background noise.
[0047] There are many data analysis methods that can be applied to develop and use classification models that allow plant embryos to be classified by quality. The above described mathematical methods are a sampling of some of the major techniques. However, it should be emphasized that data analysis techniques can be put together in an almost infinite number of combinations to achieve the desired results. For example, a soft independent modeling of class analogy (SIMCA) method can be used on images of embryos which have their color information collapsed into a single array using principal components and then the result can be shrunk using wavelets. SIMCA can then be used to build principal component regression models for each classification category. The Bayes optimal classifier can then be used to combine the classification decisions from six SIMCA model pairs. Partial least squares regression can be used in place of principal component regression in the SIMCA step. Similarly, neural networks can be used in place of Bayes optimal classifier to combine classification decisions into a final classification model.
[0048] In addition, the methods described for classifying plant embryos using embryo image data or absorption, transmittance or reflectance spectral data can be combined together in a number of different ways. For example, data analysis of the acquired raw visual and spectral data can be performed in parallel to develop a unitary classification model or the analysis can be conducted in series whereby two independent classification models are developed using the image and spectral data separately. Many permutations of the methods described herein are possible to accomplish the classification of plant embryos by embryo quality.
[0049] The following nonlimiting examples illustrate the inventive methods and the use of them to classify plant embryos that are most likely to be successfully germinated and produce normal plants.
EXAMPLE 1
Mathematical Methods
[0050] There are three main steps in using light images to separate somatic embryos. They are: 1) cleaning the images to remove raw image data that is not from the plant embryo or embryo organ; 2) reducing the amount of raw image data acquired from the embryo or embryo organ while retaining as much embryo information as possible; and 3) applying one or more classification algorithms to develop and use a classification model for plant embryo quality.
[0000] Cleaning the Images
[0051] Image cleaning requires replacing the background in an image with zeros or pure black. The reason for this is to reduce variation between images. It is desired that the only differences between images be due to the embryos so that comparisons are not confounded with changes in the background. Since the images are magnified, slight variations in position, reflections, glints off leftover material from previous embryos are magnified and contribute to the differences between the images. Cleaning refers to the image processing steps used to eliminate all the variations in the background.
[0052] There is no set recipe for cleaning the embryo images since it is anticipated that as new imaging hardware and software are developed more suitable image cleaning technique will evolve. However, several techniques are generally useful. The examples described below are merely illustrative and are not meant to limit the present invention.
[0053] In the Examples that follow, the image of an embryo, its reflection on its stage and the remaining background were separated from each other using only the red component from the color image. The histogram of the red pixel values was positively skewed. A mixture distribution composed of three normal distributions was fit to the histogram by means of the EM algorithm. For a brief description of the EM algorithm see Mitchell, Tom M., Machine Learning, WCB/McGraw-Hill, pp. 191-196 (1997). The first normal picked up the background, the second normal picked up the reflection and the third component picked up the embryo. The mean of the second normal plus two times its standard deviation was used as the boundary between the reflection and the embryo. The red image was thresholded at this value. The resulting binary image still had some pixels that belonged to the reflection included in it. These were removed by using morphological operations on the binary image. Usually, one to three erosions followed by the same number of dilations are successful in cleaning up the image. Sometimes an extra couple of dilations were needed to restore the embryo part of the binary image to its proper size. Any holes in the embryo part of the binary image were then filled. The resulting binary image was then used to crop the color image and zero all non-embryo parts of the image. Each of the three color matrices in the original image were multiplied by the binary image and then cropped to within two pixels of the embryo. This method worked for all three views of the embryo.
[0054] Alternatively, a different method for cleaning each of the three embryo views can be used. In this alternative method the longitudinal top view of the embryo was preprocessed by first converting the red-green-blue values to hue. Saturation and intensity were not needed for this view. Taking the cotangent of 1/255th of the hue flattened the range of the hue values making it easier to pick up more of the dark tail of the embryo. Only the positive hue values were used since most of the background ends up with negative or zero values for hue. Sometimes the positive hue values alone were enough. A binary image was created by thresholding the cotangent values at 100. Values above 100 were set to 1. One erosion followed by two dilations eliminated the spurious pixels from the background. The largest contiguous group of ones were kept as the embryo. Erosions and dilations were not done as many times as in the previous method, in order to keep the radical or tail portion of the embryo image attached to the main embryo body. Hole filling was done before the erosion and dilations in order to maintain the radical portion of the embryo image.
[0055] The longitudinal side view of the embryo (camera angle was rotated 90 degrees relative to the top view) was preprocessed by creating a matrix of maximum color values. The maximum color values at a pixel was the largest of the red, green, and blue color values. The maximum color values were used to ensure maximum retention of the embryo radical image. The embryo had a horizontal position in this image. Therefore, the row average was calculated from the maximum color values. The lowest average value between rows 200 and 260 corresponded to the gap between the embryo and the edge of the stage on which it sits. Everything below the row corresponding to the gap was set to zero. The rest of the image was thresholded so that values above ten were set to one. Again the binary image was eroded once and dilated twice to remove spurious pixels. A blob labeling routine labeled the remaining groups of pixels with values of ones and the largest one was kept as the embryo. If a second blob of ones had at least 25% of the number of pixels in it as the largest blob then the radicle was assumed to have been separated by the morphological operations and was included. Hole filling was done and then the binary image was used to zero the background parts of the original image and crop it as in the case of the top view.
[0056] The apical or end view of the embryo was preprocessed by one of two ways. The first method was to use the same method as described for the side view with three changes. After the stage part of the image was set to zero the remaining maximum values were thresholded at 20 instead of 10. The resulting binary image was eroded 3 times and dilated 5 times. Finally, no second largest blob was kept. The second method was to create a binary image from the product of two other binary images. The first binary image was created from the matrix of maximum values by setting all values greater than 20 to one and zero otherwise. The second binary image was made by creating a matrix of hue values as for the top view and then setting the positive values to one and all others to zero. The product of these two binary images eliminates almost all background features. The resulting binary image was eroded and dilated as in the first method. Finally, the binary image was used to zero the background and crop the original image as in the top view.
[0057] The reason the images were cropped was to concentrate later analytical effort on the embryo portion of the images as much as possible and to reduce the demands on computer memory. The three views of an embryo represented three correlated measurements of a single experimental unit. It took hundreds of thousands of numbers to describe the measurements. The embryo only covers about 5% of the total area of an image, so most of an image was background. Carrying along the background information needlessly uses up memory and can hamper later methods used to classify the embryos.
[0000] Image Reduction
[0058] Since embryo image data sets are often large, further image size reduction was performed in order to get the all of the data into computer memory. Also, the embryo classification algorithms that were used to sort the embryos required that all of the images of a particular embryo view be the same size. The sizes of the largest top view, side view and end-on view were found after all the images had been preprocessed and cropped as described in the preceding section. All top views were zero padded out to the size of the largest top view with the cotyledon embryo head placed as close to one of the corners of the image as possible. In other words, the extra zeros were added to the radicle end of the image and to one of the sides. Zero padding for the side and end views was similar. The zero padding scheme was performed in an effort to get all the embryo heads in the same place in the images, while the radical tail portion of the embryo, which is highly variable in size and shape, were left to occupy what ever image space they needed.
[0059] With the images of each embryo view reset to the smallest common size, the images were then shrunk using wavelet computational methods. The first step in reducing the images was to calculate the principal components of the red, green, and blue color matrices pixelwise. Each color matrix was strung out into a single long vector by appending the columns to each other. The first column was at the top of the vector and the last column was at the bottom. The red, green, and blue vectors were formed into a matrix with three columns and the singular value decomposition of this matrix was calculated. The left eigenvectors from the decomposition were principal components with unit length. The first eigenvector corresponded to the principal component that accounted for the most variation in the color values. On average the first principal component (PC) accounted for 95% of the variation. The first PC represents the optimal weighted average of the red, green, and blue values for explaining variation and is similar to a calculated grayscale value. The first eigenvector was then reshaped into a matrix and was used in place of the color array. This step reduced the computer memory requirements by ⅓ by replacing three matrices with a single matrix whose values were similar to a gray scale image. The single matrix carries all of the geometric information of the original. The second step was to do a two level two dimensional wavelet decomposition on the first PC image in order to reduce its size. The approximation coefficient from the second level of the wavelet decomposition are used as the reduced image. The reduced image retains at least 75% of the variability in the original PC image.
[0000] Metrics
[0060] Reducing the image data using the aforementioned methods means that some of the information in the original color data is lost. In an attempt to keep some of this information, several statistics were calculated as the data reduction process was performed. First, the mean standard deviation, coefficient of skewness and coefficient of kurtosis were calculated for each color as well as hue, saturation and intensity. Next, the coefficients of the wavelet decomposition at each scale were summarized by their first five raw moments about zero. In a two level decomposition there are six matrices of detail coefficients and one of smooth coefficients. The detail coefficients contain information on texture. The first five raw moments about zero were estimated for each of these matrices as well as the smooth coefficients. The five moments about zero were the mean, mean squared value, mean cubed value, mean quartic value and mean quintic value. To obtain central moments like the variance, skewness, etc., one subtracts the mean from the individual values first. However, central moments were more similar for classification groups than for raw moments. A third set of statistics were calculated from the perimeter of the embryo and its wavelet decomposition and are intended to quantify shape information.
[0061] The perimeter of the embryo was traced in a clockwise direction and the row and column coordinates of the edge pixels were obtained. The pixel coordinates were interpolated to generate row and column vectors with 1024 elements in each. Because many of the embryo perimeters were concave curves, equiangular interpolation could not be used. Instead, linear interpolation was used to create 1024 equally spaced coordinates. The coordinates were mean centered and then radii were calculated from them. When plotted in sequence the radii formed a lumpy sinusoid. When plotted in polar coordinates they traced the embryo. A ten level wavelet decomposition was performed on the radii and the first seven raw moments about zero were calculated for each level. A similar method has been used by L. M. Bruce (“Centroid Sensitivity of Wavelet-based Shape Features,” Proceedings of SPIE, Wavelet Applications V, Harold H. Szu, Editor, 3391:358-366 (1998)) to classify breast tumors as cancerous or benign.
[0062] In addition to the moments of the wavelet coefficients from the radii, the area enclosed by the perimeter and it's length were calculated from the original coordinates. Also, the area and length of the convex hull of the perimeter were calculated. Lastly, the ratio of the perimeter area to the convex hull area and the ratio of the perimeter length to the convex hull length were calculated. If the embryo perimeter was a convex curve, then the last two ratios will be unity. Otherwise, the area ratio will decrease toward zero and the perimeter ratio will increase.
[0063] In all, 142 metrics were described for the above embryo images. These metrics were intended to capture some of the information on color, shape and texture that is lost when the somatic embryo images are reduced in size. Some of the information such as the perimeter shape information was still in the reduced images. Adding the metrics the classification model emphasizes the metrics information. In some analyses, (see Example 4, Tables 2 and 3) the logarithm of the metric is taken to reduce variability.
[0000] Embryo Classification Models
[0000] Principal Component Analysis/SIMCA
[0064] The primary classification method used in the Examples of the present invention was soft independent modeling of class analogy SIMCA. See Jolliffe, I. T., Principal Component Analysis, Springer-Verlag p. 161 (1986). SIMCA was used on each set of reduced images and metrics. This resulted in six intermediate classification of each embryo. These six intermediate classifications were combined using the Bayes optimal classifier. See Mitchell, Tom M., Machine Learning, WCB/McGraw-Hill pp. 174-176, 197, 222 (1997). SIMCA works by calculating a separate set of principal components for each category based on training data. The principal components which account for the majority of the variation are kept. Then data from a new sample is regressed on the principal components from each group. The residual mean square errors are calculated for each category. The category with the smallest residual mean square error is the category to which the new sample is assigned. Six SIMCAs are done for each embryo.
[0065] Combining the Intermediate Classifications Using the Bayes Optimal Classifier
[0066] Two to six or so intermediate classifications can be combined into a single classification rule by first converting the resulting strings of zeros and ones into a binary code. For two intermediate classifications there are four binary combinations, for three intermediate classifications there are eight binary combinations, and so on. For ‘k’ intermediate classifications there are 2 k binary combinations. Each binary combination is assigned a label or code. For each embryo quality class the probability of observing each code is estimated. Then the embryo-quality-class-by-binary-code probabilities are divided by the probability of the corresponding code occurring in all the data from both embryo quality classes. The resulting probabilities are the conditional probability of an embryo quality class given a code. An embryo's binary code is calculated and the embryo is assigned to the embryo quality class for which the conditional probability is highest for the observed binary code. Ties can be assigned randomly or assigned to one of the embryo quality classes based on other considerations such economics.
[0000] Using the Lorenz Curve for Classifying Embryos
[0067] Originally, the Lorenz curve was developed to compare income distribution among different groups of people. A Lorenz curve is created by plotting the fraction of income versus the fraction of the population that owns that fraction of the income. In the present invention, the Lorenz curve is viewed as a comparison of two paired cumulative distribution functions where the fractional values of one cumulative distribution function are plotted verses the fractional values of the second cumulative distribution function. If the two distributions are the same the Lorenz curve will plot the straight line y=x. The point farthest from the line y=x corresponds to the balance point between accumulating more of one distribution than the other. The balance or extreme point is an objective point at which to separate the two distributions.
[0068] The Lorenz curve classification method of the present invention has four steps. First, Lorenz curves are calculated for each metric in a set of metrics. The points on these Lorenz curves the furthest from the line, y=x, are found. Second, the metric values corresponding to the extreme points on the Lorenz curves are used as the threshold values to make single metric classifications of the embryos: values of a metric less than its threshold are assigned to one embryo quality class and values greater than the threshold are assigned to the other embryo quality class. Third, the set of metrics is subsetted to reduce the number of combinations that must be searched in the final stage. Fourth, pairs, triples, quadruples, etc., of the single metric classifications are combined into binary codes and used in the Bayes optimal classifier to create classification models for assigning embryos to one of two quality classes. Classification models are made for all possible pairs, triples, quadruples, etc., and the best model is retained in each case.
[0069] Calculating the Lorenz Curve for a Single Metric
[0070] The metric values for the two embryo quality classifications are combined and all the distinct metric values identified. Alternatively, the minimum and maximum value of all the metric values for both embryo quality classifications combined are found and a user specified number of equally spaced steps between the minimum and maximum are used. When there are too many distinct values, this second option is useful. In either case, for each distinct metric value, the fraction of metric values less than or equal to the distinct value is recorded for each embryo quality class. Thus, two paired cumulative distribution curves are obtained. Plotting these two sets of fractions against each other constitutes the Lorenz curve. If the two distributions are the same, the Lorenz curve is the line, y=x.
[0071] Finding the Extreme Points on the Lorenz Curves
[0072] The distance of a point, (x 0 ,y 0 ) from the line, y=x, is the absolute value of the difference between y 0 and x 0 divided by the square-root of two: |y o −x 0 |√{square root over (2)}. The absolute value of the difference between the cumulative distribution functions of the two classes of embryo quality for a metric is searched for its highest point. The corresponding metric value is used as the threshold. This extreme point is the balance point between one distribution accumulating more probability than the other distribution. The extreme point was used as the threshold in the metric classification models developed in Example 4. Other points on the Lorenz curve may be used as thresholds based on other considerations such processing costs. If a point other than the extreme point is used as the threshold, the Lorenz curve can be used to determine the tradeoff in miss-classification error rates.
[0073] Single Metric Classifications
[0074] Metric values less than the threshold are assigned to one of the embryo quality classes and values greater than the threshold are assigned to the other quality class. These single metric classifications result in an embryo metric value being assigned a zero or one. This is done for each metric used, one embryo quality class is set to one and the other is set to zero. Several single metric classifications can then be combined to yield a final classification that has a lower misclassification error rate than any of the individual single metric classifications.
[0075] Combining the Lorenz Curve Single Metric Classifications Using the Bayes Optimal Classifier
[0076] Two or more single metric classification models can be combined into a single classification rule using the same Bayes optimal classifier method previously described to combine intermediate SIMCA classification models. Alternatively, single metric classification models or intermediate SIMCA classification models can serve as the input data to neural network algorithm to arrive at a final classification model for plant embryo quality. However, as described below, when single metric classification models are combined to arrive at a final classification rule special problems arise.
[0077] Subsetting the Metrics to be Combined Into a Single Classification Model
[0078] The Lorenz curve can be used to find an optimal threshold value for a single metric. Optimal is here defined in the sense of balancing probability accumulation. However, the Lorenz curve cannot handle the case when several metrics are considered together because the Lorenz curve can only compare two distributions at a time. One solution is to feed sets of metrics into an artificial neural network to find an optimal classification rule. However, with hundreds of metrics, it would be necessary to either fit very large networks or fit a very large number of small networks. For the purpose of this application, the simpler the classification rule the better. It is recognized that the thresholds found for individual metrics may not be the best ones to use when combining several metrics through their single metric classifications. Nevertheless, it is possible to search large numbers of combinations of single metric classifications by calculating the results of the Bayes optimal classifier approach outlined above and comparing them for various combinations of the single metric classifications. Yet there are still limitations on the number of combinations that can be searched. When there are 682 metrics being considered, then there are 8.935 billion distinct four-metric combinations alone. As computers get faster such a number will not pose much of a problem. However, for limited computing hardware, subsetting the metrics will greatly reduce the amount of work.
[0079] Two subsetting criterion present themselves. First, the metrics whose single metric classifications are above some limit can be kept. Second, many of the metrics are correlated with each other. The metrics highly correlated with the better metrics can be dropped from consideration since they are informational twins to the better metrics: a metric perfectly correlated with another contains no information not already in the other metric. Metrics with very low correlations among them are more likely to create useful binary codes. These subsetting criterion can be used together to reduce the number of metrics.
[0080] Several different examples of classification techniques are specifically demonstrated in the Examples 2-4.
EXAMPLE 2
[0081] Somatic Embryo Sorting Based Upon Visual Embryo Quality
[0082] Douglas-fir somatic embryos were cultured to the cotyledon stage by the methods outlined in Gupta et al., U.S. Pat. No. 5,036,007, and Gupta, U.S. Pat. No. 5,563,061, which patents are herein incorporated in their entirety by reference. Embryos were individually removed from the development stage medium. From this point they would normally be manually screened and selected for germination.
[0083] In the present case, two hundred embryos from the same clone of Douglas-fir genotype 5 were preselected by morphology using the usual zygotic embryo criteria of color, axial symmetry, freedom from obvious flaws, and cotyledon development. Half of the sample was considered to be “good” embryos; i.e., embryos that met visual criteria for further processing in germination medium. The other half were “bad” embryos that did not meet the criteria, The “truth criterion” for the following analysis was the presence or absence of normal zygotic-like morphology.
[0084] After selection, the embryos were placed against a dark background and illuminated by cool fiber optic light. Each embryo was individually color-imaged in rapid sequence by three cameras mounted perpendicular to each other. Two longitudinal views 90° to each other and an apical end-on view of the cotyledon region were acquired. Images were acquired as digitized data suitable for computer analysis. Prior to analysis the images were preprocessed to isolate the embryo and thus eliminate interfering background data.
[0085] In this example, a subset of the embryo top view images were used to calculate the principal components. The first 80 components were kept as they account for about 98% of the variation in the images. Principal components were calculated for the “good” embryos, i.e., those embryos that possess good visual criteria that are associated with a high germination rate, as well as for embryos that lack the good visual features. The principal components were calculated using the singular value decomposition algorithm. The singular value decomposition algorithm is available with any software capable of handling matrices. The principal components used were the left eigenvectors from the singular value decomposition which were the principal components normalized to have unit length. This normalization process does not have an adverse effect because the principal components were being used in this method as a set orthogonal basis vectors in a multiple regression. The embryos that were not included in the training data set were then regressed on the two sets of principal components exactly as done in multiple regression. For each regression the residual mean square error was calculated. A test embryo was classified as having either good or bad embryo visual quality depending on which category has the smaller residual mean square error. Using this method test embryos were classified based on the longitudinal top view of an embryo.
[0086] Similar to the longitudinal top view images, the longitudinal side view and end view images were divided into a training set and test set of embryos. The training set of embryos were used for calculating the principal components and the test set of embryos were regressed on them and classified. Likewise, the metrics were used to calculate principal components and classify the embryos in the test set. In the case of the metrics, 40 principal components were kept and they were based on the natural logarithm of the absolute value of the metrics multiplied by the sign of the metric or the Box-Cox transformation (Myers, R. H. and D.C. Montgomery, Response Surface Methodology: Process and Product Optimization Using Designed Experiments, Wiley, pp. 260-264 (1995)) of the metrics using an odd root such as a 1/101 which approximates the natural logarithm, preserves the sign, and still works on zero. The transformation helps reduce the variability of the higher order moments. As a result each embryo in the test set ends up with six classifications from each of the SIMCAs: three classifications from the three images and three classifications from the three sets of metrics.
[0087] The six classifications were combined into a single classification using Bayes optimal classifier as follows. See Mitchell, T. M. Machine Learning, WCB/McGraw-Hill, pp. 174-176, 197, 222 (1997). Each classification was either zero or one: one meaning that the embryo had a good visual quality and zero meaning that the embryo did not have good visual characteristics. These six binary classification scores were converted to a multi-valued code by multiplying the side view image score by 32 and adding it to 16 times the end view image score plus 8 times the top view image score plus 4 times the side view metric score plus 2 times the end view metric score plus the top view metric score. This composite score takes on integer values ranging from 0 to 31. For each composite score, the number of good visual quality embryos were counted as well as the number of bad visual quality embryos. Dividing by the total number of embryos in the test set yields the probabilities of observing each score and one of the embryo categories. The probability of each composite score occurring was calculated by counting how many times each score occurred and dividing by the total number of embryos in the test set. Next, each probability of observing a composite score and one of the categories was divided by the probability of the composite score occurring. This calculation gave the probability of a category given a composite score. Composite scores where the probability of observing a visually correct embryo was greater than or equal to 50% were assigned as having a good embryo quality. All other scores were assigned to the bad embryo quality category. In this way the information from the six SIMCA classifications were combined into a single classification.
[0088] Basically, the Bayes optimal classifier assigns a composite score to the category which generates the most of that particular score. If an embryo has a value that is in the middle it was put into the good embryo quality category. The whole process was repeated many times and the average performance reported.
[0089] Using the above methods two additional sets of somatic embryos of two different genotypes (genotypes 6 and 7 ) were classified as having good or bad morphological qualities as compared to normal zygotic embryos. The results of the three sets are given in Table 1.
TABLE 1 Visual Quality Classification Results From the Bayes Optimal Classifier for Three Genotypes of Douglas-Fir Somatic Embryos Percent of Embryos Percent of Embryos Classified Correctly as Correctly Classified as Having “Good” Visual Having “Bad” Visual Douglas-fir Genotype Embryo Quality Embryo Quality 5 (Three views of 80.0 75.0 200 embryos) 6 (Three views of 88.7 70.5 1000 embryos) 7 (End & Top views 87.0 78.5 of 1000 embryos)
EXAMPLE 3
[0000] Somatic Embryo Sorting Based Upon Visual Embryo Quality and Actual Germination
[0090] A sample of 400 embryos judged to be of high morphological quality, as previously defined, from the Douglas-fir genotype 5 was evaluated in two ways. After evaluation the embryos were germinated to determine whether germination success correlated with predicted success based on eight additional morphological features. The base case was visual selection based on morphology. The first procedure was a nonparametric statistical treatment based on four observed features (symmetry, surface roughness, presence of fused cotyledons, and presence of gaps between cotyledons) and four measured embryo dimensions (hypocotyle length, radical length, cotyledon length, and cotyledon number) the measurements being made on digital color images acquired under sterile conditions from a single viewpoint perpendicular to the long axis of the embryo. This statistical procedure is known as binary recursive classification and was carried out using software named CART™ (for Classification and Regression Tree) (Salford Systems, San Diego, Calif.). Reliability of this classification method was assessed and probabilities for future similar data sets were derived by validating the classification on a specified number; e.g., 20, random subsets of the data. CART™ classification is binary and all possible splits were tested on all variables. The second evaluation method was principal components analysis of the images.
[0091] Results showed principal components analysis was superior to the CART™ statistical procedure and was a major improvement over technician selection. A 66.3% germination rate was found for the base populations (selected for good similarity to normal zygotic embryos). This improved to 75.0% for embryos classified by the CART™ procedure as most likely to germinate. A germination success of 79.7% was achieved in embryos chosen by the principal components/SIMCA analysis method.
EXAMPLE 4
Somatic Embryo Sorting Based Embryo Germination
A Comparison of Classification Methods
[0092] The methods in Examples 1-3 were used to develop classification models and classify 1000 somatic embryos of Douglas-fir genotype 6 by their capability to germinate. Table 2 contains the results of presenting different inputs to the Bayes optimal classifier when classifying the germination versus nongermination capabilities of the Douglas-fir genotype 6 embryos. When the data input was somatic image data that was first preprocessed using the method of Example 1 the training set model for the classification of embryos by germination was accurate 59% of the time at correctly classifying embryos as embryos that would germinate and about 64% accurate at classifying embryos that would not germinate. This is an average accuracy of 61.7%. In contrast, when metrics image data was captured and added to the preprocessed image data following the methods in Example 1, the accuracy of embryo classification into germinating and non-germinating embryos was increased to about 71% (column 4 of Table 2). Thus, as in Example 2, an increased accuracy in classifying potential germinants was achieved using the present invention.
TABLE 2 Germination Classification of Douglas-Fir Genotype 6 Somatic Embryos Using Different Inputs to Bayes Optimal Classifier Compared With Germination Results of Manual Selection Based on Morphology Percent of Percent of Germinating Non-Germinating Average Combinations of Embryos Embryos Success SIMCA Results Used in Correctly Correctly in Bayes Optimal Classified as Classified as Classifying Classifier Germinating Non-Germinating Correctly Images Only 59.3 64.1 61.7 Images + Metrics 67.6 74.6 71.1 Images + Log (Metrics) 68.5 74.1 71.3 Manual Selection Based 71.7 66.2 68.9 on Morphology
[0093] Table 3 presents the germination classification results for Douglas-fir genotype 6 of the individual SIMCA runs from each set of images and metrics of the somatic embryos. Comparing the results presented in Table 3 with those shown in Table 2 demonstrates the statistical advantage of combining the individual SIMCA classifications using the Bayes optimal classifier of each of three different somatic embryo views. Also, the utility of adding the metrics is illustrated.
TABLE 3 Germination Classification of Douglas-Fir Genotype 6 Somatic Embryos: Results From the Individual SIMCA Runs Percent of Percent of Germinating Non-Germinating Embryos Correctly Embryos Correctly Classified Classified Data Used as Germinating as Non-Germinating Top View Images 66 54 Top View Log(Metrics) 46 63 End View Images 70 45 End View Log(Metrics) 52 52 Side View Images 48 59 Side View Log(Metrics) 52 53
Additional Classification Methods
[0094] Two additional classification methods were performed with data collected from somatic embryos: neural networks (Douglas-fir genotype 6 ) and a classification method based on the Lorenz curve (Douglas-fir genotypes 6 and 7 ). The method based on SIMCA uses hyperplanes as boundaries between categories. A two dimensional hyperplane is a line and a three dimension hyperplane is a regular plane or flat surface. In short, hyperplanes are just higher dimensional cousins to lines and regular planes. As a result they are best for separating categories that are linearly separable, i.e., they have straight boundaries and can be separated by a “line”. Often nature does not have linear boundaries but very curved boundaries. Simple back-propagation neural networks using nonlinear transfer functions for the hidden nodes and output nodes can handle very nonlinear boundaries between categories. See Hagan, M. T., H. B. Demuth, and M. Beale, Neural Network Design, PWS Publishing Company, Chapters 11 and 12 (1996). These have been used to discriminate between images of people looking in different directions. Id. pp. 112-115.
[0000] Neural Network
[0095] Back-propagation neural networks were used to classify embryos of genotype 6 as germinating or non-germinating. The end view and top view somatic embryo images were reduced in size by wavelets in order to reduce the number of network input nodes as was suggested by T. M. Mitchell ( Machine Learning, WCB/McGraw-Hill, pp. 112-115 (1997)). Mitchell used adjacent averages to reduce his images. Here the smooth coefficients from the 3 rd level of the two-dimensional wavelet decomposition were used since they preserve much more detail than averages. The embryo side view was not included to reduce the amount of computation and because as shown in Table 3 this view carries the least amount of information about germination of three views. The input layer of the network just fed in the pixel values from the reduced images from both views. The hidden layer had either 18 or 80 hidden nodes using the logistic transfer function, 1/(1+exp(−x)). The output layer had two nodes again using logistic functions. The output target values were (0.9, 0.1) for germinating somatic embryos and (0.1, 0.9) for non-germinating embryos. The sum of the squared differences between the target vectors and their predicted vectors were minimized. Half the data was used for training and half was used for validation. Any training set and even all of the embryos could be perfectly classified with the 18 hidden node model. The best either of the neural network models could do on a validation or test set was 61% correct classification of embryos into both the germinating and non-germinating classes.
[0000] Use of the Lorenz Curve Classification Method to Classify Embryos
[0096] As previously noted the Lorenz curve classification method has four steps. In this example, 625 and 457 different metrics were calculated for Douglas-fir genotypes 6 and 7 , respectively. Metric values corresponding to the extreme points on the Lorenz curves for each metric were set as threshold values for classifying embryo quality. In addition, the set of single metric classifications which were searched for robust combination classification models was reduced using the subsetting routine described in Example 1. Lastly, double, triple, quadruple, etc., combinations of the single metric classification models were combined into binary codes and used in the Bayes optimal classifier to create classification rules for assigning embryos to one of the two embryo quality classes. Classification models were made for all possible pairs, triples, and quadruples and the best model was retained in each case.
[0097] Table 4 contains the results of classifying embryos according to their morphological similarity to normal zygotic embryos by using the Lorenz Curve classification method combining 1, 2, 3, and 4 single metric classifications via the Bayes optimal classifier.
TABLE 4 Morphology Classification Results From the Best Bayes Optimal Classifier Combining 1, 2, 3 & 4 Lorenz Curve Single Metric Classifications for Douglas-Fir Genotypes 6 and 7 Percent of Good Percent of Bad Morphology Morphology Number of Metrics Embryos Correctly Embryos Correctly Used to Create Classified as Having Classified as Having Douglas-fir Genotype Classification Model Good Morphology Bad Morphology 6 1 82.30 70.44 (end, side & top views) (Skewness coefficient, β 1 , of all the intensity pixel values from the embryo end view) 6 2 72.63 83.27 (end, side & top views) (Skewness coefficient, β 1 , of all the intensity pixel values from the embryo end view, and Range of the perimeter radii from the embryo end view) 6 3 79.69 78.96 (end, side & top views) (Skewness coefficient, β 1 , of all the intensity pixel values from the embryo end view, range of the perimeter radii from the end view, and standard deviation of the area of the cotyledons from the embryo end view) 6 4 84.72 75.75 (end, side & top views) (Skewness coefficient, β 1 , of all the intensity pixel values from the embryo end view, range of the perimeter radii from the end view, standard deviation of the area of the cotyledons from the embryo end view, and mean area of the cotyledons touching the bounding convex hull of the embryo end view) 7 1 88.59 71.61 (end & top views only) (Lower quartile of the perimeter radii from the embryo top view) 7 2 71.33 89.74 (end & top views only) (Lower quartile of the perimeter radii from the embryo top view and skewness coefficient, β 1 , of the blue pixel values from the embryo end view) 7 3 85.71 84.97 (end & top views only) (Skewness coefficient, β 1 , of all the blue pixel values from the end view, standard deviation of all the green pixel values from the end view, and 4 th moment about zero of the detail coefficients of the 8 th level of a 10 level wavelet decomposition of the embryo end view perimeter) 7 4 85.10 87.05 (end & top views only) (Skewness coefficient, β 1 , of all the blue pixel values from the end view, standard deviation of all the green pixel values from the end view, 4 th moment about zero of the detail coefficients of the 8 th level of the wavelet decomposition of the end view perimeter, and lower quartile of the perimeter radii from the embryo top view)
[0098] Comparing the results in Table 4 with the corresponding results in Table 1 from combining 6 SIMCA intermediate classifications by the Bayes optimal classifier suggests that the Lorenz curve based method performs as well as or better than the SIMCA based method for classifying embryos according to morphology. Similarly, Table 5 contains the results from classifying embryos according to germination classes by the Lorenz curve method. Comparing Table 5 with Table 2 shows that the Lorenz curve method does not perform as well as the SIMCA based method. Also, Table 4 and Table 5 show that combining the information in multiple metrics reduces the misclassification error rate.
TABLE 5 Germination Classification Results From the Best Bayes Optimal Classifier Combining 1, 2, 3 & 4 Lorenz Curve Single Metric Classifications for Douglas-Fir Genotype 6 Douglas- Percent of fir Germinating Percent of Genotype Embryos NonGerminating using (end, Number of Metrics Correctly Embryos Correctly side & top Used to Create Classified as Classified as views) Classification Model Germinating NonGerminating 6 1 70.51 60.12 (Skewness coefficient, β 1 , of all the blue pixel values from the embryo end view) 6 2 66.51 65.45 (Skewness coefficient, β 1 , of all the blue pixel values from the embryo end view, and 10 th level detail coefficient from a 10 level wavelet decomposition of the embryo side view perimeter) 6 3 71.56 62.40 (Skewness coefficient, β 1 , of all the blue pixel values from the embryo end view, kurtosis coefficient, β 2 , the perimeter radii from the embryo top view, and mean of the level 9 detail coefficients from a 10 level wavelet decomposition from the embryo side view perimeter) 6 4 65.33 70.70 (Skewness coefficient, β 1 , of all the blue pixel values from the embryo end view, kurtosis coefficient, β 2 , the perimeter radii from the embryo top view, mean of the level 9 detail coefficients from a 10 level wavelet decomposition from the embryo side view perimeter, and kurtosis coefficient, β 2 , of all the green pixel values from the embryo side view)
Classification Trees Based on the Lorenz Curve
[0099] An alternative method for classifying embryos uses Lorenz curve as the method for splitting nodes in classification trees. Usually to construct a classification tree the metrics are searched to find a variable that separates the quality classes the most based on a measure of distance or spread. Multivariate statistics can also be used to examine sets of metrics, however, the computation required increases rapidly with the number of metrics in a set. The Lorenz curve method outlined above can also be used as a node splitting criterion. The Lorenz curve method outlined above was used to search for a single best metric to split the embryo quality classes. The two subsets thus created were each submitted to the Lorenz method to find a metric that best split them. This process can be repeated as long as the number of metric values from each embryo quality class are large enough to provide a good estimate of the distribution functions. The entire set of metrics is searched each time because the act of splitting the distributions, alters the distributions, and metrics that at first provided poor separation may provide good separation at later stages. This method of method of creating a classification tree is very computationally intensive. As a result the metrics can be subsetted in order to get the computations done in a reduced time. A two level classification tree based on the Lorenz curve was created for Douglas-fir genotype 7 . The results are in Table 6.
TABLE 6 Morphology Classification Results From a Two Level Classification and Regression Tree Using Lorenz Curves to Split Nodes for Douglas-Fir Genotype 7 Percent of Good Percent of Bad Douglas-fir Morphology Embryos Morphology Embryos Genotype 7 using Number of Metrics Correctly Classified Correctly Classified (end & top views Used to Create as Having Good as Having Bad only) Classification Model Morphology Morphology 2 81.22 82.25 (Standard deviation of all the red pixel values from the embryo end view, and 2 nd moment about zero of all the pixel values in the 1 st principal component image (the view created by collapsing the red, green, and blue color matrices into a single matrix using principal components) of the end view)
[0100] The techniques described in Examples 1-4 can be readily adapted to continuous examination of somatic embryos as might be required in a large scale production facility. In addition, these methods can be combined in series with themselves or with the spectroscopy methods described in Example 5 to create an efficient and cost effective screening methodology for classifying somatic embryos by their germination potential.
EXAMPLE 5
[0000] Spectrophotometric and Multivariate Methods for Classifying Somatic Embryos
[0101] Spectral data was collected and analyzed from zygotic and somatic embryos populations that from experience are known to differ considerably in germination vigor.
[0000] Zygotic Embryos
[0102] Fresh zygotic embryos were collected at two intervals about three weeks apart from one orchard grown Douglas-fir tree ( Pseudotsuga menziesii ). The degree of embryo development corresponded to Stages 7 and 8 a in the classification published by Pullman et al. (Pullman, G. S. and D. T. Webb, “An Embryo Staging System for Comparison of Zygotic and Somatic Embryo Development,” Proc. TAPPI [Technical Association of the Pulp and Paper Industry] Biological Sciences Symposium, Minneapolis, Minn., Oct 3-6, 1994, pp. 31-33. TAPPI Press, Atlanta, Ga. (1994)) for the July 23 and August 13 collections, respectively. These stages may be described as “just cotyledonary” and “cotyledonary, immature.” In addition, fully mature zygotic embryos were obtained from mature seed obtained from a seed store collected from a mix of different trees grown in the same orchard. Immature loblolly pine ( Pinus taeda ) zygotic embryos were collected from one tree on August 10, at which date they were at Stage 7 in Pullman et al.'s classification system cited above. Mature loblolly pine seed embryos were obtained from freezer storage, and the decoated seed allowed to imbibe water for 14 hours before extraction of the embryos for analysis. Cones and seed were stored at 4-6° C. after collection until spectral analysis was performed.
[0000] Somatic Embryos
[0103] Douglas-fir somatic embryos of four different genotypes, designated 1, 2, 3, and 4, were analyzed in this study. The Douglas-fir somatic embryos were cultured as described in Example 2. Where a cold treatment is noted, the Douglas-fir somatic embryos received cold treatment at 4-6° C. for four weeks prior to spectral analysis. Two genotypes of loblolly pine somatic embryos were used in the study, designated genotypes 5 and 7 . After completing their development to the cotyledonary embryo stage on petri plates, half of the somatic loblolly pine embryos from each genotype received a partial drying treatment for 10 days at about 97% relative humidity while still on the culture medium, followed by cold treatment at 4-6° C. for four weeks. The other half of the loblolly somatic embryos did not receive this treatment. The loblolly somatic embryos were produced using standard somatic embryo plating methods described in Gupta et al., U.S. Pat. No. 5,036,007 and Gupta, U.S. Pat. No. 5,563,061.
[0104] For each population, spectral analysis was performed on about 10 embryos except for some somatic embryos where spectral data was collected from about 15-40 embryos . Spectra were taken usually from the cotyledon region of an embryo ( FIG. 1 ). However, it should be understood that the inventive method can be practiced by collecting spectral data from the entire embryo or from the hypocotyl ( 12 ) or radical ( 14 ) portions of the embryo as diagrammed in FIG. 1 . In some instances the classification was improved by using both cotyledon ( 10 ) and radical ( 14 ) data in sequence.
[0000] Collection of Spectral Data
[0105] The experimental setup consisted of a light source, a binocular microscope, a NIR sensor, and a portable NIR processor with computer. A FieldSpec FR (350-2500 nm) Spectrometer (Analytical Spectral Devices, Inc., Boulder, Colo.) equipped with a fiber optic probe which gathers light reflected from any surface was used to collect embryo spectral data. The fiber optic probe of the spectrometer was fitted with a 5 degree fore-optic and inserted into the auxiliary observation (camera) port of a binocular microscope.
[0106] Spectra were acquired sequentially from groups of ten somatic embryos immediately after hand-transferring from a culture plate, and from zygotic embryos on a one-by-one basis immediately after excision from decoated seeds using the apparatus and procedures described below. The halogen lamp was set at 40 degree angle from the vertical at a distance of 17 cm from the embryos. Samples were placed on a white Teflon surface to minimize background absorption while being viewed with the 6.5×, 10×, or 40× microscope objective. A “white balance” program that is part of the spectrometer, was run periodically throughout the measurements to recalibrate the instrument against the white background when no embryos were present.
[0107] Spectra were measured in the region from visible to very near IR range (350 to 2500 nm). Spectral intensities were measured at 1 nm increments. The spectrometer was programmed to complete 30 spectral scans of each embryo in order to obtain a representative average spectrum—a process which took a total of 30 seconds per embryo for separate cotyledon and radical sampling, including the time to reposition for the next embryo.
[0000] Data Processing and Information Extraction
[0108] Analysis of spectral data was performed using a Principal Component Analysis software package (“The Unscrambler” by Camo ASA, Oslo, Norway). The scores and loadings matrices were converted to the “scoreplots” and “loadings spectra” shown in the figures. The principal component analysis algorithm extracted the best set of axes that described the data set. The scoreplots show the relationships among the embryos, and embryo classes, while the loadings spectra show which spectral features were responsible for the class distinctions.
[0000] Principal Component Analysis of Spectra from Zygotic and Somatic Embryos
[0109] A comparison of Douglas-fir zygotic embryos of three different developmental stages and somatic embryos from Genotype 1 was performed. The three zygotic stages consisted of two immature cotyledonary stages, identifiable as stages 7 and 8 in Pullman et al. (Pullman, G. S. and D. T. Webb, “An Embryo Staging System for Comparison of Zygotic and Somatic Embryo Development,” Proc. TAPPI [Technical Association of the Pulp and Paper Industry] Biological Sciences Symposium, Minneapolis, Minn., Oct. 3-6, 1994, pp. 31-33. TAPPI Press, Atlanta, Ga. (1994)) collected from the field in Rochester, Wash., on July 23 and August 14, respectively, and mature dry seed from a seedstore. Previous data showed that whereas 90-95% of the mature-seed embryos would germinate normally in vitro, only about 75% and 43% of the stage 8 and stage 7 embryos respectively would so germinate. The rates of shoot and root elongation—measures of germination vigor—had even greater sensitivity to developmental stage, these rates being reduced to 80% and 20% for the two immature stages. Germination was reduced to about 15% and zero, respectively, for the two immature stages after desiccation of the embryos to 10% moisture content. These data exemplify, for Douglas-fir, the large contrast in embryo quality between embryos at these stages of development, which is well-known to those skilled in plant embryo development. In further contrast, quality of the somatic embryos, which were closest, but not truly equivalent to, zygotic developmental stage 8 , was characterized by significantly lower germination normalcy and vigor than the stage 7 zygotic embryos. The genotype tested was representative of many somatic embryo genotypes.
[0110] Inspection of the scoreplot in FIG. 2A shows that these four populations of contrasting embryo quality separate into four clearly distinct groups when plotted with respect to the first three principal components. The embryo groups are: mature dry zygotics (black circles), August 14 zygotics (inverted white triangles), July 23 zygotics (black squares) and genotype 1 somatics (“+” symbol). The centroid of the somatic embryo group was shifted 8-10 standard deviations to the right along the PC 1 axis compared with all stages of zygotic embryos, which were separated primarily along the axes for PCs 2 and 3 . Variability within the somatic embryos was much greater than within any of the zygotic embryo groups.
[0111] The loadings spectrum for PC1 ( FIG. 2B , curve 20 ) contained mainly two peaks, at 1450 and 1920 nm, attributable to water, indicating that the large separation and variability was due to a greater amount and variability of somatic embryo water. In contrast, separation among the zygotic groups was mainly along PCs 2 (curve 22 ) and 3 (curve 24 ), whose loadings spectra suggest a basis in greater lipid content (the double peak at 1720-1750 nm, and the peak at 2300 nm) for more mature embryos. Also, there are negative peaks around 1400 and 1900 nm that may have to do with hydrogen-bonded water. The somatic embryos were also separated from the two more mature zygotic groups along the PC 2 axis, due in part to their putative lower lipid concentration, as well as absorption differences in the visible region. The percent of total spectral variation accounted for by each PC was 84% for PC 1 , 8% for PC 2 , and 4% for PC 3 . Table 7 summarizes the quality of separation obtained among the four embryo groups after principal component analyses of the spectral data. The summary data tables for the various somatic embryo classifications list the chemical features that are inferred to be associated with specific wavelengths based upon the known spectrophotometric behavior of that chemical class.
TABLE 7 Douglas-Fir Zygotic Embryos at Three Developmental Stages Compared With One Another, and With Somatic Embryos Immature Zygotic Embryos Principal Wavelength/Inferred Stage 7 Stage 8 Mature Seed Somatic Components Chemical Features embryos embryos Embryos Embryos Needed Involved 15/15* 14/14* 8/9* 9/10* 1st Water (1450 nm + 1920 nm) (100%) (100%) (89%) (90%) 2nd Lipid (1700-1750 nm) 3rd Lipid + feature at 1890 nm Lipid (2300 nm) + feature at 1870 nm *Number correctly classified/number tested
[0112] The results with loblolly pine somatic and zygotic embryos are shown in FIG. 3A and Table 8. In this case, stage 8 zygotic embryos (black squares) and water-imbibed mature zygotic embryos (black triangles) are compared with two genotypes of somatic embryos (genotype 5 denoted as “+” and genotype 7 denoted as “o”) pretreated by partial drying then cold. Somatic embryos were separated from zygotic embryos mainly by PC 1 , which, as in case of Douglas-fir embryos, was probably due to the somatic embryos' higher water content relative to lipids (curve 26 ). Also, many loblolly pine somatic embryos were separated from zygotic embryos along PC 2 , which featured a dominant broad peak around 1800 nm of unknown source (curve 28 ). PC 3 further distinguished the mature imbibed zygotic embryo group from the somatic embryo group, based on a combination of features, including a lipid (−ve) peak, pigmentation in the visible region, and a small −ve peak around 1210 nm (which is about where the second overtone of C—H stretches in protein lie) shown in curve 30 . Together, these three PCs accounted for 97% of variation in the spectra ( FIG. 3B ). The percent of total spectral variation accounted for by each PC was 92% for PC 1 (curve 26 ), 4% for PC 2 (curve 28 ), and 1% for PC 3 (curve 30 ).
TABLE 8 Loblolly Pine Zygotic Embryos at Two Developmental Stages and Loblolly Pine Somatic Embryos Mature Immature (stage 8) Zygotic Principal Zygotic Embryos Embryos Somatic Components Wavelength/Inferred Chemical (Aug. 10) (October) Embryos Needed Features Involved 10/10* 13/13* 28/29* 1st Water (1450 + 1920 nm) (100%) (100%) (97%) 2nd Lipid (1700-1750 nm) 3rd 1800 nm broad peak Lipid (−ve 2300 nm) Protein (1210 nm) Lipid (1700-1750 nm) Pigments (400-500 nm) *Number correctly classified/number tested
[0113] Taken together, these data demonstrate that embryos can be accurately separated by their NIR spectral characteristics into groups of differing germination potential.
[0000] Principal Component Analysis of Spectra From Somatic Embryos of High- and Low-Quality Appearance
[0114] Ten cotyledonary-stage somatic embryos of high- and low-quality appearance were selected from a single plate each of Douglas-fir (genotype 2 ) and loblolly pine (genotype 5 ) embryos, based upon traditional morphological indications of embryo quality, i.e., morphologies that are most likely to result in a high or low frequency of germination.
[0115] A summary of the separation obtained is presented in Table 9. For Douglas-fir, it was possible to draw a straight line on the scoreplot of PC 3 versus PC 1 that completely separated the high quality (“+”) and low quality (black circles) groups ( FIG. 4A ). Most of this separation occurred along the third PC ( FIG. 4B , curve 32 ), which represented about 2% of the overall variation. PC 3 was distinguished in part by absorption bands from pigments in the visible region, including chlorophyll. PC 1 (curve 34 ) represented about 96% of the total spectral variation.
TABLE 9 Cotyledon Stage Somatic Embryos With “High” vs. “Low” Quality Morphology High Quality Low Quality PC's Wavelength/Inferred Morphology Morphology Needed Chemical Features Douglas-Fir 10/10* 9/9* 1 Water (1450, 1920 nm) (100%) (100%) 3 Pigments in visible region shoulder feature (1850-1920 nm) Loblolly Pine 9/10* 9/10* 1 Water (1450, 1920 nm) (90%) (90%) 3 Unknown (1400-1500 nm) Lipid (1710, 2300 nm) Bound water (1870 nm) *Number correctly classified/number tested
[0116] FIG. 5A shows the scoreplot obtained from loblolly pine somatic embryos having high quality morphology (“+”) as compared to embryos having low quality morphology (black circles). Almost complete (90%) separation was achieved, with the first and third PCs combined. In the PC 3 loadings spectrum ( FIG. 5B , curve 40 ), there was a strong, slightly bimodal negative peak around 1450 nm (not water), plus putative lipid (1700 and 2300 nm) and bound water (1870 nm) features, as well as absorption peaks in the visible region (380-600 nm). PC 3 accounted for about 1% of the total spectral variation. PC 1 (curve 36 ) represented about 95% of the total spectral variation and was mostly water. PCs 1 and 2 combined also provided good separation, the PC 2 loadings spectrum (curve 39 ) being dominated by the shoulder feature between 1760 and 1900 nm. PC 2 accounted for about 3% of the total spectral variation. These results demonstrate that principal component analysis of spectral data from somatic embryos having high- and low-quality morphological appearance provides a basis for developing a classification model that will allow somatic embryos to be rapidly categorized with regards to their germination potential.
[0000] Principal Component Analysis of Spectra from Somatic Embryos in the Cotyledon (stage 8 ) and “Dome” (stage 5 ) or “Just Cotyledon” (JC) (stage 6 ) Stages
[0117] Douglas-fir somatic embryos in two distinct developmental stages were selected from plates of genotype 3 . Somatic embryos in the cotyledon stage are known to have a much higher frequency of germination than somatic embryos that are in the less mature “dome” or “just cotyledonary” (JC) developmental stages.
[0118] Dome/JC embryos (black circles in FIG. 6A ) and cotyledonary (stage 8 ) embryos (“+”) that were plucked from the same plate formed two distinct groups on a 3D scoreplot formed from PCs 1 - 3 , such that only one embryo of the 19 just fell within the wrong group ( FIG. 6A ). The strongest contributors to separation were PCs 1 (curve 42 ) and 2 (curve 44 ), which are associated with (1) water and (2) lipid, possibly protein N—H, regions, plus the 1800 nm ‘shoulder’ feature, respectively ( FIG. 6B ). PCs 1 and 2 account for 82% and 9% of the total spectral variation, respectively, whereas PC 3 (curve 46 ) accounted for 4% of the total spectral variation. Table 10 presents a summary of the accuracy of the spectral separations obtained using the cotyledon stage and “dome” or “just cotyledonary” stage somatic embryos.
TABLE 10 Cotyledon vs. Earlier Developmental Stages of Douglas-Fir Somatic Embryos From Genotype 3 “Dome” or “Just PC's Wavelength/Inferred Cotyledon Stage Cotyledon” Stage Needed Chemical Features 10/10* 8/9* 1 Water (100%) (89%) 2 Lipid (1700-1800 nm) Unknown (1420 nm) *Number correctly classified/number tested
[0119] These results demonstrate that NIR spectral data can accurately distinguish between early developmental stages of somatic embryos, which are germination-incompetent, and the final stage of development on petri plates (approximately equivalent to zygotic stage 8 embryos), many of which are capable of germinating and producing seedlings.
[0000] Principal Component Analysis of Spectra from Cold-treated and Control Somatic Embryos
[0120] Subjecting embryos to a 4-7° C. cold treatment on low-osmolality media in the dark for 1-5 weeks may increase the frequency of subsequent embryo germination by 20 to 200%.
[0121] Principal component analysis of spectral data collected from cold-treated and control Douglas-fir somatic embryos of two genotypes ( 3 and 4 ) are presented in FIGS. 7A and 7B . In FIG. 7A solid black circles or triangles identify cold-treated embryos for genotypes 3 and 4 , respectively, and the corresponding open symbols identify non-cold-treated embryos of the same two genotypes. For each genotype, a straight line can be drawn that will largely separate the two populations with the degree of success (from 79-100%) shown in Table 11. The separation was determined mainly by the PC 2 axis, whose loadings spectrum ( FIG. 7B , curve 50 ) has both lipid and pigment components and accounts for about 4% of the total spectral variation. PC 1 (curve 48 ) accounts for about 91% of the spectral variation.
TABLE 11 Somatic Embryos That Have or Have Not Received Cold Treatment Specific Species and PC's Wavelength/Inferred Genotype Control Cold-treated Needed Chemical Features Douglas-Fir Genotype 3 9/10* 10/10* 2 Lipids (1700-1750 nm) (90%) (100%) Shoulder region (1800-1900 nm) Genotype 4 26/33* 9/10* 1 Water (79%) (90%) Loblolly Pine Genotype 5 19/20* 10/10* 1 Water (95%) (100%) Genotype 7 28/40* 17/20* 3 Lipid (1700-1750 nm) (70%) (85%) 2 Shoulder region (1800-1900 nm) *Number correctly classified/number tested
[0122] The results of principal component analysis for the equivalent contrast using loblolly pine somatic embryos appears in FIGS. 8A and 8B . Loblolly pine somatic embryos from genotype 5 (circles) exhibit a clear separation of cold-treated (solid circles) and control groups (open circles) in ( FIG. 8A ). Loblolly pine genotype 7 (triangles) exhibits a similar tendency in regard to these two treatment groups. In general, embryos that were partially dried then cold-treated show higher, and greater variation in, water contents than those that were not. The separations, for each genotype, were by PCs 1 and 2 combined, which incorporate the water, lipid and 1800-1900 nm shoulder features noted for Douglas-fir. PC 1 (curve 52 ) and PC 2 (curve 54 ) account for 92% and 4% of the total spectral variation, respectively.
[0123] These results demonstrate that NIR spectral data can distinguish between developmentally similar (approx. stage 8 ) somatic embryos having higher germination potential (on account of prior cold or cold and partial drying treatment) from those embryos of lower germination potential (having not received such treatments).
[0124] While the preferred embodiment of the invention has been illustrated and described, it will be appreciated that various changes can be made therein without departing from the spirit and scope of the invention.
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The present invention is directed towards methods for the classification of plant embryos by the application of one or more classification algorithms to analyze digitized images and absorption, transmittance, or reflectance spectra. The methods are generally applicable and emphasize the importance of acquiring and using as much image and absorption, transmittance, or reflectance spectral information as possible, based on objective criteria. The present invention allows automated selection of embryos most suitable for further culture and rejection of those seen as less suitable.
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BACKGROUND OF THE INVENTION
The invention relates to a connectable pneumatic apparatus comprising a body having:
a first face intended for its fixation on a support,
a second face parallel to and opposed to the first intended to receive a removable pneumatic fluid switching apparatus,
a third and a fourth face, parallel to each other and perpendicular to the first face, these third and fourth faces each respectively presenting a first and a second orifice for the passage of fluid under pressure, and respectively a first and a second orifice for passage of fluid to exhaust,
coupling means disposed in the vicinity of the said third and fourth faces to ensure the connection of two adjacent bases, these means comprising on the one hand some stop surfaces and on the other hand some headed screws each having a threaded portion and the axes of which are inclined with respect to the first face in such a manner that, when the heads bear on inclined bearing surfaces integral with a first base and the threaded portions are engaged in tapped holes in a second base adjacent to the first, the third and fourth faces respectively of the first base and of the second base are applied one against the other to form a fluid-tight coupling of the first, second, third and fourth orifices respectively belonging to these bases,
this base comprising finally orifices for distribution of fluid and orifices for the arrival of signals for control of a switching member.
Such bases are particularly utilised in systems for automation by pneumatic means where the property of association that they present permits the erection of rows of apparatus having a clear constitution for the builder, the user, and the repair worker.
PRIOR ART
The known bases corresponding to the form mentioned hereinabove have inconveniences which particularly arise from the fact that the coupling means are disposed externally on relatively narrow faces themselves carrying means for pneumatic connection, the access to which becomes very awkward for this reason, and to which it is difficult to impart a lateral orientation: furthermore, the tightening screws, which must be introduced or removed by a lateral movement, necessitate a large spacing between two rows of associated bases, and can become lost; finally, the presence of stop surfaces which are carried by extensions largely extending beyond the associated faces necessitate the carrying out of a large separation for either the disengagement of a base, or the separation of adjacent bases, to which it is necessary to resort for substituting or introducing a new pneumatic apparatus after the initial construction.
OBJECT OF THE INVENTION
The invention proposes to provide a simple and effective connecting device which is exempt from the inconveniences referred to hereinabove, and the use of which will provide a gain of space and a gain of time for construction.
SUMMARY OF THE INVENTION
According to the invention, this result is obtained by reason of the fact that the threaded holes which receive a threaded portion of the screw, are each carried by a member pivoting about an axis parallel to the first face and to the fourth face,
that a first housing of the body opening on this fourth face and on this second face contains a portion of said member having the threaded hole,
that the portion of the screw which is not engaged into the threaded hole becomes situated in this housing in a first position representing its rest position,
that a second housing of the body, opening on this third face and on this second face, has two portions of different widths coupled one to the other by a bearing surface which constitutes the said inclined portion, on which bears the head of the screw when the latter is placed in a second position which is inclined with respect to the first position and which represents its working position,
that the planes in which the screws pivot are comprised between the two planes respectively containing the fifth and sixth faces,
and that the said stop surfaces are comprised between the said planes.
BRIEF DESCRIPTION OF THE DRAWINGS
Further advantages and features of the invention will appear better from reading of the following description, which is accompanied by the drawings, wherein:
FIG. 1 shows an apparatus in accordance with the invention seen in perspective from a first side;
FIG. 2 illustrates in perspective an apparatus similar to that of FIG. 1, seen from a second side;
FIG. 3 shows in elevation a longitudinal section of two apparatuses taken on a plane passing through the coupling means;
FIG. 4 shows a view from above in partial transverse section on a plane passing through the pivoting axes of the coupling means;
FIGS. 5 and 6 show an apparatus in side view respectively when mounted on a conventional profile, and when de-mounted therefrom.
DESCRIPTION OF THE PREFERRED EMBODIMENT
A pneumatic apparatus the body of which is constituted by way of non-limiting example by the assembly of two bodies 1 and 2 is shown in FIGS. 1 and 2, and is intended to be associated to other pneumatic apparatuses having an anologous or identical configuration.
In the example of construction illustrated, the half-body 1 is a base intended to be fixed by a first face 3 on a support not shown in this figure.
This base comprises a second face 4 parallel and opposed to the first, a third face 5 and a fourth face 6 parallel to each other, and perpendicular to the first face, as well as a fifth face 7 and a sixth face 8 which are opposed.
Channels such as 9, 10 and 11 pass partially or wholly through the base, and enter therein by first orifices such as 12 and 13 which open on the face 5 and for ensuring for example the circulation of a fluid under pressure, and the circulation of an exhausting fluid to second orifices 14, 15 opening at the face 6. If the half-body 1 of the base does not contain itself any member to ensure a break, a switching or an orientation of fluid, a distributor member 16 can be placed for this purpose in the half-body 2 which is secured in removable manner on the face 4 by means of screws such as are shown at 17, which engage into threaded holes such as 18, of the face 4.
In this case, orifices (not shown) open at the face 4 to communicate with orifices (not shown) placed opposite to the face 19 of the half-body 2 to provide couplings to the distribution member. Further, this half-body 2 can comprise an external control member such as 20 intended to cause a change of state of the distributor member.
As shown in FIG. 2, where there is shown an apparatus analogous to or identical with the preceding one formed by half-bodies 51, 52, the face 7 comprises connectors 21 and 22 which are most often orientatable, which couple the base by flexible tubes such as 23, 24, either to generators of pneumatic control signals adapted to cause a change of state of the distributing member, or coupling the base respectively to utilising apparatuses such as jacks.
The face 8 can likewise comprise such connectors, and in this case, the choice would be made to preferably place the connectors having analogous functions on a same face. In all cases, the putting to use of the properties of orientation of these connectors and the access for the tightening tools used for fixing them, necessitate that the faces 7, 8 shall be as free as possible of any protruberance.
The connection of the apparatuses between themselves is achieved when the third face of a particular base is applied against the fourth fae of a base placed upstream, or that the fourth face of this particular base is applied against the third face of a base place downstream, and that in all cases, the orifices carried by these opposed and associated faces are placed opposite one another in a fluid-tight manner.
For this purpose of association, tightening means are disposed in the region of the faces, as can generally be seen in FIGS. 1 and 2, and in particular in FIG. 3.
It will be seen in FIG. 1 that two housings 25, 26 open at the third face and at the second face, and that two housings 27, 28; open on the fourth and on the second face.
These housings are centered about two planes PP' and QQ' which are parallel to each other, perpendicular to the first face and are in their turn placed between the parallel planes RR' and SS' passing through the fifth face 7 and sixth face 8 respectively, as can be seen in FIG. 4.
The housings 25, 26 and 27, 28 each comprise two successive portions 29, 30 and 31, 32 respectively and 33, 34 and 35, 36 respectively with substantially parallel walls, these two portions being of different widths d 1 and d 2 , and being coupled one to the other by transverse bearing surfaces such as those shown respectively at 37, 38, 39 in FIG. 4, these surfaces visible also in FIGS. 1 and 2 not having any reference numerals but being darkened for clarity of the drawing.
In the vicinity of a base 40 of a housing such as 25 visible in FIG. 1 and adjacent to the first face 3 there is formed a cylindrical opening 42 the axis XX' of which is perpendicular to the plane P, and which opens at the fifth face 7; this cylindrical opening likewise opens in this housing 25 in such a manner that a cylindrical pivot 43, placed in this opening and comprising a zone provided with a radial threaded hole 44, presents this latter in the said housing.
A screw 45 comprising a threaded portion 46, a shank 47 and a head 48 is engaged in the threaded hole and can pivot in this housing about the axis XX', whilst preventing axial movements of the member 43.
This screw can in particular assume, in the housing 25 of a base 51, a first position I called the rest position, in which its head will bear, by screwing up of the screw, on the bearing surface 37, by reason of the fact that the portions 29 and 39 of the housing are respectively less than and greater than the diameter of the head.
The housing 26 has an identical configuration, whilst the housings 27, 28 terminating at the fourth face 6 each have a comparable appearance to that which has been described, that is to say with the presence of the two successive portions 33, 34 of different widths which are joined one to the other by a respective bearing surface 38 and 39. For these latter housings, the bearing surfaces are nevertheless inclined with respect to the first face, as can be seen in particular in FIG. 3.
The third and fourth faces 55, 56 of a second base 41 analogous to the base 51 comprises, in the region of the bottoms 57, 58 of the first and second housings such as 60 and 61 respectively, stop surfaces carried by two studs 62, 53 protruding slightly from these faces, and respectively by two cylindrical openings 64, 65 of the same diameter as the studs. A stud and an opening placed in the vicinity of the two opposed housings situated in a same plane are concentric with a same axis YY', which passes between the face 3 and each housing bottom 57, 58.
When two bases 51 and 41 are associated by their third and fourth faces, as shown in FIG. 3, a housing 27 of the base 51 placed upstream comes opposite to a housing 60 of the base 41 placed downstream when a stud 62 of the latter enters the cylindrical opening 63 of 51.
If the screw 53 of the base 41, assumed at the start to be in its rest position I, is slightly unscrewed, it is possible to make it leave its bearing surface 49 and to make it pivot in the direction opposite to the hands of a clock until the momment when its head comes, for the working position II, opposite to the bearing surfaces 38 of the base 59. Tightening again of the screw then brings this head to bear on the bearing surface 39 and only communicates to the adjacent base 51 a movement towards the base 41 in the direction of the arrow F, by reason of the cooperation between the stop surfaces carried by the studs such as 62 and the cylindrical holes such as 63.
The association of several bases with the means and in the manner described hereinabove, has the advantage of not requiring any member passing beyond the faces 7, 8, and obtains a very effective tightening; further, the coupling screw which is retained in its housing in rest position, cannot get lost, whilst the access for a tool to the head for tightening is much facilitated by reason of the terminating of these housings either on the second face 54 of the base 41 or on the second face 57 of the base 51.
In order to ensure the fixing of the bases on a support, there is disposed on the face 2 a means for rapid engagement on a conventional profile.
These means comprise, as is shown in FIG. 5, a longitudinal rib 66 of the base and a resilient screw 67 movable in the vicinity of the face 3 which has a ramp 68 to bring about its reverse movement at the moment of engagement on wings 69,70 placed in a same plane of a profile 71, known as a "hat," as can be seen in FIG. 6.
This feature permits rapid placing of a series of bases on a same profile, to then bring them easily into contact one with the other, and finally to achieve in simple manner the placing in working position and the tightening of the screws to assure a positive connection.
A possible modification of this connection can be achieved readily by sliding along the profile a portion of a group of bases already connected, whilst the provision of flexible conduits is particularly facilitated by the lateral disposition of the connectors and the total absence of obstacles to their rotation.
The use of a "hat" profile again provides the advantage of leaving free a large longitudinal space 72 placed between the parallel arms 73, 74 of this profile carrying wings at their ends; in an advantageous manner of construction of the invention, this space is occupied by a longitudinal rib 75 of the base placed between the flange and the screw, an auxiliary channel 10 being situated in this rib.
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A connecting device is for pneumatic apparatus intended particularly to control the distribution of fliuds passing to receptor apparatus. The body (1) of each apparatus can be coupled to that of an identical or analogous apparatus, placed upstream or downstream, by orientatable screws (45) placed in housings opening in the region of faces (5,6) coming into contact during association (25,26). This device is applicable to all apparatus intended to constitute a group of identical apparatuses, and is applied advantageously to the construction of an assembly for the control of jacks.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a National Stage of International patent application PCT/EP2010/052118, filed on Feb. 19, 2010, which claims priority to foreign French patent application No. FR 09 51104, filed on Feb. 20, 2009, the disclosures of which are incorporated by reference in their entirety.
FIELD OF THE INVENTION
Zinc containing pigment compounds are confronted with restrictions which are increasingly severe in terms of use in order to meet the various European environmental requirements and directives and notably in fields such as transport, storage and recycling.
BACKGROUND OF THE INVENTION
Over the past few years, many regulations have appeared, among which mention may be made of the following regulations:
WEEE—Waste Electrical and Electronic Equipment-2002 ROHS—Restriction of the use of certain Hazardous Substances-2002 End-of-Life Vehicle Recycling—ELV Recycling-2002 REACH—Registration, Evaluation and Authorization of Chemicals-2007 GHS—Globally Harmonized System of Classification and Labelling of Chemicals-2005.
Thus, by virtue of their ecotoxicity, the use of zinc containing pigment compounds has become more and more complex over the years.
This is notably the case of zinc phosphate and zinc oxide.
The classification of zinc salts, including notably zinc phosphate and zinc oxide, was thus established in 2004. Zinc phosphate is particularly mentioned in the 28 th A.T.P.—Adaptation to Technical Progress—of European directive 67/548/EEC. Zinc phosphate is labeled N/dangerous for the aquatic environment, and R50/53—“Very toxic to aquatic organisms, may cause long-term adverse effects in the aquatic environment”.
Table 1 recapitulates, according to the amounts of zinc phosphate Zn 3 (PO 4 ) 2 , 2 to 4H 2 O that are used in a product, the labeling restriction and also the associated working code risk phrases in accordance with directive 99/45/EC.
TABLE 1
Labeling and risk phrases for zinc phosphate
use in a product according to 1999/45/EC.
Quantity of
Zn 3 (PO 4 ) 2
Labeling
Risk phrase
>25%
R50/53
Very toxic to aquatic organisms,
may cause long-term adverse effects in
the aquatic environment
2.5%-25%
R51/53
Toxic to aquatic organisms, may
cause long-term adverse effects in the
aquatic environment
0.25%-2.5%
None
R52/53
Harmful to aquatic organisms, may
cause long-term adverse effects in the
aquatic environment.
<0.25%
None
None
Thus, any formulation which contains more than 2.5% by weight of this compound is consequently labeled N/Dangerous for the aquatic environment. A new need has thus emerged since certain markets do not accept this labeling and require pigment and compounds which do not lead to the N labeling.
In accordance with directive 99/45/EC, the formulator, in order to avoid the N labeling, is restricted to the use of less than 2.5% by weight of a product N, R50/53 such as zinc phosphate; however, in the case of anti-corrosion paints and coatings, resistance effectiveness increases with the zinc phosphate content.
It should be noted that, conventionally, according to European directive 1999/45/EC, the term “substances” defines chemical elements and their compounds in the natural state or as obtained by any method of production, including any additive necessary for preserving the stability of the product and any impurity deriving from the method, but with the exclusion of any solvent which can be separated without affecting the stability of the substance or modifying its composition.
It should also be noted that, conventionally, the term “preparations” defines mixtures or solutions composed of two substances or more.
In this context, Zinc free pigment and compounds used in anti-corrosion paints, which had been developed over the past few years, are of renewed interest. Patents have notably been filed on β-tricalcium phosphate (Budenheim, 1991, DE 4014523 A1), and on mixtures of β-tricalcium or dicalcium phosphate and trimagnesium phosphate (Budenheim, 1996-1997, DE 195 41 895 A1-U.S. Pat. No. 5,665,149A).
It has also been demonstrated that anti-corrosion pigments containing magnesium phosphate have an advantageous appeal in paint (Albright and Wilson, 1976, U.S. Pat. No. 3,960,611A), without however equaling zinc phosphate.
These zinc-free pigments are effective in certain paint systems but are not as universal as zinc phosphate. Indeed, zinc phosphate is effective in most of the formulations used in anti-corrosion paint.
SUMMARY OF THE INVENTION
In this context, the objective sought is to develop a detoxification method for obtaining a pigment compound free from acute and chronic aquatic ecotoxicity comprising at least one zinc-based component with good anti-corrosive properties but high toxicity, such as: powder of zinc metal, or zinc oxide or hydroxide, or phosphate, borate, stearate, laurate, carbonate, hydroxycarbonate, polyphosphate, phosphite, pyrophosphate, phosphonate, silicate or ferrite, characterized in that it comprises a mixture of said zinc-based component with at least one phosphate or hydrogenophosphate of the following type:
magnesium, which can be MgHPO 4 .3H 2 O or Mg 3 (PO 4 ) 2 .5H 2 O; sodium, which can be Na 3 PO 4 .10H 2 O or Na 3 PO 4 .12H 2 O or Na 2 HPO 4 .7H 2 O or Na 2 HPO 4 .12H 2 O; potassium, which can be K 3 PO 4 or K 2 HPO 4 ; calcium, which can be CaHPO 4 .2H 2 O or Ca 3 (PO 4 ) 2 ; strontium, which can be SrHPO 4 or Sr 3 (PO 4 ) 2 ; aluminum AlPO 4 ; ammonium, which can be (NH 4 ) 3 PO 4 .3H 2 O or (NH 4 ) 2 HPO 4 ; organic, which can be of guanidine type,
or any other compound based on said cations Mg, Ca, Sr, etc, such as carbonates, oxides, silicates, phosphites, pyrophosphates or phosphonates, said phosphates or hydrogenocarbonates or carbonates or oxides or silicates or phosphites or pyrophosphates free from toxicity enabling to strongly decrease the toxic power of said zinc-based component, while maintaining the good anti-corrosive properties thereof.
According to one variant of the invention, said pigment component free from toxicity has an algae inhibition rate of less than 50% according to OECD protocol 201, a daphnia immobilization rate of less than 50% according to OECD protocol 202, a fish mortality rate of less than 50% according to OECD protocol 203, which results in LC50s (lethal concentration by ingestion for 50% of the population) and EC50s (lethal concentration by inhalation for 50% of the population) above 100 mg/l, and an NOEC (No Observed Effect Concentration) strictly above 1 mg/l on daphnia reproduction according to OECD protocol 211.
According to one variant of the invention, the mixing is carried out with zinc phosphate Zn 3 (PO 4 ) 2 .0 to 4H 2 O and/or zinc oxide, and magnesium phosphate MgHPO 4 .3H 2 O, the weight ratio between the zinc salts and the magnesium phosphate being non-zero and included respectively between approximately 0 and 99.5%.
According to one variant of the invention, the weight ratio between the zinc phosphate and the magnesium phosphate is approximately 90%/10%, and the weight ratio between the zinc phosphate, the magnesium phosphate and the zinc oxide is approximately 80%/10%/10%.
The subject of the invention is also a method for producing an anti-corrosion paint, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
According to one variant of the invention, the method for producing paint comprises the use of a pigment compound in combination with a non-ecotoxic filler, for instance talc, barite, kaolin, silica, aluminum silicates or carbonates, calcium silicates or carbonates, magnesium silicates or carbonates, potassium silicates or carbonates, iron oxide, chromium oxide green, mica, titanium dioxide, carbonate or ferrite, for producing a paint.
According to one variant of the invention, the detoxification method for obtaining a pigment compound comprises a mixing process via a physical or a chemical process, such as sequential precipitation, sequential crystallization, coprecipitation, cocrystallization, grinding, kneading, dispersion, extrusion, forming a slurry, or granulation.
The subject of the invention is also a method for obtaining a coating comprising a polymer of epoxy, alkyd, acrylic, vinyl, polyurethane, polyester, aminoplast, polyolefin, phenolic, butyral, butadiene, PVDF, rubber, or synthetic or natural oil type, characterized in that it uses the pigment compound obtained by means of the detoxification method of the invention.
A subject of the invention is also the use of an anti-corrosion coating obtained according to the method of the present invention, for treating a metal part or object such as a motor vehicle, ship, aircraft, bridge, civil engineering vehicle, rail vehicle, agricultural building, industrial building, coil coating, electronic, computer and household appliances materials, gas plant and oil plant.
A subject of the invention is also a method for obtaining a plastic, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
A subject of the invention is also a method for obtaining a mastic, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
A subject of the invention is also a method for obtaining an adhesive, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
A subject of the invention is also a method for obtaining an ink, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
A subject of the invention is also a method for obtaining a natural or synthetic rubber material, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
A subject of the invention is also a method for obtaining a solid or liquid lubricant, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
A subject of the invention is also a method for obtaining a fertilizing substance, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
A subject of the invention is also a method for obtaining an anti-UV compound for plastics, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
Finally, a subject of the invention is a method for obtaining an anti-UV compound for cosmetics, characterized in that it uses the pigment compound obtained by means of the detoxification method according to the invention.
A subject of the invention is also the use of an anti-corrosion coating according to the invention, for treating a metal part or object such as a motor vehicle, ship, aircraft, bridge, heavy construction machine, rail vehicle, agricultural building, industrial building, coil coating, electronic, computer and household appliance material, gas plant and oil plant.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be understood more clearly and other advantages will become apparent on reading the description which follows and which is given without implied limitation, and by virtue of the appended figures among which:
FIG. 1 illustrates paint tests for evaluating the anti-corrosion performance levels, carried out according to the ASTM 1654 standards for plate blistering and degree of rusting, of a coating comprising an anti-corrosion adhesion primer of a first type of epoxy amide incorporating a standard zinc phosphate, of a coating comprising an anti-corrosion adhesion primer of a first type of epoxy amide incorporating a first compound according to the invention, and of a coating comprising an anti-corrosion adhesion primer of a second type of epoxy amide incorporating a second compound according to the invention;
FIG. 2 illustrates paint tests for evaluating the anti-corrosion performance levels, carried out according to the ASTM 1654 standards for plate blistering and degree of rusting, of a coating comprising an anti-corrosion adhesion primer of a first type of epoxy amine incorporating a standard zinc phosphate, of a coating comprising an anti-corrosion adhesion primer of a first type of epoxy amine incorporating a first compound of the invention, and of a coating comprising an anti-corrosion adhesion primer of a first type of epoxy amine incorporating a second compound according to the invention.
The rest of the description is more particularly presented in the context of magnesium monohydrogen phosphate, which is very suitable because it has very good compatibility with zinc phosphate.
DETAILED DESCRIPTION
Example of an Anti-Corrosion Compound Based on Zinc Phosphate, on Zinc Oxide and on Magnesium Phosphate
The following compound was tested:
PZATB: 80% PZ/10% PAT30/10% ZnO with PZ: Zn 3 (PO 4 ) 2 .0 to 4H 2 O and PAT30: MgHPO 4 .3H 2 O
1) Ecotoxicity Tests on the Anti-Corrosion Compounds based on Zinc Phosphate, on Zinc Oxide and on Magnesium Phosphate
There are two possible routes for determining the “dangerous for the environment” labeling of preparations:
a first route governs the determination according to the substance mixture rule, i.e. according to the composition of the product. By this route, any product containing zinc is consequently dangerous for the environment; a second route governs the determination according to the ecotoxicity tests in accordance with OECD protocols 201, 202 and 203 for acute ecotoxicity on the preparation containing dangerous materials, this second possible route prevailing over the first route as defined in regulations 1999/45/EC and 1272/2008/EC reiterating the criteria for classification of a tested preparation or mixture containing at least one dangerous material.
According to the second route, the tests are carried out on the following three species: algae, daphnia and fish.
From a regulatory point of view, the applicant followed amended annex 5 of directive 67/548/EEC, directive 99/45/EEC relating to modified preparations, and the GHS report prepared in 2003—part 3, paragraph 3.10.3 relating to the criteria for the classification of mixtures, and tests were carried out according to the OECD guidelines 201 adopted on Mar. 23, 2006, 202 adopted on Apr. 13, 2004, and 203 adopted on Jul. 17, 1992.
The conventional labeling of a compound is subsequently carried out in relation to the poorest result of the three acute tests and makes it possible to provide the results recapitulated in table 2, in which the labelings possibly imposed are defined according to a concentration C, a test duration expressed in hours and a rate of 50 percent of species succumbing at the end of the number of hours identified.
TABLE 2
Labeling and risk phrases according to the results obtained
in the ecotoxicity tests according to 1999/45/EC
Concen-
Tests
tration C
Labeling
Risk phrase
96H LC50 (fish)
≦1 mg/l
R50/53
48H EC50 ( daphnia )
Very toxic to aquatic
72H LC50 (algae)
organisms, may cause
long-term adverse
effects in the aquatic
environment
96H LC50 (fish)
between
R51/53
48H EC50 ( daphnia )
1 and
Toxic to aquatic organisms,
72H LC50 (algae)
10 mg/l
may cause long-term
adverse effects in the
aquatic environment
96H LC50 (fish)
between
None
R52/53
48H EC50 ( daphnia )
10 and
Harmful to aquatic
72H LC50 (algae)
100 mg/l
organisms, may
cause long-term
adverse effects in the
aquatic environment
96H LC50 (fish)
>100 mg/l
None
R53 or no risk phrase
48H EC50 ( daphnia )
according to the chronic
72H LC50 (algae)
ecotoxicity
The globally harmonized labeling system GHS, in its latest revision of 2009, reiterates and confirms the maximum limits of 1 (category 1) 10 (category 2 [1 to 10 mg/l]) and 100 mg/l (category 3 [10 to 100 mg/l]) as criteria for classification of acute aquatic toxicity of categories 1 to 3. Above 100 mg/l for acute toxicity, the substance or the preparation is not classified for its toxicity.
In addition, the GHS also specifies that, when the chronic toxicity exhibits a no observed effect concentration of greater than 1 mg/l, then this substance or this mixture is not subject to classification for its chronic nature.
The tests were carried out at the CIT, Centre International de Toxicologie [International Center for Toxicology] in Evreux (France).
The preparation was produced by physical mixing.
The term GLP denotes tests carried out according to Good Laboratory Practice.
The following terms are used:
the reference LC50 denotes: the lethal concentration by ingestion for 50% of the population; the reference EC50 denotes: the lethal concentration by inhalation for 50% of the population.
1.1. Acute ecotoxicity on Pseudokirchneriella subcapitata algae
TABLE 3
Results of acute ecotoxicity on Pseudokirchneriella subcapitata
algae
GLP/non GLP
Inhibition
LC50
Preparation
test
algae (%)
(mg/l)
PZATB
Non GLP
36.2
>100
Table 3 shows that the inhibition of the algae is less than 50%. The preparation is not therefore ecotoxic to the algae owing to an acute ecotoxicity LC50>100 mg/l according to OECD protocol 201.
1.2. Acute ecotoxicity on Daphnia magna crustaceans
TABLE 4
Results of acute ecotoxicity on Daphnia magna crustaceans
GLP/non GLP
Immobilization
EC50
Preparation
test
daphnia (%)
(mg/l)
PZATB
Non GLP
0
>100
Table 4 shows that no daphnia is immobilized. The preparation is not therefore ecotoxic to crustaceans owing to an acute ecotoxicity EC50 >100 mg/l according to OECD protocol 202.
1.3. Acute ecotoxicity on Oncorhynchus mykiss fish
TABLE 5
Results of acute ecotoxicity on Oncorhynchus mykiss fish
Number
Trout
GLP/non GLP
of
mortality
LC50
Preparation
test
trout
(%)
(mg/l)
PZATB
Non GLP
10
0
>100
Table 5 shows that no trout died. The preparation does not exhibit any toxicity to the fish owing to an acute ecotoxicity LC50 >100 mg/l according to OECD protocol 203.
It thus emerges from these test that PZATB does not exhibit any acute toxicity.
Example of Anti-Corrosion Compounds Based on Zinc Phosphate and on Magnesium Phosphate
Various compounds were produced and tested with weight ratios between zinc phosphate and magnesium monohydrogen phosphate ranging from 99%/1%) to 4.3%/95.7%, and identified as follows:
PZAT 99:PZ 99%/PAT30 1%
PZAT 95:PZ 95%/PAT30 5%
PZAT 90:PZ 90%/PAT30 10%
PZAT 80:PZ 80%/PAT30 20%
PZAT 70:PZ 70%/PAT30 30%
PZAT 60:PZ 60%/PAT30 40%
PZAT 50:PZ 50%/PAT30 50%
PZAT 40:PZ 40%/PAT30 60%
PZAT 04:PZ 4.3%/PAT30 95.7%
with PZ:Zn 3 (PO 4 ) 2 ,0 to 4H 2 O and
PAT30:Mg HPO 4 ,3H 2 O
2) Acute Ecotoxicity Tests on the Anti-Corrosion Compounds based on Zinc Phosphate and on Magnesium Phosphate
Tests were carried out at the CIT, Centre International de Toxicologie [International Center for Toxicology] in Evreux (France).
The preparations were produced by physical mixing.
The term GLP denotes tests carried out according to Good Laboratory Practice.
The following terms are used:
the reference LC50 denotes: the lethal concentration by ingestion for 50% of the population; the reference EC50 denotes: the lethal concentration by inhalation for 50% of the population.
2.1. Acute Ecotoxicity on Pseudokirchneriella subcapitata algae
TABLE 6
Results of acute ecotoxicity on Pseudokirchneriella subcapitata
algae
GLP/non GLP
Inhibition
LC50
Preparation
test
algae (%)
(mg/l)
PZ 99%/PAT30 1%
GLP
16.29
>100
PZ 95%/PAT30 5%
GLP
6.76
>100
PZ 90%/PAT30 10%
GLP
11.67
>100
PZ 80%/PAT30 20%
Non GLP
23.58
>100
PZ 70%/PAT30 30%
Non GLP
19.16
>100
PZ 60%/PAT30 40%
Non GLP
17.5
>100
PZ 50%/PAT30 50%
Non GLP
13.72
>100
PZ 40%/PAT30 60%
Non GLP
6.58
>100
PZ 4.3%/PAT30 95.7%
GLP
12.24
>100
Table 6 shows that the inhibition of the algae is less than 50%. The preparation is not therefore ecotoxic to the algae owing to an acute ecotoxicity LC50>100 mg/l according to OECD protocol 201.
2.2. Acute Ecotoxicity on Daphnia magna crustaceans
TABLE 7
Results of acute ecotoxicity on Daphnia magna crustaceans
GLP/non GLP
Immobilization
EC50
Preparation
test
daphnia (%)
(mg/l)
PZ 99%/PAT30 1%
GLP
0
>100
PZ 95%/PAT30 5%
GLP
0
>100
PZ 90%/PAT30 10%
GLP
0
>100
PZ 80%/PAT30 20%
Non GLP
0
>100
PZ 70%/PAT30 30%
Non GLP
0
>100
PZ 60%/PAT30 40%
Non GLP
0
>100
PZ 50%/PAT30 50%
Non GLP
0
>100
PZ 40%/PAT30 60%
Non GLP
0
>100
PZ 4.3%/PAT30 95.7%
GLP
0
>100
Table 7 shows that no daphnia is immobilized. The preparation is not therefore ecotoxic to crustaceans owing to an acute ecotoxicity EC50 >100 mg/l according to OECD protocol 202.
2.3. Acute Ecotoxicity on Oncorhynchus mykiss fish
TABLE 8
Results of acute ecotoxicity on Oncorhynchus mykiss fish
Number
Trout
GLP/non GLP
of
mortality
LC50
Preparation
test
trout
(%)
(mg/l)
PZ 99%/PAT30 1%
GLP
10
0
>100
PZ 95%/PAT30 5%
GLP
10
0
>100
PZ 90%/PAT30 10%
GLP
10
0
>100
PZ 80%/PAT30 20%
Non GLP
10
0
>100
PZ 70%/PAT30 30%
Non GLP
10
0
>100
PZ 60%/PAT30 40%
Non GLP
10
0
>100
PZ 50%/PAT30 50%
Non GLP
10
0
>100
PZ 40%/PAT30 60%
Non GLP
10
0
>100
PZ 4.3%/PAT30 95.7%
GLP
10
0
>100
Table 8 shows that no trout died. The preparation does not exhibit any toxicity to the fish owing to an acute ecotoxicity LC50>100 mg/l according to OECD protocol 203.
Various compounds were produced and tested with weight ratios between zinc phosphate and magnesium monohydrogen phosphate ranging from 99%/1% to 25%/75%, and identified as follows:
PZAT 99:PZ 99%/PAT30 1%
PZAT 92:PZ 92%/PAT30 8%
PZAT 25:PZ 75%/PAT30 25%
with PZ:Zn 3 (PO 4 ) 2 .0 to 4H 2 O and
PAT30:MgHPO 4 .3H 2 O
3) Chronic Ecotoxicity Tests on the Anti-Corrosion Compounds based on Zinc Phosphate and on Magnesium Phosphate
There are two possible routes for determining the “dangerous for the environment in the long term” labeling of preparations:
a first route governs the determination according to the substance mixture rule, i.e. according to the composition of the product. Via this route, any product containing more than 25% of an R53 product (1999/45/EC) consequently exhibits a chronic ecotoxicity; a second route governs the determination according to ecotoxicity tests on the most sensitive species, which, in the case of zinc salts, is daphnia , in accordance with OECD protocol 211 relating to preparations containing dangerous materials, this possible second route prevailing over the first.
From a regulatory point of view, the applicant followed amended annex 5 of directive 67/548/EEC, directive 99/45/EEC relating to modified preparations in table 9, regulation 1272/2008 EC resulting from the recommendations of the UNO report of the GHS prepared in 2003 modified—part 3, paragraph 3.10.3 in table 10 relating to the criteria for the classification of mixtures, and tests were carried out according to the OECD guidelines 211 adopted on Oct. 3, 2008.
The term “NOEC” denotes the No Observed Effect Concentration.
TABLE 9
Chronic ecotoxicity labeling and risk phrases according to the GHS
Labeling and risk phrases according
Tests
to the GHS
If NOEC < or = 1 mg/l
May cause long-term adverse effects
in the aquatic environment
If NOEC > 1 mg/l
No labeling
No risk phrase
TABLE 10
Chronic ecotoxicity labeling and risk phrases according
to regulation 1999/45/EC for preparations or mixtures
Labeling and risk phrases according
Content
to current regulations
If the content of R53
R53
substance >25% (in the
May cause long-term adverse effects
absence of R50 or 51 or 52)
in the aquatic environment
If the content of R53
No labeling
substance <25% (in the
No risk phrase
absence of R50 or 51 or 52)
Tests were carried out at the CIT, Centre International de Toxicologie [International Center for Toxicology] in Evreux (France).
The preparations were produced by physical mixing.
The tests were carried out under GLP. The term GLP denotes tests carried out according to Good Laboratory Practice.
TABLE 11
Results of the chronic ecotoxicity tests
Preparation
Mortality
Growth
Reproduction
NOEC
PZAT99
No effect
No effect
No effect
> or = 1.5 mg/l
PZAT92
No effect
No effect
No effect
> or = 1.5 mg/l
PZAT25
No effect
No effect
No effect
> or = 1.5 mg/l
Table 11 shows that the preparations do not exhibit chronic ecotoxicity owing to an NOEC>1 mg/l according to OECD protocol 211.
None of the preparations containing zinc phosphate and magnesium phosphate have any dangerous for the environment labeling (no acute or chronic toxicity).
Since preparations containing 0 to 25% of zinc phosphate do not exhibit any chronic ecotoxicity according to the substance mixture rule, it was demonstrated that any compound containing from 0 to 99% of zinc phosphate as a mixture with magnesium phosphate is consequently exempt from dangerous for the environment labeling.
It thus emerges from these analyses that none of these preparations mentioned above in points 2 and 3 are dangerous for the environment, in terms of both acute and chronic characteristics.
The corresponding compounds listed above were evaluated in terms of toxicity and, by way of industrial illustration, are also evaluated in terms of anti-corrosion performance levels.
For this, conventional anti-corrosion adhesion primers of solvent-phase epoxy system type, incorporating the various pigment compounds, were prepared without there being any notable losses of performance levels compared with PZ.
Indeed, in the context of the problem of anti-corrosion coating, it is sought to develop anti-corrosion adhesion primers corresponding to the first coat intended to coat a metal surface, itself intended to support in a conventional manner a second coat of paint generally carrying the color of said coating and frequently called topcoat.
4) Anti-Corrosion Tests in Paint
Thus, the applicant carried out tests in paint proving the good anti-corrosion performance levels in paint of the compounds. These tests were carried out with solvent-phase epoxy primers.
Illustration 1: Tests of the Preparation in a Solvent-Phase Vinyl Alkyd Primer
The formula of table 12 was prepared.
TABLE 12
Formula of a solvent-phase vinyl alkyd primer
%
STARTING MATERIALS
WEIGHT
DESCRIPTION
SUPPLIERS
SETAL 199-SS-55
25.5
Medium oil alkyd
NUPLEX
ACETONE
5.00
solvent
SHELL
NUODEX 10% Ca
0.50
Dispersant
ELEMENTIS Specialities
BENTONE SD2
0.30
Rheological additive
NL Chemicals
SOLVESSO 100
7.5
Aromatic solvent
EXXON CHEMICAL
ZINC PHOSPHATE PZ20
8.00
Corrosion inhibitor
SNCZ
TALC 10 M2
4.00
filler
RIO TINTO Minerals
MICA MU M 2/1
9.00
filler
CMMP
MICRONOX
11.00
Micronized natural iron
KEYSER AND MACKAY
oxide
THIXATROL ST
0.30
Thixotropic additive
NL Chemicals
grinding for 40 minutes until
Hegman fineness of 6 is
obtained
LAROFLEX MP35/S100 at
21.10
Vinyl chloride copolymer
BASF
28.5%
SOLVESSO 100
2.93
Aromatic solvent
EXXON CHEMICAL
ISOPROPYL ALCOHOL
1.20
solvent
SHELL
CERECLOR 42
0.60
Chloroparaffin, plasticizer
INEOS
NUODEX 8% Co
0.05
siccative
ELEMENTIS Specialities
NUODEX 10% Zr
0.12
siccative
ELEMENTIS Specialities
DUOMEEN TDO
0.30
Cationic surfactant
AKZO Chemie
MEKO
0.50
Methyl ethyl ketoxime,
anti-skinning agent
% PVC
30.21
(pigment volume
concentration)
Dry extract, % by weight
60.49
Dry extract, % by volume
41.62
Pigment/binder ratio
0.43
(by volume)
Comparison of the Compounds PZ, PZATB, and PZAT90 in Alkyd Primer
PZ, the preparation PZ 80%/PAT30 10%/ZnO 10%, and the preparation PZ 90%/PAT30 10% were compared. PZATB and PZAT90 were prepared by physical mixing.
A metal surface was given a coat of anti-corrosion primer incorporating the pigment compounds in an alkyd resin, having a thickness of 40 μm. This coat is covered with a film of an alkyd coat having a thickness of 25 μm, also commonly called topcoat.
The whole is exposed to a salt fog (standard ASTM B117) for 300 hours.
FIG. 1 illustrates the results obtained.
A rating made it possible to evaluate the degree of rusting and the degree of blistering.
For the degree of rusting, standard NF ISO 4628-3 T30-140-3 was used.
Ri0: no rusting, 0% rusted surface area
Ri1: very little rusting, 0.5% rusted surface area
Ri5: highly rusted, 40 to 50% rusted surface area
For the degree of blistering, standards NF ISO 4628-1 T30-140-2 and NF ISO 4628-3 T30-140-2 were used.
DOS0: no detectable defect of size invisible at 10× magnification
D2S2: small amount of small blisters
D5S5: large amount of large blisters.
The “scribe rating” and the “global rating” are produced according to standard ASTM D 1654 January 2005—“Standard Test Method for Evaluation of Painted or Coated Specimens Subjected to Corrosive Environments”—tables 1 and 2 respectively, page 3.
Rating at Scribe:
10 represents 0 mm at scribe 0 represents 16 mm and more at scribe
Global Rating:
10 represents 0% degradation 0 represents more than 75% degradation.
The rating in table 13 is produced according to the standards described above.
TABLE 13
Rating of the solvent-phase vinyl alkyd primer
Degree of
Degree of
rusting
blistering
NF-ISO
NF-ISO
Scribe
Full plate
4828-3
4828-3
corrosion
global rating
T 30140-3
T 30140-3
ASTM 1654
ASTM 1654
PZ
RI1
D2S2
6
6
PZAT90
RI1
D3S2
4
4
PZATB
RI0
D0S0
8
9
PZATB is as effective as PZ, and more effective than PZAT90.
Illustration 2: Tests of the preparation in a solvent-phase epoxy amide primer
The formula of table 14 was prepared.
TABLE 14
Formula of a solvent-phase epoxy amide
%
STARTING MATERIALS
WEIGHT
DESCRIPTION
SUPPLIERS
PART A
Introduce with mixing in
the following order
EPIKOTE 1001/XYLENE
22.90
Epoxy resin
HEXION
50/50 weight/weight
SOLVESSO 100
7.20
Aromatic hydrocarbon
TOTAL Chimie
solvent
ISOBUTYL ALCOHOL
1.60
Solvent
SHELL
DOWANOL PMA
7.30
Glycol ester, solvent
DOW
NUODEX 10% Ca
0.50
Dispersant
ELEMENTIS Specialities
BENTONE SD2
0.15
Rheological additive
ELEMENTIS Specialities
TiO 2 TR92
4.30
Rutile
HUNSTMANN
ZINC PHOSPHATE PZ20
8.00
Corrosion
SNCZ
inhibitor
YELLOW IRON OXIDE
5.10
Pigment, colorant
BAYER
3920
TALC 10 M2
9.30
Filler
RIO TINTO Minerals
MICA MU 2/1
10.70
Filler
CMMP
THIXATROL ST
0.20
Thixotropic additive
ELEMENTIS Specialities
Grinding in ball mill for 40
minutes until Hegman
fineness of 5 obtained
BUTYL ACETATE
2.50
Ester, solvent
TOTAL chimie
CERECLOR M50
2.40
Chloroparaffin, plasticizer
INEOS
DUOMEEN TDO
0.15
Cationic surfactant
AKZO Chemie
PART B
XYLENE
3.00
Aromatic
TOTAL Chimie
hydrocarbon,
solvent
EPILINK 230
0.30
Accelerator
AKZO Chemie
ARADUR 115 X70 BD
14.40
Polyamidoamide
VANTICO
hardener
% PVC
34.5
(pigment volume
concentration)
Dry extract, % by weight
62.39
Dry extract, % by volume
44.75
Pigment/binder ratio
0.53
(by volume)
Comparison of the compounds PZ, PZATB and PZAT90 in epoxy amide primer
PZ, the preparation PZ 80%/PAT30 10%/ZnO 10%, and the preparation PZ 90%/PAT30 10% were compared. PZATB and PZAT90 were prepared by physical mixing.
A metal surface was given a coat of anti-corrosion primer incorporating the pigment compounds in an epoxy amide resin, having a thickness of 50 μm. This coat is covered with a film of polyurethane PU having a thickness of 100 μm, also commonly called topcoat.
The whole is exposed to a salt fog (standard ASTM B117) for 600 hours.
FIG. 2 illustrates the results obtained.
The rating in table 15 is produced according to the same standards as mentioned above.
TABLE 15
Rating of the solvent-phase epoxy amide primer
Degree of
Degree of
rusting
blistering
NF-ISO
NF-ISO
Scribe
Full plate
4828-3
4828-3
corrosion
global rating
T 30140-3
T 30140-3
ASTM* 1654
ASTM* 1654
PZ
RI1
D2S2
4
7
PZAT90
RI1
D2S2
6
8
PZATB
RI1
D2S2
3
6
PZAT90 is as effective as PZ, and more effective than PZATB.
Illustration 3: Tests of the Preparation in a Solvent-Phase Epoxy Amine Primer
The formula in table 16 was prepared.
TABLE 16
Formula of a solvent-phase epoxy amine primer
%
STARTING MATERIALS
WEIGHT
DESCRIPTION
SUPPLIERS
PART A
Introduce with stirring in the
following order
EPIKOTE 1001/XYLENE
25.40
Epoxy resin
HEXION
50/50 weight/weight
SOLVESSO 100
7.90
Aromatic hydrocarbon,
TOTAL chimie
solvent
ISOBUTYL ALCOHOL
1.80
Solvent
SHELL
DOWANOL PMA
8.00
Glycol ester, solvent
DOW
NUODEX 10% Ca
0.50
Dispersant
ELEMENTIS Specialities
BENTONE SD2
0.20
Rheological additive
ELEMENTIS Specialities
TiO 2 TR92
4.80
Rutile
HUNSTMANN
ZINC PHOSPHATE PZ20
8.00
Corrosion
SNCZ
inhibitor
YELLOW IRON OXIDE
5.70
Pigment, colorant
BAYER
3920
TALC 10 M2
9.00
Filler
RIO TINTO Minerals
MICA MU 2/1
10.00
Filler
CMMP
THIXATROL ST
0.20
Thixotropic additive
ELEMENTIS Specialities
Grinding in bead mill for 40
minutes until Hegman
fineness of 5 obtained
BUTYL ACETATE
2.60
Ester, solvent
TOTAL chimie
CERECLOR M50
2.60
Chloroparaffin, plasticizer
INEOS
DUOMEEN TDO
0.20
Cationic surfactant
AKZO Chemie
PART B
XYLENE
4.10
Aromatic hydrocarbon,
TOTAL chimie
solvent
DOWANOL PMA
4.10
Glycol ester, solvent
DOW
EFFIDUR 433
4.90
Cycloaliphatic polyamine
France INDUSTRIE
% PVC
39.27
(pigment volume
concentration)
Dry extract, % by weight
58.56
Dry extract, % by volume
39.27
Pigment/binder ratio
0.65
(by volume)
Comparison of the Compounds PZ, PZATB and PZAT90 in Epoxy Amine Primer
An anti-corrosion primer based on epoxy amine incorporating the pigment preparations is prepared, having a thickness of 50 μm. This coat is covered with a film of polyurethane PU having a thickness of 100 μm, also commonly called topcoat.
The whole is exposed to a salt fog—standard ASTM B117—for 600 hours.
FIG. 3 illustrates the results obtained.
The rating in table 17 is produced according to the same standards as mentioned above.
TABLE 17
Rating of the solvent-phase epoxy amine primer
Degree of
Degree of
rusting
blistering
Complete
NF-ISO
NF-ISO
Scribe
plate
4828-3
4828-3
corrosion
general rating
T 30140-3
T 30140-3
ASTM* 1654
ASTM* 1654
PZ
RI1
D0S0
6
6
PZAT90
RI0
D0S0
8
9
PZATB
RI1
D0S0
6
6
PZATB is as effective as PZ, PZAT90 is more effective than these other two compounds.
A comparison of PZ and of the PZAT90 pigment in an epoxy amide system, and solvent-phase epoxy amide shows very satisfactory results regarding the performance of the PZAT90 pigment.
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A detoxification method for obtaining a pigment compound free from acute and chronic aquatic ecotoxicity by mixing at least one zinc-based component with good anti-corrosive properties but high toxicity-with a phosphate or hydrogen phosphate of a magnesium, sodium, potassium, calcium, strontium, aluminum, ammonium, or organic type or any other compound based on such cations, such as carbonates, oxides, silicates, phosphites, pyrophosphates or phosphonates, said phosphates or hydrogen carbonates or carbonates or oxides or silicates or phosphites or pyrophosphates freed from toxicity enabling a very considerable reduction of the toxic power of said zinc-based component, while maintaining the good anti-corrosive properties thereof.
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BACKGROUND
Premium articles have been used to promote the sale of products enclosed within cartons. For example, toys and other novelty items have been mounted in cartons containing food products in order to enhance the salability of the products. U.S. Pat. No. 5,379,886 to Brauner et al. discloses one such product. Brauner's package, however, requires the use of a separate premium tray to house a promotional product, which increases the cost and difficulty of manufacture of the package.
SUMMARY
According to a first embodiment, a carton blank comprises a front panel having a display window, a first side panel, a back panel, a second side panel, a display panel, at least one top flap extending across a first marginal potion of the blank, and at least one bottom flap extending across a second marginal portion of the blank. When the carton is assembled from the blank, a portion of the display panel faces the display window.
According to the first embodiment, an article can be mounted within the carton between the display panel and the display window, where it is visible from the exterior of the carton. Additional mounting trays or inserts are not required, which reduces the cost of manufacture. In alternative embodiments, graphical and/or textual information can be printed on the display panel such that it is visible through the display window.
The article may kept separate from the contents of the carton, which prevents contamination of the carton contents and reduces the likelihood of damage to the article. The size of the display window can be selected so that the article may not be removed through the display window, which reduces the likelihood of pilferage of the article.
Other aspects, features, and details of the present invention can be more completely understood by reference to the following detailed description of a preferred embodiment, taken in conjunction with the drawings and from the appended claims.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
FIG. 1 is a plan view of a blank used to form a carton according to a first embodiment.
FIG. 2 is a perspective view of the blank partially erected.
FIG. 3 is a perspective view of the carton partially erected.
FIG. 4 is a perspective view of the carton partially erected.
FIG. 5 is a section view taken on line 5 - 5 in FIG. 4 .
FIG. 6 is a perspective view of the assembled carton.
FIG. 7 is a plan view of a blank used to form a carton according to a second embodiment.
DETAILED DESCRIPTION
The present embodiments are addressed to cartons having display features which allow a premium, product information, and/or other items to be viewed from an exterior of the cartons.
FIG. 1 is a plan view of a first, interior side 5 of a blank 8 used to form a carton 100 (illustrated in FIG. 6 ) according to a first embodiment. The first side 5 will be disposed in the interior of the assembled carton 100 .
The blank 8 comprises a first side panel 10 foldably connected to a front panel 20 at a first transverse fold line 21 , a second side panel 30 foldably connected to the front panel 20 at a second transverse fold line 31 , a back panel 40 foldably connected to the first side panel 30 at a third transverse fold line 41 , a third side panel 50 foldably connected to the back panel 40 at a fourth transverse fold line 51 , a display panel 60 foldably connected to the third side panel 50 at a fifth transverse fold line 61 , and an adhesive flap 80 foldably connected to the display panel 60 at a sixth transverse fold line 81 .
The first side panel 10 is foldably connected to a side top flap 12 and a side bottom flap 14 . The front panel 20 is foldably connected to a front top flap 22 and a front bottom flap 24 . The second side panel 30 is foldably connected to a side top flap 32 and a side bottom flap 34 . The back panel 40 is foldably connected to a back top flap 42 and a back bottom flap 44 . The flaps 12 , 22 , 32 , 42 extend along a top marginal area of the blank 8 , and the flaps 14 , 24 , 34 , 44 extend along a bottom marginal area of the blank 8 . When the carton 100 is assembled, the flaps 12 , 22 , 32 , 42 close a top opening of the carton 100 , and the flaps 14 , 24 , 34 , 44 close a bottom opening of the carton 100 .
The front top flap 22 can include a closure tab 26 that is sized to be received in a closure slit 46 formed in the back top flap 42 . The closure tab 26 and closure slit 46 provide for recloseable sealing of the carton 100 after the top of the carton 100 has been opened. Glue release cuts 48 can also be included in the back top flap 42 to aid in opening of the carton 100 .
A display window or aperture 26 is formed in the front panel 20 . The display window 26 is arranged in the front panel 20 so that when the carton 100 is erected, a premium article A (shown in FIG. 2 ) mounted on a display side of the display panel 60 is visible through the window 26 . The premium article A, as shown in FIG. 2 , will be mounted on the opposite, exterior, side of the blank 8 , at a location generally indicated by the area M in FIG. 1 . The display panel 60 includes struts 70 cut from the display panel 60 . Each strut 70 includes a base panel 76 connected to the display panel 60 at a fold line 78 , and an adhesive flap or tab 72 connected to the base panel 76 at a fold line 74 . The struts 70 provide an offset spacing of the display panel 60 from the front panel 20 . In the assembled carton 100 , the offset spacing between the display panel 60 and the front panel 20 is generally defined by the length L 3 of the base panels 76 . The length L 1 of the first side panel 30 may be, for example, approximately equal to the length L 2 of the second side panel 30 plus the length L 3 of the base panels 76 .
FIG. 2 is a perspective view of the blank 8 partially erected. In practice, the blank 8 may remain generally flat during this stage of erection, with 180 degree folding occurring at fold lines 61 and 41 . For the purpose of illustrating the final arrangement of the display panel 60 and the struts 70 , however, FIG. 2 shows the blank 8 folded about fold lines 51 and 61 , and the struts 70 in an erect position. Initially, glue or other adhesive is applied to the adhesive flap 80 as indicated by the stippling, as well as on the tabs 72 . Adhesive is also applied to the display panel 60 at a location where the article A is to be applied, and to the exterior side of the third side panel 50 . The blank 8 is then folded 180 degrees about the fold line 61 , and the article A is adhered to the display panel 60 . After adhering the article A to the panel 60 , the blank 8 is then folded 180 degrees about the fold line 41 . Folding about the fold line 41 brings the second side panel 30 into contact with the adhesive on the adhesive flap 80 , and the adhesive on the struts 70 into contact with the front panel 20 .
Referring to FIG. 3 , the first side panel 10 is adhered to the third side panel 50 , and the resulting article is “opened” so that it has a tubular configuration. FIG. 4 is a front perspective view of the partially assembled carton, and FIG. 5 is a section view taken on line 5 - 5 in FIG. 4 . As shown in FIG. 5 , the struts 70 offset the display panel 60 from the front panel 20 by a distance that may be equal to or approximately equal to the length L 3 of the base panels 76 . The article A is disposed on the display panel 60 so that it is visible through the display window 26 in the front panel 20 .
Referring also to FIG. 6 , the flaps 12 , 14 , 22 , 24 , 32 , 34 , 42 , 44 may be adhered by glue or other adhesives in a conventional manner, resulting in the carton 100 illustrated in FIG. 6 . A bag (not shown) or other vessel filled with product may be inserted in the carton in a conventional manner before closing the flaps 12 , 14 , 22 , 24 , 32 , 34 , 42 , 44 . As shown in FIG. 6 , the finished carton 100 has a top panel 90 formed from the flaps 12 , 22 , 32 , 42 , and a bottom panel 92 formed from the flaps 14 , 24 , 34 , 44 . The display window 26 allows a consumer to view the premium article A, and if desired, to touch or otherwise evaluate the article A.
The premium article A can be, for example, any item used to enhance the salability or desirability of a product contained within the assembled carton 100 . For example, the premium article A is illustrated in FIG. 2 as a compact disc. As an alternative to or in combination with the premium article A, the display panel 60 could also include, for example, an image or other graphical, textual, or product information. If there is no premium article A applied to the display panel 60 , a printing step may be used to apply an image to the display panel 60 , and an article adhesion step may be omitted. If desired, the display window 26 may be covered by a clear layer of film or other material.
FIG. 7 is a plan view of a blank 208 used to form a carton according to a second embodiment. The blank 208 is generally identical to the blank illustrated in FIG. 1 , except that the display window 226 in the front panel 220 is formed from a plurality apertures 228 . The apertures 228 are generally rectangular and are arranged in a grid of columns and rows. The grid of apertures 228 can be used to create special optical effects for a consumer viewing an article disposed behind the window 226 .
According to the above embodiments, product salability can be enhanced by an article mounted within the carton between the display panel and the display window, where it is visible from the exterior of the carton. The article is kept separate from the contents of the carton, which prevents contamination of the carton contents and reduces the likelihood of damage to the article. In some embodiments, the size of the display window can be selected so that the article may not be removed through the display window, which reduces the likelihood of pilferage of the article. Graphical and/or textual information can also be printed on the display panel such that it is visible and/or accessible through the display window.
In the exemplary embodiments discussed above, the blanks may be formed from clay coated newsprint (CCN). In general, the blanks may be constructed of paperboard, having a caliper of at least about 14 , so that they are heavier and more rigid than ordinary paper. The blanks, and thus the cartons, can also be constructed of other materials, such as cardboard, or any other material having properties suitable for enabling the cartons to function at least generally as described above. The first and second sides of the blanks can be coated with, for example, a clay coating. The clay coating may then be printed over with product, advertising, and other information or images. The blanks may then be coated with a varnish to protect any information printed on the blank. The blanks may also be coated with, for example, a moisture barrier layer, on either or both sides of the blanks. The blanks can also be laminated to or coated with one or more sheet-like materials at selected panels or panel sections.
In accordance with the exemplary embodiments, a fold line can be any substantially linear, although not necessarily straight, form of weakening that facilitates folding therealong. More specifically, but not for the purpose of narrowing the scope of the present invention, fold lines include: a score line, such as lines formed with a blunt scoring knife, or the like, which creates a crushed portion in the material along the desired line of weakness; a cut that extends partially into a material along the desired line of weakness, and/or a series of cuts that extend partially into and/or completely through the material along the desired line of weakness; and various combinations of these features. In situations where cutting is used to create a fold line, typically the cutting will not be overly extensive in a manner that might cause a reasonable user to incorrectly consider the fold line to be a tear line.
The above embodiments may be described as having one or panels adhered together by glue. The term “glue” is intended to encompass all manner of adhesives commonly used to secure carton panels in place.
The foregoing description of the invention illustrates and describes the present invention. Additionally, the disclosure shows and describes only selected preferred embodiments of the invention, but it is to be understood that the invention is capable of use in various other combinations, modifications, and environments and is capable of changes or modifications within the scope of the inventive concept as expressed herein, commensurate with the above teachings, and/or within the skill or knowledge of the relevant art.
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A carton is formed from a blank having a longitudinal length and a transverse width. The blank has a front panel with a display window, a first side panel, a back panel, a second side panel, and a display panel. The display panel has a central portion and a marginal portion that circumscribes the central portion. The marginal portion is at least partially defined by at least two spaced-apart transverse fold lines and at least two longitudinal edges extending between the fold lines. At least a portion of the display panel is positionable to face the display window in the carton formed from the blank. At least one strut is cut from the central portion of the display panel. Each strut comprises a base panel foldably connected to the display panel and an adhesive flap foldably connected to the base panel.
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FIELD OF THE INVENTION
The present invention relates generally to a drum type washing machine with balancing devices provided to a spin basket which rotates about a horizontal axis.
BACKGROUND OF THE INVENTION
A conventional drum type washing machine, which performs a washing/hydro-extracting (spin-drying) task with the rotation of its spin basket, has balancers that prevent the spin basket from producing abnormal vibrations due to laundry not being evenly arranged therein. There are two types of balancing devices: a counterweight balancer that reduces the vibration by means of a counterweight having a predetermined weight, and a liquid balancer which is provided on a washing machine's spin basket in order to oppose an imbalance of laundry and restrain the generation of vibration.
FIG. 7 schematically illustrates a conventional drum type washing machine with counterweights.
The drum washing machine includes a housing 1, a tub 2 held by suspension arms in the housing 1, and a spin basket 3 rotatably provided in the tub 2. An electric motor 8, installed below the tub 3, rotates the tub 3 about a shaft (not illustrated) horizontally installed, thereby performing a washing/hydro-extracting task. Counterweights 4a and 4b, each of predetermined weight, are attached to the tub 2 to prevent the production of vibration during the washing/hydro-extracting operation. The counterweight 4a attached to the front of the tub 2 is 11.4 kg, and the counterweight 4b provided to the top of the tub 2 is 12.2 kg. These counterweights 4a and 4b are made from cast iron and are joined to the tub 2 by bolts 4c.
The above-described conventional drum type washing machine has the following disadvantages:
First, the conventional balancer using the counterweights only lowers the amplitude of vibrations generated during operation rather than eliminating them entirely. Second, since these counterweights are quiet heavy, it is difficult to install them on the tub and the overall weight of the washing machine is increased, resulting in difficult construction and transport. Third, the bolts which fasten the counterweights to the tub, over long periods of use, loosen due to corrosion or fatigue, resulting in noise, and, in the worst case, the possibility of damage to the balancer and the washing machine as well.
To solve the aforementioned problems, a liquid balancer directly installed in a washing machine's spin basket was proposed in EP Publication No. EP 0 390 343 A2.
FIG. 8 depicts a conventional drum washing machine employing such a liquid balancer.
The drum washing machine of FIG. 8 includes a housing 1, a tub 2 held by suspension arms in the housing 1, an spin basket 3 rotatably installed within the tub 2, and an electric motor 8 installed below the tub 2 to rotate the spin basket 3. The tub 2 serves as a water tub, and the spin basket 3 is disposed within the tub 2 parallel to the ground rather than upright. One end 5a of a horizontally-supported shaft 5 is joined to the back of the spin basket 3. The other end 5b of the shaft 5 extends to the outside of the tub 2, and is connected to the motor 8 through a drive belt 6 so that the motor 8 can rotate the spin basket 3.
The washing operation of such a drum washing machine is carried out by suds created by the rotation of the spin basket 3. After the washing and rinsing of the clothes, excess water is removed from the clothes by centrifugal force created by the spin basket 3 turning at high speeds during the hydro-extracting process so that they contain only enough moisture for ironing.
A balancer is provided to the front of the spin basket 3 so as to prevent vibration from being produced during the high-speed rotation. The balancer is realized as an annular passageway 7 and a liquid, commonly a saline solution, of given quantity contained therein.
The center of gravity S-S' of the basket 3 is offset from the geometric center O-O' of the spin basket 3 due to the laundry being gathered on one spot in the spin basket 3. The liquid housed in the passageway 7 is moved to oppose an imbalance resulting from of the centrifugal force caused by that offset relationship.
In such a conventional drum washing machine, however, the liquid used to counteract the imbalance and decrease the vibration amplitude of the spin basket cannot eliminate the vibration completely. Consequently, the spin basket rotates eccentric relative to the center of gravity thereby creating abnormal vibrations, causing the washing machine's components such as bearings to wear out prematurely and the deterioration of the durability of the washing machine.
Additionally, when the magnitude of the spin basket's unbalance exceeds the critical point of counterbalance, the liquid balancer is incapable of dynamically balancing the spin basket. In order to compensate for such an imbalance sufficiently, the liquid balancer must be of great bulk. However, it is not easy to install such a heavy liquid balancer on the washing machine.
SUMMARY OF THE INVENTION
The present invention is a drum washing machine with improved balancing devices that can satisfy the aforementioned need.
It is an objective of the present invention to provide a drum type washing machine that can eliminate the vibration of its spin basket and prevent the spin basket's axis of rotation from deviating from its center of gravity.
It is another objective of the present invention to provide a drum type washing machine with balancing devices which can more effectively counteract an imbalance in its spin basket.
In order to obtain the aforementioned objectives of the present invention, the inventive drum type washing machine includes: a housing, a tub suspended horizontally within the housing, a spin basket rotatably mounted horizontally inside the tub, a motor rotating the spin basket, and balancing devices having radially spaced annular chambers provided to at least one of the two sides of the spin basket and a plurality of balls freely movable within the respective chambers which dynamically counterbalance imbalances produced during the rotation of the spin basket.
The chambers are concentrically formed and contain a given amount of liquid with a prescribed viscosity. The diameter of the balls in the inner chamber is smaller than that of the balls in the outer chamber, and the outer chamber's corners are less tightly curved than the inner chamber's corners. The chambers are formed by connecting the spin basket's side panel, which has a first annular groove formed therein, with a plate member, which has a second groove corresponding to the first groove. The plate member is joined to the side panel by the use of either bolts or rivets. The first and second grooves are designed to be substantially different from each other in axial depth, and the depth of one of the grooves is larger than the radius of the respective balls.
The chambers are respectively provided to both sides of the spin basket, and each chamber is connected to the outer circumference of the spin basket by bolts attached to the spin basket's outer surface. A third groove may be formed on a portion of the side panel of the spin basket corresponding to the first groove so as to accommodate the first groove of the first plate member.
BRIEF DESCRIPTION OF THE ATTACHED DRAWINGS
In the drawings:
FIG. 1 is a side-sectional view of a drum type washing machine with balancing devices using balls in accordance with the present invention;
FIGS. 2A and 2B are exploded and assembled views, respectively, depicting a chamber coupling structure in accordance with the first preferred embodiment of the present invention;
FIG. 3 depicts a chamber coupling structure in accordance with the second preferred embodiment of the present invention;
FIG. 4 depicts a chamber coupling structure in accordance with the third preferred embodiment of the present invention;
FIG. 5 depicts a chamber coupling structure in accordance with the fourth preferred embodiment of the present invention;
FIG. 6 depicts chambers each formed with a predetermined depth and having curved corners in accordance with the present invention;
FIG. 7 schematically illustrates a front perspective view of a convention drum type washing machine with counterweights for counteracting an imbalance in a spin basket; and
FIG. 8 depicts a vertical sectional view of a conventional drum type washing machine employing a liquid balancer.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings.
FIG. 1 is a side-sectional view of a drum washing machine with a balancing device using balls in accordance with the present invention.
The drum washing machine of FIG. 1 includes a housing 10, a tub 20 held in the housing 10, a spin basket 30 rotatably installed within the tub 20, and an electric motor 40, which rotates the spin basket 30, installed below the tub 20. The housing 10 is a quadrangular case, and the spin basket 20 is cylindrical in shape and horizontally held by four buffer springs 12 arranged at four locations in the housing 10. The spin basket 30, also of cylindrical shape, is horizontally disposed within the tub 20. Each of the buffer springs 12 has an upper end connected to the housing 10 and a lower end connected to the top of the tub 20. A pair of shock absorbers 13 are installed between the lower part of the tub 20 and the housing 10.
Openings 11, 21 and 32a are formed respectively on: the front of the housing 10, a predetermined spot of the tub 20 corresponding to that of the housing 10, and a corresponding spot of the spin basket 30. A door (not illustrated) is disposed on the front of the housing 10 that opens and closes the entrance to the tub 20 and the spin basket 30. The spin basket 30 consists of a cylindrically-shaped body 31, and side panels 32 and 33 each constituting the front and back of the body 31. A plurality of holes 31a are uniformly distributed in the body 31 so that water can flow freely between the spin basket 30 and the tub 20. A plurality of lifters 31b are provided to the body 31 and designed to protrude inward in the form of a "V", spaced 60° from each other. These lifters 31b raise and drop laundry during washing. A horizontally-supported shaft 41 has one end 41a connected to the side panel 33 that forms the back of the spin basket 30, and the other end 41b extending to the rear of the tub 20 and connected to a first pulley 42. A belt 44 is provided between the first pulley 42 and a second pulley 43 that is connected to the motor shaft 40a so that the rotating force of the motor 40 is transmitted to the spin basket 30.
As described above, the shaft 41 is horizontally supported by a pair of bearings 46a and 46b placed in a bearing housing 45. A supporting member 47 has an outer end diverged in three directions and extends to the side panel 33's edge to be joined to the side panel 33 of the spin basket 30 so that the one end 41a of the shaft 41 is connected to the center of the supporting member 47.
The spin basket 30 includes a pair of balancing devices 50 provided to respective side panels 32 and 33 so as to remove the vibration and imbalance created during rotation. The balancing devices 50 are oppositely disposed respectively to each other thereby offsetting movement created during rotation and enhancing the balancing characteristics. Each of balancing devices 50 comprises annular chambers 51a and 51b that are formed on radially inner and outer parts of each of the side panels 32 and 33, and spherically balls 52a and 52b that are seated in the chambers 51a and 51b, respectively. The balls move along the corresponding chambers to oppose an imbalance in the spin basket 30. A secondary plate member 53 closes the chambers 51a, 51b (as will be described in more detail subsequently). The plate members in FIG. 1 are secured to respective side panels 32, 33 by means of bolts 60 which extend completely through the spin basket. Each bolt includes a head 62 at one end, and a coupling nut 61 is threaded to the other end of each bolt 60.
The chambers 51a and 51b contain a liquid of a predetermined viscosity, such as an oil, in order to facilitate the movement of the balls 52a and 52b and to enhance the balancing characteristics. In other words, when there is an imbalance in the spin basket 30, the balls 52a and 52b and the liquid relocate to a predetermined position to oppose the imbalance. If the magnitude of the imbalance does not exceed a predetermined critical point of counterbalance of the balancing devices, the balls 52a and 52b move close to each other to make the vibration amplitude zero so the liquid does not flow.
If the magnitude of the imbalance still exceeds the critical point of counterbalance, after the balls have moved into their counterbalancing position, the liquid is then also moved to oppose the imbalance, thereby countering the unbalanced state of the basket 30.
Each of the balancing devices 50 includes at least one chamber and a plurality of the balls seated therein. The inner and outer chambers 51a and 51b are concentric to the axis of rotation and radially spaced from each other by a predetermined distance. They are sealed by means to be subsequently described. The balls 52a in the inner chambers 51a are designed to be smaller than the balls 52b in the outer chambers 51b so that there is a difference between the balancing effects of the inner and outer chambers 51a and 51b to thereby ensuring a more delicate counterbalancing action.
The balancing effect is in proportion to the centrifugal force (F=MRW 2 ), and the control effect of the radially inner balancing device is designed to be smaller than that of the outer one by reducing the mass of the balls 52a seated in the inner chambers 51a so that the overall control technique is more sophisticated.
The coupling structure of the chambers 51a and 51b will be more fully described as follows.
As described above, the balancing devices 50 provided to the both side panels 32 and 33 are formed symmetrically, and the structure of the chambers 51a and 51b on the side panel 32 will be described by way of example. The inner chambers 51a and the outer chambers 51b of different size have essentially the same construction, and the inner chambers 51a are now described as an example.
FIGS. 2A and 2B are enlarged views of an alternative coupling structure of the chambers 51a and 51b.
Each of the chambers 51a, 51b is formed by the combination of a first groove 32b formed axially inward on the side panel 32 of the spin basket 30 and a second groove 53a formed in axial alignment with to the first groove 32b. More specifically, the second groove 53a is formed on a secondary plate member 53, and the plate member 53 is joined to the side panel 32 of the spin basket 30 by the use of small bolts 70. Nuts 72 are then screw onto the bolts whose bolt heads 71 are axially facing the inside of the spin basket 30. The panel 32 (and also 33) includes three bent portions 32c arranged to straddle both of the chambers 51a, 51b. Those bent portions form projections which oppose respective recesses formed by bent portions 53b of the plate member 53. Packing material 90 is inserted between the bent portions 32c and 53b and compressed to form a seal so as to eliminate leakage of the oil from the chambers 51a, 51b.
FIG. 3 depicts a chamber coupling structure in accordance with a second preferred embodiment of the present invention.
In this embodiment, the plate member 53 is joined to the side panel 32 of the spin basket 30 by the use of rivets 80. The rivets 80 are pressed from the outside of the spin basket 30 to fasten the panel 32 and side panel 32 together.
FIG. 4 depicts a chamber coupling structure in accordance with a third preferred embodiment of the present invention.
In this embodiment, the plate member 53 is joined to the side panel 32 of the spin basket 30 by welding.
FIG. 5 depicts a chamber coupling structure in accordance with a fourth preferred embodiment of the present invention.
A radially inner 151a is formed by the combination of a first plate member 54 with a first annular groove 54a formed inward thereon and a second plate member 55 with a second annular groove 55a formed outward thereon corresponding in location to the first groove 54a. A radially outer chamber 151b is also formed by the plate members 54, 55. The first plate member 54 is connected to the second plate member 55 by welding, and a bolt 60 disposed closely to the outer surface of a lifter 31b is used to fasten the members 54 and 55 to the side panel 32. The bolt 60 is similar to that disclosed earlier in connection with FIG. 1.
Accordingly, the parts where the members 54 and 55 are joined together by welding are not exposed to the inside of the spin basket 30, thereby eliminating corrosion and oxidization on those joints, and making the inside of the spin basket 30 smooth. The bolt 60 extends along the outer surface of the lifter 31b, and its bolt head 62 (see FIG. 1) abuts against the outside of the balancing device 50 located at the axial rear. A nut 61 screws onto the bolt 60 in front of the axial other balancing device 50 placed on the front so that the front and rear balancing devices 50 are joined together, with the spin basket 30 disposed therebetween. The bolt 60 is situated radially between the radially inner chamber 151a and the radially outer chamber 151b.
To create the inner chamber 115a, a third groove 32d is formed on a portion of the side panel 32 corresponding in location to the first groove 54a of the first plate member 54 in order to accommodate the first groove 54a, and the combination of the first and second plate members 54 and 55 is designed to lie flush with the side panel 32.
Referring now to FIG. 6, another chamber structure is fully described as follows.
The contact points (i.e., the interface) between the plate member 253 and the side panel 232, which form the chambers 251a and 251b, do not lie in the plane created by the centers of the balls 52a and 52b. This is so because the depth h 2 of the axial inner groove 232b' is different from the depth h 1 of the axial outer groove 253a', allowing the balls 52a and 52b to freely move along the chambers. In other words, the first groove 232b' and the second groove 253a' are designed to respectively have different depths h 2 and h 1 , and the depth h 1 of the second groove 253a' is larger than each radius "r" of the balls 52a. Also, the depth h 1 of the second groove 253a is larger than 1/2 of the overall depth "h" of the chamber 251a. The above-described relationship between the groove depths and ball radii pertaining to the chamber 251a is also true of the corresponding relationships pertaining to the other chamber 251b.
Each corner of the radially inner chamber 251a and radially outer chamber 251b is designed to be rounded to form curved portions R 1 and R 2 . The curvature of the curved portion R 1 is different from that of the curved portion R 2 so that the balls 52a and 52b move along the respective inner and outer chambers 251a and 251b at the same speed. In other words, should the difference in curvature not exist, the relatively small and light ball 52a would move through the inner chamber 251a faster than the ball 52b in the outer chamber 251b. The curved portions R 1 of the inner chamber 251a being more tightly curved than those of the outer chamber 251b ensures that the balls 52a and 52b move along the corresponding inner and outer chambers 251a and 251b at the same speed.
The following description relates to the operation of the drum washing machine with the inventive balancing devices.
The washing machine removes soil from the garments by agitation accomplished by the spin basket 30 during washing. During the hydro-extracting (spin-drying) action of the washing process, the garments are located on the lower part of the spin basket 30. If the spin basket 30 becomes unbalanced as it rotates at high speeds, the centrifugal force of the spin basket 30 moves the balls 52a and 52b along the chambers 51a and 51b (or 151a and 151b, or 251a and 251b) to a position which will rebalance the basket 30, thereby eliminating vibrations and eccentric rotation of the spin basket 30.
More specifically, once there is an imbalance in the spin basket 30, movable bodies consisting of the balls 51a and 51b and liquid become situated on the opposite side of the imbalance. When the magnitude of the imbalance remains below a critical point of counterbalance of the balls, the balls 51a and 51b move close to each other to eliminate the vibration (i.e. to make the center of gravity and center of rotation of the spin basket 30 the same). As the vibration amplitude becomes zero, the flow of the liquid within the chambers is minimal. If the magnitude of the imbalance still exceeds the critical point of counterbalance, after the balls have moved into their counterbalancing position, the liquid is then also moved to oppose the imbalance, thereby countering the unbalanced state of the basket 30.
As described above, the balls of the present invention make the vibration amplitude zero and counteract an imbalance in the spin basket to thereby eliminate resultant deformation of the spin basket. The inventive balancing devices may prevent unnecessary wear of the components used to support the rotation of the spin basket and noise created by friction. The balancing devices employ the balls and liquid at the same time, and have superior balancing characteristics with reduced bulk. The chambers of the balancing devices are easily formed by bolts and nuts or by welding, and the parts where the plate member and the side panel join together by welding are not exposed to the inside of the spin basket thereby preventing corrosion and oxidization of those joints. Additionally, the interface formed by chamber-forming plates is not aligned with the center of each ball so that the balls are freely movable in the chambers.
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A front loading clothes washing machine includes a spin basket rotatably driven about a horizontal axis. Axially spaced front and rear sides of the spin basket are formed by panels. Disposed on each of the front and rear panels is a dynamic balancing mechanism comprised of an annular chamber arranged coaxially with the axis of rotation. The chamber contains a liquid and a plurality of balls freely movable within the liquid.
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RELATED APPLICATION
[0001] This is a continuation-in-part of application Ser. No. 09/223,666, filed Dec. 30, 1998, entitled MODULAR STRUCTURAL MEMBERS FOR CONSTRUCTING BUILDINGS AND BUILDINGS CONSTRUCTED OF SUCH MEMBERS now ______.
BACKGROUND OF THE INVENTION
[0002] A. Field of the Invention
[0003] This invention relates to the art of constructing buildings, especially relatively small and low cost residential, institutional and commercial buildings, utilizing modular prefabricated structural members therefor. More specifically, this application pertains to a novel apparatus and method for prefabricating the structural members.
[0004] B. Background of the Invention
[0005] Small buildings today are constructed using methods developed before the Industrial Revolution. These types of buildings, as opposed to steel frame building types, are constructed either by cutting up trees into boards of different sizes and nailing the boards together or by erecting stacks of stone or masonry held together with mortar. Historically, such raw materials have been delivered to the construction sites where they are then made into buildings by the process of assembling the cut-up parts of the trees and/or the blocks of stone or masonry into simple “post and beam” type structures the parts of which work independently of one another.
[0006] Heretofore, it has been attempted, with a good deal of progress having been made in the more recent past, to achieve factory production of buildings in various forms of modular, panelized and mobile home unit construction, but these never were and still do not represent and embody new technologies; they are simply examples of the same historical “post and beam” technology executed indoors-off-site instead of outdoors-on-site. However, although some cost savings may have been achieved through the use of modern techniques such as bulk raw material purchasing and through the utilization of newer and faster tools, the final products have not only remained basically the same but, because labor and materials are still being used inefficiently, are vulnerable to damage and destruction by fire, hurricanes, earthquakes, moisture and insects.
[0007] Building codes, which in the United States serve as minimum standards of construction quality, actually tend to exacerbate these inefficiencies by trying to mandate better quality and greater safety of buildings while anticipating the mediocre labor skills currently found on construction sites. Architects and engineers tend to design buildings in light of the government-specified parameters and then follow up by specifying the use of the already available construction materials and methods. This not only reinforces the use of existing methods but also inhibits innovation in building construction. The construction industry tolerates these disadvantages because a better way has not yet been found and perfected.
[0008] The availability and price of lumber have changed drastically over the past decade or so, with availability decreasing and price increasing. The deleterious results of indiscriminate tree cutting are giving rise to alarm over the ecological consequences of global deforestation and have led to great pressure, primarily from environmental groups around the world, on forest products companies and governments to control and slow down such activity. As a consequence, lumber has become increasingly more expensive as distances from source to destination increase transportation costs. Furthermore, skilled craftsmen such as carpenters and masons currently command very high salaries and, even worse, are neither as abundant nor as skilled as they once were. In sum, therefore, small buildings being currently constructed make inefficient use of raw materials, cost more to build, operate and maintain than is necessary, are highly combustible, and are expensive to reinforce to mitigate the threats of fire, earthquakes, hurricanes and floods.
OBJECTIVES AND SUMMARY OF THE INVENTION
[0009] An objective of the present invention is to provide a fixture that can be used to assemble a modular type structural member quickly and effectively.
[0010] A further objective is to provide a fixture which may be easily adapted to assemble or prefabricate modular structural members of various sizes and shades.
[0011] A further objectives and advantages is to provide a fixture which can assemble a structural member automatically.
[0012] In the above-mentioned co-pending application Ser. No. 09/223,666 a class of novel prefabricated hollow shell-type modular structural members is described, each of which members includes a triangulated wire core disposed between and secured to a pair of spaced shell panels defining the faces of the structural member, and which members are adapted, in appropriate forms and strengths, for serving as foundations, walls, floors, roofs and partitions of low cost, relatively small buildings. The modular structural members which, in their manufactured form, are adapted to be easily assembled and interconnected at the construction site so as to define both the structural configuration of the building (including its doors, windows and surface finishes) as well as the infrastructure for its life support systems (including its plumbing systems, electrical systems, heating, ventilation and air conditioning systems, fire protection systems, etc.) as the building is being erected.
[0013] A plurality of such modular structural members can be used per se either to form a complete self-contained building or to form a part of or an adjunct to an existing building for purposes of renovation and/or expansion, and which can also be used in conjunction with conventional building materials (steel, concrete and wood) to form composite building structures.
[0014] Generally speaking, the fundamental concept of the modular structure which is incorporated in the modular structural members disclosed herein and which may be briefly described as follows.
[0015] The strength of any structure results from a combination of the materials of which it is made and the shape or geometry of those materials. Stated in other words, strength is a function not only of the physical properties of the materials which are used but also of the manner in which they are used, i.e., of their geometric configurations.
[0016] A force applied to the top apex of a triangular structure will channel down the two sides of the triangle to the two points or apexes at the bottom. The two points at the bottom of the triangular structure will tend to be pushed outward by that force, i.e., away from each other, unless they are restrained and held in place. It is the bottom member of the triangular structure, of course, which holds those two points in place. This is an efficient system because (1) each member is in either simple tension or simple compression as the force imposed at the top of the triangular structure is resisted by the three members and as the load is transferred to the associated supports, and (2) the connections of the three members can be simple because they do not have to be strong enough to resist turning or bending.
[0017] It will also be understood that if several triangular structures are grouped together, the force applied thereto will be distributed throughout an appropriately larger number of members. For example, if a four-sided pyramidal arrangement of triangular structures is used instead of a single triangular structure, the applied force is distributed between eight members instead of three. Such an arrangement obviously increases the efficiency of the system.
[0018] It will further be understood that multiple pyramidal arrangements of triangular structures can be interconnected with each other horizontally and vertically as well. In such a system, as the number of connected pyramidal arrangements of triangular structures increases, the forces applied thereto in one area are distributed over a large network of members. Moreover, the individual members need not be very strong, since they work together. Thus, a large number of small members can coact to carry large loads, and by using the same size member repeatedly, a very large structure can be constructed.
[0019] In practical applications, the tops and bottoms of such triangular structures either per se or in pyramidal arrangements thereof can be individual members or they can be extensive flat plates. If they are plates, then they can form the solid faces of walls, floors, ceilings and roofs required to enclose building structures and their interior spaces. The plates transmit pressure loads applied to the surfaces of these plates to the network of frame members, in addition to resisting the forces in the top and bottom chords of the pyramids.
[0020] By applying the efficiencies of these principles to an entire structure, a building constituted by modular structural members according to the present invention can be made to be much stronger than one constructed by conventional methods. For small to medium-size buildings, the forces at the connections between the modular structural members will be small, which will permit simple connections. Using concrete as a covering for the shell panels of the structural members will result in buildings which will not burn.
[0021] For the purposes of clarity, by way of definition a building constructed of modular structural members according to the present invention may be considered as consisting of “components”, “elements” and “cells”. The components are the general working units or building blocks of the desired end product and are used for forming the foundation of the building structure as well as the walls, the floors, the roof and the interior partitions thereof. They are made in large sizes of up to 40 feet by 12.5 feet (12.2 m by 3.8 m) and in thicknesses from 4.5 inches to 1.5 feet (11.4 cm to 45.7 cm). The “elements” are smaller parts of a building including items such as windows, doors, cabinets, closets, and stairs. The “cells” are full building volumes which are prefabricated assemblies of components and elements such as entry foyers, bathrooms, and kitchens. In a building structure of the present invention, the components and cells are uniquely interconnected.
[0022] The components, elements and cells are designed to enable various materials to work together synergetically to perform the various functions required of the building. The technology underlying and incorporated in the system of the present invention facilitates both low volume manual and high volume automated manufacturing applications.
[0023] The components, i.e., the various modular structural members, are preferably fabricated from the same basic materials and by the same techniques. Each component has a block-like form which consists of two spaced parallel shell panels defining the sides and faces of the block and of an inner portion or core between the shell panels. In all components, the core between the associated two shell panels basically consists of a triangulated wire frame to which the shell panels are secured. To the extent there are any differences between some of the components, these differences are in the structural strengths, the architectural design details, and the thermal performance properties of the components.
[0024] The structural strength of each component varies by virtue of differences in the triangulation, the thickness, and the nature and strength of the material of which the “wire” of the wire frame is made (the material used for the “wire” may be steel, structural plastic, or any other comparable linear material); the material strength of the shell panels; and the depth or thickness of the component. The wire frame consists of zig-zag shaped wire “trusses” placed next to each other in the space between the shell panels and having their tips or apexes connected. The arrangement in particular is such that in each group of three adjacent wire trusses, the middle one thereof has its bottom apexes connected to the bottom apexes of the wire truss located on one side of the middle wire truss and has its top apexes connected to the top apexes of the wire truss located on the other side of the middle wire truss.
[0025] In addition, at each of the inside faces of the shell panels bounding the core-accommodating space therebetween, there are provided a set of mutually parallel first wire cables or chord members each of which extends along and is connected to the apexes of a respective one of the wire trusses in a direction parallel to the longitudinal axis of the wire core, and a set of likewise mutually parallel second wire cables or chord members each of which extends perpendicular to the first chord members and is connected thereto at irs intersections with the first chord members and the respective apexes of the various wire trusses. A plurality of anchors located at those intersections connect the chord members and the apexes of the wire trusses to the shell panels.
[0026] The shell panels can be made from a variety of materials including concrete, metal, combinations thereof, or other rigid panel material. The most typical is a layer of concrete into which the anchors are embedded. The concrete layer, which is about 2 inches (5.1 cm) thick, may be reinforced with plastic fibers and may additionally be reduced in weight by being transformed into cellular concrete through the incorporation therein of many small air bubbles or a cellular plastic foam. The shell casting material may vary in strength from 150 to 4,000 pounds per square inch (psi) in density from 30 to 120 pounds per cubic foot, as well as in insulating properties. These different shell panel characteristics result from variations in the proportions of the ingredients of the shell mixture that includes cement, sand, reinforcing fibers, and cellular foam. The shell panels are formed to provide the final exposed finish and texture thereof and, in conjunction with the wire frame core, to impart to the modular structural members the required structural load-bearing capacity.
[0027] For certain conditions, a metal shellpan may be embedded in the concrete shell panel. The shellpan is designed to provide additional strength, so as to enable the component to accommodate ducts or conduit for electrical wiring or to accommodate reinforcements for openings, holes to receive fasteners at the positions of various life support system parts, etc.
[0028] The thickness or diameter of the wire used to form the wire trusses varies from ⅛ inch (0.32 cm) to ½ inch (1.3 cm), and its strength varies further according to the strength of the material from which the wire is made. Moreover, as already pointed out, the apexes of the wire truss triangles are fastened to the perpendicularly intersecting first and second chord members and jointly therewith to the shell panels (and, where applicable, to the shellpans as well). The completed wire frame thus is a deep, three dimensional, open “mesh” consisting of interconnected triangulated shapes formed by small diameter lightweight wire. As a result, the shell panels and the wire frame members all work together to transfer and resist the forces acting on the various components.
[0029] The overall depth or thickness of the structural members will vary from 4½ inches (11.4 cm) in the case of a partition-forming component to 16 inches (40.6 cm) in the case of a large floor-forming component. Typically, as the depth increases, the wire size or thickness of the wire trusses will also increase. The greater depth, of course, increases the capacity of the structural member to resist loads perpendicular to its face (e.g., wind load for walls, floor load for floors, snow load for roofs).
[0030] Each modular structural member according to the present invention, therefore, becomes a complete, structurally integral unit. A wall-forming structural member or component actually performs structurally as a large beam (the height of a wall). Tension loads (pulling up on walls) thus are resisted by the entire length of the wall since, the stress from any one point is to be distributed throughout the entire wall-forming component by the interior wire frame. Correspondingly, a floor-forming component acts as a two way-slab spanning up to approximately 24 feet (7.3 m). As such, they are less vulnerable than conventional structures to failure when a section of continuous support is lost, such as due to foundation failure. The substantial portion of structural material is positioned on the outer faces of the component where the greatest efficiency can be attained in all conditions, including the most demanding ones.
[0031] In a finished building, furthermore, where the components are connected, the floor-forming components are connected to and supported by the wall-forming components in a way that is different from typical comparable structures. Floors of most conventional structures are supported on beams or joists which themselves are simply supported at their ends by the walls. While the walls do their job supporting the floor load which is brought to them by the floor, they do not help the floor in its job of supporting the weight of the floor load. The floor-forming components in a building according to the present invention are connected to the wall-forming components in a way that enables the walls to help the floor carry its load. The top and bottom shell panels of the floor-forming components are connected to the wall-forming components in a fashion establishing a moment connection between them.
[0032] More particularly, in the system of the present invention, at the regions of the floor-to-wall connections the triangulation of the wire trusses, i.e., the spacing of adjacent wire trusses from each other as well as the spacing of adjacent apexes thereof from each other, in the wall-forming components is more compact, which makes the connections stronger and helps the floor-forming component resist its tendency to bend under the load. Each such floor-to-wall connection is continuous along the entire perimeter of the floor-forming component. This substantially increases the load-bearing capacity of the floor-forming components as well as the wind load-bearing capacity of the wall-forming components. For example, engineering calculations indicate that the load-bearing capacity of an 18.8 square foot floor-forming component increases from 60 to 90 pounds per square foot by this connection method.
[0033] Furthermore, this changes the nature of the entire assembled structure. Instead of the building being an assembly of independent pieces (studs, joists, or blocks), it becomes a complete whole structural element. This provides excellent resistance to earthquakes, hurricanes and floods.
[0034] Advantageously, the structural member is assembled or prefabricated on a fixture formed of a plurality of posts. The posts have a holder at one end adapted to hold the several chords and other members defining a joint. At the opposite end, the posts are mounted on a structure including post rails which may be movable on rail guides. The post rails are used to move the posts and the chords attached thereto to a coupling member such as a welding gun. The coupling member permanently couples or secures the chords together to form the respective joints.
[0035] The posts can be formed into a three dimensional lattice defining the dimensions of the structural member. A plurality of guns may be provided to weld several joints simultaneously. In an advantageous arrangement the rail posts move toward the guns and the guns are activated when respective sensors detect the holders with the chords. In this manner the process, or at least the welding of the chords together is easily automated.
BRIEF DESCRIPTION OF THE DRAWINGS
[0036] The foregoing and other objects, characteristics and advantages of the present invention will be more clearly understood from the following detailed description when read in conjunction with the accompanying drawings, in which:
[0037] [0037]FIG. 1 is a schematic illustration, in perspective, of a section of a building structure according to the present invention and shows a group of modular structural members constituting two wall components, a floor component and two roof components, the various components being shown in the form of their triangulated wire cores only and without their associated shell panels;
[0038] [0038]FIG. 2 is a perspective illustration, on a somewhat enlarged scale, of the floor component, without its shell panels, constituting a part of the building structure shown in FIG. 1;
[0039] [0039]FIG. 3 is an elevational illustration, in perspective and on a reduced scale, of one of the wall components, without its shell panels, constituting a part of the building structure shown in FIG. 1, the wall component being illustrated as provided with vertically spaced horizontal compacted regions of its triangulated wire core designed for supporting respective floor components;
[0040] [0040]FIG. 3A is a schematic side edge view of the triangulated wire core structure of the wall component shown in FIG. 3;
[0041] [0041]FIG. 4 is a diagrammatic illustration of a first stage of the formation of the triangulated wire core of a modular structural member according to the present invention, this view showing the positioning of the first zig-zag shaped wire truss for the core of the structural member;
[0042] [0042]FIG. 5 is a diagrammatic illustration of the second stage of the formation of the triangulated wire core of a modular structural member according to the present invention, this view showing the positioning of the second zig-zag shaped wire truss relative to the first wire truss;
[0043] [0043]FIG. 6 is a diagrammatic illustration of the third stage of the formation of the triangulated wire core of a modular structural member according to the present invention, this view showing the positioning of a third zig-zag shaped wire truss for relative to the second wire truss;
[0044] [0044]FIG. 7 is a schematic sectional representation of a layer of cellular concrete used as a part of the shell panel of a modular structural member according to the present invention and illustrates the provision of collapsed air cells in the layer of concrete adjacent the outer surface of the shell panel;
[0045] [0045]FIG. 8 is a schematic cross-sectional view of a modular structural member according to the present invention and illustrates the same as constituted of two separate shell panels spaced from but connected to each other by a triangulated wire core;
[0046] [0046]FIG. 9 is an enlarged representation of a section of the structural member shown in FIG. 8 and illustrates certain details thereof;
[0047] [0047]FIG. 10 is a vertical section taken through a part of a building structure according to the present invention constituted of a vertical wall or partition component extending between and connected at its top and bottom edges to two associated vertically spaced floor/ceiling components, the section being taken along a plane located in front of a duct riser incorporated in the wall or partition component;
[0048] [0048]FIG. 11 is a sectional view similar to FIG. 10 but with the section being taken along a plane located axially of the duct riser incorporated in the wall or partition component;
[0049] [0049]FIG. 12 is an enlarged horizontal section through the connection region between the abutting vertical side edges of two horizontally aligned wall components and illustrates the interfitted male and female connector members of the joint (these are the same as the ones shown in FIGS. 10 and 11) prior to the activation and expansion of the male connector member of the joint;
[0050] [0050]FIG. 13 is a view similar to FIG. 12 but illustrates the male connector member of the joint after its activation and expansion in the female connector member of the joint;
[0051] [0051]FIG. 14 is an enlarged perspective illustration of a channel-shaped female connector member constituting a part of the joint shown in FIGS. 12 and 13; and
[0052] [0052]FIG. 15 is an enlarged perspective illustration of the activated and expanded male connector member of the joint shown in FIGS. 12 and 13;
[0053] FIGS. 16 - 18 show how the chords are assembled with an anchor to form joints for the structural member;
[0054] FIGS. 19 shows an orthogonal view of a post terminating in holder;
[0055] FIGS. 20 - 24 show how the chords interact with the holder of FIG. 19 to form the joints;
[0056] [0056]FIG. 25 shows an orthogonal view of the fixture without the chords;
[0057] [0057]FIG. 26 shows a top view of the fixture of FIG. 25;
[0058] [0058]FIG. 27 shows an orthogonal view of the fixture with the chords in place and before the chords are welded; and
[0059] [0059]FIG. 28 shows a plan view of the fixture with chords in FIG. 27.
DETAILED DESCRIPTION OF THE INVENTION
[0060] The structural members and building structures made from these members are first described. Referring now to the drawings in greater detail, a section of a gabled-roof building structure 20 is shown in FIG. 1 as being constructed of a multiplicity of modular structural members according to the present invention (obviously only a small number of them are shown) which constitute wall components 22 , floor components 24 (see also FIG. 2), and roof components 26 of the building structure. Although only arrangements of triangulated wires are shown in these views, each of the various structural members 22 , 24 and 26 actually has the form of a block composed, as shown in FIGS. 8 and 9, of a pair of shell panels 28 and 30 separated from one another by a space 31 and connected to one another by an intermediate triangulated wire core 32 located in the space 31 . The shell panels have been omitted from FIGS. 1 and 2 for the sake of simplicity. For ease of identification, furthermore, the shell panels 28 and 30 are hereinafter occasionally referred to as the interior shell and the exterior shell, respectively.
[0061] In the preferred embodiment of the invention, the shell panels 28 and 30 have the form of respective layers 28 a and 30 a of concrete. If deemed advisable for a particular type of building structure, a respective metal reinforcing plate or shellpan (not shown) may be embedded in each layer of concrete over substantially its entire expanse for enhancing the strength and fire resistance of the shell panels 28 and 30 individually and thereby of the structural members 22 , 24 and 26 composed thereof as well. Alternatively, however, the shell panels may be made of metal or other sufficiently strong and fire-resistant materials. In the illustrated embodiment, furthermore, certain adjuncts of the triangulated wire core 32 , shown in FIG. 9 and more fully described hereinafter, are also embedded in the layers of concrete and constitute means by which the shell panels 28 and 30 and their associated wire core are connected to each other. In the illustrated embodiment, furthermore (see FIG. 9), the outer face 28 b of the interior shell 28 is that face thereof which in use is directed toward and defines the boundary wall surface of the associated enclosed building space, while the outer face 30 b of the exterior shell 30 is that face thereof which in use is directed away from the enclosed building space. The inner faces 28 c and 30 c of the interior and exterior shells of a building component are, of course, those faces of the shells which are directed toward each other and between which the space 31 and the triangulated wire core 32 are located.
[0062] Referring now to FIGS. 4, 5 and 6 , according to the present invention the triangulated wire core 32 of the basic structural members 22 , 24 or 26 consists, as previously indicated, of a plurality of zig-zag shaped wire elements or “trusses” 34 placed next to each other across the width of the structural member, with their tips or apexes interconnected. To prepare such a core, a group of mutually parallel first wire cables or chord members, designated 32 a in FIG. 9, are laid out in a suitable jig or fixture (not shown) so as to extend in a direction parallel to the intended longitudinal axis of the wire core, and a group of mutually parallel second wire cables or chord members, designated 32 b in FIG. 9, are laid out in the same fixture crosswise over the first chord members.
[0063] A first zig-zag wire truss 34 a (FIG. 4) is then arranged along a first one of the longitudinal wire chord members 32 a in a substantially upright position in a plane which is slightly inclined relative to the vertical plane of the first longitudinal chord member in a direction away from the next adjacent longitudinal chord member, with the bottom vertices or apexes of the first wire truss 34 a located at respective intersections of the first longitudinal chord member with the cross chord members. A second zig-zag wire truss 34 b (see FIG. 5) is then placed next to the first wire truss is 34 a, with the bottom vertices of the second truss being located at the same intersections between the underlying longitudinal and cross chord members 32 a and 32 b as the bottom vertices of the first truss and with all those elements at each intersection being connected to each other by means of suitable anchor members. Thereafter, a third zig-zag wire truss 34 c (see FIG. 6) is placed next to the second wire truss, with the bottom vertices of the third truss being located away from the bottom vertices of the second truss and along a separate longitudinal chord member 32 a but with the top vertices or apexes of the third truss 34 c being located adjacent to the top vertices of the second truss.
[0064] The procedure is then continued as needed in the same fashion as described so far, until a core structure 32 of the desired length and width has been built up. It will be understood that care must be taken to ensure that in any group of three directly adjacent wire trusses across the width of the core structure, the middle one of those wire trusses has its bottom apexes connected only to the bottom apexes of the wire truss located on one side of the middle wire truss and has its top apexes connected only to the top apexes of the wire truss located on the other side of the middle wire truss. At that stage, an additional group of longitudinal chord members 32 d and an additional group of cross chord members 32 e are put in place on top of the assembled wire trusses, with the intersections of those chord members being positioned over the top apexes of the wire trusses, and the top apexes of the wire trusses together with the underlying intersecting longitudinal and cross chord members are connected to each other by respective sets of anchor members 32 f . Where the structural member is to include a shellpan within each of the concrete shell panels, it is further contemplated that the shellpans will be positioned across the entire expanse of the wire core structure at both faces thereof and hence in contact with the apexes of the wire trusses, for enabling the shellpans to be welded to the wire trusses and to the intersections of the longitudinal and cross chord members.
[0065] Attention is called to the fact that, although the arrangement of the zig-zag shaped wire trusses in a triangulated wire core for a modular structural member according to the present invention is normally uniform over the entire expanse of such member, that arrangement is modified somewhat, as shown in FIGS. 3 and 3A, in the case of the floor-to-wall connection region of a wall-forming component. For that situation, each wall-forming component 22 is provided with a more compact distribution of the wire trusses 34 at each level 22 a, 22 b, etc., where it is to be connected to a floor-forming component 24 . The narrower spacing of the adjacent wire trusses from each other and the narrower spacing of the adjacent apexes of each wire truss from each other, both of which are clearly visible in FIG. 3A, in conjunction with the fact that each floor-to-wall connection is continuous along the entire perimeter of the floor-forming component, ensures that the connections are stronger and helps the floor-forming component resist its tendency to bend under the load. This substantially increases the load-bearing capacity of the floor-forming components as well as the wind load-bearing capacity of the wall-forming components.
[0066] Reverting now to the assembly of the structural member, once the wire core structure 32 is complete, the opposite face regions of the core structure are introduced into a mold (this may be effected either simultaneously or sequentially, depending on the type of equipment available and on existing production requirements) which has the desired contours of the two shell panels 28 and 30 . Concrete, preferably admixed with air bubbles or a cellular plastic foam, is then poured into the mold and permitted to set so as to form the layers 28 a and 28 b with the grids of longitudinal and cross chord members 32 a - 32 b and 32 d - 32 e and the sets of anchors 32 c and 32 f embedded in the concrete and held firmly in place.
[0067] It should be noted at this point that the durability and the water resistance of the structural members or components 22 , 24 and 24 will be primarily a function of the surface density of the concrete utilized in the shell panels 28 and 30 . Durability, strength and water resistance of concrete advantageously increase with density, yet thermal values, fire performance characteristics, weight and cost decrease with higher densities. To take advantage of this property of the concrete, vibrations can be applied at the surface region 36 of the shell mixture (see FIG. 7) where the forms are in contact with the mixture, which results in a collapse of the air cells at that surface region while the air cells in the region 38 away from that surface remain fully expanded. Vibrations can also be transmitted into the mixture through the steel wire core structure to increase the density of the concrete at the juncture between the metal and the concrete. In this way, a density of the concrete which is in general correct for a particular component or structural load can be maintained without increasing it to address a surface requirement. This is especially useful for floor components and for the exterior faces of outside wall and roof components.
[0068] In this regard, it is well known that whereas rain and snow are one source of water problems for buildings, another one is condensation. The transmission of cold to the warm side of standard (non-cellular) concrete causes condensation to form on the warm side. Cellular concrete has thermal characteristics which are superior to standard concrete and, therefore, it assists in resisting the formation of moisture on the insides of wall and roof components. Experience with buildings indicates, however, that even when proper steps have been taken to resist water penetration, provision must nonetheless still be made for the escape of moisture which may accumulate. To this end it is contemplated by the present invention to design the shellpans incorporated in the concrete shell panels so as to include channels for directing moisture to holes through which it can escape.
[0069] It should also be noted that even though the basic structure of the wall, floor and roof components of the present invention is the same, there will nevertheless be some differences between certain ones of such components in terms of their structural strengths, architectural design details, and thermal performance. For example, it may be deemed advisable to provide an outside wall component or a roof component of a building structure with a thermal insulation material 35 (see FIG. 9) within the space 31 between the shell panels 28 and 30 occupied by the triangulated wire core. On the other hand, an inside wall component or a floor component of the building structure may not require as much insulation or, for that matter, may not require any insulation at all.
[0070] A practical example of an interconnection of a partition (inside wall) component between a ceiling and a floor is illustrated by FIGS. 10 and 11. As there shown, the partition component 40 is a block-shaped structure composed of a pair of spaced parallel concrete shell panels 42 and 44 which are connected to each other by a triangulated wire core 46 disposed in the space between the shell panels. Set into the molded concrete top and bottom edges 40 a and 40 b of the partition component are respective upwardly and down-wardly open identical female connector channels 50 of the type shown in FIG. 14, the function of which will be more fully explained presently. Above the top edge 40 a of the partition component there is located a downwardly projecting molded concrete ceiling ledge or molding 52 which has a bottom edge 52 a aligned with the top edge 40 a of the partition component 40 and supporting a molded-in downwardly open female connector channel 50 identical to the one in the partition component. The ceiling ledge 52 is shown as depending from a ceiling component 54 which could be either an adjunct of a roof component (not shown) or an adjunct of an upper floor component (not shown).
[0071] Correspondingly, located below the bottom edge 40 b of the partition component 40 is a floor component 56 which, like the partition component, is composed of two spaced parallel concrete shell panels 58 and 60 connected to each other by a triangulated wire core 62 . Here again, the floor component 56 could be the lowest level of the building structure or its bottom panel could be the ceiling component of a lower room. In a fashion similar to that of the ceiling component 54 , the floor component 56 has an upwardly projecting ledge or molding 64 the top edge 64 a of which is aligned with the bottom edge 40 b of the partition component and has an upwardly open molded-in female connector channel 50 . As an illustration of a utilitarian use of the partition component other than as a space divider, there is provided in the floor component a duct 66 , for example, for conducting a heating or cooling fluid from a source thereof, and a duct riser 68 is shown as ascending from the duct 66 through a sleeve-lined opening 65 in the floor component 56 (FIG. 11) into the interior of the partition component and terminating after a lateral bend 68 a in a discharge end 68 b outside the partition component and covered by a suitable register or grille.
[0072] The interconnection of the partition component 40 with the ceiling and floor ledges 52 and 64 is effected with the aid of a set of identical expansible/contractible male connector elements 70 , which correspond in shape to the connector channels 50 and in a more refined form are of the type shown in FIG. 15. As there shown, each male connector element includes two jaw-like members 72 and 74 which have flat proximal faces 72 a and 74 a and are arranged, with the aid of guide pins 73 , to be linearly displaced toward and away from each other by means of a screw drive shaft 76 which is rotatably received in an internally threaded bore or sleeve 78 carried by the member 72 and is provided with a pair of spaced lateral projections 78 a and 78 b bracketing the ends of the shaft-receiving bore in the member 74 . The jaw-like members 72 and 74 further have identical upper parts in the form of ridges or ribs 72 b and 74 b of generally trapezoidal cross-section which project away from one another, and identical lower parts in the form of ridges or ribs 72 c and 74 c of generally trapezoidal cross-section which project away from one another, all such ribs or ridges being configured to fit into respective lateral recesses 50 a and 50 b (FIG. 14) of an associated one of the female connector channels 50 . The open mouth 50 c of each connector channel is sufficiently wide to permit passage of the contracted male connector element 70 . In the system of FIGS. 10 and 11, therefore, when both of the male connector elements 70 are expanded as shown in FIG. 10 (the upper male connector element in FIG. 11 is contracted), they cannot be extracted from the respective connector channels 50 , whereby the partition component 40 is securely locked to the upper ceiling component 54 as well as to the lower floor component 56 .
[0073] [0073]FIGS. 12 and 13 represent a connection between the vertical edges of two horizontally aligned and abutting exterior wall components 80 and 82 . The connection is, however, effected in exactly the same way, utilizing two confronting female connector channels 50 and a two-part expandable/contractable male connector element 70 , as the connections shown in FIGS. 10 and 11, the only difference being that in the system of FIGS. 10 and 1 the connection is vertical between two horizontal abutting edges whereas in the system of FIGS. 12 and 13 the connection is horizontal between two vertical abutting edges. Accordingly, a more detailed description of the connection shown in FIGS. 12 and 13 is not believed necessary.
[0074] Methods of prefabricating the structural members shall now be described in conjunction with FIGS. 16 - 28 . As discussed above, the principal elements of each structural member, are chords which intersect at joints. Since the structural member has a modular design, the joints are positioned at predetermined locations and are typically spaced at equal distances from each other. As shown in FIG. 16, a typical joint 90 defines the intersection between several diagonal chords 34 , a parallel chord 34 a and a cross chord 34 b. These elements are held together by an anchor 91 and are mechanically joined to each other by any well known means such as by one or more weld zones. One such weld zone 92 is shown in FIG. 17.
[0075] The chords 34 may be made from steel wire having a diameter of ⅛-½″. The choice of this dimension depends on a number of factors, including the designated use for the structural member, the load to be supported by the structural member, the dimensions of the structural member, the ratio of each chord length to its diameter, and so on. Frequently these factors are dictated by national or local building codes. Typically, for exterior walls the wires may have a diameter of ¼″, ⅜″-½″ for floors and roofs, and ¼″ for interior walls.
[0076] The anchor 91 may be made from steel, aluminum, an alloy or may be a plastic/metal composite. While in the Figures, the anchor 91 has generally a C-shape, it could have other shapes selected to support the various chords and other elements (discussed in more detail below) which may be attached to the structural member. Preferably, the anchor 91 is shaped to allow the chords to be welded to each other after the anchor 91 is installed. In FIG. 17 the anchor is shown remote from the joint so that the welds 92 can be seen better.
[0077] [0077]FIG. 19 shows the completed joint with the chords 34 , 34 a, 34 b welded to each other and held together by the anchor 91 .
[0078] A separate piece of wire may be used for each chord. Alternatively, as shown in FIGS. 16 - 18 , a long piece of wire may be bent at the joints to form more than one chord.
[0079] While the joints described in FIGS. 16 - 18 could be assembled manually, for relatively large structural members (which most of them are expected to be), such a process may be too difficult, time consuming and impractical. Therefore a fixture 93 has been devised which can be used to perform this assembly automatically. The fixture is shown in detail in FIGS. 25 and 26 and is designed to hold the chords, anchors and any additional elements of a structural member together in a predetermined configuration until the joints are completed. Once a structural member is completed, it can be removed and the fixture may be used to assemble another structural member.
[0080] As shown in the Figures, fixture 93 is formed of a plurality of clusters 95 used to hold the joints during assembly, a plurality of posts, including short posts 96 and long posts 97 used for supporting the clusters, a plurality of vertical post rails 98 disposed in parallel to the parallel chords 34 a and used to support the posts 95 , 97 , and a plurality of guide rails 99 disposed in parallel to the cross chords 34 b. The post rails 98 are equipped with wheels 101 . The wheels 101 ride on guide rails 99 so that the whole fixture 93 can be moved as desired. The post rails are maintained at a predetermined positions by a spacer bar 100 .
[0081] Finally electric welding guns 102 are also provided which are operated by electrical controls to weld the chords.
[0082] [0082]FIG. 19 shows a typical arrangement for a cluster 95 attached to a long post 97 . It includes a horizontal member 97 a, a vertical member 97 b and a plurality of holding members 94 . Holding members preferably comprise remotely operated electromagnets, but may also includes permanent magnets, springs, clamps or any other electrical, hydraulic, pneumatic or other mechanical means of holding the joints 93 before and after welding, which can be remotely activated.
[0083] The fixture 93 is used as follows. First, the posts 95 , 97 are mounted on post rails 98 , the post rails are assembled on the guide rails 99 and their relative position is fixed by spacer bar 100 . The clusters 95 on the short posts 95 define the positions of the joints 90 on the back face of the structural member 24 and the clusters 95 on the long posts 97 define the positions of the joints 90 on the front face of the structural member 24 . In this manner, as described above, each joint 90 is located at a position consistent with the desired shape and configuration of structural member 24 and, thus, the fixture 93 defines the geometry of the structural member 24 during its assembly.
[0084] In addition, the welding guns 102 are also positioned so that they line up with the joints 90 .
[0085] Next, the chords are assembled at each joint 90 as illustrated sequentially in FIGS. 20 - 24 . As seen in these Figures, the chords are mounted on the cluster 95 and maintained in position by the magnets 94 . Once all the chords are in position, the anchor 91 is positioned into place, as shown in FIG. 24. Other elements may also be added at this point, such as doors, windows, etc. The resulting assembly is shown in FIGS. 27 and 28.
[0086] Once the chords are positioned, the joints are welded using electrical welding guns 102 . In the simplest case, the welding guns are manually or automatically positioned at each joint and the joints are welded. However, it is much more efficient to weld the joints automatically. Therefore, preferably the position of the assembly of chords is controlled by a motor 105 which may be used to move the post rails 98 along the guide rails. The motor 105 , holders 98 and the welding guns 102 may all be controlled by a control panel 107 which includes a microprocessor (not shown). Once the chords are positioned, the control panel 107 is activated. The panel then activates the motor 105 to move the post rails 98 so that the joints approach the welding guns. The welding guns 102 are equipped with sensors 102 a. As shown in FIGS. 27 and 28, the welding guns 102 may be arranged in two rows corresponding to the joints of the back and the front face. As each joint 90 approaches a corresponding welding gun 102 , it gets sensed by a sensor 102 a and the welding gun 102 is activated by the control panel 107 . The welding gun 102 then applies welds 92 to the joints 90 . The control panel 107 operates the welding guns for predetermined times calculated to generate welds of predetermined sizes. These sizes are dependent on the speed of the assembly and the time that each gun is operated.
[0087] After all the joins have been welded, the holders 94 can be deactivated thereby releasing the joints. The completed structural member 24 can then be removed and the fixture 93 can be reconfigured for another structural member.
[0088] In FIGS. 26 and 28 straight guide rails 99 are shown resulting in structural members that have planar front and back faces. However, these guides could also be curved, as shown in FIG. 28 by line C to make structural members with curved faces.
[0089] It will be understood that the foregoing description of the present invention is for purposes of illustration only, and that the various structural and operational features herein disclosed are susceptible to a number of modifications and changes none of which entails any departure from the spirit and scope of the present invention as defined in the hereto appended claims.
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Novel prefabricated modular structural members for use in low cost construction of relatively small residential, institutional and commercial buildings with high degrees of resistance to damage by fire, hurricanes, earthquakes, moisture, etc., are disclosed. A structural member of this class basically consists of two spaced shell panels and an intermediate core. The shell panels may be made of metal or concrete or combinations thereof, or of other rigid materials having the required physical properties. The core is a triangulated wire frame composed of a plurality of zig-zag shaped wire trusses having their sets of top and bottom apexes anchored to associated sets of longitudinal and transverse chords and the respective proximate inside faces of the shell panels. The arrangement of the wire trusses is such that, in each group of three adjacent wire trusses, the middle one has its bottom apexes also connected to the bottom apexes of the wire truss located on one side of the middle wire truss and has its top apexes also connected to the top apexes of the wire truss located on the other side of the middle wire truss. A fixture is provided which includes posts for holding the wires before they are welded. The posts and a coupling member such as a welding gun can move with respect to each other to form the joints between the wires.
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FIELD OF THE INVENTION
The present invention relates to fluid filled resilient bushing assemblies, and more particularly the present invention relates to fluid filled resilient bushing assemblies having both radial and axial damping.
BACKGROUND OF THE INVENTION
Bushing assemblies are generally located at a connecting joint between a base member and a member movable about the connecting joint in such applications as machinery, airplanes, boats and vehicular transportation. Generally, the base member has two ends, one end affixed to a frame and a second end having a mating member forming a part of a housing of the connecting joint. The member movable about the connecting joint also has two ends, one end affixed to an element movable with respect to the frame, and a second end having a mating member which along with the mating member of the base member forms the housing of the connecting joint. The bushing assembly is affixed within the housing of the connecting joint and serves to control forces and accommodate movement from the movable element.
Various forms of movements occur at the connecting joint including static and dynamic vibratory motions which induce radial and axial motions at the connecting joint. It is desirable that the bushing assembly be capable of damping such vibratory motions thereby reducing the transmittal of such vibratory motions to the base member while accommodating all static deflections.
Bushing assemblies are widely used in vehicular transportation such as joints in primary suspension assemblies for automobiles. One concern in automobiles is the reduction of vibrations induced from the road surface and isolation of the passenger compartment from such vibrations. Such vibrations may comprise a range of amplitudes and frequencies and motions in various directions. Relative to the road, the vibratory motion may be vertical, such as up and down motion induced by the road, or it may be horizontal, such as the sway motion incurred in cornering of a car. Automotive suspension systems are designed to reduce such vibrations. A front end suspension system is made up of components including various arms, rods, links, etc. intermediate of the frame and the wheel assembly of the car. Generally, an elongated arm extends from the wheel assembly, and another arm extends from the frame which are connected together at a connecting joint having a bushing assembly.
The most common type of bushing assembly is a rubber bushing. Rubber bushings generally comprise annular elongate inner and outer members with elastomer disposed therebetween. Such bushings are used to control and transmit movement but have limited capability in damping vibrations. Damping of vibrations is attained by dissipating the energy of the vibratory motion. The damping provided by elastomers is a function of the hysteresis property of the elastomer. In general, rubber bushings can be said to provide little damping.
One form of bushing assembly which can provide improved damping are fluid filled bushings. Fluid filled bushings generally include a cylindrical elongate inner rigid member, an elongate outer rigid sleeve member concentrically disposed and radially spaced from the inner member and a resilient means disposed between the inner member and outer sleeve member wherein the resilient elastomeric means defines a pair of circumferentially spaced and diametrically opposed fluid filled chambers fluidly connected by an elongate restricted passageway. In operation, in response to vibratory motions along the radial direction of the bushing assembly between the inner member and outer sleeve member, fluid is displaced from one chamber via the restricted passageway to the second chamber in a direction opposite to the vibratory motion. In particular, when a first chamber is contracted, the fluid is displaced therefrom through the restricted passageway to an expanding second chamber. In the reverse cycle of the vibratory motion, when the first chamber is expanding and the second chamber is contracting, the fluid is reversibly moved through the restricted passageway. As can be seen, an oscillatory motion of the fluid is generated within the restricted passageway between two chambers diameter about a radial direction.
The restricted passageway confines movement of the fluid. The oscillatory fluid in the restricted passageway creates a fluid resistance and/or a mass or inertia resistance to the pumping forces of the chambers resulting in damping of the vibratory motions along the radial direction. The chambers may be circumferentially spaced to provide damping along more than one radial direction in directions other than that which the chambers are located. Intermediate of the chambers, the bushing assembly comprises a solid rubber member, extending along the axial direction of the bushing assembly wherein these sections of the bushing assembly have the characteristics of the rubber bushing with respect to vibratory motion. Such fluid filled bushing assemblies provide damping limited to the radial direction along which fluid chambers are located. Damping is not provided along the axial direction of the bushing assembly.
An example of such a fluid filled bushing is disclosed in U.S. Pat. No. 3,642,268. The bushing there disclosed utilizes hydraulic fluid displaceable between two diametric chambers via a restricted orifice. The chambers are located in the bushing along a first radial direction whereas along a second radial direction perpendicular to the first radial direction is a solid rubber member which extends along the axial direction of the bushing. Such a fluid filled bushing exhibits low stiffness and high damping along the first radial direction dependent on the flow characteristics between the chambers and the fluid properties as described heretofore and high stiffness and low damping along the second radial direction and the axial direction.
Vibratory motions transmitted through bushing assemblies are not limited to motions in radial directions of the bushing but also include vibratory motions along the axial direction of the bushing assembly. Although the movement along the axial direction is controlled, the bushing assemblies described above provide limited damping of axial vibratory motions.
A fluid filled bushing for damping vibrations in both the radial and axial direction is disclosed in U.S. Pat. No. 4,667,942. The bushing therein disclosed utilizes hydraulic fluid displaceable between two sets of two chambers, the first set of two chambers provides damping in the axial direction and the second set of two chambers provides damping in the radial direction. The two sets of two chambers are fluidly interconnected via two restricted passageways. Vibratory motions in the radial direction are dampened by the transfer of fluid between the first set of two chambers via the two restricted passageways and vibratory motions in the axial direction are dampened by the transfer of fluid between the second set of two chambers via the two restricted passageways. Although this bushing assembly provides damping in the radial and axial direction, it is of complicated design. Furthermore, damping provided by such a bushing is diminished when the vibratory motion is changing from between the axial and radial directions.
There is a need for a fluid filled bushing assembly of less complicated design which can provide damping to vibratory motion in both axial and radial direction.
OBJECTS OF THE INVENTION
With the foregoing in mind, a primary object of the present invention is to provide an improved fluid filled resilient bushing assembly particularly suited for connecting relatively moveable components.
Another object of the present invention is to provide a novel fluid filled resilient bushing assembly providing damping of vibratory motion at excitations of various amplitudes and frequencies in the axial direction and radial direction or combinations thereof.
Another object of the present invention is to provide a novel fluid filled resilient bushing assembly of relatively uncomplicated design.
Another object of the present invention is to provide a novel fluid filled resilient bushing wherein damping of vibratory motion in the radial and axial direction is provided by a pair of axially spaced chambers interconnected by a unique restricted passageway.
SUMMARY OF THE INVENTION
More specifically, in the Present invention a fluid filled resilient bushing assembly is described having an elongate inner rigid member, an elongate outer rigid sleeve member disposed about and radially spaced from the inner member to define a space therebetween. A resilient means is disposed about the inner member between the inner and outer members. The resilient means defines at least two spaced chambers interconnected by a restricted passageway wherein the two chambers are axially and circumferentially spaced. An incompressible fluid is contained in the spaced chambers and restricted passageway. Such a fluid filled resilient bushing assembly provides damping of vibratory motion in the axial direction and radial direction or combination thereof. In one embodiment, the two spaced chambers are interconnected by a spirally disposed restricted passageway.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other objects, features and advantages should become apparent from the following description when taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a partial longitudinal sectional view taken along the mid axial plane of a bushing assembly of the present invention showing the circumferentially and axially spaced chambers and spirally disposed restricted passageway; and
FIG. 2 is a view taken along lines 2--2 of FIG. 1 showing a cross sectional view of one chamber.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, FlG. 1 illustrates a partial longitudinal sectional view wherein the sectional view is taken along the mid axial plane of a fluid filled resilient bushing assembly 10 which embodies the present invention. For clarity, FIG. 2 illustrates an elevational cross-sectional view taken along lines 2--2 of FIG. 1. The bushing assembly 10 includes a cylindrical elongate inner riqid member 14 having an annular bore 16 there through suitable to receive a member (not shown) to connect the bushing assembly 10 to an external structure such as two components of a suspension system. A cylindrical elongate outer rigid sleeve member 20 is concentrically disposed about and radially spaced from the inner member 14 to define an annular space therebetween. In the present embodiment the inner member 14 and the outer sleeve member 20 are made of a cold drawn low carbon steel. Other rigid materials may be used depending on the designers choice.
As shown in FIG. 1, a resilient means 32 is disposed between the inner rIgId member 14 and the outer rigid sleeve member 20. In the present invention the resilient means 32 is molded of elastomeric material such as high temperature natural rubber in a unitary piece which is inserted sealingly combined between the inner and outer members. The inner member 14 and outer 20 are preferably bonded to the resilient means 32. The outer rigid sleeve member 20 has two outer axial edges 22, 24 which are crimped radially inwardly to sealingly secure the resilient means 32 in place.
The resilient means 32 and outer sleeve member 20 define two circumferentially and axially spaced chambers 40, 42 and a spirally disposed restricted passageway 50 fluidly interconnecting the two chambers 40, 42. As shown in FIG. 1, the chambers 40, 42 are on opposite sides of the rigid inner member 14 and are axially spaced such that, the one chamber 40 is located near one end of the bushing assembly 10 and the second chamber 42 is located near the other end of the bushing assembly 10 in an opposed relation about the medial axial plane. Each of the chambers 40, 42 is defined by at least one flexible thin wall 41, 43. The thin wall 41, 43 allows each chamber 40, 42 to expand or contract responsive to vibratory motions.
The restricted passageway 50 is defined by the resilient means 32 and the outer sleeve member 20 wherein the restricted passageway 50 extends spirally about the longitudinal axis of the inner member 14 in the periphery of the resilient means 32 from one chamber 40 to the second chamber 42. In the shown embodiment, the restricted passageway has a semi-circular cross-sectional configuration. The restricted passageway 50 has a port 50a at one end opening into the first chamber 40 and a port 50b at its opposite end opening into the second chamber 42. The cross section area of the chambers 40, 42 is enlarged relative to the cross sectional area of the passageway 50. The pair of chambers 40, 42 and the restricted passageway 50 are filled with a substantially incompressible working fluid (not shown) such as a mixture of ethylene glycol and water.
The efficiency with which the working fluid is displaced between the chambers 40, 42 is affected by the flexibility of the thin wall, 41, 43 which can be defined as volume compliance. This compliance is defined as the ratio of a change in pressure of a chamber to the change in volume caused thereby. Thus, C=dP/dV. Thus, when a small change in volume results in a large change in pressure, the compliance is high. It is known that maximum damping occurs when compliance is in resonance with the fluid inertia of the passageway.
The compliance of the thin wall portion 41, 43 of each chamber 40, 42 is greater than that of its adjacent wall portions so that it is capable of being flexed readily by hydrodynamic pressure developed in the chambers in the course of operation of the bushinq assembly 10. In particular, the flexural motion of the thin walls 41, 43 occurs as a result of alternatinq pressure resultinq from the vibratory motions.
The efficiency of the displacement of the working fluid between the chambers 40,42 is also affected by the restructed passageway 50. As shown in FIG. 1, the restructed passageway 50 extends from one chamber 40 to the other chamber 42, extending greater than 360°. The efficiency of the displacement of the working fluid is affected by the inertia (ρ1wherein ρ=mass density; 1 =length of passageway; and A=area of passageway) of the fluid and the fluid losses within the restricted passageway. The increased inertia as found in the bushing assembly of the present invention provides for increased flexibility and performance to accommodate lower tuning frequencies and a wide range of vibratory motions.
During operation, vibratory motions in the radial and axial direction represented in FIG. 1 by the arrows A, B respectively cause the working fluid to oscillate in the restricted passageway 50 between the first chamber 40 and the second chamber 42. Oscillation of the fluid acts as a damping effect against the vibratory motion. In FlG. 1, the two chambers 40, 42 are on opposite sides of the rigid inner member 14, lying in a singular radial plane. The chambers 40, 42 are described as being circumferentially spaced by 180°. The vibratory motions along the radial plane of the two chambers 40, 42, induce oscillating movement of the inner member 14 relative to the outer sleeve member 20 causing the working fluid to oscillate in the restricted passageway 50 between the first chamber 40 and the second chamber 42. In particular, when the vibratory motion pushes the inner member 14 towards the outer sleeve member 20 contracting the first chamber 40, the working fluid is pushed from the first chamber 40, through the port 50a into the restricted passageway 50 and on to the expanding second chamber 42. The inertia of the fluid in the passageway 50 causes a resistance to the contraction of the first chamber resulting in a damping affect against the vibratory motion of the inner member 14 towards the outer sleeve member 20. When the vibratory motion reverses and pushes the inner member 14 towards the outer sleeve member 20 the second chamber 42 is contracted, wherein the vibratory motion is dampened by the resistence of the fluid flow through the restricted passageway 50. It is well known that the two chambers may be offset from the 180° circumferentially spacing to provide damping of vibratory motion in two radial directions. Because vibratory motions also occur in the axial direction, it is accordingly advantageous to affect damping in that direction as well.
The present invention satisfies the damping of the vibratory motion in the axial direction B by the use of only two chambers 40, 42 and one restricted passageway 50. Such damping is effected by the axial spacing of the chambers 40, 42 as shown in FlG. 1. Although the chambers 40, 42 are shown to be equally axially spaced about an imaginary medial axial plane, other suitable spacings could be used to effect damping in the axial direction. When a vibratory motion in the axial direction pushes against one end of the busing assembly 10, the left hand side say, the first chamber 40 is contracted in the axial direction, pushing the working fluid from the first chamber 40 through the port 50a into the restricted passageway and on to the expanding second chamber 42. The resistance against the inertia of the fluid in the passageway 50 causes a resistance to the contraction of the first chamber 40 in the axial direction resulting in a damping effect against the vibratory motion in the axial direction. When the vibratory motion is in the reverse direction, the working fluid resists the contraction of the second chamber 42. The damping effect may be suitably controlled by design of the restricted passageway 50 and the axial spacing of the chambers 40, 42.
The manufacture of fluid filled bushing assemblies is well-known to those skilled in the art and may be accomplished by several different methods. Fluid filled bushing assemblies of the present invention are manufactured by separately manufacturing the components and then combining them. In particular, the inner member 14 and outer sleeve member 20 are formed according to standard metal working methods where after the parts are cleaned, a primer and suitable rubber to metal adhesive is applied to surfaces to which rubber will be bonded. The resilient means 32 is molded wherein the chambers 40, 42 and restricted passageway 50 are molded therein. The inner member 14 and sleeve member 20 are assembled around resilient means 32 and the ends crimped in place. The assembly is then placed in a mold and a vulcanizing press. The mold is preheated to a suitable curing temperature dependent on the rubber used. Whereafter the inner member 14, sleeve member 20 and resilient means 32 are suitably sealingly banded together.
After vulcanization, the bushing assembly 10 is demolded, cleaned and readied for finishing. The chambers and the restricted passageway 50 are filled with incompressible fluid through the fill hole whereafter a rubber plug (not shown) is inserted.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teaching of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.
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A fluid filled resilient bushing assembly for vibration control in the radial and axial directions or combinations thereof, particularly adapted for use in a suspension system, which comprises an elongate inner rigid member and an elongate outer rigid sleeve member, a resilient member interposed between the inner and outer members. The resilient member together with the outer member defines two circumferentially and axially-spaced chambers and a restricted passageway connecting the chambers. The chambers and passageway contain an incompressible fluid. By axially and circumferentially spacing the chambers, the desired damping in the axial and radial direction is obtained.
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BACKGROUND OF THE INVENTION
This invention relates to injection laser manufacture and in particular to the manufacture of an (In,Ga)(As,P) laser having the structure referred to sometimes as an Inverted Rib Waveguide (IRW) laser, and also referred to as a Plano-Convex Waveguide (PCW) laser.
An IRW laser is characterized by having, between the active layer and the substrate, an intermediate layer which provides a measure of dielectric waveguiding effect in the lateral direction by virtue of a rib formed in its surface facing the substrate, this rib extending into a material of lower refractive index. In the case of (In,Ga)(As,P) lasers grown upon InP substrates, the low refractive index of InP relative to that of (In,Ga)(AsP) makes it possible to adopt a relatively simple structure in which the intermediate layer is grown directly onto the surface of the substrate so that its rib extends into the substrate material.
The manufacture of (In,Ga)(As,P) IRW lasers has been described by M. Ueno et al in IEEE Journal of Quantum Electronics, Vol. QE-17, No. 9, pp. 1930-40 (September 1981), by K. Sakai et al in the same Journal, Vol. QE-17, No. 7, pp. 1245-50 (July, 1981), and by Y. Noda et al in Electronics Letters, Vol. 17, No. 6, pp. 226-7 (March 1981). However, the approaches described in these articles have certain disadvantages which will be discussed in some detail later and which are overcome by the present invention.
SUMMARY OF THE INVENTION
Accordingly, it is a general object of the present invention to avoid the disadvantages of the prior art.
More particularly, it is an object of the present invention to provide an inverted rib waveguide laser which does not possess the disadvantages of the known lasers of this type.
Still another object of the present invention is so to construct the laser of the type here under consideration as to be able to keep the thickness of an intermediate layer situated between an active layer and a substrate of the laser, and thus between the active layer and a rib of the intermediate layer which achieves a measure of lateral waveguiding effect, to a minimum.
It is yet another object of the present invention to develop a method of producing a laser of the above type, which achieves relatively rapid and excellent liquid epitaxy growth of the intermediate layer material especially in a channel of the substrate during the formation of the rib, and which results in the formation of a planar surface of the intermediate layer facing away from the substrate for the formation of the active layer thereon.
A concomitant object of the present invention is to devise a method of the above type which is easy to accomplish, inexpensive to perform, can be accomplished on already existing equipment, and achieves reliable results nevertheless.
In pursuance of these objects and others which will become apparent hereafter, one feature of the present invention resides in a method of producing an inverted rib waveguide laser including an InP substrate having a (100) surface, and an (In,Ga)(As,P) active layer, this method including the steps of forming at the (100) surface of the substrate a channel extending in the [011] direction by an etching process producing side walls of the channel that deviate from A-planes; epitaxially growing in the channel and on the (100) surface of the substrate an (In,Ga)(As,P) intermediate layer of larger band gap material than that of the active layer to thereby form a rib filling the channel and providing a measure of dielectric waveguiding effect for the laser in the lateral direction; and providing the active layer on the intermediate layer.
According to another aspect of the present invention there is provided in an inverted rib waveguide laser including an InP substrate having a (100) surface, and an (In,Ga)(As,P) active layer, the combination comprising means for bounding at the (100) surface, of the substrate a channel extending in the [011] direction, including side walls deviating from A-planes; and an (In,Ga)(As,P) intermediate layer of larger band gap material than that of the active layer on the (100) surface of the substrate and in the channel forming a rib filling the channel and providing a measure of dielectric waveguiding effect for the laser in the lateral direction, the active layer being provided on the intermediate layer.
In the articles referred to above, it has not been specified whether the orientation is such that the rib extends in a [011] or a [011] direction along the (100) plane. We have found that there is a distinct advantage in using the [011] direction rather than the [011]. A channel extending in the [011] direction is readily etched to a reproducible shape having A-plane side walls, whereas when etching a channel extending in the [011] direction the side walls may be A-plane, B-plane, (011) and (011) planes, or some mixture of these, depending upon the nature of the etchant and the nature of the masking material used to delineate the channel. The difference between {111}A and {111}B faces affects the growth characteristics. Liquid phase epitaxy of InP and its related alloys is normally based on solutions in liquid In metal, so that the concentration of In in the system is much higher than that of P. The attachment of a new atom to both types of the {111} surface is relatively weak, since it consists of a single bond. The high concentration of In in the liquid would be expected to increase the probability of attachment of In atoms to a {111}B surface, whereas the probability of attaching P atoms to produce nucleation on a {111}A surface is much lower. For this reason growth on {111}A faces does not occur readily. Growth on {011} surfaces can be initiated by the attachment of either In or P atoms and thus growth occurs readily.
The slow growth of material on A-planes means that a channel with A-plane sides is not filled by subsequent liquid phase epitaxial growth nearly as quickly as when the sides are formed by planes deviating from A-planes. This in turn means that adequate filling of the channel to produce a substantially planar surface upon which the active layer can be grown requires the use of a thicker intermediate layer when filling channels with A-plane sides than when filling channels with differently oriented sides. This problem of growing sufficient material to provide a planar surface upon which the active layer can be grown is expressly referred to in the Ueno et al article to which previous reference has been made, and the authors of that article stated that they found it necessary to grow a layer whose thickness beyond the confines of the channel was greater than the depth of the channel formed in the substrate. We have found that this restriction can be avoided by using channels which do not have A-plane sides. Remembering that the laser must be designed so that the optical field extends deep enough for the rib to have the requisite lateral waveguiding effect, a consequence of being able to use a thinner intermediate layer is that the rib can be closer to the active layer, thereby relaxing a design constraint by making possible the use of designs in which the optical field does not have to extend so far from the active layer.
BRIEF DESCRIPTION OF THE DRAWING
Above-mentioned and other features and objects of this invention will become more apparent by reference to the following description taken in conjunction with the accompanying sole FIGURE of the drawing which is a diagrammatic cross-sectional view of a laser according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawing in detail, it may be seen that the reference numeral 1 has been used therein to identify a substrate. A (100) surface of an n+-type wafer of InP, which is to form the substrate 1 of the laser, is polished and then etched in a bromine-methanol etch to remove approximately 10 microns of material that may have suffered polish damage. A silica masking layer (not shown) is then pyrolytically deposited on the substrate 1 from a mixture of oxygen and silane in nitrogen at a temperature of typically 400°-450° C. Windows extending in the [011] direction are etched through the mask with buffered hydrofluoric acid etch. Typically these windows are 2.75 microns wide. Then the etch is changed for a 1:1 hydrobromic: phosphoric acid etch (50% and 85% concentrated, respectively) to form channels 2 extending in the [011] direction in the substrate 1. This etch slightly undercuts the mask and leaves {111}B channel walls 3. (Each laser requires only one channel but in accordance with conventional semiconductor device manufacturing processing many devices are made at the same time on a single wafer which is subsequently divided up to give the individual devices.) The ability of this etchant to undercut the mask appears to be important to achieve the production of the {111}B sides, for if (In,Ga) (As,P) deposited by liquid phase epitaxy is used as the masking material, little if any undercutting occurs, and {111}A walls are produced instead of {111}B ones. In view of the propensity of the etch to produce etch pits at dislocations, it is desirable to choose a substrate with a low dislocation density. This is usually achieved by using a highly sulphur doped substrate 1. The etch time is usually quite short (typically between 5 and 10 seconds) to produce a channel 2 typically about 0.5 microns deep. After this the silica mask is removed with buffered hydrofluoric acid and then the substrate 1 is given a short etch (typically 20 seconds) in 0.1% bromine by volume in methanol to remove damage that may have occurred during the deposition of the mask. It is believed that this final etch also improves growth quality. It results in a slight rounding of channel shoulders which may ease LPE growth at the sides of the channel 2.
At this stage the channelled substrate wafer 1 is ready for the growth of its epitaxial layers and is mounted in a liquid phase epitaxy reactor. The first layer to be grown is an intermediate or guide layer 4 of lattice matched n-type (In,Ga)(As,P) material having a composition whose luminescence peak is centered at about 1.05 microns. This layer 4 is typically grown to a thickness of about 0.3 microns in regions remote from the channel 2, and by virtue of the face that the channel walls, 3 are not A-plane walls this thickness is sufficient to provide a substantially planar upper surface to the layer 4 notwithstanding the fact that this thickness is not as great as the depth of the channel 2. The next layer to be grown is an active layer 5, typically about 0.24 microns thick of lattice matched (In,Ga)(As,P) material typically having a composition whose luminescence peak is centered at about 1.3 microns. This active layer 5 is in turn covered by p-type passive and capping layers 6 and 7. The passive layer 6 is a low refractive index layer made of indium phosphide as is typically 1.5 microns thick while the capping layer 7 is made of lattice matched (In,Ga)(As,P) material typically having a composition whose luminescence peak is centered at 1.2 microns, or of (In,Ga) As material. In either instance the capping layer 7 is typically 0.3 microns thick.
The next stage of manufacture involves depositing an electrically insulating silica mask layer 8 and opening up windows 9 in that layer 8 to register with the channel 2. The silica material of the mask layer 8 is deposited by a plasma deposition process. The windows 9 are opened up with buffered hydrofluoric acid, using conventional photolithography.
If the growth of the epitaxial layers 4, 5, 6 and 7 has been prevented from extending right to the edge of the wafer 1, for instance by arranging for the wafer 1 to extend a few millimeters under the walls of the sliding boat containing the melts, then the requisite registry of the windows 9 with the grooves 2 can be obtained simply by visually aligning the mask with the channels 2 of the substrate wafer 1 where they lie exposed to view at the periphery of the wafer 1.
If, however, the epitaxy has been allowed to proceed up to the edge of the wafer 1, a preliminary processing stage is required to remove a portion of the layers 4 to 7 at the periphery of the wafer 1 so as to expose the locations of the channels 2. This can be done by etching the p-type capping layer 7 with a potassium iodide/iodine etch, etching the p-type passive layer 6 with a hydrochloric/phosphoric acid etch, etching, etching the active layer 5 with a nitric acid etch, and finally determining the position of the channel filled by the intermediate or guide layer 4 by etching it alternately with bromine-methanol and with hydrochloric/phosphoric acid etches. The etching of the guide layer 4 involves more complicated processing than the corresponding etching of the capping layer 7 because the guide layer composition is too close to indium phosphide to be selectively etched with a potassium iodide/iodine etch. The bromine-methanol etch is a non-selective etch that would etch both the material of the guide layer 4 and the material of the underlying substrate 1. On the other hand, the hydrochloric/phosphoric acid etch will only etch the substrate material. Therefore this etch is used to test whether or not the previous etching, the bromine-methanol etch, has proceeded deep enough to expose any substrate material. Once the guide layer 4 has been breached, the hydrochloric/phosphoric acid etch serves to reveal the channels 2 in reverse relief.
Once the windows 9 have been opened in the silica mask layer 8, a short zinc diffusion is performed to produce a p+ region immediately under the window 9 for facilitating the making of a good electrical connection with the capping layer 7. The device is then thinned to reduce the substrate thickness to approximately 80 microns before the application of metal contact layers 10 and 11, which are evaporated and alloyed contacts, respectively.
In a modification of the above described method of manufacture a 4:1 phosphoric:hydrochloric acid etch is substituted for the 1:1 phosphoric:hydrobromic acid etch when etching the channels 2 in the indium phosphide substrate 1. This produces (011) and (011) side walls 3 to the channels 2 instead of the B plane walls.
It is also possible to redesign the structure so as to be able to use a p-type substrate. This entails growing each of the epitaxial layers in material of the opposite conductivity type to that used with the n-type substrate.
While I have described above the principles of my invention in connection with specific laser constructions, it is to be clearly understood that this description is made only by way of example and not as a limitation to the scope of my invention as set forth in the objects thereof and in the accompanying claims.
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A method of making an (In,Ga)(As,P) inverted rib waveguide laser in which a lateral waveguiding effect is provided by an inverted rib formed in intermediate index material spacing the active layer from the substrate which accommodates the rib in a channel in the substrate includes forming the channel with {111}B or {011} plane side walls, thereby permitting the use of a thinner intermediate index material layer than is possible when using a channel with {111}A plane sides.
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CROSS-REFERENCE TO RELATED APPLICATIONS
Not Applicable
STATEMENT RE: FEDERALLY SPONSORED RESEARCH/DEVELOPMENT
Not Applicable
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention pertains generally to steam desuperheaters or attemperators and, more particularly, to a uniquely configured spray nozzle assembly for a steam desuperheating or attemperator device. The nozzle assembly is specifically adapted to, among other things, prevent thermal shock to prescribed internal structural components thereof, to prevent “sticking” of a valve stem thereof, and to create a substantially uniformly distributed spray of cooling water for spraying into a flow of superheated steam in order to reduce the temperature of the steam.
2. Description of the Related Art
Many industrial facilities operate with superheated steam that has a higher temperature than its saturation temperature at a given pressure. Because superheated steam can damage turbines or other downstream components, it is necessary to control the temperature of the steam. Desuperheating refers to the process of reducing the temperature of the superheated steam to a lower temperature, permitting operation of the system as intended, ensuring system protection, and correcting for unintentional deviations from a prescribed operating temperature set point. Along these lines, the precise control of final steam temperature is often critical for the safe and efficient operation of steam generation cycles.
A steam desuperheater or attemperator can lower the temperature of superheated steam by spraying cooling water into a flow of superheated steam that is passing through a steam pipe. By way of example, attemperators are often utilized in heat recovery steam generators between the primary and secondary superheaters on the high pressure and the reheat lines. In some designs, attemperators are also added after the final stage of superheating. Once the cooling water is sprayed into the flow of superheated steam, the cooling water mixes with the superheated steam and evaporates, drawing thermal energy from the steam and lowering its temperature.
A popular, currently known attemperator design is a probe style attemperator which includes one or more nozzles or nozzle assemblies positioned so as to spray cooling water into the steam flow in a direction generally along the axis of the steam pipe. In many applications, the steam pipe is outfitted with an internal thermal liner which is positioned downstream of the spray nozzle attemperator. The liner is intended to protect the high temperature steam pipe from the thermal shock that would result from any impinging water droplets striking the hot inner surface of the steam pipe itself.
One of the most commonly encountered problems in those systems integrating an attemperator is the addition of unwanted water to the steam line or pipe as a result of the improper operation of the attemperator, or the inability of the nozzle assembly of the attemperator to remain leak tight. The failure of the attemperator to control the water flow injected into the steam pipe often results in damaged hardware and piping from thermal shock, and in severe cases has been known to erode piping elbows and other system components downstream of the attemperator. Along these lines, water buildup can further cause erosion, thermal stresses, and/or stress corrosion cracking in the liner of the steam pipe that may lead to its structural failure.
In addition, the service requirements in many applications are extremely demanding on the attemperator itself, and often result in its failure. More particularly, in many applications, various structural features of the attemperator, including the nozzle assembly thereof, will remain at elevated steam temperatures for extended periods without spray water flowing through it, and thus will be subjected to thermal shock when quenched by the relatively cool spray water. Along these lines, typical failures include spring breakage in the nozzle assembly, and the sticking of the valve stem thereof. Further, in probe style attemperators wherein the spray nozzle(s) reside in the steam flow, such cycling often results in fatigue and thermal cracks in critical components such as the nozzle holder and the nozzle itself. Thermal cycling, as well as the high velocity head of the steam passing the attemperator, can also potentially lead to the loosening of the nozzle assembly which may result in an undesirable change in the orientation of its spray angle.
With regard to the functionality of any nozzle assembly of an attemperator, if the cooling water is sprayed into the superheated steam pipe as very fine water droplets or mist, then the mixing of the cooling water with the superheated steam is more uniform through the steam flow. On the other hand, if the cooling water is sprayed into the superheated steam pipe in a streaming pattern, then the evaporation of the cooling water is greatly diminished. In addition, a streaming spray of cooling water will typically pass through the superheated steam flow and impact the interior wall or liner of the steam pipe, resulting in water buildup which is undesirable for the reasons set forth above. However, if the surface area of the cooling water spray that is exposed to the superheated steam is large, which is an intended consequence of very fine droplet size, the effectiveness of the evaporation is greatly increased. Further, the mixing of the cooling water with the superheated steam can be enhanced by spraying the cooling water into the steam pipe in a uniform geometrical flow pattern such that the effects of the cooling water are uniformly distributed throughout the steam flow. Conversely, a non-uniform spray pattern of cooling water will result in an uneven and poorly controlled temperature reduction throughout the flow of the superheated steam. Along these lines, the inability of the cooling water spray to efficiently evaporate in the superheated steam flow may also result in an accumulation of cooling water within the steam pipe. The accumulation of this cooling water will eventually evaporate in a non-uniform heat exchange between the water and the superheated steam, resulting in a poorly controlled temperature reduction.
Various desuperheater devices have been developed in the prior art in an attempt to address the aforementioned needs. Such prior art devices include those which are disclosed in Applicant's U.S. Pat. No. 6,746,001 (entitled Desuperheater Nozzle), U.S. Pat. No. 7,028,994 (entitled Pressure Blast Pre-Filming Spray Nozzle), U.S. Pat. No. 7,654,509 (entitled Desuperheater Nozzle), and U.S. Pat. No. 7,850,149 (entitled Pressure Blast Pre-Filming Spray Nozzle), the disclosures of which are incorporated herein by reference. The present invention represents an improvement over these and other prior art solutions, and provides a nozzle assembly for spraying cooling water into a flow of superheated steam that is of simple construction with relatively few components, requires a minimal amount of maintenance, and is specifically adapted to, among other things, prevent thermal shock to prescribed internal structural components thereof, to prevent “sticking” of a valve stem thereof, and to create a substantially uniformly distributed spray of cooling water for spraying into a flow of superheated steam in order to reduce the temperature of the steam. Various novel features of the present invention will be discussed in more detail below.
BRIEF SUMMARY OF THE INVENTION
In accordance with the present invention, there is provided an improved spray nozzle assembly for an attemperator which is operative to spray cooling water into a flow of superheated steam in a generally uniformly distributed spray pattern. The nozzle assembly comprises a nozzle housing and a valve element which is movably interfaced to the nozzle housing. The valve element, also commonly referred to as a valve pintle or a valve plug, extends through the nozzle housing and is axially movable between a closed position and an open (flow) position. The nozzle housing defines a generally annular flow passage. The flow passage itself comprises three identically configured, arcuate flow passage sections, each of which spans an interval of approximately 120°. One end of each of the flow passage sections extends to a first (top) end of the nozzle housing. The opposite end of each of the flow passage sections fluidly communicates with a fluid chamber which is also defined by the nozzle housing and extends to a second (bottom) end of the nozzle housing which is disposed in opposed relation to the first end thereof. A portion of the second end of the nozzle housing which circumvents the fluid chamber defines a seating surface of the nozzle assembly. The nozzle housing further defines a central bore which extends axially from the first end thereof, and is circumvented by the annular flow passage collectively defined by the separate flow passage sections, i.e., the central bore is concentrically positioned within the flow passage sections. That end of the central bore opposite the end extending to the first end of the nozzle housing terminates at the fluid chamber.
The valve element comprises a valve body or nozzle cone, and an elongate valve stem which is integrally connected to the nozzle cone and extends axially therefrom. The nozzle cone has a tapered outer surface, with the junction between the nozzle cone and the valve stem being defined by a continuous, annular groove or channel formed within the valve element. The valve stem is advanced through the central bore of the nozzle housing. Disposed within the central bore of the nozzle housing is a biasing spring which circumvents a portion of the valve stem, and normally biases the valve element to its closed position.
In the nozzle assembly, cooling water is introduced into each of the flow passage sections at the first end of the nozzle housing, and thereafter flows therethrough into the fluid chamber. When the valve element is in its closed position, a portion of the outer surface of the nozzle cone thereof is seated against the seating surface defined by the nozzle housing, thereby blocking the flow of fluid out of the fluid chamber and hence the nozzle assembly. An increase of the pressure of the fluid beyond a prescribed threshold effectively overcomes the biasing force exerted by the biasing spring, thus facilitating the actuation of the valve element from its closed position to its open position. When the valve element is in its open position, the nozzle cone thereof and the that portion of the nozzle housing defining the seating surface collectively define an annular outflow opening between the fluid chamber and the exterior of the nozzle assembly. The shape of the outflow opening, coupled with the shape of the nozzle cone of the valve element, effectively imparts a conical spray pattern of small droplet size to the fluid flowing from the nozzle assembly. Importantly, fluid flow through the nozzle assembly normally bypasses the central bore, and thus does not directly impinge the biasing spring therein. In one embodiment of the present invention, prescribed portions of the valve stem of the valve element may include grooves formed therein in a prescribed pattern, such grooves being sized, configured and arranged to prevent debris accumulation in the central bore which could otherwise result in the sticking of the valve element during the reciprocal movement thereof between its closed and open positions.
The present invention is best understood by reference to the following detailed description when read in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
These, as well as other features of the present invention, will become more apparent upon reference to the drawings wherein:
FIG. 1 is a bottom perspective view of a nozzle assembly constructed in accordance with the present invention, depicting the valve element thereof in a closed position;
FIG. 2 is a top perspective view of the nozzle assembly shown in FIG. 1 ;
FIG. 3 is a bottom perspective view of the nozzle assembly of the present invention, depicting the valve element thereof in an open position;
FIG. 4 is a top perspective view of the nozzle assembly shown in FIG. 3 ;
FIG. 5 is a cross-sectional view of the nozzle assembly of the present invention, depicting the valve element thereof in its closed position;
FIG. 6 is a cross-sectional view of the nozzle assembly of the present invention, depicting the valve element thereof in its open position;
FIG. 7 is a top perspective view of the nozzle housing of the nozzle assembly of the present invention;
FIG. 8 is a cross-sectional view of the nozzle housing shown in FIG. 7 ;
FIG. 9 is cross-sectional view of a variant of the nozzle assembly of the present invention wherein the valve element thereof is provided with debris grooves in a prescribed arrangement therein;
FIG. 10 is a bottom perspective view of the nozzle assembly of the present invention as partially inserted into a complementary nozzle holder and retained therein via a tab washer; and
FIG. 11 is a top perspective view of the tab washer shown in FIG. 10 in an original, unbent state.
Common reference numerals are used throughout the drawings and detailed description to indicate like elements.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings wherein the showings are for purposes of illustrating a preferred embodiment of the present invention only, and not for purposes of limiting the same, FIGS. 1-6 depict a nozzle assembly 10 constructed in accordance with a present invention. In FIGS. 1 , 2 and 5 , the nozzle assembly 10 is shown in a closed position which will be described in more detail below. Conversely, in FIGS. 3 , 4 and 6 , the nozzle assembly 10 is shown in an open position which will also be described in more detail below. As indicated above, the nozzle assembly 10 is adapted for integration into a desuperheating device such as, but not necessarily limited to, a probe type attemperator. As will be recognized by those of ordinary skill in the art, the nozzle assembly 10 of present invention may be integrated into any one of a wide variety of different desuperheating devices or attemperators without departing from the spirit and scope of the present invention.
The nozzle assembly 10 of the present invention comprises a nozzle housing 12 which is shown with particularity in FIGS. 7 and 8 . The nozzle housing 12 has a generally cylindrical configuration and, when viewed from the perspective shown in FIGS. 1-8 , defines a first, top end 14 and an opposed second, bottom end 16 . The nozzle housing 12 further defines a generally annular flow passage 18 . The flow passage 18 comprises three identically configured, arcuate flow passage sections 18 a , 18 b , 18 c , each of which spans an interval of approximately 120°. One end of each of the flow passage sections 18 a , 18 b , 18 c extends to the top end 14 of the nozzle housing 14 . The opposite end of each of the flow passage sections 18 a , 18 b , 18 c fluidly communicates with a fluid chamber 20 which is also defined by the nozzle housing 12 and extends to the bottom end 16 thereof. A portion of the bottom end 16 of the nozzle housing 12 which circumvents the fluid chamber 20 defines an annular seating surface 22 of the nozzle housing 12 , the use of which will be described in more detail below.
As is most easily seen in FIGS. 5-8 , the nozzle housing 12 defines a tubular, generally cylindrical outer wall 24 , and a tubular, generally cylindrical inner wall 26 which is concentrically positioned within the outer wall 24 . The inner wall 26 is integrally connected to the outer wall 24 by three (3) identically configured spokes 28 of the nozzle housing 12 which are themselves separated from each other by equidistantly spaced intervals of approximately 120°. As best seen in FIG. 8 , one end of each of the spokes 28 terminates at the top end 14 of the nozzle housing 12 , with the opposite end of each spoke 28 terminating at the fluid chamber 20 . The inner wall 26 of the nozzle housing 12 defines a central bore 30 thereof. The central bore 30 extends axially within the nozzle housing 12 , with one end of the central bore 30 being disposed at the top end 14 , and the opposite end terminating at but fluidly communicating with the fluid chamber 20 . Due to the orientation of the central bore 30 within the nozzle housing 12 , the same is circumvented by the annular flow passage 18 collectively defined by the separate flow passage sections 18 a , 18 b , 18 c , i.e., the central bore 30 is concentrically positioned within the flow passage sections 18 a , 18 b , 18 c.
As further seen in FIG. 8 , the central bore 30 is not of a uniform diameter. Rather, when viewed from the perspective shown in FIG. 8 , the inner wall 26 is formed such that the central bore 30 defines a top section which is of a first diameter and a bottom section which is of a second diameter less than the first diameter. As a result, the top and bottom sections of the central bore 30 are separated by a continuous, annular shoulder 32 of the inner wall 26 . In the nozzle assembly 10 , the flow passage sections 18 a , 18 b , 18 c are each collectively defined by the outer and inner walls 24 , 26 and an adjacent pair of the spokes 28 , with the fluid chamber 20 being collectively defined by the outer wall 24 and that portion of the inner wall 26 which defines the shoulder 32 thereof. As is most apparent from FIGS. 1-4 and 7 , a portion of the outer surface of the outer wall 24 is formed to define a multiplicity of flats 34 , the use of which will be described in more detail below. In the nozzle assembly 10 , it is contemplated that the nozzle housing 12 having the structural features described above may be fabricated from a direct metal laser sintering (DMLS) process in accordance with the teachings of Applicant's U.S. Patent Publication No. 2009/0183790 entitled Direct Metal Laser Sintered Flow Control Element published Jul. 23, 2009, the disclosure of which is also incorporated herein by reference. Alternatively, the nozzle housing 12 may be fabricated through the use of a die casting process.
The nozzle assembly 10 further comprises a valve element 36 which is moveably interfaced to the nozzle housing 12 , and is reciprocally moveable in an axial direction relative thereto between a closed position and an open or flow position. The valve element 36 comprises a valve body or nozzle cone 38 , and an elongate valve stem 40 which is integrally connected to the nozzle cone 38 and extends axially therefrom. The nozzle cone 38 defines a tapered outer surface 42 , with the junction between the nozzle cone 38 and the valve stem 40 being defined by a continuous, annular groove or channel 44 formed in the valve element 36 . As is best seen in FIGS. 5 and 6 , the valve stem 40 of the valve element 36 is not of uniform outer diameter. Rather, when viewed from the perspective shown in FIGS. 5 and 6 , the valve stem 40 includes a top flange portion 46 and a bottom flange portion 48 which each protrude radially outward relative to the remainder thereof. The top and bottom flange portions 46 , 48 are separated from each other by a prescribed distance, with the bottom flange portion 48 extending to the channel 44 . As also seen in FIGS. 5 and 6 , the outer diameter of the bottom flange portion 48 is substantially equal to, but slightly less than, the diameter of the bottom section of the central bore 30 .
In the nozzle assembly 10 , the valve stem 40 of the valve element 36 is advanced through the central bore 30 such that the nozzle cone 38 predominately resides within the fluid chamber 20 . The nozzle assembly 10 further comprises a helical biasing spring 50 which is disposed within the central bore 30 and circumvents a portion of the valve stem 40 extending therethrough. More particularly, as seen in FIGS. 5 and 6 , the biasing spring 50 circumvents that portion of the outer surface of the valve stem 40 which extends between the top and bottom flange portions 46 , 48 thereof. The biasing spring 50 is operative to normally bias the valve element 36 to its closed position shown in FIGS. 1 , 2 and 5 . A preferred material for both the nozzle housing 12 and the biasing spring 50 is Inconel 718 , though other materials may be used without departing from the spirit and scope of the present invention.
The nozzle assembly 10 further comprises a nozzle guide nut 52 which is cooperatively engaged to the valve stem 40 of the valve element 36 . When viewed from the perspective shown in FIGS. 2 , 5 and 6 , the nozzle guide nut 52 includes a generally cylindrical first, top portion 54 and a generally cylindrical second, bottom portion 56 . The outer diameter of the top portion 54 exceeds that of the bottom portion 56 , with the top and bottom portions 54 , 56 being separated from each other by a continuous, annular groove or channel 58 . The outer diameter of the bottom portion 56 is substantially equal to, but slightly less than, the diameter of the top section of the central bore 30 . As such, the bottom portion 56 of the nozzle guide nut 52 is capable of being slidably advanced into the top section of the central bore 30 .
The nozzle guide nut 52 further includes a bore which extends axially therethrough, and is sized to accommodate the advancement of a portion of the valve stem 40 through the nozzle guide nut 52 . More particularly, as seen in FIGS. 5 and 6 , the nozzle guide nut 52 is advanced over that portion of the valve stem 40 extending between the top flange portion 46 and the distal end of the valve stem 40 disposed furthest from the nozzle cone 38 . Such advancement is limited by the abutment of a distal, annular rim 60 defined by the bottom portion 56 of the nozzle guide nut 52 against a complimentary shoulder defined by the top flange portion 46 of the valve stem 40 . When such abutment occurs, the bore of the nozzle guide nut 52 , the central bore 30 of the nozzle housing 12 , and the valve stem 40 of the valve element 36 are coaxially aligned with each other.
In the nozzle assembly 10 , the nozzle guide nut 52 is maintained in cooperative engagement to the valve stem 40 through the use of a locking nut 62 and a complimentary pair of lock washers 64 . As seen in FIGS. 2 , 5 and 6 , the annular lock washers 64 are advanced over the valve stem 40 , and effectively compressed and captured between the locking nut 62 and an annular end surface 65 defined by the top portion 54 of the nozzle guide nut 52 . In this regard, a portion of the valve stem 40 proximate the distal end thereof is preferably externally threaded, thus allowing for the threadable engagement of the locking nut 62 thereto. The tightening of the locking nut 62 facilitates the compression and capture of the nozzle guide nut 52 between the lock washers 64 and top flange portion 46 of the valve stem 40 .
As indicated above, the valve element 36 of the nozzle assembly 10 is selectively moveable between a closed position (shown in FIGS. 1 , 2 and 5 ) and an open or flow position (shown in FIGS. 3 , 4 and 6 ). When the valve element 36 is in either of its closed or open positions, the biasing spring 50 is confined or captured within the top section of the central bore 30 , with one end of the biasing spring 50 being positioned against the shoulder 32 of the inner wall 26 , and the opposite end of the biasing spring 50 being positioned against the rim 60 defined by the bottom portion 56 of the nozzle guide nut 52 . Irrespective of whether the valve element 36 is in its closed or opened positions, at least the bottom portion 56 of the nozzle guide nut 52 remains or resides in the top section of the central bore 30 defined by the inner wall 26 of the nozzle housing 12 . Similarly, at least a portion of the bottom flange portion 48 of the valve stem 40 remains within the bottom section of the central bore 30 .
When the valve element 36 is in its closed position, a portion of the outer surface 42 of the nozzle cone 38 is firmly seated against the complimentary seating surface 22 defined by the nozzle housing 12 , and in particular the outer wall 24 thereof. At the same time, a substantial portion of the bottom flange portion 48 of the valve stem 40 resides within the bottom section of the central bore 30 , as does approximately half of the width of the channel 44 between the valve stem 40 and nozzle cone 38 . Still further, while the bottom portion 56 of the nozzle guide nut 52 resides within the top section of the central bore 30 , the channel 58 between the top and bottom sections 54 , 56 of the nozzle guide nut 52 does not reside within the central bore 30 , and thus is located exteriorly of the nozzle housing 12 . As previously explained, the biasing spring 50 captured within the top section of the central bore 30 and extending between the rim 60 of the nozzle guide nut 52 and the shoulder 32 of the nozzle housing 12 acts against the nozzle guide nut 52 (and hence the valve element 36 ) in a manner which normally biases the valve element 36 to its closed position.
In the nozzle assembly 10 , cooling water is introduced into each of the flow passage sections 18 a , 18 b , 18 c at the top end 14 of the nozzle housing 12 , and thereafter flows therethrough into the fluid chamber 20 . When the valve element 36 is in its closed position, the seating of the outer surface 42 of the nozzle cone 36 against the seating surface 22 blocks the flow of fluid out of the fluid chamber 20 and hence the nozzle assembly 10 . An increase of the pressure of the fluid beyond a prescribed threshold effectively overcomes the biasing force exerted by the biasing spring 50 , thus facilitating the actuation of the valve element 36 from its closed position to its open position. More particularly, when viewed from the perspective shown in FIG. 6 , the compression of the biasing spring 50 facilitates the downward axial travel of the nozzle guide nut 52 further into the top section of the central bore 30 , and hence the downward axial travel of the valve element 36 relative to the nozzle housing 12 . The downward axial travel of the nozzle guide nut 52 is limited by the abutment of a distal rim 66 of the inner wall 26 located at the top end 14 of the nozzle housing 12 against a complimentary shoulder 68 defined by the top portion 54 of the nozzle guide nut 52 proximate the channel 58 .
When the valve element 36 is in its open position, the nozzle cone 38 thereof and that portion of the nozzle housing 12 defining the seating surface 22 collectively define an annular outflow opening between the fluid chamber 20 and the exterior of the nozzle assembly 12 . The shape of such outflow opening, coupled with the shape of the nozzle cone 38 , effectively imparts a conical spray pattern of small droplet size to the fluid flowing from the nozzle assembly 12 . When the valve element 36 is in its open position, the bottom flange portion 48 of the valve stem 40 still resides within the bottom section of the central bore 30 , though the channel 44 resides predominantly within the fluid chamber 20 . Further, both the bottom portion 56 and channel 58 of the nozzle guide nut 52 reside within the top section of the central bore 30 . As will be recognized, a reduction in the fluid pressure flowing through the nozzle assembly 10 below a threshold which is needed to overcome the biasing force exerted by the biasing spring 50 effectively facilitates the resilient return of the valve element 36 from its open position shown in FIG. 6 back to its closed position as shown in FIG. 5 .
Importantly, fluid flow through the nozzle assembly 10 , and in particular the flow passage sections 18 a , 18 b , 18 c and fluid chamber 20 thereof, normally bypasses the central bore 30 . As previously explained, the top section of the central bore 30 is effectively cut off from fluid flow by the advancement of the bottom portion 56 of the nozzle guide nut 52 into the top section of the central bore 30 proximate the rim 66 of the inner wall 26 irrespective of whether the valve element 36 is in its closed or open positions, and the positioning of the bottom flange portion 48 of the valve stem 40 within the bottom section of the central bore 30 irrespective of whether the valve element 36 is in its open or closed positions. As a result, fluid flowing through the nozzle assembly 10 does not directly impinge the biasing spring 50 residing within the top section of the central bore 30 . Thus, even when the nozzle assembly 10 heats up to full steam temperature when no water is flowing and is shocked when impinged with cold water, the level of thermal shocking of the biasing spring 50 will be significantly reduced, thereby lengthening the life thereof and minimizing occurrences of spring breakage. Further, as is most apparent from FIGS. 2 , 4 and 7 , the inflow ends of the flow passage sections 18 a , 18 b , 18 c at the top end 14 of the nozzle housing 14 are radiused, which increases the capacity thereof. This shape of the inflow ends is a result of the use of the DMLS or casting process described above to facilitate the fabrication of the nozzle housing 12 .
In addition, in the nozzle assembly 10 , the travel of the valve element 36 from its closed position to its open position is limited mechanically by the abutment of the shoulder 68 of the nozzle guide nut 52 against the rim 66 of the inner wall 26 of the nozzle housing 12 in the above-described manner. This mechanical limiting of the travel of the valve element 36 eliminates the risk of compressing the biasing spring 50 solid, and further allows for the implementation of precise limitations to the maximum stress level exerted on the biasing spring 50 , thereby allowing for more accurate calculations of the life cycle thereof. Still further, the aforementioned mechanical limiting of the travel of the valve element 36 substantially increases the pressure limit of the nozzle assembly 10 since it is not limited by the compression of the biasing spring 50 . This also provides the potential to fabricate the nozzle assembly 10 in a smaller size to function at higher pressure drops, and to further provide better primary atomization with higher pressure drops. The mechanical limiting of the travel of the valve element 36 also allows for the tailoring of the flow characteristics of the nozzle assembly 10 , with the cracking pressure being controlled through the selection of the biasing spring 50 .
Referring now to FIG. 9 , it is contemplated that the valve element 36 and the nozzle guide nut 52 of the nozzle assembly 10 may optionally be provided with additional structural features which are specifically adapted to prevent any undesirable sticking of the valve element 36 during the reciprocal movement thereof between its closed and open positions. More particularly, it is contemplated that the bottom flange portion 48 of the valve stem 40 of the valve element 36 may include a series of elongate debris grooves 70 formed in the outer peripheral surface thereof, preferably in prescribed, equidistantly spaced intervals. As is apparent from FIG. 9 , the debris grooves 70 circumvent the entire periphery of the bottom flange portion 48 , and each extend in spaced, generally parallel relation to the axis of the stem portion 40 .
Similarly, the bottom portion 56 of the nozzle guide nut 52 may include a series of debris grooves 72 within the peripheral outer surface thereof, preferably in prescribed, equidistantly spaced intervals. The debris grooves 72 circumvent the entire periphery of the bottom portion 56 , and each extend in spaced, generally parallel relation to the axis of the bore of the nozzle guide nut 52 , and hence the axis of the valve stem 40 of the valve element 32 .
When the valve element 32 is in either its closed position (as shown in FIG. 9 ) or its open position, the debris grooves 70 , 72 effectively reduce the contact area between the nozzle guide nut 52 and the nozzle housing 12 , and further between the valve element 36 and the nozzle housing 12 , as reduces the likelihood of the valve element 36 sticking as a result of foreign particles. Though the debris grooves 70 , 72 may allow for some measure of the flow of cooling water into the top section of the central bore 30 and hence into contact with the biasing spring 50 therein, the amount of cooling water flowing into the top section of the central bore 30 is still insufficient to thermally shock the biasing spring 50 . The inclusion of the debris grooves 70 , 72 is particularly advantageous in those applications wherein the nozzle assembly 10 may be integrated into a system wherein large amounts of particulates are present in the cooling water.
Referring now to FIGS. 10 and 11 , in a conventional application, the nozzle assembly 10 is cooperatively engaged to a complimentary nozzle holder 74 . As indicated above, thermal cycling, as well as the high velocity head of steam passing through an attemperator including the nozzle assembly 10 , can potentially lead to the loosening thereof within the nozzle holder 74 resulting in an undesirable change in the orientation of the spray angle of cooling water flowing from the nozzle assembly 10 . To prevent any such rotation of the nozzle assembly 10 relative to the nozzle holder 74 , it is contemplated that the nozzle assembly 10 may be outfitted with a tab washer 76 which is shown in FIG. 11 in an original, unbent state. The tab washer 76 has an annular configuration and defines a multiplicity of radially extending tabs 78 which are arranged about the periphery thereof. As is apparent from FIG. 11 , one diametrically opposed pair of the tabs 78 is enlarged relative to the remaining tabs 78 .
When used in conjunction with the nozzle assembly 10 , the tab washer 76 , in its originally unbent state, is advanced over a portion of the nozzle housing 12 and rested upon an annular shoulder 80 which is defined thereby and extends in generally perpendicular relation to the above-described flats 34 . Thereafter, upon the advancement of the nozzle assembly 10 into the nozzle holder 74 , the enlarged tabs 78 of the tab washer 76 are bent in the manner shown in FIG. 10 so as to extend partially along and in substantially flush relation to respective ones of a corresponding pair of flats 82 formed in the outer surface of the nozzle holder 74 in diametrically opposed relation to each other. Of the remaining tabs 78 of the tab washer 76 , every other such tab 78 is bent in a direction opposite those engaged to the flats 82 so as to extend along and in substantially flush relation to corresponding ones of the flats 34 defined by the nozzle housing 12 . The bending of the tab washer 76 into the configuration shown in FIG. 10 effectively prevents any rotation of loosening of the nozzle assembly 10 relative to the nozzle holder 74 . Along these lines, though not shown in FIGS. 1-9 , it is contemplated that the portion of the outer surface of the housing 12 extending between the shoulder 80 and the top end 14 will be externally threaded as allows for the threadable engagement of the nozzle assembly 10 to complementary threads formed within the interior of the nozzle holder 74 . In this regard, the nozzle assembly 10 and the nozzle holder 74 are preferably threadably connected to each other, with the loosening of this connection as could otherwise be facilitated by the rotation of the nozzle assembly 10 relative to the nozzle holder 74 being prevented by the aforementioned tab washer 76 .
This disclosure provides exemplary embodiments of the present invention. The scope of the present invention is not limited by these exemplary embodiments. Numerous variations, whether explicitly provided for by the specification or implied by the specification, such as variations in structure, dimension, type of material and manufacturing process may be implemented by one of skill in the art in view of this disclosure.
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An improved spray nozzle assembly for use in a steam desuperheating device that is adapted to spray cooling water into a flow of superheated steam. The nozzle assembly is of simple construction with relatively few components, and thus requires a minimal amount of maintenance. In addition, the nozzle assembly is specifically configured to, among other things, prevent thermal shock to prescribed internal structural components thereof, to prevent “sticking” of a valve element thereof, and to create a substantially uniformly distributed spray of cooling water for spraying into a flow of superheated steam in order to reduce the temperature of the steam.
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BACKGROUND OF THE INVENTION
The present invention relates to a truss assembly and more particularly to a truss assembly which is constructed in a way so as to support a brick wall or other heavy mortar construction.
The most prevalent prior art is a continuous horizontal shelf angle, upon which brickwork is placed, and which is hung from the main building floor and roof steel. Vertical studs are fitted behind the hung angles and connected individually to the building steel and hung angle and braced to the building frame.
One problem with the prior art, steel support assembly is the cost of erecting the steel support and then attaching a brick or masonry wall to the steel support.
An object of the present invention is to minimize the cost of material and labor for constructing a brick wall and steel support assembly.
Another object of the present invention is to avoid complicated attachment parts for attaching the brick wall to the truss.
Another object of the present invention is to permit shop assembly of the truss, and to permit field assembly on the ground of the sheetrock and most attachment parts for the brick wall before lifting the truss into place.
Another object of the invention is to prevent cracking of the brick by removing support of the brick veneer from the floor and roof support beams, which deflect and move under service loads, and apply the support of the brick directly to the columns which are unyielding.
Another object of the present invention is the shop fabrication of the truss in one piece for quicker mounting, leveling, and attachment to the building.
Another object of the present invention is to improve the method of bracing the truss to the building concrete slab.
Another object is to eliminate the need for a separate concrete metal stop at the slab end and incorporate the concrete stop as part of the truss.
SUMMARY OF THE INVENTION
According to the present invention, a truss assembly for supporting a building, brick or masonry wall comprises a top and bottom chord; a plurality of vertical and diagonal stud members interconnected between the chords; and, a lintel angle, for supporting the brick wall, connected to the bottom of the stud members. Tieback members are secured to the truss assembly and hold the brick wall to the truss assembly. Vertical and horizontal adjustment of the truss can be accomplished insuring a level wall assembly. A further stud member spans the truss assembly horizontally. This provides the edge support for the interior concrete floor and facilitates the fabrication of the floor. Bracing is provided, between the column supports, by interconnecting members between the floor slab and the bottom portion of the truss assembly.
It should be understood that the facing material instead of brick can be stone, granite, slate, etc. tied back to the truss in similar manner.
The above advantages and the subsequent description will be more readily understood by reference to the following drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an elevation view of a truss assembly according to the present invention;
FIG. 2 is a section view as taken along the line 2--2 of FIG. 1;
FIG. 3 is an enlarged view of a portion of FIG. 2;
FIG. 4 is an enlarged view of another portion of FIG. 2 without the sheetrock and cap depicted;
FIG. 5 is an enlarged view of yet another portion of FIG. 2;
FIG. 6 is an enlarged view of a portion of FIG. 1;
FIG. 7 is a section view as taken along the line 7--7 of FIG. 6;
FIG. 8 is an enlarged view of another portion of FIG. 1;
FIG. 9 is a view as taken along the line 9--9 of FIG. 8;
FIG. 10 is a section view as taken along the line 10--10 of FIG. 1;
FIG. 11 is a section view as taken long the line 11--11 of FIG. 1;
FIG. 12 is an enlarged view of an alternate scheme to that depicted in FIG. 3.
DETAILED DESCRIPTION OF THE INVENTION
In FIG. 1, a truss structure assembly 10 is shown. Assembly 10 includes a truss structure or frame 12.
Truss 12 includes a bottom chord 16, a top chord 18, a plurality of vertical studs, 20, 22, 24, 26, 28, 30, 32, 34, 36, 38, 40, 42, 44, 46, 48, a plurality of intermediate diagonals, 50, 52, 54, 56, 58, 60, 62, 64, 66, 68, 70, 72, 74, 76 and a pair of end diagonals 78, 80. Truss 12 is preferably welded in the shop and delivered to the field for subsequent attachment of sheetrock, facing, etc.
Truss 12 is supported on end columns 82, 84, which have respective centerlines 86, 88.
Bottom chord 16, and top chord 18, are each a pair of structural angles welded back to back; or a "tee" section. The vertical studs 20 through 48, which are identical, are each a channel shaped sheet metal member as can be best appreciated from FIGS. 7 or 9. Diagonals 50 through 76, which are identical, are each a formed angle, such as a two and one half inch by two and one half inch structural angle.
Assembly 10 includes an exterior sheetrock 90, which is preferably field applied to the truss 12. Assembly 10 also includes an interior sheetrock 92, which is also field applied to truss 12, as shown in FIG. 2. Assembly 10 also has a sheet metal cap 94, which is field applied over top chord 18 if needed.
In FIGS. 2 and 4, top chord 18 is shown, and is preferably two, three inch by three inch structural angles that are disposed back to back, giving a "tee" appearance in section.
In FIGS. 2 and 5, bottom chord 16 is shown and has preferably the same size angles as top chord 18 and is connected similarly.
As shown typically in FIG. 4, stud 34 has a notch 96 in order to fit the angle legs of top chord 18. As can be seen in FIG. 5, the bottom of the various studs is likewise notched to fit the angle legs of the bottom chord. The studs are welded at top and bottom to the respective chords. As shown in FIGS. 6 and 7, diagonals 70 and 72, which are typical diagonals, are welded to top chord 18. As shown in FIG. 8, diagonals 68 and 70, again typical, are welded to bottom chord 16. Generally, the diagonals alternate on opposite sides of the chord centers (see FIG. 7).
For purposes of this description, wall 14 is a brick veneer. The wall has vertical rows of brick ties 98, which are field applied through the exterior sheetrock 90 to each of the studs 20 through 48, as shown in FIGS. 2 and 12.
Truss 12 has a lintel or shelf angle 100 for supporting the brick wall 14. Lintel 100, as shown in FIGS. 2 and 5, is welded to studs 20 through 48, and welded to bottom chord 16. The brick wall 14 is field applied and bears on lintel angle or plate, 100. It is retained in the vertical plane by the connection of the free end of brick ties 98 to the mortar between the bricks.
Sheetrock 90 and 92, generally, will have insulation batts 102 disposed therebetween. The batts are easily installed in the field between studs and the alternate location of the diagonals allows for installation of the standard size batts without a break in the insulation.
Truss 12 also has a horizontal stud 104 which is welded to studs 20 through 48. Generally, this is channel shaped as shown.
As shown in FIGS. 10 and 11, truss 10 has top end members, e.g. 106, which are connected to the chord member 18 at its ends. A seating bracket 107 is welded to column 82 and is positioned to provide a seat for member 106.
Member 106 sits on bracket 107 and includes a pair of bolt openings 108 which align with slotted holes 109 in bracket 107.
A support angle bracket 110 is also welded at the bottom of the supporting columns, e.g. 82. The support brackets include a vertical face 111 having a bolt hole 112 which is used to secure the truss assembly lintel 100, thereto. The latter also includes a bolt hole 113 which, in set up, aligns with opening 112.
Shims can be used in the spaces 114 and 115. These, together with the slotted holes allow for both vertical and horizontal adjustment of the truss assembly during field assembly.
As shown in FIG. 2 and in greater detail in FIG. 5, lintel 100 is welded to bottom chord 16. Stud 34 is welded to bottom chord 16. The depth of stud 34 is approximately six inches and the distance from the outside face of brick wall 14 to the outside face of stud 34 approximately five inches. Lintel 100 is also welded to the flange of stud 34 for the height of the lintel.
Referring once again to FIG. 2, building 15 includes a composite floor system 116 such as described in applicant's U.S. Pat. Nos. 4,259,822 or 4,295,310. Such systems include typically a concrete slab layer 117 and an underhanging chord assembly 118. The latter is connected to the slab layer via joist webbing 119. The system rests on a truss or beam supporting joist (e.g., an H beam) 120, which spans columns 82 and 84 near or on the centerline, 86, 88, thereof.
Interconnecting the floor system 116 to the truss assembly 10 is a top connecting plate 121. This typically is welded to and spans from a webbing member, 118a, over and behind horizontal stud 104. Typically it is a piece of strap sheet metal (i.e., 2" wide) located at every floor joist or every other joist.
Interconnecting the system 116 to the bottom of horizontal stud 104 is a form work or plate 122. This spans between truss or beam 120 and the bottom upwardly extending channel of stud 104. The plate acts to prevent excessive leakage of concrete, when poured, below the floor level. In applicant's prior systems identified above, particularly the one described in U.S. Pat. No. 4,259,822, the portion of the pan member normally disposed on the beam, can be extended beyond the lower channel of stud 104 to effect the purposes of the form work (see FIG. 3, pan member 124).
After the truss is erected and secured in place, it may require temporary bracing until the slab is poured on the corrugated decking of the composite floor system. This is accomplished by top connecting flange 121 and bracing bars such as shown at 126. The latter are welded to chord assembly 118 on the one end and either joist 120, brace support plate, 129, or some appropriate place along the inside vertical face of the truss; or the floor beams. The top connecting strap 121 becomes encased in concrete; and the bottom brace members can be left in permanently.
Channel, or stud member, 104 serves as a level screed line to which the concrete is poured. It also serves as an edge form to contain the concrete. The horizontal stud allows for vertical deflection of the floor while the concrete is being poured. When the concrete hardens, the vertically extending members 128 and 130, of the channel 104 engage the concrete and the concrete slab automatically gives a secure lateral tie between the truss and slab with no further field connection. I.e., there is no direct structural connection between the truss and the floor members other than bracing. This is important, because the truss is extremely stiff in a vertical direction and the floor member is considerably less stiff. Without the isolation there would be a transmission of unwanted loading to the truss assembly.
It may be desirable to allow some subsequent movement between the slab and the truss assembly after the concrete hardens. This facilitates top and bottom chord lateral adjustment. To accomplish this a less rigid connection of the horizontal stud 104 to the vertical studs 20, 22, etc., is necessary. This can be accomplished using the scheme shown in FIG. 12. Here sheet metal clip angles 132 are employed. This is a more flexible scheme than the direct weld. Realignment of both the top and bottom chords laterally can be accomplished by adjustment of the bracing 126. The more flexible clip angle allows for some rotation of the studs at the floor line.
Although one embodiment has been described particularly, of course the present invention is not to be considered as limited thereto. Alternate embodiments reflecting the breadth of the invention as defined by the scope of the appended claims should now be apparent in view of the above and of course are intended to be covered by the claimed invention.
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A truss assembly for supporting a building brick or masonry wall comprising a top and bottom chord, a plurality of vertical and diagonal stud members interconnected between the chords; and a lintel angle, for supporting the brick wall, connected to the bottom of the stud members at least. Tieback members are provided which secure the wall to the truss assembly. Adjustment provisions allow aligning the truss assembly both vertically and horizontally before the wall is constructed. A further stud member spans the truss assembly horizontally and provides a physical connection between the truss and the concrete floor systems. Bracing is provided between the column supports, by interconnecting members between the floor slab and the bottom portion of the truss assembly.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a continuation in part of, and claims priority to, Applicant's co-pending, commonly owned U.S. patent application Ser. No. 14/014,658, filed Aug. 30, 2013, which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to determination or mapping of reservoir pressure over a region of interest in a subsurface reservoir with integration of static bottom-hole pressure survey data and simulation modeling.
[0004] 2. Description of the Related Art
[0005] In the oil and gas industries, massive amounts of data are required to be processed for computerized simulation, modeling and analysis for exploration and production purposes. For example, the development of underground hydrocarbon reservoirs typically includes development and analysis of computer simulation models of the reservoir. These underground hydrocarbon reservoirs are typically complex rock formations which contain both a petroleum fluid mixture and water. The reservoir fluid content usually exists in two or more fluid phases. The petroleum mixture in reservoir fluids is produced by wells drilled into and completed in these rock formations.
[0006] A computer reservoir model with realistic geological features and properties, appropriate distribution of in-situ fluids, as well as initial pressure conditions of the fluids also help in forecasting the optimal future oil and gas recovery from hydrocarbon reservoirs. Oil and gas companies have come to depend on such models as an important tool to enhance the ability to exploit a petroleum reserve.
[0007] It is desirable to be able to monitor pressure conditions in such a reservoir so that production is optimized. Adjustments can be made in production or injection rates to remove undesirable high or low pressure regions that might be observed from such monitoring. For reservoir planning purposes, the reservoir is simulated in a computer and runs are made of estimated production for a range of times over the projected life of the reservoir.
[0008] In simulation models, the reservoir is organized into a number of individual cells. Seismic data with increasing accuracy has permitted the cells to be on the order of 25 meters areal (x and y axis) intervals. For what are known as giant reservoirs, the number of cells is at least hundreds of millions, and reservoirs of what is known as giga-cell size (a billion cells or more) are encountered.
[0009] An example reservoir of the type for which production data are simulated over the expected reservoir life as illustrated by the model M ( FIG. 1 ) is usually one which is known to those in the art as a giant reservoir. A giant reservoir may be several miles in length, breadth and depth in its extent beneath the earth and might, for example, have a volume or size on the order of three hundred billion cubic feet.
[0010] The reservoir is organized into a matrix which corresponds to the three dimensional extent of the reservoir and is composed of a number of contiguous 3-dimensional cells. It is common for a reservoir matrix to contain millions of cells to obtain as accurate an indication of reservoir conditions as feasible. Actual reservoir models may have several millions of such cells.
[0011] For reservoirs of this type, the actual number of wells may also be on the order of a thousand, with each well having a number of perforations into producing formations. Typically, not all of the wells in a reservoir have what are known as permanent downhole pressure gauges in them to monitor reservoir at those locations. This however represents a pressure measurement at only one point in the huge volume of the reservoir.
[0012] Thus, only a relatively small number of wells in a reservoir have such pressure gauges and as mentioned, the reservoir may have a substantial extent in terms of subsurface breadth, width and depth, leading to a very large number of cells in the model. The data points are extremely scarce when compared to the reservoir volume.
[0013] Therefore, the conditions and spatial quantity under which the actual well pressure is measured are completely different than the reservoir pressure which reservoir engineers are interested in for reservoir production optimization. Pressure measurements at the limited number of wells having gauges in the reservoir do not provide an accurate indication of reservoir pressure conditions of interest over the full 3-dimensional extent of the reservoir.
[0014] So far as is known, in previous isobaric mapping techniques, the well's static bottom-hole pressure (SBHP) readings were used to generate isobaric maps. Each SBHP reading was a control point based on which the isobaric map was generated. The interpolation between the control points was a simple linear interpolation that did not account for geological features or for reservoir dynamics during production.
SUMMARY OF THE INVENTION
[0015] Briefly, the present invention provides a new and improved computer implemented method of forming a two-dimensional pressure map with a data processing system of reservoir pressures in a region of interest in a subsurface hydrocarbon producing reservoir partitioned for modeling purposes into a reservoir model partitioned as an array of a grid of cells extending over the three dimensions of the reservoir, the reservoir having a plurality of wells with perforations for fluid passage from the reservoir into the wells, with selected ones of the wells having downhole pressure measurement systems installed therein, the array of a grid of cells of the reservoir model comprising well cells at the locations of the wells and reservoir cells at the remaining cells of the grid.
[0016] The computer processing receives pressure data from the wells based on measurements from the downhole pressure measurement systems, and performs simulated pressure calculations on a reservoir simulator in the data processing system for the cells in an array of well cells for an area of interest of the reservoir. Well cells at an uppermost perforation of each of the wells are populated with assigned pressure values from the received pressure data. Pressure values are propagated for the well cells of the wells below the uppermost perforations and for the reservoir cells of the area of interest to form a three-dimensional grid pressure array for the area of interest. The three-dimensional grid pressure array is then collapsed or transformed to a two-dimensional layer of pressure values for the region of interest. The two-dimensional layer of pressure values for the region of interest are assembled in memory of the data processing system and an output image map is formed of the two-dimensional layer of pressure values for the region of interest.
[0017] The present invention also provides a new and improved data processing system for forming a two-dimensional pressure map with a data processing system of reservoir pressures in a region of interest in a subsurface hydrocarbon producing reservoir partitioned for modeling purposes into a reservoir model partitioned as an array of a grid of cells extending over the three dimensions of the reservoir, the reservoir having a plurality of wells with perforations for fluid passage from the reservoir into the wells, with selected ones of the wells having downhole pressure measurement systems installed therein, the array of a grid of cells of the reservoir model comprising well cells at the locations of the wells and reservoir cells at the remaining cells of the grid.
[0018] The data processing system includes a processor which receives pressure data from the wells based on measurements from the downhole pressure measurement systems, and performs simulated pressure calculations on a reservoir simulator in the data processing system for the cells in an array of well cells for an area of interest of the reservoir. The processor then populates well cells at an uppermost perforation of each of the wells with assigned pressure values from the received pressure data, and propagates pressure values for the well cells of the wells below the uppermost perforations and to the reservoir cells of the area of interest to form a three-dimensional grid pressure array for the area of interest. The processor then reduces the three-dimensional grid pressure array to a two-dimensional layer of pressure values for the region of interest, and assembles in memory of the data processing system the measure of two-dimensional layer of pressure values of the region of interest. The data processing system also includes a memory storing the two-dimensional layer of pressure values for the region of interest an output display forming a display of the two-dimensional layer of pressure values for the region of interest of the reservoir.
[0019] The present invention also provides a new and improved data storage device which has stored in a computer readable medium non-transitory computer operable instructions for causing a data processing system to form a two-dimensional pressure map with a data processing system of reservoir pressures in a region of interest in a subsurface hydrocarbon producing reservoir partitioned for modeling purposes into a reservoir model partitioned as an array of a grid of cells extending over the three dimensions of the reservoir. The reservoir has a plurality of wells with perforations for fluid passage from the reservoir into the wells, with selected ones of the wells having downhole pressure measurement systems installed therein, the array of a grid of cells of the reservoir model comprising well cells at the locations of the wells and reservoir cells at the remaining cells of the grid.
[0020] The instructions stored in the data storage device cause the data processing system to receive pressure data from the wells based on measurements from the downhole pressure measurement systems, and perform simulated pressure calculations on a reservoir simulator in the data processing system for the cells in an array of well cells for an area of interest of the reservoir. The instructions also cause the data processing system to populate well cells at an uppermost perforation of each of the wells with assigned pressure values from the received pressure data, and then propagate pressure values for the well cells of the wells below the uppermost perforations and to the reservoir cells of the area of interest to form a three-dimensional grid pressure array for the area of interest. The instructions further cause the data processing system to reduce the three-dimensional grid pressure array to a two-dimensional layer of pressure values for the region of interest, and assemble in memory of the data processing system the two-dimensional layer of pressure values for the region of interest, then form an output image map of the two-dimensional layer of pressure values for the region of interest.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] FIG. 1 is a schematic diagram of a model of a subsurface hydrocarbon reservoir.
[0022] FIG. 2 is a schematic diagram showing a pressure downhole measuring system installed in a selected number of wells in the reservoir of FIG. 1 .
[0023] FIG. 3 is a functional block diagram of a set of data processing steps performed in a data processing system for two dimensional reservoir pressure estimation with integrated static bottom-hole pressure survey data and simulation modeling according to the present invention.
[0024] FIGS. 4, 5 and 6 are functional block diagrams of a set of data processing steps performed in connection with processing according to FIG. 3 .
[0025] FIGS. 7A, 7B and 7C are schematic diagrams of grid cells of a subsurface reservoir model illustrative of the workflow according to FIGS. 3 and 4 for propagating pressure determinations to each perforation in a vertical well.
[0026] FIGS. 8A and 8B are schematic diagrams of grid cells of a subsurface reservoir model illustrative of the workflow according to FIGS. 3 and 5 for propagating pressure determinations for a single perforation in a vertical well to other grid cells in the reservoir.
[0027] FIG. 9 is a schematic diagram of a subsurface reservoir model illustrative of the workflow according to FIGS. 3 and 6 for propagating pressure determinations for a single perforation in a horizontal well to other grid cells in the reservoir.
[0028] FIGS. 10A and 10B are schematic diagrams illustrating notations for directions and for grid nomenclature in a reservoir model.
[0029] FIG. 11 is a schematic block diagram of a data processing system for two dimensional reservoir pressure estimation with integrated static bottom-hole pressure survey data and simulation modeling according to the present invention.
[0030] FIG. 12 is an example simulated plot of a 2-dimensional isobaric pressure map based on governing reservoir actual thermodynamics and geophysics relationships according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0031] In the drawings, the letter M designates a simplified model of a portion of a subsurface hydrocarbon reservoir for which production results based on operating conditions and parameters are simulated over an estimated production life according to the present invention based on geological and fluid characterization information obtained for the cells of the reservoir. The results obtained are thus available and used for simulation of historical performance and for forecasting of production from the reservoir. Based on the results of such simulation, models such as those described and shown in U.S. Pat. No. 7,526,418 are then formed and are available for evaluation and analysis. U.S. Pat. No. 7,526,418 is owned by the assignee of the present invention and is incorporated herein by reference.
[0032] For a giant reservoir, the physical size of the reservoir may be several miles in length, breadth and depth in its extent beneath the earth and might, for example, have a volume or size on the order of three hundred billion cubic feet. The number of cells for a reservoir of this size is, for example, typically on the order of hundreds of millions.
[0033] For reservoirs of this type, the actual number of wells may also be on the order of a thousand, with each well having a number of perforations into producing formations. Typically, a limited number of the wells in a reservoir have what are known as permanent downhole pressure gauges in them to monitor reservoir at those locations. This, however, represents a pressure measurement at only one point in the volume of the reservoir.
[0034] Thus, only key wells in a reservoir have such pressure gauges and as mentioned, the reservoir may have a substantial extent in terms of subsurface breadth, width and depth, leading to a very large number of cells in the model. The reservoir pressure data points are extremely scarce when compared to the reservoir volume.
[0035] FIG. 2 illustrates an example placement of a group G of wells W from a portion of a large reservoir R of the type and size exemplified by the model M of FIG. 1 . The wells in the group G typically include production wells, injection wells and observation wells and are spaced over the extent of the reservoir. As indicated, certain ones of the wells W represented by the group G are provided with permanent downhole measurement systems 20 , which are known as PDHMS. The PDHMS 20 may, for example be of the type described in U.S. Pat. Nos. 8,078,328 and 8,312,320, commonly owned by the assignee of the present application. The subject matter disclosed in U.S. Pat. Nos. 8,078,328 and 8,312,320 is incorporated herein by reference.
[0036] The PDHMS 20 include surface units which receive reservoir and well data in real time from downhole sensors 22 . The downhole sensors 22 obtain data of interest, and for the purposes of the present invention the downhole sensors include downhole pressure and temperature sensors located in the wells W at selected depths and positions in the selected group G of wells among the much larger number of wells in the reservoir.
[0037] The downhole sensors 22 furnish the collected real-time pressure and temperature data from the wells W in which they are installed, and a supervisory control and data acquisition (SCADA) system with a host computer or data processing system D ( FIG. 4 ) collects and organizes the collected data form the wells in the group G. The PDHMS 20 also includes sensors to record production and injection data for the injection wells in the group G, which data is also collected and organized by the supervisory control and data acquisition.
NOMENCLATURE
[0038]
[0000]
P av
Average reservoir pressure
P colav
Average reservoir pressure for a column of grid blocks
P SBHP
Static Bottom-hole pressure
ΔP cf
Pressure correction factor for a column of cells
P cal
i-Reservoir calculated pressure
(PV i )
Pore volume of cell or grid block i, where i = 1, 2 . . . n
(BV) i
Bulk Volume of cell or grid block i, where i = 1, 2 . . . n
PV i =
(Gridblock Bulk Volume) * porosity of grid block i where
(BV) I * Ø i
i = 1, 2 . . . n
(S w ) i
Water saturation
(1 − S w ) i
Hydrocarbon Saturation at grid block i where i = 1, 2 . . . n
I
Grid block index in x-direction with reference to a layer
in the 3D reservoir grid
J
Grid block index in y-direction with reference to a
layer in the 3D reservoir grid
K
Grid block index in z-direction with reference to a column
in the 3D reservoir grid
SUBSCRIPTS
[0039]
[0000]
C:
column
cf:
correction factor
cal:
calculated
colav:
column average
e:
grid block index
av:
average
i:
grid block index
s:
start
w:
water
HC:
hydrocarbon
avHC:
hydrocarbon weighted average
avWC:
average pressure above contacts (free phase table)
avHCWC:
hydrocarbon average above contacts (free phase table)
[0040] Turning to FIG. 3 , a flow chart F displays a set of processor steps performed according to the methodology of the present invention in a data processing system D ( FIG. 10 ) for three-dimensional reservoir pressure determination using real time pressure data from downhole gauges and reservoir simulation values determination to determine and form 2-dimensional isobaric pressure maps according to the present invention. The flowchart F indicates the basic computer processing sequence of the present invention and the computation taking place in the data processing system D for the 3-dimensional pressure determination reservoir simulation and map formation according to the present invention.
[0041] Processing according to the flow chart F of FIG. 3 is performed in conjunction with results of processing according to Applicant's co-pending, commonly owned U.S. patent application Ser. No. 14/014,658, filed Aug. 30, 2013, and in particular to the determination of an i-Reservoir calculated pressure P cal and the pressure gradients between cells of the reservoir model. In connection with the processing according to the flow chart F, certain input parameters are provided as indicated at step 30 by users interested in reservoir management according to the present invention. The input parameters are identifications of each of the following: Field, Reservoir(s), Pressure Survey Data (SBHP), and Target Date for which a two dimensional reservoir pressure estimation map is to be formed.
[0042] As shown at step 32 , input perforation and production/injection data obtained by the reservoir simulator R in the data processing system D are also provided and subjected to quality checking as shown at step 34 . The reservoir simulation model is thus updated with the latest perforations and production/injection data for the wells of interest in the reservoir or field.
[0043] The reservoir simulation is then performed by reservoir simulator R ( FIG. 10 ) during step 36 with the quality-checked and verified updates to perforation and production/injection data which have been updated during step 34 to the date of interest. During step 36 , pressure gradients between the reservoir model grid blocks or reservoir cells of the model M are determined according to the techniques of U.S. patent application Ser. No. 14/014,658, mentioned above. The gradients between grid blocks are indicative of pressure changes in the reservoir due to geological heterogeneity, fluid dynamics, model constrains, and production/injection activities.
[0044] During step 38 , the pressure gradients determined by reservoir simulator R as a result of step 36 are evaluated. In the evaluation during step 38 , a perforation file of the reservoir data in the reservoir data is parsed and stored. The perforation file is also sorted by depth for each well in the reservoir. Pressure survey or SBHP survey data is also parsed and stored during step 38 , as is needed data, which include samples of SBHP and of perforation data from the reservoir simulation model output. Inactive cells which are to be excluded from processing computation are then identified during step 38 and then discarded along with their data content.
[0045] In step 39 , pressure survey data obtained from the reservoir in the manner described above as illustrated schematically in FIG. 2 is then used to determine reservoir pressure values at well top perforations of the wells 22 in the reservoir according to the techniques of U.S. patent application Ser. No. 14/014,658, mentioned above. Then, in step 40 , pressure values are propagated for each of the perforations of each of the wells 22 .
[0046] According to the present invention, there are three methods of performing step 40 for propagation of pressure values based on pressure survey data to be propagated to the perforations in the reservoir model and further to the reservoir models cells away from one or more of the wells. They are: an All Perforation Method as indicated schematically at 42 in FIG. 4 ; a Single Perforation Column Method shown schematically at 44 in FIG. 5 ; and an All-Perforation Column Method shown at 46 in FIG. 6 .
All Perforation Method
[0047] As shown in FIG. 4 , the All Perforation processing 42 begins with step 48 where SBHP values are assigned to the first or uppermost perforation in a well. During step 50 , measures from the simulation model of pressure gradient between the perforated cells are used to propagate pressure calculation successively from the first or uppermost cells to last lowest cells in the well. All perforations thus used are control points used in step 52 to propagate pressure assignments to non-perforated cells according to suitable statistical methods as describe in U.S. patent application Ser. No. 14/014,658. A suitable such method is that known as Distance-Weighted Moving Average or DWMA.
[0048] As shown schematically in FIG. 7A , during All Perforation processing step 42 SBHP values are assigned to the first or uppermost perforation 54 in an example vertical well 56 . FIG. 7B illustrates schematically lower performance of step 52 , where pressure gradient measures for reservoir simulation are successively propagated from perforation 54 successively to lower perforations 58 and 60 . Since inactive cells have, as described above, been excluded from processing, perforations 54 , 58 and 60 are shown vertically adjacent each other in FIGS. 7A, 7B and 7C . FIG. 7C illustrates schematically the assignment of pressure values to non-perforated cells 62 according to Distance-Weighted Moving Average or DWMA methods, as will be described.
Single-Perforation Column Method
[0049] In the Single-Perforation Column Method shown at 64 ( FIG. 5 ), only a first perforation of 56 well is considered as the pivot for calculating pressure along the well and away from it. As shown in FIG. 5 , the All Perforation processing 64 begins with step 66 where after the first perforation is identified and the column of cells where, the first perforation is located is marked, the average column pressure (P colav ) is determined from the simulation model:
[0000]
P
colav
=
∑
i
=
1
c
(
P
i
)
c
[0050] During step 68 , a correction factor (ΔP cf ) is determined by subtracting the pressure survey reading SBHP (P SBHP ) from the average column pressure P sim ) determined during step 66 :
[0000] Δ P cf =P colav −P SBHP
[0051] During step 70 , for each cell pressure value from simulation model, the correction factor (ΔP cf ) is subtracted from cell pressure (P sim ) and the resultant i-Reservoir calculated pressure value P cal assigned to i-Reservoir grid pressure, as follows:
[0000]
P
cal
=P
sim
−ΔP
cf
[0052] In this manner pressure for each of the grid blocks is determined. FIG. 8A illustrates schematically the Single-Perforation Column Method step 64 where average column pressure measures as shown at 72 are determined and a pressure correction factor is subtracted as indicated at 74 resulting in an i-Reservoir pressure as shown at 76 and 78 for different cells in a column 80 .
[0053] FIG. 8B illustrates schematically step 82 where the resultant i-Reservoir calculated pressure value P cal is determined for the cells 84 of the grid of the simulation model M. As a result, the average column pressure is the (P SBHP ).
All-Perforation Column Method
[0054] For the All-Perforation Column Method as shown at 84 ( FIG. 6 ), each of the i perforations of a well are considered for calculating pressure along the well and away from it. The perforations of a well are identified, and measures of pressure along the perforations are determined according to the Single-Perforation Column Method described above. As shown in FIG. 6 , the All Perforation processing begins with step 86 , where the average column pressure (P colayv i ) is determined for the perforations of each column i from the simulation model:
[0000]
(
P
colav
i
)
=
∑
i
=
1
c
(
P
i
)
c
[0055] During step 88 , a correction factor (ΔP cf i ) is determined for each column i by subtracting the pressure survey reading SBHP (P SBHP ) from the average column pressure (P colav i ) determined during step 86 :
[0000] Δ P cf i =P colav i −P SBHP
[0056] Then, during step 90 , for each column i and for each cell pressure value from simulation model in that column, the correction factor (ΔP cf i ) is subtracted from cell pressure (P sim ) and assigned as the pressure value P cal to i-Reservoir grid pressure:
[0000]
P
cal
=P
sim
−ΔP
cf
i
[0057] Next, in step 92 , pressure assignments are determined and propagated to the remained or non-perforated grid blocks according to suitable statistical methods as described in U.S. patent application Ser. No. 14/014,658. For a vertical well, the All-Perforation Column Method produces the same results as the Single-Perforation Column Method, as illustrated schematically in FIGS. 8A and 8B and described above.
[0058] FIG. 9 illustrates schematically the All-Perforation Column Method step 84 ( FIG. 6 ) for a horizontal well model 93 having a plurality of well perforations 94 as shown. In step 92 of the All-Perforation Column Method, pressure assignments are determined and propagated to the remained or non-perforated grid blocks 95 ( FIG. 9 ) of the horizontal well model 93 according to suitable statistical methods as described in U.S. patent application Ser. No. 14/014,658, as indicated schematically at 96 .
[0059] After performance of step 40 ( FIG. 3 ) for pressure computation along the well completions of a selected one of the three alternatives: All Perforation Method; Single-Perforation Column Method or All-Perforation Column Method in the manner described above, the reservoir model has been adjusted. The reservoir model M indicates propagated pressure measures which incorporate measured reservoir pressures as adjusted to indicate the effects of physics and geology on the reservoir and its fluids indicated by reservoir simulation processing.
[0060] During step 97 ( FIG. 3 ), a user is able to specify one of several techniques for data filtering, such as the type known as a Distance Weighted Moving Average or DWMA. The DWMA filtering is a nonlinear filter, designed to be a robust version of a traditional moving average. DWMA filtering is then performed during step 98 to reduce the impact of outlier propagated pressure measures in the reservoir model data. The result of step 98 , as indicated at 100 is a 3-dimensional pressure array of reservoir pressure data which is stored for further processing by the data processing system D.
[0061] The 3-dimensional grid pressure array indicated at 100 is then in step 102 according to the present invention collapsed or changed in format from a 3-dimensional pressure array to 2-dimensional pressure of a region of interest (or entirety of the reservoir) in the reservoir M. There are a number of methods of collapsing the 3-dimensional grid to 2-dimensional maps, the simplest being simple averaging of the propagated pressure measures of the model adjacent the various specified map co-ordinates for 2-dimensional map being formed.
[0062] Preferably, however, one of several forms of Pore-Volume Weighted Averaging for step 102 is utilized for collapsing the 3-dimensional grid to a 2-dimensional map of the region of interest. Examples of such pore-volume weighted averaging to indicate average reservoir pressure for 2-dimensional isobaric maps are set forth below. Reference is made to the Nomenclature Section for an explanation of the physical measures indicated in the relationships of pore-volume weighted averaging expressed.
Pore-Volume Weighted Average Reservoir Pressure
[0063]
P
av
=
∑
i
=
1
n
(
P
i
(
PV
i
)
)
∑
i
=
1
n
(
PV
i
)
Hydrocarbon Pore-Volume Weighted Average Reservoir Pressure
[0064]
P
avHC
=
∑
i
=
1
n
(
P
i
[
(
PV
)
i
*
(
1
-
S
w
)
i
]
)
∑
i
=
1
n
(
PV
)
i
Pore-Volume Weighted Average Reservoir Pressure Above Free Water Table
[0065]
P
avWC
=
∑
i
=
1
n
(
P
i
(
PV
i
)
)
∑
i
=
1
n
(
PV
i
)
[0000] where i is the index of all grid block with depth greater than the specified contact's depth.
Hydrocarbon Pore-Volume Weighted Average Reservoir Pressure Above Free Water Table
[0066]
P
avHCWC
=
∑
i
=
1
n
(
P
i
[
(
PV
)
i
*
(
1
-
S
w
)
i
]
)
∑
i
=
1
n
(
PV
)
i
[0000] where i is the index of all grid block with depth greater than the specified contact's depth.
[0067] As mentioned a user engineer or analyst is able to select an area of interest in the reservoir model M for which an isobaric 2-dimensional pressure map is to be formed. The display is formed by the data processing system D during performance of step 104 of FIG. 3 . For this processing step, an engineer can specify an area of interest using an n-sided polygon where all variety of isobaric maps can be generated as indicated at step 106 along with average reservoir pressure calculations.
[0068] As shown in FIG. 12 , an example plot 140 represents a simulated 2-dimensional isobaric pressure map which could be obtained according to the present invention based on governing equations and relationships for a selected area of interest, and representing the interplay of principles of thermodynamics and geophysics formed according to the present invention.
[0069] Example values of SBHP survey data and sample perforation location data according coordinates for perforations are set forth below:
[0000]
Sample SBHP Survey Data
FIELD
WELL NO.
Oct. 1, 2015
ABCD
1
1500
ABCD
2
1300
ABCD
3
2000
ABCD
4
1655
ABCD
5
1582
ABCD
6
1340
ABCD
7
1790
ABCD
8
2469
ABCD
9
4467
ABCD
10
1200
ABCD
11
1400
ABCD
12
4500
ABCD
13
3000
ABCD
14
1500
ABCD
15
4064
ABCD
16
3261
ABCD
17
2531
ABCD
18
5092
ABCD
19
2452
ABCD
20
2401
ABCD
21
2244
ABCD
22
2194
WELLS_BLOCK
WELL_Name=ABCD0001
PERF I=301 J=71 K=51 Rf=1.0 CD=‘Z’ Skin=1.0/MDEPTH=3873.5
PERF I=301 J=71 K=52 Rf=1.0 CD=‘Z’ Skin=2.0/MDEPTH=3880.5
PERF I=301 J=71 K=53 Rf=1.0 CD=‘Z’ Skin=1.0/MDEPTH=3887.5
PERF I=301 J=71 K=54 Rf=1.0 CD=‘Z’ Skin=0.0/MDEPTH=3898.5
PERF I=301 J=71 K=55 Rf=1.0 CD=‘Z’ Skin=0.0/MDEPTH=3913.5
PERF I=301 J=71 K=56 Rf=1.0 CD=‘Z’ Skin=0.0/MDEPTH=3928.5
PERF I=301 J=71 K=57 Rf=1.0 CD=‘Z’ Skin=1.0/MDEPTH=3941.5
WELL_Name=ABCD0002
PERF I=101 J=71 K=41 Rf=1.0 CD=‘Z’ Skin=0.0/MDEPTH=4873.0
PERF I=101 J=71 K=42 Rf=1.1 CD=‘Y’ Skin=0.0/MDEPTH=4880.0
PERF I=101 J=71 K=43 Rf=1.0 CD=‘Z’ Skin=0.0/MDEPTH=4887.0
PERF I=101 J=71 K=44 Rf=1.0 CD=‘Z’ Skin=0.0/MDEPTH=4898.0
PERF I=101 J=71 K=45 Rf=1.2 CD=‘Y’ Skin=0.0/MDEPTH=4913.0
PERF I=101 J=71 K=46 Rf=1.0 CD=‘Y’ Skin=0.0/MDEPTH=4928.0
PERF I=101 J=71 K=47 Rf=1.3 CD=‘Z’ Skin=0.0/MDEPTH=4941.0
ENDWELLS_BLOCK
DATE Dec. 1, 2010
WELLS_BLOCKS
WELL_Name=ABCD0005
PERF I=20 J=113 K=83 Rf=1.0 CD=‘Z’ Skin=0.0/MDEPTH=3890.50
PERF I=21 J=113 K=83 Rf=1.1 CD=‘X’ Skin=0.0/MDEPTH=3900.50
PERF I=21 J=113 K=84 Rf=1.0 CD=‘Z’ Skin=0.0/MDEPTH=3887.50
PERF I=22 J=113 K=81 Rf=1.0 CD=‘X’ Skin=3.0/MDEPTH=3887.50
PERF I=30 J=113 K=81 Rf=1.2 CD=‘X’ Skin=0.0/MDEPTH=3887.50
PERF I=31 J=113 K=83 Rf=1.0 CD=‘X’ Skin=0.0/MDEPTH=3887.50
PERF J=32 J=113 K=83 Rf=1.3 CD=‘Z’ Skin=0.0/MDEPTH=3890.50
ENDWELLS_BLOCK
[0070] As can be seen in FIG. 12 , the map plot 140 indicates by x, y co-ordinates the location in a reservoir model M of a selected area of interest and by contour lines 142 , areas of common isobaric pressures at the location. Indications of pressures represented as the 2-dimensional isobaric pressure areas in the reservoir map 140 may be indicated by variations in color, as schematically shown by varying stipple patterns in areas of common pressure within the contour lines. The pressures displayed indicate reservoir pressures over the area of interest while also taking into account geological features, aerial and vertical heterogeneity, and numerical model constraints. The maps formed according to the present invention are not merely estimates of reservoir pressures based only on readings from pressure measurement instrumentation located at a limited number of wells in a reservoir.
[0071] FIG. 10A is a graphical depiction of an example specification of I, J, and K co-ordinates, having reference to FIG. 10B for the orientation of the axial disposition of the co-ordinates. Set forth below are examples of numerical dimensions.
Example 1
[0072] The area of interest, given model dimensions (I×J×K): 500×300×200, is bounded by 4-sided polygon indicated by these two corners (1, 1, 1) and (500, 300, 200) is basically the whole reservoir. Therefore the numerical co-ordinates of the user-specified region of interest in the reservoir model M are as set forth below in Table 1:
[0000]
TABLE 1
1
1
1
300
1
200
500
500
1
300
1
200
1
500
1
1
1
200
1
500
300
300
1
200
Example 2
[0073] The area of interest, given model dimensions (I×J×K): 500×300×200 is bounded by corners (1, 50, 10) and (350, 100, 190). The numerical co-ordinates of the user-specified region of interest in the reservoir model M are as set forth below in Table 2:
[0000]
TABLE 2
1
1
50
100
10
190
350
350
50
100
10
190
1
350
50
50
10
190
1
350
100
100
10
190
[0074] As illustrated in FIG. 11 , the data processing system 1 ) according to the present invention includes a computer C having a processor 150 and memory 152 coupled to the processor 100 to store operating instructions, control information and database records therein. The data processing system D can be a computer of any conventional type of suitable processing capacity, such as a mainframe, a personal computer, laptop computer, or any other suitable processing apparatus. It should thus be understood that a number of commercially available data processing systems and types of computers may be used for this purpose. As indicated, the data processing system also operates as a reservoir simulator R for simulation of performance and for forecasting of production from the reservoir M. The simulator may thus be of the type described and shown in U.S. Pat. No. 7,526,418.
[0075] The computer C has a user interface 154 and an output data display 156 for displaying output data or records of three-dimensional reservoir pressure deter using real time pressure data from downhole gauges according to the present invention. The output display 156 includes components such as a printer and an output display screen capable of providing printed output information or visible displays in the form of graphs, data sheets, graphical images, data plots and the like as output records or images.
[0076] The user interface 154 of data processing system D also includes a suitable user input device or input/output control unit 158 to provide a user access to control or access information and database records and operate the computer C. Data processing system D further includes a database 160 stored in computer memory, which may be internal memory 152 , or an external, networked, or non-networked memory as indicated at 162 in an associated database server 164 .
[0077] The data processing system D includes program code 166 stored in non-transitory form in memory 152 of the computer C. The program code 166 according to the present invention is in the form of non-transitory computer operable instructions causing the data processor 100 to perform the computer implemented method of the present invention in the manner described above and illustrated in FIG. 3 .
[0078] It should be noted that program code 166 may be in the form of microcode, programs, routines, or symbolic computer operable languages that provide a specific set of ordered operations that control the functioning of the data processing system D and direct its operation. The instructions of program code 166 may be stored in non-transitory form in memory 152 of the computer C, or on computer diskette, magnetic tape, conventional hard disk drive, electronic read-only memory, optical storage device, or other appropriate non-transitory data storage device having a computer usable medium stored thereon. Program code 166 may also be contained on a data storage device such as server 164 as a non-transitory computer readable medium.
[0079] With the present invention, Bottom-Hole Pressure (SBHP) or pressure survey data measured at or near the depth of a producing formation interval data is entered and honored at the well locations with respect to the desired reference datum depth. Establishing the wells SBHP pressures as control points, the 3-dimensional pressure between the wells is estimated based on results of the numerical simulation by reservoir simulator R based on governing equations and relationships representing actual thermodynamics and geophysics, as well as the most updated geological realization of the subsurface reservoir illustrated as model M. The present invention reduces turnaround time for generation of maps and quality checking the data contents displayed in the maps and stored in the data processing system for evaluation of further processing or analysis.
[0080] The integration between the SBHP pressure points and simulation pressure results in a 3D grid populated with estimated reservoir pressure based on appropriate reliability and conformance with statistical quality analysis and control methods (such as Distance-Weighted Moving Average or DWMA). The data processing system D then adjusts the pressure values to the datum reference depth, if needed. Several alternative methods are then available for collapsing the 3-dimensional pressure grid array into a single layer (2-dimensional) while also taking into account geological features, aerial and vertical heterogeneity, and numerical model constraints. The resultant product, a 2-dimensional isobaric map of a reservoir region of interest is the provided and made available to a variety of visualization and quality control tools for reservoir management engineers to utilize.
[0081] The invention has been sufficiently described so that a person with average knowledge in the matter may reproduce and obtain the results mentioned in the invention herein Nonetheless, any skilled person in the field of technique, subject of the invention herein, may carry out modifications not described in the request herein, to apply these modifications to a determined methodology, or in the performance of the same, requires the claimed matter in the following claims; such techniques and procedures shall be covered within the scope of the invention.
[0082] It should be noted and understood that there can be improvements and modifications made of the present invention described in detail above without departing from the spirit or scope of the invention as set forth in the accompanying claims.
|
Estimates are formed of reservoir pressure between the wells for subsurface hydrocarbon producing reservoir. The estimation is based on field data and physical laws governing the hydrocarbon flow in porous media. Information from 3-dimensional fine geological and numerical reservoir simulation models, statistical interpolation between the wells, and static bottom-hole pressure (SBHP) surveys (measurement) at wells are used to more rapidly determine 2-dimensional isobaric reservoir pressure maps for times of interest during the reservoir simulation.
| 4
|
BACKGROUND OF THE INVENTION
1. Field of the Invention. This invention relates to a case assembly for motorcycle including an innovative coupling system.
2. Description of the Related Art. In the field of equipments for motorcycles there is the common known problem to provide a stable and safe coupling system for removable side cases. Usually the case assembly includes a specific frame which is fixed irremovably to the motorcycle and a case including suitable coupling means for the removable coupling to the frame. Various types of coupling means have been proposed in the prior art in the attempt to supply a secure coupling of the case avoiding accidental disengagements or false couplings and at the same time to allow the user to easily intentionally engage and disengage the case.
The general object of this invention is to supply a case assembly for motorcycles with safety and stability features greatly improved in comparison to known systems, retaining at the same time operational easiness and a simple but strong structure.
SUMMARY OF THE INVENTION
A case assembly for motorcycles according to the invention comprises a frame for coupling to the motorcycle and a case including means that allow its removable coupling to the frame, the characterizing feature of the assembly is that the coupling means include U-shaped elements which move between a non-active position to accommodate therein a complementary element of the frame and an active rotated position to secure therein said element of the frame.
BRIEF DESCRIPTION OF THE DRAWINGS
In order to further explain the innovative principles of this invention and its advantages in comparison to the prior art, an embodiment of the invention is described hereinafter by reference to the enclosed drawings. Therein:
FIG. 1 shows a schematic and prospective view of the case assembly according to the invention,
FIG. 2 shows a lateral, schematic and partial view of the coupling system of the case assembly according to FIG. 1 , in a position of partial engagement,
FIG. 3 shows a view similar to the one of FIG. 2 but in a position of full engagement,
FIG. 4 shows an enlarged partial view of the coupling mechanism of the case assembly according to FIG. 1 ,
FIG. 5 shows a further detail of the coupling means according to the invention, and
FIG. 6 shows an embodiment of the coupling system according to the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the figures, in FIG. 1 a case assembly according to the invention, generally indicated as 10 , is depicted.
Such case assembly 10 comprises a frame 11 which has to be fixed to a motorcycle by known means, not shown herein, and a rigid case 12 . Between the frame 11 and the case assembly 10 there are suitable means for the removable coupling. The case 12 has a shape and features which are already known, thus, it will not be described in detail herein.
Conveniently, the frame 11 is a tubular frame adequately shaped to obtain lateral support points for the case 12 and an upper hooking bar 13 . The case 12 has a side to be coupled with the frame 11 on which there are coupling means. The coupling means include a pair of passive coupling means 14 conveniently having mushroom shape (better visible in FIG. 2 ), to be coupled with adequate hollows 15 made near the lower edge of the case 12 . The hollows 15 are open at the bottom in order to allow the insertion of the mushroom shaped coupling means 14 by moving the case 12 downwards.
Near the upper edge, the case 12 has an active coupling mean 16 including a pair of movable U-shaped elements 17 aligned to form a tube to accommodate the horizontal hooking bar 13 of the frame 11 .
The U-shaped elements 17 can be rotated on demand (conveniently along a common axis 20 parallel to the hooking bar 13 ) to move between a disengaged non-active position and an active position of fix engagement onto the horizontal hooking bar 13 of the frame 11 .
In the disengaged position, shown in FIGS. 1 and 2 , the U-shaped elements 17 look outward from the back side of the case 12 , in particular, they are aligned horizontal having the opening looking outward, so that the hooking bar 13 can freely enter or exit the tube formed by the two aligned U-shaped elements. In the engaged position shown in FIG. 3 , the U-shaped elements 17 are parallel to the back side of the case 12 , in particular they look downward so that they prevent the case 12 to move away from the frame 11 .
Conveniently, the case 12 has also a resting groove 34 above the hooking bar 13 when the U-shaped elements 17 are in the active position, so that the weight of the case 12 is partially relieved from the U-shaped elements 17 .
The pivoting of the U-shaped elements 17 is in an upper position relative to the horizontal hooking bar 13 in such a manner, that the thrust of the hooking bar 13 inside the U-shaped elements 17 makes them automatically rotate into the engaged position.
There are also blocking means in order to prevent the case 12 to slide upward when being engaged onto the frame 11 . Conveniently, these blocking means comprise a central tooth 18 protruding from the frame 11 and inserting into a specific seat 19 in the wall of the case 12 when the case 12 is in the engaged position of FIG. 3 .
In FIG. 6 an alternative embodiment is shown in which the central tooth 18 is replaced by a pair of rigid protuberances 118 which projects from the wall of the case 12 in order to be placed immediately beneath the horizontal hooking bar 13 of the frame 11 in such a manner, that the engaged case 12 cannot move upward.
Hence, as it will be clear, the movement from the non-active position of FIG. 2 to the engaged active position of FIG. 3 is obtained by means of a spring simply pushing the case 12 against the frame 11 after having inserted the lower mushrooms shaped coupling means 14 into their seats in the case 12 . Once in the active position, the U-shaped elements 17 are steadily kept in such position by a block mechanism 21 which can be released through a push button 22 . Conveniently, further, a lock 23 can be added to prevent the possibility of disengagement of the case 12 . Further conveniently, the lock 23 can also at the same time block the locking mechanism of the case 12 , for example realized by a hook 24 which engages a complementary rim in the covershell of the case 12 .
In FIG. 4 the detail of the block mechanism 21 is shown from the back, after removing the covershell of the case 12 (the mechanism is in engaged position, with the U-shaped elements 17 facing downward). As it can be seen in this FIG., each U-shaped element 17 has a spring 25 required to push it in the non-active horizontal position, and a tooth 26 on the back which inserts in the end of a sliding element 27 when the U-shaped element 17 is in active position. The two sliding elements 27 are pushed toward the engagement position respectively by two springs 28 . In this way, when the U-shaped element 17 is pushed in the active position by the action of its spring 25 , the sliding element 27 clicks into the engagement position under the tooth 26 , blocking the U-shaped element 17 into the active position.
The push button 22 operates on the sliding elements 27 in such a way that, when it is pushed, it retreats the sliding elements 27 from the engagement position with the U-shaped elements 17 releasing back into the non-active position.
As it can be easily seen in the enlarged detail of FIG. 5 , the push button 22 operates on each sliding element 27 by an inclined plane 29 which slides on a corresponding inclined plane 30 of the sliding element 27 . The lock 23 can operate in a known way to prevent the operation of the push button 22 .
As it can be seen in FIG. 4 , the push button 22 operates also, by the action of springs 31 , a bolt 32 which has a protuberance 33 inserting into a seat in the tooth 18 . In this way, a further protection against the disengagement of the case 12 is provided.
At this point it is clear how the objects of the invention have been reached. Having the frame 11 mounted on the motorcycle, it is sufficient to insert the lower hollows 15 in the protruding mushrooms shaped coupling means 14 , which are a position reference, and to push the case 12 from the top against the frame 11 in order to engage the central tooth 18 in the corresponding seat and cause the rotation toward the block or lock position of the U- shaped elements 17 in order to engage the case 12 . In this manner, the case 12 is fixed in at least four points. The case 12 can be disengaged with only one movement by pressing the push button 22 with the lock unlocked.
Moreover, the free movement of the U-shaped elements 17 toward the operating position allows engaging the case 12 to the frame 11 even when the lock is already in the block position.
The system according to the invention grants high security, stable and reliable engagement, no vibrations and operational easiness.
As a matter off course, the description mentioned above refers to one embodiment of the innovative principles of this invention and is an exemplification of such innovative principles only, and does not have to be considered limitative for the scope of the invention hereby claimed. For example, the means which prevent the case 12 to move upward can be different from the tooth 18 . For example, they may include a tooth protruding from the case 12 to insert into the frame 11 .
In the embodiment described, the whole mechanism including the movable elements is close to the upper edge of the case 12 , this allows to easily realize a functional assembly including all the movable elements, the handle, the lock, and the push button. The frame 11 can also be different from the tubular frame described.
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A case assembly for motorcycles comprises a frame ( 11 ) for coupling to the motorcycle and a case ( 12 ) including means that allow its removable coupling to the frame. The means which allow the removable coupling include U-shaped elements ( 17 ) which move between a non-active position to accommodate therein a complementary element ( 13 ) of the frame and an active rotated position to secure therein said element ( 13 ) of the frame. Conveniently, between the case and the frame there are other passive coupling means ( 14, 15 ) at a distance of the U-shaped elements for positioning the case before the coupling movement of the U-shaped elements.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims benefit from U.S. Provisional Patent Application No. 61/062,589, entitled “Body Mount,” filed on Jan. 28, 2008, which is hereby incorporated in its entirety by reference.
FIELD OF THE INVENTION
The present invention is generally related to fasteners and, more particularly, to body mounts utilized in mounting a vehicle body to a vehicle frame or chassis.
BACKGROUND OF THE INVENTION
As is known in the art, vehicle bodies are commonly mounted on vehicle frames by the use of a plurality of body mounts. Each body mount typically includes a pair of upper and lower resilient blocks and a pair of upper and lower metal spacer members each having a generally planar flange portion and an integral elongated tubular portion. The resilient blocks are positioned on upper and lower sides of the vehicle frame in alignment with an opening in the frame, the tubular portions of the metal spacer members are respectively inserted in a central opening in a respective resilient block, and the inboard ends of tubular portions are secured together to respectively secure the resilient blocks to upper and lower sides of the vehicle frame. The vehicle body is then placed atop the upper resilient blocks and bolts are passed through respective openings in the vehicle body and threaded into respective body mounts to support the body on the frame.
Typically, the metal spacer members are complex with intricate features that allow them to be secured together and hold the resilient blocks in place until a bolt is passed through them. As such, these metal spacer members are typically manufactured through a costly deep extrusion process that not only gives the spacer members their general shape but also the aforementioned intricate securing and locking features.
Therefore, a need exists in the art for a simpler and less complicated body mount that is easier and more cost effective to produce. The body mount of the present invention is designed to provide simpler and more lightweight components thereby reducing complicated manufacturing processes.
DESCRIPTION OF THE DRAWINGS
Operation of the invention may be better understood by reference to the following detailed description taken in connection with the following illustrations, wherein:
FIG. 1 illustrates a perspective view of a prior art body mount.
FIG. 2 illustrates a perspective view of a clip of an embodiment of a body mount.
FIG. 3 illustrates a top view of the clip of FIG. 2 .
FIG. 4 illustrates a side view of the clip of FIG. 2 .
FIG. 5 illustrates a section view taken along line A-A of FIG. 3 .
FIG. 6 illustrates a section view taken along line B-B of FIG. 3 .
FIG. 7 illustrates a perspective view of a plate of an embodiment of the body mount.
FIG. 8 a top view of the clip of FIG. 7 .
FIG. 9 illustrates a section view taken along line A-A of FIG. 8 .
FIG. 10 illustrates a perspective view of a clip-and-plate subassembly of an embodiment of the body mount.
FIG. 11 illustrates a side view of the subassembly of FIG. 10 .
FIG. 12 illustrates an embodiment of the body mount.
FIG. 13 illustrates a perspective view of a clip of another embodiment of the body mount.
FIG. 14 illustrates a top view of the clip of FIG. 13 .
FIG. 15 illustrates a side view of the clip of FIG. 14 .
FIG. 16 illustrates a section view taken along line A-A of FIG. 14 .
FIG. 17 illustrates a perspective view of another clip-and-plate subassembly of another embodiment of the body mount.
FIG. 18 illustrates a side view of the subassembly of FIG. 17 .
FIG. 19 illustrates another embodiment of the body mount.
SUMMARY OF THE INVENTION
A body mount that may include at least one clip, at least one plate and a sleeve. The clip may include a generally cylindrical body having a proximal end and a distal end. The clip may also include a central aperture therethrough from the proximal end to the distal end. The clip may further include a flange located at the distal end. The plate may have an aperture sized to receive the cylindrical body and engage the flange. The sleeve may have opposed openings capable of engaging a first clip and a second clip between their respective plates. The sleeve may be capable of receiving the cylindrical body of both the first clip and the second clip through the opposed openings.
DETAILED DESCRIPTION
While the invention is described herein with reference to several embodiments, it should be clear that the invention should not be limited only to the embodiments disclosed or discussed. The description of the embodiments herein is illustrative of the invention and should not limit the scope of the invention as described or claimed.
As generally described herein, the present invention provides a body mount 10 . Referring now to FIGS. 2-12 , a first embodiment of a body mount 10 is shown. The body mount 10 may include two clip-plate subassemblies 90 connected and held together by a sleeve 40 . Each clip-plate subassembly 90 may include a clip 20 and a plate 30 . Thus, the body mount 10 may require two clips 20 and two plates 30 to be fully assembled with the sleeve 40 , as shown in FIG. 12 . When assembled, the clips 20 may be located adjacent to one another. The pair of clips 20 are preferably the same, however, it is to be understood that they may be the same or different clips.
Since the clips 20 are similar, the following description of the clip 20 will be understood to apply to both clips 20 needed for the body mount 10 . The clip 20 may include a distal end 23 and a proximal end 25 . It is to be understood that the clip 20 may be of any appropriate size, diameter and length, but is preferably of a circular shape. The body mount 10 may also include two plates 30 , where each plate 30 may be disposed about the distal end 23 of the corresponding clip 20 . The body mount 10 may further include a sleeve 40 that may be disposed about the clips 120 and located between the plates 30 .
With reference to FIGS. 2-6 , each clip 20 may have a generally tubular body 22 with a central aperture 29 located through the body 22 from the distal end 23 to the proximal end 25 . The distal end 23 of the clip 20 may include a flange 24 . The clips 20 may include a first set of prongs 26 located adjacent to the flange 24 . The first set of prongs 26 may be of any appropriate size or shape, but are preferably of a generally rectangular shape. The first set of prongs 26 may project outwardly relative to the tubular body 22 and may be angled towards the flange 24 . It will be appreciated, however, that the prongs 26 may be positioned at any appropriate angle. The flange 24 and the first set of prongs 26 may be operable to secure the plate 30 located therebetween, as shown in FIGS. 10-12 .
With further reference to FIGS. 2-6 , the clips 20 may also include a set of intermediate prongs 27 . The intermediate set of prongs 27 may be of any appropriate size or shape, but are also preferably of a generally rectangular shape. The intermediate prongs 27 may project inward relative to the tubular body 22 and into the central aperture 29 . The intermediate prongs 27 may be operable to engage the threads of a fastener (not shown), such as a bolt, screw or the like. The clips 20 may hold the fastener within the central aperture 29 until the fastener is later secured and tightened via a corresponding fastener (not shown), such as a nut or the like.
With additional reference to FIGS. 2-6 , the clips 20 may further include a third set of prongs 28 . The third set of prongs 28 may be of any appropriate size or shape, but are preferably of a generally triangular shape. The third set of prongs 28 may be formed on the tubular body 22 and may be located between the intermediate prongs 27 and the proximal end 25 of the clip 20 . The third set of prongs 28 may project outwardly relative to the tubular body 22 and may be angled towards the flange 24 . It will be appreciated, however, that the third set of prongs 28 may be positioned at any suitable angle. The third set of prongs 28 may be operable to engage the interior of the sleeve 40 and may lockingly secure the sleeve 40 about the clips 20 . While the present embodiment illustrates each set of prongs 26 , 27 , 28 comprising between two and four prongs each, it will be appreciated that any suitable and appropriate number of prongs per set may be employed.
The clips 20 may also include a longitudinal split 21 , as shown in FIGS. 4 and 5 . The longitudinal split 21 may simplify manufacturing by relaxing the tolerances of the diameter of the clips 20 while also allowing the clips 20 to flex as it is being inserted into the sleeve 40 and/or flex while receiving a fastener. The clips 20 may be formed from any durable and resilient sheet material, such as a metal, a polymer, or a composite. However, it will be appreciated that the clips 20 may be formed from any appropriate and suitable material and by any suitable process, including but not limited to stamping, drawing, pressing, extruding, molding, etc.
As illustrated in FIGS. 7-9 , each plate 30 may include a body 32 and a central aperture 34 . The central aperture 34 may be sized to coaxially receive the tubular body 22 of a clip 20 , yet may also be small enough that the first set of prongs 26 may be capable of securing the plate 30 between the prongs 26 and flange 24 of the clip 20 whereby the plate 30 may not be permitted to slide back down the tubular body 22 after the plate 30 has passed the first set of prongs 26 . The plate 30 may be constructed from any suitable material, including but not limited to metal, polymer, composite, etc.
As shown in FIG. 12 , the sleeve 40 may be of a generally tubular body 42 having a central opening 44 . The ends of the sleeve 40 may be flared, such as at 46 , to accommodate the first set of prongs 26 on each clip 20 . The sleeve 40 may also be constructed from any suitable material, including but not limited to metal, polymer, composite, etc.
The body mount 10 may typically be used in cooperation with a pair of resilient blocks (not shown) and a fastener (not shown), such as a bolt or the like, to secure a vehicle body (not shown) to a vehicle frame (not shown). For example, to utilize the body mount 10 in such a manner, a clip 20 and plate 30 subassembly may be assembled as follows, each of which will hereinafter be referred to as a “clip-and-plate subassembly” 90 , as shown in FIGS. 10 and 11 .
The body mount 10 preferably includes two clip-and-plate subassemblies 90 . The proximal end 25 of a clip 20 may be introduced to an aperture 34 of a corresponding plate 30 . The plate 30 may be slid from the proximal end 25 of the clip 20 towards the distal end 23 thereof. As the plate 30 passes the third set of prongs 28 , the third set of prongs 28 may be squeezed inwardly thereby allowing the plate 30 to pass. Thereafter, once the plate 30 has cleared the third set of prongs 28 , the third set of prongs 28 may spring outwardly to substantially return to their original position. Likewise, as the plate 30 passes the first set of prongs 26 , the first set of prongs 26 may be squeezed inwardly thereby allowing the plate 30 to pass. Thereafter, once the plate 30 has cleared the first set of prongs 26 , the first set of prongs 26 may spring outwardly to substantially return to their original position and to lockingly secure the plate 30 between the first set of prongs 26 and the flange 24 .
Next, a sleeve 40 may be coaxially disposed about the tubular body 22 of the first clip-and-plate subassembly 90 by introducing the proximal end 25 of the clip 20 to the central opening 44 of the sleeve 40 and coaxially sliding the sleeve 40 from the proximal end 25 of the clip 20 towards the distal end 23 of the clip 20 . The third set of prongs 28 may engage the interior of the sleeve 40 and permit the sleeve 40 to slide towards the distal end 23 of the clip 20 , but, at the same time, prohibit the sleeve 40 from sliding back towards the proximal end 25 of the clip 20 . The sleeve 40 may also further bias the plate 30 against the flange 24 of the clip 20 . The clip-and-plate subassembly with the sleeve 40 disposed about the tubular body 22 of the clip 20 will hereinafter be referred to as the “clip-plate-sleeve subassembly” (not shown).
An upper resilient block (not shown), having an aperture (not shown), may then be placed atop an upper face of a vehicle frame (not shown) where the aperture of the upper resilient block may be in coaxial alignment with an opening in the vehicle frame. The aforementioned clip-plate-sleeve subassembly may then be passed through the aperture of the upper resilient block and opening in the vehicle frame such that the plate 30 rests atop the upper resilient block and the clip 20 and sleeve 40 project downwardly through the aperture of the upper resilient block and frame opening.
A lower resilient block (not shown), having an aperture (not shown), may then placed against the underface of the vehicle frame (not shown) such that the aperture of the lower resilient block is in coaxial alignment with the opening in the frame. A second clip-and-plate subassembly 90 may then be passed through the aperture of the lower resilient block and opening in the vehicle frame such that the plate 30 of the second clip-and-plate subassembly 90 may rest against the outer face of the lower resilient block, and the tubular body 22 of the clip 20 may project upwardly through the aperture of the lower resilient block and frame opening. The clip 20 of the second clip-and-plate subassembly 90 may be inserted into the opening 44 of the sleeve 40 of the clip-plate-sleeve subassembly such that the third set of prongs 28 of the second clip 20 may engage the interior of the sleeve 40 , thereby securing the second clip-plate subassembly 90 to the clip-plate-sleeve subassembly so as to complete the assembly of the body mount 10 . The upper and lower resilient blocks are thus secured to the vehicle frame by the body mount 10 .
A body of a vehicle (not shown) may then be placed atop the upper resilient block such that an aperture in the vehicle body may be in coaxial alignment with the aperture 50 of the body mount 10 , where the aperture 50 of the body mount 10 is defined by the coaxially aligned apertures 29 of the respective clips 20 . A fastener (not shown), such as a bolt or the like, may then be passed through the aperture 50 of the body mount 10 whereby the respective intermediate prongs 27 of the clips 20 hold the fastener in position until the fastener is later secured and tightened via another corresponding fastener (not shown), such as a nut or the like.
Referring now to FIGS. 7-9 and 13 - 19 , an alternative embodiment of a body mount 110 is shown. The body mount 110 may include two clip-plate subassemblies 190 connected and held together by a sleeve 140 . Each clip-plate subassembly 190 may include a clip 120 and a plate 30 . Thus, the body mount 110 may require two clips 120 and two plates 30 to be fully assembled with the sleeve 140 , as shown in FIG. 19 . When assembled, the clips 120 may be located adjacent to one another. The pair of clips 120 are preferably the same, however, it is to be understood that they may be the same or different clips.
Since the clips 120 are similar, the following description of the clip 20 will be understood to apply to both clips 120 needed for the body mount 110 . With reference to FIGS. 13-16 , the clip 120 may include a distal end 123 and a proximal end 125 . It is to be understood that the clip 120 may be of any appropriate size, diameter and length, but is preferably of a circular shape. The body mount 110 may also include two plates 30 , where each plate 30 may be disposed about the distal end 123 of the corresponding clip 120 . The body mount 110 may further include a sleeve 140 that may be disposed about the clips 120 and located between the plates 30 .
As shown in FIGS. 13-16 , each clip 120 may have a generally tubular body 122 with a central aperture 129 located through the body 122 from the distal end 123 to the proximal end 125 . The distal end 123 of the clip 120 may include a flange 124 . The clips 120 may include a first set of prongs 126 located adjacent to the flange 124 . The first set of prongs 126 may be of any appropriate size or shape, but are preferably of a generally rectangular shape. The first set of prongs 126 may project outwardly relative to the tubular body 122 and may be angled towards the flange 124 . It will be appreciated, however, that the prongs 126 may be positioned at any appropriate angle. The flange 124 and the first set of prongs 126 may be operable to secure a plate 30 located therebetween.
With reference to FIGS. 13-16 , the clips 120 may also include a set of intermediate prongs 127 . The intermediate set of prongs 127 may be of any appropriate size or shape, but are preferably of a generally triangular shape. The intermediate prongs 27 may project inward relative to the tubular body 122 and into the central aperture 129 . The intermediate prongs 127 may be operable to engage the threads of a fastener (not shown), such as a bolt, screw or the like. The clips 120 may hold the fastener within the central aperture 129 until the fastener is later secured and tightened via a corresponding fastener (not shown), such as a nut or the like.
With further reference to FIGS. 13-16 , the clips 120 may further include a third set of prongs 128 . The third set of prongs 128 may be of any appropriate size or shape, but are also preferably of a generally triangular shape. The third set of prongs 128 may be formed on the tubular body 122 and may be located between the intermediate prongs 127 and the proximal end 125 of the clip 120 . The third set of prongs 128 may project outwardly relative to the tubular body 122 and may be angled towards the flange 124 . It will be appreciated, however, that the third set of prongs 128 may be positioned at any suitable angle. The third set of prongs 128 may be operable to engage the interior of the sleeve 140 and may lockingly secure the sleeve 140 about the clips 120 . While the present embodiment illustrates each set of prongs 126 , 127 , 128 comprising between two and four prongs each, it will be appreciated that any suitable and appropriate number of prongs per set may be employed.
The clips 120 may also include a longitudinal split 121 , as shown in FIGS. 15 and 16 . The longitudinal split 121 may simplify manufacturing by relaxing the tolerances of the diameter of the clips 120 while also allowing the clips 120 to flex as it is being inserted into the sleeve 140 and/or flex while receiving a fastener. The clips 120 may be formed from any durable and resilient sheet material, such as a metal, a polymer, or a composite. However, it will be appreciated that the clips 120 may be formed from any appropriate and suitable material and by any suitable process, including but not limited to stamping, drawing, pressing, extruding, molding, etc.
As discussed above, each plate 30 may include a body 32 and a central aperture 34 , as illustrated in FIGS. 7-9 . The central aperture 34 may be sized to coaxially receive the tubular body 122 of a clip 120 , yet may also be small enough that the first set of prongs 126 may be capable of securing the plate 30 between the prongs 126 and flange 124 of the clip 120 whereby the plate 30 may not be permitted to slide back down the tubular body 122 after the plate 30 has passed the first set of prongs 126 . The plate 30 may be constructed from any suitable material, including but not limited to metal, polymer, composite, etc.
As shown in FIG. 19 , the sleeve 140 may be of a generally tubular body 142 having a central opening 144 . The ends of the sleeve 140 may be flared, such as at 146 , to accommodate the first set of prongs 126 on each clip 120 . The sleeve 140 may also be constructed from any suitable material, including but not limited to metal, polymer, composite, etc.
As also discussed above, the body mount 110 may typically be used in cooperation with a pair of resilient blocks (not shown) and a fastener (not shown), such as a bolt or the like, to secure a vehicle body (not shown) to a vehicle frame (not shown). For example, to utilize the body mount 110 in such a manner, a clip 120 and plate 30 subassembly may be assembled as follows, each of which will hereinafter be referred to as a “clip-and-plate subassembly” 190 , as illustrated in FIGS. 17 and 18 .
The body mount 110 preferably includes two clip-and-plate subassemblies 190 . The proximal end 125 of a clip 120 may be introduced to an aperture 34 of a corresponding plate 30 . The plate 30 may be slid from the proximal end 125 of the clip 120 towards the distal end 123 thereof. As the plate 30 passes the third set of prongs 128 , the third set of prongs 128 may be squeezed inwardly thereby allowing the plate 30 to pass. Thereafter, once the plate 30 has cleared the third set of prongs 128 , the third set of prongs 128 may spring outwardly to substantially return to their original position. Likewise, as the plate 30 passes the first set of prongs 126 , the first set of prongs 126 may be squeezed inwardly thereby allowing the plate 30 to pass. Thereafter, once the plate 30 has cleared the first set of prongs 126 , the first set of prongs 126 may spring outwardly to substantially return to their original position and to lockingly secure the plate 30 between the first set of prongs 126 and the flange 124 .
Next, a sleeve 140 may be coaxially disposed about the tubular body 122 of the first clip-and-plate subassembly 190 by introducing the proximal end 125 of the clip 120 to the central opening 144 of the sleeve 140 and coaxially sliding the sleeve 140 from the proximal end 125 of the clip 120 towards the distal end 123 of the clip 120 . The third set of prongs 128 may engage the interior of the sleeve 140 and permit the sleeve 140 to slide towards the distal end 123 of the clip 120 , but, at the same time, prohibit the sleeve 40 from sliding back towards the proximal end 125 of the clip 120 . The sleeve 140 may also further bias the plate 30 against the flange 124 of the clip 120 . The clip-and-plate subassembly with the sleeve 140 disposed about the tubular body 122 of the clip 120 will hereinafter be referred to as the “clip-plate-sleeve subassembly” (not shown).
An upper resilient block (not shown), having an aperture (not shown), may then be placed atop an upper face of a vehicle frame (not shown) where the aperture of the upper resilient block may be in coaxial alignment with an opening in the vehicle frame. The aforementioned clip-plate-sleeve subassembly may then be passed through the aperture of the upper resilient block and opening in the vehicle frame such that the plate 30 rests atop the upper resilient block and the clip 120 and sleeve 140 project downwardly through the aperture of the upper resilient block and frame opening.
A lower resilient block (not shown), having an aperture (not shown), may then placed against the underface of the vehicle frame (not shown) such that the aperture of the lower resilient block is in coaxial alignment with the opening in the frame. A second clip-and-plate subassembly 190 may then be passed through the aperture of the lower resilient block and opening in the vehicle frame such that the plate 30 of the second clip-and-plate subassembly 190 may rest against the outer face of the lower resilient block, and the tubular body 122 of the clip 120 may project upwardly through the aperture of the lower resilient block and frame opening. The clip 120 of the second clip-and-plate subassembly 190 may be inserted into the opening 144 of the sleeve 140 of the clip-plate-sleeve subassembly such that the third set of prongs 128 of the second clip 120 may engage the interior of the sleeve 140 , thereby securing the second clip-plate subassembly 190 to the clip-plate-sleeve subassembly so as to complete the assembly of the body mount 110 . The upper and lower resilient blocks are thus secured to the vehicle frame by the body mount 110 .
A body of a vehicle (not shown) may then be placed atop the upper resilient block such that an aperture in the vehicle body may be in coaxial alignment with the aperture 150 of the body mount 110 , where the aperture 150 of the body mount 110 is defined by the coaxially aligned apertures 129 of the respective clips 120 . A fastener (not shown), such as a bolt or the like, may then be passed through the aperture 150 of the body mount 110 whereby the respective intermediate prongs 127 of the clips 120 hold the fastener in position until the fastener is later secured and tightened via another corresponding fastener (not shown), such as a nut or the like.
The embodiments of the invention have been described above and, obviously, modifications and alternations will occur to others upon reading and understanding this specification. The claims as follows are intended to include all modifications and alterations insofar as they come within the scope of the claims or the equivalent thereof.
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A body mount included at least one clip, at least one plate and a sleeve. The clip may include a generally cylindrical body having a central aperture therethrough. The clip may further include at least one set of inwardly extending prongs. The clip may further include at least one set of outwardly extending prongs. The sleeve may have opposed openings capable of engaging a first clip and a second clip between their respective plates.
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FIELD OF THE INVENTION
The present invention generally relates to a method and system for creating an accurate skills inventory for skills retained by each independent human resource within a business concern. More particularly, the invention relates to a method and system that generates a metric for each resource, e.g., employee, contractor, etc., at the disposal of the business with respect to each of several identifiable skills.
BACKGROUND OF THE INVENTION
To be competitive in the market, it is important for a business to have an accurate skills inventory. That is, it is important for the business to accurately keep track of all of the available skill resources the business has at its disposal. Furthermore, because the acquisition of new skills as well as the expansion of existing skills for a given individual is constantly changing, for example, as individuals gain experience with respect to different tasks, it is increasingly more important for the business to be cognizant of its available skills. The cost of using inaccurate skills data can be very high and potentially lead to less efficient operation of the business, low customer satisfaction, erroneous site selection to deliver a service, etc.
Also, skills are a unit of measure by which services deals are costed and priced. Accordingly, maintaining accurate skills data is non-trivial. In accordance with at least some known related art methodology, skills databases are deterministically populated using an employee's “claimed” skills, a practice that does not reflect the “true” skill value. Also, as employees evolve in their job, the skills may not be updated to reflect the evolving skill value.
FIG. 2 illustrates a related art system where records 200 for each employee in a business are stored in a skills inventory database 100 . Each of these records comprises information related to what skills the particular employee has. For example, resumes 300 provided by the employees indicate particular skills the employees have. Using a skills specification (not shown) to determine what data is important/relevant, one of the records 400 corresponding to a particular employee might include data informing that this employee has five years experience with Oracle, ten years of experience using the SAP application and four years of experience with the AIX operating system.
Although this information is beneficial to a degree, it is not completely accurate. For example, the information provided is done so by the employee and may not reflect the actual proficiency this employee has attained regarding the specified skills. Instead, the data only indicates years of experience, which does not always reflect an accurate level of proficiency. Further, the data provided regarding the number of years is very discrete. That is, it is provided in one year increments. It is unlikely that the employee has exactly five, ten and four years, respectively, experience with each of the skills. It is more likely that the respective amount of experience for each skill includes a partial year.
Accordingly, it is desirable to provide a method and a system for accurately assessing and storing the skills available to a business with respect to each employee and other human resources available.
SUMMARY OF THE INVENTION
Illustrative, non-limiting embodiments of the present invention address the aforementioned and other disadvantages associated with related art methods of skills inventory development and maintenance. In particular, in accordance with the present invention, the above and other drawbacks related to known skill data management are addressed by capturing, observing and analyzing data from runtime operations that impact skill values corresponding to the human resources of a business group.
In accordance with one exemplary embodiment, a method of establishing a skills inventory is provided, the method comprising monitoring the activity of a resource object with respect to an activity performed by the resource object, wherein the activity performed requires at least one skill identified in a list of specified skills, extracting data relevant to the at least one skill from results of said monitoring, computing a metric value indicative of a skill level attained by the resource object with respect to each of the at least one skill and updating a skills inventory database with the computed metric value.
According to a further exemplary embodiment of the invention, a computer program product for providing a service to reuse IT system knowledge is provided, the program product comprising a computer readable medium, first program instruction means for monitoring the activity of a resource object with respect to an activity performed by the resource object, wherein the activity performed requires at least one skill identified in a list of specified skills, second program instruction means for extracting data relevant to the at least one skill from results of said monitoring, third program instruction means for computing a metric value indicative of a skill level attained by the resource object with respect to each of the at least one skill, and fourth program instruction means for updating a skills inventory database with the computed metric value.
According to a further exemplary embodiment of the invention, a system for establishing an accurate skills inventory is provided. A system in accordance with this embodiment comprises means for monitoring at least one activity performed by a resource object (e.g., a first server portion), wherein the activity performed requires at least one skill identified in a list of specified skills; means for extracting data (e.g., the first server portion), wherein the data is relevant to the at least one skill from results of the monitoring of the activity; means for computing a metric value (e.g., a second server portion), wherein the metric value is indicative of a skill level attained by the resource object with respect to each of the at least one skill and means for updating a skills inventory database with the computed metric value (e.g., the second server portion). This embodiment further may include a skills inventory database that comprises at least one record corresponding to the resource object and each record comprises at least one independent metric value corresponding to a skill that the resource object possesses.
According to an even further exemplary embodiment of the invention, a system for establishing an accurate skills inventory is provided where the system comprises a first server portion operable to execute a skills data retrieval application, wherein the skills data retrieval application receives data from a runtime application that monitors the performance of a resource object while the resource object performs at least one task and a second server portion operable to calculate at least one metric value corresponding to the at least one task performed by the resource object, wherein each metric value accounts for a plurality of predetermined parameters relevant to its respective task.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a process flow diagram of an embodiment in accordance with the invention.
FIG. 2 is a process flow diagram of a related art method.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
The present invention is related to the IT services area and, thus many technology-specific terms are used in describing the invention and providing the environment in which it operates. Skilled artisans would understand the intended meaning of the technology-specific terms used below, however, the following, non-exhaustive list of term definitions is provided to assist the reader. Although the list below provides a general definition of the respective terms, the definitions provided are not meant to be limiting. That is, the definitions provided are not exclusive and one skilled in the art should apply alternative or modified definitions where appropriate.
Employee Database: A database that maintains employee records and information about their skill set. Typically maintained by the HR organization in a company.
Skills Taxonomy: A classification methodology for specifying the types of skills relevant to an organization. For example, in IBM's services business, a taxonomy called JRSS (Job Requisition Skill Set) is used.
Runtime System/Runtime Operations: Refers to any system maintained by an organization that tracks and captures the history of the work done by its employees.
Ticketing System: An example of a runtime system in the services business. Records and tracks the various IT systems management requests made by a customer. Information includes the names of person(s) who work on the requests through various stages, the time taken, the kind of IT system the request applies to, etc. Examples used in the services business (by IBM and others) include eESM, Remedy, Peregrine, etc.
Information Model/Data Model: Refers to a data structure imposed on top of the records/logs of a runtime system that extracts the relevant fields in the records for further processing.
Exemplary, non-limiting, embodiments of the present invention are discussed in detail below. While specific configurations and process flows are discussed to provide a clear understanding of the invention, it should be understood that the disclosed process flows and configurations are provided for illustration purposes only. A person skilled in the relevant art will recognize that other process flows and configurations may be used without departing from the spirit and scope of the invention.
An embodiment consistent with the present invention comprises a method to accurately capture a value indicative of a person's skill with respect to various skills impacted by the person's activities. More particularly, a value which is indicative of the person's skill level is calculated by observing and analyzing the data from runtime operations that gather data in near-real-time as the person is gaining, or in some cases losing, experience with respect to various skills.
In accordance with at least one embodiment, data from various information sources, for example, problem and change ticketing systems, is analyzed to determine what tasks a particular person has worked on in the recent past. The tasks are then mapped to a standard skills classification methodology, or taxonomy, such as IBM's JRSS skill codes, or another taxonomy for which skill values can be gleaned.
For each skill code relevant to the particular person, a metric is computed that captures the skill level. The computed metric takes into account various relevant parameters, such as, the number of relevant tasks completed by the person, the time that was required to complete the task(s) and how long ago these tasks were performed. The calculated metric, together with the skill codes, is associated with the particular person and stored in a database.
In addition to the parameters mentioned above, those skilled in the art would know that other parameters of interest can be used without straying from the spirit of the invention.
First, a metrics database M with one record for each employee is created. Each record further contains a sub-record for each type of skills the employee has. This sub-record includes a score assigned to the employee for that skill type. For an employee with unique identifier 1 , the sub-record is referred to for skill type S, e.g., M(I,S).
The following represents exemplary pseudo-code for the calculation of the metric value. In particular, for each record r in the runtime log the following is performed:
{
Apply information model on the record to get structured record R;
N = Extract employee name from R;
I = Unique identifier for this employee;
S = Extract skill type from R;
T = Extract time the task was performed;
Modify the skill sub-record for this employee as follows:
M(I,S) = f ( M(I,S) , T , S ); This applies a function f to the
metrics record, which depends on the previous value of the skill sub-
record, the time and the skill used.
}
When the above loop ends, each record in the runtime database will have been processed, each kind of skill an employee has exercised will have been identified, and a score will have been assigned to each such skill.
The function f can be very general, since we can store any information in the skill sub-records and pass it as a parameter to the next computation of the sub-record.
An exemplary environment in which the present invention might be used is in the context of a company's Help Desk. In particular, a resource object, such as an employee working at the Help Desk, performs various tasks to achieve a particular result. For instance, a Help Desk employee may be working remotely over a network to resolve a customer's IT-related problem.
According to one Help Desk method, when a customer calls into the Help Desk to report a problem, a “ticket” is created for that call. The ticket includes data such as, the particular problem; to what hardware and/or software components the problem relates; the time problem resolution began; the time the problem was resolved, or, in some cases the time problem resolution was abandoned; what steps were taken in pursuit of a resolution, and any other relevant data.
FIG. 1 illustrates an embodiment in accordance with the invention and described in the context of the Help Desk example mentioned above.
While the resource object is performing his or her job function to resolve the customer's problem, at least one runtime application, such as runtime applications 10 and 20 , gather data with respect to the process the employee undertakes in resolving the issue. That is, runtime applications 10 and 20 capture data with respect to the performance of the resource. For example, a runtime application such as eESM (IBM's eEnterprise Solutions Management application), logs data relevant to change management. Another example of a runtime application that captures data relevant to the resource's performance is ManageNow, which logs data for problem management. In addition to the applications mentioned, those skilled in the art would understand that various runtime applications that capture relevant data can be used in accordance with the present invention. That is, any application, or number of applications, that captures data in accordance with a specified taxonomy, described below, can be used in accordance with this embodiment.
As illustrated in FIG. 1 , results of the runtime application(s), 10 and 20 , are fed into an information model, 40 , where the classification methodology, or taxonomy, 30 , is implemented. More particularly, specific data is parsed from the runtime operations to be used in the calculation of the skills metric, 50 , described in detail below. The skills metric calculated, e.g., for each resource object and for each skill determined by the given taxonomy, 30 , is then recorded in a skills inventory database 60 . As shown, the skills database, 60 , includes at least one record, 70 , corresponding to each resource object. The record comprises data, 80 , indicating the calculated metric for each of the skills determined by the taxonomy, 30 , to be of importance for that particular resource object. For the example shown in FIG. 1 , the metric value calculated for Oracle skill is “10”, the value for the SAP application skill is “5” and the value for the AIX operating system skill is “4”.
Calculation of a metric in accordance with one exemplary embodiment of the present invention will now be described.
Using the Help Desk example discussed above, as an employee is working at the Help Desk, runtime programs such as eESM and ManageNow log data regarding the employee's performance. Data is extracted from the logs and an information model is imposed on the data using IBM's JRSS taxonomy.
According to this embodiment, three time periods are considered, i.e., periods 0 , 1 and 2 , each of a duration T. X(t) is the set of tickets closed in the t th time period, S(X(t)) is the total severity of these tickets, N(X(t)) is the number of tickets in the set and a is a weighting parameter. For example, a has a value less than 1 such that the larger values give more weight to activities performed by the resource object more recent in time and, alternatively, gives less weight to actions performed in the more distant past.
Based on the information model presented, the metric value for the given resource object with respect to a given skill is:
S(X(O))/N(X(O))X(1−a) 2 +S(X(1))/N(X(1))Xa(1−a)+S(X(2))/N(X(2))Xa
After the metric is calculated, the skills inventory is updated with the calculated skill value, i.e., metric value calculated, for the given resource object for the particular skill type.
The invention can take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment containing both hardware and software elements.
In a further embodiment, the invention is implemented in software, which includes but is not limited to firmware, resident software, microcode, etc.
Furthermore, the invention can take the form of a computer program product accessible from a computer-usable or computer-readable medium providing program code for use by or in connection with a computer or any instruction execution system. For the purposes of this description, a computer-usable or computer readable medium can be any apparatus that can contain, store, communicate, propagate, or transport the program for use by or in connection with the instruction execution system, apparatus, or device.
The medium can be an electronic, magnetic, optical, electromagnetic, infrared, or semiconductor system (or apparatus or device) or a propagation medium. Examples of a computer-readable medium include a semiconductor or solid state memory, magnetic tape, a removable computer diskette, a random access memory (RAM), a read-only memory (ROM), a rigid magnetic disk and an optical disk. Current examples of optical disks include compact disk-read only memory (CD-ROM), compact disk-read/write (CD-R/W) and DVD.
A data processing system suitable for storing and/or executing program code will include at least one processor coupled directly or indirectly to memory elements through a system bus. The memory elements can include local memory employed during actual execution of the program code, bulk storage, and cache memories which provide temporary storage of at least some program code in order to reduce the number of times code must be retrieved from bulk storage during execution.
Input/output or I/O devices (including but not limited to keyboards, displays, pointing devices, etc.) can be coupled to the system either directly or through intervening I/O controllers.
Network adapters may also be coupled to the system to enable the data processing system to become coupled to other data processing systems or remote printers or storage devices through intervening private or public networks. Modems, cable modem and Ethernet cards are just a few of the currently available types of network adapters.
It would be understood that a method incorporating any combination of the details mentioned above would fall within the scope of the present invention as determined based upon the claims below and any equivalents thereof.
Other aspects, objects and advantages of the present invention can be obtained from a study of the drawings, the disclosure and the appended claims.
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A method and system for obtaining and storing accurate skills data relative to human resource objects of an enterprise. Relevant data is extracted from runtime processes that monitor the activities of the human resource objects and a metric value indicative of a skill level attained for each of a list of skills is calculated for each human resource object.
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FIELD OF THE INVENTION
[0001] The invention relates to loading of scrap metal into containers, and more particularly to an apparatus and method for loading of scrap metal into containers that prevents damage to the containers and allows the amount of scrap by weight to be precisely monitored.
BACKGROUND OF THE INVENTION
[0002] Shipping of non-uniform material such as scrap metal can be accomplished in several manners. The scrap material can be compressed into predetermined shapes, such as cubes, and those shapes can be loaded into shipping containers and stacked based on the approximate dimensions of the shapes. The amount of handling required to ship scrap metal in this manner and the cost of the compression equipment can exceed the savings that may be realized by increasing the volume of scrap that can be shipped in a container. In addition, the cost for shipping a container may be based in whole or in part on weight, which may eliminate the primary incentive to increase the amount of material that can be loaded into a container.
[0003] Nevertheless, shipment of uncompressed or loose metal scrap can also be problematic, as such scrap metal can be difficult to load into shipping containers. The non-uniform configuration of the loose metal scrap can result in jagged edges that damage the shipping containers while loading. It can also be difficult to clearly document the weight of the loose metal scrap that has been loaded into a shipping container, and the owner of the shipping container may provide weight measurements that conflict with those of the scrap metal provider.
SUMMARY OF THE INVENTION
[0004] An apparatus and method for loading loose scrap metal into a shipping container are provided that prevent the shipping container from being damaged during loading, that facilitate the loading of loose scrap into a shipping container, and that provide additional points at which to measure the weight of the scrap that has been loaded into the shipping container, thus facilitating the shipment of loose/uncompressed scrap.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0005] FIG. 1A is a diagram of a system for loading scrap metal into shipping containers in accordance with an exemplary embodiment of the present invention;
[0006] FIG. 1B is a diagram of a system in operation for loading scrap metal into shipping containers in accordance with an exemplary embodiment of the present invention;
[0007] FIG. 1C is a diagram of a system with a shipping container fully encasing a loader, in accordance with an exemplary embodiment of the present invention;
[0008] FIG. 1D is a diagram of a system with a shipping container partially loaded with the scrap metal from a loader, in accordance with an exemplary embodiment of the present invention;
[0009] FIG. 1E is a diagram of a system with a shipping container fully loaded with the scrap metal from a loader, in accordance with an exemplary embodiment of the present invention;
[0010] FIGS. 2A and 2B are diagrams showing an alternate view of a shipping container fully loaded with the scrap metal from a loader, in accordance with an exemplary embodiment of the present invention;
[0011] FIG. 3 is a diagram of a system for controlling the operation of a loader in accordance with an exemplary embodiment of the present invention; and
[0012] FIG. 4 is a flow chart of an algorithm for controlling the operation of a loader in accordance with an exemplary embodiment of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0013] In the description that follows, like parts are marked throughout the specification and drawings with the same reference numerals, respectively. The drawing figures might not be to scale and certain components can be shown in generalized or schematic form and identified by commercial designations in the interest of clarity and conciseness.
[0014] FIG. 1A is a diagram of a system 100 for loading scrap metal into shipping containers in accordance with an exemplary embodiment of the present invention. System 100 allows a standard shipping container to be loaded with loose scrap metal or other suitable materials in a manner that prevents the shipping container from being damaged while allowing the exact weight of the scrap metal that has been loaded into the shipping container to be independently verified. While loading and handling of scrap metal is described herein as an example, wood, paper, glass, rock or other suitable materials can also or alternatively be used.
[0015] System 100 includes loader 102 , which is a metal-walled trough having dimensions that allow loader 102 to be inserted into the cavity of a shipping container. Loader 102 is filled with scrap metal, and is then inserted into shipping container 112 , such as by backing shipping container 112 over loader 102 using a tractor-trailer. An adjustment mechanism (not explicitly shown in FIG. 1A ) can be used to move loader 102 horizontally, vertically or rotationally, so as to align loader 102 to slide directly into shipping container 112 . A swivel, tracks, rollers or other suitable devices can also or alternatively be provided where suitable to loader 102 to allow loader 102 to be readily inserted into shipping container 112 .
[0016] Loader supports 106 provide support for loader 102 , and rest on load cells 108 A and 108 B. Load cells 108 A and 108 b can be used to determine the empty weight of loader 102 , the weight of loader 102 after it has been filled with scrap, and the weight of loader 102 after shipping container 112 has been completely filled with scrap, to the extent that there is any remaining scrap in loader 102 . In this manner, the weight of the scrap metal that has been placed into shipping container 112 from loader 102 can be independently verified.
[0017] System 100 also includes control cabin 110 and hydraulic drive 104 . Control cabin 110 is situated to allow an operator to observe the operation of loader 102 , which is described in further detail herein. Hydraulic drive 104 drives a push plate (not explicitly shown in FIG. 1A ) that is used to push loose scrap metal into shipping container 112 from loader 102 . A cog drive, an electric motor or other suitable motive devices can also or alternatively be used to apply a motive force to the push plate. Hydraulic, electric or other suitable devices can also be used to position loader 102 in a vertical, horizontal or rotational orientation relative to the shipping container, to apply a vibrational force to loader 102 to disrupt jammed configurations of scrap, or for other suitable purposes.
[0018] In operation, system 100 allows a shipping container 112 to be loaded with scrap metal from a loader 102 in a manner that prevents damage to the shipping container 112 and that allows the weight of the scrap metal to be independently verified.
[0019] FIG. 1B is a diagram of a system 100 in partial operation for loading scrap metal into shipping containers in accordance with an exemplary embodiment of the present invention. In FIG. 1B , shipping container 112 has been moved partially over loader 102 , without disturbing the scrap metal contained in loader 102 and without exposing shipping container 112 to any damage from the scrap metal. As previously discussed, rollers, swivels, or vertical and horizontal placement controls can be used to align loader 102 with shipping container 112 , and to prevent shipping container 112 from being inadvertently damaged if loader 102 is not perfectly aligned with shipping container 112 or if the driver of the tractor trailer connected to shipping container 112 mistakenly changes direction while moving shipping container 112 into position.
[0020] FIG. 1C is a diagram of a system 100 with shipping container 112 fully encasing loader 102 , in accordance with an exemplary embodiment of the present invention. Once the tractor trailer holding shipping container 112 has moved shipping container 112 to a position where loader 102 is fully enclosed, the tractor trailer drive train is placed into neutral, to allow the shipping container to move as the scrap metal contained within loader 102 is pushed into shipping container 112 by hydraulic drive 104 . In this manner, as the scrap metal is moved into shipping container 112 , the operator in control cabin 110 can observe the progress of the loading and can adjust the speed of the hydraulic drive 104 as necessary to avoid pushing shipping container 112 faster than the rate at which the scrap metal is being loaded into shipping container 112 , as such loading might be indicative of blockage in the scrap metal assembly that will result in empty space within shipping container 112 . Likewise, if shipping container 112 is moving away from loader 102 at a slower rate than the rate at which the scrap metal is being loaded into shipping container 112 , that condition can indicate possible damage to shipping container 112 , and the operator can reverse the movement of the push plate to disentangle the scrap metal from the damaging configuration. System 100 provides an operator with considerable flexibility to prevent potentially damaging conditions from developing.
[0021] FIG. 1D is a diagram of a system 100 with shipping container 112 partially loaded with the scrap metal from loader 102 , in accordance with an exemplary embodiment of the present invention. As shown in FIG. 10 , shipping container 112 has moved away from fully enclosing loader 102 in response to hydraulic drive 104 moving push plate 114 from the front of loader 102 towards the back of loader 102 . Loader 102 is fabricated from heavy gauge metal, unlike shipping container 112 which is fabricated from a lighter gauge metal. As a result, as push plate 114 applies force to the scrap metal in loader 102 , the scrap metal moves into shipping container 112 and applies a transmitted force to shipping container 112 from push plate 114 , which moves away from push plate 114 because the tractor trailer drive is in neutral. The operator in control cabin 110 can observe the progress of the loading and can adjust the speed of the hydraulic drive 104 as necessary to avoid pushing shipping container 112 faster than the rate at which the scrap metal is being loaded into shipping container 112 , or can increase the speed where push plate 114 is closely tracking the movement of shipping container 112 away from loader 102 . Likewise, if push plate 114 enters into shipping container 112 , which can potentially cause the scrap metal to damage shipping container 112 , push plate 114 can be retracted, a vibrator mechanism can be activated to facilitate the movement of scrap metal out of loader 102 and into shipping container 112 , or other suitable processes can be implemented.
[0022] In addition, the loading of shipping container 112 can be automated, such as by using a metering mechanism to track the position of push plate 114 relative to the end of shipping container 112 , the amount of force being applied by push plate 114 , or other suitable indicators.
[0023] FIG. 1E is a diagram of a system 100 with shipping container 112 fully loaded with the scrap metal from loader 102 , in accordance with an exemplary embodiment of the present invention. As shown in FIG. 1E , shipping container 112 has moved completely away from loader 102 , and push plate 114 is being retracted by hydraulic drive 104 back to a starting position to allow loader 102 to receive a new load of scrap metal. The weight of loader 102 can be determined using load cells 108 a and 108 B, and this data can be recorded to provide an additional data source for verifying the amount of scrap metal that has been loaded into shipping container 112 . While it is common for shipping container 112 to be weighed on a scale or other suitable device both before and after loading, the additional data point for determining the amount of scrap metal that has been loaded can be used if any discrepancies are later noticed. For example, it is possible that scrap may be removed from the shipping container while it is en route, mistakes might be made in the weight amounts reported by the driver of the tractor trailer, or other sources of error may be encountered. Inconsistency between the weights measured using load cells 108 a and 108 B and other weighing mechanisms can help to identify misoperating equipment, clerical errors, or other sources of discrepancy.
[0024] FIGS. 2A and 2B are diagrams showing an alternate view of shipping container 112 fully loaded with the scrap metal from loader 102 , in accordance with an exemplary embodiment of the present invention. As shown in FIG. 2A , shipping container 112 has moved completely away from loader 102 , and push plate 114 is being retracted by hydraulic mechanism 116 . Detail drawing FIG. 2B shows hydraulic mechanism 116 withdrawing push plate 114 back to the loading position. As previously noted, cog drives, electric motors or other suitable mechanisms can be used to provide a motive force to push plate 114 .
[0025] FIG. 3 is a diagram of a system 300 for controlling the operation of a loader in accordance with an exemplary embodiment of the present invention. System 300 includes loader controller 302 , loader position system 304 , push plate controller 306 , push plate accelerator 308 , loader vibrate system 310 and display/record weight system 312 , each of which can be implemented in hardware or a suitable combination of hardware and software, and which can be one or more software systems operating on a general purpose processing platform or mechanical controls within control cabin 110 . As used herein and by way of example and not by limitation, “hardware” can include a combination of discrete components, an integrated circuit, an application-specific integrated circuit, a field programmable gate array, a digital signal processor, or other suitable hardware. As used herein and by way of example and not by limitation, “software” can include one or more objects, agents, threads, lines of code, subroutines, separate software applications, one or more lines of code or other suitable software structures operating in one or more software applications or on one or more processors, or other suitable software structures. In one exemplary embodiment, software can include one or more lines of code or other suitable software structures operating in a general purpose software application, such as an operating system, and one or more lines of code or other suitable software structures operating in a specific purpose software application.
[0026] Loader position system 304 aligns a loader with a shipping container. In one exemplary embodiment, a user can manually position the loader so that it is aligned with the shipping container, such as by moving the loader up or down, to the left or to the right, by swiveling the loader about a central swivel point, or in other suitable manners. In another exemplary embodiment, the loader and/or shipping container can include one or more sensors that are used to provide position data that is used to adjust the horizontal position, vertical position or angular position of the loader relative to the shipping container.
[0027] Push plate controller 306 controls the movement of a push plate to offload scrap metal from a loader into a shipping container. In one exemplary embodiment, a shipping container can be placed in position to enclose the loader, and a user can manually control a push plate using a hydraulic press, such as by moving the push plate forward at a rate that matches the rate at which the shipping container is pushed away from the loader as the scrap in the loader is transferred to the shipping container. Likewise, if the shipping container stops moving relative to the push plate, the user can slow or stop the movement of the push plate to prevent damage to the shipping container. In another exemplary embodiment, load sensors can be used to control the rate at which the push plate is moved, such as to accelerate the push plate when resistance is at a minimum and to slow or stop the push plate if resistance reaches predetermined thresholds.
[0028] Push plate accelerator 308 controls the rate at which the push plate is moved, either while being extended or retracted. In one exemplary embodiment, the push plate can be accelerated if no resistance is being encountered while the shipping container is receiving scrap from the loader. In another exemplary embodiment, the push plate can be retracted if resistance to movement is encountered, and can be accelerated into the scrap metal to break any obstructions, such as where the scrap metal has formed an obstruction within the loader.
[0029] Loader vibrate system 310 controls a vibrational force on a loader, such as to dislodge jammed scrap while the loader is being used to fill a shipping container. In one exemplary embodiment, loader vibrate system can be used to manually control a vibrational force applied to the loader, such as by pulsing a lateral or horizontal positioning device or by using other suitable devices, such as when a push plate of the loader encounters resistance while loading scrap metal into a shipping container. Likewise, a feedback control can be provided where the push plate is automatically controlled, or other suitable controls can be provided, such as to activate, increase or decrease a vibrational force as a function of an amount of resistance measured by a hydraulic power source that moves the push plate of the loader.
[0030] Display/record weight system 312 allows a user to display and record an amount of weight of scrap metal contained within a loader, and additional data such as a date, time, load identifier or other suitable data. Display/record weight system 312 allows the weight of a load of scrap metal that is being loaded into a shipping container to be measured and recorded, such as to address any future discrepancies that may be reported.
[0031] In operation, system 300 allows a scrap loader to be controlled to load scrap metal from the loader into a standard shipping container while avoiding damage to the shipping container. System 300 also allows the amount of scrap that has been loaded into the shipping container to be determined and recorded.
[0032] FIG. 4 is a flow chart of an algorithm 400 for controlling the operation of a loader in accordance with an exemplary embodiment of the present invention. Algorithm 400 begins at 402 , where a loader is filled with scrap, such as scrap metal, and the increase in the weight of the loader is recorded. The algorithm then proceeds to 404 .
[0033] At 404 , it is determined whether the loader is aligned with a shipping container. If it is determined that the loader is aligned, such as by manual observation or measurement, by using telemetry sensors or in other suitable manners, then the algorithm proceeds to 408 . Otherwise, the algorithm proceeds to 406 , where the loader is raised, lowered, swiveled, or otherwise adjusted to align the loader with the shipping container. The algorithm then proceeds to 408 .
[0034] At 408 , the shipping container is backed over the loader, such as by moving the shipping container with a tractor trailer or in other suitable manners. The loader is configured to fit within a standard shipping container, so as to allow the shipping container to be backed onto the loader through the shipping container access doors. After the shipping container has fully enclosed the loader, the algorithm proceeds to 410 .
[0035] At 410 , the shipping container carrier, such as a tractor trailer, is placed in a neutral gear, so as to allow the shipping container to move out from the loader as the scrap metal or other materials are pushed into the shipping container from the loader. The algorithm then proceeds to 412 , where a hydraulic push plate of the loader is activated. The loader can include a hydraulic mechanism or other suitable motive device that moves the push plate from a front end of the loader towards a back end of the loader, so as to push the scrap metal in the loader into the shipping container. The loader is formed from plate steel having a sufficient gauge to prevent damage from being inflicted on the loader while the scrap metal is pushed into the shipping container, which allows the shipping container (which generally has walls that are of a lighter gauge metal and which may be damaged by scrap metal that is pushed through the container) to receive the metal as it exist the end of the loader without any relative movement between the scrap metal and the shipping container. As the scrap metal exits the loader, it forces the shipping container to move away from the loader, as long as the carrier for the shipping container is in a neutral gear and is able to move in response to the force exerted against the shipping container by the loader push plate as it pushes the scrap metal into the shipping container. The algorithm then proceeds to 414 .
[0036] At 414 , it is determined whether the shipping container is moving properly. For example, if the shipping container is moving away from the loader faster than the scrap metal is being pushed into the shipping container, then the configuration of the scrap metal or other random conditions might be preventing the scrap metal from filling the shipping container properly. Likewise, if the shipping container is moving away from the loader slower than the scrap metal is being pushed into the shipping container, the scrap metal might be causing damage to the shipping container. If the shipping container is moving properly, such as at the same rate as the push plate or at other acceptable speeds, then the algorithm proceeds to 420 where loading continues. Otherwise, the algorithm proceeds to 416 , where the push plate speed is adjusted, such as to increase or decrease the push plate speed, to reverse the push plate so as to try and dislodge a blocked scrap metal configuration, or in other suitable manners. The algorithm then proceeds to 418 , where the loader is vibrated if a vibrational mechanism is available, such as to dislodge a blocked scrap metal configuration. The algorithm then proceeds to 422 .
[0037] At 422 , it is determined whether the shipping container is full. If the shipping container is not full, such as if the shipping container continues to enclose a portion of the loader and there is remaining scrap metal in the loader, the algorithm returns to 414 , otherwise the algorithm proceeds to 424 . At 424 , the weight of the loader is recorded, so as to generate a record of the amount of scrap that has been loaded into the shipping container.
[0038] In operation, algorithm 400 allows a loader to be used to fill a shipping container with scrap metal in a manner that prevents the shipping container from being damaged and that allows the weight of scrap metal that has been loaded into the shipping container to be documented.
[0039] While certain exemplary embodiments have been described in detail and shown in the accompanying drawings, it is to be understood that such embodiments are merely illustrative of and not restrictive on the broad invention. It will thus be recognized to those skilled in the art that various modifications may be made to the illustrated and other embodiments of the invention described above, without departing from the broad inventive scope thereof. It will be understood, therefore, that the invention is not limited to the particular embodiments or arrangements disclosed, but is rather intended to cover any changes, adaptations or modifications which are within the scope and the spirit of the invention defined by the appended claims.
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An apparatus for loading a shipping container comprising a metal trough having a bottom, a front end, a back end and two sidewalls. A push plate disposed at the back end of the metal trough. A force mechanism coupled to the push plate and configured to move the push plate from the back end of the metal trough to the front end of the metal trough. A support mechanism configured to support the metal trough to allow a shipping container to be moved into a position to encompass the metal trough through a door of the shipping container.
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BACKGROUND OF THE INVENTION
The present invention relates in general to a portable display system, and more particularly, a display system that is relatively easy to set up and which lends itself readily to large display requirements.
Among the objects of this invention is to provide a display system wherein the display panels are hinged together so that they may be opened and closed into various different display configurations.
Another object of the present invention is to provide a versatile display system which can be formed in displays of various sizes and configurations and yet which is readily portable. The display of the present invention preferably employs lightweight wallboards secured by border strip means.
Another object of the present invention is to provide border strip means of improved construction.
Still another object of the present invention is to provide an improved portable display system having means of relatively simple construction for interlocking adjacent panel assemblies.
Still another object of the present invention is to provide an improved portable display system having an improved hinging arrangement.
Reference is also made herein to my earlier U.S. Pat. No. 4,147,198 which shows a portable display system. This patent also refers to other references of general pertinence to the field of this invention.
SUMMARY OF THE INVENTION
According to the invention, there is provided a portable display system which comprises a plurality of panel assemblies, each comprising detachable removable front and rear panels preferably constructed of a wall board or the like, and border strip means which preferably comprise two basic types of border strips, namely, first and second peripheral support members for supporting and positioning the detachable panels in a substantially parallel and confronting relationship. The first peripheral support means preferably includes a fixed member and an outer removable member which is removable for the purpose of removing one or both panels. This first peripheral support means is positioned along at least one outer edge of the detachable front and rear panels. The second peripheral support means is positioned along the other edges of these panels. The display system also includes hinge means for interconnecting the plurality of panel assemblies with said panel assemblies being divided into first and second array. In the disclosed embodiment, each array comprises four panels, however, in a smaller embodiment, each array could comprise two or three panels. Each of these arrays include a main panel assembly and at least one other connected panel assembly. The hinge means comprises at least first and second pairs of side hinges and a pair of corner hinges. Means are provided for securing the first pair of side hinges to side disposed second peripheral support means of adjacent panel assemblies of the first array. Similarly, means are provided securing the second pair of side hinges to side disposed second peripheral support means of adjacent panel assemblies of the second array. Means are also provided securing the pair of corner hinges between main panel assemblies of the first and second arrays with one of the corner hinges disposed along said side disposed second peripheral support means of first and second array main panel assemblies. The other of said corner hinges is disposed along the opposite side disposed second peripheral support means of the first and second array main panel assemblies.
In accordance with another aspect of the present invention there is provided for a portable display system having a plurality of panel assemblies, an improved border strip means for supporting each panel comprising first peripheral support means including a fixed member and an outer removable member engageable with the fixed member, and second peripheral support means positioned along the other edges of said panel. The removable members of facing panel assemblies are provided with registration means which is preferably in the form of a tongue and groove arrangement to maintain the panel assemblies in planar relationship. Furthermore, in order to provide a proper alignment of the tongue and groove arrangements, the removable members are preferably keyed for only single position interconnection with its corresponding fixed member.
In accordance with the present invention the portable display system is arranged so that the panel assemblies may be hinged together to be opened and closed into various display configurations including the one disclosed herein. When in an entirely closed position, the entire display case is similar in appearance to a suitcase and affords the use of a highly portable display device. When fully opened, in the disclosed embodiment the display system may be provided in an eight panel arrangement.
BRIEF DESCRIPTION OF THE DRAWINGS
Numerous other objects, features and advantages of the invention should now become apparent upon a reading of the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a perspective view showing the entire portable display system in an embodiment having eight total panel assemblies, being arranged in a typical display configuration;
FIG. 2 is an enlarged fragmentary perspective view showing further detail of the hinging arrangement disclosing both a corner hinge and a double hinge;
FIG. 3 is a cross-sectional view showing the detail of one type of the border strip means taken along line 3--3 of FIG. 1; and
FIG. 4 is another cross-sectional view taken along line 4--4 of FIG. 1 showing the further detail of the other type of border strip device that is employed.
DETAILED DESCRIPTION
Referring now to the drawings, there is shown, in FIG. 1 a portable display system in accordance with the present invention. FIGS. 2-4 show further details of construction particularly with regard to the border strip means that is employed in the invention. The display system comprises a plurality of panel assemblies separated into an upper array 10 and a lower array 12. Each of these arrays comprises four separate panel assemblies. The upper array 10 includes a main panel assembly 14, and three other connected panel assemblies 15. Similarly, the lower array includes a main panel assembly 16 and three other interconnected panel assemblies 17. Each of the panel assemblies comprises a rectangular frame 18 also referred to herein as a border strip device, and a pair of parallel confronting panels or wallboards 20 and 21.
The main panel assembly 14 has the next adjacent section 15 hinged thereto by means of a suitable double hinge 25. Other similar hinges are employed to hinge the remaining panel assemblies 15 adjacent to each other. Further details of the double hinge are depicted in FIGS. 2 and 4. Similarly, the main panel assembly 16 of array 12 has the next adjacent section 17 hinged thereto by means of the same type of double hinge 25. Also, the remaining sections 17 are hinged in succession by means of such a double hinge 25. This double hinge arrangement permits essentially two-way hinging as depicted in the middle two assemblies of each array 10 and 12 of FIG. 1. Two hinges are employed between each panel assembly although in an alternate embodiment more than two hinges could be employed.
In addition to the double hinges 25 that are used between panel assemblies in each array, there are also provided two corner hinges 26. These corner hinges 26 are disposed on opposite sides of the main panel assemblies 14, 16. Thus, one of the hinges 26 connects between border strips 18A of panel assemblies 14 and 16 while the other corner hinge 26 extends between border strips 18B of main panel assemblies 14 and 16. FIG. 2 shows also the corner hinge 26 on one side of the main panel assemblies.
With the arrangement depicted in FIG. 1, the entire upper array 10 can be pivoted relative to the lower array 12 by means of the two corner hinges 26. The remaining panel assemblies are not hinged between arrays, but instead are interlocked into position by means of an interlocking or registration technique described hereinafter.
FIGS. 2 and 4 show the double hinges 25 which include outer hinge plates 25A and 25B and intermediate hinge plate 25C. This hinge may be of the type described in my previous U.S. Pat. No. 4,147,198. As depicted in the drawing, the hinge is attached by bolts or screws 28 which pass through the hinge and into the border strip means 18. Similarly, the corner hinge 26 may be of the type described in my U.S. Pat. No. 4,147,198 with screws or bolts 30 being provided for securing the corner hinge to the respective border strip means.
As depicted in the drawings, there are basically two different border strip arrangements depicted respectively in FIGS. 3 and 4. The first of these peripheral support means is shown in FIG. 3 comprising a fixed member 34 that is preferably hollow, as shown, and a removable member 36 that is adapted to snap fit with the fixed member 34. The members 34 and 36 are adapted to be interconnected in only one of two possible positions by means of a keying arrangement including a slot 35 at one corner of the fixed member cooperating with a shoulder 37 of the removable member 36. Each of the removable members also includes a tongue and groove arrangement including tongue 39 and groove 40. The keying arrangement including the slot 35 and the shoulder 37 prevents misalignment between the tongue and groove arrangement of one member 36 which is adapted to interlock with an adjacent member 36. FIG. 3 shows the correct position. However, if one of the members 36 was snap-fitted in an opposite direction, then the tongues and grooves would not line up but instead a tongue would line up with a tongue and a groove with a groove which is not desired.
When the removable outer member 36 is disengaged from the fixed member 34 the overall panel assembly stays intact. This may be accomplished in the same manner as in the construction of my prior art patent such as by the use of a corner locking device inserted within the hollow of member 34.
The tongue and groove interlock arrangement extends along each removable member a distance less than the length of the removable member as illustrated in FIGS. 1 and 2 leaving interlock free ends that enable corresponding ones of the panel assemblies of the adjacent arrays to be maintained folded as illustrated in FIG. 1, out of interlock relationship, while the main panel assemblies 14 and 16 are interlocked as also illustrated in FIG. 1. The interlock means extend at least in part out of the outer surface of the removable member such as illustrated in FIGS. 2 and 3.
Between the member 34 and walls 42 of the member 36 there is defined a channel for receiving the panels 20, 21. However, when the member 36 is disengaged from the fixed member 34, then the panels 20 and 21 are free to be withdrawn from the display system. In the disclosed embodiment of FIG. 1, this first type of border strip, including a removable section is provided only at the interface between the upper and lower arrays. Thus, the tongue and groove interlocking arrangement occurs between each of the panel assemblies 15 and 17 and also between the panel assemblies 14 and 16. The remaining border strip means may all be of the type depicted in FIG. 4 wherein the entire border strip is of the fixed type particularly, where the hinges 25 are fastened. A border strip device as depicted in FIG. 4 is used.
In FIG. 4 the border strip device includes an inner member 46 integral with an outer section 48. The inner member 46 is similar to member 34 in that it is hollow and forms the means by which different linear sections of the border strip are interconnected by means of a corner locking device not shown in the drawings. This locking device as previously mentioned may be of the type shown in my previous U.S. Pat. No. 4,147,198. The outer section 48 includes walls 49 defining with the inner member 46 oppositely disposed channels for the panels 20 and 21. The border strip device shown in FIG. 4 may be employed in the embodiment of FIG. 1 on all vertical portions of the frames of the panel assemblies. Also, this form of a border strip device may be used at the bottom of the frame in array 12 and at the top of the frame in array 10.
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A portable display system having a plurality of hollow panel assemblies with each comprising two parallel and facing wall boards secured within a border strip device. Eight panel assemblies are hinged together to fold and unfold between a folded position in which all panel assemblies are in parallel stacked relation and an unfolded position in which the panels are open in any one of a number of different positions including a continuous wall arrangement.
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FIELD OF THE INVENTION
[0001] Current application relates to a studded leather garment which has inner lining, especially to a leather garment easy to repair damaged studs due to hidden zipper installed on the inner lining.
BACKGROUND OF THE INVENTION
[0002] Studded leather garment of jacket, skirt and pants are one of the “Punk” fashion, which started from 1970's in U.S and U.K. Spike bands and other studded or spiked jewelry; safety pins, and silver bracelets were worn by both men and women. Leather, rubber and vinyl clothing have been common. Even these days punk fashion were common on both sides of the Atlantic Ocean and studded, customized leather jackets or denim vests became more popular. However, due to the complex stud's structure on garments most of the studded garments are made by hand of the owner using leather or denim garment of her/his own. Otherwise, production cost is very expensive because of the hand job. One of the method of studding a garment, in most cases leather, comprises three steps of 1) mark the place, with a marker pen, where the studs are located on the garment, 2) make holes penetrating the garment on the marked spot with a nail and hammering, and 3) assemble the male part, which usually locates inner hidden surface of the garment, and female part, which usually locates outer surface of the garment, of the stud. The other method is to use a diamond shape stud which has two sharp edged legs. The method of studding are similar to the previous method. Mark positions where the studs are to be located. Puncture the leather garment and push the sharp edged legs. The legs are folded on the opposite surface of the studs. In both cases the opposite surface of the studs, mostly metal parts and some of them are sharp edged, would touch and may hurt the skin of wearer or inner wears. So, most of studded garment attach inner linings to protect the wearer's skin and inner wear. However, this kind of inner lining makes it difficult when some studs on the garment is damaged or lost. Because all the threads of the inner lining should be removed and re-sewing the lining to repair the studs. It is purpose of the current application to provide a studded garment easy to repair the damaged/lost studs without removing thread of stitching on the linings and sewing again.
DESCRIPTION OF PRIOR ARTS
[0003] U.S. D727, 885 to Requea discloses an attachable studded jacket for mobile phone.
[0004] U.S. D696, 513 to Louboutin discloses a studded card case.
[0005] YouTube at the internet address https://www.youtube.com/watch?v=KyWbMsqpeGk discloses a method of studding a leather jacket with studs. The studs used is comprised of female part and male part. Usually female part is conical shape metal piece having female screw inside developed from the bottom and male part is flat headed screw bolt. A groove for screw driver is developed on the head. The method of studding a leather jacket comprises three steps of 1) mark the position, with a marker pen, where the studs are located on the leather jacket, 2) make holes penetrating the leather jacket on the marked spot with a nail and hammering, and 3) assemble the male part, which usually locates inner hidden surface of the garment, and female part, which usually locates outer surface of the garment, of the stud and tighten the male part with screw driver.
[0006] YouTube at the internet addresses of https://www.youtube.com/watch?v=EDCUrmHt-kk and https://www.youtube.com/watch?v=gNbhwF31cMY illustrates a method of studding a leather jacket with diamond shape studs. The method of studding are similar to the previous method. Mark positions where the studs are to be located. Puncture the leather garment and push the sharp edged legs. The legs come out on the opposite side of the studs are folded.
[0007] In both cases the opposite surface of the studs, in case of metal parts, make the wearer feel cold when the parts touch the wearer's skin. And some of them are sharp edged, would hurt the skin of the wearer or inner wears. So, most of studded garment attach inner linings to protect the wearer's skin and inner wear. However, this kind of inner lining makes it difficult when some stud on the garment is damaged or lost. Because part of the threads of stitching on the inner lining should be removed and re-stitched to repair the studs.
[0008] It is purpose of the current application to provide a studded garment easy to repair the damaged/lost studs without removing thread of the linings and sewing again.
SUMMARY OF THE INVENTION
[0009] Studded leather garment of jacket, skirt and pants are one of the “Punk” fashion, which started from 1970's in U.S and U.K. Spike bands and other studded or spiked jewelry were worn by both men and women. Leather, rubber and vinyl clothing have been common. Even these days punk fashion were common on both sides of the Atlantic Ocean and studded, customized leather jackets or denim vests became more popular. However, due to the complex stud's structure on garments most of the studded garments are made by hand of the owner using leather or denim garment of her/his own. Otherwise, production cost is very expensive because of the hand job. One of the method of studding a garment, in most cases leather, comprises three steps of 1) mark the place, with a marker pen, where the studs are located on the garment, 2) make holes penetrating the garment on the marked spot with a nail and hammering, and 3) assemble the male part, which usually locates inner hidden surface of the garment, and female part, which usually locates outer surface of the garment, of the stud. The other method is to use a diamond shape stud which has two sharp edged legs. The method of studding are similar to the previous method. Mark positions where the studs are to be located. Puncture the leather garment and push the sharp edged legs. The legs are folded on the opposite surface of the studs. In both cases the opposite surface of the studs, mostly metal parts and some of them are sharp edged, would touch and may hurt the skin of wearer or inner wears. So, most of studded garment attach inner linings to protect the wearer's skin and inner wear. However, this kind of inner lining makes it difficult when some studs on the garment is damaged or lost. Because all the threads of the inner lining should be removed and re-sewing the lining to repair the studs. It is purpose of the current application to provide a studded garment easy to repair the damaged/lost studs without removing thread of stitching on the linings and sewing again. A studded leather garment is provided. The studded leather garment according to current application comprises of; 1) leather garment, including but not limited to, coat, jacket, skirts, belts, and pants, etc., which has inner lining, 2) pluralities of studs made of, including but not limited to, stainless steel, aluminum, and plastic, etc., 3) and hidden zippers on the inner lining. The studded leather garment according to the current application enables easy repair of the damaged studs without removing thread of stitching on the inner lining and sewing again.
BRIEF DESCRIPTION OF DRAWINGS
[0010] FIG. 1 is a typical studded ladies leather jacket available on the market.
[0011] FIG. 2 is a perspective drawing of conical shape stud.
[0012] FIG. 3 is a schematic drawing of cross sectional view of the conical shape stud studded on a leather jacket of prior art.
[0013] FIG. 4 is a perspective drawing of diamond shape stud with two sharp edged legs.
[0014] FIG. 5 is a schematic drawing of cross sectional view of the diamond shape stud studded on a leather jacket of prior art.
[0015] FIG. 6 is a schematic drawing of cross sectional view of the diamond shape stud studded on a leather jacket with inner lining of prior art.
[0016] FIG. 7 is a schematic drawing of a studded leather jacket with inner lining of prior art seen from inside of the jacket.
[0017] FIG. 8 is a schematic drawing of a studded leather jacket with inner lining according to current application seen from inside of the jacket.
[0018] FIG. 9 is a perspective drawing of the studded leather jacket according to current application reversed inside-out.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0019] Following descriptions of a stud jacket explains the key features of the current invention. FIG. 1 is a typical studded ladies leather jacket ( 1 ) available on the market. Most popular studded jacket available on the market these days are decorated with conical shape stud ( 2 ) and diamond shape stud ( 3 ). FIG. 2 is a perspective drawing of conical shape stud ( 2 ). The conical shape stud ( 2 ) comprises of a male part ( 2 - 1 ) and a female part ( 2 - 2 ). Method of studding a leather jacket with the conical shape stud ( 2 ) comprises three steps of 1) marking the place, with a marker pen, where the studs are located on the garment, 2) making holes penetrating the garment on the marked spot with a nail and hammering, and 3) assemble the male part ( 2 - 1 ), which usually locates inner hidden surface of the garment, and female part ( 2 - 2 ), which usually locates outer surface of the garment, of the stud. Usually female part ( 2 - 2 ) is conical shape metal piece having female screw ( 2 - 3 ) inside developed from the bottom and male part ( 2 - 1 ) is flat headed male screw bolt ( 2 - 4 ). A groove ( 2 - 5 ) for screw driver is developed on the head.
[0020] FIG. 3 is a schematic drawing of cross sectional view of the conical shape stud ( 2 ) studded on a leather jacket ( 1 ) of prior art. The female part ( 2 - 2 ) of the conical shape stud ( 2 ) locates outer surface ( 4 ), usually decorating surface of the leather jacket ( 1 ). The male part ( 2 - 1 ) locates inner surface ( 5 ) of the leather jacket ( 1 ).
[0021] Since the male part ( 2 - 1 ) of the conical shape stud ( 2 ) locates inside ( 5 ) of the jacket ( 1 ), as shown in the FIG. 3 , the male part ( 2 - 1 ) faces wearer's body. When the wearer wears inner wear, such as shirts, the male part ( 2 - 1 ) will touch the inner wear. If the groove ( 2 - 5 ) for screw driver of the male part ( 2 - 1 ) has some sharp cut edge, the groove ( 2 - 5 ) may damage the inner wear. And when the sharp cut edged groove ( 2 - 5 ) touches the wearer's skin, it hurts the wearer. To avoid this situation the conical shape studs ( 2 ) are fabricated with finish touching. So, the price of such finish touched conical shape studs ( 2 ) are expensive especially when they are made of stainless steel.
[0022] Such damages by studs may be more serious with diamond shape studs ( 3 ) with sharp edged legs ( 3 - 1 ). FIG. 5 is a schematic drawing of cross sectional view of the diamond shape stud ( 3 ) with two sharp edged legs ( 3 - 1 ) studded on a leather jacket ( 1 ).
[0023] FIG. 4 is a perspective drawing of diamond shape stud ( 3 ). The diamond shape stud ( 3 ) has two sharp edged legs ( 3 - 1 ). Method of studding a jacket with the diamond shape stud ( 3 ) is similar to the previous method of studding with conical shape studs ( 2 ). Mark positions where the studs are to be located. Puncture the leather garment and push the sharp edged legs ( 3 - 1 ). The legs ( 3 - 1 ) come out on the opposite side of the diamond shape studs ( 3 ) are folded. FIG. 5 is a schematic drawing of cross sectional view of the diamond shape stud ( 3 ) studded on a leather jacket ( 1 ) of prior art. The diamond shaped side ( 3 - 2 ) of the diamond shape stud ( 3 ) locates outer surface ( 4 ), usually decorating surface of the leather jacket ( 1 ). The sharp edged legs ( 3 - 1 ) locates inner surface ( 5 ) of the leather jacket ( 1 ).
[0024] Since the sharp edged legs ( 3 - 1 ) of the diamond shape stud ( 3 ) locates inside ( 5 ) of the jacket ( 1 ), as shown in the FIG. 5 , the sharp edged legs ( 3 - 1 ) faces wearer's body. When the wearer wears inner wear, such as shirts, the sharp edged legs ( 3 - 1 ) will touch the inner wear. If the sharp edged legs ( 3 - 1 ) are stretched, the sharp edge ( 3 - 2 ) will damage the inner wear. And when the sharp edge ( 3 - 2 ) touches the wearer's skin, it hurts the wearer.
[0025] In any case of the prior art, when the fixing parts, male part ( 2 - 1 ) of the conical shape stud ( 2 ) and sharp edged leg ( 3 - 1 ) of the diamond shape stud ( 3 ), may touch the wearer's skin or damage the inner wear of the wearer. Then it makes the wearer uncomfortable. To avoid such an unpleasant situation, one layer of inner lining ( 6 ) is added on the inner surface of the studded leather jacket to cover the male part ( 2 - 1 ) of the conical shape stud ( 2 ) and sharp edged leg ( 3 - 1 ) of the diamond shape stud ( 3 ). FIG. 6 is a schematic drawing of cross sectional view of the diamond shape stud ( 3 ) studded on a leather jacket ( 1 ) and covered with an inner lining ( 6 ) of prior art. Like many others the inner lining ( 6 ) is stitched ( 7 ) to the leather jacket ( 1 ) from inside to cover the sharp edged legs ( 3 - 1 ) of the diamond shape stud ( 3 ). Similar drawings can be created for the conical shape stud ( 2 ) too.
[0026] Whenever a wearer wears a studded jacket ( 1 ) and moves; wearing the jacket ( 1 ), putting off the jacket ( 1 ), swing and folding arms while walking, bending the body, etc., the leather of the jacket ( 1 ) stretches and shrinks repeatedly. Then the screw ( 2 - 4 ) of the male part ( 2 - 1 ) of the conical shape stud ( 2 ) is loosen and fall out from the female screw ( 2 - 3 ) of the female part ( 2 - 3 ). In case of diamond shape stud ( 3 ), the sharp edged legs ( 3 - 1 ) fall out of the hole on the leather skin. But, the problem is repairing the damaged/lost studs. FIG. 7 is the schematic drawing of stitched ( 7 ) inner linings ( 6 ) of the prior arts seen from inside of a leather jacket ( 1 ). As shown the FIG. 7 , the threads of the stitched ( 7 ) lines should be removed to repair damaged or lost studs ( 2 ), ( 3 ) wherever the studs located. After repair the inner ling ( 6 ) should be stitched again to recover the original ornamentality. Especially when the studs ( 2 ), ( 3 ) are decorated on the arms/sleeves, it is very tedious job to reverse the arms/sleeves, remove threads of stitches and stitching again.
[0027] To avoid such tedious and costing job, hidden zippers ( 8 ) are installed on the inner lining ( 6 ′). FIG. 8 is a schematic drawing of a studded leather jacket ( 1 ′) with inner lining ( 6 ′) according to current application seen from inside of the jacket ( 1 ′). Like most of the jacket, the inner lining ( 6 ′) for a studded leather jacket ( 1 ′) of the current application is stitched ( 7 ) to inner leather skin ( 9 ) around the brim of the jacket ( 1 ′) and arm portions ( 10 ) only. Therefore, the zippers ( 11 ) installed on left side ( 12 ) and right side ( 13 ) stitch lines of the
[0000] allow a repairer's hand ( 14 ) access to the damaged stud's point ( 15 ) easily. Likewise, another zippers ( 11 ′) are installed on the inner side of both arm's inner lining ( 6 ′). Third zipper ( 11 ″) is optionally installed on the folding portion of the collar ( 16 ) if the collar is also decorated with studs ( 2 ), ( 3 ). FIG. 9 is a schematic drawing of the studded leather jacket ( 1 ′) according to current application reversed inside-out.
[0028] The hidden zippers ( 11 ), ( 11 ′), ( 11 ″) installed on the inner lining ( 6 ), ( 6 ′) of the studded leather jacket according to current application, enables the owner of the jacket repair the damaged/lost stud without handing over his/her studded jacket of favorite to a professional alteration shop.
[0029] Application to other garments such as coat, pants, skirts, etc., is not limited by the above example.
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A studded leather garment is provided. The studded leather garment according to current application comprises of; 1) leather garment, including but not limited to, coat, jacket, skirts, belts, and pants, etc., which has inner lining, 2) pluralities of studs made of, including but not limited to, stainless steel, aluminum, and plastic, etc., 3) and hidden zippers on the inner lining. The studded leather garment according to the current application enables easy repair of the damaged studs without removing thread of stitching on the inner lining and sewing again.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates to skylights and, more particularly, to a skylight system with a tubular light conduit connecting to a roof skylight device to a ceiling skylight device.
[0002] Roof skylights are a means to provide daylight into a room with limited amounts of available daylight. Usually, such rooms have no windows or one window. Townhouses or row houses in particular are faced with light limitations, except for end units, they only receive sun light from two directions. As the earth rotates about the sun and depending on which direction a house faces, a room may receive a lot or a little sunlight. To overcome the limited available sunlight coming into a room, skylights were invented.
[0003] The early skylights had metal frames and glass panes with wire mesh embedded in the panes for safety purposes. The skylight was mounted on a roof over a shaft leading from the roof to a ceiling. Generally, the shaft was covered with wood or plaster board. The problem is that the sunlight reflects off the shaft, which has been painted, some of the light is absorbed, particularly when the angle of the sunlight is low. Another problem is when a skylight and shaft are added after a house is built, the alignment of a skylight opening and a ceiling opening may be off.
[0004] Recent developments of skylights, including the patented art, use modern materials to create skylights. With the use of modern plastics, sunlight at any angle cap be reflected through a skylight shaft into a room and skylights can be bent to align a skylight shaft with a skylight opening and a ceiling opening.
[0005] A patent of interest to the present invention is U.S. Pat. No. 5,502,935, issued to Demmer. In the Demmer disclosure, a skylight, shown in FIG. 1 has a skylight module 12 and a ceiling mounted fixture module 16 connected by a flexible, tubular, light conveyance module 20 . The flexible, tubular light conveyance module 20 has an inner wall portion 54 , an outer wall portion 56 , and a middle portion on an insulation material 58 . The inner wall portion 54 is white to facilitate light reflection. Both the inner and outer wall portion 54 and 56 , respectively, are made of a durable, flexible vinyl material. The middle portion 58 insulation is an injected foam, fiberglass or any other known, flexible insulating material.
[0006] For the purposes of the present invention, Demmer provided the flexible, tubular light conveyance module with a series of pleats 52 to facilitate bending into alignment with the skylight module 12 and the ceiling mounted fixture module 16 . Module 20 can be reinforced with a wire spiral.
[0007] Demmer also discusses the use of flexible, tubular light conveyance modules 20 of circular, rectangular or other shape in cross-sections.
SUMMARY OF THE INVENTION
[0008] The present invention relates to a light and air conducting tube which connects between a skylight and a ceiling opening through an attic or like space between the roof and the ceiling of a house. The light and air conducting tube is somewhat flexible to allow bending of the tube to match the locations of a skylight and a ceiling opening should they not be aligned. At the same time the tube is firm enough to not collapse under its own weight. The inner surface of the light and air conducting tube has a highly reflective tube for greater light transmission. To further increase the amount of light transmitted, the tube has a square or rectangular cross-section, which increases the area approximately 27% more than a circle.
[0009] The construction of the light and air tube includes a reflective liner of a suitable plastic, a center insulation, such as bubble wrap, and an outer liner of aluminum foil. This construction provides good light transmission, insulation against cold and heat, and a good fire retardant radiant barrier.
[0010] The skylight has a dome covering the top opening, such dome is preferably white to further maximize the light transmitted to the interior of the building.
[0011] It is therefore and object of the present invention to provide a new and improved roof to ceiling skylight which may be easily manufactured as a reasonable cost.
[0012] Another object of the present invention is to provide a skylight assembly that has the flexibility to bend and conform in an attic space to align with both a skylight and a ceiling opening.
[0013] It is a further object of the invention to provide a light and air tube with a light reflective inner wall, an insulation center core, and a fire retardant outer wall.
[0014] Still a further object of the present invention is to provide a new and improved roof to ceiling skylight apparatus which eliminates the need for a customized construction of a light conveyance between a roof-mounted skylight and a ceiling-mounted translucent fixture.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] [0015]FIG. 1 shows the outline of a roof and a partial ceiling connected by a light and air conducting tube where one end of the tube is connected to a skylight and at the other end to a ceiling translucent or transparent fixture.
[0016] [0016]FIG. 2 shows a partial cross-section of a light and air conducting tube of the invention.
[0017] [0017]FIG. 3 shows another embodiment of a cross-section of a light and air conducting tube of the invention.
DESCRIPTION OF THE INVENTION
[0018] Referring to the drawings, FIGS. 1 to 3 , there is shown the outline of a house or building roof 10 , having a skylight 12 , and a partial section of an interior ceiling 14 having an opening 16 covered by a light panel 18 , a light and air conducting tube 20 connects the skylight 12 to the ceiling light panel 18 . As can be seen, the skylight 12 and the ceiling light panel 18 are out of alignment. That is to say, they are not in vertical alignment therefore, the light and air conducting tube 20 is flexible in order to connect skylight 12 to ceiling light panel 18 . While the tube 20 is flexible, it is still firm enough to support its own weight.
[0019] It is shown in FIG. 1, that the light and air conducting tube has a square or rectangular cross-section which among other things provides a larger light area than would a round or circular cross-section.
[0020] [0020]FIG. 2 shows a partial cross-section of a light and air conducting tube 20 . Having an interior liner 22 , a center insulation core 24 and an outside layer 26 . The interior liner has metallized polyester such as WMP-50 building facing material by Lamtech or similar materials made by Alpha Associates, Inc. such as VR-R which use a white polypropylene (PP) film with a metallized polyester film backing and fiberglass scrim tear stopper. Alternately, the reflective coating can also be achieved by using a silver sputter process on various flexible plastic films or specialty film such as 3M Silverlux or the newer High Reflective Mirror Films. The main concern is to achieve the highest degree of light reflectance at the most economical cost. Currently a hot-melt glue is used to laminate the reflective liner to the “top side” of the Astro-Foil bubble wrap. This “top side” can be sealed with a plastic cap or alternately finished with aluminum foil if extra strength or firmness is desired.
[0021] The center insulation core 24 is made of {fraction (3/16)} single polyethylene air bubble material (FIG. 1) or ⅜ polyethylene air bubble material (FIG. 2). The air bubble provides insulation from hot and cold air convection. Currently our preferred material in production is the single bubble ({fraction (3/16)}″) which is . 1875 thick plus the WMP-50 reflective liner which is about 9 mils thick which with glue is about 0.200″ thick (200 mils)-or one fifth of an inch. The combination of all of these materials provides a very firm composite that is highly compact for shipping, flexible for installation and suitably rigid after fabricating and installing in place as a skylight tube. The double-bubble material might be preferred for larger skylight tubes to enhance firmness (rigidity) or where more insulation is needed to meet more extreme temperature conditions. Outside layer 26 has a plastic cap usually extruded from the same material as the air bubble chambers lined with a commercial grade aluminum foil for strength and durability. The aluminum foil is typically 99% pure AL and acts as a barrier against radiant heat gain or loss from the invented skylight tube. The plastic cap is a minimum part of the bubble-wrap insulation material, but normally comes with aluminum foil bonded to at least one side. Although the aluminum foil is optional, it is the preferred construction method because of its inexpensive fire retardant radiant barrier advantages.
[0022] The light reflective material can by made of virtually any high polished metal of metallized film or metallized fabric material. There are at least several commercially available which are already fire related and/or ASTM or UL listed, etc. Currently a commercial grade metallized film is used with a polypropylene scrim weave core for added strength and durability such as WMP-50 by Lamtech. The key is to have the reflective material attached (bonded or laminated, etc.) to a firm-yet flexible backing which is also code and fire rated for use as building material, such as the above mentioned Astro-Foil bubble wrap. The bubble foil core 24 can range in thickness from about ⅛″ to ¼ thick (preferably 0.200″ thick) but should consist of a firmness able to hold up it's own weight when held out about 24″ in length or width. The suitable material should ideally insulate well and yet be flexible enough to be easily cut such as scissor trimmed for ease of installation. At the top and bottom it would be attached by staples or similar fastening means such as rivets, screws or tape. After installation, a quick hand or pole insertion would help unfold or open up any area(s) inside the tube such as around bends. The seam or seams could run where ever needed to accommodate standard and/or custom fit size runs. However, normally a seam would run parallel to the length of the tube for smaller tubes and for larger or longer tubes there may be more than one seam running either length wise or perhaps also two or more around the circumference of the tube to accommodate unique sizes. As mentioned before, the outside layer 26 of the tube is optional and can come with a reflective material as a further insulation barrier or may also come without it. The outside layer of reflective aluminum foil is being used in the current preferred embodiment.
[0023] In FIG. 3, a double air bubble core is shown to increase the insulation quality of the core 24′.
[0024] While only one embodiment of the invention has been shown, it is understood that one skilled in the art may realize other embodiments. Therefore, one should consider the drawings, description and claims in their entirety.
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This invention relates to a flexible light conduit having two ends, one end mounted to an outdoor support such as a roof and at it's other end to a ceiling or other support inside a structure such as a house, garage, shed or other structure, said light conduit being of any shape in cross section, preferably square or rectangular and lined with any material or combination of materials for insulation, ornamentation and the like.
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BACKGROUND OF THE INVENTION
The present invention is broadly concerned with a spinal fusion cage system. More particularly, it is directed to an articulated implant which can be installed between a pair of adjacent vertebrae and selectively expanded in situ to form a wedge with an adjustable angle of inclination for supporting and stabilizing the vertebrae in normal curved alignment in order to promote fusion of the aligned vertebrae.
The spine is a column of stacked vertebrae which are normally axially aligned along the median plane. When viewed from the front or back, the spine appears to be straight. When viewed from a lateral perspective, however, it is shown to be comprised of four distinct curves. Each vertebra is angularly displaced in the coronal plane in accordance with its position along one of the respective curves.
The structure of each vertebra includes a rounded, weight bearing anterior element, or vertebral body, which is separated from the adjacent superior and inferior vertebral bodies and cushioned by fibrocartilage pads or discs. These intervertebral discs support the adjacent vertebrae in an appropriate angular orientation within a respective spinal curve and impart flexibility to the spine so that it can flex and bend yet return to its original compound curvate configuration.
Aging, injury or disease may cause damage to the discs or to the vertebrae themselves. When this occurs, it may be necessary to surgically remove a disc and fuse the adjacent vertebral bodies into a single unit. Such surgical arthrodesis is generally accomplished by implanting a cage-like device in the intervertebral or disc space. The cages are apertured, and include a hollow interior chamber which is packed with live bone chips, one or more gene therapy products, such as bone morphogenic protein, cells that have undergone transduction to produce such a protein, or other suitable bone substitute material. Following implantation, bone from the adjacent vertebrae above and below the cage eventually grows through the apertures, fusing with the bone of the adjacent vertebral bodies and fixing the adjacent vertebrae as well as the cage in position.
Once the disc has been removed from the intervertebral space, the angular orientation of the adjacent vertebrae is established and stabilized by the three dimensional geometry of the implanted fusion cage, and the vertebrae will eventually fuse in this orientation. The lumbar curve presents a region of normal anterior convexity and posterior concavity or lordosis. There is a need for an anterior implant for use in this region which can be adjusted in situ to achieve and maintain normal lordosis of the vertebrae.
Previous attempts to achieve normal spinal curvature with fusion cages have involved trial insertion of cages of various different sizes into the intervertebral space. The cage is repeatedly removed and replaced with another unit of a slightly different size until an optimal angular incline is achieved. There is a need for a modular and articulated implant which can be installed in a first configuration, and adjusted in situ into a wedge configuration from an anterior access position.
Once installed in an intervertebral space, spinal implants are subject to compressive forces exerted by gravity and movement of the spinal column. Normal forward bending activity exerts substantially greater compressive force on the vertebrae than backward bending. Consequently, there is a need for an implant which will accept an increased anterior preload to withstand anterior compressive forces and to maintain the disc space height.
Spinal implants are also subject to twisting forces caused by unequal lateral distribution of weight on the adjacent vertebral bodies. This may occur, for example, during normal sideward bending and reaching activity. There is also a need for an implant which will provide torsional stability to resist such twisting forces. In particular, in order to withstand the greater compressive forces associated with forward bending movements, there is a need for an implant that will provide enhanced anterior torsional stability.
The apparatus of the present invention is specifically designed to provide a modular intervertebral implant which can be both installed and selectively expanded in situ from an anterior access position to form a wedge which stabilizes the adjacent vertebrae in normal curved alignment while providing lateral stability, increased anterior preload and enhanced anterior torsional stability.
SUMMARY OF THE INVENTION
The present invention is directed to an articulated modular cage system for implantation in the intervertebral space and adjustment in situ from an anterior access position to support the adjacent vertebrae in a normal curved alignment while permitting fusion of the adjacent bones. The fusion cage system of the present invention includes a first leg having a pivot member, a second leg having a socket for receiving the pivot member and a driver. The socket permits movement of the first leg about an axis of pivotal rotation from a closed, parallel insertion position to an anteriorly open, wedge-shaped orientation which may be selectively adjusted to provide appropriate angular support. The socket and pivot member are laterally elongated to provide lateral support. The pivot member includes a cylindrical notch or aperture, and the socket includes a threaded bore which are aligned for receiving a driver.
The driver is operable to engage a sloped interior surface of the first leg and to urge the anterior end of the first leg apart from the anterior end of the second leg while causing the pivot member to rotate within the socket. Registry of the driver within both the bore and the aperture serves to prevent lateral displacement of the pivot member within the socket. The pivot member and socket are inset or positioned anteriorly of the posterior ends of the respective legs in order to enhance torsional stability and to optimize the anterior preload. This is achieved by decreasing a moment arm length between an effective area of engagement of the adjacent vertebrae and the location of the connection between the legs of the cage. Positioning the pivot axis anterior of the posterior ends of the legs also helps to optimize the intervertebral spacing and angular alignment of the adjacent vertebrae to avoid undesirably stressing the next vertebrae beyond the vertebrae engaged by the fusion cage.
Objects and advantages of this invention will become apparent from the following description taken in conjunction with the accompanying drawings wherein are set forth, by way of illustration and example, certain embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partially exploded perspective view of an articulated expandable spinal fusion cage system in accordance with the present invention, illustrating a threaded driver.
FIG. 2 is a fragmentary side elevational view of the cage of FIG. 1 installed between adjacent vertebrae, showing a bore and interior surfaces in phantom to illustrate the path of installation of the driver.
FIG. 3 is a view similar to FIG. 2, illustrating the driver installed between the bearing surfaces of the legs and the anterior portions of adjacent vertebrae displaced to achieve lordosis.
FIG. 4 is a front elevational view taken along line 4 — 4 of FIG. 3 showing an anterior end of the top leg with the driver omitted.
FIG. 5 is a rear elevational view taken along line 5 — 5 of FIG. 3 showing a posterior end of the top leg with the driver omitted.
FIG. 6 is a bottom plan view taken along line 6 — 6 of FIG. 2, showing a bottom side of the top leg of the cage with the driver omitted.
FIG. 7 is a front elevational view taken along line 7 — 7 of FIG. 3 showing an anterior end of the bottom leg with the driver omitted.
FIG. 8 is a top plan view taken along line 8 — 8 of FIG. 2 showing a top side view of the bottom leg with the driver omitted.
The drawings constitute a part of this specification and include exemplary embodiments of the present invention and illustrate various objects and features thereof.
DETAILED DESCRIPTION OF THE INVENTION
As required, detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which may be embodied in various forms. Therefore, specific structural and functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed structure.
Certain terminology will be used in the following description for convenience in reference only and is not intended to be limiting. For example, the words “anterior”, “posterior”, “superior” and “inferior” and “lateral” and their derivatives will refer to the device as it may be installed in anatomical position as depicted in FIGS. 2-3.
Referring now to the drawings, an articulated anterior expandable spinal fusion cage system in accordance with the invention is generally indicated by the reference numeral 1 and is depicted in FIGS. 1-8. FIGS. 2 and 3 illustrate a partial side view of a human spine showing an intervertebral region 2 , which is the functional location of implantation of the fusion cage system 1 , between the vertebral bodies of selected upper and lower adjacent vertebrae 3 and 4 .
Referring again to FIG. 1, the fusion cage system 1 broadly includes a fusion cage 10 and a driver 11 . The cage 10 includes a first leg 12 depicted and normally installed in a superior orientation and adjustably coupled with a second, normally inferior leg 13 by a pivot joint or bearing 14 positioned posteriorly of a centerline C, passing midway between the ends. The first leg 12 has an anterior end 15 , a posterior end 16 and a pair of opposed sides 20 interconnected by a central web portion 21 . The sides of the cage 20 are depicted as generally planar and orthogonal to the web portion 21 , although they may also be of curvate, angular or compound curvate or angular construction. The legs 12 and 13 are normally of the same width and length, but it is also foreseen that either of the legs 12 and 13 may be of somewhat broader construction in order to selectively enhance the superior or inferior bone-supporting surface area.
The first leg 12 includes an outer, bone-supporting surface 22 and an inner surface 23 , best shown in FIG. 6 . The web 21 is apertured by one or more ports or windows 24 , which extend between the outer and inner surfaces 22 and 23 .
The leg inner surface 23 includes an anterior portion 30 and a posterior portion 31 . The anterior portion 30 has a linear cam or bearing surface 32 that terminates posteriorly in a first abutment surface or stop 33 that is generally orthogonal to the outer surface 22 . When viewed from the side (FIGS. 1 - 3 ), the bearing surface 32 slopes downwardly at an angle as it approaches the second end 16 in the configuration of a ramp or wedge having the abutment surface 33 as its base. The posterior portion 31 extends in generally parallel relationship with the web outer surface 22 except for a dependent, generally cylindrical pivot member 34 having a pivot axis P. The pivot member 34 depends the entire width of the cage 10 between the sides 20 and includes a central notch, aperture or groove 35 (FIGS. 4-6) for receiving the driver 11 .
The leg outer surface 22 includes a series of serrations or teeth 40 for engaging the surface of a respective adjacent vertebra 3 against slippage along an anterior-posterior axis within the intervertebral joint 2 . The leg inner surface 23 is generally smooth. The anterior bearing surface 32 is axially grooved to form a channel 41 (FIG. 6) adapted for sliding reception of the driver 11 .
The second leg 13 has an anterior first end 42 , a posterior second end 43 and a pair of opposed sides 44 interconnected by a central web portion 45 . The leg 13 also includes an outer, bone-supporting surface 50 and an inner surface 51 , best shown in FIG. 8 . The web 45 is apertured by one or more ports or windows 52 , which extend between the outer and inner surfaces 50 and 51 .
The leg inner surface 51 includes an anterior portion 53 and a posterior portion 54 . The anterior portion 53 has a support surface 55 that extends in generally parallel relationship with the leg outer surface 50 . The posterior portion 54 also extends in generally parallel relationship with the leg outer surface 50 , except for an upstanding, approximately rectangular knuckle 60 . The knuckle 60 is elongated laterally, so that it extends the full width of the cage 10 between the sides 44 .
The knuckle 60 includes anterior, posterior, and upper or superior surfaces 61 , 62 and 63 (FIG. 3 ). The superior surface 63 includes a laterally extending, generally cylindrical channel which serves as a socket 64 for receiving the cylindrical pivot member 34 of the first leg 12 in pivoting relationship to form the pivot bearing 14 . The laterally elongated pivot member 34 and socket 64 cooperatively provide lateral support to the cage 10 against sideward bending stresses which may be brought to bear following installation.
The anterior and posterior knuckle surfaces 61 and 62 are generally orthogonal to the outer surface 50 , and the anterior surface 61 serves as an abutment surface or stop for the first leg abutment surface 33 . The upper knuckle surface 63 is generally parallel with the outer surface 50 , except that the posterior aspect is somewhat relieved so that it does not serve as a stop when the first leg 12 pivots in the socket 64 of the second leg 13 . As shown in FIGS. 7 and 8, the knuckle 60 includes a central bore 65 having flighting or threads 70 for receiving and engaging the driver 11 .
Like the first leg 12 , the second leg outer surface 50 includes a series of bone-engaging serrations or teeth 71 (FIG. 2 ). The leg inner surface 51 is generally smooth. The first and second leg anterior portions 15 and 42 cooperatively define an open-sided chamber 72 when the cage 10 is assembled as depicted in FIGS. 1-3.
The driver 11 is depicted in FIG. 1 to include a radially expanded head 73 and a shaft 74 terminating in a generally flattened driving end 75 . The shaft 74 is sized and shaped for reception within channel 41 , and preferably includes threads 80 for operable reception within matingly threaded bore 65 , with the radially expanded driver head 73 engaging the angled bearing surface 32 of the upper leg 12 . It is also foreseen that in certain applications the shaft 74 could be smooth and unthreaded. The driver head 73 is coupled with the shaft 74 by a generally frustoconical shank portion 81 , and terminates in a narrow, generally cylindrical bearing surface 82 . The head 73 also includes a non-round socket or receiver 83 configured for non-slip reception of a driving tool such as a wrench (not shown). While the receiver 83 is depicted as being generally hexagonal in shape, it is understood that it may be configured as a square, slot, multi-lobular or any other shape corresponding to a preselected driving tool.
The diameter of the driver head 73 and the length of the shaft 74 are sized so that the driver 11 extends posteriorly through the channel 41 of the upper leg 12 for driving registry of the shaft 74 within the groove 35 of the first leg and central bore 65 of the lower leg 13 and engagement of the driver head bearing surface 82 with the angled bearing surface 32 of the upper leg 12 . In this manner, the channel 41 , groove 35 and bore 65 cooperate with the shaft 74 of the driver 11 to effectively lock the legs 12 and 13 against lateral displacement.
The legs 12 and 13 and driver 11 may be constructed of a non-metallic material such as carbon fiber reinforced composite or tissue-derived polymer material, or of a strong, inert material having a modulus of elasticity such as a metal, like stainless steel or titanium alloy, or of porous tantalum or any other biocompatible material or combination of materials. It is foreseen that it may be desirable in certain applications to employ a radiolucent material such as carbon fiber reinforced composite which will not block post operative radiographic images of bridging bone growth.
It is also foreseen that the fusion cage system 1 may also include a pair of independently adjustable cages 10 , installed in generally side-by-side relationship within a single intervertebral space 2 , as set forth more fully in U.S. Pat. No. 6,454,807 and incorporated herein by reference.
In use, the anterior surface of a selected intervertebral region 2 of the spine of a patient is surgically exposed. The soft tissues are separated, the disc space is distracted and the disc is removed, along with any bone spurs which may be present. The disc space is distracted to a predetermined height which serves to decompress any affected nerve roots and to permit preparation of the intervertebral region 2 .
The fusion cage system 1 is assembled by a surgeon or assistant by laterally aligning the cylindrical pivot member 34 of the first leg 12 with the socket 64 of the second leg 13 and sliding the pivot member 34 laterally into engagement with the socket 64 until the groove 35 is aligned with the bore 65 . The driver 11 is next grasped and the threaded end 75 is introduced into the bore 65 and rotated by hand or with the use of an insertion tool until the threads 80 of the driver shaft 74 engage the threads 70 of the bore 65 . Registry of the driver 11 within both the groove 35 of the first leg 12 and the bore 65 of the second leg serves to prevent any lateral movement or play of the pivot member 34 within the socket 64 . The driver 11 may be rotated a few additional turns in order to secure against disengagement from the bore 65 during insertion. However, unless the intervertebral space 2 is substantially larger than the cage 10 , rotation is generally stopped when the conical shank 81 engages the bearing surface 32 of the first leg 12 , so that the cage 10 can be inserted in its smallest, or closed configuration.
The first and second leg anterior first ends 15 and 42 are next grasped and pressed together until the first leg abutment surface 33 comes to rest against the second leg abutment surface or stop 61 and the cage 10 is maximally compressed. The assembled fusion cage 10 presents a closed, overall rectangular configuration, with the outer surfaces 22 and 50 of the legs 12 and 13 in a generally parallel orientation, as depicted in FIGS. 1 and 2 and the driver 11 projecting slightly anteriorly from the cage 10 .
The cage 10 may be press-fit directly into the distracted intervertebral region 2 , or the vertebrae 3 and 4 may be predrilled to receive the cage system 1 . Although an anterior approach is preferred, it is foreseen that a posterior or even lateral approach could also be employed.
The surgeon next positions a tool (not shown) in the driver head 73 and rotates the tool in a clockwise or posteriorly advancing direction to drive or pull the threaded shaft 74 further into the bore 52 and advance the head 73 in a posterior direction. Continued rotation of the driver 11 simultaneously causes the end 75 to advance posteriorly, the pivot member 34 to rotate within the socket 64 , and the bearing surface 32 of the first leg 12 to ride up over the beveled shank 81 until the bearing surface 82 of the driver 11 engages the bearing surface 32 of the first leg 12 . In this manner, rotational advancement of the driver 11 causes it to progressively wedge the bearing surface 32 apart from the support surface 55 of the second leg 13 until the cage 10 begins to assume a generally wedge shape when viewed from the side.
In this manner, the angle formed by the outer, bone supporting surfaces 22 and 50 of the legs 12 and 13 , is determined by the displacement of the bearing surfaces 32 of the first leg 12 away from the support surface 55 of the second leg 13 , which in turn is determined by the posterior advancement of the driver bearing surface 82 along the first leg bearing surface 32 . The driver 11 is of a preselected size to cause displacement of the first leg 12 to form the cage 10 into an appropriate wedge shape which will support the adjacent vertebrae 3 and 4 at the proper height as well as the desired angular alignment to achieve normal curvature of the respective spinal region.
Advantageously, the laterally elongate cylindrical configuration and anteriorly inset or forward positioning of the pivot bearing 14 cooperatively formed by the pivot member 34 and socket 64 , relative to the posterior ends 16 and 43 of the legs 12 and 13 , enhance both the lateral and torsional stability of the cage system 1 as well as its anterior-preload. The configuration of the channel 41 for receiving the driver shaft 74 and the anterior preload also cooperate to enhance torsional stability.
The surgeon next transplants a quantity of packed bone cells or a suitable bone substitute material into the chamber 72 by a lateral approach through the open area between the first and second legs 12 and 13 . Alternatively, the bone cells may be introduced into the chamber 72 by a posterior approach through the bore 65 prior to installation of the driver 11 or by any combination of these methods. Bone for use in the graft may be harvested from the patient as live bone, from a bone bank or from a cadaver. Demineralized bone matrix, bone morphogenic protein or any other suitable material may also be employed.
Following implantation, the bone grows between vertebrae 3 and 4 , through the windows 24 and 52 with the bone in the chamber 72 and around the cage system 1 to fuse the bodies of vertebrae 3 and 4 together.
Those skilled in the art will appreciate that the fusion cage 10 may also be assembled and installed into the intervertebral space 2 prior to insertion of the driver 11 into the bore 65 . In addition, while a single exemplary driver 11 and cage 10 having a wedge-shaped first leg 12 is depicted, a variety of drivers 11 and cages 10 , having variously configured bearing surfaces 32 of different shapes, each producing a different degree of displacement of the first leg 12 may be incorporated in a set to allow the surgeon to preselect a cage system 1 to achieve a desired angle of displacement and consequent positioning of the vertebrae 3 , 4 relative to each other. It is foreseen that various other configurations of the pivot bearing 14 could be advantageously employed in the cage system 1 .
The cage system 1 of the invention is designed to permit adjustment by rotation of the driver 11 in situ until the desired alignment between the vertebra 3 and 4 is achieved. However, if necessary, the cage system 1 may also be removed and the installation repeated using a cage 10 and driver 11 having different configurations until the desired angular alignment is achieved.
It is to be understood that while certain forms of the present invention have been illustrated and described herein, it is not to be limited to the specific forms or arrangement of parts described and shown.
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An articulated modular spinal fusion cage is implanted in the intervertebral space and adjusted in situ from an anterior access position to support adjacent vertebrae in normal curved alignment. The cage includes a first leg having a cylindrical pivot member and a second leg having a socket. The socket permits pivotal movement of the first leg with respect to the second leg to an anteriorly open, wedge-shaped orientation which may be selectively angularly adjusted. The laterally elongated socket and pivot member form a fulcrum that is positioned anteriorly from the posterior leg ends to enhance torsional stability and increase anterior preload. A driver is inserted through a bore in the socket and corresponding groove in the flange and is operable to engage a sloped interior surface of the first leg and to urge the anterior end upwardly by rotating the pivot member within the socket.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a magnetic disk device that incorporates a driving unit for driving a magnetic disk and can be mounted to and removed from the body of an apparatus, and an electronic apparatus including the magnetic disk device and a body for mounting the magnetic disk device thereto.
[0003] 2. Description of the Related Art
[0004] A removable magnetic disk device that can be mounted to and removed from the body of various apparatuses is one type of magnetic disk device usable in, for example, a vehicle-installed electronic apparatus, an information appliance, or a video recorder. This type of magnetic disk device is disclosed in Japanese Unexamined Patent Application Publication No. 6-176555 and PCT Japanese Translation Patent Publication No. 2001-502103.
[0005] In this type of magnetic disk device, a hard disk is mounted as a recording medium in a case formed of a hard metal or synthetic resin. In addition, a rotary driver for rotationally driving the hard disk, a magnetic head unit for recording digital signals onto the hard disk and reproducing the digital signals recorded on the hard disk, a control circuit for controlling driving operations of the rotary driver and the magnetic head unit, a digital signal processing circuit, an interface circuit, etc., are mounted in the case.
[0006] The case has a predetermined thickness and a rectangular shape. Connector means connected to the various circuits is disposed at the front portion of the case.
[0007] A connector for connecting with the connector means is disposed at the body of an apparatus. The various circuits in the case and circuits of the body of the apparatus are connected by mounting the magnetic disk device to the body of the apparatus and fitting the connector means at the case to the body connector.
[0008] Unlike a related magnetic disk device that has a hard disk mounted thereto and is fixed in a computer or various information apparatuses, the removable magnetic disk device can be removed from the body of the apparatus. Therefore, the removed magnetic disk device needs to be protected from shock that is produced, for example, when it is dropped.
[0009] As disclosed in the aforementioned Japanese Unexamined Patent Application Publication No. 6-176555 and PCT Japanese Translation Patent Publication No. 2001-502103, a dampener is installed in the case of the magnetic disk device in order to protect the rotary driver and the magnetic head unit from shock produced, for example, when the magnetic disk device is dropped.
[0010] In the removable magnetic disk device, the use of a soft elastic member having a low elastic modulus is used as the dampener for protecting the rotary driver and the magnetic head unit in the case may increase the error rate of the recording operation and that of the reproducing operation.
[0011] In a magnetic disk device used for high recording density, the recording track density of the hard disk is high, the recording/reproduction track width of the magnetic head is small, and the linear recording density along the tracks is high. In this type of magnetic disk device, in order to prevent damage to a recording surface of the hard disk, sliding friction force between a magnet head chip and the recording surface of the hard disk is reduced by forming an air bearing between the magnetic head chip and the recording surface of the hard disk.
[0012] In recording information onto and reproducing the information from the hard disk, the magnetic head chip carries out a very precise operation. That is, it searches for a sector in a recording area of the hard disk at a high speed, and instantaneously performs tracking of tracks in the searched sector.
[0013] Therefore, when the rotary driver and the magnetic head unit are supported by a soft elastic member in the case, the hard disk and the magnetic head unit tend to move due toby vibration generated when the magnetic head unit performs the aforementioned searching operation. When this occurs, the spacing between the magnetic head chip and the surface of the hard disk changes to a value equal to or greater than a standard value, and the tracking operation is affected. As a result, the error rates of data recorded on the hard disk and of data reproduced from the hard disk are increased.
[0014] Consequently, it is necessary to use a hard dampener having a high elastic modulus for the dampener disposed in the case of the magnetic disk device. However, such a hard dampener cannot sufficiently protect the components in the case. As a result, a large shock applied to the magnetic disk device when, for example, it is dropped by mistake tends to result in, for example, scratching of a surface of the hard disk or damage to the magnetic head chip.
SUMMARY OF THE INVENTION
[0015] Accordingly, it is a first object of the present invention to provide a magnetic disk device that sufficiently protects a hard disk and a magnetic head unit in a case from, for example, external shock when the magnetic disk device is not mounted to the body of an apparatus, and to prevent a dampener from adversely affecting the magnetic disk device when the magnetic disk device is mounted to the body of the apparatus. A second object of the present invention is to provide an electronic apparatus for mounting the magnetic disk device thereto.
[0016] According to one embodiment of the present invention, there is provided a magnetic disk device removable from an apparatus body. The magnetic disk device comprises a case including an elastic supporting member and a locking member; a driving unit including a magnetic disk and a rotary driver for rotationally driving the magnetic disk, the driving unit being installed in the case; and a connector for connecting the driving unit and the apparatus body. The elastic supporting member elastically supports the driving unit. The locking member is movable between a lock position and an unlock position, the driving unit being locked at the lock position and being unlocked at the unlock position in the case. In addition, the locking member moves to the lock position and the unlock position by operational force from the exterior of the case.
[0017] According to another embodiment of the present invention, there is provided an electronic apparatus comprising a body for mounting the magnetic disk device thereto. The body comprises a body connector for connecting with the connector of the magnetic disk device, and a switching unit for moving the locking member to the lock position when the magnetic disk device is mounted.
[0018] When the magnetic disk device is removed from the body of the apparatus, the driving unit is set in an elastically supported state in the case by externally operating the locking member, thereby protecting the magnetic disk device from external shock. Immediately before mounting the magnetic disk device to the body of the apparatus or after mounting it to the body of the apparatus, the driving unit is locked in the case by operating the locking member in order to restrict unnecessary movement of the hard disk and the magnetic head unit when performing a recording operation or a reproducing operation, thereby making it possible to reduce error rate.
[0019] In the magnetic disk device and the electronic apparatus for mounting the magnetic disk device in a preferred embodiment of the present invention, the locking member may be moved to the lock position and the unlock position by operation of the locking member by a user with his/her finger or by the switching unit disposed at the body of the apparatus.
[0020] For example, a structure may be used in which the locking member reaches the unlock position by moving towards a front portion of the magnetic disk device relative to the case, and reaches the lock position by moving towards a rear portion of the magnetic disk device relative to the case, the front portion corresponding to a side of the magnetic disk device where the connector is disposed and the rear portion corresponding to a side opposite thereto.
[0021] By virtue of such a structure, it is possible to move the locking member to the lock position by making use of mounting force is produced when the magnetic disk device is mounted.
[0022] The locking member may be biased in the direction of the unlock position by a biasing member.
[0023] By virtue of such a structure, the driving unit is unlocked by operating the locking member by biasing force of the biasing member, such as a spring, when the magnetic disk device is not mounted to the body of the apparatus. In addition, the driving unit may be locked by moving the locking member to the lock position against the biasing force of the biasing member when the magnetic disk device is mounted to the body of the apparatus.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] FIG. 1 is an exploded perspective view of a magnetic disk device according to an embodiment of the present invention;
[0025] FIG. 2 is a perspective view showing a state of a mounting portion of the body of an electronic apparatus when the magnetic disk device is not mounted according to an embodiment of the present invention.
[0026] FIG. 3 is a perspective view showing a state of the mounting portion of the body of the electronic apparatus when the magnetic disk device is mounted according to an embodiment of the present invention.
[0027] FIGS. 4A and 4B are partial enlarged perspective views illustrating a locking member in an unlocked position and a locked position, respectively.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0028] A magnetic disk device 1 shown in FIG. 1 comprises a lower case portion 2 , an upper case portion 3 , and a connector case portion 4 . Each case portion is injection molded out of synthetic resin. The lower case portion 2 comprises a bottom surface 2 a , a left surface 2 b , a right surface 2 c , and a rear surface 2 d ; has a rectangular shape; and has a recess. The front portion of the bottom surface 2 a is formed as a fitting portion 2 e having a somewhat smaller width. The upper case portion 3 comprises a ceiling surface 3 a , a left frame 3 b , a right frame 3 c , and a rear frame 3 d ; has a rectangular shape; and has a shallow recess. The front portion of the ceiling surface 3 a is formed as a fitting portion 3 e having a somewhat smaller width.
[0029] The connector case portion 4 comprises a fitting recess 4 a at its upper surface and a fitting recess 4 b at its lower surface. The connector case portion 4 has positioning holes 4 c and 4 c passing through the fitting recess 4 a and the fitting recess 4 b . A pair of upwardly protruding positioning protrusions 5 and 5 are formed on the front portion of the bottom surface 2 a of the lower case portion 2 . A pair of downwardly protruding positioning protrusions 6 and 6 are formed on the front portion of the ceiling surface 3 a of the upper case portion 3 .
[0030] When the fitting portion 2 e of the lower case portion 2 is fitted to the fitting recess 4 b of the connector case portion 4 , and the fitting portion 3 e of the upper case portion 3 is fitted to the fitting recess 4 a of the connector case portion 4 , the positioning protrusions 5 and 5 on the lower case portion 2 and the positioning protrusions 6 and 6 on the upper case portion 3 are vertically fitted to the positioning holes 4 c and 4 c , so that the lower case portion 2 , the upper case portion 3 , and the connector case portion 4 are combined, thereby forming a rectangular case C having a hollow interior. The lower case portion 2 and the upper case portion 3 are secured by, for example, screws.
[0031] A rectangular driving unit 10 is installed in the case C. The volume of the driving unit 10 is smaller than the volume of the space in the case C that is formed when the lower case portion 2 and the upper case portion 3 are combined. Spaces are formed between the driving unit 10 and the bottom surface 2 a , the ceiling surface 3 a , the left surface 2 b , the right surface 2 c , and the connector case portion 4 , respectively.
[0032] A plurality of elastic supporting members 7 are disposed between the bottom surface 2 a of the lower case portion 2 and the driving unit 10 . A plurality of elastic supporting members 8 are similarly disposed between the ceiling surface 3 a of the upper case portion 3 and the driving unit 10 . It is desirable that elastic supporting members are disposed between the driving unit 10 and the left surface 2 b of the lower case portion 2 , the driving unit 10 and the right surface 2 c of the lower case portion 2 , and between the driving unit 10 and the rear surface 2 d of the lower case portion 2 .
[0033] Each elastic supporting member 7 and each elastic supporting member 8 is formed of soft synthetic rubber having a low elastic modulus, such as butyl rubber or silicone rubber, and is, desirably, formed of viscoelastic rubber and has a sheet shape or a columnar shape. Each elastic supporting member 7 and each elastic supporting member 8 may be a damper comprising a bag formed of a flexible material, such as rubber, and which is filled with a fluid such as air or a liquid. The driving unit 10 is elastically supported by the elastic supporting members 7 and the elastic supporting members 8 so as to be movable leftward, rightward, upward, downward, forward, or backward within a range of approximately 0.1 to 2 mm.
[0034] The driving unit 10 comprises a hard case portion 11 which is thin and has a cubic shape. The hard case portion 11 is formed by bending a nonmagnetic metallic plate, or by using synthetic resin. A pair of protrusions (locks) 18 are spaced apart in the forward-and-backward directions and fixed to one of the side surfaces of the hard case portion 11 . Similarly, a pair of protrusions 18 are spaced apart in the forward-and-backward directions and fixed to the other side surface of the hard case portion 11 .
[0035] A hard disk 12 , which is a magnetic disk, and a rotary driver 13 , such as a spindle motor, for rotationally driving the hard disk 12 are disposed in the hard case portion 11 . In the driving unit 10 , the hard disk 12 in the hard case portion 11 cannot be replaced and is rotationally driven in a closed space in the hard case portion 11 .
[0036] A magnetic head unit 14 is installed in the hard case portion 11 . The magnetic head unit 14 comprises a magnetic head chip 14 a opposing a magnetic recording surface of the hard disk 12 , a load beam 14 b for applying a predetermined load pressure to the magnetic head chip 14 a , and an access actuator 14 c for rotating the load beam 14 b around a shaft 14 d.
[0037] The magnetic head chip 14 a comprises a slider opposing the magnetic recording surface of the hard disk 12 , a reading unit comprising a magnetoresistive element mounted to the slider, and a writing unit comprising a thin-film inductive head. In recording digital signals onto the hard disk 12 , or in reproducing the digital signals from the hard disk 12 , the magnetic head chip 14 a floats slightly through an air bearing at the surface of the hard disk 12 rotating at a high speed. Then, the load beam 14 b is rotated by the access actuator 14 c , so that the magnetic head chip 14 a searches for a sector on the magnetic recording surface of the hard disk 12 , and the reading unit or the writing unit performs a tracking operation in order to read or write the signals.
[0038] A circuit board (not shown) is mounted in the hard case portion 11 , and has various circuits mounted thereto. The various circuits include a control circuit for controlling a driving operation of the rotary driver 13 ; a control circuit for controlling the operation of the magnetic head unit 14 ; a digital signal processing circuit for, for example, formatting a write signal and deformatting a read signal; and an interface circuit.
[0039] A connector 16 is installed in the connector case portion 4 . Each terminal of the connector 16 and each of the circuits in the driving unit 10 are in electrical conduction through an electrically conductive pattern on a flexible printed circuit board 17 . The flexible printed circuit board 17 is in a slightly flexed state, and can allow the driving unit 10 to move in the magnetic disk device 1 . The flexible printed circuit board 17 also operates as an elastic supporting member for elastically supporting the driving unit 10 in the case C.
[0040] A groove 21 is continuously formed in the forward-and backward-directions from the left surface of the connector case portion 4 to the outer side of the left surface 2 b of the lower case portion 2 . A slit 22 passing through the left surface 2 b of the lower case portion 2 and extending in the forward-and-backward directions is opens in the groove 21 . Similarly, a groove 21 and a slit 22 are also formed in the right surface of the connector case portion 4 and in the right surface 2 c of the lower case portion 2 .
[0041] A locking member 23 is disposed at the inner side of the left surface 2 b of the lower case portion 2 . The locking member 23 is supported by guide means (not shown) so as to be movable towards the front and back along the left surface 2 b . A switching protrusion 23 a is integrally formed with the outer surface of the locking member 23 , and is exposed in the groove 21 through the slit 22 . The slit 22 is wider than the switching protrusion 23 a in the forward-and-backward directions, so that the switching protrusion 23 a can slide in the slit 22 in the forward-and-backward directions. Therefore, when a user moves the switching protrusion 23 a with his/her finger towards the front or the back, the locking member 23 slides towards the front or the back in the case C.
[0042] Lock grooves 23 b that are spaced apart in the forward-and-backward directions are formed in the locking member 23 . Each lock groove 23 b has a recess which opens at the back. The lock grooves 23 b oppose the protrusions (locks) 18 protruding from the associated left surface of the driving unit 10 . Similarly, a locking member 23 which moves in the forward-and-backward directions is also formed at the inner side of the right surface 2 c of the lower case portion 2 . This locking member 23 also has a switching protrusion 23 a and lock grooves 23 b . Although in this embodiment the two locking members 23 operate separately, it is desirable that the locking members 23 both move together in the forward-and-backward directions by integrally connecting both of the locking members 23 .
[0043] FIGS. 2 and 3 illustrate a mounting portion 30 in an apparatus body 100 for removably mounting the above-described magnetic disk device 1 .
[0044] The mounting portion 30 comprises a mounting frame 31 . The mounting frame 31 is formed by bending a metallic plate, and comprises a bottom plate 31 a, a left plate 31 b, and a right plate 31 c. An engager 31 d is formed by bending the top end portion of the left plate 31 b inward, and an engager 31 e is formed by bending the top end portion of the right plate 31 c inward. The engager 31 d moves into the groove 21 in the left surface 2 b of the magnetic disk device 1 , and the engager 31 e moves into the groove 21 in the right surface 2 c of the magnetic disk device 1 . The rear end of the engager 31 d and the rear end of the engager 31 e are formed as a first engager portion 31 d 1 and a first engager portion 31 e 1 , respectively.
[0045] A flat sliding member 32 is disposed on the bottom plate 31 a. A guide slot 33 extending in a straight line in forward and backward is formed in the sliding member 32 . The sliding member 32 is slidable in the forward and backward by guiding the guide slot 33 by guide protrusions 34 secured to the bottom plate 31 a. The left and right front end portions of the sliding member 32 are bent upwards at right angles to form contacts 32 a.
[0046] A pair of switching holes 35 that are spaced apart are formed, one at the right ride and one at the left side of the rear portion of the sliding member 32 . Each switching hole 35 comprises a non-engaging switching portion 35 a , an engaging switching portion 35 b , and an inclined portion 35 c . The non-engaging switching portions 35 a oppose each other with a certain distance therebetween and extend parallel to each other in the forward-and-backward directions. The engaging switching portions 35 b are disposed behind the non-engaging switching portions 35 a , oppose each other with a distance therebetween that is smaller than the certain distance, and extend parallel to each other in the forward-and-backward directions. The inclined portions 35 c connect the corresponding non-engaging switching portions 35 a and the corresponding engaging switching portions 35 b.
[0047] As shown in FIG. 3 , a pair of engaging plates 41 are disposed at the lower surface of the bottom plate 31 a. The engaging plates 41 are guided by a guide mechanism (not shown) and are supported so as to be slidable in the forward-and-backward directions and in the leftward-and-rightward directions perpendicular thereto. Sliding protrusions 42 are secured to the respective engaging plates 41 , and are inserted in the respective switching holes 35 of the sliding member 32 through respective guide holes 43 (see FIG. 3 ) that are formed in a straight line towards the left and right in the bottom plate 31 a.
[0048] Engagers 41 a which are formed at right angles are integrally formed with ends of the respective engaging plates 41 , and operate as second engager portions.
[0049] In this embodiment, the first engager portions 31 d 1 and 31 e 1 operate as first switching portions that allow the locking members 23 to move backward relative to the case C in the magnetic disk device 1 and reach lock positions. The engagers 41 a, which are second engager portions operate as second switching portions which allow the locking members 23 to move forward relative to the case C and reach unlock positions. As described later, by the first switching portions and the second switching portions, the locking members 23 move from the unlock positions to the lock positions when the magnetic disk device 1 is inserted into the apparatus body 100 , whereas the locking members 23 move from the lock positions to the unlock positions when the magnetic disk device 1 is removed from the apparatus body 100 .
[0050] The engaging plates 41 , the sliding protrusions 42 , and the switching holes 35 formed in the sliding member 32 operate as a switching setting mechanism for engaging the engagers 41 a, which are second engager portions, with the respective locking members 23 by moving the engagers 41 a towards each other, and for disengaging the engager portions 41 a from the respective locking members 23 by moving the engager portions 41 a and 41 a away from each other.
[0051] As shown in FIG. 3 , a slot 3 If extending in the forward-and-backward directions is formed in the left plate 31 b. A protrusion 32 b is integrally formed with the sliding member 32 , and protrudes towards the left and outwards from the slot 31 f. An ejector 45 for pushing the protrusion 32 b backwards is disposed at the outer side of the left plate 31 b . It is desirable that the sliding member 32 be biased backwards by a weak spring material as shown in FIG. 2 .
[0052] A body connector 50 is disposed in front of the mounting frame 31 . A fitting portion 51 of the body connector 50 faces backward.
[0053] Next, the mounting of the magnetic disk device 1 will be described.
[0054] FIGS. 4A and 4B are partial perspective views for describing the mounting of the magnetic disk device 1 . Here, the lower case portion 2 of the magnetic disk device 1 , the sliding member 32 disposed at the mounting portion 30 , etc. are not shown. The relationship between the driving unit 10 and the locking member 23 in the magnetic disk device I is only illustrated. In the mounting portion 30 , the operations of the first engager portion 31 d 1 and the engager 41 a are only described. Since the operation of the locking member 23 disposed at the right surface 2 c of the lower case portion 2 is the same as the operation of the locking member 23 shown in FIGS. 4A and 4B , only the operation of the locking member 23 at the left surface 2 b will be described.
[0055] When the magnetic disk device 1 is not mounted to the mounting portion 30 of the apparatus body 100 , and before the magnetic disk device 1 is completely mounted to the mounting portion 30 , in the magnetic disk device 1 , as shown in FIG. 4A , the locking member 23 is at the unlock position which it reaches by moving forward, and the protrusions (locks) 18 are not inserted in the respective lock grooves 23 b of the locking member 23 . Therefore, in the case C of the magnetic disk device 1 , the driving unit 10 is elastically supported by the elastic supporting members 7 and the elastic supporting members 8 .
[0056] A structure for increasing the sliding load of the locking member 23 with the locking member 23 and a sliding plate spring (not shown) being fixed in the lower case portion 2 may be used as means for stabilizing the locking member 23 at the unlock position shown in FIG. 4A when the magnetic disk device 1 is not mounted to the mounting portion 30 . It is desirable to use a structure for stabilizing the locking member 23 at the unlock position by biasing the locking member 23 by biasing force of a biasing member, such as a pulling force of a pulling coil spring S (see FIG. 1 ) or a pushing force of a compression coil spring, in the forward direction (that is, in the direction f in FIG. 4B ).
[0057] When the magnetic disk device 1 is not mounted to the mounting portion 30 of the apparatus body 100 , the driving unit 10 in the case C is elastically supported by the elastic supporting members 7 and the elastic supporting members 8 without being locked by the locking member 23 . Therefore, even if a large shock is accidentally applied to the magnetic disk device 1 , it is possible to prevent an excessive shock from being directly applied to the driving unit 10 . Consequently, it is possible to prevent a surface of the hard disk 12 from becoming damaged due to collision with the magnetic head chip 14 a , or to prevent the magnetic head chip 14 a from becoming damaged.
[0058] When the magnetic disk device 1 is not mounted to the apparatus body 100 , as shown in FIG. 2 , the sliding member 32 is moved back in the mounting portion 30 . At this time, since the sliding protrusions 42 at the respective engaging plates 41 are positioned in the non-engaging switching portions 35 a of the respective switching holes 35 in the sliding member 32 , the engaging plates 41 are moved outwards to the left and right, respectively, and are disposed away from each other. Therefore, when the magnetic disk device 1 is mounted to the mounting portion 30 , the engagers 41 a will not prevent insertion of the magnetic disk device 1 .
[0059] The magnetic disk device 1 having its connector case portion 4 faced forward is inserted into the mounting portion 30 from an insertion opening 101 of the apparatus body 100 shown in FIG. 2 . In the insertion of the magnetic disk device 1 , the engager 31 d bent at the left plate 31 b and the engager 31 e bent at the right plate 31 c move into the groove 21 in the left surface 2 b and the groove 21 in the right surface 2 c of the lower case portion 2 shown in FIG. 1 , respectively. While being guided by the engagers 31 d and 31 e, the magnetic disk device 1 is inserted. Accordingly, the engagers 31 d and 31 e function as guide members when mounting the magnetic disk device 1 to or ejecting it from the mounting portion 30 .
[0060] When the magnetic disk device 1 is inserted, and the front surface of the connector case portion 4 strikes the contacts 32 a of the sliding member 32 shown in FIG. 2 , the sliding member 32 thereafter moves forward along with the magnetic disk device 1 by the force that is generated by the insertion of the magnetic disk device 1 .
[0061] When a front end 23 a 1 of the switching protrusion 23 a protruding in the groove 21 in the left surface 2 b of the magnetic disk device 1 contacts the first engager portion 31 d 1 at the rear end of the engager 31 d, or immediately before or after the contact, as shown in FIG. 3 , the sliding protrusions 42 move into the engaging switching portions 35 b of the respective switching holes 35 in the sliding member 32 , so that the engaging plates 41 move towards each other. Therefore, as shown in FIG. 4B , after the switching protrusion 23 a on the locking member 23 has moved forward along the inner side of the engager 41 a, when the front end 23 a 1 contacts the first engager portion 31 d 1 or immediately before or after the contact, the engager 41 a moves into a vertical groove 21 a in the left surface 2 b shown in FIG. 1 , and opposes a rear end 23 a 2 of the switching protrusion 23 a with a slight gap therebetween.
[0062] When the magnetic disk device 1 is further inserted into the apparatus body 100 towards the body connector 50 , the whole magnetic disk device 1 moves forward while the switching protrusion 23 a on the locking member 23 engaging the first engager portion 31 d 1 does not move. Therefore, as shown in FIG. 4B , the protrusion 18 on the driving unit 10 moves from a position 18 - 1 to a position 18 - 2 where it is inserted in the lock groove 23 b . In other words, in the magnetic disk device 1 , the locking member 23 moves backward relative to the case C and reaches the lock position where the driving unit 10 is locked in the case C. The front end of the connector 16 at the front portion of the driving unit 10 is fitted to the body connector 50 .
[0063] Therefore, with the magnetic disk device 1 being mounted to the mounting portion 30 , the driving unit 10 is secured, and recording and reproducing of information are carried out in the magnetic disk device 1 . Here, with the driving unit 10 being locked by the locking member 23 in the case C, the hard disk 12 is rotationally driven to operate the magnetic head unit 14 . Therefore, it is possible to prevent, for example, the recording surface of the hard disk 12 from becoming scratched or the magnetic head chip 14 a from becoming damaged when the hard disk 12 or the magnetic head unit 14 is inadvertently moved due to, for example, vibration.
[0064] When the magnetic disk device 1 is ejected from the apparatus body 100 , the ejector 45 shown in FIG. 3 is moved backward, for example, by direct operation of the ejector 45 by the user, or by motor power. At this time, the ejector 45 pushes the protrusion 32 b backward, causing the sliding member 32 to slide backward. The contacts 32 a of the sliding member 32 push back the magnetic disk device 1 along with the sliding member 32 , so that the connector 16 of the magnetic disk device 1 is separated from the body connector 50 .
[0065] At this time, the magnetic disk device 1 moves backward while the locking member 23 is stopped by the engagement of the rear end 23 a 2 of the switching protrusion 23 a of the locking member 23 with the engager 41 a. Therefore, the protrusion 18 moves from the position 18 - 2 to the position 18 - 1 shown in FIG. 4B , and moves out of the lock groove 23 b in the locking member 23 , so that the driving unit 10 is elastically supported by the elastic supporting members 7 and the elastic supporting members 8 in the case C. In other words, in the magnetic disk device 1 , the locking member 23 moves forward relative to the case C and reaches the unlock position.
[0066] Backward movement of the sliding member 32 immediately after the protrusion 18 has moved out of the lock groove 23 b causes the sliding protrusions 42 to move into the non-engaging switching portions 35 a of the respective switching holes 35 . This causes the engaging plates 41 to move towards the left and right, respectively, so that the engagers 41 a move away from their respective switching protrusions 23 a . By this, the magnetic disk device 1 can be removed from the mounting portion 30 . That is, the magnetic disk device 1 can be removed from the insertion opening 101 of the apparatus body 100 .
[0067] The present invention is not limited to the above-described embodiment. Rather, various modifications can be made.
[0068] For example, in the magnetic disk device 1 , when the magnetic disk device 1 is not mounted to the mounting portion 30 , if the locking member 23 is stabilized at the unlock position by the biasing force of the biasing member, such as the pulling coil spring S or the compression coil spring, in the direction in which the protrusion 18 moves out of the lock groove 23 b (that is, the direction f in FIG. 4B ), the engager (second engager portion) 41 a does not necessarily have to be used.
[0069] In this case, if the first engager portions 31 d 1 and 31 e 1 are provided, while the magnetic disk device 1 is being inserted into the mounting portion 30 , the front end 23 a 1 of the switching protrusion 23 a and a front end 23 a 1 of the switching protrusion 23 a strike the first engager portions 31 d 1 and 31 e 1 , respectively. Thereafter, by the force produced by inserting the magnetic disk device 1 , the locking members 23 are moved to the lock positions against the biasing force of the corresponding biasing member and that of a corresponding biasing member in the magnetic disk device 1 . Then, when the magnetic disk device 1 is removed from the mounting portion 30 , the locking members 23 automatically move to the unlock positions by the biasing force of the biasing members.
[0070] In this case, it is desirable to provide, for example, a pushing member for holding down the rear surface 2 d of the mounted magnetic disk device 1 so that, while the magnetic disk device 1 is mounted to the mounting portion 30 , the magnetic disk device 1 is prevented from moving away from the body connector due to opposing force of the biasing members which bias the respective locking members 23 .
[0071] It is to be understood that a wide range of changes and modifications to the embodiments described above will be apparent to those skilled in the art and are contemplated. It is therefore intended that the foregoing detailed description be regarded as illustrative, rather than limiting, and that it be understood that it is the following claims, including all equivalents, that are intended to define the spirit and scope of the invention.
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A magnetic disk device is removable from an apparatus body includes a case, a driving unit, and a connector. The driving unit is installed in the case, and includes a magnetic disk and a rotary driver for rotationally driving the magnetic disk. The connector connects the driving unit and the apparatus body. The case includes an elastic supporting member and a locking member. The elastic supporting member elastically supports the driving unit. The locking member is movable between a locked position and an unlocked position, the driving unit being locked at the locked position and being unlocked at the unlocked position in the case. The locking member moves to the locked position and the unlocked position by operational force from the exterior of the case.
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FIELD OF INVENTION
The present invention relates in general to hydraulic fracturing, and in particular to systems and methods for controlling silica dust during the handling of frac sand.
BACKGROUND OF INVENTION
Hydraulic fracturing (“fracing”) is a well known technique for releasing oil and natural gas from underground reservoirs within rock formations having a limited permeability. For example, fracing is often used to release oil and natural gas, such as natural gas or oil, from shale formations.
Fracing is a well completion technique performed after the drilling of the wellbore, which in the case of releasing natural gas from shale, is commonly a horizontal wellbore, although occasionally the wellbore is vertical. Fracing fluid, which is primarily water and chemicals that form a viscous gel, is pumped into the well to create fractures within the surrounding rock. The viscous gel carries a “proppant” into the fractures, such that when the pumping stops, the fractures remain substantially open and allow the oil and natural gas to escape into the wellbore.
One typical proppant is “frac sand.” Frac sand is normally high purity silica sand with grains having a size and shape capable of resisting the crushing forces applied during the closing of the fractures when the hydraulic force provided by the pumping is removed. However, given that frac sand contains a high proportion of silica, the loading, transportation, and unloading of frac sand presents significant safety challenges.
The United States Occupational Safety and Health Administration (“OSHA”) lists silica as a carcinogen. In particular, the exposure and inhalation of silica dust has been linked to silicosis, which is an irreversible lung disorder characterized by inflammation and scarring of the upper lobes of the lungs. The best, and perhaps only way, to reduce or eliminate the threat of silicosis is to carefully control worker exposure to silica dust.
OSHA lists a number of different ways to limit worker exposure to silica dust, including limiting worker time at a worksite, limiting the number of workers at a worksite, watering roads and other worksite areas, enclosing points where silica dust is released, and requiring workers to wear respirators. These techniques do not, at least on their own, provide a complete solution to the problem of controlling silica dust. Furthermore, these existing techniques, while commendable, are nonetheless burdensome, time-consuming, inefficient, and impractical.
SUMMARY OF INVENTION
According to one representative embodiment of the principles of the present invention, a system is disclosed for controlling silica dust generated during the transfer of frac sand from a storage container through a conveyor system and includes a system of conduits having a plurality of inlets for collecting silica dust generated at selected points along the conveyor system. An air system pneumatically coupled to the system of conduits generates a negative pressure at each of the inlets to induce the collection of silica dust at the selected points along the conveyor, including container access ports, belt-to-belt drops, and belt-to-blender drops.
The present inventive principles advantageously provide for efficient and flexible systems and methods for collecting the silica dust generated during the offload of frac sand from one or more trailers or other storage facility at a fracing worksite. In particular, silica dust may be collected, as needed, at the base of the conveyor integral to each trailer (“trailer conveyor”), the point of discharge from each trailer conveyor to an associated portable conveyor system, at points along the portable conveyor system, and from within the trailer itself. The application of these principles improves the efficiency and flexibility of the frac sand offloading process by allowing increased worker time at the worksite and/or for more workers to be present at the worksite at one time, reducing the need for watering of worksite areas and the enclosure of points where silica dust is released, reducing the need for respirator wear, and decreasing the amount of silica dust intake by the engines of nearby vehicles and equipment.
BRIEF DESCRIPTION OF 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 perspective diagram of a representative frac sand transportation and unloading system including a frac sand silica dust control system according to a preferred embodiment of the principles of the present invention;
FIG. 2 is a plan view diagram of the frac sand transportation and unloading system of FIG. 1 , which emphasizes the airflow paths through the frac sand silica dust control system;
FIG. 3 is a plan view diagram of the frac sand transportation and unloading system of FIG. 1 , which generally indicates the locations of particular structures of the frac sand silica dust control subsystem shown in more detail in FIGS. 4-6 ;
FIG. 4A is a diagram showing in further detail the pneumatic connections between the inlets of the silica dust control unit and the manifolds of FIG. 1 ;
FIG. 4B is a diagram showing in further detail the direct airflow path between the silica dust control unit and the silica dust control conduit subsystem servicing one selected trailer of FIG. 1 ;
FIG. 4C is a diagram showing in further detail the pneumatic connection between a selected manifold and the silica dust control conduit subsystem serving another selected trailer of FIG. 1 ;
FIG. 4D is a diagram showing in further detail the pneumatic connections between a selected manifold and the silica dust capture hose controlling silica dust generated during the operation of a corresponding trailer discharge conveyor shown in FIG. 1 ;
FIG. 4E is a diagram showing in further detail the pneumatic connections between a selected manifold and the silica dust capture hoses controlling silica dust generated by the system discharge conveyor of FIG. 1 ;
FIG. 5A is a diagram showing in further detail a selected silica dust capture hose controlling silica dust generated by the discharge of frac sand from the tank of representative trailer to the base of the corresponding trailer discharge conveyor shown in FIG. 1 ;
FIG. 5B is a diagram showing in further detail a selected silica dust capture hose controlling silica dust generated by the discharge of frac sand from the outlet of a corresponding representative trailer conveyor to the lateral transfer conveyor section of FIG. 1 ;
FIG. 5C is a diagram showing the hoses controlling silica dust generated during the movement of sand by the upwardly angled conveyor section of FIG. 1 to a point above the bin of the blender of FIG. 1 , along with the silica dust capture hose controlling silica dust generated during the discharge of sand into the blender bin from the conveyor section spout;
FIG. 6A is a diagram showing in further detail the pneumatic connections of the silica dust control conduit subsystem of a representative one of the trailers of FIG. 1 ;
FIG. 6B is a diagram showing in further detail one of the T-fittings interconnecting the air conduits of the silica dust control conduit subsystem shown in FIG. 6A ;
FIG. 6C is a diagram showing a one of the end fittings terminating the air conduits of the silica dust control conduit subsystem shown in FIG. 6A ;
FIG. 6D is a diagram showing the four-way fitting interconnecting the air conduits of the silica dust control subsystem of one particular trailer with the silica dust control unit, as shown in FIG. 4B ;
FIG. 7A is a diagram showing an alternate embodiment of the principles of the present invention in which a cover is provided over portions of the representative frac sand transportation and unloading system of FIG. 1 for containing silica dust generated during movement of sand through the system;
FIG. 7B is a conceptual diagram providing a first detailed view of a representative embodiment of the cover shown in FIG. 7A ; and
FIG. 7C is a conceptual diagram providing a second detailed view of the representative embodiment of the cover shown in FIG. 7A .
DETAILED DESCRIPTION OF THE INVENTION
The principles of the present invention and their advantages are best understood by referring to the illustrated embodiment depicted in FIGS. 1-7 of the drawings, in which like numbers designate like parts.
FIG. 1 is a diagram of an exemplary frac sand transportation, storage, and unloading system 100 including a frac sand silica dust control system according to a preferred embodiment of the principles of the present invention. System 100 is also shown in the plan views of FIGS. 2 and 3 , with FIG. 2 emphasizing the air flow paths of the silica dust control system and FIG. 3 generally showing the locations of particular features of the silica dust control system shown in further detail in FIGS. 4-6 .
Generally, system 100 is assembled at a hydraulic fracturing worksite and is used to offload frac sand transported to the worksite from a frac sand supplier via trailers and offloaded into a blender. The blender mixes the sand with the water and chemicals to form the fracing fluid. Given the significantly large amounts of frac sand that are typically required during typical hydraulic fracturing operations, a substantial amount of potentially hazardous silica dust is commonly generated during conventional trailer offloading operations. The principles of the present invention advantageously provide for the control of frac sand produced silica dust, which consequently improves personnel safety, helps reduce the need for respirators and other burdensome safety equipment, and allows personnel to work longer and more efficiently at the worksite.
In the illustrated embodiment of system 100 shown in FIGS. 1 , 2 , and 3 , four (4) conventional sand storage trailers 101 a - 101 d are shown at a fracing worksite. While four (4) trailers 101 are shown as an example, the actual number of sand storage trailers 101 utilized in any particular embodiment or configuration of system 100 may vary based on the needs and restrictions at the worksite. The size and configuration of system 100 in any given worksite application will depend on such factors as the amount of sand that must be offloaded, the speed at which sand must be offloaded, and the size and capabilities of the offloading conveyor system. In the illustrated embodiment of system 100 , each trailer 101 includes a retractable trailer discharge conveyor (transfer belt) 102 a - 102 d , which receives sand from the compartments of the trailer internal tank via a lateral transfer belt running underneath the trailer tank (not shown). Trailers 101 are, for example, Sand King 3000/4000 frac sand trailers from Convey-All Industries, Inc., although there are a number of other commercially available sand storage trailers known in the art. It should also be recognized that the principles of the present invention are also applicable to embodiments of system 100 in which sand is stored and discharged from other types of fixed and transportable storage systems, such as tanks, silos, compartmented vehicles, and so on.
Each trailer discharge conveyor 102 a - 102 d discharges sand to a conventional transportable conveyor system, for example, Unibelt conveyor system from Convey-All Industries, Inc., which includes a continuous transfer belt running through a lateral conveyor section 103 and a upwardly angled discharge conveyor section 105 . During typical offloading operations, one or more randomly selected trailers 101 discharge sand to the lateral conveyor section 103 at a given time.
Sand being discharged by each trailer discharge conveyor 102 a - 102 d falls through slots 104 and onto lateral conveyor section 103 . Lateral conveyor section 103 then carries the sand to upwardly angled discharge conveyor section 105 , which discharges the sand to a bin of a blender truck 119 ( FIGS. 3 and 5C ), which mixes the sand with water and chemicals in quantities needed for the formulation of the particular fracing fluid being used.
The amount of sand being transferred at any one time in system 100 can be substantial. For example, a Convey-All Unibelt conveyor can nominally transfer and discharge 22,000 pounds per minute of sand from trailers 101 a - 101 d . The generation of a corresponding substantial amount of fine silica dust is a natural consequence of this transfer and discharge process.
According to the principles of the present invention, silica dust generated during the offloading of trailers 101 a - 101 d is collected by suction at selected points around system 100 most susceptible to the generation and discharge of silica dust. In the preferred embodiment, silica dust is collected: (1) within the compartments of the tanks of trailers 101 a - 101 d ; (2) at the base of each trailer discharge conveyor 102 a - 102 d , near the point at which sand is received from the trailer lateral conveyor and the trailer tanks; (3) at the point sand is discharged from trailer discharge conveyors 102 a - 102 d through slots 104 and onto lateral conveyor section 103 ; (4) at multiple points along upwardly-angled discharge conveyor section 105 ; and (5) near the point sand is discharged from the spout of discharge conveyor 105 in to the bin of blender 119 . It should be noted that in alternate embodiments, silica dust may be collected at additional points, or even fewer points, within system 100 , as required.
The silica dust control function of system 100 is driven by a silica dust control unit 106 , which draws silica dust-bearing air collected at points across the system though a pair of large manifolds 107 and 108 . In the illustrated embodiment of system 100 , silica dust control unit 106 also draws silica dust-bearing air directly from trailer 101 d through flexible hosing 109 , although this is not a strict requirement of the principles of the present invention. Silica dust control unit 106 , which may include a baghouse and/or cyclone, separates the silica dust from the air and discharges substantially silica dust-free air into the surrounding environment. One exemplary silica dust control unit, suitable for use as silica dust control unit 106 of system 100 , is an ETI Cyclone 20 DC system, available from Entech Industries, which includes multiple twenty-inch (20″) inlets and produces a nominal airflow of 20000 cubic feet per minute (cfm).
Silica dust control unit 106 establishes airflow in the direction shown by arrows in FIG. 2 . In the preferred embodiment, two intake ports of silica dust control unit 106 are pneumatically connected with manifolds 107 and 108 , which run along corresponding sides of lateral conveyor section 103 , and one intake port of silica dust control unit 106 is directly pneumatically connected to trailer 101 d through flexible hosing 109 .
Silica dust generated in each of the compartments of trailers 101 a - 101 d is collected through a corresponding set of fittings 110 a - 110 f and hoses 111 a - 111 e . In the illustrated embodiment of system 100 , the compartments of trailers 101 a - 101 c are pneumatically coupled to manifold 107 through flexible hosing 113 a - 113 c . For trailer 101 d , one fitting 110 is replaced with a four-way fitting 112 , which directly pneumatically couples the compartments of trailer 101 d with silica dust control unit 106 .
Flexible hoses 114 a - 114 c , which tap manifold 107 , and the flexible hose 114 d , which taps manifold 108 , collect silica dust at the bases of each trailer discharge conveyor 102 a - 102 d . Flexible hoses 115 a - 115 d , which tap manifold 108 , collect silica dust at the discharge points of trailer discharge conveyor 102 a - 102 d into slots 104 a - 104 c of lateral conveyor section 103 . Flexible hoses 116 a - 116 d , which tap manifold 108 , collect silica dust moving up upwardly angled discharge conveyor section 105 . It should be noted that the pneumatic paths between silica dust collection hoses 113 , 114 , 115 , and 116 and silica dust control unit 106 may vary between embodiments of system 100 . In the preferred embodiment of system 100 shown in FIG. 1 , the tapping point, as well as the manifold 107 or 108 being tapped, minimizes the lengths of manifolds 107 and 108 and silica dust collection hoses 113 , 114 , 115 , and 116 . Generally, so long as sufficient suction is available at a given silica dust collection point, the manifold 107 or 108 tapped, the point on the manifold 107 or 108 tapped the corresponding flexible hose, or both, may be varied.
A flexible hose 117 , which taps manifold 107 , captures silica dust generated by the discharge of sand from upwardly angled discharge conveyor 105 into the bin of blender 119 . (While flexible hose 117 taps manifold 107 , in alternate embodiments flexible hose 117 may tap manifold 108 ).
Manifolds 107 and 108 include a number of straight sections 120 and bent or curved sections 121 and are preferably constructed as tubes or pipes of rigid metal, such as aluminum. Rigid metal embodiments provide durability, particularly when manifolds 107 and 108 sit on or close to the ground and/or are exposed to contact by personnel or to other structures within system 100 . However, in alternate embodiments, manifolds 107 and 108 may be constructed, either in whole or in part, from sections of semi-rigid conduit or flexible (corrugated) hose. For example, semi-rigid conduit or flexible hose may be used in sections 121 of manifolds 107 and 108 that must be bent to provide a path around, over, or under, other structures in system 100 .
Preferably, manifolds 107 and 108 are each constructed in multiple straight sections 120 and multiple bent or curved sections 121 , which are clamped together using conventional clamps. This preferred construction allows manifolds 107 and 108 to be efficiently assembled and disassembled at the worksite, allows the most direct paths to be taken to silica dust control unit 106 , and allows the overall system of conduits to be adapted to different configurations of system 100 (e.g., different types and number of trailers 101 , different transportable conveyor systems, different surface conditions).
Additionally, the diameters of the various sections of manifolds 107 and 108 may increase or decrease, depending on the airflow provided by the given silica dust control unit 106 . The diameters of manifolds 107 and 108 are determined by a number of factors, including the intake diameters of silica dust control unit 106 , the airflow produced by silica dust control unit 106 , and the amount of suction needed at the silica dust collection points. Similarly, the diameters of silica dust collection hoses 113 , 114 , 115 , and 116 will depend on factors such as the airflow available from silica dust control unit 106 , the diameters of manifolds 107 and 108 , and the amount of suction required at a given hose inlet. In one typical embodiment of system 100 , manifolds 107 and 108 have a nominal diameter of twenty inches (20″) and silica dust collection hoses 113 , 114 , 115 , and 116 are nominally within the range of six to sixteen inches (6″-16″) in diameter. In other words, the principals of the present invention advantageously allow for variations in the components and configuration of system 100 .
It should be recognized that the transportable conveyor system, including lateral conveyor section 103 and discharge conveyor section 105 , is not always required. In this case, one or more trailer discharge conveyors 102 discharge sand directly from the corresponding trailers 101 into the bin of blender 119 . In embodiments of system 100 that do not utilize the transportable conveyor system, only a corresponding number of flexible hoses 114 and 115 are required for collecting silica dust at the base and outlet of each trailer discharge conveyor 102 discharging to blender 119 . (Along with the desired connections for removing dust within the trailers 101 themselves.) Advantageously, only single manifold 107 or 108 may be required in these embodiments.
FIG. 4A is a more detailed diagram showing the pneumatic connections between manifolds 107 and 108 and silica dust control unit 106 . FIG. 4B shows the direct pneumatic connection between trailer 101 d and silica dust control unit 106 through flexible hose 109 in further detail.
FIGS. 4C-4E illustrate representative tapping points between the heavier rigid sections 120 of manifolds 107 and 108 and selected flexible hoses utilized in system 100 . In particular, FIG. 4C shows a representative pneumatic connection between manifold 107 and hose 113 c collecting silica dust from the tank compartments of trailer 101 c . FIG. 4D shows representative pneumatic connections between manifold 108 and hose 114 d , which collects silica dust generated at the base of trailer discharge conveyor 102 d , and hoses 115 c and 115 d , which collect silica dust generated at corresponding outlets of trailer discharge conveyors 102 c and 102 d . FIG. 4E shows representative pneumatic connections between manifold 108 and hoses 116 a - 116 d collecting silica dust generated by discharge conveyor section 105 .
As well known in the art, numerous techniques are commonly utilized for connecting flexible hose with a rigid conduit or pipe, many of which are suitable for use in system 100 . In the illustrated embodiment shown in FIGS. 4C-4D , an aperture is tapped through the wall of the given manifold 107 or 108 and the lower periphery of a fitting (e.g., aluminum or steel pipe) 401 is attached, for example, by welding or brazing. The lower section of a coupling 402 is attached to the upper periphery of fitting 401 , for example by welding or brazing. The tubular upper section 403 of coupling 402 is received with the periphery of the corresponding hose, which is then clamped in place by one or more conventional clamps 404 . When necessary, an extension or elbow (not shown) may be provided between upper section 403 of coupling 402 and the corresponding hose. Similarly, a reduction coupling (see FIG. 5A , designator 501 ) may be provided between upper section 403 and coupling 402 , as required to transition to the selected hose diameter.
In the preferred embodiment shown in FIGS. 4C-4E , each coupling 402 includes a slide gate, which provides for air flow control between the given silica dust capture hose 113 , 114 , 115 , and 116 and the corresponding manifold 107 or 108 . In addition to allowing control of the amount of suction produced at the capture hose inlet, these slide gates also allow any unused taps to manifolds 107 and 108 to be completely shut off, particularly when a hose is not connected to coupling 402 .
FIG. 5A depicts in further detail representative silica dust collection hose 114 b collecting silica dust generated at the base of trailer discharge conveyor 102 b . Hose 114 b pneumatically couples with manifold 107 through a reduction coupling 501 . The inlet end of hose 114 b , which includes an optional nozzle or shroud 502 , is disposed proximate the point where the lateral conveyor of trailer 101 b discharges sand to the base of trailer discharge conveyor 102 b . Silica dust generated during sand transfer is captured by the suction created by silica dust control unit 106 at the discharge end of hose 114 b and carried through manifold 107 to silica dust control unit 106 to be filtered from the air. Silica dust collection hoses 114 a , 114 b , 114 c , and 114 d , which respectively collect silica dust generated at the bases of trailer discharge conveyors 102 a , 102 b , 102 c and 102 d , are similar in configuration and operation.
FIG. 5B depicts in further detail representative silica dust collection hose 115 b collecting silica dust generated during the discharge of sand from trailer discharge conveyor 102 b into lateral conveyor section 103 . In the illustrated embodiment, trailer discharge conveyor 102 b discharges through a section of flexible hose (conduit) 503 into the corresponding slot 104 of lateral conveyor section 103 . The inlet 504 of silica dust collection hose 115 b is disposed proximate the outlet of flexible hose 503 . The suction produced by silica dust control unit 106 gathers silica dust generated during the transfer of sand, which in turns moves to silica dust control unit 106 for filtering through manifold 108 . The configuration and operation of silica dust collection hoses 115 a , 115 b , 115 c , and 115 d , which respectively collect silica dust from the discharge points of trailer conveyors 102 a , 102 b , 102 c , and 102 d into lateral conveyor section 103 are similar.
Silica dust collection hoses 116 a - 116 d , and the suction generated by silica dust control unit 106 , collect silica dust generated by the lifting and discharge of sand by discharge conveyor section 105 . As shown in FIG. 5C , silica dust collection hoses 116 a - 116 d extend from apertures through the body of discharge conveyor section 105 at selected spaced-apart points. During operation, silica dust generated as sand moves upwards towards the outlet spout is removed through silica dust collection hoses 116 a - 116 d and manifold 108 for filtering by silica dust control unit 106 .
FIG. 5C also one possible configuration for flexible 117 with respect to the spout of upwardly angled conveyor 105 . Generally, the intake end of flexible hose 117 is located near the discharge point of the spout of conveyor 105 and creates an updraft, which captures silica dust generated as sand falls into the bin of blender 119 . The actual attachment point of flexible hose 117 to the spout of conveyor 105 , as well as the proximity of the intake end of hose 117 to the blender bin, may vary in actual practice of system 100 .
As discussed above, silica dust generated in the compartments of the tanks of trailers 101 a - 101 d is collected by a set of fittings 110 and hoses 111 . FIGS. 6A-6C depict this subsystem in further detail, using trailer 101 a as an example.
Each trailer 101 includes a set of inspection hatches 601 through the trailer roof. In the illustrated embodiment, trailers 101 include two rows of hatches 601 that run along opposing sides of the trailer roof. (In other embodiments of trailers 101 , the number and location of inspection hatches 601 may differ. For example, some commercially available sand storage trailers utilize a single row of inspection hatches that run along the centerline of the trailer roof.)
In addition, FIG. 6A shows optional skirts 610 , which run along each side of the depicted trailer 101 . Skirts 610 , which are preferably constructed from a durable flexible material, such as heavy plastic or canvas, contain silica dust generated by the movement of sand through the lateral conveyor that runs underneath the trailer tank.
In the preferred embodiment of system 100 , silica dust collection is performed using the hatches 601 running along one side of the trailer tank, although in alternate embodiments silica dust collection could be performed using the hatches running down both sides of the trailer tank. For a given compartment, the regular hatch 602 is pulled back and replaced with corresponding cover 603 attached an associated fitting 110 ( FIGS. 6B-6D ).
FIG. 6B shows in further detail an example of a T-shaped (three-way) fitting 110 e interfacing with corresponding hoses 111 d and 111 e . FIG. 6C shows an example of a elbow (two-way) fitting 110 a and the final section of hose 111 a in the trailer silica dust subsystem. The remaining connections between the given trailer 101 and fittings 110 and 111 are similar. The four-way fitting 112 used to connect trailer 101 d and silica dust control unit 106 through hose 109 is shown in detail in FIG. 6D . In each case, fittings 110 include well-known transitions and clamps to connect to hoses 111 . Similar to the taps shown in FIGS. 4C-4E , each fitting, such as T-shaped (three-way) fitting 110 e , elbow fitting 110 a , and four-way fitting 112 , includes a slide gate for controlling airflow between the space within the given trailer 101 and manifold 107 .
FIGS. 7A-7C illustrate an enhancement to system 100 , which includes a flexible cover system 700 for containing the silica dust generated during the movement of sand through the system. Preferably, flexible cover system 700 extends over the discharge ends of trailer discharge conveyors 102 a - 102 d , the length of lateral conveyor section 103 , and the length of upwardly angled discharge conveyor section 105 . (In alternate embodiments, flexible cover system 700 may only cover portions of system 100 , as necessary to effectively control silica dust.)
In the preferred embodiment, flexible cover system 700 is constructed as separate sections 701 a - 701 c and 702 , as shown in FIGS. 7B and 7C . Sections 701 a - 701 c cover corresponding portions of lateral conveyor section 103 and section 702 covers upwardly angled discharge conveyor section 105 . Boots 703 are provided to allow insertion of corresponding flexible capture hoses 115 and 116 into the underlying silica dust containment spaces when cover system 700 is deployed. Boots 704 extend over the ends of trailer discharge conveyors 102 a - 102 d.
Section 702 also includes a lateral extension 705 for covering the spout of upwardly angled discharge conveyor section 105 . A boot 707 provides for the insertion of flexible hose 117 into extension 702 for fastening on or near the outlet of the discharge spout of conveyor 105 .
Flexible cover system 700 is preferably constructed of canvas, heavy plastic, or other flexible material that is durable, relatively easy to deploy and remove, and transportable. Preferably, the surfaces of the selected material are impervious to frac sand, as well as able to withstand the normal wear and tear expected at a fracing worksite. When deployed, sections 701 and 702 are attached to each other with areas of Velcro 706 or similar attachment system, which minimizes the escape of silica dust at the seams between the sections.
In sum, the principles of the present invention provide for the efficient capture and removal of silica dust generated during the offloading of frac sand at a worksite. Silica dust removal is performed near, but not limited to, substantial sources of hazardous silica dust, including at trailer to trailer conveyor sand transfer point, each point of transfer from the trailer discharge conveyors and the lateral site conveyor, and points along the lifting/discharge conveyor. The embodiments of the inventive principles are scalable, and can be applied to any discharging system serving single or multiple frac sand storage trailers and can be implemented with various commercially available cyclone/baghouse silica dust removal systems. Moreover, the configuration and construction of these embodiments are also variable, allowing silica dust control to be effectively implemented under widely varying worksite conditions.
Although the invention has been described with reference to specific embodiments, these descriptions are not meant to be construed in a limiting sense. Various modifications of the disclosed embodiments, as well as alternative embodiments of the invention, will become apparent to persons skilled in the art upon reference to the description of the invention. It should be appreciated by those skilled in the art that the conception and the specific embodiment disclosed might 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.
It is therefore contemplated that the claims will cover any such modifications or embodiments that fall within the true scope of the invention.
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A system for controlling silica dust generated during the transfer of frac sand from a storage container through a conveyor system includes a system of conduits having a plurality of inlets for collecting silica dust generated at selected points along the conveyor system. An air system pneumatically coupled to the system of conduits generates a negative pressure at each of the inlets to induce the collection of silica dust at the selected points along the conveyor.
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RELATED APPLICATION
[0001] This application claims priority from U.S. Provisional Patent Application No. 60/671,793, entitled “A POYNTING-VECTOR BASED METHOD FOR DETERMINING THE BEARING AND LOCATION OF ELECTROMAGNETIC SOURCES,” filed on Apr. 15, 2005, and is incorporated by reference in its entirety.
[0002] The United States Government has rights in this invention pursuant to Contract No. W-7405-ENG48 between the United States Department of Energy and the University of California for the operation of Lawrence Livermore National Laboratory.
BACKGROUND OF THE INVENTION
[0003] 1. Field of the Invention
[0004] The present invention relates to the detection of radiating electromagnetic waves, and more particularly, the present invention relates to the detection and location of radiating sources, often low-frequency radiating electromagnetic sources operating within the near-field, using Poynting vector E and B field measurements.
[0005] 2. Description of Related Art
[0006] Near-field radiation (NF) includes electric and magnetic fields that have a more static character (quasi-static) and are localized “near” the surface of objects, while far-field radiation (FF) also known as “normal radiation”, generally refers to propagating radiation. In general, all radiating objects have both NF and FF components; however, most conventional detection methods of radiating sources generally avail themselves to propagative components in the FF. A source of radiation generally has three components: the tangential electric field, E t , the radial electric field, E r and the tangential magnetic field, H t . The Poynting Theorem itself generally states that for any superimposed electric and magnetic fields, there must be energy flowing in the medium. Thus, the accepted theory for radiating fields can be derived from an electric field E and a magnetic field H in a cross-product Poynting vector E×H=S (watts per meter squared).
[0007] All electric power systems that involve electricity generation, transmission and loads are subject to transmission loss. One form of loss that is virtually impossible to eliminate is the radiated field loss (NF & FF) that comes with changing loads or loads that respond to applied voltage in a nonlinear fashion in a power generation and utilization system. This is energy loss due to the non-ideal flow of electrical currents resulting in a radiated electromagnetic field that is highly dependent on the specifics of the generator and loads and the result of an imbalanced system. An isolated and remote power source such as a generator will always produce an electromagnetic field that can be detected at some stand-off range. The range, however, will be strongly dependent on the power utilization purpose and the specific layout of the generator and loads.
[0008] Accordingly, a need exists for novel methods and instrumentation to locate radiating sources, often low-frequency radiating sources within the near-field based on Poynting vector E and B field measurements. The present invention is directed to such a need.
SUMMARY OF THE INVENTION
[0009] Accordingly, the present invention is directed to a method of sensing one or more radiating electrical sources so as to produce one or more data formats characteristic of said sources; and calculating one or more Poynting vectors resulting from the data formats so as to produce a bearing, a distribution of harmonics, a spatial mapping of the sources and/or a temporal assessment.
[0010] Another aspect of the present invention provides a method of locating one or more radiating electrical sources that includes sensing along three orthogonal axes to determine electric- and magnetic-field components, one or more broadband signals and quasi-static field signals; transforming to thereby convert the sensed signals to the frequency domain for each electric field axial component (E) and magnetic field axial component (B); filtering the transformed signals to enable selection of characteristic one or more predetermined harmonics of the one or more broadband signals; and calculating one or more Poynting vectors resulting from the filtered one or more predetermined harmonics generated at the same point in time so as to provide a bearing of one or more radiating sources.
[0011] Another aspect of the present invention provides an apparatus for detecting and locating one or more radiating electrical sources having electric (E) and magnetic (B) field components so as to provide a bearing, a spatial mapping and/or a temporal assessment of such sources.
[0012] A final aspect of the present invention provides a network of sensors for detecting and locating one or more radiating electrical sources having electric (E) and magnetic (B) field components so as to provide a bearing, a spatial mapping and/or a temporal assessment of such sources.
[0013] Accordingly, the present invention provides a method and apparatus suitable for the detection and source location of stationary radiating electric (E) and magnetic (B) fields emitted by, for example, A.C. generators, transmitters, electrical conductors and loads. Such techniques and devices, as disclosed herein, also enables spatial mapping of fields and remote source characterization and temporal assessment of electrical usage for stationary objects as well as for tracking movement of any radiating mobile source/load systems for which a cross-product Poynting vector may be determined as might be associated with, but not limited to cars, trucks, tanks, boats, submarines, airplanes, and space vehicles.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The accompanying drawings, which are incorporated into and constitute a part of the specification, illustrate specific embodiments of the invention and, together with the general description of the invention given above, and the detailed description of the specific embodiments, serve to explain the principles of the invention.
[0015] FIG. 1 ( a ) shows a simplified diagram of a Poynting vector system in the field.
[0016] FIG. 1 ( b ) shows an example hand held device of the present invention.
[0017] FIG. 2 shows experimental digitized frequency spectra of Electric (E) and Magnetic (B) field channels.
DETAILED DESCRIPTION OF THE INVENTION
[0018] Referring now to the drawings, specific embodiments of the invention are shown. The detailed description of the specific embodiments, together with the general description of the invention, serves to explain the principles of the invention.
[0019] Unless otherwise indicated, numbers expressing quantities of ingredients, constituents, reaction conditions and so forth used in the specification and claims are to be understood as being modified by the term “about.” Accordingly, unless indicated to the contrary, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained by the subject matter presented herein. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques. Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the subject matter presented herein are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contain certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
[0000] General Description
[0020] The apparatus and methods, as disclosed herein, explores stand-off detection and location of radiating electrical sources, such as, a generator source powering realistic loads in the field, through Poynting vector E and B field measurements. Detection of signals by the present invention at common radiating source frequencies of, for example, 60 Hz (and higher harmonics) are well within the complex electromagnetic near-field region for stand-off ranges of less than about 1000 km. The present invention beneficially provides digitized (e.g., up to about 100,000 data points per second) time averaged detection and filtering of such E-field and B-field information to remove unwanted near-field quasi static fields (i.e. noise stream data) to enhance the signal-to-noise ratios of the desired received signals. The resultant high sensitivity three-axis E-field measurements, along with corresponding B-field measurements, as disclosed herein, enables calculation of a back-azimuth (i.e., a bearing with one or more measurements) as well as provide the distribution of electrical harmonics to a source. Such a method and corresponding system/apparatus thus enables determination of the location of a source within the near-field regime and source location capability at low frequency based on Poynting vector E and B field measurements.
[0000] Specific Description
[0021] Turning now to the drawings, a basic diagram that illustrates an exemplary basic embodiment of a system constructed in accordance with the present invention is shown in FIG. 1 ( a ). Such a system, designated generally by the reference numeral 10 , can be configured as a portable unit or extended to networks of sensors allowing determination of the bearing and location of both stationary and moving sources within a stand-off range of less than about 1000 meters.
[0022] System 10 , can be directed by a user via a computer 16 having a control software program that can include a graphical user interface (GUI) configured from Visual Basic, MATLAB®, LabVIEW®, Visual C++, or any programmable language or specialized software programming environment to enable ease of operation when directing commands and acquiring desired information. LabVIEW® and/or MATLAB® in particular, is specifically tailored to the development of instrument control applications and facilitates rapid user interface creation and is particularly beneficial as an application to be utilized as a specialized software embodiment that can be automated when desired so as to provide a bearing and/or a spatial location of one or more radiating electrical sources/load systems, as well as provide the distribution of electrical harmonics, temporal assessment and/or spatial mapping of produced fields of one or more stationary or moving radiating sources.
[0023] Computer 16 can be configured with analog to digital (A/D) integrated circuit capabilities as known by those of ordinary skill in the art and also constructed with means, such as, software, available firmware (ROM's, EPROM's) and integrated computational, storage, etc., circuit means, such as, but not limited to, large scale Integrated Circuits LSIC (LSIC), very large scale Integrated Circuits (VLSIC), and field-programmable gate arrays (FPGA's). Such software means, firmware means, and other integrated circuit means can provide the filtering, storage and computational manipulations that is desired for the present application. The FPGA array, in particular, is a beneficial semiconductor device to be utilized in the present invention as such devices contain programmable logic components and programmable interconnects. The programmable logic components can be programmed, for utilization in the present invention, such as, for example, in system 10 as shown in FIG. 1 ( a ), or in remote hand-held applications, as shown in FIG. 1 ( b ) and as discussed in detail below, to duplicate the functionality of basic logic gates (such as AND, OR, XOR, NOT) or more complex combinatorial functions such as decoders or simple math functions. In most FPGAs, these programmable logic components (or logic blocks, in FPGA parlance) also include memory elements, which may be simple flip-flops or more complete blocks of memories.
[0024] Computer 16 , capable of being configured with such devices, is thus operably coupled to a sensor 4 (shown within a dashed box) or a network of such sensors (not shown), configured with triaxial B-field 8 and E-field 12 sensing units via wireless communication means and/or predetermined communication lines (denoted by the letter L and shown with double arrowed line) such as, USB or RS232 cables. Such wireless communication means and/or communication lines L are constructed and arranged to allow for the exchange of information between computer 16 and each sensor 4 outputting a stream of triaxial (i.e., X-Y-Z electrical (E) and magnetic (B)), A/D recorded data to effect operation of system 10 and to transfer acquired digitized information to computer 16 for storage, post-processing, and/or immediate analysis.
[0025] The B-field 8 and E-field 12 sensing units, as shown above in FIG. 1 ( a ), thus senses desired radiation source signals and unwanted quasi-static (noise stream) signals and converts such sensed signals to a digital form using an electronic A/D converting circuit 6 means that can digitize up to about 100,000 bits per second of received information. The B-field 8 and E-field 12 sensing units can be specially designed units or commercially configured triaxial units, often configured with deployable antenna elements, an associated preamplifier to add gain to the output signals from the antennas. The B-field units, in particular, as utilized herein, often can include three orthogonal (i.e., perpendicular) metallic alloy cores with predetermined sets of windings designed to produce flux in the core and predetermined sets of windings to detect the flux. After B-field 8 and E-field 12 sensing units receives analog radiating signals 3 as shown in FIG. 1 ( a ), at for example, 1 Hz or greater, such received signals are converted to a digital format by integrated circuit means well known by those of ordinary skill and the vector components of the recorded E and B fields (e.g., up to six channels corresponding to the three-axis measurements of the E and B fields) are each analyzed by a respective provided means (e.g., software, firmware, LSIC, VLSIC, FPGA's) residing in computer 16 .
[0026] Thereafter, the Poynting vector S 22 , as shown in FIG. 1 ( a ), is determined, often by time averaging (e.g., of at least one period) such signals, to provide a stable Poynting vector S 22 signal in addition to removing the noise signals. Such a manipulation can thus provide a bearing and/or a spatial location of a radiating electrical source/load system(s), a temporal assessment of the electrical usage of such system(s), spatial mapping of produced fields, as well as the distribution of electrical harmonics.
[0027] As another beneficial arrangement, the sensor 4 , as shown in FIG. 1 ( a ), and designated generally by the reference numeral 10 ′, can be configured as a hand-held sensor 24 (as shown within a dashed box in FIG. 1 ( b )), for ease of operation and movement in a variety of harsh or otherwise environments. Such a hand-held sensor 24 can include computational and operational specialized software means, often with a graphical user interface (GUI), as discussed above, configured from Visual Basic, MATLAB®, LabVIEW®, Visual C++, or any programmable language or specialized software programming environment to enable ease of operation when directing commands and acquiring desired information. The graphical user interface, in addition to a host of other configured operations, can be arranged to display a spectrum of triaxial frequencies 28 , of one or more selected frequencies and/or harmonics 30 for filtering or monitoring so as to provide a resultant bearing 30 and/or a spatial location upon application of the Poynting vector calculations 34 by various integrated, software, or firmware means, as discussed above.
[0028] Moreover, in an additional arrangement, sensor 24 , as shown in FIG. 1 ( b ), may include commercial wireless interfaces (not shown), such as, but not limited to, infrared and/or microwave technologies, to enable communication and integration into a wireless network system (not shown) for triangulating a location of one or more predetermined sources or for downloading information to a central processor (not shown) for post processing and/or immediate analysis. The wireless technology itself may include any of the communication methods and hardware presently available, such as, but not limited to, ultra-wideband methods (UWB), International Electronic and Electrical Engineers (IEEE) protocols, or Bluetooth, a registered trademark of Bluetooth SIG, INC., Corporation by Assignment, Delaware, located in Washington D.C., or any of the new IEEE protocols for wireless communication over, as one example arrangement, a network system, such as an ad hoc system network (e.g., a system wherein one or more sensors relay messages through other sensor apparatus in order to communicate with, for example, a central processing unit or one or more other sensor apparatus that is out of range). Such example sensor arrangements can also provide a bearing and/or a spatial location of one or more radiating electrical sources/load systems as well as provide the spatial mapping of fields, and a distribution of electrical harmonics of radiating sources, as disclosed herein.
[0029] Similar to the arrangement, as shown in FIG. 1 ( a ), sensor 24 , as shown in FIG. 1 ( b ), also includes an analog to digital (A/D) converter 36 , capable of digitizing up to about 100,000 bits per second, for conversion to a digital format upon sensing alternating radiating fields from B-field 8 and E-field 12 sensing units. The E-field sensing units 12 and the B-field sensing units 8 can be the commercially configured triaxial units, as discussed above, for the system in FIG. 1 ( a ). Also, as discussed above, sensor 24 can be configured with a preamplifier (not shown) to add gain to the output signals from the antennas and deployment mechanism drive electronics. After B-field 8 and E-field 12 sensing units receives analog radiating signals 3 at 1 Hz or greater, such received signals are converted to a digital format and the vector components of the recorded E and B fields (e.g., up to six channels corresponding to the three-axis measurements of the E and B fields) are each capable of being analyzed by a respective computational means, such as, firmware, software, LSIC, VLSI, and FGPA as discussed above, and displayed 28 by the graphical user interface capable of being configured in sensor 24 . Thereafter, desired filtering of predetermined harmonics (e.g., 50 Hz and exceeding the 31 st harmonic of 50 Hz) can be time averaged by such computational means (e.g., averaged over at least one period) to remove the noise and analyzed to determine the Poynting vector S 34 , as shown in FIG. 1 ( b ), so as to provide, for example, a displayed bearing 32 of one or more electromagnetic radiating sources 2 .
[0030] FIG. 2 shows experimental digitized Fast Fourier Transform (FFT) spectra of Electric (E) and Magnetic (B) field channels as generated by the present invention. To illustrate the capabilities of the present invention, example 56.7 Hz 40 and 60 Hz 44 peaks can be clearly observed in some of the spectra and are distinctly separated. The harmonics most apparent are associated with the generator, not harmonics of background 60 Hz. The spectra, top to bottom are the magnetic-field (B) triaxial components in the X-Y-Z plane, i.e., Bx 48 , By 52 , Bz 56 , and the electric-field (E) triaxial components in the X-Y-Z plane, i.e., Ex 60 , Ey 64 , Ez 66 . The fundamental and higher harmonics (e.g., see reference numeral 72 , which is the fifth harmonic of 56.7 Hz) can vary greatly in signal-to-noise between E and B field components.
[0031] In the method of the invention, the first stage involves signal sensing and converting the analog signal from the E- and B-field sensors to a digital format. Six channels are recorded corresponding to the three-axis measurements of both the electric and magnetic fields. The vector components of the E and B fields are necessary for determination of the Poynting vector, S.
[0032] The second stage involves analyzing the broadband digital data stream resulting from the first acquisition and analog-to digital conversion stage. From the second stage, two methods of analysis can be used to calculate required E- and B-field components from the signal and noise data stream.
[0033] The first method requires calculating the transform, often calculating the Fast Fourier Transform (FFT), of the broadband signal and noise data stream. The FFT gives the spectrum of signal and noise amplitude versus frequency. Using the FFT, harmonics of a signal of interest (e.g., 56.7 Hz 40 and higher harmonics ( 72 ), as shown in FIG. 2 , and exceeding the 31 st harmonic) can be selected, wherein information from each harmonic common to the E and B vector fields can be beneficially utilized to determine a Poynting vector. The calculation of such Poynting vectors can be used to increase the certainty of source location. In addition, the Poynting vector of each harmonic can be used as a characteristic to identify a set of harmonics associated with a common source. Narrow bandpass filters (e.g., Butterworth, Bessel, Chebyshev, combinations thereof or similar) can be constructed to filter the broadband signal and a quasi-static field (noise data stream) for the selected harmonics. Such filtering of the broadband signal and noise data stream of each component of B and E produces a digital wave train having a frequency characteristic of each harmonic. This is performed for the data stream associated with each B and E component (e.g., 52 , 56 , 60 , 64 , and 66 , as shown in FIG. 2 ).
[0034] Samples of the wave train amplitude corresponding to the same point in time are then taken from each of the six wave trains. These six amplitudes correspond to the instantaneous value of the E and B fields associated with a given harmonic and are used to calculate an instantaneous value of the Poynting vector, S. Because the Poynting vector is time dependent, averaging over at least one period is performed to obtain a stable quantity S.
[0035] B. The second analysis method takes the digitized broadband signal and noise stream, as discussed above, and calculates, for example, the FFT giving both phase and amplitude information. The amplitudes of selected harmonics along with phase information can be obtained from the FFT for each of the three components of E and B, as shown in FIG. 2 . This information can then be used to calculate an instantaneous value of the Poynting vector that can be averaged over time to yield the Poynting vector S. The time average of the oscillatory Poynting vector yields directional information such as the azimuthal angle between a reference direction and the direction of energy flux associated with a remote source.
[0036] The present invention can thus locate (i.e., provide a bearing and/or a spatial location of a radiating electrical source/load system) as well as provide the distribution of electrical harmonics of one or more radiating sources of 50 Hz or greater, such as, but not limited to, stationary radiating electric (E) and magnetic (B) fields sources (e.g., A.C. generators, transmitters, electrical conductors and loads), in addition to spatially mapping fields and remote source characterization and temporal assessment of electrical usage produced by stationary objects of up to about 1000 meters. Moreover, the present invention is configured to track the movement of any radiating mobile source/load systems for which a Poynting vector may be determined as might be associated with, but not limited to cars, trucks, tanks, boats, submarines, airplanes, and space vehicles.
[0037] Applicants are providing this description, which includes drawings and examples of specific embodiments, to give a broad representation of the invention. Various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this description and by practice of the invention. The scope of the invention is not intended to be limited to the particular forms disclosed and the invention covers all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the claims.
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A method and apparatus is utilized to determine the bearing and/or location of sources, such as, alternating current (A.C.) generators and loads, power lines, transformers and/or radio-frequency (RF) transmitters, emitting electromagnetic-wave energy for which a Poynting-Vector can be defined. When both a source and field sensors (electric and magnetic) are static, a bearing to the electromagnetic source can be obtained. If a single set of electric (E) and magnetic (B) sensors are in motion, multiple measurements permit location of the source. The method can be extended to networks of sensors allowing determination of the location of both stationary and moving sources. It is emphasized that this abstract is provided to comply with the rules requiring an abstract which will allow a searcher or other reader to quickly ascertain the subject matter of the technical disclosure. It is submitted with the understanding that it will not be used to interpret or limit the scope or the meaning of the claims.
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BACKGROUND OF THE INVENTION
[0001] This invention relates in general to board games and, in particular, to a game for toy vehicles such as cars and trucks and to a game board used to play the game.
[0002] Board games are well known. Some board games have provided intellectual stimulation, such as Scrabble® and Trivial Pursuit®, by supplying questions to answer or words to form from a given set of letters. The person who correctly answered the most questions or formed the most words in the shortest amount of time generally was declared the winner. Other board games, such as “Monopoly®”, which imitated real estate acquisition in Atlantic City, N.J., attempted to simulate real-life circumstances. Still other board games have attempted to simulate sporting events, including football, baseball, and basketball. Board games, regardless of whether they simulate real-life circumstances, provide intellectual stimulation, or simulate a sporting event, typically utilize a game board, game pieces, chance devices, such as dice or a shuffled deck of cards, and a means for recording a player's score.
[0003] Automobile racing, most notably the National Association for Stock Car Auto Racing (NASCAR) racing circuit, has seen a large increase in popularity in recent years. An increasing number of races per year, rising attendance and national broadcasts on radio and network television, have all contributed to the booming popularity of the sport. “Open-wheeled” racing, including Formula One (F-1), the Championship Auto Racing Teams (CART) and the Indy Racing League (IRL) racing circuits, also continues to be popular. As the popularity of auto racing has increased, numerous board games have emerged attempting to simulate the thrill and excitement of an automobile race. These games generally consist of a game board laid out in the shape of a racetrack, game pieces in the shape of racecars, a means for the players to move the game pieces around the racetrack, and a means for scorekeeping.
[0004] The U.S. Pat. No. 5,934,673 discloses an auto racing board game with a game board laid out in the shape of a racetrack and game pieces in the shape of automobiles. The game board is divided into lanes that simulate positions on a racetrack. Players advance around the track by drawing cards from a shuffled deck. The cards make provisions for actual racing conditions including good handling, contact with other racecars and, of course, racecar crashes.
[0005] The U.S. Pat. No. 6,095,522 discloses a stock car racing board game with a game board laid out in the shape of a “tri-oval” race track, which is also divided into lanes, and tokens that represent racecars. Players advance around the track by rolling dice. In addition, cards from a shuffled deck are utilized to simulate mechanical problems, and the lanes are divided into ‘drafting’ lanes, where the actual drafting technique of racecar drivers is simulated to allow cars trailing other cars to draw nearer to the leading cars.
[0006] While the above examples of prior art all relate to board games that simulate automobile racing, the above examples require a good deal of familiarity with the intricacies of automobile racing and associated mechanical failures and conditions of the racecars. In addition, the prior art does not teach a board game designed for simulating a race season. While the prior art could possibly be adapted to simulate a race season, the myriad of rules and specific mechanical problems provided for in the prior art are not conducive to producing quick games to simulate an entire racing season.
[0007] It is desirable, especially for children, to provide a board game that is easy to learn and understand. It is also desirable to provide a board game where an entire racing season may be simulated in a manner that is rapid and easy while keeping the individual races interesting to the players. It is desirable to provide a game with quick and exciting action that does not get mired in the minutiae of racing strategy or the various mechanical problems and failures that are possible in an actual racecar. It is also desirable, though, in order to appeal to those with more knowledge of automobile racing, to provide a board game that does present some degree of realism by simulating some of the more familiar features of an actual automobile race.
[0008] It is an object of the present invention, therefore, to provide an automobile racing board game that is exciting but also easy to learn and play, especially for children.
[0009] It is another object of the invention to provide an automobile racing board game that simulates a racing season, by allowing players to race a set of races in order for a winner to be determined after the last of the set of races.
[0010] It is still another object of the invention to provide a board game that simulates an automobile race that is quick and easy to play, yet also provides some details for those familiar with automobile racing.
[0011] It is yet another object of the invention to provide an automobile racing board game that may be utilized with toy vehicles already in possession of the players.
SUMMARY OF THE INVENTION
[0012] The present invention concerns a game for entertainment that uses toy vehicles on a racetrack. The racetrack is printed on a game board that can be folded and easily stored. The game includes the game board, a twenty-sided die, a twelve-sided die, a six-sided die, and markers (for identifying name and lap). The game optionally includes the toy race vehicles. Numerous variations of the game and game board can be contemplated.
[0013] The present invention allows players to enjoy the thrill and excitement of an automobile race and a racing season, but does not require detailed knowledge of actual racing strategy or mechanical failures of racecars. The present invention does, however, provide some of the particulars that are encountered in an actual automobile race. The racetrack printed on the foldable game board is preferably divided into at least three lanes. The racetrack contains both straight sections (“straightaways”) and curved sections (“curves”.) The racetrack lanes are further divided into spaces for the toy race vehicles and simulate an actual racetrack by providing additional spaces in the outermost lanes, thereby giving an advantage to those players situated in the inside lane.
[0014] In order to begin play, players twice roll all the dice in order to determine the pole, or starting point positions for their respective toy vehicles. The player with the highest roll total will become the pole leader; the players with next highest successive roll totals will take the next positions. Up to nine players may race in a single game. Three rows of three race vehicles are the preferred pole positions. The players continue the race by rolling the twelve-sided die until the race, preferably five laps of the racetrack, is completed.
[0015] After the pole positions are set, the players begin the game by rolling the twelve-sided die in their pole position order. A player may change lanes, but may not ‘leapfrog’ or drive through other players' vehicles. Pit stops are required, providing a degree of realism in the present invention. A player must make a pit stop twice during a five-lap race, and cannot drive two consecutive laps without making a pit stop.
[0016] The present invention also provides a degree of realism in that a player's race vehicle will crash if the player is driving too fast (rolls too high of a number) in any one of the crash zones, which are located on the turns of the race course. When a crash occurs, the crashed race vehicle preferably blocks two of the three lanes and the remaining race vehicles slow to one half of their speed, as determined by the roll of the twelve-sided die. This provides a further degree of realism, in that trailing vehicles may now draw nearer to the leading vehicles. No lane changes are permitted when maneuvering through the racetrack curves.
[0017] The present invention provides a further degree of realism, by allowing the last place car to ‘draft’ by rolling the six-sided die, as well as the twelve-sided die, when driving to simulate the extra speed gain possible when utilizing the drafting technique of professional race vehicle drivers. The last place vehicle is allowed the full amount of the draft roll in a crash situation, allowing the last place vehicle to quickly draw nearer the leading vehicles.
[0018] The present invention provides a means for determining the winner of the race by providing points for pole positions, winning laps, and finish positions. The present invention further provides a means for determining the winner of a racing season by summing up the points for the individual races. The present invention accomplishes this by providing uncomplicated rules that lead to quicker games. The present invention does not utilize cards to simulate mechanical failures, strategy decisions or the like, and is thus easier to learn and quicker to play, while still providing exciting action during play. The quicker games lead to enhanced enjoyment of the game by all players involved because the players realize that misfortune in one game can be regained by a better performance in the next game or later in the racing season.
[0019] The present invention may provide toy vehicles for game play, but optionally, players may utilize their own matchbox toys or similar size toy vehicles. Thus, the present invention does not require race vehicle game pieces and allows players to use their favorite toys to play the game. This provides an opportunity for a game to be more personal, with players' own vehicles racing against each other.
DESCRIPTION OF THE DRAWINGS
[0020] The above, as well as other advantages of the present invention, will become readily apparent to those skilled in the art from the following detailed description of a preferred embodiment when considered in the light of the accompanying drawings in which:
[0021] [0021]FIG. 1 is a top view of a first embodiment of a game board used for playing a race vehicle game according to this invention;
[0022] [0022]FIG. 2 is a top view of a second embodiment of a game board used for playing a race vehicle game according to this invention; and
[0023] [0023]FIG. 3 is a top view of a third embodiment of a game board used for playing a race vehicle game according to this invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0024] Referring now to FIG. 1, a game for entertainment is indicated generally at 10 in FIG. 1. The game simulates a vehicular race wherein miniature vehicles such as cars and trucks are used with the game board 10 . Specifically, the game board 10 is sized to accommodate a popular size ({fraction (1/64)} scale) of toy vehicles (not shown) sold under the trademark “Matchbox.” Other brands of {fraction (1/64)} scale toy vehicles can also be used with the game board 10 . Preferably, the other brands of toy vehicles will have a similar length and width as the Matchbox brand of toy vehicles. The toy vehicles may be provided with the game 10 or, alternatively, may be provided by the game's players (not shown.)
[0025] The game board 10 includes a racetrack 12 having a start/finish line 14 preferably marked by alternating black and white rectangles. The track 12 includes a straight section 16 , a first turn 18 , and second turn, 20 , a backstretch 22 , a third turn 24 , a fourth turn 26 , and a pit area 28 .
[0026] A series of rectangular spaces 30 are provided on the straight section 16 , the backstretch 22 , and the pit area 28 . Spaces 30 are also provided between the turns 18 and 20 and turns 24 and 26 . The turns 18 , 20 , 24 , and 26 include curved spaces 34 . A series of transition spaces 36 are provided at the beginning and finish of the pit area 28 .
[0027] Each of the rectangular spaces 30 is sized to fit one toy vehicle. For example, a preferred {fraction (1/64)} scale line of toy vehicles is accommodated by spaces 30 having approximately three inches in length and approximately two inches in width. Preferably, the game board 10 of FIG. 1 includes spaces 30 of approximately three inches in length and approximately two inches in width so that the overall dimensions of the game board 10 are approximately forty-four (44) inches in length and twenty-eight (28) inches in width. Preferably, the game board 10 is divided into two equal sections and folded along a mid-line of its length.
[0028] The spaces 30 are divided into at least three circumferential lanes 31 a, 31 b, and 31 c, so that a player can pass the other players during a game described below. For clarification, lane 31 a will be referred to as the inside lane, lane 31 b will be referred to as the middle lane, and lane 31 c will be referred to as the outside lane. In turns, 18 , 20 , 24 , and 26 , there is only one curved space 34 in the inside lane 31 a, while there are two curved spaces 34 in the middle lane 31 b, and three curved spaces 34 in the outside lane 31 c. This provides an advantage to those players in the inside lane 31 a, in that a player can use less spaces to complete one lap of racetrack 12 .
[0029] A game played with game board 10 is described below. The game is intended for play of two to nine players (not shown.) The game preferably includes the game board 10 , a twenty-sided die (not shown), a twelve-sided die (not shown), a six-sided die (not shown), and markers (not shown) for identifying name and lap for use with the game board 10 . The game optionally includes toy race vehicles (not shown.)
[0030] The game starts by the players twice rolling all three dice (not shown) to determine their respective qualifying, or starting, positions A through I. The roll totals may be recorded on a qualifying sheet (not shown.) The player with the highest roll total receives the first, or pole, position A. The player with the second highest roll total receives the second starting position B. The player with the third highest roll total receives the third starting position C, the player with the fourth highest roll total receives the fourth starting position D, and so on, until the player with the ninth highest roll total receives the ninth starting position I. Race vehicles (not shown) are then placed in their respective starting positions A through I. Although only nine players may compete in a given race, up to twelve players may attempt to qualify for a race.
[0031] After the pole positions A through I are set, the players begin the game by rolling the twelve-sided die in their pole position order and move the toy vehicles in a counterclockwise direction around the racetrack 12 . The toy vehicles are moved the number of spaces 30 equal to the roll of the die. The players continue the game by rolling the twelve-sided die until all players finish the race, preferably five laps of the racetrack 12 . A player completes a lap when the player has completely crossed the start/finish line 14 , but not counting the first time the player crosses the start/finish line 14 at the beginning of the race. Players may move into adjacent spaces 30 only and may not move backwards, or in a clockwise direction around the racetrack 12 . A player may change lanes 31 a to 31 b, to 31 c, but may not ‘leapfrog’ other players' vehicles. No lane changes, however, are permitted when the player is located in any of the spaces 34 in curves 18 , 20 , 22 , and 24 . Stopping in the pit area 28 , referred to as making a “pit stop”, is required. A player must make a pit stop twice during a five-lap race, and cannot drive two consecutive laps without making a pit stop. The pit area 28 has numbers that preferably correspond to the player's starting position. A player must stop in the appropriate space in the pit area 28 before continuing out to the racetrack 12 via the transition spaces 36 .
[0032] A player's toy vehicle will crash if the player is driving too fast (rolls the highest number on the die) in any one of the crash zones, indicated by shaded spaces 30 and 34 on the racetrack 12 . The crash zones are located in all of spaces 34 in the turns 18 , 20 , 24 , and 26 and in the spaces 30 provided between the turns 18 and 20 and turns 24 and 26 . Alternatively, crash zones may be placed at other locations along the racetrack 12 . A player may avoid crashing by making an emergency pit stop if he or she can advance the required number of spaces 30 to the pit area 28 with the roll. If not, the toy vehicle moves the number of spaces 30 and crashes at that spot. When a crash occurs, the crashed race vehicle preferably blocks two of the three lanes 31 a, 31 b, or 31 c, and the remaining race vehicles slow to one half of their speed, as determined by the roll of the twelve-sided die, rounding up in the case of odd numbers. The crashed vehicle is removed when it becomes the crashed player's turn to roll, and the remaining players resume normal speed after the crashed vehicle is removed.
[0033] The last place vehicle, the toy vehicle in the farthest position in the outermost lane, is allowed to ‘draft’ by rolling the six-sided die, as well as the twelve-sided die, when it is the last place player's turn to roll. This simulates the extra speed gain possible when utilizing the drafting technique of professional race vehicle drivers. In addition, the last place vehicle is allowed the full amount of the draft roll in a crash situation, providing a further way for the last place vehicle to draw nearer to the rest of the field during a crash situation.
[0034] Alternatively, the players may use the twenty-sided die to advance around the racetrack 12 . The twenty-sided die is preferably used when a physically larger track is utilized, for example racetrack 200 noted below. The use of a twenty-sided die will assist in keeping the game moving at its preferred quick pace.
[0035] The present invention provides a means for awarding points to the players by providing points for obtaining the pole position, for winning individual laps, and for the final race placing positions. The present invention further provides a means for determining the winner of a racing season by summing up the awarded points for the individual races. Points may be tallied on a point standings card (not shown) and are awarded according to the following table:
Placing in Race Points Notes 1 st Place 20 points 2 nd Place 16 points 3 rd Place 14 points 4 th Place 12 points 5 th Place 10 points 6 th Place 8 points 7 th Place 6 points 8 th Place 5 points 9 th Place 4 points 10 th Place 3 points Non-qualifying cars still win points even though they don't race 11 th Place 2 points See 10 th Place Notes 12 th Place 1 point See 10 th Place Notes Bonus Points Winning pole 1 point Leading a lap 1 point
[0036] The player amassing the most total points at the end of a ten-race season is declared the season champion.
[0037] A second embodiment of a game board according to this invention is indicated generally at 100 in FIG. 2. The game board 100 includes a racetrack 112 having a start/finish line 114 preferably marked by alternating black and white rectangles. The racetrack 112 includes a straight section 116 , a first turn 118 , a second turn 120 , a third turn (180 degrees) 122 , a fourth turn (180 degrees) 124 , a backstretch 125 , a fifth turn 126 , a sixth turn 127 , a pit area 128 , and starting positions A through I. The racetrack 112 also includes crash zones indicated by shaded spaces 130 and 134 on the racetrack 112 .
[0038] As in game board 10 , the spaces 130 are divided into at least three circumferential lanes 131 a, 131 b, and 131 c, so that a player can pass the other players during the game described above. Similarly, lane 131 a will be referred to as the inside lane, lane 131 b will be referred to as the middle lane, and lane 131 c will be referred to as the outside lane. Lanes 131 a, 131 b, and 131 c are provided in the straight section 116 . The racetrack 112 narrows to lanes 131 b and 131 c through the first, second, third, and fourth turns 118 , 120 , 122 , and 124 . The racetrack 112 expands back to lanes 131 a, 131 b, and 131 c on the backstretch 125 and continues until the start/finish line 114 . Also as in game board 10 , the number of spaces 134 in turns 118 , 120 , 122 , and 124 is the greatest in outside lane 131 c. Similarly, the number of spaces 134 in middle lane 131 b is greater than the number of spaces 134 in inside lane 131 a, but less than outside lane 131 c.
[0039] When spaces 130 are approximately three inches in length and two inches in width, the game board 100 is approximately forty-four inches in length and twenty-eight inches in width. Preferably, the game board 100 is divided into two equal sections and folded along a mid-line of its length.
[0040] The game board 100 can also be played according to the game rules as outlined above.
[0041] A third embodiment of a game board according to this invention is indicated generally at 200 in FIG. 3. The game board 200 includes a racetrack 212 having a start/finish line 214 preferably marked by alternating black and white rectangles. The track 212 includes a straight section 216 , a first turn (180 degrees) 218 , a second turn (180 degrees) 220 , a third turn (180 degrees) 222 , a backstretch 223 , a fourth turn (180 degrees) 224 , a fifth turn (180 degrees) 226 , a sixth turn (180 degrees) 227 , a pit area 228 , and starting positions A through I. The racetrack 212 also includes crash zones indicated by shaded spaces 230 and 234 on the racetrack 212 .
[0042] As in game boards 10 and 100 , the spaces 230 are divided into at least three circumferential lanes 231 a, 231 b, and 231 c, so that a player can pass the other players during the game described above. Similarly, lane 231 a will be referred to as the inside lane, lane 231 b will be referred to as the middle lane, and lane 231 c will be referred to as the outside lane. Lanes 231 a, 231 b, and 231 c are provided in the straight section 216 , in backstretch 223 , and in each of turns 218 , 220 , 222 , 223 , 224 , 226 , and 227 . Also as in game boards 10 and 100 , the number of spaces 234 in turns 218 , 220 , 222 , 223 , 224 , 226 , and 227 is the greatest in outside lane 131 c. Similarly, the number of spaces 234 in middle lane 231 b is greater than the number of spaces 234 in inside lane 231 a, but less than outside lane 231 c.
[0043] When spaces 230 are approximately three inches in length and two inches in width, the game board 200 is approximately sixty-six inches in length and twenty-eight inches in width. Preferably, the game board 200 is divided into equal third along its length for folding and easy storage.
[0044] The game board 200 can also be played according to the game rules as outlined above.
[0045] Alternatively, the game boards 10 or 100 may be printed with racetracks 12 or 112 on opposing planar sides of the game board 10 or 100 , as they are contemplated to be approximately the same size. Similarly, game board 200 may be printed with racetrack 212 and a similar-sized racetrack with a different configuration on opposing planar sides of the game board 200 . In this way, players in the game could race on alternating courses through the length of the season, adding another element to the games, and increasing the enjoyment of the players.
[0046] In accordance with the provisions of the patent statutes, the present invention has been described in what is considered to represent its preferred embodiment. However, it should be noted that the invention can be practiced otherwise than as specifically illustrated and described without departing from its spirit or scope. For example, other tracks and variations may be designed for the game boards 10 , 100 , and 200 . Other rules, scoring means and variations may be designed for use with the games described above.
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A vehicle racing board game includes a racetrack having a start/finish line crossed by lanes and a pit area connected to the lanes. The lanes and the pit area are divided into a plurality of spaces including starting positions and a crash zone. Toy vehicles are used as playing pieces for advancing around the racetrack according to numbers generated by dice. The dice also are used to determine starting positions that set the order of play and identify a “crash”. Points are awarded for winning the pole position, winning a lap and finishing position in each race of a season to determine a champion.
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BACKGROUND OF THE INVENTION
The present invention relates to a device to reduce airflow noises on elevator cars travelling at high speed. The device is in the form of an aerodynamically favorably formed dome that is attached either on the car roof or under the car floor or in both positions.
An elevator car is part of an elevator installation, which consists essentially of the following components: an elevator hoistway with guiderails, the elevator car mentioned above with its car frame, a counterweight, the suspension ropes for car and counterweight, and a drive unit with traction sheave which drives these suspension ropes. High-speed cars are also connected on their underside to the counterweight by a compensating rope that runs over a pulley in the hoistway pit. The elevator car is elastically supported in the car frame, which hangs from the suspension ropes, is guided in the direction of travel by the guiderails acting on guiding elements, and is constructed robustly to allow for the stresses occurring in operation and when breakdowns occur.
Cars of elevator installations are usually constructed as aerodynamically unfavorable cuboid bodies with sharp edges and move in mostly narrow elevator hoistways. At travel speeds above about 4 m/s the occurrence of air eddies and flow separation cause noises that are unpleasant or even highly irritating. To reduce these noises, dome-like attachments of aerodynamically favorable shape are attached to high-speed elevator cars in one, or both, directions of travel with the objective of guiding the displaced air volume around the car body with as little eddying or separation as possible. The U.S. Pat. No. 5,220,979 discloses several solutions for attachments to elevator cars to improve airflow. All the solutions described there have the characteristics that on the same side as the entrance of the elevator car they have flat surfaces extending in the direction of the continuation of the car front wall downward, or downward and upward, and that their walls are constructed as robust plates or shaped parts.
The British patent document GB 2 280 662 also describes devices to improve the flow characteristics of elevator cars, the passenger car being built into a closed housing which is constructed in an aerodynamically favorable manner. As in the U.S. Pat. No. 5,220,979, the aerodynamically favorable housings shown in the patent document GB 2 280 662 also have on the same side as the entrance of the elevator car flat surfaces extending in the direction of the continuation of the car front wall upward or downward and the walls of these housings are constructed of robust, shaped parts.
Both the solutions mentioned have the disadvantages that the disclosed aerodynamically favorable attachments and housings are heavy and bulky components which require voluminous packing, are difficult to transport and install, and enormously increase the weight of the car to be moved by the elevator installation. Furthermore, manufacturing domes with multiaxially curved surfaces, as they are described in both documents, is very costly, particularly as the domes must be adapted to a large number of different car dimensions.
SUMMARY OF THE INVENTION
The present invention concerns aerodynamically favorable elevator car domes that can be manufactured inexpensively and flexibly, be packed into a small volume, are easy to transport and install, and have low mass.
According to the invention, this is achieved by such aerodynamically favorable car domes being made not from robust shaped parts but from a membranous, flexible, and foldable foil.
By comparison with known car attachments for improving airflow, car domes made in this way have the following important advantages:
No special machines, molds, or patterns are needed for their manufacture, as is the case with robust shaped parts. In view of the numerous different combinations of car dimensions, this results in decisive cost savings.
The folded flexible dome has only a small volume, is inexpensive to transport, and easy to install.
Thanks to the thin, membranous wall of the dome, the mass of the dome which has to be moved by the elevator installation in addition to the car remains minimal.
BRIEF DESCRIPTION OF THE DRAWINGS
The above, as well as other advantages of the present invention, will become readily apparent to those skilled in the art from the following detailed description of a preferred embodiment when considered in the light of the accompanying drawings in which:
FIG. 1 is a perspective view of an elevator car with two aerodynamically favorable elevator car domes of membranous, flexible foil in accordance with the present invention;
FIG. 2 is a perspective view of the elevator car shown in the FIG. 1 with an attached supporting construction of rod-shaped elements, which stiffen the wall of the dome;
FIG. 3 is a horizontal section view through the elevator car dome according to the present invention;
FIG. 4 is an enlarged portion “B” of the FIG. 3 showing the attachment of the membranous dome wall to the vertically oriented rods of the supporting construction;
FIG. 5 is an enlarged fragmentary vertical section view taken along the line V—V in the FIG. 3 through part of the elevator car dome showing the fastening of the dome wall to the base frame of the supporting structure and to the car roof;
FIG. 6 is a vertical section view through an alternate embodiment elevator car dome according to the present invention that has tube-like air chambers built into the membranous dome wall as a supporting construction; and
FIG. 7 is an enlarged cross-sectional view taken along the line VII—VII in the FIG. 7 .
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows two elevator car domes 1 formed of a membranous, flexible foil material according to the present invention that are fastened on an elevator car 2 above the car roof 3 as well as under the car floor 4 . The foil material is tear-resistant and consists preferably of plastic, e.g. PVC, of tent fabric, rubber, or similar materials. The elevator car 2 is guided on a pair of vertically extending guiderails 5 by guide rollers 6 and suspended between suspension ropes 7 and so-called compensating ropes 8 for travel in a hoistway (not shown). The drawing shows a preferred embodiment of the aerodynamically favorable dome 1 , which resembles a slightly truncated pyramid, the surface of whose base corresponds to the horizontal outline of the car 2 , and the side surfaces of which are curved to such an extent that vertical sections through their center form a close approximation to half an ellipse. The point of the dome 1 lies above or below the center of the car 2 . The car dome 1 can be constructed of several partial surfaces or panels suitably cut and welded together. Aerodynamically favorable domes of a different shape can, of course, also be realized with the technique according to the present invention.
Formed in the side walls of the elevator car domes 1 are closable openings 9 which are constructed at suitable points in the membranous dome wall and permit passage for passengers being evacuated, as well as making the spaces above the car roof 3 and below the car floor 4 accessible for service work. Preferred means of closure are zip fasteners, but other types of closure such as Velcro fasteners, cord/eyelet fasteners, etc. can also be used. While the openings 9 are formed in at least one and can be formed in all of the side walls, recesses 10 are formed on both sides of the elevator car dome 1 facing the guiderails to make space and provide clearance for the guide rollers 6 and the safety devices (not shown) integrated into this area.
FIG. 2 shows the car 2 with the lower dome 1 removed and the flexible foil removed from the upper dome 1 to expose a supporting construction or frame 13 fastened on an upper transverse yoke 11 of a car frame 12 which gives the necessary stiffness to the car dome flexible foil. Visible are a base frame 14 of the supporting frame 13 , with fastening elements 15 for fastening the base frame to the car frame, a small upper rectangular frame 16 for the suspension ropes 7 to pass through, as well as a number of vertically oriented ribs in the form of supporting rods 17 arranged corresponding to the shape of the dome 1 and bent elliptically in the aerodynamically favorable shape. The positions of the rods 17 are determined in part by the recesses 10 in the sides, which are described above. The rods 17 each have one end attached to the base frame 14 and an opposite end attached to the upper frame 16 .
During installation of the upper one of the domes 1 on the car 2 , the base frame 14 is bolted tightly to the upper transverse yoke 11 of the car frame 12 mentioned above. Since the elevator car 2 is supported in this frame 12 by vibration-isolating elements 18 , using this manner of fastening the dome 1 largely avoids transmission of structure borne noise between the dome and the car. Using bolted joints at suitable points makes it possible to dismantle the supporting construction 13 into parts of suitable size for transportation. On installations with high maximum speed and high noise reduction requirements, an additional identical dome 1 can be fastened facing the opposite way under the car floor 4 (as shown in FIG. 1) with the base frame of this second dome attached to the lower transverse yoke of the car frame 12 . There, the opening in the small rectangular frame 16 is required for the passage of the compensating rope 8 mentioned above.
FIG. 3 is a horizontal section through the flexible elevator car dome 1 showing the arrangement and fastening of the parts of the dome wall which are prefabricated by welding foil components or panels that have been cut to shape. Normally, the dome wall comprises a front panel 1 . 1 , a rear panel 1 . 2 , and two side panels 1 . 3 for closing the recesses 10 at the sides. It can also be seen in FIG. 3 how the dome wall parts mentioned above are fastened to the vertically oriented supporting rods 17 of the supporting frame 13 , and tightened with the aid of eyelets fastened to their edges and cords 19 .
FIG. 4 shows this fastening of the dome wall 1 . 1 to the rods 17 by means of eyelets 20 and the cords 19 in more detail. Fastening strips 21 are welded in the correct position during prefabrication of the dome parts and have the required number of eyelets 20 .
From FIG. 5 it can be seen how the flexible dome wall front panel 1 . 1 is fixed to the base frame 14 of the supporting frame 13 with the same eyelet/cord technique (fastening strips 21 , eyelets 20 and cords 19 ) and to the car roof 3 with bolts 22 and a strip 23 .
FIG. 6 shows schematically a further possible embodiment of a flexible car dome 31 . Here, the required stiffness is not obtained by means of a supporting frame of bent rod ribs, but by ribs of inflatable air chambers 24 in the form of tubes which are fastened to the inside of the prefabricated dome. Fastening takes place by means of brackets 25 welded onto the inside wall of the dome, as can be seen in FIG. 7, a sectional view taken along the line VII—VII in the FIG. 6 .
The spatial arrangement of these air chambers 24 corresponds approximately to that of the supporting rods 17 of the supporting frame 13 in FIG. 2 . The shape of the dome 31 , which is held erect by air pressure in the chambers 24 , is derived from the shape of the dome panels which are cut and welded together to form a dome wall 31 . 1 . The air chambers 24 consist preferably of fabric-reinforced, flexible, and airtight tubes, which are closed at both ends with stoppers 26 , and have an inflation valve 27 . Horizontally extending pieces of tube 28 are fastened to the base frame 14 and the upper rectangular frame 16 to receive the ends of the tubular air chambers 24 and force them into the desired initial direction.
The advantage of this alternate embodiment supporting frame over the supporting frame 13 with the rigid rods 17 is that the air chambers 24 can be built into the prefabricated flexible dome wall in the correct position. This dispenses with the need to fasten the dome wall to the supporting rods during installation. Moreover, with this technique, the dome wall can be made in one piece.
In accordance with the provisions of the patent statutes, the present invention has been described in what is considered to represent its preferred embodiment. However, it should be noted that the invention can be practiced otherwise than as specifically illustrated and described without departing from its spirit or scope.
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An apparatus for reducing wind noises on elevator cars traveling at high speed includes domes with an aerodynamically favorable shape that are attached above the car roof and/or under the car floor. The domes are made of a flexible material attached over a supporting frame of rods or tubular air chambers. Closable openings in the dome walls permit evacuation of passengers and access to the car roof and the underside of the car.
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BACKGROUND OF THE INVENTION
This invention relates to certain 1-(3,5-dichlorobenzoyl)-3-phenylpyrazolines which are useful as a mildewicide.
DESCRIPTION OF THE INVENTION
The compounds of the present invention are certain 1-(3,5-dichlorobenzoyl)-3-phenylpyrazolines and have the following structural formula ##STR2## where R is hydrogen, alkyl having 1 to 4 carbon atoms, preferably methyl, alkoxy having 1 to 4 carbon atoms, preferably methoxy or halo, preferably chloro.
In the above description of the compounds of this invention, alkyl includes both straight chain and branched chain configurations, for example, methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl or tert. butyl. The term halo includes chlorine, bromine, iodine and fluorine.
The compounds of the present invention can be prepared by the following general method.
Reaction No. 1 ##STR3## wherein R is as previously defined.
Generally, a mole amount of the acetophenone reactant and a slight excess of both dimethylamine hydrochloride and paraformaldehyde dissolved in a solvent such as ethanol are heated to reflux with stirring. Next, the reaction mixture is refluxed for about 4 hours with a catalytic amount of hydrochloric acid. Thereafter, the mixture is cooled and acetone is added to precipitate the desired reaction product.
Reaction No. 2 ##STR4## wherein R is as previously defined.
Generally, mole amounts of hydrazine hydrate and sodium hydroxide (as 50% solution in water) dissolved in methanol are heated to reflux with stirring. Next, a mole amount of the reaction product from Reaction No. 1 dissolved in a solvent such as methanol is added and the resulting mixture is refluxed for about 2 hours. Next, the solvent is removed under vacuum and methylene chloride solvent is added under an inert atmosphere to dissolve the reaction product. This solution is washed with NaHCO 3 solution and the organic phase dried under an inert atmosphere with Na 2 SO 4 in the presence of a small amount of Na 2 CO 3 . The solution is filtered and the solvent stripped by vacuum to yield the desired solid reaction product. The product should be stored in the darkened area under an inert atmosphere in the cold.
Reaction No. 3 ##STR5## wherein R is as previously defined.
Generally, a mole amount of 3,5-dichlorobenzoylchloride dissolved in methylene chloride is added to a solution of a mole amount of the reaction product of Reaction No. 2 and a mole amount of triethylamine at a temperature of -10° C. to -5° C. The mixture is stirred at room temperature for 2 hours and for 1/2 hour at 40° C. The resulting mixture is cooled, washed three times with water, twice with a dilute NaHCO 3 solution and one time with a saturated NaCl brine solution followed by drying. The solvent is removed by vacuum to yield the desired product.
Preparation of the compounds of this invention is illustrated by the following examples.
EXAMPLE I
3-(Dimethylamino)-4'-methyl propiophenone hydrochloride ##STR6##
This example teaches a method of preparation for the reactant 3-(dimethylamino)-4'-methyl propiophenone hydrochloride.
53.6 Grams (g) (0.4 mole) of p-methylacetophenone, 42.4 g (0.52 mole) dimethylamine hydrochloride, 15.6 g (0.52 mole) paraformaldehyde and 64 milliliters (ml) ethanol were placed in a round-bottom flask equipped with a condenser and the mixture was heated to reflux with stirring. Next, 0.8 ml of concentrated hydrochloric acid was added to the mixture and refluxing was continued for 4 hours. The mixture was cooled and 600 ml of acetone was added. The desired product precipitated and was filtered and dried. m.p. 162°-163°. Yield: 70 g (76.9%).
EXAMPLE II
3-(4-Methylphenyl)-pyrazoline ##STR7##
This example teaches a method of preparation for the reactant 3-(4-methylphenyl)-pyrazoline.
22.4 ml hydrazine hydrate, 50% sodium hydroxide solution (11.5 ml) and 28.8 ml methanol were placed in a round-bottom flask equipped with a stirrer and condenser and the mixture heated to reflux with stirring. Next, a solution of 24.8 g (0.16 mole) of 3-(dimethylamino)-4'-methyl propiophenone hydrochloride of Example I dissolved in 112 ml methanol was added to the above mixture and refluxing was continued for 2 hours with stirring.
The methanol was removed in vacuo. 200 ml methylene chloride was added to the residue under an argon atmosphere and this solution was washed rapidly with two 150 ml portions of a warm, saturated sodium bicarbonate solution. The organic phase was dried under an argon atmosphere with sodium sulfate in the presence of a small amount of sodium carbonate. The solution was kept in a darkened area and refrigerated during drying.
The solution was then filtered through Dicalite and the solvent removed in vacuo. The residue was pumped out under high vacuum to yield a light yellow solid which was stored in a refrigerator in a darkened area under an argon atmosphere. Yield: 16.1 g (62.5%).
EXAMPLE III
1-(3,5-Dichlorobenzoyl)-3-(4-methylphenyl)-pyrazoline ##STR8##
This example teaches a method of preparation for the compound 1-(3,5-dichlorobenzoyl)-3-(4-methylphenyl)-pyrazoline.
A solution of 6.3 g (0.03 mole) 3,5-dichlorobenzoyl chloride in 25 ml methylene chloride at -10° C. to -5° C. was added to a solution of 5.1 g (0.032 mole) pyrazoline, reactant of Example II, and 3.5 g (0.03 mole) triethylamine in 70 ml methylene chloride. The mixture was stirred for 2 hours at room temperature and 1/2 hour at 40° C. The resulting mixture was cooled, washed three times with water, twice with a dilute sodium bicarbonate solution, one time with saturated brine and dried. The solvent was removed in vacuo and the crude product was recrystallized from toluene to yield the desired product. m.p. 165°-168°. A yield of 3.5 g (35%) was realized and the structure was confirmed by infrared and mass spectroscopy.
The following is a table of certain selected compounds that are preparable according to the procedure described hereto. Compound numbers are assigned to each compound and are used throughout the remainder of the application.
TABLE I______________________________________ ##STR9##Compound MeltingNumber R Point______________________________________1 H 120-132° C.2 p-CH.sub.3 O 129-130° C.3 p-Cl 190-191° C. 4* p-CH.sub.3 165-168° C.______________________________________ *Prepared in Example III
FOLIAR MILDEWICIDE EVALUATION TESTS
A. Evaluation for Preventive Action
1. Bean Powdery Mildew Test
Pinto bean plants (Phaseolus vulgaris L.) approximately 10 cm tall are transplanted into sandy loam soil in three-inch clay pots. The plants are then inverted and dipped for two to three seconds in 50-50 acetone water solution of the test chemical. Test concentrations range from 1000 ppm downward. After the leaves are dried, they are dusted with spores of the bean powdery mildew (Erysiphe polygoni De Candolle) and held in the greenhouse until fungal growth appears on the leaf surface. Effectiveness is recorded as the lowest concentration, in ppm, which will provide 75% or greater reduction in mycelial formation as compared to untreated, inoculated plants. These values are recorded in Table II.
2. Barley Powdery Mildew Test
Barley leaves (Hordeum vulgare) are grown from seed in sandy loam soil to a height of approximately 10 cm in three-inch clay pots. The plants are then inverted and dipped for two to three seconds in 50-50 acetone water solution of the test chemical. Test concentrations range from 1000 ppm downward. After the leaves are dried, they are dusted with spores of the barley powdery mildew fungus (Erysiphe graminis) and held in the greenhouse until fungal growth appears on the leaf surface. Effectiveness is recorded as the lowest concentration, in ppm, which will provide 75% or greater reduction in mycelial formation as compared to untreated, inoculated plants. These values are recorded in Table II.
TABLE II______________________________________Preventive ActionCompound Bean Powdery Barley PowderyNumber Mildew Mildew______________________________________1 1.0 10.02 5.0 10.03 * 5004 1.0 5.0______________________________________ *Not active at 1,000 ppm and not tested at a higher concentration
The compounds of this invention are generally embodied into a form suitable for convenient application. For example, the compounds can be embodied into a pesticidal composition which is provided in the form of emulsions, suspensions, solutions, dusts and aerosol sprays. In general, such compositions will contain, in addition to the active compound, the adjuvants which are found normally in pesticide preparations. In these compositions, an active compound of this invention can be employed as the sole pesticide component or it can be used in admixture with other compounds having similar utility. The pesticide compositions of this invention can contain, as adjuvants, organic solvents, such as sesame oil, xylene range solvents, heavy petroleum, etc.; water; emulsifying agents; surface active agents; talc; pyrophyllite; diatomite; gypsum; clays, propellants, such as dichlorodifluoromethane, etc. If desired, however, an active compound can be applied directly where control is desired.
The precise manner in which the pesticidal compositions of this invention are used in any particular instance will be readily apparent to a person skilled in the art. The concentration of the active compound in the present compositions can vary within rather wide limits, ordinarily the compound will comprise not more than about 15.0% by weight of the composition. Preferably, however, the pesticide compositions of this invention will be in the form of a solution or suspension containing up to about 1.0% by weight of the active pesticide compound.
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Certain 1-(3,5-dichlorobenzoyl)-3-phenylpyrazolines which have the structural formula ##STR1## where R is hydrogen, alkyl, alkoxy or halo and their uses as a mildewicide.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This is a continuation application of PCT/JP2007/56389, filed on Mar. 27, 2007.
FIELD
[0002] The embodiments discussed herein are related to a semiconductor component in which a semiconductor element is enclosed, and a manufacturing method of the semiconductor component.
BACKGROUND
[0003] Recently, in semiconductor packages in which a semiconductor element is enclosed, the heat generation rate has been increasing as the operation frequency and the wiring density of the semiconductor element increase and the density of wiring increases, and there is a need to securely dissipate the generated heat and to effectively reduce the thermal resistance. Moreover, as a semiconductor package which is superior in the convenience of additional installation, version upgrading, and maintenance etc. of electronic equipment after it is brought into operation, semiconductor packages of an LGA (Land Grid Array) structure in which thin plate-shaped electrodes are arranged in a grid-like pattern on the surface are widely used.
[0004] FIG. 1 is a sectional view of a conventional semiconductor package of an LGA structure.
[0005] The semiconductor package 10 includes a wiring board 11 in the lower face of which thin plate-shaped electrodes are disposed, a semiconductor element 12 to which I/O terminals 14 are attached, a heat spreader 17 which dissipates heat generated in the semiconductor element 12 , a spacer 16 which supports the heat spreader 17 , where the semiconductor element 12 and the heat spreader 17 are joined by a joining member 13 , and the spacer 16 , the wiring board 11 , and the heat spreader 17 are bonded by an adhesive 15 . In order to reduce the thermal resistivity of the semiconductor element 12 , it is necessary to effectively transfer heat generated at the semiconductor element 12 to the heat spreader 17 , and therefore the thickness of the joining member 13 for joining the semiconductor element 12 with the heat spreader 17 is precisely adjusted.
[0006] The semiconductor package 10 , in which the wiring board 11 is displaced so as to face a socket with pins arranged in a grid-like pattern, is mounted into electronic equipment by being strongly pressed against the socket. Thus, a semiconductor package 10 of LGA structure has an advantage in that it may be attached to and detached from electronic equipment more easily and may be powered more efficiently compared with semiconductor packages including raised electrodes made up of pins and solder etc.
[0007] Incidentally, in a semiconductor package 10 of LGA structure, the registration with the socket is performed by the outer dimensions, and the semiconductor package 10 is mounted into electronic equipment by being strongly pressed against the socket. For this reason, if the wiring board 11 , the heat spreader 17 , and others are obliquely bonded due to the squeeze-out of the adhesive 15 or any other factor, the pressing force F from the socket will be applied leaning toward one part of the surface of the wiring board 11 posing risks of such as fracture of the wiring board 11 and breakage of the internal wiring. Further, if the adhesive 15 is squeezed out beyond the outer dimension of the semiconductor package 10 , misregistrations between the semiconductor package 10 and the socket may take place resulting in connection deficiencies.
[0008] In this respect, Japanese Laid-open Patent Publications No. 2006-80927 and No. 2004-296739 describe a technique in which there is provided a step in the end face of the spacer so that the squeezed-out adhesive is accommodated therein. According to the technique described by Japanese Laid-open Patent Publications No. 2006-80927 and No. 2004-296739, since an excess adhesive will be pressed out to the end face of the spacer entering into the step, it is possible to mitigate the squeeze-out of the adhesive.
[0009] However, since the semiconductor package 10 itself is small-sized, a problem remains in that the amount of adhesive which may be accommodated in the step in the spacer end face is very small and is not enough to solve the fracture of the wiring board and the connection deficiencies due to the squeeze-out of the adhesive.
SUMMARY
[0010] According to an aspect of the invention, a semiconductor component includes a semiconductor element that has a plurality of signals, a wiring board that is disposed below the semiconductor element and that draws the plurality of signals of the semiconductor element, a heat conduction member that dissipates heat generated by the semiconductor element, a joining member that is disposed between the semiconductor element and the heat conduction member and that joins the heat conduction member to the semiconductor element, a support member formed with an opening so as to surround the semiconductor element that supports the heat conduction member, a first adhesive member that is disposed between the support member and the wiring board to bond the support member with the wiring board and a second adhesive member that is disposed between the support member and the heat conduction member to bond the support member with the heat conduction member.
BRIEF DESCRIPTION OF DRAWINGS
[0011] FIG. 1 is a sectional view of a conventional semiconductor package of an LGA structure;
[0012] FIG. 2 is a schematic block diagram of a semiconductor component which is an embodiment of the present invention;
[0013] FIG. 3 illustrates a spacer;
[0014] FIG. 4 illustrates a manufacturing method of a semiconductor component;
[0015] FIG. 5 illustrates a spacer in a second embodiment of the present invention;
[0016] FIG. 6 illustrates a spacer in a third embodiment of the present invention;
[0017] FIG. 7 illustrates a spacer in a fourth embodiment of the present invention;
[0018] FIG. 8 illustrates a manufacturing method of a semiconductor component to which the spacer illustrated in FIG. 7 is applied;
[0019] FIG. 9 illustrates a spacer in a fifth embodiment of the present invention;
[0020] FIG. 10 is an exploded perspective view of a semiconductor component which is a sixth embodiment of the present invention;
[0021] FIG. 11 illustrates an adhesive sheet in a seventh embodiment of the present invention;
[0022] FIG. 12 illustrates an adhesive sheet in an eighth embodiment of the present invention; and
[0023] FIG. 13 illustrates a semiconductor component which is a ninth embodiment of the present invention.
DESCRIPTION OF EMBODIMENTS
[0024] Hereafter, embodiments of the present invention will be described with reference to appended drawings.
[0025] FIG. 2 is a schematic block diagram of a semiconductor component which is an embodiment of the present invention.
[0026] FIG. 2A is an exploded perspective view to illustrate a semiconductor component 100 .
[0027] The semiconductor component 100 is formed such that on a wiring board 110 , there are placed a joining member 123 , an adhesive sheet 130 , a spacer 140 , and a heat spreader 150 etc. on top of one another.
[0028] There are thin plate-shaped electrodes disposed in the lower face of the wiring board 110 , which exchanges signals and power with external apparatuses as the result of those electrodes being pressed against a socket. The wiring board 110 corresponds to an example of the wiring board referred to in the present embodiment.
[0029] There is disposed a semiconductor element beneath the joining member 123 , and the semiconductor element and the heat spreader 150 are bonded by the joining member 123 . The semiconductor element and the joining member 123 will be illustrated below. Moreover, the adhesive sheet 130 and the spacer 140 are provided with openings 131 and 142 respectively, and the semiconductor element and the joining member 123 are disposed inside those openings 131 and 142 .
[0030] The adhesive sheet 130 is made up of a thermosetting adhesive material and two sheets thereof are provided interposing the spacer 140 therebetween. The adhesive sheet 130 disposed between the wiring board 110 and the spacer 140 is an example of the first adhesive member referred to in the present embodiment and also corresponds to an example of the first thermosetting adhesive member referred to in the present embodiment. Further, the adhesive sheet 130 disposed between the spacer 140 and the heat spreader 150 is an example of the second adhesive member referred to in the present embodiment and also corresponds to an example of the second thermosetting adhesive member referred to in the present embodiment.
[0031] FIG. 3 illustrates the spacer 140 .
[0032] FIG. 3A illustrates the face (hereafter, referred to as an upper face) of the spacer 140 on the side facing the heat spreader 150 , and FIG. 3B illustrates the face (hereafter, referred to as a lower face) of the spacer 140 on the side facing the wiring board 110 .
[0033] The spacer 140 , which is adapted to support the heat spreader 150 , is formed with grooves 141 having the same length with one another in the outer peripheral section of each of the upper and lower faces as illustrated in FIG. 3 . The spacer 140 is an example of the support member referred to in the present embodiment, and the grooves 141 are an example of “the depressions” referred to in the present embodiment, and also correspond to an example of “the grooves” referred to in the present embodiment.
[0034] Now, description will return to FIG. 2 .
[0035] The heat spreader 150 is adapted to dissipate heat generated by the semiconductor element disposed beneath the joining member 123 . The heat spreader 150 corresponds to an example of the heat conduction member referred to in the present embodiment.
[0036] FIG. 2B illustrates an outer perspective view of the semiconductor component 100 .
[0037] The heat spreader 150 is formed, from outward appearances, such that a spacer 140 etc. is interposed between the wiring board 110 and the heat spreader 150 and, in the space formed by the wiring board 110 , the heat spreader 150 , and spacer 140 , the semiconductor element and the joining member 123 are enclosed.
[0038] Next, a manufacturing method of the semiconductor component 100 will be described.
[0039] FIG. 4 illustrates a manufacturing method of the semiconductor component 100 .
[0040] Upon manufacturing the semiconductor component 100 , first, a first adhesive sheet 130 , a spacer 140 , and a second adhesive sheet 130 are disposed in this order on a wiring board 110 , and a semiconductor element 122 , to which an I/O terminal 121 is bonded by a adhesive material 121 a , and a joining member 123 are successively disposed inside each of the openings 131 and 142 of the adhesive sheet 130 and the spacer 140 (step S 11 of FIG. 4 ). The semiconductor element 122 is an example of the semiconductor element referred to in the present embodiment, and the joining member 123 corresponds to an example of the joining member referred to in the present embodiment. Moreover, the process of disposing the adhesive sheet 130 and the spacer 140 illustrated in step S 11 of FIG. 4 corresponds to an example of “the step of disposing a first thermosetting adhesive member, a support member, and a second thermosetting adhesive member on top of one another” in the manufacturing method of the semiconductor component of the present embodiment.
[0041] It is noted that in the present embodiment, an adhesive sheet 130 having a thickness larger than conventionally used is applied so that the thickness of the two adhesive sheets 130 interposing the spacer 140 therebetween is larger than the thickness of the semiconductor element 122 with the joining member 123 placed thereon.
[0042] Then, a heat spreader 150 is overlaid on the joining member 123 and the adhesive sheet 130 to form a semiconductor component 100 in the state before various elements are bonded thereto (hereafter, the semiconductor component 100 before the bonding process is referred to as an “unbonded semiconductor component 100 ′”). In step S 12 — a of FIG. 4 , a section taken across near the center of unbonded semiconductor component 100 ′ is illustrated and, in step S 12 — b of FIG. 4 , a section view taken across the outer peripheral section of the unbonded semiconductor component 100 ′ is illustrated. As illustrated in step S 12 — b , the grooves 141 are formed in the upper and lower faces of the spacer 140 , and at this time, the adhesive sheet 130 has not gotten into the inside of those grooves 141 . This step S 12 of overlaying the heat spreader 150 corresponds to one example of “the step of disposing the heat conduction member” in the manufacturing method of the semiconductor component of the present embodiment.
[0043] When the heat spreader 150 is overlaid and the unbonded semiconductor component 100 ′ is heated, the surface of the joining member 123 melts thereby increasing the viscosity, and two adhesive sheets 130 melt into a liquid. Further, the heat spreader 150 is pressed against the joining member 123 (step S 13 of FIG. 4 ). In the present embodiment, an adhesive sheet 130 of a thickness larger than conventionally used is used, and as a result of the heat spreader 150 being pushed in up to the height of the upper face of the joining member 123 , the thermosetting adhesive material 132 , which has resulted from the melting of the two adhesive sheets 130 , is pushed out into the grooves 141 formed in the upper and lower faces of the spacer 140 . Step S 13 of pushing out the thermosetting adhesive material 132 into the grooves 141 corresponds to an example of “the step of filling the grooves with the thermosetting adhesive member” in the manufacturing method of the semiconductor component of the present embodiment.
[0044] Next, the unbonded semiconductor component 100 ′ is cooled down (step S 14 of FIG. 4 ). As a result, the joining member 123 and the thermosetting adhesive material 132 are hardened, thereby the joining member 123 being bonded to the heat spreader 150 , and the spacer 140 being bonded to the heat spreader 150 and the wiring board 110 . This step S 14 of hardening the thermosetting adhesive material 132 corresponds to an example of “the step of hardening the thermosetting adhesive member” in the manufacturing method of the semiconductor component of the present embodiment.
[0045] The hardened thermosetting adhesive material 132 ′ is present between the spacer 140 and the heat spreader 150 and between the spacer 140 and the wiring board 110 thereby bonding them, and an excess part thereof has gotten into the grooves 141 of the spacer 140 . Thus, since the semiconductor component 100 , in which no squeeze-out of the thermosetting adhesive material 132 has occurred, has a uniform thickness, it is possible to avoid deficiencies such as that the wiring board 110 fractures by being pressed hard against the socket, and misregistration with the socket, which is registered by the outer dimension, takes place leading to connection deficiencies. Further, since as a result of a rather thick adhesive sheet 130 being used, the clearances between the spacer 140 and the wiring board 110 , and between the spacer and the heat spreader 150 are filled with an excess thermosetting adhesive material 132 , it becomes possible to omit the process of charging and hardening liquid resin such as underfill materials into clearances, which is conventionally carried out in a later stage of step S 14 , thus reducing the manufacturing cost.
[0046] So far, the description of the first embodiment of the present invention has been completed, and a second embodiment thereof will be described. Since the second embodiment of the present invention has a similar structure as the first embodiment excepting the shape of the grooves formed in the spacer, like elements as those of the first embodiment will be given like reference symbols to omit the description thereof and only the differences from the first embodiment will be described.
[0047] FIG. 5 illustrates a spacer 140 _ 2 in the second embodiment of the present invention.
[0048] The spacer 140 _ 2 of the present embodiment is formed, unlike the spacer 140 of the first embodiment illustrated in FIG. 2 , such that the length L 1 of the groove in a corner portion is less than the length L 2 of the groove 141 in a middle side portion. Even if the spacer 140 _ 2 is bonded to the heat spreader 150 and the wiring board 110 illustrated in FIG. 2 , the corner portions of the spacer 140 _ 2 are susceptible to peeling off. According to the spacer 140 _ 2 of the present embodiment, the length of the groove 141 is reduced as closer to a corner portion so that the contact area with the adhesive sheet 130 becomes larger, and thereby it is made possible to securely bond the corner portions to the heat spreader 150 and the wiring board 110 .
[0049] So far, the description of the second embodiment of the present invention has been completed, and a third embodiment thereof will be described. Since the third embodiment of the present invention has a similar structure as the first embodiment excepting the shape of the grooves provided in the spacer, like elements as those of the first embodiment will be given like reference symbols to omit the description thereof and only the differences from the first embodiment will be described.
[0050] FIG. 6 illustrates a spacer 140 _ 3 of the third embodiment of the present invention.
[0051] The spacer 140 _ 3 of the present embodiment is formed such that the grooves 141 in a corner portion P are radially provided at an angle with one another so as to intersect at the inside of the opening 142 . In the spacer 140 _ 3 illustrated in FIG. 6 , the corner portion P, which is susceptible to peeling off even when bonded, is formed such that the spacing between grooves 141 becomes larger as closer to the outer peripheral side, and the contact area with the adhesive sheet 130 becomes larger. Thus, by providing radial grooves 141 in the corner portions P of the spacer 140 _ 3 , it is also possible to prevent the squeeze-out of the thermosetting adhesive material while maintain the bonding accuracy of the spacer 140 _ 3 .
[0052] So far, the description of the third embodiment of the present invention has been completed, and a fourth embodiment thereof will be described. Since the third embodiment of the present invention also has a similar structure as the first embodiment excepting that cut-outs instead of the grooves are provided in the spacer, like elements as those of the first embodiment will be given like reference symbols to omit the description thereof and only the differences from the first embodiment will be described.
[0053] FIG. 7 illustrates a spacer 160 in the fourth embodiment of the present invention.
[0054] The spacer 160 of the present embodiment is, unlike the spacer 140 of the first embodiment illustrated in FIG. 2 , formed with cut-outs 161 instead of the grooves 141 in the outer peripheral section. Moreover, the spacer 160 of the present embodiment is formed such that the length L 1 of the cut-out 161 in a corner portion is less than the length L 2 of the cut-out 161 in a middle side portion, intending to maintain the bonding accuracy of the spacer 160 .
[0055] FIG. 8 illustrates a manufacturing method of a semiconductor component 101 to which the spacer illustrated in FIG. 7 is applied.
[0056] Similarly to the manufacturing method of the semiconductor component 101 of the first embodiment illustrated in FIG. 4 , the present embodiment also has a structure such that on the wiring board 110 , there are disposed a first adhesive sheet 130 , a spacer 160 , and a second adhesive sheet 130 in this order, and the semiconductor element 122 provided with the I/O terminals 121 , and the joining member 123 are successively disposed inside the respective openings 131 and 162 of the adhesive sheet 130 and the spacer 160 (step S 21 of FIG. 8 ).
[0057] Next, the heat spreader 150 is overlaid to form an unbonded semiconductor component 101 ′. In step S 22 — a of FIG. 8 , a section taken across near the center of the unbonded semiconductor component 101 ′ is illustrated, and in step S 22 — b of FIG. 8 , a sectional view taken across the peripheral portion of the unbonded semiconductor component 101 ′ is illustrated. In the present embodiment, cut-outs 161 are provided in the spacer 160 as illustrated in step S 22 — b.
[0058] Further, the unbonded semiconductor component 101 ′ is heated to melt the joining member 123 and the two adhesive sheets 130 (step S 23 of FIG. 8 ). As a result, the thermosetting adhesive material 132 resulting from the melting of the two adhesive sheets 130 is pushed out and filled into the cut-outs 161 of the spacer 160 . Step S 23 of pushing out the thermosetting adhesive material 132 into the cut-outs 161 corresponds to an example of “the step of filling the cut-outs with the thermosetting adhesive member” in the manufacturing method of the semiconductor component of the present embodiment.
[0059] When the cut-outs 161 are filled with the thermosetting adhesive material 132 , the unbonded semiconductor component 100 ′ is cooled down (step S 24 of FIG. 8 ). In the present embodiment, an excess part of the hardened thermosetting adhesive material 132 ′, which has not been used for bonding the spacer 160 with the heat spreader 150 and the wiring board 110 , has gotten into the cut-outs 161 of the spacer 160 . Thus, by providing the cut-outs 161 instead of grooves in the spacer 160 , it is possible to more efficiently accommodate the excess thermosetting adhesive material 132 ′.
[0060] So far, the description of the fourth embodiment of the present invention has been completed, and a fifth embodiment thereof will be described. Since the fifth embodiment of the present invention has a similar structure as the fourth embodiment of the present invention excepting the shape of the cut-outs provided in the spacer, like elements as those of the fourth embodiment will be given like reference symbols to omit the description thereof and only the differences from the fourth embodiment will be described.
[0061] FIG. 9 illustrates a spacer 160 _ 2 in the fifth embodiment of the present invention.
[0062] The spacer 160 _ 2 of the present embodiment is formed such that cut-outs 161 in a corner portion P are radially provided at an angle with one another so as to intersect at within the opening 162 . Since in the spacer 160 of the present embodiment, the contact area with the adhesive sheet 130 is larger in the corner portions P than in other portions, it is possible to achieve both the maintenance of the bonding accuracy and the prevention of the squeeze-out of the thermosetting adhesive material.
[0063] So far, the description of the fifth embodiment of the present invention has been completed, and a sixth embodiment thereof will be described. Since the sixth embodiment of the present invention has a similar structure as the first embodiment of the present invention excepting the shapes of the spacer and the adhesive sheet, like elements as those of the first embodiment will be given like reference symbols to omit the description thereof and only the differences from the first embodiment will be described.
[0064] FIG. 10 is an exploded perspective view of a semiconductor component 200 which is the sixth embodiment of the present invention.
[0065] Similarly to the semiconductor component 100 of the first embodiment illustrated in FIG. 2 , the semiconductor component 200 of the present embodiment is formed such that on the wiring board 110 , there are placed two adhesive sheets 180 , a spacer 170 , and a heat spreader 150 on top of one another, and a semiconductor section 129 is disposed inside the respective openings 181 and 171 provided in the adhesive sheet 180 and the spacer 170 . Moreover, unlike the semiconductor component 100 of the first embodiment, neither groove nor cut-out is provided in the spacer 170 and instead, cut-outs 182 are formed in the respective outer peripheral sections of the two adhesive sheets 180 .
[0066] When the adhesive sheet 180 illustrated in FIG. 10 is melted, an excess thermosetting adhesive material may spread over the portions of the cut-outs 182 of the adhesive sheet 180 . As a result of this, it is possible to securely bond the spacer 170 and to avoid the deficiency that the thermosetting adhesive member is squeezed out to the outer face of the semiconductor component 200 .
[0067] So far, the description of the sixth embodiment of the present invention has been completed, and a seventh embodiment thereof will be described. Since the seventh embodiment of the present invention has a similar structure as the sixth embodiment of the present invention excepting the shape of the cut-out of the adhesive sheet, only the differences from the sixth embodiment will be described.
[0068] FIG. 11 illustrates an adhesive sheet 180 _ 2 in the seventh embodiment of the present invention.
[0069] The adhesive sheet 180 _ 2 of the present embodiment is formed such that the length L 1 of the cut-out 182 of a corner portion is less than the length L 2 of the cut-out 182 of a middle side portion. Since, in the adhesive sheet 180 _ 2 of the present embodiment, the contact area between the adhesive sheet 180 _ 2 and the spacer 170 is larger in corner portions where spacer 170 is more susceptible to peeling off, it is possible to avoid the squeeze-out of the thermosetting adhesive material while maintaining the bonding accuracy of the spacer 170 .
[0070] So far, the description of the seventh embodiment of the present invention has been completed, and an eighth embodiment thereof will be described. Since the eighth embodiment of the present invention has a similar structure as the sixth embodiment of the present invention excepting the shape of the cut-out of the adhesive sheet, only the differences from the sixth embodiment will be described.
[0071] FIG. 12 illustrates an adhesive sheet 180 _ 3 in the eighth embodiment of the present invention.
[0072] Since the adhesive sheet 180 _ 3 of the present embodiment is formed such that the cut-outs 182 in a corner portion are radially provided at an angle with one another so as to intersect within the opening 181 , the contact area between the adhesive shut 180 - 3 and the space 170 becomes larger closer to the outer peripheral side where peeling off is more likely to take place. Thus, by providing radial cut-outs 182 in the corner portions P of the adhesive sheet 180 _ 3 , it is also possible to prevent the squeeze-out of the thermosetting adhesive material while maintaining the bonding accuracy of the spacer 170 .
[0073] So far, the description of the eighth embodiment of the present invention has been completed, and a ninth embodiment thereof will be described. Since the ninth embodiment of the present invention has a similar structure as the sixth embodiment excepting the shape of the spacer, only the differences from the sixth embodiment will be described.
[0074] FIG. 13 illustrates a semiconductor component 300 which is the ninth embodiment of the present invention.
[0075] FIG. 13A illustrates an exploded perspective view of the semiconductor component 300 of the present embodiment.
[0076] Similarly to the semiconductor component 200 of the sixth embodiment illustrated in FIG. 10 , the semiconductor component 300 of the present embodiment is formed such that cut-outs 182 are formed in an adhesive sheet 180 , and further cut-outs 142 are also formed in a spacer 140 . Moreover, two adhesive sheets 180 and spacer 140 are placed on top of one another with the respective cut-outs 182 and 142 being lined up.
[0077] FIG. 13B illustrates a sectional view of the outer peripheral section of the semiconductor component 300 .
[0078] When the adhesive sheet 180 illustrated in FIG. 13B is melt, an excess thermosetting adhesive material, which has been left without been used for the bonding of the spacer 170 with the heat spreader 150 and the wiring board 110 , may spread over the portion of the cut-outs 182 of the adhesive sheet 180 , and also may be pushed out into the cut-outs 142 of the spacer 170 . For this reason, even when the adhesive sheet 180 has a larger thickness, it is possible to securely avoid the squeeze-out of the thermosetting adhesive material.
[0079] Here it is noted that although description has been made on the cases in which grooves are provided in both the upper and lower faces of the spacer, the support member according to the present invention may be one in which grooves are provided only in one face.
[0080] Further, although, in the above, description has been made on a case in which cut-outs are provided in each of the spacer and the adhesive sheet, the support member and the adhesive member according to the present invention may be formed such that cut-outs are provided in one of the members and grooves are provided in the other.
[0081] Although description has been made on the case in which grooves are provided only in the outer peripheral section of the spacer, the support member according to the present invention may be formed such that grooves are provided in the entire upper face.
[0082] As so far described, according to the present invention, it is possible to provide a semiconductor component in which the deficiencies due to the squeeze-out of the adhesive member are mitigated.
[0083] All examples and conditional language recited herein are intended for pedagogical purposes to aid the reader in understanding the invention and the concepts contributed by the inventor to furthering the art, and are to be construed as being without limitation to such specifically recited examples and conditions, nor does the organization of such examples in the specification relate to a showing of the superiority and inferiority of the invention. Although the embodiments of the present invention has been described in detail, it should be understood that the various changes, substitutions, and alterations could be made hereto without departing from the spirit and scope of the invention.
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A semiconductor component includes a semiconductor element that has a plurality of signals, a wiring board that is disposed below the semiconductor element and that draws the plurality of signals of the semiconductor element, a heat conduction member that dissipates heat generated by the semiconductor element, a joining member that is disposed between the semiconductor element and the heat conduction member and that joins the heat conduction member to the semiconductor element, a support member formed with an opening so as to surround the semiconductor element that supports the heat conduction member, a first adhesive member that is disposed between the support member and the wiring board to bond the support member with the wiring board and a second adhesive member that is disposed between the support member and the heat conduction member to bond the support member with the heat conduction member.
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REFERENCE TO RELATED APPLICATIONS
This is a continuation-in-part of U.S. Patent Application Ser. No. 60/602,579 filed Aug. 18, 2004.
TECHNICAL FIELD
This invention relates to ion exchange fuel cells.
BACKGROUND OF THE INVENTION
The performance of conventional lithium battery systems is limited because they must include cathode materials that constrain the energy storage capacity of these cells on a per unit volume and mass basis. Typically, cathode materials include inorganic or organic compounds such as manganese oxide, vanadium oxide, lithium cobalt oxide and (CF) n . Although lithium has the highest columbic capacity, most available cathode materials have specific capacities that are less than 200 mAh/g. Metal/oxygen batteries offer high performance because cathode active materials are not stored in the battery. Oxygen from the environment is reduce at a catalytic air electrode surface forming either an oxide or peroxide ion that then reacts with cationic species in the electrolyte. The oxygen content of the battery accumulates as the battery discharges.
Accordingly, it is seen that a need exists for a system that provides regenerative energy source without a very large mass. It is to the provision of such therefore that the present invention is primarily directed.
SUMMARY OF THE INVENTION
In a preferred form of the invention a regenerative ion exchange fuel cell having an anode, a metal ion conductor coupled to the anode, an aqueous electrolyte solution positioned adjacent the metal ion conductor, a proton conductor mounted adjacent the aqueous electrolyte solution opposite the metal ion conductor, a cathode positioned adjacent the proton conductor opposite the aqueous electrolyte solution, and a cathode current collector associated with the cathode.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic view of a regenerative ion exchange fuel cell embodying principles of the invention in a preferred form, shown during discharge phase.
FIG. 2 is a schematic view of the regenerative ion exchange fuel cell of FIG. 1 shown in a recharge phase.
FIG. 3 is a schematic view of the regenerative ion exchange fuel cell in another preferred embodiment.
FIG. 4 is a schematic view of the regenerative ion exchange fuel cell in yet another preferred embodiment.
FIG. 5 is an exploded view of the regenerative ion exchange fuel cell of FIG. 4 .
FIG. 6 is a schematic view of a regenerative ion exchange fuel cell in yet another preferred embodiment.
FIG. 7 is a schematic view of a regenerative ion exchange fuel cell shown in an oxygen tank.
DETAILED DESCRIPTION
The explosive energy potential produced by this cell in the form of accumulated hydrogen and oxygen suggests that a more optimal cell design may be possible that could have even higher energy storage potential. One could use a fuel cell to generate electrical energy using the hydrogen and oxygen; however, the associated tanks and gas transport requirements would have an overall degrading impact on energy density. However, if this energy can be harvested efficiently, it represents a further energy gain in the basic battery system. FIGS. 1 and 2 suggest the general structure of such a combined cell, indicating the required layers and transport processes for a functional cell. The proposed system shown in FIGS. 1 and 2 indicate how the energy of the hydrogen can be simultaneously harvested resulting in a safe reversible lithium battery with high energy density. The actual cell may require additional layers for material compatibility or structural reasons.
The key to this new approach is a shared ion exchange medium, possibly aqueous, but not limited to water, which allows a transfer of charge carrier species from that of Li + to H + Lithium metal at the anode converts to lithium ions (Li + ) and electrons. The lithium ions are transported through a lithium electrolyte material to react in an aqueous intermediary ion exchange electrolyte resulting in the formation of LiOH and protons as shown previously in Equation 1. The resulting protons are transported from the ion exchange medium and on through a third electrolyte layer (proton conducing only) to react with oxygen producing water and additional energy. The overall by-products of this process are LiOH and water. To reverse the reaction, an applied voltage splits water at the cathode of the proton-conducting electrolyte. Protons transported to the intermediary electrolyte cause polarization at the surface of the lithium electrolyte resulting in the dissociation of LiOH from solution with lithium ions being driven back to the anode.
Dependent upon the intermediate species formed, the cell reactions may include the following reactions:
Li( s )=>Li + +( aq )+ e − −3.05 Volts
2H 2 O( l )+2 e − =>H 2 ( g )+20H − ( aq ) −0.83 Volts
2H + +2 e − =>H 2 ( g ) 0.00 Volts
O 2 ( g )=4H + ( aq )+4 e − =>2H 2 O( l ) 1.23 Volts
as observed by Visco 5 et al., who attained a voltage of 3.05 volts for the lithium water cell alone when the water was saturated with LiOH or LiCl/HCl, indicating the ability to bypass the losses in the H 2 O to OH+H + reaction. Additionally, the charge transfer to protons and harvesting of protons to create an additional 1.23 volts yields an overall cell voltage of up to 4.28 volts.
A practical approach for constructing the proposed cell is illustrated in FIG. 3 . Ridged substrates are used to provide structural support for the thin, solid Li + and H + electrolyte barrier layers. The H + electrolyte glass is on the order of 1 to 5 um thick and therefore does not have sufficient thickness for use as a stand alone film. This application requires the electrolyte to be a barrier to the electrolyte solution to prevent vaporization/dry out, and prevent lithium ion transport to the surface of the cathode. Lithium-oxygen reactions at the cathodic surface of the proton membrane would form solid Li 2 O, which could act as a barrier to oxygen limiting further reactions, thereby shutting down the cell. A catalyst layer with an embedded current collector will be applied to the surface of the proton conductive layer to form the cathode side of a fuel cell type membrane electrode assembly (MEA). The outer surface of the MEA is to be covered by an oxygen permeable hydroscopic polymer material such as that used for extended wear contact lenses. This coating will retain water produced during operation of the cell at the location where it is generated and later required for regeneration. With this approach, separate plumbing associated with a complex water management system is not necessary.
On the other side, a Li + electrolyte, that conducts only lithium ions and acts as a protective barrier, prevents the aqueous electrolyte from contacting and reacting with the lithium metal anode. Considering the lithium ion conductivity of the glass selected for this application, Li 1.3 (Sc 0.3 Ti 1.7 ) (PO 4 ) 3 , it is anticipated that this layer will be 10 to S0 um thick. A 0.1 to 1.0 um coating of LIPON electrolyte will be applied between the glass barrier and the lithium anode. The LiPON coating is necessary because direct contact between lithium and the selected glass barrier material would otherwise form an unstable interface.
Scalability of Lithium Air Batteries
Table 3 shows representative battery requirements for a High Altitude Airship. Considering a lO, 600 lb weight allocation for the battery and an energy storage requirement of 675 kWhr, the specific energy is 140 Wh/kg, which is consistent with state of the art lithium polymer battery technology. The technology proposed herein will eventually provide this level of energy storage capability with close to an order of magnitude reduction in weight. An additional goal is to provide a battery that will be capable of extended stand by shelf life and at least 300 charge discharge cycles at 80 percent retention of original capacity.
TABLE 3 Representative Performance Parameters for HAA Battery External Temperature −80° C. Cycle Life 300 Operational Periods 10 to 16 his Storage Life 1 yr Operating Life 2 yrs Depth of Discharge Up to 90% Capability (DoD) Max Weight 6500 lbs
Energy Capacity 675 kW-hrs
Current Capacity 2.5 kAh
Operating Voltage=270 VDC
Power Under Standby Operations 12.5 kW
Nominal Operating Power 37.5 kW
Peak Operating Power 62.5 kW
Peak Out Put Current 231 A
The performance objectives will be achieved using a modular battery configuration. As presented in Table 4, each module will be self-contained including oxygen. The design is based on the use of 83 cells configured as panels within a given module. The module will have a total open circuit voltage of 300V and 270V under load. Calculations are included below which show that the described structure would be able to meet electrical output power requirements in terms of IR losses associated with current collectors and busses within the battery. The battery modules will be electrically connected in parallel for a total peak output capability of 54 kW (@200 A). Oxygen diffusion within the cathode and ionic conductivity polarization losses will be addressed in detail over the course of the proposed project.
The proposed design is based on the use of 25 battery modules connected in parallel. Each of the 25 modules will be capable of delivering 1OA with an energy storage capacity of 27 kWhr. The total energy storage capability for the 25 modules is 675 kWh. A cell voltage allocation of 1V is assigned for internal battery losses under peak operating current conditions. Given a cell open circuit voltage of 4.25V, the 1V internal loss allocation results in a net cell output voltage of 3.25V at peak current. The internal impedance loss allocation is distributed as follows: 1) 0.4V for H 2 —O 2 cathode activation polarization, and 2) 0.6V for internal resistance and current collector buss losses. The required total peak current of 231 A and the use of 25 modules suggest that each module should be capable of supplying 9.25 A. An output requirement of 10 A is assumed for each module. To attain the desired 270V operation per module from cells with an anticipated output of 3.25V under peak load conditions suggests that 83 cells (270V/3.25 V/cell) connected in series within each module will be required to achieve the required operating voltage. The open circuit voltage for the 83 cells connected is 352V (83 cells×4.25V). To achieve the desired 27 kWh output, each cell must store 1OOAhr (27 kWh/270V).
Given that a nominal current density for rechargeable battery cells is in the range of 10 mA/cm 2 , the 10 A per cell requirement can be achieved using a cell area of 1000 cm 2 (10 A/10 mA/cm 2 ). Given a cell storage capacity of 1OOAhr and a surface area of 1000 cm 2 , the required storage capacity is 0.1 Ah/cm 2 (1OOAhr/1000 cm 2 ). A lithium thickness of 500 um is required to achieve this storage density.
The battery module performance specifications presented in Tables 3 and 4 are based on the energy density calculation for the cell illustrated in FIG. 4 . No design consideration is given for external power bus requirements and the conceptual design does not address mass allocations for the pressure containment vessels. The vessel weight required for O 2 containment would ultimately depend on operating pressure. Estimates below are based on a preliminary operating pressure of 200 psi.
TABLE 4
Total capacity for proposed HAA
Number of Battery Modules
25 modules
Individual Module Specifications:
Peak Current Per Module
10
A
Open Circuit Voltage
352
VDC
Voltage at 10A
270
VDC
Peak Power
2.5
kW
Energy Storage Capacity
27
kWh
02 Containment Pressure
200
psi
02 Volume @ 200 psi
0.18
m 3 (6 ft 3 )
Equation 7 gives the molecular balance reactions for the proposed ion exchange cell. In the stated reaction, one mole of water is required in the exchange electrolyte for each mole of lithium. LiOH formation in the solution should result in precipitation, which is anticipated to tie up another mole of water as LiOH*H 2 O. In addition, the reaction of protons with oxygen at the cathodic side of the proton electrolyte will generate a further ½ mole of water per mole of lithium. The total water required then is 2.5 moles per mole of lithium or approximately 6.5 g of water per gram of lithium. Similarly, this yields a volume of 3.5 cc of water per cubic centimeter of lithium. Assuming that excess lithium is required in the anode for electrical continuity, similar excess quantities of water would be available for maintaining the aqueous electrolyte throughout battery cycling.
4Li=4H 2 O→4Li + +4H + +4 e − →4H + +O 2 +4 e − =>2H 2 O E°=4.25V
FIG. 4 shows the targeted configuration for a HAA lithium oxygen cell. The cell functions as a lithium/hydrogen ion exchange fuel cell. It uses a lithium metal anode protected by a glass barrier electrolyte. The electrolyte barrier prevents moisture from attacking the lithium while at the same time providing for lithium ion transport. The cell includes an aqueous lithium/hydrogen ion exchange layer. As lithium ions enter this layer during discharge, they displace hydrogen ions from water molecules elevating the level of LiOH in the solution. The displaced hydrogen ions are conducted through the proton conductive membrane to the cathode current collector where it gains an electron and reacts with oxygen forming water at the exterior surface of the cell. The data included in FIG. 4 indicates that a power density of 1445 Wh/l can be attained with a specific energy of 1416.4 Wh/kg. Cells are to be constructed into panels as shown in FIG. 5 .
Electrical losses anticipated in individual components of such a system are shown in FIG. 6 . These losses are calculated based on the anticipated thickness and resistivity for each system component. The total voltage drop anticipated is 0.7V during cell operation. This data along with the data from FIG. 4 were used as a basis for estimating the size, surface area, power density and weight requirement for the individual cell panels of a large scale HAA battery. These values are presented in Table 5 and show the power density for modules including associated oxygen/water as 1.01 kWh/kg. FIG. 7 represents a schematic for the assembly of panels into the battery module.
While this invention has been described in detail with particular reference to the preferred embodiments thereof, it should be understood that many modifications, additions and deletions, in addition to those expressly recited, may be made thereto without departure from the spirit and scope of invention as set forth in the following claims.
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A regenerative ion exchange fuel cell having an anode, a metal ion conductor coupled to the anode, an aqueous electrolyte solution positioned adjacent the metal ion conductor, a proton conductor mounted adjacent the aqueous electrolyte solution opposite the metal ion conductor, a cathode positioned adjacent the proton conductor opposite the aqueous electrolyte solution, and a cathode current collector associated with the cathode.
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The present application is a Continuation of U.S. patent application Ser. No. 14/807,064, filed on Jul. 23, 2015 and claims priority thereto under 35 U.S.C. 120. The disclosure of the above-referenced parent U.S. patent application is incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is related to integrated circuits incorporating digital circuits, such as logic, memory and latch blocks, and more specifically to techniques for dynamically boosting the voltage of a virtual power supply rail prior to and during an evaluation time of a digital circuit block.
2. Description of Related Art
Static and Dynamic digital circuits are used in memories and logic devices to provide high frequency operation with a minimum of die area for performing logical operations and providing storage functionality. Both synchronous static and dynamic digital circuits have controlled evaluation times in that the operation of the circuit before and during a time at which an output value of the digital circuit block evaluates or changes state, i.e., is determined from the input logic, latch input or storage cell value is used advantageously to reduce circuit complexity and/or power consumption.
Groups of digital circuits, which are sometimes referred to as “macros”, have been power-managed in existing circuits to reduce power consumption, except during certain intervals of time in which power supply current is drawn to provide a read or write of a storage cell value, or the determination of a logic combination. For example, a dynamic logic circuit may draw no current, or have very low leakage current levels, except when a signal node is pre-charged with a voltage and then selectively discharged to produce the combinatorial output or storage cell value. A static logic circuit or storage cell only draws significant current when a state change occurs.
Digital circuits have been implemented that include virtual power supply nodes that can be disabled or set to a reduced voltage when the logic circuits are not evaluating, or multiple power supplies can be used to supply higher voltages to critical circuits. In some implementations, circuits have been provided that boost the power supply voltage supplied to the digital circuits during their evaluation phase to reduce the static power supply voltage by including a boost transistor. Such boosting reduces overall power supply voltage requirements. However, the energy expended in changing the voltage of the virtual power supply node voltage offsets any advantage gained, since the virtual power supply nodes typically have large shunt capacitance, i.e., capacitance between the virtual power supply node and the corresponding power supply return, due to the large numbers of devices that are connected to the virtual power supply nodes.
It would therefore be desirable to provide a virtual power supply circuit for synchronous digital circuits, and other circuits having a predictable evaluate time, that provides for reduction in overall power supply voltage and energy consumption.
BRIEF SUMMARY OF THE INVENTION
The invention is embodied in a method of operation of a virtual power supply rail booster circuit that provides reduced power consumption and supply voltage requirements.
The booster circuit includes a first transistor that couples a dynamic internal power supply node of a group of digital circuits to a static power supply that supplies a substantially constant power supply voltage to the group of digital circuits. The first transistor is disabled in response to a first phase of a boost clock that is synchronized with a functional clock of the group of digital circuits that controls evaluation for dynamic digital circuits and/or state changes for static digital circuits. The booster circuit also includes an inductor coupled to the dynamic internal power supply node for resonating with at least one capacitance coupled to the dynamic internal power supply node, which may be just the capacitance of the circuits connected to the dynamic internal power supply node. When the first transistor is disabled according to a second phase of the boost clock that corresponds to an evaluation time of the group of digital circuits, a voltage of the dynamic internal power supply node increases in magnitude to a value substantially greater than a magnitude of the power supply voltage of the by the inductor resonating with the capacitance couple to the dynamic internal power supply node. The energy used to raise the voltage of the dynamic internal power supply node is stored by the inductor and recycled. A second boost transistor, which may be a FINFET device, may be controlled by another phase of the clock to couple a rising edge of the clock to start the resonant boost. The other phase of the clock may be a delayed version of the boost clock signal.
In another aspect, the booster circuit may include multiple boost transistors that are controlled by different phases of the clock so that the resonant boost circuit is successively stimulated to increase the amount of voltage rise at the dynamic internal power supply node, and in some embodiments, multiple inductors may be coupled through multiple boost devices to the dynamic internal power supply node and stimulated in succession to increase the amount of voltage rise.
The foregoing and other objectives, features, and advantages of the invention will be apparent from the following, more particular, description of the preferred embodiment of the invention, as illustrated in the accompanying drawings.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
The novel features believed characteristic of the invention are set forth in the appended claims. The invention itself, however, as well as a preferred mode of use, further objectives, and advantages thereof, will best be understood by reference to the following detailed description of the invention when read in conjunction with the accompanying Figures, wherein like reference numerals indicate like components, and:
FIG. 1 is a block diagram illustrating an exemplary integrated circuit 10 .
FIG. 2 is a schematic diagram of a virtual supply boost circuit 20 A according to a first example that may be used in the integrated circuit of FIG. 1 .
FIG. 3A is a waveform diagram illustrating signals within virtual power supply/boost circuit 20 A of FIG. 2 , and FIG. 3B is a waveform diagram illustrating signals within virtual power supply/boost circuit 20 B of FIG. 4 .
FIG. 4 is a schematic diagram of a virtual supply boost circuit 20 B according to a second example that may be used in the integrated circuit of FIG. 1 .
FIG. 5 is a schematic diagram of a virtual supply boost circuit 20 C according to a third example that may be used in the integrated circuit of FIG. 1 .
FIG. 6 is a schematic diagram of a virtual supply boost circuit 20 D according to a fourth example that may be used in the integrated circuit of FIG. 1 .
FIG. 7 is a schematic diagram of a virtual supply boost circuit 20 E according to a fifth example that may be used in the integrated circuit of FIG. 1 .
FIG. 8 is a schematic diagram of a virtual supply boost circuit 20 F according to a sixth example that may be used in the integrated circuit of FIG. 1 .
FIG. 9 is a schematic diagram of a virtual supply boost circuit 20 G according to a seventh example that may be used in the integrated circuit of FIG. 1 .
FIG. 10 is a schematic diagram of a virtual supply boost circuit 20 H according to a eighth example that may be used in the integrated circuit of FIG. 1 .
FIG. 11 is a flow diagram of a design process that can be used to fabricate, manufacture and test the integrated circuit of FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to devices containing digital circuits such as memory devices, processors and other circuits in which low-voltage and low power operation are desirable. Instead of a typical static power supply, virtual power supply rails are used to reduce the power supply rail voltage, and thus the power consumption due to leakage when the circuits in a given “macro” or circuit block are not active. In the exemplary device disclosed herein, the static power supply voltage can be further reduced, as one or more techniques for dynamically boosting the virtual power supply rail voltage are included, which extend to the use of an inductor to form a resonant circuit and/or sequencing multiple resonant or non-resonant boost circuits to increase the amount of available voltage boost. In the resonant boost configurations, the energy used to boost the virtual power supply rail voltage is stored and recycled when the voltage decreases after the boost interval, which has a timing related to a clock that controls evaluation in the digital circuit. The clock may be a clock that controls pre-charge and evaluation cycles in a dynamic digital circuit or a clock that time state changes in a static digital circuit, which is also considered an evaluation as the term is used herein.
With reference now to the figures, and in particular with reference to FIG. 1 , an exemplary integrated circuit (IC) 10 is shown, which may represent a processor integrated circuit, a memory device, or another very-large scale integrated circuit (VLSI) that contains logic and storage. Within IC 10 , a digital circuit group 11 (or “macro”) contains exemplary logic gates 12 , latches 14 and memory 16 , all of which are provided operating power from a dynamic internal power supply node 5 that has a voltage V DDV that may be varied dynamically to reduce power consumption when digital circuit group 11 is not operating or, in the case of the present example, when the circuits in digital circuit group 11 are not being readied to generate a state change. The state changes in digital circuit group 11 are synchronized by one or more clock signals provided from a clock generator 18 . Exemplary clock generator 18 includes a phase-lock loop (PLL) 24 that generates a high-frequency clock, and a divider logic 26 that generates various clock phases and control signals from the high-frequency clock, including a clock signal clk that is provided to an input of a programmable timing block 22 that generates clock signals clk 0 , clk 1 , clk 2 provided to digital circuit group 11 , and a boost clock boost that is provided to a virtual power supply/boost circuit 20 within digital circuit group 11 .
Techniques included in virtual power supply/boost circuit 20 generate peak boosted values of voltage V DDV on dynamic internal power supply node 5 that are substantially greater than a static power supply voltage V DD supplied to the input of virtual power supply/boost circuit 20 and that operates other circuits within integrated circuit 10 , so that the value of static power supply voltage V DD can be reduced, while still meeting performance requirements within digital circuit group 11 . Particular techniques to provide the boosted voltage V DDV are described below with reference to FIGS. 2-9 . In general, virtual power supply/boost circuit 20 generates voltage V DDV to align a boosted portion value of output voltage V DDV with particular times for which the value of the voltage supplied to exemplary logic gates 12 , latches 14 and memory 16 is the most critical for performance, which allows the static value of a static power supply voltage V DD that supplies virtual power supply/boost circuit 20 to be reduced. Generally, the boosted portion of output voltage V DDV is placed at the set-up interval before a static or dynamic evaluation is commenced by clock signals clk 0 , clk 1 , clk 2 . Programmable timing block 22 includes tapped delay lines 28 formed by buffers/inverters and selectors so that the timing of clk 0 , clk 1 , clk 2 and boost clock boost are optimized for instant frequency, voltage and other environmental and circuit conditions. However, integrated circuit 10 as illustrated in FIG. 1 is only an example and fixed clock buffer chains can be employed as an alternative.
Referring now to FIG. 2 , a first example of a virtual power supply/boost circuit 20 A that may be used to implement virtual power supply/boost circuit 20 of integrated circuit 10 of FIG. 1 is shown. Virtual power supply/boost circuit 20 A includes a first transistor P 1 that clamps output virtual power supply voltage V DDV at the value of static power supply voltage V DD when boost clock boost is de-asserted, i.e., in the low voltage state in the example. Virtual power supply/boost circuit 20 A also includes a second transistor, boost transistor N 1 , which has a body voltage stabilized initially at the value of static power supply voltage V DD as input clock signal boost is de-asserted. In an alternative embodiment that may be integrated with any of the embodiments shown herein, boost clock boost can be provided to the gate terminal of boost transistor N 1 as described above, but the gate terminal of transistor P 1 can be driven with a signal that is set to a state that disables transistor P 1 when a control signal/sleep is asserted or when boost clock boost is active as provided by optional logical-NAND gate 3 . By providing separate signals to control the gate terminals of transistors P 1 and N 1 , a suspended operating mode can be provided, which reduces leakage current though virtual power supply/boost circuit 20 A.
During operation of virtual power supply/boost circuit 20 A, the rising edge of boost clock boost is capacitively coupled through the gate of boost transistor N 1 to a terminal of an inductor L 1 that couples first transistor P 1 and boost transistor N 1 to dynamic internal power supply node 5 as boost transistor N 1 turns on. Since the current through inductor L 1 is zero before the rising edge of boost clock boost and since the body of boost transistor N 1 is at the value of static power supply voltage V DD , when the rising edge of boost clock boost is coupled through inductor L 1 to the dynamic internal power supply node 5 , a rapid increase in current through inductor L 1 causes dynamic internal power supply node voltage V DDV to rise with a waveshape controlled by the series resonant frequency of inductor L 1 combined with the capacitance C CKT of all of the circuits connected to dynamic internal power supply node 5 and any additional capacitance C 1 that may optionally be included in virtual power supply/boost circuit 20 A. However, since boost transistor N 1 is also turning on, and since shunt capacitance C CKT is also in parallel with leakage and active currents of the devices connected to the dynamic internal power supply node 5 , the resonant behavior of inductor L 1 with the total capacitance is damped and the conduction of boost transistor N 1 works to prevent dynamic internal power supply node voltage V DDV from falling much below static power supply voltage V DD . In general, internal power supply node voltage V DDV should not fall below V DD −V T , where V T is the threshold voltage of boost transistor N 1 . To prevent internal power supply node voltage V DDV from falling below a certain voltage level in any of the embodiments depicted herein, an optional diode D 1 may be added between dynamic internal power supply node voltage V DDV and static power supply voltage V DD as illustrated, to prevent internal power supply node voltage V DDV from falling below V DD −V F , where V F is the forward voltage drop of diode D 1 . In the embodiments depicted herein, boost transistor N 1 may be a FinFET device, which has a large gate to body capacitive coupling and is advantageous for such applications.
Referring now to FIG. 3A , waveforms within virtual power supply/boost circuit 20 A are shown. At time t 0 , boost clock boost rises, turning transistor P 1 off, which causes the voltage across inductor L 1 to rise. Boost clock boost also couples through the gate of boost transistor N 1 to the source of boost transistor N 1 , further contributing to the voltage rise of dynamic internal power supply node voltage V DDV . When boost clock boost is asserted on a next cycle at time t 1 , because inductor L 1 has decoupled dynamic internal power supply node voltage V DDV from the source of transistor P 1 , the source terminal of transistor P 1 and the source of boost transistor N 1 will be clamped to static power supply voltage V DD , while dynamic internal power supply node voltage V DDV continues to follow a sinusoidal shape that peaks just prior to the next de-assertion of boost clock signal boost. As seen in FIG. 3A when boost clock boost is de-asserted at time t 2 , dynamic internal power supply node voltage V DDV is substantially greater than static power supply voltage V DD and has been for an interval sufficient to ensure set-up times for the dynamic circuits that evaluate when boost clock boost is de-asserted. As an example, a digital circuit clock dclk is shown, which controls an evaluation of a circuit block via a falling edge. An example set-up interval t SU is shown to illustrate how the timing of boost clock boost is controlled with respect to another clock that controls digital circuit state evaluation (including memory stores or reads) so that dynamic internal power supply node voltage V DDV has a boosted value during a critical timing period during which the boosted voltage improves performance over performance that would be achieved at the lower value of static power supply voltage V DD , i.e. without boost circuit 20 A. Not only does virtual power supply/boost circuit 20 A provide a timed increase in dynamic internal power supply node voltage V DDV , but the energy required to produce the increase, which is substantial due to the large shunt capacitance C SHUNT of all of the devices connected to dynamic internal power supply node 5 , is stored in inductor L 1 during the time before the assertion of boost clock boost and used to aid in producing the next peak of dynamic internal power supply node voltage V DDV prior to the next de-assertion of boost clock boost, i.e. the next evaluation.
Referring now to FIG. 4 , a second example of a virtual power supply/boost circuit 20 B that may be alternatively used to implement virtual power supply/boost circuit 20 of integrated circuit 10 of FIG. 1 is shown. Virtual power supply/boost circuit 20 B is similar to virtual power supply/boost circuit 20 A of FIG. 2 , so only differences between virtual power supply/boost circuit 20 B and virtual power supply/boost circuit 20 A will be described below. In virtual power supply/boost circuit 20 B, a clock buffer B 1 is shown that isolates the gate of boost transistor N 1 and transistor P 1 from boost clock boost. Buffer B 1 will generally be present in other implementations of virtual power supply/boost circuit 20 B, such as in virtual power supply/boost circuit 20 A of FIG. 1 , but in the instant virtual power supply/boost circuit 20 B, a capacitor C 2 is included to couple boost clock boost to dynamic internal power supply node 5 , so that the rising edge of boost clock boost imposes a transient of greater magnitude on dynamic internal power supply node voltage V DDV . FIG. 3B shows a simulation result for virtual power supply/boost circuit 20 B, in which a sharp increase dynamic internal power supply node voltage V DDV occurs at the rising edge of boost clock boost, i.e., at the beginning of the evaluation cycle.
Referring now to FIG. 5 , a third example of a virtual power supply/boost circuit 20 C that may be alternatively used to implement virtual power supply/boost circuit 20 of integrated circuit 10 of FIG. 1 is shown. Virtual power supply/boost circuit 20 C is similar to virtual power supply/boost circuit 20 A of FIG. 2 , so only differences between virtual power supply/boost circuit 20 C and virtual power supply/boost circuit 20 A will be described below. In virtual power supply/boost circuit 20 C, inductor L 1 couples the dynamic internal power supply node 5 to static power supply voltage V DD , so that a parallel resonant circuit is formed by inductor L 1 and the total capacitance provided by circuit capacitance C CIRCUIT and optional capacitance C 1 , with respect to dynamic internal power supply node 5 . The behavior of virtual power supply/boost circuit 20 C is very similar to the behavior of virtual power supply/boost circuit 20 A illustrated in FIG. 2 .
Referring now to FIG. 6 , a fourth example of a virtual power supply/boost circuit 20 D that may be alternatively used to implement virtual power supply/boost circuit 20 of integrated circuit 10 of FIG. 1 is shown. Virtual power supply/boost circuit 20 D is similar to virtual power supply/boost circuit 20 C of FIG. 5 , so only differences between virtual power supply/boost circuit 20 D and virtual power supply/boost circuit 20 C will be described below. In virtual power supply/boost circuit 20 C, inductor L 1 couples dynamic internal power supply node 5 to static power supply voltage V DD , so that a parallel resonant circuit is formed by inductor L 1 and the total capacitance provided by circuit capacitance C CKT and optional capacitance C 1 , with respect to dynamic internal power supply node 5 . However, no boost transistor is included, so the entire control of the behavior of dynamic internal power supply node voltage V DDV is controlled directly by transistor P 1 and the resonant behavior of inductor L 1 with the total capacitance provided by circuit capacitance C CKT and optional capacitance C 1 .
Referring now to FIG. 7 , a fifth example of a virtual power supply/boost circuit 20 E that may be alternatively used to implement virtual power supply/boost circuit 20 of integrated circuit 10 of FIG. 1 is shown. Virtual power supply/boost circuit 20 E is similar to virtual power supply/boost circuit 20 B of FIG. 4 , so only differences between virtual power supply/boost circuit 20 E and virtual power supply/boost circuit 20 B will be described below. In virtual power supply/boost circuit 20 E, inductor L 1 is coupled to the output of an inverter INV 1 and a capacitor C 3 is included to store energy after the time when a transistor P 3 is enabled by control signal enb 1 , by holding the voltage across capacitor C 3 when transistor P 3 turns off. Control signal enb 1 is generally in phase with boost clock boost, so that when boost clock boost rises and the output of inverter INV 1 falls, transistor P 3 turns off, holding the voltage across capacitor C 3 and storing energy. When boost clock boost falls, the output of inverter INV 1 rises and transistor P 3 turns on, further increasing the boost provided by inductor L 1 at the output of inverter INV 1 by applying the voltage across capacitor C 3 to the other terminal of inductor L 1 . Inductor L 1 resonates with the capacitance at the output of inverter INV 1 , which when control signal enb 1 is active, includes the capacitance of capacitor C 3 and which also includes the input capacitance of another inverter INV 2 which drives the gates capacitances of boost transistor N 1 and transistor P 1 . Since changes in output of inverter INV 1 are followed through inverter INV 2 at the gate of boost transistor N 1 , which is then followed at the source of boost transistor N 1 , the boosted waveform produced by the resonant circuit formed by inductor L 1 and the capacitance at the output of inverter INV 1 will be imposed on dynamic internal power supply node voltage V DDV .
Referring now to FIG. 8 , a sixth example of a virtual power supply/boost circuit 20 F that may be alternatively used to implement virtual power supply/boost circuit 20 of integrated circuit 10 of FIG. 1 is shown. Virtual power supply/boost circuit 20 F is similar to virtual power supply/boost circuit 20 E of FIG. 7 , so only differences between virtual power supply/boost circuit 20 F and virtual power supply/boost circuit 20 E will be described below. In virtual power supply/boost circuit 20 F, the circuit formed by inductor L 1 , capacitor C 3 and transistor N 3 is connected to the output of inverter INV 2 and a control signal enb 2 , which has a phase generally opposite that of boost clock boost, operates transistor P 3 , so that when the voltage at the output of inverter INV 2 rises, transistor P 3 is enabled, further increasing the boosted voltage.
Referring now to FIG. 9 , a seventh example of a virtual power supply/boost circuit 20 G that may be alternatively used to implement virtual power supply/boost circuit 20 of integrated circuit 10 of FIG. 1 is shown. Virtual power supply/boost circuit 20 G is similar to virtual power supply/boost circuit 20 A of FIG. 2 , so only differences between virtual power supply/boost circuit 20 A and virtual power supply/boost circuit 20 G will be described below. In virtual power supply/boost circuit 20 G, just as in the example virtual power supply/boost circuit 20 A of FIG. 2 , a boost is achieved by the coupling of the rising edge of boost clock boost through the gates of boost transistors N 1 and N 2 . In virtual power supply/boost circuit 20 G multiple boosts are provided by delaying boost clock boost through buffer B 1 and delay circuit DY 1 , which can be tuned by selection of delay circuit DY 1 to locate the peak of boosted dynamic internal power supply node voltage V DDV at the desired point in the evaluation cycle of boost clock boost.
Referring now to FIG. 10 , an eighth example of a virtual power supply/boost circuit 20 H that may be alternatively used to implement virtual power supply/boost circuit 20 of integrated circuit 10 of FIG. 1 is shown. Virtual power supply/boost circuit 20 H is similar to virtual power supply/boost circuit 20 G of FIG. 9 , so only differences between virtual power supply/boost circuit 20 H and virtual power supply/boost circuit 20 G will be described below. In virtual power supply/boost circuit 20 G, inductor L 1 is omitted, however, just as in the example virtual power supply/boost circuit 20 B of FIG. 4 , a boost is achieved by the coupling of the rising edge of boost clock boost through the gates of boost transistors N 1 and N 2 . As in virtual power supply/boost circuit 20 G of FIG. 9 , instant virtual power supply/boost circuit 20 H can be tuned by selection of delay circuit DY 1 to locate the peak of boosted dynamic internal power supply node voltage V DDV at the desired point in the evaluation cycle of boost clock boost.
It is understood that the above examples are not exhaustive, and other combinations and implementations in accordance with the examples above are possible, such as including additional boost circuits to any of the embodiments, including additional capacitive coupling of boost clock boost in the boost circuits that did not include such coupling and using multiple inductors to resonate both the dynamic internal power supply node 5 and buffered nodes such as in virtual power supply/boost circuit 20 E of FIG. 7 .
FIG. 11 shows a block diagram of an exemplary design flow 100 used for example, in semiconductor IC logic design, simulation, test, layout, and manufacture. Design flow 100 includes processes, machines and/or mechanisms for processing design structures or devices to generate logically or otherwise functionally equivalent representations of the design structures and/or devices described above and shown in FIGS. 1-2 and 4-10 . The design structures processed and/or generated by design flow 100 may be encoded on machine-readable transmission or storage media to include data and/or instructions that when executed or otherwise processed on a data processing system generate a logically, structurally, mechanically, or otherwise functionally equivalent representation of hardware components, circuits, devices, or systems. Machines include, but are not limited to, any machine used in an IC design process, such as designing, manufacturing, or simulating a circuit, component, device, or system. For example, machines may include: lithography machines, machines and/or equipment for generating masks (e.g. e-beam writers), computers or equipment for simulating design structures, any apparatus used in the manufacturing or test process, or any machines for programming functionally equivalent representations of the design structures into any medium (e.g. a machine for programming a programmable gate array).
Design flow 100 may vary depending on the type of representation being designed. For example, a design flow 100 for building an application specific IC (ASIC) may differ from a design flow 100 for designing a standard component or from a design flow 100 for instantiating the design into a programmable array, for example a programmable gate array (PGA) or a field programmable gate array (FPGA) offered by Altera Inc. or Xilinx, Inc.
FIG. 11 illustrates multiple such design structures including an input design structure 120 that is preferably processed by a design process 110 . Input design structure 120 may be a logical simulation design structure generated and processed by design process 110 to produce a logically equivalent functional representation of a hardware device. Input design structure 120 may also or alternatively comprise data and/or program instructions that when processed by design process 110 , generate a functional representation of the physical structure of a hardware device. Whether representing functional and/or structural design features, input design structure 120 may be generated using electronic computer-aided design (ECAD) such as implemented by a core developer/designer. When encoded on a machine-readable data transmission, gate array, or storage medium, input design structure 120 may be accessed and processed by one or more hardware and/or software modules within design process 110 to simulate or otherwise functionally represent an electronic component, circuit, electronic or logic module, apparatus, device, or system such as those shown in FIGS. 1-2 and 4-10 . As such, input design structure 120 may comprise files or other data structures including human and/or machine-readable source code, compiled structures, and computer-executable code structures that when processed by a design or simulation data processing system, functionally simulate or otherwise represent circuits or other levels of hardware logic design. Such data structures may include hardware-description language (HDL) design entities or other data structures conforming to and/or compatible with lower-level HDL design languages such as Verilog and VHDL, and/or higher level design languages such as C or C++.
Design process 110 preferably employs and incorporates hardware and/or software modules for synthesizing, translating, or otherwise processing a design/simulation functional equivalent of the components, circuits, devices, or logic structures shown in FIGS. 1-2 and 4-10 to generate a Netlist 180 which may contain design structures such as input design structure 120 . Netlist 180 may comprise, for example, compiled or otherwise processed data structures representing a list of wires, discrete components, logic gates, control circuits, 110 devices, models, etc. that describes the connections to other elements and circuits in an integrated circuit design. Netlist 180 may be synthesized using an iterative process in which netlist 180 is resynthesized one or more times depending on design specifications and parameters for the device. As with other design structure types described herein, netlist 180 may be recorded on a machine-readable data storage medium or programmed into a programmable gate array. The medium may be a non-volatile storage medium such as a magnetic or optical disk drive, a programmable gate array, a compact flash, or other flash memory. Additionally, or in the alternative, the medium may be a system or cache memory, buffer space, or electrically or optically conductive devices and materials on which data packets may be transmitted and intermediately stored via the Internet, or other networking suitable means.
Design process 110 may include hardware and software modules for processing a variety of input data structure types including Netlist 180 . Such data structure types may reside, for example, within library elements 130 and include a set of commonly used elements, circuits, and devices, including models, layouts, and symbolic representations, for a given manufacturing technology (e.g., different technology nodes, 32 nm, 45 nm, 90 nm, etc.). The data structure types may further include design specifications 140 , characterization data 150 , verification data 160 , design rules 170 , and test data files 185 which may include input test patterns, output test results, and other testing information. Design process 110 may further include, for example, standard mechanical design processes such as stress analysis, thermal analysis, mechanical event simulation, process simulation for operations such as casting, molding, and die press forming, etc. One of ordinary skill in the art of mechanical design can appreciate the extent of possible mechanical design tools and applications used in design process 110 without deviating from the scope and spirit of the invention. Design process 110 may also include modules for performing standard circuit design processes such as timing analysis, verification, design rule checking, place and route operations, etc.
Design process 110 employs and incorporates logic and physical design tools such as HDL compilers and simulation model build tools to process input design structure 120 together with some or all of the depicted supporting data structures along with any additional mechanical design or data (if applicable), to generate a second design structure 190 . Design structure 190 resides on a storage medium or programmable gate array in a data format used for the exchange of data of mechanical devices and structures (e.g. information stored in a IGES, DXF, Parasolid XT, JT, DRG, or any other suitable format for storing or rendering such mechanical design structures). Similar to input design structure 120 , design structure 190 preferably comprises one or more files, data structures, or other computer-encoded data or instructions that reside on transmission or data storage media and that when processed by an ECAD system generate a logically or otherwise functionally equivalent form of one or more of the embodiments of the invention shown in FIGS. 1-2 and 4-10 . In one embodiment, design structure 190 may comprise a compiled, executable HDL simulation model that functionally simulates the devices shown in FIGS. 1-2 and 4-10 .
Design structure 190 may also employ a data format used for the exchange of layout data of integrated circuits and/or symbolic data format (e.g. information stored in a GDSII (GDS2), GL1, OASIS, map files, or any other suitable format for storing such design data structures). Design structure 190 may comprise information such as, for example, symbolic data, map files, test data files, design content files, manufacturing data, layout parameters, wires, levels of metal, vias, shapes, data for routing through the manufacturing line, and any other data required by a manufacturer or other designer/developer to produce a device or structure as described above and shown in FIGS. 1-2 and 4-10 . Design structure 190 may then proceed to a stage 195 where, for example, design structure 190 : proceeds to tape-out, is released to manufacturing, is released to a mask house, is sent to another design house, is sent back to the customer, etc.
While the invention has been particularly shown and described with reference to the preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing and other changes in form, and details may be made therein without departing from the spirit and scope of the invention.
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A booster for a digital circuit block provides speed and reliability at lower static power supply voltages, reducing overall power consumption of the circuits. The booster includes a transistor that couples a dynamic power supply node to a static power supply and is disabled in response to a boost clock. An inductor and capacitance, which may be the block power supply shunt capacitance, coupled to the dynamic power supply resonates so that the voltage of the dynamic power supply increases in magnitude to a value greater the static power supply voltage. A boost transistor is included in some embodiments to couple an edge of the clock to the dynamic power supply, increasing the voltage rise. Another aspect of the booster includes multiple boost transistors controlled by different boost clock phases so that the resonant boost circuit is successively stimulated to increase the amount of voltage rise.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. Provisional Application No. 62/074,466 filed Nov. 3, 2014, the entire contents of which are hereby incorporated by reference.
BACKGROUND
[0002] Minimizing noise contributions of devices is important in RF circuits. This starts with the device design, and continues with the circuit design and system design. The parameters used to design or evaluate the noise performance of devices and circuits are called noise parameters. Noise parameters, used with s-parameters, provide low noise designers the information that they need.
[0003] Noise parameters typically include a set of values that describe how the noise figure of a device varies with impedance match. Note that in this document, impedance and gamma may be used interchangeably. As is known in the art, they contain equivalent information.
[0004] The noise parameters generally vary with measurement parameters such as frequency, bias, or temperature which are associated with a Device Under Test (DUT). The measurement parameters are independent stimulus values that setup specific measurement conditions. Device parameters comprise noise parameters and s-parameters, and are values that are typically measured for each desired set of measurement parameters. Gain parameters are derived from s-parameters, so may also be considered part of the device parameters.
[0005] There are different mathematical forms of the noise parameters, but generally include a set of four (4) scalar values. A commonly used set is:
[0006] 1. Fmin=minimum noise figure.
[0007] 2. Gamma_opt magnitude=magnitude of gamma_opt, the optimum source gamma that will produce Fmin
[0008] 3. Gamma_opt phase=phase of gamma_opt, the optimum source gamma that will produce Fmin
[0009] 4. rn=equivalent noise resistance, which determines how fast the noise figure will change as the source gamma moves away from Gamma_opt.
[0010] With this set of noise parameters, the noise figure of the device for any source gamma is then generally described by the equation
[0000] F=F min+4 *rn *|gamma_opt−gamma_ s|̂ 2/(|1+gamma_opt|̂2*(1−|gamma_ s|̂ 2))
[0011] Where gamma_s=source reflection coefficient seen by the DUT and F=Noise figure.
[0012] Other noise parameter forms include a correlation matrix (of which there are multiple configurations), and a set with forward and reverse noise parameters used by the National Institute for Standards and Technology (NIST). Generally, all of the noise parameter forms contain the same basic information. So if one form of the noise parameters is known, the noise parameters can be converted to any other form with a math formula.
[0013] Noise parameters are commonly determined by measuring the DUT under multiple impedance conditions, in a setup similar to that shown in FIG. 1 . The bias system is used to apply the desired DC voltages and currents to the DUT. Then, the input and output switches are set to connect the DUT to the network analyzer, and the s-parameters of the DUT are measured with the impedance tuner set to a Z0 or matched condition. Next, the input and output switches are set to connect the DUT to the noise source and the noise receiver. The impedance tuner is then sequentially set to multiple source impedances and the raw noise data is measured with the noise receiver for each impedance setting. The raw noise data is data that is read directly from the noise receiver and other equipment that may also be used in the setup. For example, bias voltages and currents may be read from the power supplies which provide the DUT bias, or they may be read with separate voltmeters or current meters.
[0014] An alternate setup for measurement of noise parameters is shown in FIG. 2 . Instead of using a noise source, a power meter is used to calibrate the noise receiver inside the network analyzer.
[0015] Another alternate setup for measurement of noise parameters is shown in FIG. 3 . Here, the RF source in the network analyzer is used to create a signal, and the receivers inside the network analyzer are setup to measure the signal to noise ratios of the DUT. The noise figure of the DUT is the signal to noise ratio on the input divided by the signal to noise ratio on the output. In a practical device the output signal to noise ratio will always be smaller than the input signal to noise ratio because of the noise added by the device.
[0016] The raw noise data may be collected using the standard method, which is to measure the raw noise data at every impedance at one measurement parameter value, such as frequency. When the data collection is finished for that measurement parameter value, the process is then repeated for other measurement parameter values.
[0017] The raw noise data may also be collected using the newer fast method, which is to set the source impedance tuner to one state, and measure the raw noise data for a sweep of a measurement parameter value, for example at multiple values of frequency. The impedance tuner is then set to another state, and the raw data is measured for another sweep of the measurement parameter value. This is repeated until the raw data has been collected for every desired source impedance. With this fast method, the measurement parameter sweep could also include different values of multiple measurement parameters, such as frequency, temperature, or bias values. See, U.S. Pat. No. 8,892,380, the entire contents of which are incorporated herein by this reference.
[0018] The bias values that may be used as swept measurement parameters depend on the type of device. For example, a device such as an FET will typically be biased with two voltages, one on the output terminal of the device, and one on the input terminal of the device. Either of these voltages may be used as a swept measurement parameter during the noise parameter measurements. The input or output current may also be used as a measurement parameter in some cases. Other devices may have additional control terminals, so additional voltage or currents may be used as measurement parameters in that case. The DC bias is typically provided by using power supplies connected to the DUT using bias tees.
[0019] After collecting the data for all the desired impedance settings, the noise parameters are determined by fitting the data to the noise equations. Since the noise parameters comprise four scalar values, a minimum of four measurements are required to determine the four values. However, the noise measurement is very sensitive and measurement equipment is never perfect, so normally some small errors are included in the data. To minimize the effect of these errors, the measurement is commonly done at more than four impedance settings. This results in over-determined data which can be reduced using Least Means Squares (LMS) methods which reduce sensitivity to some of the errors. But in any practical measurement setup, there are always some residual errors. If the measurement is done at multiple frequencies, for example, the error at one frequency will be different than the error at the next frequency. In fact, the error at adjacent frequencies could move in the opposite direction, so a plot vs. frequency will show some scatter, as shown in the plots of Fmin and gamma_opt vs. (i.e. as a function of) frequency in FIGS. 4 and 5 . The same thing can happen vs. other measurement parameters, such as a measurement vs. DC bias or temperature, for example.
[0020] This is a significant limitation of the prior art, that the noise parameter solution is determined independently for every measurement parameter value, such as frequency or bias for example. Because noise measurements are very sensitive, the noise parameters thus determined can show significant scatter vs. a measurement parameter such as frequency. However, this scatter of data comes from the measurement process, not from the device, so it is not a true representation of the device.
[0021] In the prior art, it is common to apply smoothing to plotted data after the noise parameter determination is complete, as shown in FIG. 6 . This is done because the general knowledge of the device operation indicates that the true data should be smooth. But FIG. 6 still shows that the real measured values of Fmin have scatter. This method of smoothing data tries to account for the known fact that Fmin should be smooth with frequency, but is still limited by the scatter and the bandwidth of the measurement. Often the scatter is not symmetrical, and then smoothing of the scattered data will give the wrong slope to the plot. Also, measurements over a narrow band will give a slope that is very sensitive to error.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Features and advantages of the disclosure will readily be appreciated by persons skilled in the art from the following detailed description when read in conjunction with the drawing wherein:
[0023] FIG. 1 is a schematic block diagram illustrating a typical noise parameter measurement setup using a noise source.
[0024] FIG. 2 is a schematic block diagram illustrating a typical noise parameter measurement setup using a power meter.
[0025] FIG. 3 is a schematic block diagram illustrating a typical noise parameter measurement setup using an RF source and receivers to measure the signal to noise ratios.
[0026] FIG. 4 is typical plot of measured Fmin vs. frequency which includes some scatter.
[0027] FIG. 5 is typical plot of measured gamma_opt vs. frequency which includes some scatter.
[0028] FIG. 6 is typical plot of measured Fmin vs. frequency with smoothing applied, but the measured Fmin includes some scatter.
[0029] FIG. 7 is a plot of Fmin vs. frequency calculated from a model.
[0030] FIG. 8 is a plot of gamma_opt vs. frequency calculated from a model.
[0031] FIG. 9 is a plot of Fmin vs. input bias voltage calculated from a model.
[0032] FIG. 10 is an example of an equivalent electrical schematic of the device model of an FET.
[0033] FIG. 11 is an equivalent electrical schematic of the Pospieszalski noise model of an intrinsic transistor.
[0034] FIG. 12 is an exemplary noise parameter measurement setup. This setup can be used to determine a device noise model, and the DUT noise parameters may then be calculated from the device noise model.
[0035] FIG. 13 is an exemplary flow diagram to measure noise parameters.
[0036] FIG. 14 is an exemplary flow diagram to measure a device noise model.
DETAILED DESCRIPTION
[0037] In the following detailed description and in the several figures of the drawing, like elements are identified with like reference numerals. The figures are not to scale, and relative feature sizes may be exaggerated for illustrative purposes.
[0038] Another way of representing the noise performance of a device is with a device model. Device models are often developed for use in circuit simulators. One advantage of a device model, for example, is that calculation of device or circuit performance is not limited to the measurement parameter range at which the device parameters were measured. A compact device model may consist of an equivalent circuit that will simulate the device performance, and the element values of that equivalent circuit are often determined by adjusting the values until the calculated performance matches DC and small signal measured data, including noise parameters.
[0039] Another important advantage of a device model is that it does not calculate the device performance independently at each value of a measured parameter such as frequency. The model will typically predict that the noise contribution varies with frequency in a smooth manner, without the scatter that is typical with measured noise parameters. Determination of the noise part of a device model is often done using noise figure or noise parameters which were previously calculated from raw noise data.
[0040] There is known device information that is not used in the prior art to determine measured noise parameters. Even without knowing any element values of a device model, the general nature of the device operation can be known. For example, a model structure may indicate that the Fmin value vs. frequency should be smooth and monotonically increasing with increasing frequency. Another example is that a model may indicate the value of Fmin at DC (where frequency=0). Another example is that a model may show that some of the noise parameters should fit a polynomial curve vs. frequency or bias. A simple polynomial curve could even be considered to be a simple model. FIGS. 7 and 8 are examples of Fmin and Gamma_opt calculated from a model, showing the smooth response vs. frequency. FIG. 9 shows an example of Fmin calculated from a model vs. DC bias.
[0041] The known or assumed information about a device may be represented by different types of models. A “response model” would be a simple model that describes the general nature or response of the device operation. For example, It might be known or assumed that a noise parameter value (such as Fmin) of a device should be smooth vs. a measurement parameter (such as frequency). If this smooth behavior is modeled as a polynomial function, then the model parameters (model element values) would be the polynomial coefficients. An “equivalent circuit model” would be a model that represents the device with a schematic of electrical components such as resistors, capacitors, inductors, and current generators, as in FIGS. 10 and 11 . The electrical values (i.e. resistance, capacitance, or inductance, for example) of each circuit element would be the model parameters. The electrical value of a circuit element may be fixed, or it may be represented by an equation. In the latter case, each value that goes into the equation would be a model parameter or model element value. A “hybrid model” may use a response model to describe part of the device, and an equivalent circuit for another part of the device. For example, a hybrid model could use an equivalent circuit for the parasitic capacitance and inductance, and a response model for the intrinsic device.
[0042] Embodiments of the invention improve on the prior art by using known information about device performance vs. a measurement parameter or multiple measurement parameters, in addition to the measured raw noise data, to determine noise parameters. Examples of the measurement parameter include frequency, DC bias, or temperature. A wide range of information may be used, quantified by an appropriate model such as a response model, an equivalent circuit model, or a hybrid model. Other model types may alternatively be used.
[0043] Exemplary embodiments of the method are different from conventional smoothing. For example, the data in FIGS. 6 and 7 come from the same raw data, but the slope of the smoothed Fmin vs. frequency in FIG. 6 is different from Fmin vs. frequency from the model in FIG. 7 . Trying to use additional known information to post process the data with smoothing will often give poor or wrong results, and is not the same as using the additional known information to solve directly for the noise parameters. So even though post processed smoothing of noise parameters was known in the prior art, using additional known information like this (smoothness vs. frequency) about the device operation vs. a measurement parameter has not been used in the prior art for the measurement of the noise parameters.
[0044] To illustrate the principle of an exemplary embodiment of this invention, let us use a simple response model that says Fmin vs. frequency is a straight line rising with frequency, and zero when frequency is zero. This leads to the following equations:
[0000] F min= Fa *Frequency
[0000] F=F min+4 rn |gamma_ s− gamma_opt|̂2/(|1+gamma_opt|̂2(1−|gamma_ s|̂ 2))
[0045] The first equation is additional information that was not used in the prior art. These two equations may be combined to give the following equation:
[0000] F=Fa* Frequency+4 rn| gamma_ s− gamma_opt|̂2/(|1+gamma_opt|̂2(1−|gamma_ s|̂ 2))
[0046] In this example, Fa is the slope of Fmin vs. frequency, and is an element value of the model. Fa is independent of frequency, so if measurements are made at five frequencies, gamma_opt magnitude should be determined at all five frequencies, gamma_opt phase at all five frequencies, rn at all five frequencies, but only one value of Fa needs to be determined instead of Fmin at all five frequencies. Once the value of Fa is known, Fmin may be calculated from the first equation. If over-determined data, i.e. more data than theoretically required to obtain a more robust result, is used with LMS reduction, the best fit will be obtained for gamma_opt and rn vs. frequency, and guarantee that Fmin meets the model of a straight line vs. frequency, and zero when frequency is zero.
[0047] In this simple example, the amount of variables that must be determined has been reduced, which simplifies the work. Results that match additional known information about the DUT are also obtained.
[0048] The response model of this illustration may be extended to include gamma_opt. Now a model is used that says Fmin vs. frequency is a straight line rising with frequency, and zero when frequency is zero, as in the prior illustration. In addition, this model says that gamma_opt magnitude is 1 when frequency is zero, and decreases with frequency by a second order polynomial. Also this model says that gamma_opt phase is zero degrees when frequency is zero, and moves in a straight line vs. frequency, becoming more positive as frequency increases. This leads to the following equations:
[0000] F min= Fa *Frequency
[0000] Gamma_opt magnitunde=1 −G ma*frequency− G mb*frequency*frequency
[0000] Gamma_opt phase= G p*frequency
[0000] F=F min+4 rn |gamma_ s −gamma_opt|̂2/(|1+gamma_opt|̂2(1−|gamma_ s|̂ 2))
[0049] In this response model example, three new equations with additional information have been used that was not used in the prior art. The variable Fa is the slope of Fmin vs. frequency, as before. Gma is the first order coefficient of the gamma_opt_mag polynomial vs. frequency. Gmb is the second order coefficient of the gamma_opt_mag polynomial vs. frequency. Gp is the slope of gamma_opt_phase vs. frequency. All of the variables Fa, Gma, Gmb, and Gp, are element values of the model, and are independent of frequency, so only one value or measurement is needed for each of them. Measurements of rn at all five frequencies are still required. This is a total of only 9 values and guarantees that both Fmin and Gamma_opt will follow the model criteria vs frequency. This is a large improvement over the prior art, which would need to determine all four noise parameters at all five frequencies, for a total of twenty values with no connection between frequencies. Of course, the improvement would be even greater when more frequencies are used. This example model uses a combination of model elements; model elements Fa, Gma, Gmb, and Gp are independent of the measurement parameter, frequency, while rn is determined separately for each measurement frequency.
[0050] In both examples, the exemplary solution may use over-determined noise raw data to reduce errors, and standard LMS routines which are well known in the art would be used to reduce the over-determined data to get the final solution.
[0051] The prior example may be appropriate for some transistors or applications. But more complex models can have more detailed or complete information, especially for device performance vs. multiple measurement parameters. A typical example of a more complete FET equivalent circuit device model is shown in FIG. 10 . The schematic may vary with different implementations, but the general intent is for the model to allow device performance to be calculated for a range of stimulus values. The device performance calculated with such a model will generally include gain and impedance data, as well as noise data. Many of the model element values having to do with gain performance may be determined with s-parameter vs. bias measurements. The noise portion of the model has generally been determined from noise parameters. In an exemplary implantation of the invention, the noise portion of the model would be determined from raw noise data instead of noise parameters.
[0052] The Pospieszalski equivalent circuit noise model, illustrated in FIG. 11 , represents the intrinsic noise of the transistor with two model parameters or model element values Tg and Td. In the prior art, these model element values have been determined by fitting the model element values to previously determined noise parameters. In accordance with an embodiment of this invention, the device model element values are determined by fitting at least one of the device model element values to measured raw noise data.
[0053] Once the model element values are known, the noise parameters can then be determined, i.e. calculated from the model.
[0054] The noise parameters thus determined from any type of device model make use of information that was not used in the prior art to determine the noise parameters. The result is noise parameter data that more truly represents the performance of the DUT.
[0055] Another aspect of this invention is a more direct method of determining the element values of a device noise model. In the past, the element values of device noise models were fit to noise figure or noise parameters that were calculated from raw noise data.
[0056] In accordance with this aspect of the invention, the element values of a device model are fitted directly from the raw measured noise data instead of first calculating the corrected noise figure or noise parameters from raw noise data. The raw measured noise data that is available depends on the noise receiver that is used. For example, the raw measured noise data may be uncorrected readings from the noise receiver, which are typically proportional to power or voltage. Another example is that the raw measured noise data could comprise partially corrected data calculated by the noise receiver, such as noise figure not corrected for mismatches.
[0057] In accordance with another aspect, a subset of the measured data may be used for determination of the noise model element values. The subset of the measured data may be selected to remove data measured at impedances where the DUT is unstable or the measurement accuracy is reduced. As is known in the art, calibration or measurement uncertainty at some impedances may produce outlier data, which are inconsistent with true device performance and the majority of data. Also, some impedances can cause a device to oscillate, which would invalidate the measured data for those impedances. Multiple determinations of the model element values may be performed, with each determination comprising a calculation using a different subset of the measured data, and where the best results are kept as the final calculated noise model. In like fashion, a subset of the measured data may also be used to determine the noise parameters. In this case, the subset would first be used to determine the model element values, and the noise parameters then determined from the model.
[0058] A block diagram of an exemplary noise parameter measurement setup or system 100 is shown in FIG. 12 . It includes a controller 110 that has a processor 112 , a database 114 of device model types, Least Mean Squares algorithms 116 for fitting over-determined data, a digital memory ( 118 ), a file system 120 for saving data, and I/O ports 122 for communicating with and controlling the instruments in the system. As with the system of FIG. 1 , the system 100 includes a noise source 130 , a network analyzer 150 , and an input switch 132 for connecting either the noise source or the network analyzer to the impedance tuner 134 . The impedance tuner 134 is configured to present a variable impedance to the DUT 10 , under control of the controller 110 . Impedance tuners are well known in the art, e.g. as described in U.S. Pat. No. 8,890,750. A bias system 140 is connected to the DUT 10 . The output side of the DUT is connected through output switch 138 to either a noise figure meter 136 or to the network analyzer 150 . The noise figure meter is a stand-alone noise receiver. In some implementations, the noise receiver may be incorporated in the network analyzer, rather than being a stand-alone instrument. The solid lines indicate RF connections, and the dashed lines indicate control or communication connections. This controller 110 may comprise a computer, a stand-alone controller, or it may be built into one of the instruments, such as a network analyzer or a tuner. The controller will control the instruments 130 , 132 , 134 , 136 , 138 , 140 , 150 to setup the swept measurement parameters and measure the raw noise data. It will then use the model type selected from the device model type database by the user with the standard LMS algorithms to solve for the model values from over-determined data. Once the model element values are determined, the noise parameters can be calculated from the model. Such noise parameter calculations are known in the art, see, for example, “Modeling of Noise Parameters of MESFET'S and MODFET'S and Their Frequency and Temperature Dependence,” Marian W. Pospieszalski, 1989 IEEE MTT-S Digest, pages 385-388; and “A New Method to Calculate the Pospieszalski Model Noise Parameters for a HEMT Transistor,” Julian Chereches et al., International Symposium for Design and Technology of Electronic Packages, 14 th Edition, ISSN 1843-5122, pages 101-105, 2008, pages 101-105.
[0059] The database of device model types provides the capability of selecting a noise model prior to calculating the noise parameters, an improvement over the prior art. The database may comprise one or more models; if only one type of DUT is to be measured, multiple model types in the database may not be necessary.
[0060] A flow chart of an exemplary noise parameter measurement procedure 200 in accordance with an embodiment of this invention is shown in FIG. 13 . The measurement sequence includes the following steps.
[0061] 1. Setup ( 202 ) the measurement bench with all of the required measurement equipment; an exemplary measurement bench or setup is illustrated in FIG. 12 .
[0062] 2. Calibrate ( 204 ) the system components in-situ.
[0063] 3. Calibrate ( 206 ) the noise and gain parameters of the noise receiver.
[0064] 4. Select ( 208 ) the desired device noise model type from the database of device noise models. Different devices may require different model types. Multiple model types may apply to the same DUT type. For example, some model types may be more complete, but require more work and measurements to develop. Other model types may be simpler, but less complete, yet sufficient for a given application.
[0065] 5. Connect the DUT, and apply the initial DC bias ( 210 ).
[0066] 6. Measure ( 212 ) the s-parameters of the DUT.
[0067] 7. Measure ( 214 ) the raw noise data as a function of the selected measurement parameters, such as frequency, DC bias, or temperature.
[0068] 8. Calculate ( 216 ) the element values of the selected device noise model that will give the best fit to the measured raw noise data.
[0069] 9. From the device noise model with the element values determined in step 8 ( 216 ), calculate ( 218 ) the noise parameters of the DUT.
[0070] 10. Save ( 220 ) the noise parameters in a noise data file.
[0071] 11. If ( 222 ) there are more DUTs to measure, return to step 5 ( 210 ) and connect the next DUT.
[0072] A variation of the flow diagram is shown in FIG. 14 . This may be used if the desired measured output is the device model, and noise parameters are not explicitly required. FIG. 14 is the same as FIG. 13 , with the same reference numbers referring to the same steps as in FIG. 13 , except that when the model is determined, the model parameters are saved ( 252 ), and the step of calculating the noise parameters is skipped.
[0073] Another exemplary variation of the flow diagram would be to combine FIG. 13 and FIG. 14 , and save both the device noise model and the noise parameters.
[0074] Although the foregoing has been a description and illustration of specific embodiments of the subject matter, various modifications and changes thereto can be made by persons skilled in the art without departing from the scope and spirit of the invention.
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Systems and methods of measuring and determining noise parameters. An exemplary method measures noise data and determines element values of a device noise model for a device under test (DUT), using a test system including an impedance tuner coupled to an input of the DUT for presenting a controllable variable impedance to the DUT and a noise receiver coupled to an output of the DUT. Noise data is measured as a function of at least one measurement parameter. The measured data includes raw noise data read from the noise receiver, and is used to determine element values of the device noise model. The system may include a database of device models
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] The present application is based on U.S. provisional patent application No. 60/247,400, filed Nov. 10, 2000, entitled “Highlevel Active Pen Matrix”.
[0002] The present application is also related to application Ser. No. (Atty docket 3797.00066), entitled “Method and Apparatus For Improving the Appearance of Digitally Represented Handwriting”, filed Nov. 10, 2000; to application Ser. No. (Atty docket 3797.00069), entitled “Selection Handles in Editing Electronic Documents”, and filed Nov. 10, 2000; to application Ser. No. (Atty docket 3797.00070), entitled “Insertion Point Bungee Space Tool”, and filed Nov. 10, 2000; to application Ser. No. (Atty docket 3797.00072), entitled “Simulating Gestures of a Mouse Using a Stylus and Providing Feedback Thereto”, and filed Nov. 10, 2000; to application Ser. No. (Atty docket 3797.00074), entitled “System and Method For Accepting Disparate Types Of User Input”, and filed Nov. 10, 2000; to application Ser. No. (Atty docket 3797.00075), entitled “In Air Gestures”, and filed concurrently with the present application; to application Ser. No. (Atty docket 3797.00076), entitled “Mouse Input Panel Windows Class List”, and filed Nov. 10, 2000; to application Ser. No. (Atty docket 3797.00077), entitled “Mouse Input Panel and User Interface”, and filed Nov. 10, 2000; and to application Ser. No. (Atty docket 3797.00079), entitled “System and Method For Inserting Implicit Page Breaks”, and filed Nov. 10, 2000; each of which is incorporated by reference herein.
FIELD OF THE INVENTION
[0003] Aspects of the present invention are directed generally to apparatus and methods for controlling a graphical user interface (GUI). More particularly, the present invention relates to receiving user input, determining based on the user input what the user wants to do, and performing a function related to the desired input.
BACKGROUND OF THE INVENTION
[0004] Typical computer systems, especially computer systems using graphical user interface (GUI) systems such as Microsoft WINDOWS, are optimized for accepting user input from one or more discrete input devices such as a keyboard and for entering text, and a pointing device such as a mouse with one or more buttons for driving the user interface. Virtually all software applications designed to run on Microsoft WINDOWS are optimized to accept user input in the same manner. For instance, many applications make extensive use of the right mouse button (a “right click”) to display context-sensitive command menus. The user may generate other gestures using the mouse such as by clicking the left button of the mouse (a “left click”), or by clicking the left or right button of the mouse and moving the mouse while the button is depressed (either a “left click drag” or a “right click drag”).
[0005] In some environments, a mouse is not usable or desirable. For example, in a digitizer tablet environment, the primary input device may be a stylus. While a stylus attempts to provide pad and paper-like feel to a computing environment, current systems are limited. For example, the use of a stylus in a graphical user interface is limited to tapping on various items for selection. See, for example, the Palm-series of products using the Palm OS 3.0 operating system. Further, in stylus-based input environments, a user is continually forced to select tools or operations from a remote tool bar, generally on a top or bottom of a screen. While a user can type in letters or have the digitizer recognize handwriting, these operations require selecting a keyboard input mode and writing in a predefined portion of the digitizer, respectively. In short, requiring a user to tell the computer, for every new input, what a user wants to do makes stylus-based computing difficult for the average user. Accordingly, stylus based inputs have been relegated to personal data assistants (PDAs) where significant user input is not possible. Mainstream computing still requires the use of at least a keyboard and mouse (or mouse-based input device, for example, trackballs, touch-pads, and other mouse substitutes).
[0006] Accordingly, a need exists for permitting a user to perform all operations of a mouse-type device using a stylus.
SUMMARY OF THE INVENTION
[0007] As discussed in the various copending patent applications incorporated herein by reference, aspects of the present invention are directed to a tablet-like computer that allows users to directly write on a display surface using a stylus. The display surface may physically, optically, and or electro magnetically detect the stylus. The computer may allow the user to write and to edit, manipulate, and create objects through the use of the stylus. Many of the features discussed in these copending applications are more easily performed by use of the various aspects of the present invention discussed herein.
[0008] An aspect of the present invention is directed to methods and apparatus for simulating gestures of a mouse by use of a stylus on a display surface. The present invention determines the operation a user wants to perform based on the user's input. This determination may include reference to other information including the location of the user's input on a digitizer (e.g., location on a screen) and the status of other objects or elements as displayed. By using this information, the system determines what the user wants to do and implements the action.
[0009] A number of inputs with a stylus are possible. For example, a user may Lap a stylus, stroke the stylus, hold the stylus at a given point, or hold then drag the stylus. Other inputs and combinations are possible as noted by the above-identified applications, which are expressly incorporated herein by reference.
[0010] As to a stroke operation, the system may drag an object, may maintain a current state or operation, or being inking. Inking may include writing, drawing, or adding annotations as described in greater detail in U.S. Ser. No. 60/212,825, filed Jun. 21, 2000, entitled “Methods for Classifying, Anchoring, and Transforming Ink Annotations” and incorporated by reference.
[0011] As to a tap operation, the system may add to existing writing, may select a new object, insert a cursor or insertion point, or may perform an action on a selected object.
[0012] As to a hold operation, the system may simulate a right mouse button click or other definable event.
[0013] As to a hold and drag operation, the system may drag a selected object or perform other functions.
[0014] These and other features of the invention will be apparent upon consideration of the following detailed description of preferred embodiments. Although the invention has been defined using the appended claims, these claims are exemplary in that the invention is intended to include the elements and steps described herein in any combination or subcombination. Accordingly, there are any number of alternative combinations for defining the invention, which incorporate one or more elements from the specification, including the description, claims, and drawings, in various combinations or subcombinations. It will be apparent to those skilled in the relevant technology, in light of the present specification, that alternate combinations of aspects of the invention, either alone or in combination with one or more elements or steps defined herein, may be utilized as modifications or alterations of the invention or as part of the invention. It is intended that the written description of the invention contained herein covers all such modifications and alterations.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The foregoing summary of the invention, as well as the following detailed description of preferred embodiments, is better understood when read in conjunction with the accompanying drawings, which are included by way of example, and not by way of limitation with regard to the claimed invention. In the accompanying drawings, elements are labeled with three-digit reference numbers, wherein the first digit of a reference number indicates the drawing number in which the element is first illustrated. The same reference number in different drawings refers to the same element.
[0016] [0016]FIG. 1 is a schematic diagram of a general-purpose digital computing environment that can be used to implement various aspects of the invention.
[0017] [0017]FIG. 2 is a plan view of a tablet computer and stylus that can be used in accordance with various aspects of the present invention.
[0018] FIGS. 3 - 7 are flowcharts showing a variety of steps for interpreting a user's input in accordance with embodiments of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0019] The present invention may be more readily described with reference to FIGS. 1 - 7 . FIG. 1 illustrates a schematic diagram of a conventional general-purpose digital computing environment that can be used to implement various aspects of the present invention. In FIG. 1, a computer 100 includes a processing unit 110 , a system memory 120 , and a system bus 130 that couples various system components including the system memory to the processing unit 110 . The system bus 130 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. The system memory 120 includes read only memory (ROM) 140 and random access memory (RAM) 150 .
[0020] A basic input/output system 160 (BIOS), containing the basic routines that help to transfer information between elements within the computer 100 , such as during start-up, is stored in the ROM 140 . The computer 100 also includes a hard disk drive 170 for reading from and writing to a hard disk (not shown), a magnetic disk drive 180 for reading from or writing to a removable magnetic disk 190 , and an optical disk drive 191 for reading from or writing to a removable optical disk 192 such as a CD ROM or other optical media. The hard disk drive 170 , magnetic disk drive 180 , and optical disk drive 191 are connected to the system bus 130 by a hard disk drive interface 192 , a magnetic disk drive interface 193 , and an optical disk drive interface 194 , respectively. The drives and their associated computer-readable media provide nonvolatile storage of computer readable instructions, data structures, program modules and other data for the personal computer 100 . It will be appreciated by those skilled in the art that other types of computer readable media that can store data that is accessible by a computer, such as magnetic cassettes, flash memory cards, digital video disks, Bernoulli cartridges, random access memories (RAMs), read only memories (ROMs), and the like, may also be used in the example operating environment.
[0021] A number of program modules can be stored on the hard disk drive 170 , magnetic disk 190 , optical disk 192 , ROM 140 or RAM 150 , including an operating system 195 , one or more application programs 196 , other program modules 197 , and program data 198 . A user can enter commands and information into the computer 100 through input devices such as a keyboard 101 and pointing device 102 . 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 110 through a serial port interface 106 that is coupled to the system bus, but may be connected by other interfaces, such as a parallel port, game port or a universal serial bus (USB). Further still, these devices may be coupled directly to the system bus 130 via an appropriate interface (not shown). A monitor 107 or other type of display device is also connected to the system bus 130 via an interface, such as a video adapter 108 . In addition to the monitor, personal computers typically include other peripheral output devices (not shown)., such as speakers and printers. In a preferred embodiment, a pen digitizer 165 and accompanying pen or stylus 166 are provided in order to digitally capture freehand input. Although a direct connection between the pen digitizer 165 and the processing unit 110 is shown, in practice, the pen digitizer 165 may be coupled to the processing unit 110 via a serial port, parallel port or other interface and the system bus 130 as known in the art. Furthermore, although the digitizer 165 is shown apart from the monitor 107 , it is preferred that the usable input area of the digitizer 165 be co-extensive with the display area of the monitor 107 . Further still, the digitizer 165 may be integrated in the monitor 107 , or may exist as a separate device overlaying or otherwise appended to the monitor 107 .
[0022] The computer 100 can operate in a networked environment using logical connections to one or more remote computers, such as a remote computer 109 . The remote computer 109 can be 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 100 , although only a memory storage device 111 has been illustrated in FIG. 1. The logical connections depicted in FIG. 1 include a local area network (LAN) 112 and a wide area network (WAN) 113 . Such networking environments are commonplace in offices, enterprise-wide computer networks, intranets and the Internet.
[0023] When used in a LAN networking environment, the computer 100 is connected to the local network 112 through a network interface or adapter 114 . When used in a WAN networking environment, the personal computer 100 typically includes a modem 115 or other means for establishing a communications over the wide area network 113 , such as the Internet. The modem 115 , which may be internal or external, is connected to the system bus 130 via the serial port interface 106 . In a networked environment, program modules depicted relative to the personal computer 100 , or portions thereof, may be stored in the remote memory storage device.
[0024] It will be appreciated that the network connections shown are exemplary and other techniques for establishing a communications link between the computers can be used. The existence of any of various well-known protocols such as TCP/IP, Ethernet, FTP, HTTP and the like is presumed, and the system can be operated in a client-server configuration to permit a user to retrieve web pages from a web-based server. Any of various conventional web browsers can be used to display and manipulate data on web pages.
[0025] [0025]FIG. 2 illustrates a tablet PC 201 that can be used in accordance with various aspects of the present invention. Any or all of the features, subsystems, and functions in the system of FIG. 1 can be included in the computer of FIG. 2. Tablet PC 201 includes a large display surface 202 , e.g., a digitizing flat panel display, preferably, a liquid crystal display (LCD) screen, on which a plurality of windows 203 is displayed. Using stylus 204 , a user can select, highlight, and write on the digitizing display area. Examples of suitable digitizing display panels include electromagnetic pen digitizers, such as the Mutoh or Wacom pen digitizers. Other types of pen digitizers, e.g., optical digitizers, may also be used. Tablet PC 201 interprets marks made using stylus 204 in order to manipulate data, enter text, and execute conventional computer application tasks such as spreadsheets, word processing programs, and the like.
[0026] A stylus could be equipped with buttons or other features to augment its selection capabilities. In one embodiment, a stylus could be implemented as a “pencil” or “pen”, in which one end constitutes a writing portion and the other end constitutes an “eraser” end, and which, when moved across the display, indicates portions of the display are to be erased. Other types of input devices, such as a mouse, trackball, or the like could be used. Additionally, a user's own finger could be used for selecting or indicating portions of the displayed image on a touch-sensitive or proximity-sensitive display. Consequently, the term “user input device”, as used herein, is intended to have a broad definition and encompasses many variations on well-known input devices.
[0027] Region 205 shows a feed back region or contact region permitting the user to determine where the stylus as contacted the digitizer. In another embodiment, the region 205 provides visual feedback when the hold status of the present invention has been reached.
[0028] FIGS. 3 - 7 show various flowcharts for determining what a user wants to do based on a user's interaction with the digitizer. As will be discussed below, the user contacts the digitizer where the user wants to begin writing, tapping, annotating, dragging, etc. In the case where the digitizer is superimposed over a display, the user's contact with the digitizer is directed at operating at (or near) the contact point between the user's stylus and the currently displayed information at or near the contact point.
[0029] In step 301 , the system senses a contact or other indication of an action. In one embodiment the contact may be the stylus contacting the surface of the digitizer. In another embodiment, the action may be bringing the tip of the stylus near the digitizer's surface. Further, if the stylus includes another signaling method (for example, a radio transmitter transmitting a signal to the digitizer signaling a user's input), the digitizer (or related input mechanism or mechanisms) interpret the received signal as a user's input. Other methods of starting an operation or writing or contact with a digitizer are known in the art. For purposes of illustration and description, the system and method reference physical contact with the digitizer. All other ways of providing signals to a processor are considered within the scope of the invention and are not mentioned here for simplicity.
[0030] In step 302 , the system determines the contact position and what lies beneath the contact position (for example, an object, a drawing, blank space, ink, and the like). In step 303 , the system determines if the stylus has moved beyond a first threshold (time, distance, rate, or acceleration, and the like). In one embodiment, the threshold is set to the minimum resolvable movement. In another embodiment, the threshold is set higher to account for shaky hands, vibrations of the digitizer or tablet pc (for example, if trying to use the system while driving in a car over a bumpy road). It is noted that objects may have all the same threshold. Alternatively, objects may have different thresholds. This may be dependent on the object, the size of the object, the state of the system, the state of the object, and the like.
[0031] If the first threshold has been exceeded, then the system proceeds to step 304 where the user's input is classified as a stroke and the system steps to point A 305 . If the first threshold has not been exceeded, the system determines if the stylus was still in contact with the digitizer when a time threshold had expired in step 306 . If no (meaning that the stylus was still in contact with the digitizer surface), the system classifies the input as a tap in step 307 and proceeds to point B 308 .
[0032] If the stylus was still in contact with the surface after the time threshold in step 306 , the system determines if a second move threshold was exceeded in step 309 . The first and second move thresholds may be identical or different. For example, both may be 0.25 mm. Or, the first may be 0.5 mm or one mm and the second be 0.3 mm. Further, the first may be 1.2 mm or more and the second may be 0.5 mm or more. In short, any values may be used as long as they are not obtrusive to the user. The second threshold may be determined only after the time threshold of step 306 has expired. In this example, the second threshold may be higher than the first threshold (or it may be the same or smaller).
[0033] If the second move threshold was not exceeded, then the system classifies the input as a hold in step 310 and proceeds to point C 311 . If the second move threshold was exceeded, then the system classifies the input as a ‘hold and drag’ in step 312 and moves to point D 313 .
[0034] [0034]FIG. 4 shows point A as starting point 401 . Here, the system classified the input as a stroke and begins stroke processing in step 402 . In step 403 , the system determines if the stroke started on a draggable object. If yes, the system determines in step 404 whether drag threshold was exceeded (for example, 0.25 inches, 0.25 inches per second and the like). If so, the system classifies the stroke as a drag in step 405 and performs a function that is dependent on the object. For example, the drag may extend a selection as described in greater detail in “Selection Handles in Editing Electronic Documents,” filed concurrently with the present application (attorney docket 03797.00069), and expressly incorporated by reference. Also, the drag may operate a bungee tool as described in Ser. No. (Atty docket 3797.00070), entitled “Insertion Point Bungee Space Tool”, and filed concurrently with the present application, and expressly incorporated herein.
[0035] If, in step 404 , the drag threshold has not been exceeded, the system maintains the current state (with the object being selected or not) in step 407 . If the stroke was not over a draggable object in step 403 , the system determines if the area under the contact point is inkable in step 408 . For example, inkable may mean an area capable of receiving ink (including drawings, annotations, or writing) as detailed in serial No. 60/212,825, filed Jun. 21, 2000, and expressly incorporated herein by reference for essential subject matter. By contrast, a control button (for copy, save, open, etc.) may not be inkable. If inkable in step 408 , the system permits inking (drawing, writing, annotating and other related functions) in step 409 . If not inkable, the system maintains the current state (objects selected or not) in step 407 .
[0036] In FIG. 5A, the system starts at point B 501 and operates on the input as a tap 502 . The system determines whether the tap was on an area or object that is inkable in step 503 . If yes, the system determines whether any ink was recently added or “wet” (for example, less than 0.5 or 1 second old) in step 504 . If so, the system considers the tap as a dot to be added to the ink in step 505 (and adds the dot). If no wet ink exists, then the system determines if the tap was over a selectable object in step 506 It is noted that steps 503 and 504 may be combined. If the tap was over a selectable object, then the system determines if the object was already selected in step 507 . If it was not, then the system selects the tapped object in step 508 . If a previous object had been selected, the system cancels the previous or old selection in step 509 . If the object was previously selected as determined by step 507 , the system performs an action relevant to the object in step 510 . This action may include editing the object, performing a predefined operation (for example, enlarge, shrink and the like). From step 506 , if the tap was not on a selectable object, then the system proceeds to point BB 512 .
[0037] [0037]FIG. 5B shows additional processing to FIG. 5A. As point BB 512 , the system determines if the tap was in a space between text (referred to herein as an inline space) in step 513 . If yes, the system places an insertion point at the tap point in step 514 . As shown in a broken lined box, the system may also cancel any old or previous selections in step 515 . If no, then the system determines if the tap point has ink nearby in step 518 . If the system determines that the tap was nearby ink, then the system adds a dot to the ink in step 516 . If there was an old selection, then the system cancels the old selection in step 517 (as shown by a broken line box).
[0038] If not nearby ink in step 518 , the system determines if the tap is on an active object in step 519 . If the tap was not on an active object, the system places an insertion point at the tap point or performs some other definable action in step 520 . Again, if there was an old selection, then the system cancels the old selection in step 521 (as shown by a broken line box). If the tap was on an active object as determined by step 519 , the system performs an action in step 522 . The action may be definable by the user or relate to any function desirable. In one embodiment, the action may be to perform a function to operate a selection handle or bungee space tool as described in “Selection Handles in Editing Electronic Documents,” filed concurrently with the present application (attorney docket 03797.00069), and expressly incorporated by reference. Also, the drag may operate a bungee tool as described in Ser. No. (Atty docket 3797 . 00070 ), entitled “Insertion Point Bungee Space Tool”, and filed concurrently with the present application, and expressly incorporated herein. Other operations are known in the art and incorporated herein.
[0039] [0039]FIG. 6 relates to holding a stylus beyond a time threshold. Starting from point C 601 , the system classifies the user input as a hold operation in step 602 . Next, the system simulates a right mouse button click or other definable event in step 603 . The functions associated with step 603 are described in greater detail in U.S. application Ser. No. (Atty docket 3797.00072), entitled “Simulating Gestures of a Mouse Using a Stylus and Providing Feedback Thereto”, filed Nov. 10, 2000, whose contents are expressly incorporated herein by reference.
[0040] [0040]FIG. 7 relates to holding a stylus beyond a time threshold and moving the slylus. Starting from point D 701 , the system classifies the user input as a hold and drag operation in step 702 . Next, in step 703 the system drags the selected object as directed by the user.
[0041] There are a number of alternatives associated with dragging. If the hold and drag relates to an inline space, the system may use this hold and drag function to select text. Similarly, one may use this function to select a drawing encountered by the dragged stylus. Further, one may select both text and drawings in this manner. Also, the cursor's point may become a selection tool that leaves a trail behind it. In this regard, the user may loop a number of objects, drawing or text in this regard. The looping of the objects may result in the selecting of the objects.
[0042] An alternate embodiment of the present invention relates to modifying ink drawings or annotations. For example, if one added an annotation (from step 409 ) to text, one may manipulate the text (for example, by inserting new text) and have the annotation track the manipulation of the text. So, if one circled text then added text to the circled text, the annotation would expand to include the added text as well. This is described in relation to in U.S. Ser. No. 60/212,825, filed Jun. 21, 2000, entitled “Methods for Classifying, Anchoring, and Transforming Ink Annotations” and incorporated by reference.
[0043] While exemplary systems and methods embodying the present invention are shown by way of example, it will be understood, of course, that the invention is not limited to these embodiments. Modifications may be made by those skilled in the art, particularly in light of the foregoing teachings. For example, each of the elements of the aforementioned embodiments may be utilized alone or in combination with elements of the other embodiments.
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The present invention relates to a system, method and medium for receiving and acting upon user input. In one embodiment, the user may only have access to a limited input device, like a stylus. Using the present invention, a user is provided with intuitive responses from the system based on inputs from the limited input device.
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RELATED APPLICATIONS
[0001] This application claims benefit of provisional applications Ser. No. 60/180,817, filed on Feb. 7, 2000 and Ser. No. 60/215,722, filed on Jul. 3, 2000.
FIELD OF THE INVENTION
[0002] This invention relates to lottery tickets.
BACKGROUND OF THE INVENTION
[0003] The Pennsylvania State lottery game “Super 6 Lotto”, is exemplary of many. If one were to purchase a $5 ticket, one would receive a ticket with 15 groups of numbers, each group containing six numbers, for a total of 90 numbers, the numbers within each group being selected from 1 through 69. Of course, if all six of the numbers in one group later match the winning 6 numbers, the ticket purchaser is a winner. The ticket purchaser is also a winner if 3, 4 or 5 of the numbers within a group match any of the winning numbers. Comparing the numbers in the ticket to the winning numbers can become tedious, especially if, for example, a group of individuals working together decide to pool their ticket purchases. Ten $5 tickets would have 900 numbers to check. The designated ticket checker could waste upwards of an hour determining if a ticket is a winner. State lotteries fund many worthwhile causes, but the mathematical permutations and combinations required to check if a ticket is a winner is unpleasantly work-like to many individuals and inhibits ticket sales.
SUMMARY
[0004] The invention includes a method for checking lottery tickets comprising the steps of digitizing at least one lottery ticket comprising lottery numbers to form an image, performing optical character recognition (OCR) on the image to obtain the lottery numbers, comparing the lottery ticket lottery numbers to at least one winning lottery number and reporting the winning status of the at least one lottery ticket.
[0005] In a preferred embodiment, the invention allows a purchaser of lottery tickets to scan multiple lottery tickets at once, send the resulting image to a web site, where the web site will indicate to the purchaser whether any of the tickets are winners and also highlight on the image for the purchaser the location of a winning ticket in the image and also highlight where on the ticket the winning number is.
DETAILED DESCRIPTION OF THE INVENTION
[0006] The present invention provides the ability to scan multiple lottery tickets from various states, dates, and types of contests and to rapidly determine which ticket, if any, has a winning number and where in the ticket that number is. A user would scan one or more tickets to form a digital image, The digital image is then subject to an optical character recognition program to extract the lottery numbers, dates, states, and type of bet (depending on the game), the resulting information is compared to a database of winning numbers, and the user is presented with a report, that advises the user whether he has won. In a particularly preferred embodiment, the user is presented with a report that takes the form of the original image, but altered so that any winning tickets are displayed in a highlighted fashion, such as by circling the ticket, making the numbers bold, underlining, changing the text or the background color and the winning numbers within the ticket may also be highlighted. In this way, the user can select the winning ticket or tickets right off the scanner bed to present for payment, and discard the losing tickets.
[0007] The daily change of lottery numbers lends itself well to Internet-based applications. An Internet-based method could, for example, comprise the following steps: providing a web site having a user interface, receiving at the web site a user input of a digitized image of at least one lottery ticket comprising at least one lottery number, performing optical character recognition on a digitized image of the at least one lottery ticket to obtain the at least one lottery number in a computer usable form, comparing the at least one lottery number to at least one winning lottery number, reporting to the user whether the at least one lottery ticket contains a winning number.
[0008] In an embodiment of the invention, a user emails a digitized image of at least one lottery ticket to a website, the website applies OCR software to the image, compares the ticket numbers, ticket dates, state identification, type of game, and the like to a database of winning numbers and either: 1) emails the user back, reporting whether he has won, and if the user has won, reporting which ticket (by date, first number, last number or image highlighting, for example) and which number in the ticket, or 2) emailing to the user a link to the website where the user may view the results. The second method is preferred because some email systems can't handle large image files well and because the user can be presented with advertising.
[0009] In another embodiment, the website stores the image sent by the user on a computer readable medium after OCR and it has been determined that the date on at least one of the tickets indicates that the lottery has not yet occurred. Once the lottery has occurred, the user is then sent an email.
[0010] In another embodiment, the state identification(s) of the lottery tickets presented from a given email address is(are) stored on a computer readable medium and used to speed the analysis of subsequent tickets presented from the same email address, the state lottery number comparisons being selected first from the states lotteries the email sender has used in the past.
[0011] In another embodiment, winning users are charged a fee for the identification of a winning number. This can be a flat fee or a percentage of the winnings. The fee may be charged, for example, for multiple tickets presented in an email (while single tickets are done for free), or after the user has had a trial time period or used the website a certain number of times.
[0012] In another embodiment the user is told how much he has won, and optionally, how much fee the user is being charged.
[0013] In yet another embodiment, the user is registered. This is done by either prompting at the receipt of an email, (either the first time or after a certain number of uses), or when visiting the website. Registration information can comprise the user's email address, credit card information for billing and the state lotteries the user uses most frequently. Preferably, a cookie is planted in the user's computer for ease of ingress and identification when the user responds to an email with an embedded link directing the user to the website.
[0014] The digitized image may be provided by a scanner, such as a flatbed scanner, a facsimile machine or a digital camera. The format of the digitized image may be GIF, JPEG, BMP, EPS, PIC, PNG, TIFF or any other standard. It is particularly preferred to digitize a plurality of tickets simultaneously.
[0015] Optical character recognition is then performed on the image to obtain the lottery numbers. Obtaining the date can be optional, as in the absence of a date it can be assumed that the date of the most recent lottery is intended. Similarly, obtaining the information about which is the state of origin of a ticket is optional in the case where the web site is that of a given state's lottery commission, in that it can safely be presumed that users of such a site will only submit tickets from that state. Note that state of origin information is sometimes provided symbolically rather than in alphanumeric form. For example, Pennsylvania lottery tickets contain the image of a keystone to indicate state origin. Information about the type of bet, such as boxed or straight, will only be required for games that allow it. Ideally, the optical character recognition program accommodates as many popular image formats as possible. OCR programs are readily available.
[0016] The lottery number information, and other information, obtained from the lottery tickets is compared to the winning number or numbers for the corresponding state, date, game, and type of bet. The winning numbers may be obtained by sending intelligent agents out over the Internet to search state lottery or commercial web sites, or from telephone hotlines, or news programs and the like. As such numbers are collected, they can be archived on a computer readable storage medium such as magnetic media such as a hard drive or a disc, optical media such as read-write CD-ROM, semiconductor media such as random access memory, and the like for fast retrieval.
[0017] A report is then issued to the user, advising the user whether there was a winning number. Preferably, the user is also advised as to which number it was. In a particularly preferred embodiment, the image originally provided by the user is displayed with the winning number indicated by highlighting in some fashion such as underlining, circling the number, making it bold, or changing the text of the winning number or background color behind the number to locate the position of the winning number within the image. If more than one ticket was scanned, then the winning ticket may also be so highlighted.
[0018] In yet another embodiment of the invention, the user's computer can be outfitted with the software for character recognition and also for sending out intelligent agents to one or more state or commercial web sites to find winning numbers for comparison and results reporting, without the aid of a web site providing the service.
[0019] In yet another embodiment of the invention, the user's computer can be outfitted with the software for character recognition. The user then not only digitizes the lottery ticket, but also performs optical character recognition on the digitized image to extract information from the lottery ticket(s) such as lottery numbers, date, type of bet and state. Information from the lottery ticket is then forwarded to the website by, for example, e-mail.
[0020] Although various embodiments of the invention are shown and described herein, they are not meant to be limiting, for example, those of skill in the art may recognize certain modifications to these embodiments, which modifications are meant to be covered by the spirit and scope of the appended claims.
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The invention allows a purchaser of lottery tickets to scan multiple lottery tickets at once, send the resulting image to a web site, where the web site will indicate to the purchaser whether any of the tickets are winners and also highlight on the image for the purchaser the location of a winning ticket in the image and also highlight where on the ticket the winning number is. The method for checking lottery tickets comprises the steps of digitizing at least one lottery ticket comprising lottery numbers to form an image, performing optical character recognition on the image to obtain the lottery numbers, comparing the lottery ticket lottery numbers to at least one winning lottery number and reporting the winning status of the at least one lottery ticket.
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TECHNICAL FIELD
[0001] This invention relates to fuel cells. More specifically, this invention relates to fuel cells that can be operated at relatively low temperatures. Additionally, this invention relates to fuel cells utilizing molten alkali hydroxide as an electrolyte, including eutectic mixtures.
BACKGROUND OF THE INVENTION
[0002] There have been a number of examples of fuel cells for converting hydrogen to electricity. Drawbacks of these prior art designs include the relatively high temperatures at which these fuel cells are operated, and the fact that many of these designs require relatively pure, and thus expensive, hydrogen as a fuel source to avoid contamination. As such, these prior art fuel cells cannot be operated using a wide variety of hydrogen containing fuels. Drawbacks of prior art fuel cells also include the use of relatively expensive materials for electrodes and electrolytes. The present invention is designed to overcome these drawbacks.
SUMMARY OF THE INVENTION
[0003] Accordingly, it is an object of the present invention to provide a fuel cell that operates efficiently at temperatures between 200° C. and 750° C. It is a further object of the present invention to provide a fuel cell that uses a highly conductive and very low-cost electrolyte. It is yet a further object of the present invention to provide a fuel cell that uses inexpensive base metal electrocatalysts. It is yet a further object of the present invention to provide a fuel cell that operates using a wide range of fuels. It is yet a further object of the present invention to provide a fuel cell that operates with fast electrode kinetics. It is yet a further object of the present invention to provide a fuel cell that allows for the direct use of ammonia as a fuel, even at temperatures as low as 200° C. It is yet a further object of the present invention to provide a molten alkaline hydroxide electrolyte fuel cell that provides very active intermediate oxygen species within the melt.
[0004] These and other objects are accomplished by the present invention which provides a molten alkali hydroxide fuel cell. The fuel cell may be of any number of configurations associated with molten salt type fuel cells, but generally the fuel cell of the present invention will include a chamber containing a molten alkali hydroxide electrolyte in contact with an anode and a cathode, a fluid pathway allowing hydrogen containing fluids to flow to the anode, and a fluid pathway allowing oxygen containing fluids to flow to the cathode.
[0005] The present invention is also a method for producing electricity using a molten alkali hydroxide fuel cell. The method of the present invention also generally involves the operation of a fuel cell configured as in any manner normally associated with molten salt type fuel cells, except that the present invention utilizes a molten alkali hydroxide as the electrolyte. Accordingly, the method of the present invention generally involves the steps of providing a chamber containing a molten alkali hydroxide electrolyte in contact with an anode and a cathode, providing hydrogen containing fluids to the anode, and providing oxygen containing fluids to the cathode. In this manner, an electrochemical reaction is promoted wherein the hydrogen from the hydrogen containing fluids are combined with the oxygen from the oxygen containing fluids to form water and generate electricity between the anode and the cathode.
[0006] While not meant to be limiting, hydrogen containing fluids include but are not limited to ammonia, hydrogen, hydrazine, methanol, ethanol, formic acid, propane, and combinations thereof. While not meant to be limiting, oxygen containing fluids include but are not limited to oxygen, air, peroxide of hydrogen or other materials, ozone, and combinations thereof.
[0007] As will be recognized by those having ordinary skill in the art, and as is typical in fuel cell configurations, it is preferred that the chamber containing a molten alkali hydroxide electrolyte in contact with an anode and a cathode is used in combination with a plurality of additional chambers also containing a molten alkali hydroxide electrolyte in contact with an anode and a cathode. In this manner, a series of fuel cells are used in combination to produce greater currents, voltages, and power. It is also preferred that the molten alkali hydroxide electrolyte is contained within a porous ceramic matrix in the individual cells.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The following detailed description of the embodiments of the invention will be more readily understood when taken in conjunction with the following drawings, wherein:
[0009] FIG. 1 is a schematic drawing of the molten hydroxide direct ammonia fuel cell used in the proof of principle experiments described herein.
[0010] FIG. 2 is a graph showing the polarization behavior of the molten hydroxide direct ammonia fuel cell used in the proof of principle experiments described herein operating at 200° C., 250° C., 300° C., 350° C., 400° C., and 450° C.
[0011] FIG. 3 is a graph showing the power production performance of the molten hydroxide direct ammonia fuel cell used in the proof of principle experiments described herein operating at 200° C., 250° C., 300° C., 350° C., 400° C., and 450° C.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0012] For the purposes of promoting an understanding of the principles of the invention, a series of experiments were conducted reducing the present invention to practice. In these experiments, a direct ammonia fuel cell utilizing a molten alkali hydroxide eutectic melt was fabricated and tested at various operating temperatures between 200° C. and 450° C. The use of a porous nickel anode and a porous cathode of lithiated nickel oxide provided stable cell performance for the duration of the testing. The polarization characteristics of the cell at different operating temperatures indicated that ohmic potential losses dominated the cell performance. A reduction in electrode separation distance and the use of a higher surface area, highly dispersed electrocatalyst at each electrode surface should increase overall cell performance over that shown in these experiments.
[0013] Reference will now be made to those experiments, and the embodiments of the present invention used therein. It will nevertheless be understood that no limitations of the inventive scope is thereby intended, as the scope of this invention should be evaluated with reference to the claims appended hereto. Alterations and further modifications in the illustrated devices, and such further applications of the principles of the invention as illustrated herein are contemplated as would normally occur to one skilled in the art to which the invention relates. For example, the cell described herein could easily be modified to utilize different geometries, such as, for example, and not meant to be limiting, a more traditional planar fuel cell design, a uniaxial tubular design, and a single chamber design. All such designs utilizing a pure molten alkali hydroxide and/or molten alkali hydroxide mixtures are hereby expressly contemplated by the present invention. Examples include, but are not limited to lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, and combinations thereof.
[0014] A schematic for the liquid-electrolyte fuel cell used in these experiments is shown in FIG. 1 . The cell container was machined from 7 cm diameter Nickel 400 (66.5% Ni, 31.5% Cu, 1.2% Fe, 1.1% Mn) bar stock cut to 15 cm in length. Nickel-400, also known as the commercial Monel® alloy, was chosen due to its resistance to corrosion by molten hydroxides. The bar was internally bored to a depth of 11 cm with a diameter of approximately 3.8 cm. This central well served to store the molten electrolyte. The cell was heated by three 200 W cartridge heaters inserted into holes in the bottom of the container. The top of the cell container was machined with a knife edge and bolt holes to mate with a standard 7 cm stainless steel conflat flange with copper gasket, which served as a cap for the container. The cap provided conduits for fuel and oxidant entry, as well as a combined vent and thermocouple access port.
[0015] The anode and cathode electrodes (Mott Corporation) were each 6.4 mm diameter nickel tubes, 18 cm in length, each with a 1.9 cm porous nickel cup (also 6.4 mm in diameter) welded to the end of the tube to create a porous metal sparger at the tube end. The porous spargers had an external superficial surface area of approximately 4 cm 2 , and this area was used for the calculation of the current and power densities produced by the cell. The electrode tubes were isolated from one another and the cell housing by Teflon® tubing sleeves. During cell operation, the electrodes were externally water-cooled to prevent melting the Teflon® sleeves. While immersed in the molten electrolyte, the two porous electrode ends were submerged to a depth of 10 cm and were separated by a lateral center-to-center distance of 2 cm. A direct electrical connection to the cell housing served as a reference electrode. This design proved to be reliable for cell operating temperatures of up to 450° C.
[0016] The cell was operated over a range of temperatures from 200 to 450° C. In each experiment, a stream of technical grade (99.99%) anhydrous ammonia was provided to the anode tube at a rate of 15 standard cubic centimeters per minute (sccm), which was automatically regulated by a calibrated mass flow controller. The oxidant provided to the cathode tube was a slight stoichiometric excess (60 sccm) of compressed air at room temperature and approximately 10% relative humidity. The air flow was manually adjusted and was measured with a calibrated mass flow meter. The molten electrolyte for each experiment was a eutectic mixture of sodium and potassium hydroxides (51 mol % NaOH, 49 mol % KOH, Alfa Aesar). This eutectic has the benefit of a much lower melting temperature (170° C.) compared to the melting temperatures of pure sodium and potassium hydroxides (323° C. and 360° C., respectively).
[0017] Fuel cell testing was accomplished by measuring the electrical current-potential (polarization) relationship by placing the cell in series with a controlled electronic load (TL5 Test Load, Astris Energi Inc.). The cell was monitored by defining an electric current to be produced by the cell, which the test load resistance was automatically adjusted to allow. The test current was increased from 0 (open circuit) to 200 mA by small steps, and at each prescribed current a resistance-free electrochemical potential measurement was made by interrupting the current for 0.1 ms. These i-V data allowed for the construction of polarization and power production plots.
[0018] It was initially determined that a nickel cathode was not optimal for operation within the caustic melt. As is common in molten carbonate fuel cells a nickel cathode quickly oxidized to nickel oxide (NiO), which has very limited electrical conductivity. The oxidation of the cathode could then cause irreversible polarization of the cell and a reduction in the electrochemical potential and consequently the power available from the cell.
[0019] This situation is remedied by a number of techniques, including, but not limited to, lithiation of the nickel oxide cathode—doping the nickel with lithium. In this manner, the electrical resistance of the oxide layer is greatly decreased. To produce lithiated nickel oxide from the porous metallic nickel electrode, a thermal-electrochemical treatment procedure was developed. The porous nickel cathode was treated in a 3 M LiOH solution maintained at 100° C. for 24 hours while applying an anodic current of 1 mA/cm 2 . In this single-step treatment, nickel metal is thermally and electrochemically converted first into a hydrated nickel oxide, which is further electrochemically oxidized and lithiated by cationic exchange to produce stoichiometric variants of LiNiO 2 . The lithiated nickel sparger is much more stable in the melt and does not polarize or deactivate over time.
[0020] The polarization and power production characteristics of the cell at various temperatures appear in FIGS. 2 and 3 , respectively. As the cell operating temperature increased, the open cell potential dropped slightly, which is consistent with the expected cell thermodynamics. Open cell potential at 200° C. was approximately 820 mV, and 811 mV at 450° C. This small thermodynamic potential loss was more than compensated for by the increased conductivity of the electrolyte as temperature increased, leading to less potential loss at higher electrical currents. Consequently, the peak cell performance was achieved at the highest temperature (450° C.), where a power density of approximately 40 mW/cm 2 was delivered at a current density of approximately 94 mA/cm 2 .
[0021] It should be noted that, although the cell used in these proof of principle experiments did not perform at optimal levels, the electrode separation in the liquid electrolyte cell described here (2 cm) is many orders of magnitude greater than that common in current state of the art solid state fuel cells (typically less than 1 mm). Accordingly, as will be recognized by those having ordinary skill in the art, the present invention will perform at more optimal levels by decreasing the distance between the electrodes, as compared to that described in these experiments. This disclosure should be interpreted to encompass all such arrangements.
[0022] Given the superior ionic conductivity of the hydroxide melt, isolation of a molten hydroxide eutectic within a thin, inert ceramic matrix tile should greatly reduce ohmic potential losses. It is clear from the linear nature of the data appearing in FIG. 2 that ohmic potential losses are significant for this exemplary system. Additionally, the porous metal spargers are not constructed of a finely divided metal or metal oxide catalyst as is the case in state-of-the-art planar fuel cell stacks. Consequently, the available surface area for reaction and ionization (or product formation) was likely far less may be possible with advanced electrodes. Bubbling the reactant gases through the spargers had the added detriment of consistent blockage of the electrode area from the electrolyte, likely greatly reducing the cell current density. Accordingly, it is preferred that the electrocatalyst have as high a surface area as is possible on a high surface area support. Suitable supports include but are not limited to layers of porous submicron metallic particles, ceramic metal mixtures including fine particles of ceramics, fine particles of metals, and combinations thereof, finely divided catalytic metals on electrically conducting material of more limited catalytic activity.
[0023] 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. Only certain embodiments have been shown and described, and all changes, equivalents, and modifications that come within the spirit of the invention described herein are desired to be protected. Any experiments, experimental examples, or experimental results provided herein are intended to be illustrative of the present invention and should not be considered limiting or restrictive with regard to the invention scope. Further, any theory, mechanism of operation, proof, or finding stated herein is meant to further enhance understanding of the present invention and is not intended to limit the present invention in any way to such theory, mechanism of operation, proof, or finding.
[0024] Thus, the specifics of this description and the attached drawings should not be interpreted to limit the scope of this invention to the specifics thereof. Rather, the scope of this invention should be evaluated with reference to the claims appended hereto. In reading the claims it is intended that when words such as “a”, “an”, “at least one”, and “at least a portion” are used there is no intention to limit the claims to only one item unless specifically stated to the contrary in the claims. Further, when the language “at least a portion” and/or “a portion” is used, the claims may include a portion and/or the entire items unless specifically stated to the contrary. Likewise, where the term “input” or “output” is used in connection with an electric device or fluid processing unit, it should be understood to comprehend singular or plural and one or more signal channels or fluid lines as appropriate in the context. Finally, all publications, patents, and patent applications cited in this specification are herein incorporated by reference to the extent not inconsistent with the present disclosure as if each were specifically and individually indicated to be incorporated by reference and set forth in its entirety herein.
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A fuel cell having at least one chamber containing a molten alkali hydroxide electrolyte in contact with an anode and a cathode, a fluid pathway allowing hydrogen containing fluids to flow to the anode, and a fluid pathway allowing oxygen containing fluids to flow to the cathode.
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RELATED APPLICATION
[0001] This application is a continuation of U.S. patent application Ser. No. 14/534,631, filed Nov. 6, 2014 and entitled Soft Through Air Dried Tissue, which in turn is a divisional of U.S. patent application Ser. No. 13/837,685, filed Mar. 15, 2013 and entitled Soft Through Air Dried Tissue, issued as U.S. Pat. No. 8,968,517, which in turn claims priority to U.S. Provisional Application Ser. No. 61/679,337, filed Aug. 3, 2012 and entitled Soft Through Air Dried Tissue, the contents of these applications being incorporated herein by reference in their entirety.
FIELD OF THE INVENTION
[0002] The present invention is directed to tissue, and in particular to a multilayer tissue including wet end additives.
BACKGROUND
[0003] According to conventional tissue-making processes, a slurry of pulp mixture is fed to a headbox, where the mixture is laid onto a forming surface so as to form a web. The web is then dried using pressure and/or heat to form the finished tissue. Prior to drying, the pulp mixture is considered to be in the “wet end” of the tissue making process. Additives may be used in the wet end to impart a particular attribute or chemical state to the tissue. However, using additives in the wet end has some disadvantages. For example, a large amount of additive may be required in the pulp mixture to achieve the desired effect on the finished tissue, which in turn leads to increased cost and, in the case of wet end additive debonder, may actually reduce the tissue strength. In order to avoid drawbacks associated with wet end additives, agents, such as softeners, have been added topically after web formation.
[0004] The tissue web may be dried by transferring the web to a forming surface and then directing a flow of heated air onto the web. This process is known as through air drying (TAD). While topical softeners have been used in combination with through air dried tissue, the resulting products have had a tamped down or flattened surface profile. The flattened surface profile in turn hinders the cleaning ability of the tissue and limits the overall effectiveness of the softener.
SUMMARY OF THE INVENTION
[0005] An object of the present invention is to provide a tissue manufacturing method that uses through air drying without compromising softness and cleaning ability of the resulting tissue.
[0006] Another object of the present invention is to provide a tissue manufacturing method that avoids the disadvantages associated with wet end additives, and in particular avoids the use of a large amount of additive to achieve the desired effect on the resulting tissue.
[0007] A multi-layer through air dried tissue according to an exemplary embodiment of the present invention comprises a first exterior layer, an interior layer and a second exterior layer. The interior layer includes a first wet end additive comprising an ionic surfactant and a second wet end additive comprising a non-ionic surfactant.
[0008] A multi-layer through air dried tissue according to another exemplary embodiment of the present invention comprises a first exterior layer comprised substantially of hardwood fibers, an interior layer comprised substantially of softwood fibers, and a second exterior layer comprised substantially of hardwood fibers. The interior layer includes a first wet end additive comprising an ionic surfactant and a second wet end additive comprising a non-ionic surfactant.
[0009] In at least one exemplary embodiment, the first exterior layer further comprises a wet end temporary wet strength additive.
[0010] In at least one exemplary embodiment, the first exterior layer further comprises a wet end dry strength additive.
[0011] In at least one exemplary embodiment, the second exterior layer further comprises a wet end dry strength additive.
[0012] In at least one exemplary embodiment, the second wet end additive comprises an ethoxylated vegetable oil.
[0013] In at least one exemplary embodiment, the second wet end additive comprises a combination of ethoxylated vegetable oils.
[0014] In at least one exemplary embodiment, the ratio by weight of the second wet end additive to the first wet end additive in the tissue is at least eight to one.
[0015] In at least one exemplary embodiment, the ratio by weight of the second wet end additive to the first wet end additive in the first interior layer is at most ninety to one.
[0016] In at least one exemplary embodiment, the tissue has a softness (hand feel) of at least 90.
[0017] In at least one exemplary embodiment, the tissue has a bulk softness of less than 10 TS7.
[0018] In at least one exemplary embodiment, the ionic surfactant comprises a debonder.
[0019] In at least one exemplary embodiment, the tissue has a tensile strength of at least 35 N/m, a softness of at least 90 and a basis weight of less than 25 gsm.
[0020] In at least one exemplary embodiment, the tissue has a tensile strength of at least 35 N/m, a softness of at least 90 and a caliper of less than 650 microns.
[0021] In at least one exemplary embodiment, the wet end temporary wet strength additive comprises glyoxalated polyacrylamide.
[0022] In at least one exemplary embodiment, the wet end dry strength additive comprises amphoteric starch.
[0023] In at least one exemplary embodiment, the first exterior layer further comprises a dry strength additive.
[0024] In at least one exemplary embodiment, the first and second exterior layers are substantially free of any surface deposited softener agents or lotions.
[0025] In at least one exemplary embodiment, at least one of the first or second exterior layers comprises a surface deposited softener agent or lotion.
[0026] In at least one exemplary embodiment, the tissue has a softness of at least 95.
[0027] In at least one exemplary embodiment, the non-ionic surfactant has a hydrophilic-lipophilic balance of less than 10, and preferably less than 8.5.
[0028] In at least one exemplary embodiment, the tissue may have a softness of at least 95.
[0029] In at least one exemplary embodiment, the first exterior layer is comprised of at least 75% by weight of hardwood fibers.
[0030] In at least one exemplary embodiment, the interior layer is comprised of at least 75% by weight of softwood fibers.
[0031] Other features and advantages of embodiments of the invention will become readily apparent from the following detailed description, the accompanying drawings and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0032] Exemplary embodiments of the present invention will be described with references to the accompanying figures, wherein:
[0033] FIG. 1 is a schematic diagram of a three layer tissue in accordance with an exemplary embodiment of the present invention;
[0034] FIG. 2 shows a micrograph of the surface of a tissue according to an exemplary embodiment of the invention without a topical additive;
[0035] FIG. 3 shows a micrograph of the surface of a conventional through air dried tissue with a flattened surface texture; and
[0036] FIG. 4 is a block diagram of a system for manufacturing tissue according to an exemplary embodiment of the present invention.
DETAILED DESCRIPTION
[0037] The present invention is directed to a soft tissue made with a combination of a wet end added ionic surfactant and a wet end added nonionic surfactant. The tissue may be made up of a number of layers, including exterior layers and an interior layer. In at least one exemplary embodiment, pulp mixes for each tissue layer are prepared individually.
[0038] FIG. 1 shows a three layer tissue, generally designated by reference number 1 , according to an exemplary embodiment of the present invention. The tissue 1 has external layers 2 and 4 as well as an internal, core layer 3 . External layer 2 is composed primarily of hardwood fibers 20 whereas external layer 4 and core layer 3 are composed of a combination of hardwood fibers 20 and softwood fibers 21 . The internal core layer 3 includes an ionic surfactant functioning as a debonder 5 and a non-ionic surfactant functioning as a softener 6 . As explained in further detail below, external layers 2 and 4 also include non-ionic surfactant that migrated from the internal core layer 3 during formation of the tissue 1 . External layer 2 further includes a dry strength additive 7 . External layer 4 further includes both a dry strength additive 7 and a temporary wet strength additive 8 .
[0039] Pulp mixes for exterior layers of the tissue are prepared with a blend of primarily hardwood fibers. For example, the pulp mix for at least one exterior layer is a blend containing about 70 percent or greater hardwood fibers relative to the total percentage of fibers that make up the blend. As a further example, the pulp mix for at least one exterior layer is a blend containing about 90-100 percent hardwood fibers relative to the total percentage of fibers that make up the blend.
[0040] Pulp mixes for the interior layer of the tissue are prepared with a blend of primarily softwood fibers. For example, the pulp mix for the interior layer is a blend containing about 70 percent or greater softwood fibers relative to the total percentage of fibers that make up the blend. As a further example, the pulp mix for the interior layer is a blend containing about 90-100 percent softwood fibers relative to the total percentage of fibers that make up the blend.
[0041] As known in the art, pulp mixes are subjected to a dilution stage in which water is added to the mixes so as to form a slurry. After the dilution stage but prior to reaching the headbox, each of the pulp mixes are dewatered to obtain a thick stock of about 95% water. In an exemplary embodiment of the invention, wet end additives are introduced into the thick stock pulp mixes of at least the interior layer. In an exemplary embodiment, a non-ionic surfactant and an ionic surfactant are added to the pulp mix for the interior layer. Suitable non-ionic surfactants have a hydrophilic-lipophilic balance of less than 10, and preferably less than or equal to 8.5. An exemplary non-ionic surfactant is an ethoxylated vegetable oil or a combination of two or more ethoxylated vegetable oils. Other exemplary non-ionic surfactants include ethylene oxide, propylene oxide adducts of fatty alcohols, alkylglycoside esters, and alkylethoxylated esters.
[0042] Suitable ionic surfactants include but are not limited to quaternary amines and cationic phospholipids. An exemplary ionic surfactant is 1,2-di(heptadecyl)-3-methyl-4,5-dihydroimidazol-3-ium methyl sulfate. Other exemplary ionic surfactants include (2-hydroxyethyl)methylbis[2-[(1-oxooctadecyl)oxy]ethyl]ammonium methyl sulfate, fatty dialkyl amine quaternary salts, mono fatty alkyl tertiary amine salts, unsaturated fatty alkyl amine salts, linear alkyl sulfonates, alkyl-benzene sulfonates and trimethyl-3-[(1-oxooctadecyl)amino]propylammonium methyl sulfate.
[0043] In an exemplary embodiment, the ionic surfactant may function as a debonder while the non-ionic surfactant functions as a softener. Typically, the debonder operates by breaking bonds between fibers to provide flexibility, however an unwanted side effect is that the overall strength of the tissue can be reduced by excessive exposure to debonder. Typical debonders are quaternary amine compounds such as trimethyl cocoammonium chloride, trymethyloleylammonium chloride, dimethyldi(hydrogenated-tallow)ammonium chloride and trimethylstearylammonium chloride.
[0044] After being added to the interior layer, the non-ionic surfactant (functioning as a softener) migrates through the other layers of the tissue while the ionic surfactant (functioning as a debonder) stays relatively fixed within the interior layer. Since the debonder remains substantially within the interior layer of the tissue, softer hardwood fibers (that may have lacked sufficient tensile strength if treated with a debonder) can be used for the exterior layers. Further, because only the interior of the tissue is treated, less debonder is required as compared to when the whole tissue is treated with debonder.
[0045] In an exemplary embodiment, the ratio of ionic surfactant to non-ionic surfactant added to the pulp mix for the interior layer of the tissue is between 1:4 and 1:90 parts by weight and preferably about 1:8 parts by weight. In particular, when the ionic surfactant is a quaternary amine debonder, reducing the concentration relative to the amount of non-ionic surfactant can lead to an improved tissue. Excess debonder, particularly when introduced as a wet end additive, can weaken the tissue, while an insufficient amount of debonder may not provide the tissue with sufficient flexibility. Because of the migration of the non-ionic surfactant to the exterior layers of the tissue, the ratio of ionic surfactant to non-ionic surfactant in the core layer may be significantly lower in the actual tissue compared to the pulp mix.
[0046] In an exemplary embodiment, a dry strength additive is added to the thick stock mix for at least one of the exterior layers. The dry strength additive may be, for example, amphoteric starch, added in a range of about 1 to 40 kg/ton. In another exemplary embodiment, a wet strength additive is added to the thick stock mix for at least one of the exterior layers. The wet strength additive may be, for example, glyoxalated polyacrylamide, commonly known as GPAM, added in a range of about 0.25 to 5 kg/ton. In a further exemplary embodiment, both a dry strength additive, preferably amphoteric starch and a wet strength additive, preferably GPAM are added to one of the exterior layers. Without being bound by theory, it is believed that the combination of both amphoteric starch and GPAM in a single layer when added as wet end additives provides a synergistic effect with regard to strength of the finished tissue. Other exemplary temporary wet-strength agents include aldehyde functionalized cationic starch, aldehyde functionalized polyacrylamides, acrolein co-polymers and cis-hydroxyl polysachharide (guar gum and locust bean gum) used in combination with any of the above mentioned compounds.
[0047] In addition to amphoteric starch, suitable dry strength additives may include but are not limited to glyoxalated polyacrylamide, cationic starch, carboxy methyl cellulose, guar gum, locust bean gum, cationic polyacrylamide, polyvinyl alcohol, anionic polyacrylamide or a combination thereof.
[0048] FIG. 4 is a block diagram of a system for manufacturing tissue, generally designated by reference number 100 , according to an exemplary embodiment of the present invention. The includes an first exterior layer fan pump 102 , a core layer fan pump 104 , a second exterior layer fan pump 106 , a headbox 108 , a forming section 110 , a drying section 112 and a calendar section 114 . The first and second exterior layer fan pumps 102 , 106 deliver the pulp mixes of the first and second external layers 2 , 4 to the headbox 108 , and the core layer fan pump 104 delivers the pulp mix of the core layer 3 to the headbox 108 . As is known in the art, the headbox delivers a wet web of pulp onto a forming wire within the forming section 110 . The wet web is laid on the forming wire with the core layer 3 disposed between the first and second external layers 2 , 4 .
[0049] After formation in the forming section 110 , the partially dewatered web is transferred to the drying section 112 , Within the drying the section 112 , the tissue of the present invention may be dried using conventional through air drying processes. In an exemplary embodiment, the tissue of the present invention is dried to a humidity of about 7 to 20% using a through air drier manufactured by Metso Corporation, of Helsinki, Finland. In another exemplary embodiment of the invention, two or more through air drying stages are used in series. Without being bound by theory, it is believed that the use of multiple drying stages improves uniformity in the tissue, thus reducing tears.
[0050] In an exemplary embodiment, the tissue of the present invention is patterned during the through air drying process. Such patterning can be achieved through the use of a TAD fabric, such as a G-weave (Prolux 003) or M-weave (Prolux 005) TAD fabric.
[0051] After the through air drying stage, the tissue of the present invention may be further dried in a second phase using a Yankee drying drum. In an exemplary embodiment, a creping adhesive is applied to the drum prior to the tissue contacting the drum. A creping blade is then used to remove the tissue from the Yankee drying drum. The tissue may then be calendered in a subsequent stage within the calendar section 114 . According to an exemplary embodiment, calendaring may be accomplished using a number of calendar rolls (not shown) that deliver a calendering pressure in the range of 0-100 pounds per linear inch (PLI). In general, increased calendering pressure is associated with reduced caliper and a smoother tissue surface.
[0052] According to an exemplary embodiment of the invention, a ceramic coated creping blade is used to remove the tissue from the Yankee drying drum. Ceramic coated creping blades result in reduced adhesive build up and aid in achieving higher run speeds. Without being bound by theory, it is believed that the ceramic coating of the creping blades provides a less adhesive surface than metal creping blades and is more resistant to edge wear that can lead to localized spots of adhesive accumulation. The ceramic creping blades allow for a greater amount of creping adhesive to be used which in turn provides improved sheet integrity and faster run speeds.
[0053] In addition to the use of wet end additives, the tissue of the present invention may also be treated with topical or surface deposited additives. Examples of surface deposited additives include softeners for increasing fiber softness and skin lotions. Examples of topical softeners include but are not limited to quaternary ammonium compounds, including, but not limited to, the dialkyldimethylammonium salts (e.g. ditallowdimethylammonium chloride, ditallowdimethylammonium methyl sulfate, di(hydrogenated tallow)dimethyl ammonium chloride, etc.). Another class of chemical softening agents include the well-known organo-reactive polydimethyl siloxane ingredients, including amino functional polydimethyl siloxane. zinc stearate, aluminum stearate, sodium stearate, calcium stearate, magnesium stearate, spermaceti, and steryl oil.
[0054] The below discussed values for softness (i.e., hand feel (HF)), caliper and tensile strength of the inventive tissue were determined using the following test procedures:
[0055] Softness Testing
[0056] Softness of a tissue sheet was determined using a Tissue Softness Analyzer (TSA), available from emtec Electronic GmbH of Leipzig, Germany. A punch was used to cut out three 100 cm 2 round samples from the sheet. One of the samples was loaded into the TSA with the yankee side facing up. The sample was clamped in place and the TPII algorithm was selected from the list of available softness testing algorithms displayed by the TSA. After inputting parameters for the sample, the TSA measurement program was run. The test process was repeated for the remaining samples and the results for all the samples were averaged.
[0057] Caliper Testing
[0058] A Thwing-Albert ProGage 100 Thickness Tester, manufactured by Thwing Albert of West Berlin, N.J. was used for the caliper test. Eight 100 mm×100 mm square samples were cut from a base sheet. Each sample was folded over on itself, with the rougher layer, typically corresponding air layer facing itself. The samples were then tested individually and the results were averaged to obtain a caliper result for the base sheet.
[0059] Tensile Strength Testing
[0060] An Instron 3343 tensile tester, manufactured by Instron of Norwood, Mass., with a 100N load cell and 25.4 mm rubber coated jaw faces was used for tensile strength measurement. Prior to measurement, the Instron 3343 tensile tester was calibrated. After calibration, 8 strips, each one inch by eight inches, were provided as samples for testing. One of the sample strips was placed in between the upper jaw faces and clamp, and then between the lower jaw faces and clamp. A tensile test was run on the sample strip. The test procedure was repeated until all the samples were tested. The values obtained for the eight sample strips were averaged to determine the tensile strength of the tissue.
[0061] Tissue according to exemplary embodiments of the present invention has an improved softness as compared to conventional tissue. Specifically, the tissue of the present invention may have a softness or hand feel (HF) of at least 90. In another exemplary embodiment, the tissue of the present invention may have a softness of at least 95.
[0062] In another exemplary embodiment, the tissue has a bulk softness of less than 10 TS7 (as tested by a TSA). In an exemplary embodiment, the tissue of the present invention also has a basis weight for each ply of less than 22 grams per square meter. For such a soft, thin tissue the initial processing conditions may be defined so as to have a moisture content between 1.5 to 5%.
[0063] In another exemplary embodiment, the tissue of the present invention has a basis weight for each ply of at least 17 grams per square meter, more preferably at least 20 grams per square meter and most preferably at least 22 grams per square meter.
[0064] Tissue according to exemplary embodiments of the present invention has a good tensile strength in combination with improved softness and/or a lower basis weight or caliper as compared to conventional tissue. Without being bound by theory, it is believed that the process of the present invention allows the tissue to retain more strength, while still having superior softness without the need to increase the thickness or weight of the tissue. Specifically, the tissue of the present invention may have improved softness and/or strength while having a caliper of less than 650 microns.
[0065] Tissue according to exemplary embodiments of the present invention has a combination of improved softness with a high degree of uniformity of surface features. FIG. 2 shows a micrograph of the surface of a tissue according to an exemplary embodiment of the invention without a topical additive and FIG. 3 shows a micrograph of the surface of a conventional through air dried tissue with a flattened surface texture. The tissue of FIG. 2 has a high degree of uniformity in its surface profile, with regularly spaced features, whereas the tissue of FIG. 3 has flattened regions and a nonuniform profile.
[0066] The tissue of the present invention may also be calendered or treated with a topical softening agent to alter the surface profile. In exemplary embodiments, the surface profile can be made smoother by calendering or through the use of a topical softening agent. The surface profile may also be made rougher via microtexturing.
[0067] The following examples are provided to further illustrate the invention.
Example 1
[0068] Through air dried tissue was produced with a three layer headbox and a 005 Albany TAD fabric. The flow to each layer of the headbox was about 33% of the total sheet. The three layers of the finished tissue from top to bottom were labeled as air, core and dry. The air layer is the outer layer that is placed on the TAD fabric, the dry layer is the outer layer that is closest to the surface of the Yankee dryer and the core is the center section of the tissue. The tissue was produced with 45% eucalyptus fiber in the air layer, 50% eucalyptus fiber in the core layer and 100% eucalyptus fiber in the dry layer. Headbox pH was controlled to 7.0 by addition of a caustic to the thick stock before the fan pumps for all samples.
[0069] Roll size was about 10,000 meters long. The number of sheet-breaks per roll was determined by detecting the number of breaks in the sheet per every 10,000 meters of linear (MD-machine direction) sheet run.
[0070] The tissue according to Example 1 was produced with addition of a temporary wet strength additive, Hercobond 1194 (Ashland, 500 Hercules Road, Wilmington Del., 19808) to the air layer, a dry strength additive, Redibond 2038 (Corn Products, 10 Finderne Avenue, Bridgewater, N.J. 08807) split 75% to the air layer, 25% to the dry layer, and a softener/debonder, T526 (EKA Chemicals Inc., 1775 West Oak Commons Court, Marietta, Ga., 30062) added in combination to the core layer. The T526 is a softener/debonder combination with a quaternary amine concentration below 20%.
Example 2
[0071] Example 2 was produced with the same conditions as Example 1, but chemical addition rates were changed. Specifically, the amount of dry strength additive (Redibond 2038) was increased from 5.0 kg/ton to 10.0 kg/ton and the amount of softener/debonder (T526) was increased from 2.0 kg/ton to 3.6 kg/ton.
Example 3
[0072] Example 3 was produced with the same conditions as Example 1 except with T526 added to the dry layer.
Example 4
[0073] Example 4 was produced with the same conditions as Example 1 except for the addition of a debonder having a high quaternary amine concentration (>20%) to the core layer. The debonder was F509HA (manufactured by EKA Chemicals Inc., 1775 West Oak Commons Court, Marietta, Ga., 30062).
Comparative Example 1
[0074] Comparative Example 1 was produced with the same conditions as Example 1 except that wet end additives were not used
[0075] Table 1 shows performance data and chemical dose information for the TAD base-sheet of Examples 1-4 and Comparative Example 1. The basis weight (BW) of each Example was about 20.7 GSM.
[0000]
TABLE 1
Hercobond D1194
Redibond 2038
EKA
Sheet-
MD/CD
kg/ton (temporary
kg/ton (temporary
T526 kg/ton
breaks
Tensile
Lint
wet strength
dry strength
(Softener/
per
Sample
HF 1
n/m 2
Value 3
additive)
additive)
debonder)
roll
Comparative
93.8
55/27
11.5
0
0
0
3
Example 1
Example 1
98.2
54/34
9.0
1.25
5.0
2.0
0
Example 2
95.1
56/38
7.5
1.25
10
3.6
0
Example 3
91.5
57/39
12.0
1.25
5.0
2.0
1
Example 4
90.5
55/35
9.8
1.25
10
0.81 (F509HA)
0
1 All HF values are from single ply basesheet samples with dry side surface up.
2 Basesheet single ply data.
3 Post converted two ply product tested.
[0076] Examples 1 and 2 had a much higher hand-feel (HF) with lower lint value and improved machine efficiency compared to Comparative Example 1. Of note, these improved parameters were achieved while maintaining the same sheet MD/CD tensile range for both Examples 1 and 2 as in Comparative Example 1. The wet end chemical additives of Example 1 significantly improved product softness. Example 2 is a further improvement over Example 1 with a reduced lint value. This improvement in Example 2 was achieved by increasing the Redibond 2038 and T526 dose.
[0077] Softness as determined by the TSA was significantly reduced when softener/debonder was added to the dry layer (Example 3) and when a tissue debonder having a higher quaternary amine concentration was added to the core layer (Example 4). The preferred option is to add a combination of softener/debonder to core layer which allows the softener to migrate to surface layers and adjust chemical bonding in the dry layer to control product lint level (Example 1).
[0078] The tissue of the present invention also exhibits an improved surface profile that provides for improved product consistency and fewer defects that may otherwise cause sheet breaks. Specifically, the roughness of tissue can be characterized using two values, Pa (Average Primary Amplitude) and Wc (Average Peak to Valley Waviness). Pa is a commonly used roughness parameter and is computed as the average distance between each roughness profile point and the meanline. Wc is computed as the average peak height plus the average valley depth (both taken as positive values) relative to the meanline. As described in more detail below, the tissue of the present invention is measured to have Pa and Wc values that are both low and relatively uniform compared to conventional TAD tissue products.
[0079] The below discussed values for Pa and Wc of the inventive tissue were determined using the following test procedures:
[0080] Pa and Wc Testing
[0081] Ten samples of each tissue to be tested were prepared, with each sample being a 10 cm by 10 cm strip. Each sample was mounted and held in place with weights. Each sample was placed into a Marsurf GD 120 profilometer, available from Mahr Federal Instruments of Gottingen, Germany, and oriented in the CD direction. A 5 μm tip was used for the profilometer. Twenty scans were run on the profilometer per sample (ten in the forwards direction and ten in the backwards direction). The reverse scans were performed by turning the sample 180 degrees prior to scanning. Each scan covered a 30 mm length. The collected surface profile data was then transferred to a computer running OmniSurf analysis software, available from Digital Metrology Solutions, Inc. of Columbus, Ind., USA. The roughness profile setting for the OmniSurf software was set with a short filter low range of 25 microns and a short filter high range of 0.8 mm. The waviness profile setting of the OmniSurf software was set to a low range of 0.8 mm. For each sample, values for Pa (Average Primary Amplitude) and Wc (Average Peak to Valley Waviness) were calculated by the Omni Surf software. The calculated values of Pa and Wc for all twenty scans were averaged to obtain Pa and Wc values for each tissue sample. The standard deviation of the individual sample Pa and Wc values were also calculated.
[0082] The following examples are provided to further illustrate the invention.
Example 5
[0083] Two plies were produced, with each ply being equivalent to the three-layer structure formed in Example 1. The two plies were then embossed together to form a finished tissue product.
Comparative Example 2
[0084] Two plies were produced and embossed together as in Example 5, except that wet end additives were not used.
[0085] Table 2 shows the Pa and Pa standard deviation of several commercial products, Example 5, and Comparative Example 2 and 3.
[0000]
TABLE 2
LOCATION
DATE
PUR-
PUR-
SAMPLE
Pa
S.D
CHASED
CHASED
Charmin Basic
82.58245
9.038986
Wal-Mart -
July 2012
Anderson
Charmin Strong
57.03765
8.130364
Target -
July 2012
Anderson SC
Charmin Soft
47.3826
9.72459
Wal-Mart -
June 2012
Anderson
Charmin Soft
79.33375
9.620164
Wal-Mart -
January 2012
Anderson
Charmin Strong
70.6232
11.32204
Wal-Mart -
January 2012
Anderson
Cottonelle
100.9827
11.21668
Wal-Mart -
January 2012
Clean Care
Anderson
Cottonelle
90.5762
13.82119
Wal-Mart -
January 2012
Ultra
Anderson
Comfort Care
Target UP &
65.9598
12.45098
Target -
September
UP Soft and
Anderson SC
2012
Strong
Comparative
86.2806
9.46203
Example 2
Example 5
41.66115
2.19889
[0086] Table 3 shows the Wc and Wc standard deviation of several commercial products, Example 5, and Comparative Example 2.
[0000]
TABLE 3
LOCATION
DATE
PUR-
PUR-
SAMPLE
Wc
S.D
CHASED
CHASED
Charmin Basic
181.2485
31.50583
Wal-Mart -
July 2012
Anderson
Charmin Strong
163.4448
37.6021
Target -
July 2012
Anderson SC
Charmin Soft
147.54785
38.41011
Wal-Mart -
June 2012
Anderson
Charmin Soft
185.51195
30.68851
Wal-Mart -
January 2012
Anderson
Charmin Strong
216.1236
49.08633
Wal-Mart -
January 2012
Anderson
Cottonelle
307.39355
34.06675
Wal-Mart -
January 2012
Clean Care
Anderson
Cottonelle
286.33735
51.90506
Wal-Mart -
January 2012
Ultra
Anderson
Comfort Care
Target UP &
228.9568
59.57366
Target -
September
UP Soft and
Anderson SC
2012
Strong
Comparative
239.8652
54.96261
Example 2
Example 5
123.41615
14.97908
[0087] Tables 1 and 2 show the improved surface roughness characteristics of the inventive tissue as compared to commercially available products as well as similar tissue products that were not produced with wet end additives. Specifically, the tissue according to various exemplary embodiments of the present invention has an average Wc value of 140 or less, and more preferably 135 or less, with a Wc standard deviation (i.e., Waviness Uniformity) of 27 or less. Further, the tissue according to various exemplary embodiments of the present invention has an average Pa value of 50 or less, with a Wc standard deviation (i.e., Amplitude Uniformity) of 8 or less.
[0088] As known in the art, the tissue web is subjected to a converting process at or near the end of the web forming line to improve the characteristics of the web and/or to convert the web into finished products. On the converting line, the tissue web may be unwound, printed, embossed and rewound. According to an exemplary embodiment of the invention, the paper web on the converting lines may be treated with corona discharge before the embossing section. This treatment may be applied to the top ply and/or bottom ply. Nano cellulose fibers (NCF), nano crystalline cellulose (NCC), micro-fibrillated cellulose (MCF) and other shaped natural and synthetic fibers may be blown on to the paper web using a blower system immediately after corona treatment. This enables the nano-fibers to adsorb on to the paper web through electro-static interactions.
[0089] As discussed, according to an exemplary embodiment of the invention, a debonder is added to at least the interior layer as a wet end additive. The debonder provides flexibility to the finished tissue product. However, the debonder also reduces the strength of the tissue web, which at times may result in sheet breaks during the manufacturing process. The relative softness of the tissue web results in inefficiencies in the rewind process that must be performed in order to correct a sheet break. Accordingly, as shown in FIG. 4 , in an exemplary embodiment of the present invention, a switching valve 120 is used to control delivery of the debonder as a wet-end additive to the interior layer. In particular, when a sheet break is detected using, for example, conventional sheet break detection sensors, the switching valve 120 may be controlled to prevent further delivery of the debonder. This results in less flexibility and increased strength at the portion of the tissue web to be rewound, thereby allowing for a more efficient rewind process. Once the rewind process is completed, the switching valve may be opened to continue delivery of the debonder.
[0090] In addition to the use of a sheet break detection sensor, the switching valve 120 may also be controlled during turn up, the process whereby the tissue web is one transferred from on roll to another. The turn up process can result in higher stresses on the tissue web that normal operation, thus increasing the chance of sheet breaks. The switching valve 120 is turned off prior to turn up, thus increasing the strength of the tissue web. After the tissue web has begun winding on a new roll, the switching valve 120 is turned on again. The resulting roll of basesheet material thus has a section of higher strength tissue web at the center of the roll and may have a section of higher strength tissue on the outside of the roll. During finishing, the exterior section of higher strength tissue is removed and recycled. The interior section of higher strength tissue is not used to make a finished tissue. Thus, only the portion of the roll of basesheet tissue containing debonder is used to make finished tissue.
[0091] Now that embodiments of the present invention have been shown and described in detail, various modifications and improvements thereon will become readily apparent to those skilled in the art. Accordingly, the spirit and scope of the present invention is to be construed broadly and not limited by the foregoing specification.
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A process for manufacturing tissue including providing a first pulp mix, delivering a wet-end additive to the first pulp mix at a first point in the process, forming a tissue web comprising the first pulp mix after the first point in the process, monitoring the tissue web for breaks and preventing delivery of the wet-end additive to the first pulp mix at the first point in response to detecting a break in the monitoring step. In an exemplary embodiment, a switching valve is used to control delivery of the wet-end additive to the first pulp mix.
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CROSS REFERENCE TO RELATED APPLICATIONS
This is a continuation, of application Ser. No. 858,302 filed Dec. 7, 1977, now U.S. Pat. No. 4,230,700, which is a continuation of application Ser. No. 677,133 filed Apr. 15, 1976, now abandoned, which is a continuation of application Ser. No. 582,573 filed June 2, 1975, now abandoned, which is a continuation-in-part of application Ser. No. 361,354, filed May 17, 1973, now abandoned, which is a continuation-in-part of application Ser. No. 260,939, filed June 8, 1972 now abandoned.
BACKGROUND OF THE INVENTION
This invention relates to novel pharmaceutical compositions having therapeutic and prophylactic effects in disease conditions involving calcium phosphate metabolism. The invention further relates to a novel method for treating or preventing certain pathological conditions in animals.
A number of pathological conditions which can afflict warm-blooded animals are characterized by anomalous mobilization of calcium and phosphate leading to general or specific bone loss and/or excessively high calcium and phosphate levels in the fluids of the body. These conditions include osteoporosis, a disease process in which bone hard tissue is lost disproportionately to the development of new hard tissue. Osteoporosis can be subclassified as post-menopausal, senile, drug-induced (e.g., adrenocorticoid as can occur in steroid therapy), disease induced (e.g., arthritic and tumor), etc., however, the manifestations are essentially the same.
Another condition involving anomalous mobilization of calcium and phosphate is Paget's disease (osteitis deformans). In this disease, dissolution of normal bone occurs which is then replaced by soft, poorly mineralized tissue such that the bone becomes deformed from pressures of weight bearing, particularly in the tibia and femur.
Until recently, no satisfactory medical treatment for disease conditions involving anomalous mobilization of calcium phosphates has been provided, although dietary Vitamin D, calcium, fluorides, estrogens, and the hormone calcitonin (thyrocalcitonin) have been suggested on tested for these conditions. More recently it has been discovered that certain phosphonate compounds as hereinafter more fully defined are effective in the treatment of such diseases. The following U.S. patents and applications, for example, are directed to the use of various phosphonates in the treatment of such disease conditions: Francis, U.S. Application Ser. No. 51,355, filed June 30, 1970; U.S. Pat. No. 3,683,080, granted Aug. 8, 1972; U.S. Pat. No. 3,678,164, granted July 18, 1972; U.S. Pat. No. 3,662,066, granted May 9, 1972; U.S. Pat. No. 3,553,314, granted Jan. 5, 1971; U.S. Pat. No. 3,553,315, granted Jan. 5, 1971; U.S. Pat. No. 3,584,124, granted June 8, 1971; U.S. Pat. No. 3,584,125, granted June 8, 1971; and U.S. Pat. No. 3,641,246, granted Feb. 8, 1972.
While the compositions and methods of the foregoing patents and applications constitute an effective treatment for disease conditions such as osteoporosis, higher dosages of these compositions can cause certain adverse physiological responses. For example, higher dosages of such compounds as disodium ethane-1-hydroxy-1,1-diphosphonate can give rise to mineralization defects, i.e., lack of mineralization in mature bone (increased osteoid seams) or inhibition of mineralization of the growth cartilage and/or inhibition of primary spongiosa resorption in the epiphyseal region of bone in rapidly growing animals.
SUMMARY OF THE INVENTION
It has now been discovered that the therapeutic effectiveness of the phosphonate compounds can be enhanced to a degree that lower dosage levels can be used, thereby avoiding adverse responses, through the conjoint administration of Vitamin D-like antirachitic compounds (i.e., Vitamin D-active antirachitic compounds including Vitamin D and its precursors, analogs and metabolites) therewith. It is therefore an object of this invention to provide improved compositions and methods for treating disease conditions involving anomalous mobilization of calcium phosphate in animal tissue. It is a further object of this invention to provide improved compositions in dosage unit form containing active phosphonate compounds in combination with Vitamin D-active antirachitic compounds.
DETAILED DESCRIPTION OF THE INVENTION
In its composition aspect, the present invention is directed to a composition adapted to systemic administration to an animal comprising (1) an effective but non-toxic amount of a phosphonate selected from the group consisting of: ##STR1## wherein each R is hydrogen or CH 2 OH and n is an integer of from 3 to 10; ##STR2## wherein R 1 is hydrogen, alkyl containing from 1 to about 20 carbon atoms, alkenyl containing from 2 to about 20 carbon atoms, aryl (e.g., phenyl, naphthyl), phenylethenyl, benzyl, halogen (e.g., chlorine, bromine and fluorine) hydroxyl, amine, substituted amino (e.g., dimethylamino, diethylamino, N-hydroxy-N-ethylamino, acetylamino), --CH 2 COOH, --CH 2 PO 3 H 2 , CH(PO 3 N 2 )(OH), or --(CH 2 C(PO 3 H 2 ) 2 ) n -H wherein n is 1 to 15, R 2 is hydrogen, lower alkyl (e.g., methyl, ethyl, propyl and butyl), amine, benzyl, halogen (e.g., chlorine bromine, and fluorine), hydroxyl, --CH 2 COOH, --CH 2 PO 3 H 2 , or --CH 2 CH 2 PO 3 H 2 ; ##STR3## wherein n is an integer of from 3 to 9; ##STR4## wherein each R 3 is hydrogen or lower alkyl (e.g., methyl, ethyl, propyl and butyl); ##STR5## wherein n is an integer of from 2 to 4; ##STR6## wherein X and Y are each hydrogen or hydroxy; ##STR7## and the pharmaceutically acceptable salts of each of the foregoing acids, e.g., alkali metal (sodium and potassium), alkaline earth metal (calcium and magnesium), non-toxic heavy metal (stannous and indium) and ammonium and low molecular weight substituted ammonium (mono-, di- and triethanolamine) salts; and (2) from about 100 I.U. to about 50,000 I.U. of a Vitamin D-like antirachitic compound.
Operable phosphonates of the above formula (I) include propane-1,2,3-triphosphonic acid; butane-1,2,3,4-tetraphosphonic acid; hexane-1,2,3,4,5,6-hexaphosphonic acid; hexane-1-hydroxy-2,3,4,5,6-pentaphosphonic acid; hexane-1,6-dihydroxy-2,3,4,5-tetraphosphonic acid; pentane-1,2,3,4,5-pentaphosphonic acid; heptane-1,2,3,4,5,6,7-heptaphosphonic acid; octane-1,2,3,4,5,6,7,8-octaphosphonic acid, nonane-1,2,3,4,5,6,7,8,9-nonaphosphonic acid; decane-1,2,3,4,5,6,7,8,9,10-decaphosphonic acid; and the pharmaceutically acceptable salts of these acids, e.g., sodium, potassium, calcium, magnesium, ammonium, triethanolammonium, diethanolammonium, and monoethanolammonium salts.
Propane-1,2,3-triphosphonic acid and salts thereof can be prepared by a process disclosed in U.S. Pat. No. 3,743,688, filed July 3, 1973.
Butane-1,2,3,4-tetraphosphonic acid and salts thereof can be prepared by a process disclosed in U.S. Pat. No. 3,755,504, filed Aug. 28, 1973.
The higher aliphatic vicinal phosphonates and salts thereof can be prepared by the process disclosed in U.S. Pat. No. 3,584,035 granted June 8, 1971.
Among the operable phosphonates encompassed by the above formula (II) are ethane-1-hydroxy-1,1-diphosphonic acid; methanediphosphonic acid; methanehydroxydiphosphonic acid; ethane-1,1,2-triphosphonic acid; propane-1,1,3,3-tetraphosphonic acid; ethane-2-phenyl-1,1-diphosphonic acid; ethane-2-naphthyl-1,1-diphosphonic acid; methanephenyldiphosphonic acid; ethane-1-amino-1,1-diphosphonic acid; methanedichlorodiphosphonic acid; nonane-5,5-diphosphonic acid; n-pentane-1,1-diphosphonic acid; methanedifluorodiphosphonic acid; methanedibromodiphosphonic acid; propane-2,2-diphosphonic acid; ethane-2-carboxy-1,1-diphosphonic acid; propane-1-hydroxy-1,1,3-triphosphonic acid; ethane-2-hydroxy-1,1,2-triphosphonic acid; ethane-1-hydroxy-1,1,2-triphosphonic acid; propane-1,3-diphenyl-2,2-diphosphonic acid; nonane-1,1-diphosphonic acid; hexadecane-1,1-diphosphonic acid; pent-4-ene-1-hydroxy-1,1-diphosphonic acid; octadec-9-ene-1-hydroxy-1,1-diphosphonic acid; 3-phenyl-1,1-diphosphono-prop-2-ene; octane-1,1-diphosphonic acid; dodecane-1,1-diphosphonic acid; phenylaminomethanediphosphonic acid; naphthylaminomethane-disphosphonic acid; N,N-dimethylaminomethanediphosphonic acid; N-(2-dihydroxyethyl)-aminomethanediphosphonic acid; N-acetyl-aminomethanediphosphonic acid; aminomethanediphosphonic acid; dihydroxymethanediphosphonic acid; and the pharmaceutically acceptable salts of these acids, e.g., sodium potassium, calcium, magnesium, stannous, indium, ammonium, triethanol-ammonium, diethanolammonium, and monoethanolammonium salts.
Mixtures of any of the foregoing phosphonic acids and/or salts can be used in the practice of this invention.
Ethane-1-hydroxy-1,1-diphosphonic acid, an especially preferred phosphonate, has the molecular formula CH 3 C(OH)(PO 3 H 2 ) 2 . (According to nomenclature by radicals, the acid might also be named 1-hydroxyethylidone diphosphonic acid.)
While any pharmaceutically acceptable salt of ethane-1-hydroxy-1,1-diphosphonic acid can be used in the practice of this invention, the disodium dihydrogen salt is preferred. The other sodium, potassium, ammonium, and mono-, di-, and triethanolammonium salts and mixtures thereof are also suitable, provided caution is observed in regulating the total intake of cation species in the salt composition. These compounds can be prepared by any suitable method, however, an especially preferred method is disclosed in U.S. Pat. No. 3,400,149 granted Sept. 1, 1968.
Methanehydroxydiphosphonic acid and related compounds operable herein can be prepared, for example, by reaction of phosgene with an alkali metal dialkylphosphite. A complete description of these compounds and a method for preparing same is found in U.S. Pat. No. 3,422,137 granted Jan. 14, 1969.
Methanedihydroxydiphosphonic acid and salts useful herein and a method for preparing same are disclosed in U.S. Pat. No. 3,497,313 granted Feb. 24, 1970.
Methanediphosphonic acid and related compounds useful herein are described in detail in U.S. Pat. No. 3,213,030, granted Oct. 19, 1965. A preferred method of preparing such compounds is disclosed in U.S. Pat. No. 3,251,907 granted May 17, 1966.
Ethane-1,1,2-triphosphonic acid and related compounds which can be used in the compositions of this invention, as well as a method for their preparation, are fully described in U.S. Pat. No. 3,551,339 granted Dec. 29, 1970.
Propane-1,1,3,3-tetraphosphonic acid and related compounds useful herein, and a method for preparing same are fully disclosed in U.S. Pat. No. 3,400,176 granted Sept. 3, 1968. The higher methylene interrupted methylene phosphonate polymers can be prepared by the polymerization of ethylene-1,1-diphosphonic acid.
Pentane-2,2-diphosphonic acid and related compounds can be prepared in accordance with the method described by G. M. Kosolopoff in J. Amer. Chem. Soc., 75, 1500 (1953).
Operable phosphonates of formula (III) above include the following:
Methanecyclobutylhydroxydiphosphonic acid
Methanecyclopentylhydroxydiphosphonic acid
Methanecyclohexylhydroxydiphosphonic acid
Methanecycloheptylhydroxydiphosphonic acid
Methanecyclooctylhydroxydiphosphonic acid
Methanecyclononylhydroxydiphosphonic acid
Methanecyclodecylhydroxydiphosphonic acid
Each of the sodium, potassium, calcium, magnesium, stannous, indium, ammonium, monoethanolammonium, diethanolammonium and triethanolammonium salts of the above recited methanecycloalkylhydroxydiphosphonic acids as well as any other pharmaceutically acceptable salt of these acids, can be used in the practice of the present invention.
The phosphonates of formula (III) can be prepared by methods fully described in U.S. Pat. No. 3,584,125, granted June 8, 1971.
The preferred phosphonates of formula (IV) for the purpose of this invention are tris(phosphonomethyl)amine; tris(1-phosphonoethyl)amine; tris(2-phosphono-2-propyl)amine; and their pharmaceutically acceptable salts. Tris(phosphonomethyl)amine is especially preferred. The following are exemplary of compounds which can also be used.
(a) bis(phosphonomethyl)-1-phosphonoethyl amine;
(b) bis(phosphonomethyl)-2-phosphono-2-propyl amine;
(c) bis(1-phosphonoethyl)phosphonomethyl amine;
(d) bis(2-phosphono-2-propyl)phosphonomethyl amine;
(e) tris(1-phosphono-1-pentyl)amine;
(f) bis(phosphonomethyl)2-phosphono-2-hexyl amine; and
(g) the pharmaceutically acceptable salts of acids (a) through (f), e.g., sodium, potassium, calcium, magnesium, ammonium, triethanolammonium, diethanolammonium, and monoethanolammonium salts.
Mixtures of any of the foregoing tris(phosphonoalkyl)amines and/or salts can also be used in the practice of this invention.
The tris(phosphonoalkyl)amines can be prepared, for example, by first preparing the corresponding ester in accordance with the general reaction: ##STR8## wherein R is alkyl and R 1 and R 2 are hydrogen or lower alkyl.
The free acids can be prepared by hydrolysis of the ester using strong mineral acids such as hydrochloric acid. The salts are, of course, prepared by neutralizing the acid with the base of the desired cation. The preparation of tris(phosphonoalkyl)amines is fully disclosed by Irani, et al., in Canadian Pat. No. 753,207, issued Feb. 21, 1967.
The phosphonates of formula (V) include the following:
(1) 3,3,4,4,5,5-hexafluoro-1,2-diphosphonocyclopent-1-ene;
(2) 3,3,4,4-tetrafluoro-1,2-diphosphonocyclobut-1-ene; and
(3) 3,3,4,4,5,5,6,6-octafluoro-1,2-diphosphonocyclohex-1-one.
The perfluorodiphosphonocycloalkenes can be prepared, for example, by reacting trialkyl phosphites with 1,2-dichloroperfluorocycloalk-1-enes in accordance with the procedures fully described by Frank in J. Org. Chem., 31, #5, p. 1521.
The phosphonate of formula (VI) is referred to herein as cyclic tetraphosphonic acid. This compound and its pharmaceutically acceptable salts can be prepared by any suitable method, however, an especially preferred method is disclosed by Oscar T. Ouimby, U.S. Pat. No. 3,387,024 granted June 4, 1968.
Operable phosphonates encompassed by the above formula (VII) are ethene-1,2-dicarboxy-1-phosphonic acid; and the pharmaceutically acceptable salts of these acids, e.g., sodium, potassium, calcium, magnesium, stannous, indium, ammonium, triethanolammonium, diethanolammonium, and monoethanolammonium salts. While the above formula (VII) is representative of cis-isomers, the corresponding trans-isomers are also useful herein. Reference hereinafter to ethene-1,2-dicarboxy-1-phosphonic acid or salts thereof, unless otherwise specified, is intended as contemplating the cis- and trans-isomers and mixtures thereof.
Ethene-1,2-dicarboxy-1-phosphonic acid and related compounds useful herein can be prepared by reaction of an ester of acetylenedicarboxylic acid and a dialkyl phosphite followed by hydrolysis and saponification. This method is more fully described in U.S. Pat. No. 3,384,124, granted June 8, 1971.
Operable carboxyphosphonates of the above formula (VIII) include ethane-1,2-dicarboxy-1,2-diphosphonic acid; ethane-1,2-dicarboxy-1,2-dihydroxy-1,2-diphosphonic acid; ethane-1,2-dicarboxy-1-hydroxy-1,2-diphosphonic acid; and the pharmaceutically acceptable salts of these acids, e.g., sodium, potassium, calcium, magnesium, ammonium, triethanolammonium, diethanolammonium and monoethanolammonium salts.
Ethane-1,2-dicarboxy-1,2-diphosphonic acid, a preferred carboxyphosphonate herein, has the molecular formula CH(COOH) (PO 3 H 2 )CH(COOH) (PO 3 H 2 ). The most conveniently crystallizable salts of this acid are obtained when three, four or five of the acid hydrogens are replaced by sodium.
While any pharmaceutically acceptable salt of ethane-1,2-dicarboxy-1,2-diphosphonic acid can be used in the practice of this invention, the tetrasodium dihydrogen salt, the trisodium trihydrogen salt, the disodium tetrahydrogen salt, the monosodium pentahydrogen salt, and the mixtures thereof are preferred. The other sodium, potassium, ammonium, and mono-, di-, and triethanolammonium salts and mixtures thereof are also suitable, provided caution is observed in regulating the total intake of cation species in the salt composition.
Ethane-1,2-dicarboxy-1,2-diphosphonic acid and suitable salts thereof can be prepared in any convenient manner. For example, the reaction described by Pudovik in "Soviet Research on Organo-Phosphorus Compounds", 1949-1956, Part III, 547-85c. can be used to prepare the ester of ethane-1,2-dicarboxy-1,2-diphosphonic acid which in turn can, by ordinary hydrolysis reactions, be converted to the free acid form. Neutralization by alkali compounds such as sodium hydroxide, potassium hydroxide, carbonates and the like can be used to prepare a desired salt of the acid. A more detailed description of the preparation of these compounds is described in U.S. Pat. No. 3,562,166, granted Feb. 9, 1971.
Ethane-1,2-carboxy-1,2-dihydroxy-1,2-diphosphonic acid and related compounds useful herein can be prepared by reaction of an ester of ethane-1,2-dicarboxy-1,2-diphosphonic acid and an alkali metal hypohalite followed by hydrolysis and saponification. This method is more fully described in U.S. Pat. No. 3,579,570, granted May 18, 1971.
Phosphonates of formula (IX) can be prepared by a rearrangement reaction of a 2-haloethane-1-hydroxy-1,1-diphosphonic acid with about three equivalents of sodium hydroxide as described in U.S. Pat. No. 3,641,126.
The phosphonate of formula (X), ethylene-1,1-diphosphonic acid, can be prepared by the method of German Offen. No. 2,026,078.
Mixtures of any of the foregoing phosphonic acids and/or salts can be used in the practice of this invention.
The Vitamin D-like antirachitic compounds useful herein include activated ergosterol (Vitamin D 2 or calciferol), and activated 7-dehydrocholesterol (Vitamin D 3 ). These are available commercially or can be produced from their precursors (ergosterol and 7-dehydrocholesterol, respectively) by the application of energy to the molecule. The energy may be supplied by ultraviolet light, high speed electrons and the like. Thus, these precursors are themselves Vitamin D-like antirachitic compounds and can be administered and subsequently converted, in vivo, by sunlight to the D Vitamins. While both Vitamins D 2 and D 3 are useful herein, Vitamin D 3 is preferred. These compounds and their properties are described in detail by H. R. Rosenberg, Chemistry and Physiology of the Vitamins, pp. 341-432 (1945).
In vivo, Vitamin D (i.e., Vitamins D 2 and D 3 ) is metabolized and a number of the metabolites thereof have been identified as the basis for the antirachitic activity associated with Vitamin D. The metabolites can, of course, be used in the practice of the present invention. Analogs of Vitamin D also exist and are similarly useful in the present invention. The Vitamin D-like antirachitic metabolites and analogs of Vitamin D include the following which are listed together with a reference disclosing how to synthesize or isolate them or a commercial source therefore and their activity in International Units (I.U.) per μg. The activity where indicated by an asterisk (*) is estimated.
TABLE I______________________________________Name Source Activity______________________________________Vitamin D.sub.2 Widely Available 40Vitamin D.sub.3 Widely Available 40Dihydroxytachysterol.sub.2 Philips-Duphar 0.09 (Netherlands)Dihydrotachysterol.sub.3 Philips-Duphar 0.16 (Netherlands)25-hydroxydihydrotachy- U.S. Pat. No. 3,607,888 0.80sterol.sub.325-hydroxyergocalciferol U.S. Pat. No. 3,585,221 6025-hydroxycholecalciferol Philips-Duphar 60 (Netherlands)1α,25-dihydroxycholecalci- U.S. Pat. No. 3,697,559 20°ferol5,6-trans-cholecalciferol Biochemistry, Vol. 11, 20° No. 14, pp. 2715-195,6-trans-25-hydroxychole- Biochemistry, Vol. 11, 20°calciferol No. 14, pp. 2715-1924-nor-25-hydroxychole- Biochemistry, Vol. 11, 60°calciferol No. 14, pp. 2715-1924-nor-5,6-trans-25-hydroxy- Biochemistry, Vol. 11, 20-60°cholecalciferol No. 14, pp. 2715-1921,25-dihydroxycholecalci- Biochemistry, Vol. 9, 10 -ferol No. 14, pp. 2917-22 orally 20 - i.v.25,26-dihydroxycholecalci- Biochemistry, Vol. 9, <4ferol No. 24, pp.4776-8024,25-dihydroxycholecalci- U.S. Pat. No. 3,715,374 >10 -ferol orally 20 - i.v.1α-hydroxycholecalciferol Science, Vol. 180, 20° No. 4082, pp. 190-91______________________________________
The International Unit is defined in terms of the biological activity produced, as described more fully in U.S. Pharmacopiea, 15th revision, Mick Publishing Co. (1955). Strictly speaking, the I.U. is a fully accepted unit only for Vitamin D per se. The activity of Vitamin D-like antirachitic compounds is frequently referred to in the art in terms of the I.U. and since this measure of biological activity is the most nearly appropriate determinint of the levels of the Vitamin D-like compounds for use in the present invention, it is so used herein. The amount of the Vitamin D-like antirachitic compounds employed in the method of this invention must be sufficient to provide about 100 I.U. to about 50,000 I.U. per day. The preferred antirachitic compounds for use in the present invention are Vitamin D 3 and 1α-hydroxycholecalciferol which are well suited for oral administration.
The therapeutic dosage of phosphonate will vary with the particular condition being treated, the severity of the condition, and the duration of treatment; however, single dosages can range from 0.01 to 500 mg. per kilogram of body weight, preferably 0.1 to 50 mg./kg., with up to four dosages daily. The higher dosages within this range are, of course, required in the case of oral administration because of limited absorption. Repeated dosages greater than about 400 mg./kg. may produce toxic symptoms and should be avoided. Moreover, daily dosages greater than about 2000 mg./kg. (unless otherwise specified, the unit designated "mg./kg." as used herein refers to mg. of compound/kg. of body weight) are not required to produce the desired effect and may produce toxic side effects. Dosages of less than about 0.01 mg./kg. do not materially affect pathological demineralization, even administered intravenously. Table II below sets forth preferred dosages for various conditions which can be treated in accordance with this invention.
TABLE II______________________________________ Therapeutic Oral Dosage (mg./kg.) Up to FourCondition Times/Day______________________________________Osteoporosis 0.25-25(post-menopausal)*Osteoporosis 0.25-25(senile, et. al.)Paget's Disease 1-50______________________________________ *A larger initial dosage may be required, e.g., up to 500 mg./kg. followe by the specified dosage level.
The phosphonates can also be administered parenterally in aqueous solution by subcutaneous, intradermal, intramuscular, intraperitoneal, or intravenous injection. The preferred single dosage ranges by those modes of administration are as follows.
______________________________________ Therapeutic Dosage______________________________________Subcutaneous 0.1-10 mg./kg.Intradermal 0.1-10 mg./kg.Intramuscular .05-5 mg./kg.Intravenous 0.5-5 mg./kg.Intraperitoneal 0.5-5 mg./kg.______________________________________
For purposes of oral administration (the preferred mode) the phosphonates can be in elixer form or formulated in unit dosage form, i.e., in the form of capsules, tablets or pills, together with the Vitamin D-like antirachitic compounds (especially Vitamin D 3 ) and a pharmaceutical carrier. each unit dosage form contaning from 5 mg. to 10 g. of phosphonate and from about 100 to about 50,000 units of the antirachitic compound. The preferred concentration range of phosphonate in unit dosage forms intended for use by humans and smaller domesticated animals is from 10 mg. to 1000 mg., more preferably 50 mg. to 500 mg. and the preferred range of the antirachitic compounds is from 500 to about 50,000 International Units.
Representative compositions of the present invention are presented in the following examples.
EXAMPLE I
Capsules are prepared by conventional methods, comprised as folows:
______________________________________ mg perIngredient capsule______________________________________Disodium ethane-1-hydroxy-1,1-diphosphonate 350.00Vitamin D.sub.3 2000 I.U.Starch 55.60Sodium lauryl sulfate 2.90______________________________________
The above capsules administered orally twice daily substantially reduces bone decalcification in a patient weighing approximately 70 kilograms afflicted with osteoporosis. Similar results are attained when methanediphosphonic acid, methanedichlorodiphosphonic acid, methanehydroxydiphosphonic acid, ethane-1-amino-1,1-diphosphonic acid, phenylaminomethanediphosphonic acid, N,N-dimethylaminomethanediphosphonic acid, N-(2-hydroxyethyl)-aminomethanediphosphosphonic acid, N-acotylaminomethanediphosphonic acid, aminomethanediphosphonic acid, propane-1,2,3-triphosphonic acid, hexane-1,2,3,4,5,6-hexaphosphonic acid, and pent-4-ene-1-hydroxy-1,1-diphosphonic acid, respectively, are employed in the above described capsule in place of disodium ethane-1-hydroxy-1,1-diphosphonate. Comparable results are secured when the Vitamin D 2 is used in place of Vitamin D 3 in the above capsules in that no mineralization defects are observed.
EXAMPLE II
Tablets are prepared by conventional methods, formulated as follows:
______________________________________ mg perIngredient tablet______________________________________Methanediphosphonic acid 125.00Vitamin D.sub.2 750 I.U.Lactose 40.00Starch 2.50Magnesium stearate 1.00______________________________________
When administered orally four times daily, the above composition significantly reduces bone loss in a patient weighing approximately 50 kilograms suffering from Paget's disease.
Similar results are achieved with tablets formulated as above but replacing methanediphosphonic acid with the disodium salt of ethane-1-hydroxy-1,1-diphosphonic acid, the trisodium salt of methanediphosphonic acid, the disodium salt of methanehydroxydiphosphonic acid, aminomethanediphosphonic acid, the monocalcium salt of methanedichlorodiphosphoric acid, naphthylaminomethanediphosphonic acid, propane-1,2,3-triphosphonic acid; the pentasodium salt of butane-1,2,3,4-tetraphosphonic acid, the monoindium salt of octadec-9-ene-1-hydroxy-1,1-diphosphoric acid, the monostannous salt of hexadecane-1,1-diphosphonic acid, and propane-1,1-diphosphonic acid, respectively.
The lactose employed in this example is replaced by sucrose and the magnesium stearate by sodium carboxymethylcellulose without affecting the desired properties of the tablet.
Additional tablet compositions are prepared in accordance with the invention as follows:
______________________________________ Ex. Mg per TabletIngredient III IV V VI VII VIII IX______________________________________Cyclohexyl- 80.0hydroxymethane-disphosphonic acidTris(phosphono- 100.0methyl)amine3,3,4,4,5,5-hexa- 120.0fluoro-1,2-diphos-phonocyclopent-1-eneCyclic tetraphos- 50.0phonic acidEthene-1,2-dicar- 85.0 40.0boxy-1-phosphonicacidEthane-1,2-dicar- 30.0 15.0boxy-1,2-diphos-phonic acidVitamin D.sub.3 750 1000 5000 500 2000 3000 3000(InternationalUnits)Lactose 97.0 31.0 31.0 73.0 97.0 30.0 97.0Starch 45.0 13.0 13.0 57.0 45.0 45.0Stearic acid 6.0 6.0Talc 35.5 6.5 6.5 9.0 35.0 5.0 9.0Calcium stearate 1.0 1.0 1.0Ethyl cellulose 16.0 16.0 15.0______________________________________
Each of the above tablets are used in the treatment of a 90 kg. patient suffering from idiopathic osteoporosis. Bone loss is substantially reduced and no adverse symptoms are observed when these tablets are administered in a number sufficient to provide a daily dosage of phosphonate of approximately 450 mg.
EXAMPLES X TO XXVI
Tablets are formulated as in Example VIII except that disodium ethane-1-hydroxy-1,1-diphosphonate replaces the ethane-1-hydroxy-1,1-diphosphonic acid and 3000 International Units of the following Vitamin D-like antirachitic compounds are used:
______________________________________EXAMPLE COMPOUND______________________________________X Vitamin D.sub.2XI Vitamin D.sub.3XII Dihydroxytachysterol.sub.2XIII Dihydrotachysterol.sub.3XIV 25-hydroxydihydrotachysterol.sub.3XV 25-hydroxyergocalciferolXVI 25-hydroxycholecalciferolXVII 1α,25-dihydroxycholecalciferolXVIII 5,6-trans-cholecalciferolXIX 5,6-trans-25-hydroxycholeclaciferolXX 24-nor-25-hydroxycholecalciferolXXI 24-nor-5,6-trans-25-hydroxycholecalciferolXXII 21,25-dihydroxycholecalciferolXXIII 25,26-dihydroxycholecalciferolXXIV 24,25-dihydroxycholecalciferolXXV 1α-hydroxycholecalciferolXXVI Vitamin D.sub.3 (1500 units) and 1α-hydroxychole- calciferol (1500 units)______________________________________
The above tablets are administered to a 70 Kg. patient suffering from Pagets disease in a number sufficient to provide a daily dosage of about 500 mg. of phosphonate. Bone loss is substantially reduced and no adverse symptoms are observed.
Similar results are obtained when the above tablets are administered to a 70 Kg. patient suffering from osteoporosis in a number sufficient to provide a daily dosage of about 250 mg. of phosphonate.
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Compositions for inhibiting the anomalous mobilization of calcium phosphates in animal tissue comprising an effective amount of certain phosphonate compounds as herein defined in combination with Vitamin D-like antirachitic compounds, and a method for treating or preventing conditions involving hard tissue demineralization in an animal comprising concurrently administering said phosphonates and Vitamin D-like antirachitic compounds to animals.
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FIELD OF THE INVENTION
This invention relates to a novel aromatic polythioetherimide, and more particularly to an aromatic polythioetherimide which is excellent in heat resistance and can be melt-molded and is, therefore, useful as super-engineering plastics, heat resistant fibers, heat resistant film, materials for heat resistant coatings, and the like.
BACKGROUND OF THE INVENTION
It is well known that an aromatic polyimide having excellent heat resistance can be obtained by the reaction between an aromatic tetracarboxylic dianhydride and an aromatic diamine as described in C.E. Sroog, Journal of Polymer Science, Macromolecular Review, Vol. 11, page 161, (1976). However, the conventionally proposed aromatic polyimides have been limited in their application due to difficulty in melt-molding.
In order to improve melt-moldability, aromatic polyetherimides prepared by using an aryloxy acid dianhydride as acid dianhydride component have been studied, as disclosed, e.g., in Japanese Patent Publication Nos. 20966/82 and 20967/82, and have been put into the market under the trademark "ULTEM®" from General Electric Company. The aromatic polyetherimides of this type are excellent in melt-moldability (e.g., injection moldability and extrusion moldability) but, in turn, inferior in heat resistance and solvent resistance as compared with the conventional aromatic polyimides.
On the other hand, aromatic polyimides having melt-moldability without suffering great reduction of heat resistance have been reported, such as an aromatic polythioetherimide obtained by reacting an aromatic diamine having a (thio)ether linkage and pyromellitic dianhydride as disclosed in Japanese Laid-Open Patent Application Nos. 170122/84 and 250031/86, and a polyimidosulfone as disclosed in U.S. Pat. No. 4,398,021. They, however, are still unsatisfactory for practical application in the field of engineering and electronics where a balance between heat resistance and mechanical properties is required.
In order to eliminate these disadvantages of aromatic polyimides, Japanese Laid-Open Patent Application No. 15228/87 proposes an aromatic polythioetherimide obtained by the reaction between an aromatic diamine having a thioether linkage and 3,3',4,4'-benzophenonetetracarboxylic dianhydride and/or pyromellitic dianhydride. Although this aromatic polythioetherimide shows an excellent balance between heat resistance and mechanical properties, a further improvement on moldability has been demanded.
SUMMARY OF THE INVENTION
As a result of extensive investigations, the inventors have found that a novel aromatic polythioetherimide obtained by reacting an aromatic diamine having thioether linkages represented by formula (III): ##STR2## wherein Ar represents ##STR3## wherein A represents O, CO, SO, SO 2 or C y H 2y , wherein y represents an integer of from 1 to 10; Y represents an alkyl group having from 1 to 20 carbon atoms, an aralkyl group having from 7 to 20 carbon atoms, a cycloalkyl group having from 3 to 20 carbon atoms, an aryl group having from 6 to 20 carbon atoms, a halogen atom or a nitro group; and a, b, c and d each represents 0 or an integer of from 1 to 4, and/or an aromatic diamine represented by formula (IV):
H.sub.2 N--Ar'--NH.sub.2 (IV)
wherein Ar' represents a divalent aromatic residue represented by ##STR4## wherein Y is as defined above; e, f, g, h, i and j each represents 0 or an integer of from 1 to 4; X represents O or S; m represents 0 or an integer of from 1 to 20; l represents 0 or 1; and Z represents CO, SO, SO 2 or C y H 2y , wherein y is as defined above, and a tetracarboxylic dianhydride represented by formula (V): ##STR5## is well balanced between heat resistance and mechanical properties and also exhibits improved moldability. The present invention has been completed based on this finding.
That is, the present invention relates to a novel aromatic polythioetherimide having a repeating unit represented by formula (I): ##STR6## wherein Ar is as defined above.
More specifically, the present invention relates to an aromatic polythioetherimide comprising not less than 50 mol % of the repeating unit represented by formula (I), with the total of the repeating unit(s) being 100 mol %, and particularly to an aromatic polythioetherimide comprising almost 100 mol % of the repeating unit represented by formula (I), with the total of the repeating unit(s) being 100 mol %, and to an aromatic polythioetherimide comprising not less than 50 mol % of the repeating unit represented by formula (I) and up to 50 mol % of a repeating unit represented by formula (II): ##STR7## wherein Ar' is as defined above, with the total of the repeating units being 100 mol %.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an infrared absorption spectrum of the aromatic polythioetherimide obtained in Example 1.
FIG. 2 is an infrared absorption spectrum of the aromatic polythioetherimide obtained in Example 3.
DETAILED DESCRIPTION OF THE INVENTION
The aromatic polythioetherimides according to the present invention can be obtained by reacting (a) an aromatic thioether diamine represented by formula (III), and/or (b) an aromatic diamine represented by formula (IV), and (c) a biphenyltetracarboxylic dianhydride of formula (V) at a molar ratio [(a)+(b)]/(c) of 1/0.9 to 1.1 and a molar ratio (a)/(b) of 100/0 to 50/50.
The resulting aromatic polythioetherimide has a glass transition temperature of from 100° to 350° C., preferably from 120° to 280° C.
The reaction between the aromatic thioether diamine of formula (III) and, if used, the aromatic diamine of formula (IV) (these diamine compounds will hereinafter be inclusively referred to as aromatic diamine component) and the biphenyltetracarboxylic dianhydride of formula (V) is preferably carried out by the following one-stage process or two-stage process, but the process for preparing the aromatic polythioetherimide of the present invention is not limited thereto.
(1) One-Stage Process
This process comprises heating the aromatic diamine component and the carboxylic dianhydride in a dissolved or molten state to effect polymerization while removing produced water from the system to obtain a polyimide.
The one-stage process can be carried out by dissolving or dispersing 1.00 mol of the aromatic diamine component and 0.90 to 1.10 mol, preferably 0.95 to 1.05 mol, of the biphenyltetracarboxylic dianhydride in an organic solvent and heating the solution or dispersion at a temperature of from 100° to 400° C., preferably from 150° to 250° C. (solution process).
The reaction can be conducted effectively by using an azeotrope former serving for removal of water, such as benzene, toluene, xylene, chlorobenzene, etc., in combination. At the same time, addition of an organic acid, e.g., p-toluenesulfonic acid, benzene-sulfonic acid, etc., to the system as a catalyst sometimes brings good results.
The organic solvent which can be used in the above-described solution process includes halogenated aromatic hydrocarbons, e.g., dichlorobenzene, trichlorobenzene, etc.; phenolic compounds, e.g., phenol, cresol, chlorophenol, etc.; aliphatic carboxylic acids; aprotic polar solvents, e.g., N,N-dimethylacetamide, N-methylpyrrolidone, tetramethylurea, 1,3-dimethyl-2-imidazolidinone, sulforan, dimethyl sulfoxide, etc.; aliphatic glycol ethers, e.g., ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, etc.; and mixtures thereof.
The one-stage process can also be carried out by mixing 1.00 mol of the aromatic diamine component and from 0.90 to 1.10 mol of the biphenyltetracarboxylic dianhydride and heating the mixture in a molten state at a temperature of from 150° to 400° C., preferably from 250° to 350° C. (melt process).
The polymerization according to the melt process can be accelerated by forced removal of produced water from the polymerization system.
(2) Two-Stage Process
This process comprises a first step comprising reacting the aromatic diamine component and the carboxylic dianhydride in a dissolved state to obtain a polyamic acid and a second step comprising dehydration-cyclization of the polyamic acid in a dissolved state or a solid phase state to obtain a polyimide.
(i) First Step (Preparation of Polyamic Acid)
The first step can be carried out by dissolving 1.00 mol of the aromatic diamine component and from 0.90 to 1.10 mol, preferably from 0.95 to 1.05 mol, of the biphenyltetracarboxylic dianhydride in a polar organic solvent and mixing the solution at a temperature of from -20° to +80° C., preferably from -10° to +60° C., to obtain a polyamic acid solution.
The polar organic solvent to be used in the first step includes aprotic polar solvents (e.g., N,N-dimethylformamide, N,N-dimethylacetamide, N-methylpyrrolidone, 1,3-dimethyl-2-imidazolidinone, sulforan, dimethyl sulfoxide, etc.); aliphatic glycol ethers (e.g., ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, etc.); and mixtures thereof.
(ii) Second Step (Preparation of Polyimide)
The second step can be carried out by subjecting the polyamic acid obtained in the first step to dehydration-cyclization to convert it to an aromatic polythioetherimide. This step may be effected either in a liquid phase or in a solid phase.
The cyclization in a liquid phase includes thermal cyclization and chemical cyclization.
The thermal cyclization is performed by heating the polyamic acid solution at a temperature of from 50° to 400° C., preferably from 150° to 250° C. Addition of an azeotrope former serving for removal of produced water (e.g., benzene, toluene, xylene, chlorobenzene, etc.) and/or a catalyst (e.g., p-toluenesulfonic acid, benzene-sulfonic acid, etc.) to the reaction system gives good results.
The chemical cyclization is conducted by adding to the polyamic acid solution an aliphatic anhydride (e.g., acetic anhydride, propionic anhydride, etc.), a tertiary amine (e.g., triethylamine, pyridine, 4-dimethylaminopyridine, isoquinoline, etc.), a halogen compound (e.g., phosphorus oxychloride, thionyl chloride, etc.), a chemical dehydrating agent (e.g., Molecular Sieve, silica gel, alumina, phosphorus pentoxide, etc.), or the like and allowing the mixture to react at a temperature of from 0° to 120° C., preferably from 10° to 80° C.
The aromatic polythioetherimide resulted from the liquid phase cyclization may be obtained in a precipitated state or dissolved state. In the former case, the precipitate formed can be isolated by filtration. In the latter case, the resulting polymer solution is diluted with a solvent which is incapable of dissolving the polymer and compatible with the reaction solvent to thereby precipitate the polymer, which is then isolated by filtration.
The solid phase cyclization can be carried out by pouring the polyamic acid solution into water or methanol to precipitate the polymer, separating the polymer, and subjecting the polymer to heat treatment at a temperature of from 150° to 350° C. Cares should be taken not to heat the polymer for too long a period of time at a heating temperature of 250° C. or higher, since such heat treatment results in deterioration of melt flow properties or balance of mechanical properties.
Specific examples of the aromatic thioether diamine represented by formula (III) which can be used in the present invention are 4,4'-bis(4-aminophenylthio)-biphenyl, 4,4'-bis(4-aminophenylthio)diphenyl ether, 4,4'-bis(4-aminophenylthio)benzophenone, 4,4'-bis(4-aminophenylthio)diphenyl sulfoxide, 4,4'-bis(4-aminophenylthio)diphenylsulfone, 3,3'-bis(4-aminophenylthio)diphenylsulfone, 2,2-bis[4-(4-aminophenylthio)phenyl]propane, 4,4'-bis(4-aminophenylthio)diphenylmethane, and so on.
These compounds can be used either individually or in combinations of two or more thereof. They are used in a total amount of from 50 mol % up to and including 100 mol % based on the total aromatic diamine component.
Specific examples of the aromatic diamine represented by formula (IV) which can be used in combination with the compound of formula (III) are p-phenylenediamine, m-phenylenediamine, tolylenediamine, 2-chloro-1,4-phenylenediamine, 4-chloro-1,3-phenylenediamine, 4,4'-diaminobiphenyl, 3,3'-dimethyl-4,4'-diaminobiphenyl, 3,3'-dichloro-4,4'-diaminobiphenyl, 4,4'-diaminodiphenyl ether, 3,4'-diaminodiphenyl ether, 4,4'-diaminodiphenyl sulfide, 4,4'-diaminodiphenylsulfone, 3,4'-diaminodiphenylsulfone, 3,3'-diaminodiphenylsulfone, 4,4'-diaminobenzophenone, 3,3'-diaminobenzophenone, 3,4'-diaminobenzophenone, 4,4'-diaminodiphenylmethane, 3,3'-diaminodiphenylmethane, 1,4-bis(4-aminophenoxy)benzene, 1,3-bis(4-aminophenoxy)benzene, 1,3-bis(3-aminophenoxy)benzene, 4,4'-bis(4-aminophenoxy)diphenyl ether, 1,4bis(4-aminophenylthio)benzene, 1,3-bis(4-aminophenylthio)benzene, 2,4-bis(4-aminophenylthio)nitrobenzene, 2,5-dimethyl-1,4-bis(4-aminophenylthio)benzene, 4,4'-bis(4-aminophenylthio)diphenyl sulfide, 1,4-bis[4-(4-aminophenylthio)phenylthio]benzene, an α,ω-diaminopoly-(1,4-thiophenylene) oligomer, 4,4'-bis(4-aminophenoxy)biphenyl, 4,4'-bis(4-aminophenoxy)diphenyl sulfide, 4,4'-bis(4-aminophenoxy)benzophenone, 4,4'-bis(4-aminophenoxy)diphenylsulfone, 4,4'-bis(3 -aminophenoxy)diphenylsulfone, 2,2-bis[4-(4-aminophenoxy)phenyl]propane, 2,2-bis[4-(3-aminophenoxy)phenyl]propane, etc. These compounds can be used either individually or in combinations of two or more thereof. They are used in a total amount of up to and including 50 mol % based on the total aromatic diamine component.
The biphenyltetracarboxylic dianhydride which can be used in the present invention includes 2,2',3,3'-biphenyltetracarboxylic dianhydride, 2,3',3,4'-biphenyltetracarboxylic dianhydride, 3,3',4,4'-biphenyltetracarboxylic dianhydride, and a combination thereof.
In molding the polymer according to the present invention, the polymer can contain various known fillers. Typical examples of the fillers include fibrous fillers, e.g., glass fiber, carbon fiber, boron fiber, aramid fiber, alumina fiber, silicon carbide fiber, etc.; and inorganic fillers, e.g., mica, talc, clay, graphite, carbon black, silica, asbestos, molybdenum sulfide, magnesium oxide, calcium oxide, etc.
The polymer of the present invention can be used in a wide range of application, such as various electric and electronic parts, housings, automobile parts, interior materials of aircrafts, sliding parts, gears, insulating materials, heat resistant films, heat resistant varnishes, heat resistant fibers, and the like.
The present invention is now illustrated in greater detail with reference to the following Examples and Comparative Examples, but it should be understood that the present invention is not deemed to be limited thereto.
EXAMPLE 1
In a 1,000 ml-volume four-necked flask equipped with a thermometer, a water separator with a Dimroth condenser, an inlet for introducing a solid, and an inlet for introducing nitrogen gas were charged 42.8 g (0.10 mol) of 4,4'-bis(4-aminophenylthio)benzophenone and 200 ml of dried N-methylpyrrolidone. To the mixture was added 29.5 g (0.10 mol) of solid 3,3',4,4'-biphenyltetracarboxylic dianhydride at 60° C. in a nitrogen stream while vigorously stirring. Thereafter, the stirring was continued at 60° to 70° C. for 2 hours and then at room temperature for 20 hours. The mixture was diluted with 100 ml of toluene and 100 ml of dried N-methylpyrrolidone followed by heating at 165° C. for 6 hours. During the reaction, the produced water was removed as an azeotropic mixture with toluene. The reaction mixture was cooled to room temperature and then poured into water to precipitate the produced polymer. The precipitate was filtered, crushed, washed with water, and dried in a vacuum drier at 180° C. for 24 hours to obtain 68.5 g (99.7%) of the polymer. The resulting polymer was insoluble in an organic solvent (N-methylpyrrolidone) and had a glass transition temperature of 233° C.
IR Spectrum (KBr) (shown in FIG. 1):
1,780 and 1,720 cm -1 (imide), 1,650 cm -1 (ketone),
1,080 cm -1 (thioether), and 820, 760 and 740 cm -1
(aromatic ring).
The polymer could be compression molded at 350° C. to provide a brown tough resin plate.
COMPARATIVE EXAMPLE 1
The same procedure of Example 1 was repeated, except for replacing the 3,3',4,4'-biphenyltetracarboxylic dianhydride with 32.2 g (0.10 mol) of 3,3',4,4'-benzophenonetetracarboxylic dianhydride, to obtain 71.0 g (99.4%) of a polymer insoluble in an organic solvent (N-methylpyrrolidone) and having a glass transition temperature of 245° C.
IR Spectrum (KBr):
1,775 and 1,720 cm -1 (imide), 1,640 cm -1 (ketone),
1,080 cm -1 (thioether), and 820 and 720 cm -1
(aromatic ring)
Although the resulting polymer could be compression molded to provide an amber tough resin plate, the temperature permitting of compression molding was 380° C., indicating inferiority in moldability to the polymer of Example 1.
EXAMPLE 2
The procedure of Example 1 was repeated, except for using, as starting materials, 40.0 g (0.10 mol) of 4,4'-bis(4-aminophenylthio)biphenyl and 29.5 g (0.10 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride, to obtain 65.7 g (99.7%) of a polymer insoluble in an organic solvent (N-methylpyrrolidone) and having a glass transition temperature of 260° C. and a heat decomposition point of 520° C. (in air).
IR Spectrum (KBr):
1,780 and 1,720 cm -1 (imide), 1,085 cm -1 (thioether),
and 810 and 740 cm -1 (aromatic ring).
The resulting polymer could be compression molded at 370° C. to provide a brown tough resin plate.
EXAMPLE 3
In a 1,000 ml-volume four-necked flask equipped with a thermometer, an inlet for introducing a solid, a dropping funnel and an inlet for introducing nitrogen gas were charged 34.3 g (0.08 mol) of 4,4'-bis(4-aminophenylthio)benzophenone, 4.0 g (0.02 mol) of 4,4'-diaminodiphenyl ether, and 150 ml of dried N-methylpyrrolidone. To the mixture was added 29.5 g (0.10 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride in a nitrogen stream while maintaining the inner temperature at 30° C. or lower, followed by stirring at room temperature for 20 hours. After the reaction mixture was diluted with 600 ml of dried N-methylpyrrolidone, 8.1 ml (0.10 mol) of pyridine and 45.3 ml (0.41 mol) of acetic anhydride were added thereto dropwise from the dropping funnel while maintaining the inner temperature at 70° C., followed by stirring at 70° C. for 2 hours. After cooling to room temperature, acetone was added to the reaction mixture, and the precipitated polymer was collected by filtration, washed with acetone, and dried in a vacuum drier at 180° C. for 24 hours to obtain 64.2 g (100%) of a polymer insoluble in an organic solvent (N-methylpyrrolidone) and having a glass transition temperature of 253° C.
IR Spectrum (KBr) (shown in FIG. 2):
1,780 and 1,720 cm -1 (imide), 1,240 cm -1 (ether),
1,080 cm -1 (thioether), and 825 and 740 cm -1
(aromatic ring).
The resulting polymer could be compression molded at 360° C. to provide a pale brown and transparent resin plate. The molded polymer had a tensile strength (yield point) of 1.020 kg/cm 2 and a modulus of elasticity in tension of 27.600 kg/cm 2 , proving extremely tough.
EXAMPLE 4
Into a 1,000 ml-volume four-necked flask equipped with a thermometer, a water separator with a Dimroth condenser, an inlet for introducing a solid and an inlet for introducing nitrogen gas were charged 34.3 g (0.08 mol) of 4,4'-bis(4-aminophenylthio)benzophenone, 4.0 g (0.02 mol) of 4,4'-diaminodiphenyl ether, 29.5 g (0.10 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride, 0.1 g (0.00053 mol) of p-toluenesulfonic acid, and 650 ml of dried N-methylpyrrolidone, and the mixture was stirred at room temperature until the components were uniformly dissolved. To the mixture was added 100 ml of xylene, and the resulting mixture was heated at 180° C. for 6 hours. During the reaction, the produced water was azeotropically removed together with the xylene. After cooling to room temperature, the reaction mixture was poured into water, and the thus precipitated polymer was filtered, crushed, washed with water, and dried in a vacuum drier at 180° C. for 24 hours to obtain 63.8 g (99.4%) of a polymer insoluble in an organic solvent (N-methylpyrrolidone) and having a glass transition temperature of 255° C.
IR Spectrum (KBr):
1,780 and 1,720 cm -1 (imide), 1,240 cm -1 (ether),
1,080 cm -1 (thioether), and 825 and 740 cm -1
(aromatic ring).
The resulting polymer could be compression molded at 360° C. to provide a brown tough resin plate.
EXAMPLE 5
Into a 1,000 ml-volume four-necked flask equipped with a thermometer, a water separator with a Dimroth condenser, an inlet for introducing a solid, and an inlet for introducing nitrogen gas were charged 28.0 g (0.07 mol) of 4,4'-bis(4-aminophenylthio)biphenyl, 13.0 g (0.03 mol) of 4,4'-bis(4-aminophenoxy)diphenylsulfone and 150 ml of dried N-methylpyrrolidone. To the mixture was added 29.5 g (0.10 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride in a nitrogen stream while keeping the inner temperature at 30° C., followed by stirring at room temperature for 20 hours. The reaction mixture was poured into water, and the thus precipitated polymer was filtered, crushed, washed with water, and dried in a vacuum drier at 70° C. for 24 hours to obtain a polyamic acid powder having an intrinsic viscosity of 0.45 dl/g (0.2% N-methylpyrrolidone solution, 30° C.).
IR Spectrum (KBr):
1,710 cm -1 (carboxylic acid), 1,655 and 1,525 cm -1
(amide), 1,240 cm - (ether), 1,145 cm -1 (sulfone),
1,085 cm -1 (thioether), and 815 cm -1 (aromatic ring).
The resulting polyamic acid powder was put in an oven and heated at 180° C. for 24 hours to effect imidization to obtain 66.7 g (99.7%) of a polymer insoluble in an organic solvent (N-methylpyrrolidone) and having a glass transition temperature of 272° C.
IR Spectrum (KBr):
1,780 and 1,720 cm -1 (imide), 1,240 cm -1 (ether),
1,150 cm -1 (sulfone), 1,085 cm -1 (thioether), and
815 and 740 cm -1 (aromatic ring).
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
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An aromatic polythioetherimide is disclosed, which comprises at least 50 mol % of a repeating unit represented by formula (I): ##STR1## wherein Ar is as defined in the specification, with the total of the repeating unit(s) being 100 mol %. The polythioetherimide has an excellent balance between heat resistance and mechanical properties as well as improved moldability.
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FIELD OF THE INVENTION
[0001] The invention generally relates to a process for oxidizing organic compounds. In particular, the invention relates to a process utilizing hydrogen peroxide to oxidize an oxidizable organic substrate in the presence of a silylated titania/silica-containing catalyst and to a preparation of this catalyst.
BACKGROUND OF THE INVENTION
[0002] Catalytic oxidation processes are important routes to many commercial chemicals. For example, numerous commercial processes for the epoxidation of olefins have been disclosed in the art. One such process involves the reaction of an organic hydroperoxide with an olefin in the presence of catalytic amounts of certain soluble transition metal compounds (e.g., molybdenum, tungsten, or vanadium napthenates). Some drawbacks to this process include co-production of an alcohol from the hydroperoxide, recovery of the soluble metal catalyst, and the sensitivity of the reaction to water.
[0003] Heterogeneous catalysts which overcome some of the aforesaid problems have also been developed. U.S. Pat. No. 3,923,843 claims a process for the epoxidation of an olefinically unsaturated compound comprising reacting the compound in the liquid phase with an organic hydroperoxide in the presence of a catalyst comprising an inorganic siliceous compound in chemical combination with an oxide or hydroxide of titanium. The catalyst is treated with an organic silylating agent before use. In the examples shown, the epoxide selectivity is increased from about 3% to about 15% when comparing the untreated catalyst to the silylated form.
[0004] Hydrogen peroxide is often employed as an oxidizing agent for the production of organic chemicals. A wide variety of organic compounds may be oxidized utilizing hydrogen peroxide, for example, olefins can be oxidized to epoxides (oxiranes) using this reagent.
[0005] Many titanosilicates have been reported to be useful as oxidation catalysts. For example, the catalytic oxidation of alkanes and alkenes by titanium silicates is disclosed in C. B. Khouw et al., “Studies on the Catalytic Oxidation of Alkanes and Alkenes by Titanium Silicates”, Journal of Catalysis 149, 195-205 (1994). Such catalysts are used for the selective oxidation of n-octane using organic hydroperoxides as the oxidants at temperatures below 100° C. The absence of water is deemed critical for catalytic activity.
[0006] In this regard, there is a need for processes that can utilize aqueous hydrogen peroxide rather than organic hydroperoxides to provide both a safe and an efficient process for oxidizing organic compounds. The present invention satisfies that need, but yet can still be used with organic hydroperoxides, and also overcomes certain deficiencies inherent in the prior art. Other objects and advantages of the invention will become apparent to those skilled in the art upon reference to the detailed description which follows hereinafter.
SUMMARY OF THE INVENTION
[0007] The invention provides a process for oxidizing organic compounds comprising: contacting, in a zone of reaction, an oxidizable organic compound with a peroxide selected from the group consisting of hydrogen peroxide and organic hydroperoxides, in the presence of a catalytically effective amount of an insoluble catalyst comprising silicon oxide and an oxide of at least one peroxide-activating metal prepared by sol-gel techniques, wherein said catalyst is characterized by (i) the silicon to peroxide-activating atomic ratio is less than 10,000 to 1; (ii) is x-ray amorphous; (iii) possesses a Si-C infrared band; and (iv) has a surface area greater than 500 m 2 /g, a pore volume greater than 0.5 mL/g and an average pore diameter of greater than 4 nm.
[0008] Preferably, in the process of the invention, the organic compound is selected from the group consisting of:
[0009] (a) cyclic olefins and olefins according to the formula R 1 R 2 C═CR 3 R 4 ,
[0010] wherein R 1 , R 2 , R 3 and R 4 are each independently —H; alkyl, wherein the alkyl group has from 1 to 16 carbon atoms; alkylaryl, wherein the alkylaryl group has from 7 to 16 carbon atoms; cycloalkyl, wherein the cycloalkyl group has from 6 to 10 carbon atoms; or alkylcycloalkyl, wherein the alkylcycloalkyl group has from 7 to 16 carbon atoms; and wherein said olefin can optionally containing halogen atoms (i.e., Cl, Br, F, and I);
[0011] (b) cyclic ketones according to the formula wherein n is an integer from 2 to 9;
[0012] (c) compounds of the formula C 6 H 5 R 5 , wherein R 5 is —H, —OH; C 1 to C 3 straight chain, saturated or unsaturated hydrocarbon radicals, —CO 2 H; —CN; —COC m , wherein m is an integer from 1 to 6; —OC m , wherein m is an integer from 1 to 6; or NR 6 R 7 , where R 6 and R 7 are each independently —H or C 1 to C 3 alkyl groups;
[0013] (d) alicyclic hydrocarbons according to the formula R 8 R 9 CH 2 ,
[0014] wherein R 8 and R 9 together from a link of (—CH 2 —) p , wherein p is an integer from 4 to 11;
[0015] (e) aliphatic hydrocarbons of the formula C q H 2q+2 , wherein q is an integer from 1 to 20; and
[0016] (f) alcohols according to the formula R 10 R 11 CHOH, wherein R 10 and R 11 are each independently —H; alkyl, wherein the alkyl group has from 1 to 16 carbon atoms; alkylaryl, wherein the alkylaryl group has from 7 to 16 carbon atoms; cycloalkyl, wherein the cycloalkyl group has from 6 to 10 carbon atoms; cycloalkyl wherein R 10 and R 11 taken together form a link containing 4 to 11 —CH 2 — groups; or alkylcycloalkyl, wherein the alkylcycloalkyl group has from 7 to 16 carbon atoms.
[0017] The invention also provides a process for the preparation of an aerogel catalyst comprising synthesizing a catalyst comprising oxides of silicon and a peroxide-activating metal by (i) preparing a sol-gel containing silicon and a peroxide-activating metal; (ii) extracting the gel with a solvent to remove substantially all of the water from the gel and optionally removing the solvent; (iii) washing the gel with a solvent for the silylating agent; (iv) treating the gel with a silylation agent; (v) drying the treated gel at a temperature of from about ambient to about 130° C.; and optionally (vi) calcining the gel at a temperature of less than about 400° C.
[0018] The present invention further provides a catalyst composition comprising silica and an oxide of at least one peroxide-activating metal characterized by (i) having a silicon to peroxide-activating atomic ratio of less than 10,000 to 1; (ii) being x-ray amorphous; (iii) possessing a Si—C infrared band; and (iv) having a surface area greater than 500 m 2 /g, a pore volume greater than 0.5 mL/g and an average pore diameter of greater than 4 nm.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0019] Peroxide-activating metals include, for example, silver, cobalt, cerium, manganese, iron, copper, molybdenum, tungsten, vanadium, titanium, chromium and mixtures thereof. A presently preferred metal is tetrahedrally coordinated titanium. Amorphous titania/silica aerogels prepared according to the process of this invention where the weight ratio of TiO 2 to SiO 2 is between 0.0005:1 and 0.5:1 are the preferred catalyst in the above-named oxidation reactions.
[0020] In accordance with this invention, gels containing silica and an oxide of the peroxide-activating metal are prepared by combining a silicate selected from the group consisting of Si(OR 12 ) 4 and SiR 14 (OR 13 ) 3 , Si(OR 12 ) 4 and SiH(OR 13 ) 3 , where R 12 is a C 1 to C 4 alkyl group, R 13 is a C 1 to C 8 alkyl group and R 14 is H, C 6 H 5 or R 13 , where C 6 H 5 is a phenyl group, with alkoxides of the peroxide-activating metals, selected from the group consisting of —(OR 13 ) n where n is the valence of the peroxide-activating metal.
[0021] A solution of a concentrated mineral acid such as HCl, HNO 3 or H 2 SO 4 ; or an organic acid with a pK a equal to or less than 4, such as formic and trifluoroacetic acids; or a base selected from the group consisting of ammonia, and a water-soluble organic amine such as methylamine and ethylamine; optionally water; and an alcohol selected from the group consisting of R 13 OH, where R 13 is as defined above, is prepared. The C 1 to C 4 alcohols are preferred. The acidic or basic alcohol solution as defined above is added to the mixed oxide solution such that the alcohol to water ratio is greater than 2 by volume. After stirring at room temperature for at least five minutes, additional alcohol from the group described above is added in an amount such that the total alcohol to water ratio is less than 100. The mixture is stirred for between about 0.1 and 350 hours at temperature of from about 0° C. to about 50° C. to produce a gel.
[0022] For the preferred titanium-containing gels, the titanium source compound can be selected from the group consisting of Ti(OR 12 ) 4 , where R 12 is as defined above; Tyzor® organic titanates such as the acetylacetonate chelate, the ammonium lactate chelate, the triethanolamine chelate and the 2-ethylhexyl ester of orthotitanic acid; organotitanium compounds containing cyclopentadienyl groups such as (C 5 H 5 )TiCl 3 and (C 5 H 5 ) 2 TiCl 2 , where C 5 H 5 is a cyclopentadienyl group.
[0023] The water is removed from the gel by extraction with a protic solvent (e.g., an alcohol) or an aprotic solvent (e.g., acetone or tetrahydrofuran). If the silylating agent is not soluble in the extraction solvent, then a solvent in which it is soluble in such as acetone, toluene or tetrahydrofuran, is used to further extract the gel to remove the original solvent. The extracted gel is then stirred in a solution of a solvent and silylating agent. One skilled in the art would know which solvent or combination of solvents to use. The molar ratio of silylating agent:(Si +peroxide-activating metal) is between from about 0.1:1 to about 2: 1, preferably 1.5:1.
[0024] Suitable silylating agents include organosilanes, organosilylamines, and organosilazanes. Examples of suitable silanes include chlorotrimethylsilane ((CH 3 ) 3 SiCl), dichlorodimethylsilane ((CH 3 ) 2 SiCl 2 ), bromochlorodimethylsilane ((CH 3 ) 2 SiBrCl), chlorotriethylsilane ((C 2 H 5 ) 3 SiCl) and chlorodimethylphenylsilane ((CH 3 ) 2 Si(C 6 H 5 )Cl). Examples of suitable silazanes include 1,2-diethyldisilazane (C 2 H 5 SiH 2 NHSiH 2 C 2 H 5 ), 1,1,2,2-tetramethyldisilazane ((CH 3 ) 2 SiHNHSiH(CH 3 ) 2 ), 1,1,1,2,2,2-hexamethyldisilazane ((CH 3 ) 3 SiNHSi(CH 3 ) 3 ), 1,1,2,2-tetraethyldisilazane (C 2 H 5 ) 2 SiHNHSiH(C 2 H 5 ) 2 and 1,2-diisopropyldisilazane ((CH 3 ) 2 CHSiH 2 NHSiH 2 CH(CH 3 ) 2 ).
[0025] Preferred silylating agents include silazanes and N,O-bis(trimethylsilyl)-trifluoroacetamide (CF 3 C(OSi(CH 3 ) 3 )═NSi(CH 3 ) 3 ). These two agents do not generate corrosive hydrogen halides when they are used unlike the organosilanes.
[0026] The gel is separated from the solvent, washed with the solvent and dried at a temperature of from between room temperature and 110° C.
[0027] The gel exhibits a band in the infrared absorption region at about 1050 cm −1 to about 1300 cm −1 indicating the presence of an Si—C group in the gel. The Si—C group is selected from the group consisting of (CH 3 ) 3 Si, (CH 3 ) 2 SiCl, (C 2 H 5 ) 3 Si, (CH 3 ) 2 Si(C 6 H 5 ), C 2 H 5 SiH 2 , (CH 3 ) 2 SiH, (C 2 H 5 ) 2 SiH and (CH 3 ) 2 CHSiH 2 .
[0028] The peroxides useful for this invention include hydrogen peroxide and hydrocarbon hydroperoxides. For the hydrocarbon compounds, preferred are secondary and tertiary hydroperoxides of up to fifteen carbon atoms, especially tertiary alkyl hydroperoxides such as tertiary bytyl hydroperoxide; and alkyl hydroperoxides wherein the hydroperoxy group is on a carbon atom attached directly to an aromatic ring, e.g., α-hydroperoxy-substituted aralkyl compounds such as α-methylbenzyl hydroperoxide and cumene hydroperoxide.
[0029] A wide variety of organic compounds can be oxidized by the process of this invention. Presently preferred organic compounds are listed above in the “Summary of the Invention”.
[0030] Olefins useful in the process of this invention may be any organic compound having at least one ethylenically unsaturated functional group (i.e., a carbon-carbon double bond) and may be a cyclic, branched, or straight chain olefin. The olefin is reacted with hydrogen peroxide to produce an epoxide (oxirane). The olefin may contain aryl groups such as phenyl. Preferably, the olefin is an aliphatic compound containing from 2 to 20 carbon atoms. Multiple double bonds may be present in the olefin, e.g., dienes, trienes, and other polyunsaturated substrates. The double bond may be in a terminal or internal position of the olefin or may form part of a cyclic structure as in cyclohexene. Other, non-limiting examples of suitable organic compounds include unsaturated fatty acids or esters and oligomeric or polymeric unsaturated compounds such as polybutadiene.
[0031] The olefin may optionally contain functional groups such as halide, carboxylic acid, ether, hydroxy, thio, nitro, cyano, ketone, acyl, ester, amino, and anhydride.
[0032] Preferred olefins include ethylene, propylene, butenes, butadiene, pentenes, isoprene, and hexenes.
[0033] Mixtures of olefins may be epoxidized and the resulting mixtures of epoxides may be used in mixed form or separated into the component epoxides.
[0034] Olefins especially preferred for the process of this invention include those of the formula R 1 R 2 C═CR 3 R 4 , wherein R 1 , R 2 , R 3 and R 4 are each independently selected from the group consisting of H and C 1 to C 12 straight chain, saturated, or unsaturated hydrocarbon radicals.
[0035] Cyclic ketones useful in the process of this invention include cyclopentanone, cyclohexanone. The cyclic ketone is reacted with the in-situ generated hydrogen peroxide to produce lactones. For example, cyclopentanone is converted to valerolactone and cyclohexanone is converted to caprolactone. Also, in the presence of ammonia cyclohexanone is converted to cyclohexanone oxime.
[0036] Compounds of the formula C 6 H 5 R 5 , wherein R 5 is selected from a group as defined in the “Summary of the Invention”, are reacted with hydrogen peroxide to produce phenols. For example, phenol, itself, is converted to hydroquinone and toluene is converted to catechol.
[0037] Alicyclic hydrocarbons of the formula R 8 R 9 CH 2 , wherein R 8 and R 9 together form a link selected from the group consisting of (—CH 2 —) p , wherein p is an integer from 4 to 11 useful in the process of this invention include cyclohexane and cyclododecane. Alicyclic hydrocarbons of the formula R 8 R 9 CH 2 are reacted with hydrogen peroxide to produce ketones and alcohols. For example, cyclohexane is converted to a mixture of cyclohexanol and cyclohexanone and cyclododecane is converted to a mixture of cyclododecanol and cyclododecanone.
[0038] Aliphatic hydrocarbons of the formula C q H 2q+2 , wherein q is an integer from 1 to 20 useful in the process of this invention include hexane and heptane. Aliphatic hydrocarbons of the formula C q H 2q+2 are reacted with hydrogen peroxide to produce alcohols and ketones.
[0039] Alcohols according to the formula R 10 R 11 CHOH, wherein R 10 and R 11 are as defined above include 2-butanol, cyclohexanol, and cyclododecanol. These alcohols are oxidized to 2-butanone, cyclohexanone, and cyclododecanone, respectively.
[0040] In another embodiment of this invention, oximes can be prepared by reacting cyclic ketones of the formula
[0041] wherein n is an integer from 2 to 9, with hydrogen peroxide and ammonia in the liquid phase in the presence of the catalysts of this invention and then recovering the oxime product.
[0042] The reaction may also be conducted in organic solvents. Some preferred organic solvents are hydrocarbons such as hexane, benzene, methylene chloride, acetonitrile, lower aliphatic alcohols, ketones and dioxane, dimethylformamide and dimethylsulfoxide and mixtures thereof. Preferably, the solvents which are used are ones in which the substrate and products of the reaction are highly soluble.
[0043] The reaction is typically conducted at temperatures of from about 0° C. to about 200° C., preferably from about 25° C. to about 150° C. The reaction pressure is typically from about 1 atmosphere to about 100 atmospheres.
[0044] The oxidation products are recovered from the product mixtures by conventional techniques such as fractional distillation, extraction, and crystallization.
[0045] Without further elaboration, it is believed that one skilled in the art can, using the preceding description, utilize the present invention to its fullest extent. The following specific embodiments are, therefore, to be construed as merely illustrative, and are not to limit the remainder of the invention in any way whatsoever. All percentages are by weight unless otherwise indicated.
EXAMPLES
Example 1
Preparation of SiO 2 /TiO 2 Catalyst with Hexamethyldisilazane (HMDS)
[0046] a. Preparation of Modified Titanium-isopropoxide (Ti-iprop) Solution
[0047] Ti-iprop (28.4 g) and isopropyl alcohol (IPA, 30 mL) are mixed in a drybox in a 200 mL round-bottom flask. Acetylacetone (acac, 10.01 g) in IPA (10 mL) are added. This solution is refluxed for 1 hour and cooled. The IPA was removed by vacuum and the remaining yellow paste was redissolved in IPA and made up to 100 mL in a volumetric flask. This is a IM solution of Ti-acac.
[0048] b. Solgel Preparation
[0049] In the drybox, the Ti-acac solution (25 mL), tetramethylorthosilicate (45.66 mL) and IPA (44 mL) were mixed in a 500 mL plastic bottle. A solution of conc. HCl (2.4 mL), H 2 O (29.2 mL) and IPA (30 mL) were added. After stirring at room temperature for 5 minutes, additional IPA (168 mL) was added. This mixture was stirred for 90 hours. The Si:Ti atomic ratio of the gel as charged is 12:1.
[0050] c. Solgel Modification
[0051] The gel was extracted in a Soxhlet apparatus with IPA for 24 hours and twice with hexane for 24 hours. The extracted gel was stirred in a solution of hexane (500 mL) and hexamethyldisilazane (78.6 g) at room temperature for 90 hours. After filtering, the gel was washed twice with hexane (750 mL) at room temperature.
[0052] d. Drying/Calcination
[0053] The gel was then air dried at room temperature for 24 hours and then dried in a vacuum oven at 110° C. for 24 hours. The Si:Ti atomic ratio of the material was 15.6:1.
[0054] The catalyst of had an infrared band attributable to the —Si—(CH 3 ) 3 group at about 1260 cm −1 . This material was designated Cat. 1.
[0055] Another sample of Cat. 1 was calcined at 450° C. in air for 4 hours. The Si:Ti atomic ratio of the material was 21.5:1. This material was designated Cat. 1A.
Example 2
Preparation of SiO 2 /TiO 2 Catalyst with Trimethylsilylchloride (TMSiCl)
[0056] Steps a to d of Example 2 were repeated except that in step c TMSiCl (52.96 g) was used. The final product had a Si:Ti ratio of 126:1, indicating significant loss of Ti during silylation of the gel. This material was designated Cat. 2.
Example 3
Preparation of SiO 2 /TiO 2 Catalyst with Bis(trimethylsilyl)trifluoroacetamide (BSTFA)
[0057] Steps a to d of Example 2 were repeated except that in step c BSTFA (125.48 g) was used. The final product had a Si:Ti ratio of 15.7:1. This material was designated Cat. 3.
[0058] The catalysts prepared in Examples 2 and 3 had an infrared band at ˜1260 cm −1 , indicating —Si—(CH 3 ) 3 groups.
Example 4
Epoxidation of 1-Octene
[0059] A mixture of 1-octene (4.13 g), 10% hydrogen peroxide (2.04 g), and Cat. 1 (209 mg) was stirred at room temperature for 23 hours. GC analysis of the organic product showed a 10% yield to 1,2-octane epoxide based on hydrogen peroxide.
Example 5
Epoxidation of Cis-Cyclooctene
[0060] A mixture of cis-cyclooctene (2.44 g), 10% hydrogen peroxide (1.13 g), and Cat. 1 (51 mg) was stirred at room temperature for 23 hours. GC analysis of the organic product showed a 28% yield to cyclooctane epoxide based on hydrogen peroxide.
Example 6
Epoxidation of 1-Octene
[0061] A mixture of 1-octene (2.06 g), 10% hydrogen peroxide (1.01 g), and Cat. 1A (50 mg) was stirred at room temperature for 50 hours. GC analysis of the organic product showed a 0.2% yield to 1,2-octane epoxide based on hydrogen peroxide.
Example 7
Epoxidation of 1-Octene
[0062] A mixture of 1-octene (2.14 g), 10% hydrogen peroxide (1.21 g), and Cat. 2 (50 mg) was stirred at room temperature for 24 hours. GC analysis of the organic product showed a 5% yield to 1,2-octane epoxide based on hydrogen peroxide.
Example 8
Epoxidation of Cis-Cyclooctene
[0063] A mixture of cis-cyclooctene (2.44 g), 10% hydrogen peroxide (1.13 g), and Cat. 2 (53 mg) was stirred at room temperature for 2 hours. GC analysis of the organic product showed a 19% yield to cyclooctane epoxide based on hydrogen peroxide.
Example 9
Epoxidation of 1-Octene
[0064] A mixture of 1-octene (2.13 g), 10% hydrogen peroxide (1.07 g), and Cat. 3 (56 mg) was stirred at room temperature for 24 hours. GC analysis of the organic product showed a 10% yield to 1,2-octane epoxide based on hydrogen peroxide.
Example 10
Epoxidation of Cis-Cyclooctene
[0065] A mixture of cis-cyclooctene (2.35 g), 10% hydrogen peroxide (1.15 g), and Cat. 3 (55 mg) was stirred at room temperature for 24 hours. GC analysis of the organic product showed a 35% yield to cyclooctane epoxide based on hydrogen peroxide.
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Disclosed is a process for oxidizing organic compounds using hydrogen peroxide to oxidize an oxidizable organic substrate in the presence of a silylated peroxide-activating metal/silica-containing catalyst and to a method of preparing such a catalyst.
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The invention described herein may be manufactured, used, and licensed by or for the Government for governmental purposes without the payment to me of any royalties thereon.
TECHNICAL FIELD
The present invention relates to the utilization of permanent magnets to produce helically oriented magnetic fields which are particularly useful in high power broad-band radiation sources for microwave and millimeter-wave radars.
BACKGROUND OF THE INVENTION
Twister designed magnetic field generators have been provided by current carrying coils of very high amperage adapted to produce helically varying transverse magnetic fields of the magnetization desired. In recent developments, notably U.S. Pat. No. 4,764,773, incorporated herein by reference, permanent magnets have been designed and arranged in certain specific ways to form structures which produce desirable helical or "twisted" fields obviating the need for commonly used current carrying coils with their attendant weight and space problems. These structures are based upon the hollow cylindrical flux source (HCFS) principle described by K. Halbach in "Proceedings of the Eighth International workshop on Rare Earth Cobolt Permanent Magnets", Univ. of Dayton, Dayton, Ohio, 1985 (pp. 123-136). A HCFS, also referred to sometimes as a "magic ring", is essentially a cylindrical permanent magnet shell that produces an internal magnetic field which is relatively constant in magnitude. The field, which is perpendicular to the axis of the cylinder, (transverse) possesses a strength which can be greater than the remanence of the magnetic material from which the ring is made.
Ideally, the HCFS is an infinitely long annular cylindrical shell with a circular cross section, which produces an intense magnetic field in its interior working space. No magnetic flux extends to the exterior of the ring structure (except at ends of a finite cylinder). A HCFS is not limited to the ideal cylindrical structure, but may be represented by octagonal, sixteen sided, thirty-two-sided, and even higher order polygonal-sided structures which approximate the ideal HCFS structure.
In "twister" structures there also exists an undesirable longitudinal component of the magnetic field in combination with the transverse component, arising from the high helical motion, i.e. "frequency". As the frequency increases, the longitudinal component increases, weakening the transverse component. Therefore, it has been of increasing concern to produce stronger transverse magnetic fields in "twister" configurations.
SUMMARY OF THE INVENTION
It is therefore an object of this invention to provide a permanent magnet structure possessing a high transverse magnetic field strength with little or no longitudinal field strength.
It is a further object of this invention to provide a permanent magnet structure possessing a high transverse magnetic field at high operating frequency.
It is another object of this invention to provide a permanent magnet structure with minimal internal field distortion and minimal external flux leakage.
It is still another object of this invention to provide a permanent magnet structure with uniform interior magnetic flux.
The above and other objects are achieved in accordance with the present invention, which makes advantageous use of the HCFS twister structure uniquely combined with superconducting plates or sheets.
In an embodiment of the invention, a multiplicity of similarly magnetized octagonal hollow cylindrical flux source structures, each having a generally disposed hole therethrough, are arranged concentrically on an elongate axis with said holes defining an elongate axial passage extending through said structure, each octagonal structure rotated radially on the axial center line so as to displace its magnetization along a helical locus, thus giving the entire array the capacity to define a twisted or helically oriented magnetic field through the axially extending center passage. Superconducting sheets are interspersed between adjacent octagonal structures and also cover the end faces of the array. The superconducting sheets abutting the end faces of each octagonal structure confine the flux or magnetic filed to the interior of each structure, establish a uniform field in the interior, and isolate each structure from its nearest neighbors thereby preventing distortion of the field by neighbor-induced counterfields. Furthermore, high frequency may be maintained without the presence of a longitudinal magnetic field due to this isolation.
BRIEF DESCRIPTION OF THE DRAWINGS
The objects, features, and details of the invention will become more readily apparent in light of the detailed description and disclosure in connection with the accompanying drawings wherein:
FIG. 1 shows an actual magnet array comprising a series of octagonal HCFS structures with an angular displacement between successive structures; and
FIG. 2 shows an abbreviated magnet array comprising a series of octagonal HCFS structures with an angular displacement between successive structures, further including interspersing superconducting sheets between successive segments.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a multiplicity of octagonal HCFS structures 10, each having a generally centrally disposed hole 11 arranged in longitudinal array with the respective holes 11 concentrically in registration, and with each respective structure 10 displaced radially a preselected amount from its adjacent structure so that the magnetic orientation of the respective segments as the field is defined longitudinally through the extended passage goes through a twisting locus from the proximal end towards and to the distal end. The net effect of the arrangement is the production of a helically varying or twisting magnetic field through the array of holes 11 and the array can be termed a "twister". Along with this transverse magnetic field denoted by the arrow, 12, there exists a longitudinal component of magnetic field which results from the twisting, thereby weakening the transverse magnetic field.
FIG. 2 displays a preferred embodiment of the invention wherein a multiplicity of octagonal HCFS structures 10, each having a generally centrally disclosed hole 11 arranged in longitudinal array with the respective holes 11 concentrically in registration, and with each respective structure 10 displaced radially a preselected amount from its adjacent segment, are separated by superconducting sheets 13. The sheets 13 as shown in the figure are at least peripherally coextensive with the HCFS structures and can extend beyond the flux source structures, 10, in one or more directions. It is necessary that they be not less in extent than the structures 10. This figure represents a close approximation of the ideal HCFS array (which is not feasible to construct).
The superconducting sheets shown in the figure are typically quite thin. In practice, the essential requirement is that the sheets be thicker than the penetration depth of the specific superconducting material used. Materials such as tin, lead, niobium, tantalum among others are known to be superconducting below a distinct critical temperature. New ceramic-type materials have been recently developed in the field of superconductivity and are capable of achieving the superconducting state at critical temperatures above 77° K., the boiling point of liquid nitrogen. One such compound RBa 2 Cu 3 O 9-y (where R stands for a transition metal or rare earth ion and y is a number less than 9, preferable 2.1±0.05) has demonstrated superconductive properties above 90° K. Forming techniques include plasma spraying, sputtering, epitaxial film growing, etc. These materials and forming processes are merely exemplary and in no way limit the superconductivity material selected for the sheets, and the manner thereof in which the material is formed.
A bore hole is drilled through each superconducting sheet 13 along the central axis of the array thereby providing a passage in the working central cavities of the HCFS array through which an electron beam can travel. The array can be termed a "pyx twister".
In prior art twisters, the magnetic field was weakened by distortion. Distortion was caused by (1) the bending of the field lines of the end faces of open HCFS, and (2) interference with incoming flux leaking from neighboring open segments. The longitudinal component of magnetic field present due to the twisting effect, further increased with increasing frequency. By interspersing superconducting sheets between successive HCFS structures, the longitudinal magnetic field was prevented and distortion problems were overcome.
A superconducting surface prevents the penetration of a magnetic field. The addition of the superconducting sheets confines outward flux leakage from each working cavity of the array preventing flux penetration from neighboring cavities and not permitting the bending of the field lines at the end faces which would have occurred without the addition of the sheets. In this manner, the effect of interference from adjacent segments is eliminated, leaving the field within each pyx cavity unaffected by its neighbors. Each cavity thereby acts separately as one extremely long cavity, producing an intense transverse magnetic field, the longitudinal component becoming essentially nil. Consequently, the field is made substantially uniform.
Alternately, one may comprehend this effect through the concept of diamagnetic mirrors. The superconducting sheets 13 magnetically mirror the field abutting the surfaces of the sheets, thereby providing the appearance of an infinitely long cavity in both directions of each HCFS structure. Theoretically, a HCFS is infinitely long having uniform field strength. In essence, this invention magnetically creates a theoretical HCFS twister with uniform field strength through the utilization of superconducting plates.
Although octagonal HCFS structures are figuratively shown with interspersed superconducting sheets, rectangular shaped structures may also be employed in the present invention. More complex structures of HCFS design having cross sections of circles, sixteen sides, thirtytwo sides etc., may also be used in accordance with the present invention. Other components of the twister well known to those skilled in the art of design of such devices have been eliminated from the discussion. Also, greater or fewer magnetic pyxes may be desirable in any given application with no limit on the number of degrees of the angle of displacement nor the frequency of twist.
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Permanent magnet structures are fabricated from a plurality of hollow cylrical flux sources, the sources displaced radially from each other progressively along the structures' elongate axes so as to produce a heliform magnetic field extending centrally in a passage through the structures. Superconducting plates are interspersed between adjacent flux sources and also cover the end faces of the array.
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FIELD OF THE INVENTION
[0001] The present invention refers to antioxidant complexes derived from wine vinasses, wherefrom solid, semisolid or liquid formulations to be orally used as dietary supplements have been prepared. Said formulations comprise the same antioxidant complexes comprising polyphenolic compounds as contained in wine, e.g. resveratrols, and bioflavonoids, e.g. anthocyanins and polyphenols, but do not contain ethyl alcohol. Therefore, the said formulations do not present the hepatic and central toxicity problems caused by drinking wine to excess while providing for the well known benefits attributed to wine's natural constituents.
PRIOR ART
[0002] Fruit, vegetables and beverages derived therefrom contain important constituents of the non-energetic diet displaying -antioxidant activity. More than 300 organic compounds belonging to the classes of carboxylic acids, mono- and disaccharides, amines, polyphenolic compounds, volatile compounds and pigments have been identified in wine. The major source of antioxidant activity are the polyphenolic compounds, which also affect the wine taste and colour. Particularly important are flavonoids, including catechins (catechin, epicatechin), flavone glycosides, flavonols (myricetin, quercetin, rutin, campherol, isoramnetin), flavanones, anthocyanins (delphinin, cyanin, petunin, peonin, malvin) and relevant anthocyanidins, and stilbenes (cis and trans resveratrols and glycosides thereof) present at higher concentrations in red grape skins and seeds, and in red wine.
[0003] Wine also contains carboxylic acids, such as for example citric and tartaric acid; benzoic acids, e.g. gallic acid, protocatechuic acid, vanillic and hydroxybenzoic acids; cinnamic acids, e.g. caffeic, cumaric, ferulic acids and others (M. Calull et al., J. Chromatogr., 590, 212-22, 1992; F. Mattivi, G. Nicolini, Biofactors, 6, 445-448,1997; E. N. Frankel et al., J. Agric. Food Chem., 43, 890-894, 1995).
[0004] A great number of benefits are brought about by the phenolic groups, due to their antioxidant, free-radical-inhibitory and metal sequestering activity (Catherine A. Rice-Evans et Lester Packer, Flavonoids in Health and Disease, Marcel Dekker, NY, 1998). Said groups protect man against cardiovascular diseases and thromboses caused by an excess of free oxygen radicals. Resveratrols, in particular, can inhibit platelet aggregation (R. J. Gryglewski et al., Biochem. Pharmacol., 36, 317-322, 1987) and prevent oxidation of low-density lipoproteins (LDL) (E. N. Frankel et al., Lancet, 341, 454-457, 1993). Furthermore, thanks to the presence of the aforementioned compounds, the moderate consumption of wine can increase the antioxidant capacity of human serum (Whitehead et al, Clin. Chem., 41, 32-35, 1995), can increase the plasmatic level of α-tocopherol and retinol (P. Simonetti et al., Alcohol Clin. Exp.Res., 19 (2), 517-522, 1995), and reduce fibrinogen levels (N. Pellegrini et al., Eur.J.Clin. Nutr., 50, 209-213, 1996). Finally, it has been found that a glass of red wine provides the organism with a much greater amount of flavonoids than that supplied by vegetables (P. G. Pietta et al. Dietary flavonoids and oxidative stress in “Natural antioxidants and food quality in atherosclerosis and cancer prevention”, J. T. Kumpfalien, Cambridge, 249-255, 1996), but that, especially in the case of heavy consumption of wine, alcohol causes considerable untoward side effects (M. Gronbaek et al., Biochem. Pharmacol., 36, 317-322,1987).
[0005] It is, therefore, clear that alcohol contributes in turn to the beneficial effect associated with wine consumption, as it secures the solubility of antioxidant complexes—in particular polyphenols—in the intestine environment (Goldberg, Clin. Chem. 41, 14-16, 1995) and that the bioavailability of the antioxidant complexes, in particular of the polyphenols present in grapes (or in the juice, skins and seeds thereof) is lower than that of the same polyphenols contained in wine.
[0006] It is therefore an object of the present invention to provide a food-grade substance capable of fully replacing a “daily” glass of wine—recommended in medical literature—whenever wine consumption is not advisable due to dietetic reasons or is forbidden by religious regulations.
[0007] It is a further object of the present invention to provide an alcohol-free, in particular ethyl alcohol-free, dietary supplement capable of supplying the organism with the antioxidant complexes commonly contained in wine, which are highly useful to the organism itself.
[0008] It is a still further object of the present invention to provide a dietary supplement bringing about an absorption of the antioxidant complexes commonly contained in wine, which is constant in time.
[0009] It is another object of the present invention to provide a process of manufacture of a dietary supplement, which process uses cheap and easily available raw materials and does not alter the antioxidant complexes contained therein.
SUMMARY OF THE INVENTION
[0010] The above and further objects—which will be better described hereinafter—are achieved through a dietary supplement obtained from wine vinasse. In particular, according to an aspect of the present invention, a dietary supplement from wine vinasse suitable for oral administration is provided. According to a further feature of the present invention, a process for the obtainment of a dietary supplement in solid or liquid formulation from wine vinasse is provided.
DETAILED DESCRIPTION OF THE INVENTION
[0011] Vinasse is the aqueous residue resulting from the distillation of wine, intended for the production of tasty alcohol for the liquor industry. Vinasse is a waste matter to be disposed of. It still contains all aforementioned classes of compounds (carboxylic acids, mono- and disaccharides, amines, polyphenolic compounds and pigments), whereas only ethyl alcohol and, partly, the flavouring volatile compounds have been eliminated.
[0012] By way of example, one litre of red wine can averagely contain 0.6 to 11 mg resveratrols (depending on the zone of origin) and gives approx. 0.7 l vinasse with a residue of 0.5 to 2.5% by wt., containing most of the antioxidant complexes present in wine. All of the above compounds are potentially of great biological interest; however, once they are separated from the alcoholic fraction, they have such a reduced bioavailability that they of little use for the organism. That is the reason why wine vinasses or concentrates thereof cannot be used as dietary supplements capable of simulating the dietetic properties of wine.
[0013] It is an object of the present invention to overcome the considerable wasting caused by the non-usability of vinasses through the exploitation of the antioxidants contained therein and the elimination of the relevant disposal problem. Therefore, according to the present invention, the vinasses have been added with particular substances capable of increasing the solubility and absorption in vivo of their components (said substances are called “bioavailability promoters”), such as to restore all of the dietetic properties of wine. We have indeed surprisingly found that there is a series of compounds, heterogeneous with one another from a chemical standpoint, which have the specific ability of restoring (“promoting”) the bioavailability of the useful compounds contained in vinasses and, therefore, allow use of vinasses as antioxidant dietary supplements. According to the present invention, the absorption of the antioxidant complexes present in wine vinasses may be restored with bioavailability promoters selected from the group consisting of polysaccharides (such as for example dextrans, maltodextrins, and inulin) and amino acids such as for example glycine, proline, leucine, and lysine.
[0014] According to a preferred embodiment of the present invention, the absorption (and, consequently, the haematic levels) of the antioxidant complexes present in wine vinasse is rendered more constant in time by means of sustained release formulations. Such a constant absorption profile could be hardly obtained through wine consumption itself, since wine should be drunk in small quantities and continually in the space of 24 hours. Consequently, the present invention allows not only to simulate the whole dietetic properties of wine, but also to render the said properties available in a more uniform manner in time: the organism can thus better face the continuous exposure to radicals.
[0015] The Applicant has also developed processes for the preparation of solid compositions, which do not alter the active ingredients. The liquid forms are directly obtained from vinasses, preferably after addition of bioavailability promoters, followed by filtration.
[0016] The starting products utilised in the present invention are preferably marc-red and moderately sweet vinasses of red wine, whose resveratrols and anthocyans concentration is higher than that of white or rosé wines.
[0017] In the case of drinkable preparations, vinasses are added with polysaccharides, e.g. dextrans, maltodextrins or inulin, or else amino acids, e.g. such as for example glycine, proline, leucine, and lysine, as bioavailability promoters to increase the in vivo assimilation of dietetically precious compounds, i.e. of antioxidant complexes. Out of dextrans, dextran 5 (m.w. 5000) is preferably used, and out of maltodextrins, those having 9-12 dextrose equivalents (DE) are preferred, in particular Maltrin® M500. Especially the vinasses of white and rosé wines are optionally added e.g. with vitamin C or green tea, blueberry, strawberry or red currant extracts, which enhance the antioxidant capacity. If necessary, to improve the pleasant taste, vinasses are added with substances preferably but not compulsorily present in wine, e.g. organic acids, sugars and amines, colouring and flavouring agents like e.g. limonene, diethylsuccinate, hexyl acetate, trans-hexenol and/or citronellol. The solutions are then filtered through a 0.45 μm porous filter and poured into “drinkable” vials or tiny bottles.
[0018] In the case of solid preparations for packets, capsules and tablets, the aforesaid solutions containing bioavailability promoters are dried preferably by freeze-drying or spray-drying. With a view to improving granulation and compression processes, the solid residue is then mixed with the same raw materials as usually employed in food industry as diluents, binding agents, anticaking agents and absorbents. Alternatively, vinasses drying may also be carried out before addition of bioavailability promoters and/or optional additives.
[0019] In relation to the starting liquid vinasse, the bioavailability promoters used in the present invention are dextrans, inulin or maltodextrins at concentrations of 0.4% to 30% (g/100 ml), and glycine, proline, leucine or lysine at concentrations of 0.12% to 2% (g/100 ml). The optional antioxidants used, especially for vinasses from white or rosé wines, are blueberry dry extract, 25% in anthocyanidins, at concentrations of 0.015% to 0.1% (g/100 ml), decaffeinated green tea dry extract, 50% in polyphenols at concentrations of 0.1% to 2% (g/100 ml), currant dry extract, 3.8% in flavonoids, at concentrations of 0.013% to 0.08% (g/100 ml), and vitamin C at concentrations of 0.2% to 2% (g/100 ml).
[0020] For the preparation of solid forms, the starting solution or the dry residue are added with excipients, diluents, binding agents, such as for example lactose (qs) (preferably from 0.4% to 0.7% (g/l 00 ml) in the case of the solution or from 12% to 30% in the case of the dry residue); starch, e.g. from potatoes (qs) (preferably from 0.4% to 0,7% (g/100 ml) in the case of the solution or from 6% to 25% in the case of the dry residue); microcrystalline cellulose (qs) (preferably from 0.7% to 1% (g/100 ml) in the case of the solution or from 1% to 38% in the case of the dry residue); mannitol (qs) and/or silica (qs). In particular, lactose and cellulose allow a direct compression of powders or the preparation of a granulated product by the wet or dry method. In a preferred embodiment of the invention, also 10% to 50% hydroxypropyl methylcellulose, having a viscosity of 4000 cps, is used for the sustained release tablets coating.
[0021] For the drinkable solution, the use of a preservative, such as benzyl alcohol (0.5-1%) or sodium benzoate (o.02-0.5%) and a further addition of a stabiliser, e.g. citric or tartaric acid, already present in wine, is also envisaged.
[0022] Analytical Control
[0023] The following compounds were identified within vinasses as such, as well as within the antioxidant complexes obtained by dry concentration thereof: resveratrol, quercetin and catechin, total phenols and anthocyanins.
[0024] Total polyphenols were identified by a method developed at our laboratories, based on UV-VIS spectrometry. Red wine vinasses and complexes obtained therefrom were diluted up to 200 times with methanol, whereas the white wine ones were diluted up to 40 times. A catechin-methanol solution at a concentration of 10 mg/ml was used as a reference. Each determination was repeated 5 times.
[0025] The analysis showed an absorption spectrum between 200 and 500 nm for all samples with D.O. value at 280 nm. The total polyphenols content was calculated as catechin concentration (mg/1).
[0026] Resveratrols were instead determined using a liquid chromatograph comprising an UV/VIS detector, and a 100 CN 250×4 mm column (Lichrosphere). The mobile phase was water:acetronitrile:methanol (90:5:5) at a flow rate of 1 ml per minute. The wavelength was set at 306 nm. (D. M. Goldberg et al., J. Chromatogr. A 708, 89-98, 1995). The samples to be analysed were dissolved in alcohol and diluted with a 0.2 M phosphoric acid:acetonitrile solution (4:1).
[0027] For the determination of total anthocyans, use was made of a method capable of determining the concentration of same from the test sample absorbance variation resulting from the decolouration brought about by the reaction with sulphur dioxide. To this end, the sample was first diluted in ethanol and HCl; then, a part thereof was added with water and a part with a sodium bisulphite solution. The difference in absorbance between the two solutions allows for the calculation of the anthocyanes mg/l.
[0028] Quercetin and catechin were determined simultaneously by a method developed at our laboratories using a liquid chromatograph comprising a variable wavelength UV/VIS detector and a 125×4 mm column (Lichrosorb Diolo). The mobile phase was hexane:ethanol (70:30) acidified with phosphoric acid, at a flow rate of 0.8 ml per minute. The wavelength was set at 280 nm. The substances were diluted in ethyl alcohol to obtain solutions at a concentration of 10 mcg/ml; and 20 mcl of the same was injected.
[0029] The peaks were clearly distinct, the retention time being approx. 6 min for quercitin and approx. 13 min for catechin.
[0030] Antioxidant Capacity
[0031] The antioxidant capacity of vinasses and complexes was determined by the Miller-Rice-Evans method (N. J. Miller, C. Rice-Evans, Redox Rep., 2 (3), 161-171, 1996).
[0032] The chromogenic substance ABTS [2,2′-azinobis(3-ethyl-benzothiazoline-6-sulphonate] in the presence of potassium persulphate was converted into a blue-green monocationic radicalic form, ABTS −+ . The addition of an antioxidant analogous to vitamin E, denominated Trolox, caused—in proportion to the concentration of same—the decolouration of the solution, whose absorbance value was spectrographically read at 734 nm. The antioxidant capacity (TAC) of vinasses and of the new products was determined by comparing the absorbance value of the radicalic solution contacted with Trolox and with the test sample; it is expressed as mM Trolox eq./kg.
[0033] Table 1 shows, by way of example, the concentrations of some polyphenolic compounds in red wine vinasses (Recioto, 1998 vintage), in a Recioto freeze-dried vinasse, in a spray-dried rosé vinasse, 1998 vintage, in vinasses of Pinot grigio of the Veneto region, 1999 vintage, and the antioxidant capacity of same.
TABLE 1 Resveratrol Catechin Quercetin Total phenols Anthocyans TAC mM Sample mcg/ml mcg/ml mcg/ml mcg/ml mcg/ml Trolox Recioto 3.7 1.9 0.02 24. 88.9 3.9 vinasses Freeze- 3.5 1.9 0.02 26 246 6.3 dried Example 3 Atomised 1.8 1.7 0.03 21 153 4.0 Example 5 Pinot 0.05 0.02 n.d. 16.2 n.d. 0.6 grigio vinasses
[0034] Experimental Part
[0035] The following examples illustrate the claimed invention. These examples are illustrative only; in no event are they to be regarded as limiting the scope of the invention, which is defined by the claims reported hereinafter.
EXAMPLE 1
Drinkable Solution of Red Wine Vinasse with Dextran
[0036] Red wine vinasses (1 l) of a winy and moderately sweet taste were added with dextran 5 (20 g; m.w. 5000), fructose (0.6 g), blueberry dry extract (0.15 g), sodium benzoate (50 mg) and citric acid (0.2 g). The resultant solution was filtered through a 0.45 μm porous filter and bottled. A beverage of pleasant taste having an antioxidant capacity equal to 4.12 mM Trolox was obtained.
EXAMPLE 2
Freeze-Dried White Wine Vinasse with Maltodextrin
[0037] White wine vinasses (1 l) were added with maltodextrin (100 g), i.e. Maltrin® M500, blueberry extract (1 g) and green tea extract (1 g). The resultant solution was filtered through a 0.45 μm porous filter and freeze-dried according to a cycle comprising the following temperatures: −35° C. for pre-freezing, −10° C. during freeze-drying, 0° C., +10° C. and 28° C. for drying. 7.4·10 −2 mbar vacuum was maintained.
[0038] The light pink granular powder obtained (117 g) had an antioxidant capacity equal to 4.2 mM Trolox.
EXAMPLE 3
Freeze-Dried Red Wine Vinasse with Maltodextrin
[0039] Red wine vinasses (1 l) were added with maltodextrin (110 g), i.e. Maltrin® M500, and blueberry extract (0.7 g). The resultant solution was filtered and freeze-dried as described in Example 2. The residue obtained (124.5 g), in the form of a hygroscopic marc-coloured powder, had an antioxidant capacity equal to 6.3 mM Trolox.
EXAMPLE 4
Freeze-Dried Red Wine Vinasse with Inulin and Glycine
[0040] Red wine vinasses (1 l) were added with inulin (5 g), glycine (1.8 g), green tea extract (2 g), and lactose (5 g). The resultant solution was filtered and freeze-dried according to the cycle described in Example 2. The dry residue obtained (27.4 g), in the form of a pink-violet compact powder, had an antioxidant capacity equal to 8.9 mM Trolox.
EXAMPLE 5
Spray-Dried Rosé Wine Vinasse with Dextran
[0041] In pink-coloured vinasses (1 l) were dissolved dextran 5 (5 g; m.w. 5000), blueberry extract (1 g), lactose (6 g), and starch (5 g). The resultant solution was filtered through a 0.45 μm porous filter and spray-dried by means of a mini spray-dryer (Mini Buchi): jet pressure 800 mbar, inlet T° 130° C., outlet T° 50° C., suction 100%.
[0042] The light pink granular powder obtained (32 g) had an antioxidant capacity equal to 4.0 mM Trolox.
EXAMPLE 6
Spray-Dried Red Wine Vinasse with Dextran
[0043] In dark red vinasses (1 l) were dissolved dextran 5 (4 g) (m.w. 5000), microcrystalline cellulose (8 g) and vitamin C (3 g). The resultant solution was filtered and dried as described in Example 5. The garnet-red fine powder obtained (29 g) had an antioxidant capacity of 4.5 mM Trolox.
EXAMPLE 7
Granulated Product Preparation
[0044] The product described in Example 3 was mixed with microcrystalline cellulose (2 g) and wet with a 5% PVP-ethanol solution (20 ml) to give a granulation mixture. The wet mass was sieved through a No. 25 sieve, dried in an air circulated oven at 35° C. and graded by size through the same sieve.
EXAMPLE 8
Capsules Preparation
[0045] The granulated product described in Example 7 was added with silica precipitate (0.4 g). The resultant product could fill one hundred and twenty 1 g capsules.
EXAMPLE 9
Packets Preparation
[0046] The granulated product described in Example 7 was added with citric acid (3 g), sodium bicarbonate (3 g), fructose (2 g), flavouring agent (1 g), and silica (0.4 g) to give a product to be subdivided into sixty 2 g packets.
EXAMPLE 10
Tablets Preparation
[0047] The product described in Example 4 was wet with a 4% PVP solution (10 ml). The wet mass was sieved through a No. 25 sieve, dried in an air circulated oven at 35° C. and graded by size through the same sieve. It was added with microcrystalline cellulose (1 g), fructose (1.5 g), flavouring agent (0.25 g), magnesium stearate (0.35 g) and talc (0.35 g), by simple mixing.
[0048] The powder was compressed with a manual press (pressure applied: 1000 kg), using 10 mm dia. hollow punches, to give fifty-five 0.5 g tablets.
EXAMPLE 11
Chewable Tablets Preparation
[0049] The product described in Example 4 was added with microcrystalline cellulose (1 g), fructose (2 g), flavouring agent (0.4 g), magnesium stearate (0.3 g) and talc (0.3 g), by simple mixing.
[0050] The powder was compressed by a press using 13 mm dia. flat punches, with cracker, to give twenty-five 1 g tablets.
EXAMPLE 12
Effervescent Tablets Preparation
[0051] The residue of Example 6 was mixed with lactose (4.15 g), starch (2 g), fructose (2 g), flavouring agent (0.5 g), enocyanin powder (10 mg), citric acid (2.5 g) and sodium bicarbonate (2.5 g). The powder was compressed with a press using 20 mm dia. flat punches. The tablets weighing 2 g were immediately enclosed in blister packs.
EXAMPLE 13
[0052] Sustained Release Tablets Preparation
[0053] The product described in Example 4 was wet with a 4% PVP solution (10 ml). The wet mass was sieved through a No. 25 sieve, dried in an air circulated oven at 35° C. and graded by size through the same sieve. It was added with microcrystalline cellulose (1 g), magnesium stearate (0.35 g) and talc (0.35 g), by simple mixing.
[0054] The granulated product was compressed with a single manual press, using a 10 mm dia. hollow punch, to give 0.5 g tablets.
[0055] Hydroxypropyl methylcellulose (6 g), magnesium stearate (250 mg) and colloidal silica (150 mg) were mixed in a turbulator for a period of 15 min. The punch previously used was replaced by a 12 mm dia. hollow punch; then the single nuclei were coated with the mixed powder. In particular, the matrix was filled with powder (53 mg), a nucleus, further powder (53 mg) and, finally, was compressed.
[0056] The dual compression technique afforded 60 sustained release tablets, each weighing 0.6 g (±5%).
[0057] Industrial Applicability
[0058] The present invention provides compositions derived from wine vinasses added with bioavailability promoters, which may be used as dietary supplements capable of simulating the dietetic properties of wine, but without the toxic effects of alcohol. Furthermore, the sustained release compositions from wine vinasses make the beneficial effect of wine constant in time; furthermore, their effect simulates that produced by a continuous wine consumption.
[0059] The liquid and solid dietary supplements described may be added with further antioxidants, whenever necessary, in particular when derived from white or rose wine vinasses, which—as shown by the analytical data reported above—are rather poor in resveratrol.
[0060] The vinasses solid derivatives were obtained by freeze-drying and spray-drying processes, which are rapid, little expensive and do not deteriorate the antioxidant complexes.
[0061] The tablets, capsules or granulated products (preferably formulated for sustained release) are an alternative to drinkable solutions and are particularly appreciated by those who constantly use said compositions to react against radicals unbalance caused by: environmental pollution, tobacco smoke, stress, prolonged muscular efforts, incorrect diet, alcoholic drinks, some drugs, infective agents, inflammatory and neoplastic diseases.
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The present invention refers to a dietary supplement containing all of the natural components of wine, except for the volatile ones, in particular ethanol. Said dietary supplement is suitable for oral administration and contains antioxidant complexes present in wine vinasses combined with one or more bioavailability promoters. A preferred embodiment of the invention consists in a dietary supplement provided as solid or liquid formulation allowing for avoidance of wine consumption while maintaining all of the beneficial components, in particular the antioxidant ones.
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CROSS REFERENCE TO RELATED APPLICATION
This application claims priority from U.S. Provisional patent application No. 60/091,720 filed Jul. 6, 1998 titled Arched Window Blind.
FIELD OF THE INVENTION
This invention relates to the field of window coverings, and in particular window coverings in the nature of retractable blinds adapted for use in arched window.
BACKGROUND OF THE INVENTION
A common architectural feature found particularly in residential homes is the vaulted ceiling. The vaulted ceiling is desirable in that it removes the claustrophobic nature of rooms such as formal sitting rooms and dining rooms which have a limited floor area as is commonly the case in many new housing developments where the amount of square footage of a dwelling is at a premium to the land developer. The sense of openness evoked by a vaulted ceiling is enhanced if tall windows are employed to take advantage of the higher than normal elevated walls, typically where a vaulted ceiling apex intersects a room wall. It is now well accepted that on such walls windows may be extended vertically by the use of correspondingly sized arched windows, that is, windows contained within generally semi-circular arched frames.
In the prior art, attempts have been made to provide retractable window blinds for use within such arched frames, none of which exhibiting the advantages of the present invention. A problem not properly addressed in the prior art is that in conventional arched windows, the centre of curvature of the window frame falls below the upper surface of the window sill. This occurs because, generally, the window frame is formed into a semi-circle, and the window sill having a discrete thickness is mounted between the opposite ends of the semi-circular arch thereby covering the center of curvature.
SUMMARY OF THE INVENTION
In summary, the blind for an arched window of the present invention is for installation into an arched window having a semi-circular window frame and a horizontal window sills wherein the window frame has a center of curvature lying at or below an upper surface of the window sill.
The blind includes a base mountable onto the upper surface of the window sill. A pivot is mounted onto the base so as to be positionable a first distance, vertically above the center of curvature of the window frame when the base is mounted onto the window sill. An arm is pivotably mounted to the pivot so as to be pivotable 180 degrees about the pivot in a vertical plane. The vertical plane intersects the base. An accordion member such as a pleated blind, or other folding cover extendible for example in a fan-like deployment, is mounted between the arm and the base. The accordion member is collapsible and extendible between a base edge of the accordion member and a leading edge of the accordion member by collapsing into a stowed position and unfolding into a deployed position respectively a folded adjacent array of elements extending between the base edge and the leading edge. The base edge is mountable to a first side of the upper surface of the window sill, where the first side of the upper surface of the window sill extends between the pivot and a first end of the window frame when the base is mounted to the window sill. The leading edge of the accordion member is slidably mounted to the arm so as to be slidable relative to the arm in a radial direction, radial relative to the pivot.
A guideway is mounted to the base. A guideway follower on the accordion member cooperates with the guideway so as to radially position, along an arcuate trajectory relative to the pivot and the arm, the leading edge and the folded adjacent array of elements as the arm is rotated about the pivot in the vertical plane. As the leading edge follows the arcuate trajectory, a radially outermost end of the leading edge is a maximum radial distance from the pivot when the leading edge is horizontal and is a minimum radial distance from the pivot when the leading edge is vertical. The maximum radial distance is greater than the minimum radial distance by a distance equal to the first distance. Thus, the blind may be opened and closed without binding of the blind at the apex of the window frame.
A support is mountable to the base for supporting the pleated blind while in the deployed position. The support may be a curved elongate member such as a flexible rod mountable at its ends to the base.
In one embodiment the guideway is an arcuate track mounted at ends of the track to the base and parallel to the vertical plane. The guideway follower is a rigid member mounted to the leading edge of the pleated blind and extending generally perpendicularly from the vertical plane so as to slidingly engage an end of the rigid member in the track. The track may also serve as the support.
Advantageously, the base is an elongate channel and the vertical plane intersects the channel along its length.
In one aspect of the present invention, the channel is a telescopic channel, adjustable so as to abut ends of the channel against the first end of the window frame and against an opposed facing second end of the window frame.
In a further aspect, the pivot is adjustably positionable vertically on the base.
Further advantageously, the leading edge includes a slat mounted to an adjacent end element in the array so as to be parallel and adjacent the arm.
In an alternative embodiment, the guideway is an arcuate bridgeway mounted over the pivot on the base. The bridgeway lies in the vertical plane. In this embodiment, the follower is a radially innermost end of the leading edge and a radially innermost edge of the array of elements. The bridgeway is positioned for sliding engagement of the radially innermost end of the leading edge and the radially innermost edge of the array of elements over an upper surface of the bridgeway as the arm is pivoted between the stowed position and the deployed position.
In a further description, the arcuately deployable blind for arched frame windows of the present invention may be described as including a base, a pivot mounted to the base and positionable over a center of curvature of a window frame of the arched frame window, and a slide arm, rotatably mounted at first end to the pivot. An arcuate guide secured to the base. An arcuately deployable pleated blind has first and second parallel longitudinal sides and first and second parallel transverse edges. The edges extend generally at right angles to, and contiguous with, the sides. A follower on the pleated blind is in sliding cooperation with the guide. The first edge of the blind is fastened to the base. The second edge of the blind is slidably fastened to the slide arm. An actuator is provided for deploying and retracting the blind.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is, in front elevation view, the arched window blind of the present invention, with blind deployed.
FIG. 2 is, in front elevation view, the arched window blind of FIG. 1 with blind retracted.
FIG. 3 is, in partially cut-away front elevation view, the operating arm and arm track of the arched window blind of FIG. 1 in sectional view along line 3--3 in FIG. 5.
FIG. 4 is, a cross-sectional view along 4--4 in FIG. 5.
FIG. 5 is, in partially cut-away plan view, the arched window blind of FIG. 1.
FIG. 6 is, in partially cut-away enlarged plan view, the operating arm and slide assembly of the arched window blind of FIG. 1.
FIG. 7 is, in side elevation view, the operating arm and slide assembly of FIG. 6.
FIG. 8a is, in side elevation partially cut-away view, the operating arm, slide and slide arm of the arched window blind of the present invention.
FIG. 8b is, in partially cut-away plan view, the blind slat of the arched window blind of the present invention.
FIG. 8c is, in partially cut-away side elevation view, the blind slat and retracted window blind of the arched window blind of the present invention.
FIG. 9 is, in partially cut-away plan view, the slidably adjustable window blind channel of the arched window blind of the present invention.
FIG. 10 is, in front elevation view, a pull chain and gear drive assembly for operating the deployment and retraction of the arched window blind of the present invention in a first embodiment.
FIG. 11 is, in partially cut-away front elevation view, a pull rod and lever arm drive assembly for deploying and retracting the arched window blind of the present invention in a second embodiment.
FIG. 12 is, in partially cut-away end elevation view, a rod and linkage for deploying and retracting the arched window blind of the present invention in a third embodiment.
FIG. 13 is, in plan view, the rod and linkage of FIG. 12.
FIG. 14 is, in front elevation view, a modified arched window blind of the present invention, with blind deployed.
FIG. 15 is, in front elevation view, the arched window blind of FIG. 1 with blind retracted.
FIG. 16 is in enlarged partially cut-away plan view, the arched window blind of FIG. 1.
FIG. 17 is a cross sectional view along 17--17 of FIG. 16.
FIG. 18 is a cross sectional view along 18--18 of FIG. 16.
FIG. 19 is in exploded side elevation, the components of the self adjusting feature of the arched window blind of FIG. 1.
FIG. 20 is in partially cut-away front elevation a motorized drive mechanism for deploying and retracting the arched window blind of FIG. 1.
FIG. 21 is in enlarged front elevation, the radial support bridge for the arched window blind of FIG. 1.
FIG. 22 is in plan view, the radial support bridge of FIG. 21.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The arched window blind of the present invention is illustrated in its deployed position in FIG. 1 and in its fully retracted position in FIG. 2. Arched window frame 10 extends in a semi-circle between vertical frame members 12a and 12b. Horizontally disposed window sill 14 extends between the opposite ends 10a and 10b of arched window frame 10, and is rigidly mounted thereto. Arched window frame 10 is an arcuate member, preferably semi-circular, having a center of curvature 16. In the instance where arched window frame 10 is exactly semi-circular, radius A has a constant length Radius A sweeps out the radial sector of the arch between opposite ends 10a and 10b of arched window frame 10.
Window blind channel member 18 better seen in FIGS. 3-5, is rigidly mounted onto the upper surface of window sill 14 so as to be juxtaposed therealong. Channel member 18 defines a longitudinal groove extending the longitudinal length of the channel. Pleated blind 20, which may be of stiff or otherwise reinforced fabric, or pleated plastic, cardboard or stiff paper or combinations of the above, or of other appropriate material known in the art in the manufacture of pleated blinds, is stored when in its retracted filly collapsed position within one end of channel member 18.
Pleated blind 20, when laid flat, is generally rectangular and defined by opposed first and second ends (the short sides of the rectangle), and first and second opposed longitudinal sides (the longer sides of the rectangle). Pleated blind 20 is pleated by means of pleat lines 20a extending in equally spaced parallel array along the length of pleated blind 20 parallel to the first and second ends of pleated blind 20 when the blind is laid flat.
Pleated blind 20 is collapsed in the normal fashion of pleated blinds so as to leave the opposed first and second ends 22a and 22b respectively available for mounting into channel member 18. In particular, first end 22a of blind 20 is securely mounted to the bottom interior surface 18a of channel member 18 and the opposite end, being second end 22b, of pleated blind 20 is securely mounted to blind slat 24. Advantageously, blind slat 24 extends the length of second end 22b of pleated blind 20. In one embodiment, as illustrated in FIG. 8, blind slat 24 may be slidably mounted to the underside of operating arm 26 and operating arm 26 rigidly mounted to slide arm 30. In another embodiment, as illustrated in FIGS. 5-7, operating arm 26 may be slidably mounted within slide 28 on slide arm 30. Thus, blind 24 may be either rigidly or slidably mounted to the underside of operating arm 26, so long as relative movement between pleated blind 20 and slide arm 30 is provided for. Slide arm 30 is pivotally mounted between opposed side walls of channel member 18 by means of pivot pin 32 journalled in, so as to extend between, lower blind supports 34a and 34b mounted in opposed facing relation to channel side walls 18b and 18c of channel member 18. The spaced apart relation between lower blind support 34a and lower blind support 34b is maintained by spacers 36.
Opposed facing lower blind supports 34a and 34b form a radial guide channel therebetween so as to guide slide arm 30 as it rotates about pivot pin 32 in direction B. Rotation of slide arm 30 in direction B deploys or retracts pleated blind 20 between its stowed position illustrated in FIGS. 2-5 and its deployed position illustrated in FIG. 1.
The arcuate path travelled by second end 22b of blind 20 as blind 20 is deployed from its stowed position, is dictated by the shape of track 38. Following arm 40 is rigidly mounted to operating arm 26 by means of following arm bracket 40a and roller 40b or other following means, better seen in FIGS. 6-7. Rotation of slide arm 30 in direction B about pivot pin 32 causes following arm 40 to follow the translation path defined by track 38. Track 38 is formed as a semi-circle having a radius C about center of curvature 16.
Because it is desirable to retrofit the arched window blind of the present invention into conventional arched windows, channel members 18 must, as described above, be mounted onto the upper surface of the existing window sill 14. Consequently, there exists a vertical offset distance D between pivot pin 32 and center of curvature 16. Depending on the thickness of pleated blind 20 when fully retracted into channel member 18 slide arm 30 may, as illustrated, have a dogs-leg offset or be otherwise curved to account for a further vertical displacement E between pivot pin 32 and blind slat 24.
Where window frame 10 is semi-circular, that is, radius A is a constant radius, track 38 is also semi-circular and radius C is also of constant radius. Where window frame 10 is arcuate so as to, for example, deviate from strictly semi-circular, that is, so that radius A is not constant, track 38 is correspondingly arcuate so that changes in the length of radius A are reflected in corresponding changes in the length of radius C as radii A and C sweep out a 180 degree sector about center of curvature 16, between opposite ends of channel member 18, in a vertical plane containing the longitudinal axis of channel member 18.
Thus as may be seen best in FIG. 3, as slide arm 30 is rotated about pivot pin 32 in direction B, the translation path of second end 22b of blind 20 relative to pivot pin 32 is governed by following arm 40 following in track 38. Because of the vertical offset D of pivot pin 30 relative to center of curvature 16, the length of radius F, that is, the radius extending from pivot pin 32 to the center of the path followed by following arm 40 in track 38 is nonconstant. In particular, the length of radius F when vertical is less than the length of radius F when generally horizontal. Thus the requirement that operating arm 26 is slidingly mounted to slide arm 30 or that blind slat 24 is slidably mounted to operating arm 26.
As better seen in FIG. 8, which is an exploded view of the slide arm, blind slat, and blind assembly, the sliding relative movement of blind 20 relative to slide arm 30 is accomplished by means of keys 42 which may be screws or bolts, mounted to operating arm 26 slidingly cooperating with corresponding keyways 44 in blind slat 24. Keyways 44 may be slots longitudinally aligned with elongate blind slat 24 so that keys 42 are free to slide along the longitudinal slots. Thus as following arm 40 sweeps out its arcuate translation path along track 38, radius F corresponding to the distance between pivot pin 32 and following arm 40 is free to vary to account for vertical displacement D as described above because of the relative sliding movement between operating arm 26 and blind slat 24.
In order to accommodate a smooth deployment of blind 20 in direction B, blind 20 may be adjusted once deployed so that the spacing between the radially distal edge of blind 20, that being second longitudinal side edge 46b opposed to first longitudinal side edge 46a of blind 20, and the radially innermost surface of window frame 10 is constant. Thus, adjusting screws 48a and their corresponding adjusting screw nuts 48b may be adjustably secured within a vertical adjustment track provided by adjusting slot 50 on side wall 18b of channel member 18. Thus with blind 20 trimmed to snugly fit between the inner surfaces of opposite ends 10a and 10b of window frame 10, the length of radius F at the vertex of window frame 10 may be adjusted so that blind 20, and in particular longitudinal side edge 46b, smoothly and snugly slides within frame 10 by adjusting track 38 vertically.
Where window sill 14 is longer than channel member 18, extension pieces or members 52 are adjustably securably mounted to the opposite ends of channel member 18 as for example by means of mounting screws 52a journalled in sliding engagement in adjusting slots 52b as better seen in FIG. 9.
As better seen in FIGS. 10-13, deployment of blind 20 in direction B may be accomplished by various means of rotating operating arm 26 about pin 32. For example, as seen in FIG. 10, a pull chain 54 may be employed to rotate a shaft mounted worm gear 56. Worm gear 56 rotates drive sprocket 58 which is rigidly mounted to a pivot arm such as slide arm 30.
Alternatively, as seen in FIG. 11, pull rod 60 is pivotally mounted to lever arm 62 so that vertically pulling or pushing on pull rod 60 rotates lever arm 62, thereby rotating pivot pin 32 to which lever arm 62 is rigidly mounted. Rotating pivot pin 32 rotates slide arm 30 (not shown) in direction B so as to deploy or retract blind 20.
Alternatively, as better seen in FIGS. 3-5 and 12-13, an offset cantilevered arm 64 is rotatably mounted to the upper surface of the radially distal end of operating arm 26 by means of bracket 66. The outwardly cantilevered end 64a of cantilevered arm 64, which is understood would be cantilevered outwardly of operating arm 26 away from window 68, is pivotally mounted to an upper end of push rod 70. As may be appreciated from FIG. 12, cantilevered 64 is offset so as to allow retraction of operating arm 26 beneath the upper edges of side wall 18b on channel 18 so that, when blind 20 is fully retracted, its operating mechanism may not be viewed from the interior of the room as may be appreciated in FIG. 2. Manual translation of the upper end of push rod 70 in direction B deploys or retracts blind 20.
Illustrated in FIGS. 14 through 22 is an alternative embodiment of the arched window blind of the present invention. Window blind channel 112, is mounted to the upper surface of window sill 114. Channel 112 supports inner and outer parallel blind guides 116. Guides 116 may be flexible rods bent into a semi-circular curve and mounted at their ends to the inner faces of opposed vertical sides of channel 112, for example by clips 118. Clips 118 may be attached to channel 112 by means of sheet metal screws 120, or the like. Guides 116 serve to maintain lateral stability, relative to the longitudinal axis of channel 112, of pleated blind 110 during its travel from a fully stowed position seen in FIG. 15 to a fully deployed position seen in FIG. 14, and also in the reverse direction. The guide 116 positioned closest to the window glazing, may be dispensed with where the window sill is narrow. In these cases the window will act as the guide.
Mounted centrally of blind channel 112 is an arcuately shaped bridge 124. Bridge 124 contains a window blind guideway 126, the radial center 128 of which is generally coincident with the center of the semi-circular window frame 130. Window blind guideway 126 acts as a guide for a first, inner end 132 of blind 110. A second, outer end 134 of blind 110 is positioned in proximity to the inner surface of semi-circular window frame 130. Blind 110 extends between its inner and outer ends.
Blind channel 112 is adjustable to suit various window frame widths and blind lengths. As the length of the window blind varies to accommodate different sizes, arcuately shaped bridge 124 may be raised or lowered relative to the bottom of channel 112 by means of adjustment holes 122 to ensure that the blind does not bind at the apex of its travel against the apex of window frame 130.
With reference to FIG. 19, a side 136 of pleated blind 110 is attached to channel 112. The opposing side 137 of blind 110 is attached to a slat 138. Slat 138 is made from heavier material than pleated blind 110, for example plastic or wood lath, and is of a width to nest freely within window blind guideway channel 126 of bridge 124. Slat 138 has slots 140 formed near each end of the slat. Slots 140 accept in sliding engagement therealong pins 142 mounted on operating arm 144 so as to slidably mount slat 138 on to operating arm 144.
Operating arm 144 is pivotally mounted to arcuately shaped bridge 124 at pivot point 146 which is located a distance D' from the radial center 128 of the semi-circular window frame 130. The radial distance R 1 from pivot point 146 to the base of window blind guideway 126 is not constant distance, falling with the range indicated by the arrows labeled "min." and "max.". Similarly, the radial distance along radius R 2 from pivot point 146 to the inner surface of semi-circular window frame 130 is also not constant, also having a minimum radius at the vertical and a maximum radius at the horizontal. The rate of change of radius R 1 and the rate of change of R 2 , in percentage of their length, is the same as the radii sweep out 180 degrees about pivot point 146.
When pleated blind 110 is in the fully stowed position, slat 138 is slidably forced to the most radially outward position on operating arm 144 due to engagement of blind first, inner end 132 and the base end 138a of slat 138 with the base surface of window blind guideway 126 of bridge 124. As operating arm 144 commences its rotation in direction B, second outer end 134 of pleated blind 110 rubs against the inner surface of the semi-circular window frame 130. The contact, for example along rub zone 148, between sill and blind forces slat 138, and with it pleated blind 110, radially inwardly, sliding along operating arm 144.
Once past rub zone 148, gravity assists so that first, inner end 132 of blind 110 follows in contact with the base of guideway 126. Thus the blind follows a trajectory defined by a plot of radius R about pivot point 146. When operating arm 144 is rotated over-center, contact between first, inner end 132 and slat 138 against the base of window blind guideway 126, for example along rub zone 149 forces blind 110 radially outwardly into close proximity with the inner surface of semi-circular window frame 130.
As may be seen in FIG. 20, a remote means for operation of blind 110 through an electric motor is shown. Motor 150, mounted to channel 112, rotates worm gear 152 which rotates operating arm 144 about pivot 146 through spur gear 154.
As will be apparent to those skilled in the art in the light of the foregoing disclosure, many alterations and modifications are possible in the practice of this invention without departing from the spirit or scope thereof. Accordingly, the scope of the invention is to be construed in accordance with the substance defined by the following claims.
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An arcuately deployable blind for arched frame windows includes a base, a pivot mounted to the base and positionable over a center of curvature of a window frame of the arched frame window, and a slide arm, rotatably mounted at first end to the pivot. An arcuate guide secured to the base. An arcuately deployable pleated blind has first and second parallel longitudinal sides and first and second parallel transverse edges. The edges extend generally at right angles to, and contiguous with the sides. A follower on the pleated blind is in sliding cooperation with the guide. The first edge of the blind is fastened to the base. The second edge of the blind is slidably fastened to the slide arm. An actuator deploys and retracts the blind.
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CROSS REFERENCE TO RELATED APPLICATION
This is a divisional patent application of U.S. patent application Ser. No. 11/852,359 filed Sep. 10, 2007, the disclosure of which is incorporated by reference in its entirety.
TECHNICAL FIELD
The exemplary embodiments of this invention relate generally to semiconductor devices and methods to fabricate them and, more specifically, exemplary embodiments of this invention relate to a class of devices known as metal high dielectric constant (high-k or MHK) transistors.
BACKGROUND
MHK transistors are experiencing extremely active development in the industry. One observed problem relates to the presence of an elevated outer fringe capacitance (Cof), on the order of 40-80 aF/μm. The elevated value of Cof is of concern, in that it at least impairs high frequency operation of the MHK transistor.
In U.S. Pat. No. 7,164,189 B2 Chien-Chao Huang et al. describe a method that includes providing a semiconductor substrate including a polysilicon or a metal gate structure including at least one overlying hardmask layer; forming spacers selected from the group consisting of oxide/nitride and oxide/nitride/oxide layers adjacent the polysilicon or metal gate structure; removing the at least one overlying hardmask layer to expose the polysilicon or metal gate structure; carrying out an ion implant process; carrying out at least one of a wet and dry etching process to reduce the width of the spacers; and, forming at least one dielectric layer over the polysilicon or metal gate structure and spacers in one of tensile and compressive stress.
In U.S. Pat. No. 6,448,613 B1 Bin Yu describes a field effect transistor that is fabricated to have a drain overlap and a source overlap to minimize series resistance between the gate and the drain and between the gate and the source of the field effect transistor. The parasitic Miller capacitance formed by the drain overlap and the source overlap is said to be reduced by forming a depletion region at the sidewalls of the gate structure of the field effect transistor. The depletion region is formed by counter-doping the sidewalls of the gate structure. The sidewalls of the gate structure at the drain side and the source side of the field effect transistor are doped with a type of dopant that is opposite to the type of dopant within the gate structure. Such dopant at the sidewalls of the gate structure forms a respective depletion region from the sidewall into approximately the edge of the drain overlap and source overlap that extends under the gate structure to reduce the parasitic Miller capacitance formed by the drain overlap and the source overlap.
At least one drawback of this latter approach is that it does not address the reduction of parasitic Miller capacitance when metal-like materials (such as TiN) are used.
SUMMARY
The foregoing and other problems are overcome, and other advantages are realized, in accordance with the exemplary embodiments of this invention.
In a first aspect thereof the exemplary embodiments of this invention provide a method to form a metal high dielectric constant (MHK) transistor, where the method includes providing a MHK stack disposed on a substrate, the MHK stack comprising a layer of high dielectric constant material and an overlying layer comprised of a metal, the MHK stack having an overlying layer comprised of silicon; selectively removing only the layer comprised of silicon and the layer comprised of metal, without removing the layer of high dielectric constant material, to form an upstanding portion of a MHK gate structure comprised of a portion of the layer comprised of silicon, an underlying portion of the layer comprised of metal, and an overlying portion of the layer comprised of silicon; forming a sidewall layer comprised of silicon on sidewalls of the upstanding portion of the MHK gate structure; removing that portion of the layer of high dielectric constant material than does not underlie the upstanding portion of the MHK gate structure; and forming an offset spacer layer over the sidewall layer and over exposed surfaces of a remaining portion of the layer of high dielectric constant material that underlies the upstanding portion of the MHK gate structure.
In a further aspect thereof the exemplary embodiments of this invention provide a MHK transistor that comprises a substrate; a MHK gate structure disposed on the substrate between a source region and a drain region, the MHK gate structure comprising a layer of high dielectric constant material and an overlying layer comprised of a metal, the MHK gate structure having an overlying layer comprised of silicon, where a lateral extent of the layer of high dielectric constant material is greater than a lateral extent of the overlying layer of metal; a sidewall layer comprised of silicon disposed on sidewalls of the MHK gate structure to cover the layer comprised of metal and the overlying layer comprised of silicon, said sidewall layer also being disposed over a top surface of the underlying layer of high dielectric constant material; and an offset spacer layer disposed over the layer comprised of silicon and over exposed portions of the layer of high dielectric constant material.
In another aspect thereof the exemplary embodiments of this invention provide a method to reduce parasitic capacitance in a metal high dielectric constant (MHK) transistor. The method includes forming a MHK gate stack upon a substrate, the MHK gate stack comprising a bottom layer comprised of high dielectric constant material, a middle layer comprised of metal, and a top layer comprised of one of amorphous silicon or polycrystalline silicon; forming a depleted sidewall layer on sidewalls of the MHK gate stack so as to overlie the middle layer and the top layer, and not the bottom layer, said depleted sidewall layer comprised of one of amorphous silicon or polycrystalline silicon; and forming an offset spacer layer over the depleted sidewall layer and over exposed surfaces of the bottom layer.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other aspects of the embodiments of this invention are made more evident in the following Detailed Description, when read in conjunction with the attached Drawing Figures, wherein:
FIGS. 1A through 1G are each an enlarged cross-sectional view of a semiconductor-based structure and depict metal gate process flow in accordance with the exemplary embodiments of this invention.
DETAILED DESCRIPTION
Although well-known to those skilled in the art, certain abbreviations that appear in the ensuing description and/or in the Figures are defined as follows:
BOX buried oxide CMOS complementary metal-oxide semiconductor CVD chemical vapor deposition FET field effect transistor HfO 2 hafnium oxide MLD multi-layer deposition PECVD plasma enhanced chemical vapor deposition PR photoresist RIE reactive ion etch RTA rapid thermal anneal SOI silicon on insulator STI shallow trench isolation TiN titanium nitride poly polycrystalline silicon Si silicon
The inventors have realized that, as compared to conventional poly-gated FETs, the origin of the increased Cof is due to a lack of sidewall depletion in the metal gate. This added capacitance adds to the Miller capacitance (Cmiller) and thus has a tangible performance impact. It can be determined that there can exist an approximately a 3.2% per 10 aF/μm of Cof increase (assuming that N-type FETS (NFETs) and P-type FETs (PFETs) track together in Cof).
The exemplary embodiments of this invention overcome this problem by providing a silicon sidewall spacer, in combination with a MHK gate, to reduce Cof and thus also reduce Cmiller.
The use of exemplary embodiments of this invention creates a structure with a thin-polysilicon or amorphous silicon sidewall that gates the FET extension region. Since the gate sidewall is made to be silicon, the sidewall depletion that occurs beneficially lowers the C of to similar levels as in poly-silicon gated FETs. Additionally, since primarily only the extension regions are gated with silicon (and therefore a relaxed EOT is present), the scaled EOT in the MHK transistor channel is maintained.
In general, the overall fabrication scheme described below may be standard until the gate stack etch. As in a normal process flow the metal etch stops on the hi-k material (such as on a layer of HfO 2 ). At this step, in accordance with the exemplary embodiments of this invention, deposition occurs of polysilicon (either CVD or PECVD) in the thickness range of about 10-20 nm. Then, using RIE, a thin poly-silicon sidewall gate is formed that is disposed largely over the device extension region. Then, processing may continue as in a conventional MHK process flow, such as by removing the hi-k material and growing MLD nitride and subsequent diffusion spacers.
FIGS. 1A through 1G are each an enlarged cross-sectional view of a semiconductor-based structure and depict metal gate process flow in accordance with the exemplary embodiments of this invention. In these Figures an NFET and a PFET are shown arranged in a side-by-side manner for convenience of description, and not as a limitation upon the practice of the exemplary embodiments of this invention.
FIG. 1A shows a Si substrate 10 having an overlying oxide layer 12 (e.g., 3 μm) and overlying Si and STI regions 14 A, 14 B. A conventional HfO 2 /TiN deposition may provide gate stack layers 16 and 18 , respectively. The HfO 2 layer 16 may be considered as the high-k layer (e.g., k in a range of about 20-25, as compared to 3.9 for SiO 2 ) and may have a thickness in a range of about 1-3 nm. The TiN layer 18 may be considered as the metal (or metal-like layer) and may have a thickness of about 10 nm. Layers 16 and 18 together form the (as yet unpatterned) MHK gate stack. This initial structure may represent a standard SOI (or without BOX bulk) CMOS with a MHK gate stack.
Note that the exemplary embodiments of this invention are not limited for use with HfO 2 as the high-k material, and other metal oxide-based materials may be used as well, such as a uniform or a composite layer comprised of one or more of Ta 2 O 5 , TiO 2 , Al 2 O 3 , Y 2 O 3 and La 2 O 5 . Materials other than TiN that may be used for the metal-containing layer 18 include, but need not be limited to, one or more of Ta, TaN, TaCN, TaSiN, TaSi, AIN, W and Mo.
FIG. 1B shows the deposition of an amorphous Si or a poly Si layer 20 , which may have a thickness in a range of about 30-100 nm, and subsequent deposition and patterning of PR to form PR regions 22 . Each PR region 22 is located where a device gate is desired to be formed.
FIG. 1C , depicted without the underlying Si substrate 10 and oxide layer 12 for simplicity, shows the result of a gate stack etch (which also removes the PR regions 22 ). In accordance with an aspect of this invention, the gate stack etch stops at the high-k layer 16 of HfO 2 .
FIG. 1D shows a blanket deposition by, for example, CVD or PECVD of a layer 24 of amorphous Si or polycrystalline (poly) Si. The Si layer 24 may have a thickness in a range of about 10-20 nm. FIG. 1D also shows, further in accordance with the exemplary embodiments, the selective etching of the Si layer 24 so that it remains as a thin layer only on the gate sidewalls, and has a thickness in a range of about 3-6 nm. Again, the etching stops on the high-k layer 16 . Over the metal portions (the TiN portions 18 ) of the underlying gate structure the Si sidewall layer 24 is depleted, which is a desired outcome.
FIG. 1E shows the etching and removal of the high-k HfO 2 layer 16 , except for that portion within each gate stack and underlying the TiN 18 . Note that as a result of the removal of the high-k HfO 2 layer 16 a lateral extent of the remaining portion of the layer 16 of high dielectric constant material is greater than a lateral extent of the overlying layer 18 of metal. The remaining portion of the high-k HfO 2 layer 16 may be seen to resemble a pedestal-like structure that supports both the overlying metal layer 18 , the amorphous or polycrystalline Si layer 20 , and the amorphous or polycrystalline depleted Si sidewall layer 24 .
As but one example a wet etch using a dilute hydrofluoric acid (DHF) solution may be used to remove the high-k HfO 2 layer 16 , as described in an article “Etching of zirconium oxide, hafnium oxide, and hafnium silicates in dilute hydrofluoric acid solutions”, Viral Lowalekar, Srini Raghavan, Materials Research Society, Vol. 19, #4, pgs. 1149-1156.
FIG. 1E also shows a result of depositing and etching a thin (e.g., about 3-6 nm) nitride or oxide offset spacer 26 that covers the Si layer 24 remaining on the gate sidewalls.
The remainder of the metal gate process flow may be conventional for CMOS processing, and can include providing oxide and/or nitride diffusion spacers and implants and final RTA.
For example, FIG. 1F shows a result of selectively masking alternatively the NFET and PFET so as to implant the other to provide extensions 28 and halos 30 , and FIG. 1G shows the result of the deposition and etching of a final spacer 32 (nitride or oxide deposited by PECVD), typically having a thickness of about 2-10 nm. FIG. 1G involves masking the PFET and implanting the NFET (using for example As or P), and masking the NFET and implanting the PFET (using for example B or BF 2 ). Subsequent annealing provides relatively deep diffusions for forming source and drain regions separated by the gate region. Subsequent processing may provide, in a conventional manner, silicide gates and diffusions (typically with Ni or Co) to complete the NFET and PFET transistors.
It may be appreciated that even if one were to experience an increase in extension resistance of about 6%, when applied to the NFET and the PFET this would translate into a resistance penalty on the order of about 1.4%, which is more than compensated for by the improvement in the Cmiller.
The exemplary embodiments of this invention can provide an undoped (intrinsic) Si gate sidewall 24 that doping in the main poly 20 may later diffuse into. The exemplary embodiments of this invention can also provide in-situ doped or implanted silicon (poly or amorphous) sidewalls 24 , and both for the NFET and the PFET.
It can be appreciated that the MHK device fabrication processes discussed above are compatible with CMOS semiconductor processing methodology.
Various modifications and adaptations may become apparent to those skilled in the relevant arts in view of the foregoing description, when read in conjunction with the accompanying drawings and the appended claims. As but some examples, the use of other similar or equivalent MHK material systems may be attempted by those skilled in the art. However, all such and similar modifications of the teachings of this invention will still fall within the scope of this invention.
For example, it should be noted again that the exemplary embodiments of this invention are not limited for use with MHK gate structures comprised only of HfO 2 and TiN. As non-limiting examples, a ZrO 2 or a HfSi x O y material may be used instead, as both exhibit a high dielectric constant (k of approximately 20-25) needed to provide a larger equivalent oxide thickness. In addition, the various layer thicknesses, material types, deposition techniques and the like that were discussed above are not be construed in a limiting sense upon the practice of this invention.
Furthermore, some of the features of the examples of this invention may be used to advantage without the corresponding use of other features. As such, the foregoing description should be considered as merely illustrative of the principles, teachings, examples and exemplary embodiments of this invention, and not in limitation thereof.
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A method is disclosed to reduce parasitic capacitance in a metal high dielectric constant (MHK) transistor. The method includes forming a MHK gate stack upon a substrate, the MHK gate stack having a bottom layer of high dielectric constant material, a middle layer of metal, and a top layer of one of amorphous silicon or polycrystalline silicon. The method further forms a depleted sidewall layer on sidewalls of the MHK gate stack so as to overlie the middle layer and the top layer, and not the bottom layer. The depleted sidewall layer is one of amorphous silicon or polycrystalline silicon. The method further forms an offset spacer layer over the depleted sidewall layer and over exposed surfaces of the bottom layer.
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BACKGROUND OF THE INVENTION
[0001] Images are typically recorded and stored as contone images in which each image element has a color tone value. For example, consider a digitally stored color image—each image element will typically have three corresponding values setting tone, among 256 gradations, for example, for each of the primary colors.
[0002] Many printing processes, however, cannot render an arbitrary color tone value at each addressable location or pixel. Flexographic, xerographic, inkjet, and offset printing processes are basically binary procedures in which color or no color is printed at each pixel. For example, at each addressable point on a piece of paper, a laser printer can generally either lay down a dot of black or colored toner or leave the spot blank, i.e., white. However, some newer devices have a limited ability to deposit intermediate quantities of colorant, such as toner or ink, or have multidensity colorants.
[0003] Digital halftoning involves conversion of the contone image to a binary, or halftone representation. Color tone values of the contone image elements become binary dot patterns that, when averaged, appear to the observer as the desired color tone value. The greater the coverage provided by the dot pattern, the darker the color tone value.
[0004] Further, in most print systems, it is necessary to also convert the input contone image, in some color space, to a colorant space of the target device. Many times images are stored such that the pixel level data are in terms of levels of red, green, and blue (RGB). This is most convenient when rendering on common display devices. In contrast, standard printing systems are usually based on a four color pallet of cyan, magenta, yellow, and black (CMYK). The conversion is typically performed using a look-up table (LUT) that maps pixel data comprising red, green and blue levels to pixel data comprising cyan, magenta, yellow, and black levels. These look-up tables are defined by first printing combinations of cyan, magenta, yellow, and black colorants, measuring the resulting colors, and inverting the resulting color table.
[0005] To increase image smoothness and color accuracy, it is increasingly common in ink jet printing, for example, to supply more than the standard four colorants (CMYK). In particular, it is common to provide light versions of the cyan and magenta colorants. There light versions can be made with dilute solutions of the colorants. The darker colorants are needed to make fully saturated colors without overloading the paper. However, these heavy inks can make very visible dots on the page, which are especially noticeable in the lighter tones. Therefore, if the lighter inks can be used in the lighter tonal range, the halftone pattern will be less visible. In other examples, additional colorants such as orange and green are added to the device's pallet to improve color rendition.
[0006] Increasing the number of colorants results in a more complex conversion to the target device color space. The most straightforward generalization would be to use a 3-to-6 color conversion LUT. However, creating such a table becomes very difficult since it must be created by choosing an inverse from a 6-to-3 table of measurements. This table is very large, and there are many degrees of freedom.
[0007] One limitation that constrains the available degrees of freedom in practice concerns the fact that certain ink/media properties or hardware restrictions may require a printing process to limit the allowable maximum total amount of combined colorant, called the total-ink, to a value less than the sum of the maxima of each colorant. Therefore, some mechanism is required to modify the rendering process to enforce these constraints.
[0008] A practical example of the application of a total ink reduction is ink-jet printing where on some substrates and when using certain inks, the ink will not stick to the media anymore and cause bleeding of ink when too much ink is used. Another example is in the context of laser jet printing. Although a laser jet can print the maximum amount of ink without visual problems on the print-out, the age of the drum is drastically reduced and may even cause damage when using too much ink for an extended period over large areas. So many laser jet engine manufacturers require the total ink to stay below a certain tolerance level (typically 270%).
[0009] Techniques exist for addressing this problem. Some of the most common techniques for controlling total ink (also called total area coverage) are UCR/GCR (under cover removal and grey component replacement). These techniques are applied in many graphic arts related products, such as postscript raster-image processors. They address the way the amount of black colorant is calculated. By calculating first the equivalent neutral density of the desired color, then reducing the amounts cyan, magenta, and yellow colorants appropriately and replacing this neutral component by an equivalent amount of black colorant, in principle the same color is obtained but with a lower total amount of colorant, since the black colorant replaces three colorants.
[0010] Other techniques operate by imposing hard limits on the total ink that is applied to a given area. In one such example, after the half-toning of the image data, the half-tone data are analyzed to determine whether the total ink density is higher than a predetermined limit value within a given pixel matrix area. When the limit is exceeded, the ink density is reduced by determining a reduction coefficient that is applied to the quantity of ink applied for each of the chromatic colors. This yields corrected color quantities that are actually applied to the paper.
SUMMARY OF THE INVENTION
[0011] It is preferable that in a color characterization of this printing process that the total-ink limit is handled upfront and is therefore already enforced when characterization test charts are printed. However if the total-ink restriction method reduces the total number of different colors one can make with the printing process, the overall quality of color rendering will decrease and the color characterization process often becomes unstable.
[0012] According to the invention, the total-ink method ensures that the total amount of available colors remains the same and that therefore the color characterization process can treat the restricted printing process as if it is dealing with a non-restricted printing process without loss of quality. This method enhances non-lossless, black replacement methods traditionally used for total-ink restriction.
[0013] In more detail, first a total-ink amount is given, selected or automatically determined. Secondly a non-empty subset of the available colorants is chosen as target colorants. Using these two parameters a preferably smooth and bijective function, “Ψ”, is defined from the non-restricted colorant space to the restricted colorant space defined as the space of colorants where the sum of colorant amount is less than or equal to the specified total-ink amount. The bijective function will only modify the amounts of target colorants, leaving non-target colorants unaltered by the function Ψ. The preferred way of using the method is by embedding it in the printer driver. In this case the method would be part of the printer driver workflow.
[0014] One choice is to embed the function Ψ in the printing workflow, by applying Ψ to any incoming color before this color is actually rendered by the printing process. Another possibility is to make the function Ψ part of the color management workflow where it used to restrict a color when converting to the device color space and the inverse of Ψ is used to convert a device color of the printing process to another color space.
[0015] In general according to one aspect, the invention features a system for rendering an image on a target device from a contone image. The system comprises a color space converter that generates target device contone image data from input contone image data. In one example, the input contone image date is in a red, green, blue color space that is converted to a cyan, magenta, yellow, black color space of the printing device.
[0016] A halftoning stage is provided for converting the target device contone image data into target device halftone image data such that a print engine can apply colorant to media in response to the halftone image data.
[0017] According to the invention, a total ink compensating stage is further provided that modifies the target device contone image data received by the halftoning stage, for example, by limiting colorant applied to the media based on a total ink constraint. This avoids problems related to overloading the print media with ink or toner, for example. This colorant limitation, however, is achieved by providing a one-to-one mapping between each possible input contone image data value and each possible compensated target device contone image data value. In this way, the invention avoids the problem of two input contone image data values being printed on the media with the same compensated target device contone image data value, thereby defining a lossless process.
[0018] In one embodiment, the print engine is an ink jet printer, but the invention also applicable to laser printers.
[0019] In the current embodiment, the total ink compensating stage provides the one-to-one mapping between each possible input contone image data value and each possible compensated target device contone image data value using a bijective function to thereby enforce the one-to-one mapping.
[0020] In still other embodiments, the total ink constraint is applied to only a subset of colorants used by the print engine, and the total ink compensating stage is embedded in a print driver.
[0021] In general according to another aspect, the invention features a method for rendering an image at a target device from a contone image. The method comprises receiving input contone image data and converting the input contone image data to target device contone image data. According to the invention, compensated target device contone image data is generated in which colorants applied to the media are limited based on a total ink constraint by providing a one-to-one mapping between each possible input contone image data value and each possible compensated target device contone image data value.
[0022] The compensated target device contone image data is then converted into target device halftone image data and colorants applied to media in response to the halftone image data.
[0023] In general according to another aspect, the invention features a method for rendering an image at a target device from a contone image for color data in general, outside of a printer workflow. This method can be applied inside, for example, a color correction software module. Further, because of the loss-less nature of the inventive process, an inverse can also be applied for soft-proofing, for example.
[0024] The above and other features of the invention including various novel details of construction and combinations of parts, and other advantages, 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 method and device embodying the invention are shown by way of illustration and not as a limitation of the invention. The principles and features of this invention may be employed in various and numerous embodiments without departing from the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In the accompanying drawings, reference characters refer to the same parts throughout the different views. The drawings are not necessarily to scale; emphasis has instead been placed upon illustrating the principles of the invention. Of the drawings:
[0026] FIG. 1 is a block diagram showing a system for rendering an image on media from a contone image data, according to the present invention; and
[0027] FIG. 2 is a flow diagram showing the process for applying total ink constraints according to the present invention;
[0028] FIG. 3 is a flow diagram showing another process for applying total ink constraints according to the present invention; and
[0029] FIG. 4 is a flow diagram showing a process removing total ink constraints according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0030] FIG. 1 shows a rendering system, which has been constructed according to the principles of the present invention.
[0031] Specifically, it comprises a print driver 100 . Typically, this is implemented in software on a computer. However, in other examples, it is implemented in print device firmware or hardware.
[0032] Contone image data are received by the print driver 100 . The image data are usually in the red, green, blue (RGB) color space. However, in other implementations, the image data may be already in the CMYK color space.
[0033] The print driver 100 has a color space converter 110 , if required. The color space converter 110 generates target device contone image data from input contone image data, in which case the printer driver will use some method to convert the image data into CMYK (for example).
[0034] In one implementation, the color space converter 110 is similar to conventional converters. Specifically, it receives red, green, and blue contone image data. The converter 110 includes a look-up table that maps red, green, and blue levels to cyan, magenta, yellow, and black levels. As a result, the target device contone image data are produced in the color space, CMYK, of the target printing device.
[0035] Next, a total ink compensator 114 operates on the CMYK data 112 to generate compensated C′M′Y′K′ 116 that conforms to the total ink restrictions of the printing device. On the CMYK data, the total ink reduction method is used to limit the total ink to some value. Preferably the method is setup to leave the black information unchanged, and only limit the ink by changing the CMY values. This new data is denoted as C′M′Y′K′.
[0036] The changed data C′M′Y′K′ 116 is further processed using half toning techniques to convert it into dot on/dot off data for each colorant that is required by the print engine itself.
[0037] Specifically, the compensated color channels C′M′Y′K′ 116 are received at a halftoning stage 118 . This halftoning stage 118 converts the target device contone image data into target device halftone image data.
[0038] In some examples, the cyan channel, 112 -C and the magenta channel, 112 -M, are received by separate multi-level halftoners. These multi-level halftoners convert the target device contone image data for the corresponding color channel to multi-level halftone image data.
[0039] The halftone image data produced by the halftone stages 118 , for each of C′, M′, Y′, K′ channels are directly processed by the print engine controller 122 . Specifically, the print engine controller 122 converts the target device halftone image data 120 directly into commands to the print engine 124 . In the present embodiment, the print engine 124 is an ink jet print head that sprays ink droplets onto media 10 , such as paper. However, in other embodiments the print engine is a laser printer.
[0040] Referring to FIG. 2 , using the printer driver workflow as given above, the following sets forth the RGB to CMYK to C′M′Y′K′ conversion method used by converter 110 and the total ink compensator 114 of the printer driver 100 .
[0041] To setup the color space converter 110 , a “color characterization” process is used. Color characterization aims to determine the color characteristics of a device and to define a separation method that converts any or specific color data, usually RGB, into matching colors on the device, usually CMYK.
[0042] First, using the printer driver, a test target is printed, including a sub-sampling of patches of the CMYK colorant space, in step 210 .
[0043] Then, in step 212 , the printed target is measured using a color measurement device. Specifically, spectral reflectance or color matching values associated with the various colorant combinations are measured. A measurement of each patch will, thus, provide a value for that patch in a well-defined device independent color space.
[0044] In step 214 , using the measurements, a full description is deduced that gives a device independent color value for every possible CMYK combination. This is accomplished by derivation and by approximation or modeling techniques.
[0045] Based on the full description, a separation method is derived, in step 216 that relates device independent color values to corresponding device dependent CMYK value.
[0046] Then in step 218 , the CMYK values are analyzed for compliance with the total-ink constraint. Specifically, the total ink applied for each of target colorants is summed for each of the determined device dependent CMYK values. In one implementation, the analysis is performed before the color is actually rendered by the printing process. Another possibility is to perform the step as part of the color management workflow where it used to restrict a color when converting to the device color space and the inverse is used to convert a device color of the printing process to another color space.
[0047] Finally, in step 220 , the total-ink values for each of the CMYK values are reduced such that to comply with the total ink constraint by the total ink compensation stage 114 .
[0048] In the present embodiment, a bijective function for total ink reduction on n colorants is used. A bijective function is a mathematical function that is both injective, i.e., one-to-one, and subjective, i.e., onto, such that the function creates a one-to-one correspondence between possible input values and possible output values.
[0049] The function is defined as follows:
[0050] Given the total ink function for n colorants
σ ( x -> ) = ∑ i = 1 n x i
[0051] Given the maximum ink function
μ({right arrow over ( x )})=max { x i ;1≦ i≦n}
[0052] Given the total ink T and maximum ink per colorant M, then an example of a bijective total ink mapping function γ is
γ ( x -> ) = x -> iff σ ( x -> ) M ≤ T μ ( x -> ) = x -> ( μ ( x -> ) T M σ ( x -> ) ) iff σ ( x -> ) M > T μ ( x -> )
[0053] The advantage of our total-ink reduction method is that two different CMYK input values will always print as two different colors, although it may happen that they do become close when measured due to the printer physics.
[0054] This example of bijective function is not a smooth function however since the transition from the region where the function is acts to reduce ink and where it does not shows a non-continuous derivative. It is however possible, based on the given example, to define a more smooth bijective function.
[0055] To explain the motive to define a bijective function total-ink function, suppose now that the total-ink function would not be bijective, and so that two colors CMYK 1 and CMYK 2 exist that would print exactly in the same identical way. In that case measuring these two values would naturally give the identical same device independent color value, say XYZ. That is, measuring CMYK 1 and CMYK 2 both give XYZ as value. For the separation problem, which reversely has to choose a CMYK combination for the given XYZ value, this constitutes a dilemma since both CMYK 1 and CMYK 2 are equally valid candidates.
[0056] In addition to smoothness a second immediate extension of the example function is to limit its range of action to a subset of the available colorants. Suppose the target subset of colorants is the first m of the n-colorants. Then we can replace the bijective function above by first the defining a bijective function that does not change the last (n-m) colorants, and by replacing n by m and T by T−Σ i=m+1 n x i in the definition of the total-ink function.
[0057] In another extension of the total-ink function we can assign weights to the different colorants. In this case an example of a bijective total-ink function could be:
[0058] Given n-weights w1, . . . , wn, which satisfy:
0 <w i ≦1{circumflex over ( )}Σ i=1 n w i =1
[0059] Given the adjusted total ink function
σ′( {right arrow over (x)} )=Σ i=1 n w i=1 w i x i
[0060] Given the adjusted maximum ink function
μ′( {right arrow over (x)} )=max { w i x i ;1≦ i≦n}
[0061] Given the total ink T and maximum ink per colorant M, then an example of a bijective weighted total ink mapping function γ′ is
γ ′ ( x -> ) = x -> iff σ ′ ( x -> ) M ′ ≤ T μ ′ ( x -> ) = x -> ( μ ′ ( x -> ) T M ′ σ ′ ( x -> ) ) iff σ ′ ( x -> ) M ′ > T μ ′ ( x -> )
where M′ is given by
M′ =max { w i M ;1≦ i≦n}
[0063] In still other embodiments, the invention is used possibly outside of a printer workflow. This method can be thus applied inside, for example, a color correction software module.
[0064] In the case of color correction software there are two workflows that are described.
[0065] In a first example, shown in FIG. 3 , color correction software starts with or operates on color image data in step 310 . That data can be in the form of a contone image or color patch values. Generally, this initial data is not in the color space in which we intend to apply the total ink method, such as for example the printer CMYK color space.
[0066] Next, in step 312 , color correction software converts the color data from the initial color space to the color space in which compensation is to occur.
[0067] Then, the color correction software applies the total ink limitation method to restrict the total ink to a specific value in step 314 . Specifically, the total ink compensation modifies the image data, in the compensation color space, to limit colorants applied to the media based on a total ink constraint while providing a one-to-one mapping between each possible input image data value and each possible compensated image data value to thereby produce compensated image data. This compensated image data is then typically passed to a print device in which the image is rendered.
[0068] A second example, shown in FIG. 4 , is used when the color correction software needs to convert color data already in the target color space and to a second color space. This situation arises, for example in soft-proofing, where it is the goal to show on the screen how the print will look. Thus, the second color space would typically be a computer monitor RGB color space.
[0069] Here, the compensated color data is received in step 410 . These are data on which the total ink constraints have been previously applied. Further, the color space is typically the color space of the printer.
[0070] The color correction software then applies the inverse of the total ink method in step 412 . This inverse exists because of the way the total ink method is defined. Specifically, since there is a one-to-one, loss-less, mapping between each possible input image data value and each possible compensated image data value, applying the inverse returns the original data without loss of information.
[0071] Lastly, the color correction software converts from the printer color space to the other color space, such as the monitor color space in step 414 .
[0072] In this way, the inventive method is used to limit for example the total ink usage in the printing of the image already in the target color space. However, the effect of the total ink method is also undone, to enable monitoring of the rendition process on devices that do not require application of a total ink constraint.
[0073] While this invention has been particularly shown and described with references to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.
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A total-ink method ensures that the total amount of available colors remains the same such that the color characterization process can treat the restricted printing process as if it is dealing with a non-restricted printing process without loss of quality. This method enhances non-lossless, black generation methods traditionally used for total-ink restriction by generating compensated target device contone image data in which colorant applied to the media is limited based on a total ink constraint by providing a one-to-one mapping between each possible input contone image data value and each possible compensated target device contone image data value, using a bijective function, for example.
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This is a Continuation of application Ser. No. 07/211,135, filed on June 22, 1988, by Tooru Shibayama et al. entitled "PRINTING DEVICE FOR CONTINUOUS STRIP OF TAGS", now abandoned which is a continuation of application Ser. No. 06/524,128, filed on Aug. 16, 1983, by Tooru Shibayama et al. entitled "PRINTING DEVICE FOR CONTINUOUS STRIP OF TAGS", now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a printing device for printing a continuous strip of tags. More specifically, the present invention relates to a printing device for printing on a continuous strip including a plurality of tags fed to the printing device, which is capable of allowing free and easy selection of line spacing as needed.
2. Description of the Prior Art
Known printing devices of this type include drum impact, thermal and electrostatic printers. In the known devices, the line spacing is fixed. This represents a major drawback since the required line spacing is often different for each user.
In the prior art devices, the manufacturer of the apparatus presets the line spacing for each individual user. This has prevented standardization of printing devices. Furthermore, even an individual user may want to change the line spacing depending upon the size or design of the tags and the number of printing lines which, in turn, change in accordance with the selected type of tags used or the required printing contents.
BRIEF SUMMARY OF THE INVENTION
The present invention has been made in consideration of this and has for its object to provide a printing device for a continuous strip of tags which allows free selection of line spacing as needed.
It is another object of the present invention to provide a printing device for a continuous strip of tags which makes it easy to change the line spacing.
It is still another object of the present invention to provide a printing device for a continuous strip of tags which is simple in construction, is easy to operate, and can withstand use over a long period of time.
According to the present invention, line spacing data which may be freely set is stored in a memory along with character data representing the information to be printed. The line spacing is determined in accordance with the desired line spacing data.
There is provided according to the present invention a printing device for a continuous strip of tags, having a feed mechanism for feeding the continuous strip of tags, a printing mechanism for printing one or more lines on each tag of the continuous strip of tags, and a data memory circuit for storing input printing data, characterized in that the printing data stored in the data memory circuit includes both character data indicative of the desired information to be printed and line spacing data indicative of the desired spacing between successive lines of the information to be printed.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other objects of the present invention will become more apparent from the following description of preferred embodiments taken in connection with the accompanying drawings, in which:
FIG. 1 is a view showing an example of a continuous strip of tags;
FIG. 2 is a schematic view showing the overall structure of a printing device according to the present invention;
FIG. 3 is a block diagram of a control circuit of the device shown in FIG. 2;
FIG. 4 shows the preferred format of the printing data;
FIG. 5 is a flow chart of a computer program stored in the program memory circuit of FIG. 3 and used to print data on the tag of FIG. 1;
FIG. 6 is a view showing a continuous strip of another type of tag;
FIG. 7 is a view showing a main portion of the control circuit shown in FIG. 3; and
FIG. 8 is a flow chart of a computer program stored in the program memory circuit of FIG. 3 and used to print data on the tag of FIG. 6.
FIG. 9 is an enlarged view of the first data line of the tag of FIG. 1.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The preferred embodiments of the present invention will now be described with reference to the accompanying drawings.
Examples of tags which are provided in a continuous strip are price tags, tickets, labels, etc. In the embodiments disclosed, the tags as shown in FIG. 1 or 6 are used. It should be recognized, however, that other tags can be used with the present invention.
FIG. 1 shows a longitudinally continuous strip 1 of a plurality of tags 2. An aperture 3 is formed between each pair of adjacent tags 2. After printing, the strip 1 is cut at the positions of the apertures 3 so as to provide individual tags 2. A perforation 4 is formed widthwise along the center of each tag 2 so as to separate it into a user's portion 2a and a data processing portion 2b.
In the example shown in FIG. 1, the information to be printed includes seven lines of data. The first line of data specifies the name of the store, the second line of data specifies the age group which the merchandise is directed towards, the third line of data specifies the price of the goods, the fourth and fifth lines provide code information which may be representative of the department in which the goods are sold, the sixth line contains further code information which may identify the goods in question, and the seventh line also contains price information. Each line of data (hereinafter "data line") is spaced from the preceding data line (or from the beginning of the tag 2 in the case of the first data line) by a respective line spacing SP 1 , SP 2 , etc.
In the presently preferred embodiment, each of the characters printed are printed in the form of a dot matrix. FIG. 9 illustrates the manner in which the first line of data (SATO STORE) can be printed in dot matrix form. By way of example, the individual characters are illustrated in the form of a 5 (column) by 10 (row) matrix. In this manner, each character can be stored digitally in the form of a 5×10 matrix, each dot position being stored digitally as a binary "1" (representing the location of a dot at a given dot position 40) or a binary "0" (representing the absence of a dot at a given dot position 40). In the example illustrated in FIG. 9, the letter "S" is stored digitally:
11111
10000
10000
10000
11111
00001
00001
00001
00001
11111
As shown in FIG. 2, the strip 1 is wound around a tag supply drum 10. The strip 1 supplied from the tag supply drum 10 is fed by a pulse motor 12 and a feed mechanism 11 having a pair of feed rollers 13 and 14 driven by the pulse motor 12. A printing mechanism 15 prints the desired information on each tag 2 of the strip 1. In the preferred embodiment, the printing mechanism 15 is a thermal printer including a thermal transfer printing ribbon 16 (which is intermittently fed in the direction shown) and a thermal printing head 17 having a number of heaters 17a arranged along the direction of width of the strip 1 (into the plane of FIG. 2). The thermal printing head 17 prints the character information in the form of the dot matrix such as that described above. The strip 1 is intermittently stepped past the print head 17. Each time it is stopped, selected heaters 17a are enabled and brought into contact with the ribbon 16 so as to print selected dots of either a given dot line or of a given dot column. When printing a tag of the type illustrated in FIG. 1, appropriate heaters 17a print dots corresponding to a single dot line of each of the characters in a given data line (e.g., the top dot line of each of the characters in SATO STORE). When printing onto the tag of FIG. 6, appropriate heaters 17a print the dots of a single dot column of all the characters in the same column of tag 2 (e.g., S, F, P, P, V, Y in FIG. 6). By enabling selected heaters 17a for either each dot line (FIG. 1) or for each dot column (FIG. 6), and by stepping the tags through all of the dot lines of all of the data lines or all of the dot columns of all of the data columns, it is possible to print all of the character data on the tag. The manner in which this is carried out is described in greater detail below.
A photosensor 18 detects each aperture 3 of the strip 1. The feed mechanism 11 and the printing mechanism 15 operate in accordance with detection signals generated by the photosensor 18. The strip 1 is cut at the position of each aperture 3 between adjacent printed tags 2 by a cutting mechanism 19 having a stationary blade 20 and a rotary blade 21.
A drive circuit for driving the printing device as described above will now be described with reference to FIG. 3.
A CPU 30 for controlling the overall circuit is connected to a program memory circuit 32 and a data memory circuit 33 through a bus line 31. The bus line 31 is also connected to the photosensor 18, a pulse motor drive circuit 34, a printing control circuit 35 and a data input device 36. The data input device 36 is for input of the printing data and may comprise, for example, a keyboard, an external computer or the like.
The printing data is input through the data input device 36 and is stored in the data memory circuit 33. The printing data preferably has a format as shown in FIG. 4. In accordance with this format, the printing data consists of a start signal followed by character data CD, line spacing data SD, and tag number data ND. An end signal following the tag number data ND indicates the end of the printing data.
The character data CD represents the information to be printed on each tag 2 (e.g., the seven data lines of FIG. 1). The tag number data ND represents the number of tags on which the same information is to be printed. The line spacing data SD represents the number of steps of the pulse motor 12 which corresponds to the distance of each respective line spacing SP 1 , SP 2 , etc. In the presently preferred embodiment, the line spacing data SD includes ten line spacing values SL(1), SL(2) . . . SL(10) which correspond to ten respective line spacings SP 1 , SP 2 . . . SP 10 . Thus, if each step of the pulse motor 12 corresponds to 10 mils and the first line spacing SP 1 is 80 mils, the line spacing value SL(1) will correspond to eight.
The values SL(1), SL(2) . . . SL(10) may be freely preset and may be set to "0" for an unnecessary line. In the embodiment being considered, seven lines are printed as shown in FIG. 1. Therefore, the values SL(1) to SL(7) are suitably set to correspond to the line spacings SP 1 to SP 7 . The line spacing values SL(8) to SL(10) are set to "0".
The printing operation for each tag 2 of the strip 1 in accordance with the printing data stored in the data memory circuit 33 will now be described with reference to the flow chart shown in FIG. 5.
The program first proceeds to instruction block 50, wherein the printing data, shown by way of example in FIG. 4, is input through the data input device 36 and is stored at a predetermined memory area of the data memory circuit 33.
When the inputting of the printing data is completed, the program proceeds to instruction block 51 and the strip 1 is fed such that the position of the first dot line of the first data line to be printed is aligned with the heaters 17a of the thermal printing head 17. This is accomplished as follows.
The spacing of the apertures 3 is such that when a first aperture 3 is at the position corresponding to the heaters 17a, a second (e.g., the next) aperture 3 is at the photosensor 18. In response to a detection signal from the photosensor 18 (generated whenever it detects an aperture 3), the pulse motor 12 rotates for the number of steps corresponding to line spacing value SL(1). As a result, the strip 1 is fed for a distance corresponding to the line spacing SP 1 with reference to the position of the aperture 3. This causes the location of the first dot line of the first data line to be printed to align with the lined heaters 17a of the thermal printer 17.
At this point, the program proceeds to instruction block 52 wherein the line variable L is set equal to one, indicating that the first data line is being printed. Proceeding to instruction block 53, the program causes the first data line to be printed. When printing the tag of FIG. 1, each data line is printed by printing successive dot rows of each character in the data line. Referring to FIG. 9, the first dot line of each of the characters "S, A, T, O, S, T, O, R, E" will be printed followed by the second dot line of each character, etc. The manner in which this is carried out can best be understood with reference to FIG. 7 which is a block diagram of the printing control circuit 35.
As shown in FIG. 7, the printing control circuit 35 includes a counter 46, a character generator 47 and first and second shift registers 48, 49. Character generator 47 stores all of the characters in dot matrix form. One commercially available device which can be used for this purpose is a bit character generator sold by NEC Corp. under the product designation μPD 481 D-001. This product is essentially a read only memory which stores 128 characters in dot matrix form (an eight column by 16 row matrix). Individual rows of a given character may be read out of the character generator (in parallel) by applying a first address identifying a particular character to be generated and a second address identifying the specific dot row of that character to the character generator 47. In this manner, the CPU 30 can cause the character generator 47 to place any dot line of any one of the 128 characters on the bus 31 when desired. Presuming that the first dot line of the first line of data of the tag of FIG. 1 is to be printed, the CPU 30 will cause the character generator 47 to place the first dot line of the character "S" onto the data bus 31. The parallel bits of this dot row are first shifted into the first shift register 48. To this end, the CPU 30 places a count in counter 46 corresponding to the number of bits in a single dot row (eight bits in the example being considered). CPU 30 then generates clock pulses which are applied both to the counter 46 and to shift registers 48 and 49. These clock pulses decrement the count in counter 46 and cause the bits in shift register 48 to be transferred into shift register 49. This process continues until the count in counter 46 is 0 at which time all of the bits of the dot row of the character in question are shifted into shift register 49.
Once these bits have been shifted into shift register 49, a number of binary 0's corresponding to the spacing between adjacent characters (this will generally be a preset number) are then shifted into shift register 49. This is done by setting the count in counter 46 equal to a number corresponding to the spacing between adjacent characters and then applying clock signals to both the counter 46 and the shift registers 48 and 49. Each clock signal reduces the count in counter 46 by 1 and causes another bit to be transferred from shift register 48 to shift register 49. Since shift register 48 will be blank at this time, binary 0's will be shifted into shift register 49. Once the count in counter 46 is 0, the number of binary 0's corresponding to the spacing between adjacent characters will have been placed in counter 49.
At this point, the CPU 30 causes the character generator 47 to place the bit information corresponding to the first dot line of the "A" onto bus 31 and the entire process is repeated until the first dot line of each of the characters "SATO STORE" is read into shift register 49 so as to enable appropriate heaters 17a of printing head 17. At this point, the printing head 17 will be lowered into contact with the printing ribbon 16 to cause the first dot line of the first data line to be printed onto the tag 2.
After the first dot line has been printed, the print head 17 will be returned to its raised position and the CPU 13 will cause the pulse motor 12 to step a predetermined number of steps corresponding to the spacing between adjacent dot lines. The CPU will then cause the printing control circuit 35 to enable those heaters 17a corresponding to the dots of the second dot line to be printed and the process will be repeated until all of the dot lines of the first data line have been printed.
When printing of the first data line is completed, the program proceeds to decision block 54 and determines if the line variable L is equal to 10 (the maximum number of lines which can be printed on a tag in the embodiment illustrated). If not, the program proceeds to decision block 55 wherein it determines if the variable SL(L) is equal to zero. In the illustrated example, the first seven times through the loop encompassing blocks 53-57, the line spacing value will be other than zero, and the program will pass to instruction block 56. In the eighth pass through the loop, the line spacing value SL(8) will be equal to zero and the program will proceed to instruction block 58. As a result, whenever the printing mechanism has printed either the maximum number of lines (10 in the example being considered) or all the data lines of the character data CD (7 in the example being considered), it will exit the loop encompassing blocks 53-57 and will proceed to block 58. As will be described in detail below, this will cause the program to repeat the loop encompassing blocks 53-57 for each successive character data CD until all of the character data stored in data memory circuit 33 to be printed on each tag has been printed.
Returning to block 56, the variable L is increased by one. The first time through the loop, L will be increased to two. Proceeding to instruction block 57, CPU 30 causes the motor 12 to be incremented by a number of steps determined by the line spacing data SL(2) which has the effect of bringing the heaters 17a of the printing head 17 into alignment with the first dot line of the second data line. The appropriate heaters 17a are then enabled and the printing head 17 is brought into contact with the ribbon 16 so as to print the second dot line. This process is repeated until all seven data lines have been printed at which time the program proceeds to instruction block 58.
In instruction block 58, the tag number variable ND is decremented by one. The tag number variable ND corresponds to the tag number data for the character data being printed. Proceeding to decision block 59, CPU 30 determines if the variable ND is equal to zero. If not, there are additional tags to be printed and the program returns to instruction block 51. The program will continue proceeding through this loop until all of the tags corresponding to the data CD have been printed at which time the tag number index ND will be equal to zero. At this point, the program proceeds to decision block 60 wherein it determines if there is any further printing data (another set of data ND, SD, CD) to be printed. If so, it returns to instruction block 50 and the entire process is repeated. When all the data stored in data memory circuit 33 has been printed, the program proceeds to instruction block 61 which causes the strip 1 of tags 2 to be fed a predetermined distance so that all of the printed tags have been cut by the cutter 19.
In the embodiment described above, the construction and operation of the device have been described with reference to a case wherein information is printed on a strip 1 of tags 2 which are longitudinally continuous and the data lines extend traverse to the travelling direction of web 1 as shown in FIG. 1. However, the construction and operation of the device are as follows when information is printed on a strip 41 of tags 42 wherein tags 42 are transversely continuous and the data lines extend parallel to the travelling direction of web 1 as shown in FIG. 6.
As shown in FIG. 6, the strip 41 consists of a number of tags 42 continuous in the transverse direction. An aperture 43 is formed between each pair of adjacent tags 42. The strip 41 is cut after the printing operation has been completed at the portion corresponding to each aperture 43 to provide individual tags 42. A perforation 44 is formed widthwise at the center of each tag 42. The perforation 44 divides each tag 42 into a user's portion 42a and a data processing portion 42b.
When printing is to be performed on the strip 41 of tags 42 which are transversely continuous, the structure of the device and the format of the printing data remain the same as those of the embodiment described with reference to FIGS. 2 and 4.
The primary difference between the structure of the device used to print the tags of FIG. 1 and that used to print the tags of FIG. 6 lies in the character generator 47 (FIG. 7). In this embodiment, the character generator 47 again stores each character in dot matrix form. The character generator is so constructed, however, that the dot information can be read out dot column by dot column rather than dot line by dot line. One commercially available character generator which can be used for this purpose is manufactured by NEC Corp. under the product designation μPD482D. This product will store 128 characters in dot matrix form, each matrix being a 10 (column)×9 (row) matrix. The character generator 47 has two sets of addresses, the first set identifying the desired one of the 128 characters, the second set identifying the particular column of that character to be read out.
Presuming that the first dot column of the first data column of the tag 42 of FIG. 6 is to be printed, the CPU 30 will first cause the character generator 47 to place the dot information corresponding to the first dot column of the letter "S" on bus 31 and will then serially shift this parallel bit data into shift register 48. Thereafter, the information will be serially shifted into second shift register 49. Since those heaters 17a corresponding to the line spacing SP 2 must not be enabled, CPU 30 must insert a number of binary 0's corresponding to the line spacing SP 2 . To this end, CPU 30 places a count in counter 46 corresponding to the line spacing SP 2 . This will be determined by the line spacing value SL(2). Thereafter, CPU 30 begins generating clock signals which both decrease the count in counter 46 and cause the bit information in shift register 48 (all binary 0's) to shift into shift register 49. This process continues until the count in counter 46 is 0 with the result that a number of binary 0's corresponding to the line spacing value SL(2) will be placed in second shift register 49. Thereafter, CPU 30 causes character generator 47 to place the dot information corresponding to the first dot column of the character "3" to be shifted into shift registers 48 and 49 and the process is repeated until all of the character information for a single dot column of a single character column has been placed in second shift register 49.
The particular flow chart for printing data on the tag of FIG. 6 will now be described with reference to the flow chart of FIG. 8. In this flow chart, it is presumed that all of the printing data has already been entered into the data memory circuit 33. Additionally, this flow chart only describes the manner in which the first data column is printed. The process is repeated for each successive data column of the tag 42.
Proceeding first to instruction block 62, the CPU 30 sets both the line index L and the dot column index DC equal to 1. The CPU 30 then sets the count in counter 46 equal to the line spacing value SL(1). See block 63.
Once the value SL(1) is set in the counter 46, the contents in the first shift register 48 are transferred to the second shift register 49 in response to a clock signal from the CPU 30. See block 64. During this transfer operation, binary 0's are transferred from shift register 48 to shift register 49 since the first shift register 48 is in the cleared state. Each time a single bit is transferred from register 48 to register 49, the counter 46 is decremented by one in response to a clock signal from the CPU 30. A determination is then made in decision block 65 as to whether the count of the counter 46 is "0". When it is, the program proceeds to instruction block 66. When the count of the counter 46 is "0", a number of binary zeroes equal to the line spacing value SL(1) will have been transferred to the second shift register 49. The contents in the second shift register 49 thus constitute the line spacing SP 1 .
Proceeding to instruction block 66, CPU 30 causes the character generator 47 to place the DCth dot column of the first character of the Lth data line into shift register 48. As indicated by instruction block 67, CPU 30 also sets the count in counter 46 equal to the number of bits in the dot column of the single character. The contents of the first shift register 48 are then transferred to the second shift register 49 in response to a clock signal from the CPU which also decrements the count in counter 46. This process is repeated until the count in counter 46 is equal to 0 (instrument block 69) at which point all of the bits of data corresponding to the dot column of the character in question have been placed into shift register 49.
Proceeding to decision block 70, CPU 30 then determines if the line value L is equal to the maximum line value Lmax. If it is, this indicates that the dot information corresponding to a single dot column of all the data lines have been placed into shift register 49 and that the print head 17 can be brought into contact with the ribbon 16 (instruction block 72). If L is less than Lmax, then the program proceeds to instruction block 71 wherein the line index L is increased by one and the program returns to instruction block 63. This process is continued until the bit information corresponding to a single dot column of all of the data lines has been placed into shift register 49.
Once the dot information in shift register 49 has been printed (block 72), CPU 30 proceeds to decision block 73 and determines if the dot column index DC is equal to the maximum dot column index DCmax. The value of DCmax corresponds to the total number of dot columns in the standard matrix (10 columns in the example being considered). If DC is less than DCmax, CPU 30 proceeds to instruction block 74 where it increases the dot column index DC by 1 and sets the line index L equal to 1, and the program returns to instruction block 63 so that the next dot column can be printed. This process continues until all of the dot columns have been printed.
In this manner, when printing is to be performed for a strip 41 of tags 42 which are transversely continuous, the intervals between each character pattern data are set in accordance with the line spacing data SD so as to determine the line spacings SP 1 , SP 2 , etc.
In the embodiments described above, a printing device of thermal type is described. However, the present invention may be similarly applied to printing devices of various other types such as dot printers, electrostatic printers, or wire dot matrix printers. In the first embodiment wherein the strip 1 of tags 2 as shown in FIG. 1 is to be printed, the line spacings SP 1 , SP 2 , etc. are determined by controlling the distance the strip 1 of tags 2 is fed in accordance with the line spacing data SD. Accordingly, the present invention may be similarly applied to a drum impact printing device of the line printer type.
Furthermore, in the embodiments described above, the line spacings SP 1 , SP 2 , etc. are set. However, it is possible to supply character spacing data so as to freely set the spacing between characters in the row direction. In particular, when printing is to be performed on a strip 1 of tags 2 as shown in FIG. 1, the intervals between the character pattern data are set in accordance with the character spacing data. However, when printing is to be performed on a strip 41 of tags 42 as shown in FIG. 6, the strip 41 of tags 42 is fed for a distance corresponding to the character spacing data when each column is printed.
In the examples set forth above, each character was stored in a 10×9 or 8×16 matrix. While this is sufficient for many applications, a 20×20 matrix for small characters and a 20×40 matrix for large characters is preferred if additional resolution is desired, for example, if the tag is to be read by an optical scanner.
In summary, according to the present invention, the character data representing the information to be printed as well as line spacing data for printing are stored. The line spacing is determined in accordance with the line spacing data. Since a user can freely set the line spacing, the user can readily respond to tags of different sizes or designs or can also change the number of printing lines or the like as needed. Furthermore, since it is not necessary to set the line spacing for each user, standardization of printing devices is facilitated.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof and, accordingly, reference should be made to the appended claims, rather than to the foregoing specification as indicating the scope of the invention.
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A printing device for a continuous strip of tags prints a plurality of lines on each of the tags. The device allows free selection and easy changing of line spacing. The device for a continuous strip of tags has a feed mechanism for feeding the strip of tags, a printing mechanism for printing a plurality of lines on each tag of the continuous strip of tags and a data memory circuit for storing input printing data. The printing data input to the data memory circuit is required to consist of character data corresponding to contents of the plurality of lines, followed by line spacing data for each line, followed by data indicating the number of tags.
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FIELD OF THE INVENTION
[0001] The present invention relates to the field of image processing, computer vision, and computer graphical user interfaces. In particular, the present invention discloses a video image based tracking system that allows a computer to identify and track the location of a moving object within a sequence of video images.
BACKGROUND OF THE INVENTION
[0002] There are many applications of object tracking in video images. For example, a security system can be created that tracks people that enter a video image. A user interface can be created wherein a computer tracks the gestures and movements of a person in order to control some activity.
[0003] However, traditional object tracking systems are computationally expensive and difficult to use. One example of a traditional method of tracking objects in a scene uses object pattern recognition and edge detection. Such methods are very computationally intensive. Furthermore, such systems are notoriously difficult to train and calibrate. The results produced by such methods often contain a significant amount of jitter such that the results must be filtered before they can be used for a practical purpose. This additional filtering adds more computation work that must be performed. It would therefore be desirable to have a simpler more elegant method of visually tracking a dynamic object.
SUMMARY OF THE INVENTION
[0004] A method of tracking a dynamically changing probability distribution is disclosed. The method operates by first calculating a mean location of a probability distribution within a search window. Next, the search window is centered on the calculated mean location and the search window is then resized. Successive iterations of calculating a mean, centering on the mean, and resizing the search window track an object represented by the probability distribution.
[0005] Other objects, features, and advantages of present invention will be apparent from the company drawings and from the following detailed description that follows below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] The objects, features and advantages of the present invention will be apparent to one skilled in the art, in view of the following detailed description in which:
[0007] [0007]FIG. 1 illustrates an example computer workstation that may use the teachings of the present invention.
[0008] [0008]FIG. 2 illustrates a pixel sampling of a human face.
[0009] [0009]FIG. 3A illustrates a small portion of sample image being converted into a flesh hue histogram.
[0010] [0010]FIG. 3B illustrates a normalized flesh hue histogram created by a sampling a human face.
[0011] [0011]FIG. 4 illustrates a probability distribution of flesh hues of an input image.
[0012] [0012]FIG. 5 illustrates a flow diagram describing the operation of the mean shift method.
[0013] [0013]FIG. 6 illustrates an example of a continuously adaptive mean shift method applied to one dimensional data.
[0014] [0014]FIG. 7 illustrates a flow diagram describing the operation of the continuously adaptive mean shift method.
[0015] [0015]FIG. 8 illustrates example of the continuously adaptive mean shift method applied to one dimensional data.
[0016] [0016]FIG. 9 illustrates a flow diagram describing the operation of a head tracker using the continuously adaptive mean shift method.
[0017] [0017]FIG. 10A illustrates a first diagram of a head within a video frame, a head tracker search window, and an calculation area used by the search window.
[0018] [0018]FIG. 10B illustrates a second diagram of a head within a video frame that is very close to the camera, a head tracker search window, and an calculation area used by the search window.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0019] A method and apparatus for object tracking using a continuous mean shift method is disclosed. In the following description, for purposes of explanation, specific nomenclature is set forth to provide a thorough understanding of the present invention. However, it will be apparent to one skilled in the art that these specific details are not required in order to practice the present invention. For example, the present invention has been described with reference to an image flesh hue probability distribution. However, the same techniques can easily be applied to other types of dynamically changing probability distributions.
The Overall Object Tracking System
[0020] A method of tracking objects using a continuously adaptive mean shift method on a probability distribution is disclosed. To simplify the disclosure of the invention, one embodiment is presented wherein a human head is located and tracked within a flesh hue probability distribution created from video image. However, the present invention can easily be used to track other types of objects using other types of probability distribution data. For example, the present invention could be used to track heat emitting objects using an infrared detection system. The present invention can also be used to track objects that are described using non image data such as population distributions.
[0021] The disclosed embodiment operates by first capturing a “talking head” video image wherein the head and shoulders of the target person are within the video frame. Next, the method creates a two dimensional flesh hue probability distribution using a preset flesh hue histogram. Then, the location of the target person's head is determined by locating the center of the flesh hue probability distribution. To determine the orientation of the target person's head, the major and minor axis of the flesh hue probability distribution is calculated.
Capturing the Data
[0022] Example Hardware
[0023] [0023]FIG. 1 illustrates one possible system for using the teachings of the present invention. In the illustration of FIG. 1, a user 110 is seated in front of a video camera 120 . The video camera 120 is used to capture a “talking head” image of the user 110 . In the embodiment of FIG. 1, the user is using a computer workstation that comprises a visual display monitor 151 , a keyboard 153 for alphanumeric input, a mouse 155 for cursor positioning, and a computer system 157 .
[0024] Generating a Flesh Hue Histogram
[0025] The computer system 157 digitizes the “talking head” image of the user 110 captured by video camera 120 . To build a flesh hue histogram, the user positions himself such that the user's head fills a sample area of an image captured by video camera 120 . Specifically, referring to FIG. 2, an image of a “talking head” image is displayed where the user's head substantially or completely fills the sample area. The pixels in the sample area are then used to build a flesh hue histogram.
[0026] In one embodiment, each pixel in the video image is converted to or captured in a hue (H), saturation (S), and value (V) color space. Certain hue values in the sample region are accumulated into a flesh hue histogram. FIG. 3A illustrates a small nine by nine pixel block that has been divided into its hue (H), saturation (S), and value (V) components being converted into a flesh hue histogram. In the embodiment of FIG. 3A, the hue values are grouped into bins wherein each bin comprises five consecutive hue values. Hue values are only accumulated if their corresponding saturation (S) and value (V) values are above respective saturation (S) and value (V) thresholds. Referring to the example of FIG. 3A, the S threshold is 20 and the V threshold is 15 such that a pixel will only be added to the flesh hue histogram if the pixel's S value exceeds 20 and the pixel's V value exceeds 15. Starting at the upper left pixel, this first pixel is added to the flesh hue histogram since the pixel's S value exceeds 20 and the pixel's V value exceeds 15. Thus, a marker 391 is added to the 20 to 24 hue value bin. Similarly, the center pixel of the top row will be added to the 20 to 24 hue value bin as illustrated by marker 392 . The center pixel of the right most column will not be added to the flesh hue histogram since its Saturation value does not exceed 20.
[0027] After sampling all the pixels in the sample area, the flesh hue histogram is normalized such that the maximum value in the histogram is equal to a probability value of one (“1”). In a percentage embodiment of FIG. 3B, all the histogram bins contain flesh hue probability values between zero (“0”) and one hundred (“100”) as illustrated in FIG. 3B. Thus, in the normalized flesh hue probability histogram illustrated in FIG. 3B, pixel hues that are likely to be flesh hues are given high percentage values and pixel hues that are not likely to be flesh hues are given low probability values.
[0028] Generating a Flesh Hue Probability Images
[0029] Once a flesh hue probability histogram has been created, the computer system 157 can quickly convert video images captured from the video camera into flesh hue probability distributions. This is performed by replacing the pixels in a video image with the their respective flesh hue probability values by using the flesh hue histogram of FIG. 3B as a look up table. FIG. 4 illustrates an example of a two dimensional image of a talking head wherein the pixels have been replaced with a percentage probability value that specifies the probability of the pixel being flesh. As apparent in FIG. 4, the pixels that comprise the person's face are given high probabilities of being flesh.
Object Tracking Using Mean Shift
[0030] Once a probability distribution has been created, the teachings of the present invention can be used to locate the center of an object and to track the object. An early embodiment of the present invention uses a standard mean shift method to track objects that have been converted into probability distributions.
[0031] [0031]FIG. 5 graphically illustrates how the standard mean shift method operates. Initially, at steps 510 and 520 , an initial search window size and initial search window location are selected. The method then computes the “mean” location of the search window at step 530 . At step 540 , the center of the search window is moved onto the mean location that was computed in step 530 . At step 550 , the method determines if it has converged upon the center of the probability distribution. This can be done by determine if the search was moved by a value less than a preset threshold value. If the mean shift method has converged, then it is done. If the mean shift method has not converged then the method returns to step 530 where the mean of the new search window location is calculated.
[0032] An example of the mean shift method in operation is presented in FIG. 6. To simplify the explanation, the example is provided using a one dimension slice of a two dimensional probability distribution. However, the same principles apply for a two or more dimensional probability distribution. Referring to step 0 of FIG. 6, a five sample wide search window is placed at an initial location. After a first iteration of the method, the search window is moved to the left as illustrated in step 1 of FIG. 6. The search window was moved left since the mean location of the search window samples was left of the initial search window location. After a second iteration, the search window is again moved left as illustrated in step 2 . The search window was moved left since the mean location of the search window samples in step 1 is left of the center of the search window in step 1 . After a third iteration, the search window again moves left. However, for all subsequent iterations, the search window will remain stationary (provided the distribution data does not change). Thus, by the third iteration, the mean shift method has converged.
[0033] To use the mean shift method for two dimensional image data, the following procedures are followed:
[0034] Find the zeroth moment:
M 00 = ∑ x ∑ y I ( x , y ) . ( 1 )
[0035] Find the first moment for x & y:
M 10 = ∑ x ∑ y xI ( x , y ) ; M 01 = ∑ x ∑ y yI ( x , y ) . ( 2 )
[0036] Then the mean location (the centroid) is:
x c = M 10 M 00 ; y c = M 01 M 00 . ( 3 )
[0037] Where I(x, y) is the image value at position (x, y) in the image, and x and y range over the search window.
[0038] The mean shift method disclosed with reference to FIG. 5 and FIG. 6 provides relatively good results, but it does have a few flaws. For example, for dynamically changing and moving probability distributions such as probability distributions derived from video sequences, there is no proper fixed search window size. Specifically, a small window might get caught tracking a user's nose or get lost entirely for large movements. A large search window might include a user and his hands as well as people in the background. Thus, if the distribution dymanically changes in time, then a static search window not produce optimal results.
Object Tracking Using Continuously Adaptive Mean Shift
[0039] To improve upon the mean shift method, the present invention introduces a continuously adaptive mean shift method referred to as a CAMSHIFT method. The CAMSHIFT method dynamically adjusts the size of the search window to produce improved results. The dynamically adjusting search window allows the mean shift method to operate better in environments where the data changes dynamically.
[0040] [0040]FIG. 7 graphically illustrates how the CAMSHIFT method of the present invention operates. At steps 710 and 720 , an initial search window size and initial search window location are selected. The CAMSHIFT method performs one or more iterations of the mean shift method to move the search window at step 730 . At step 750 , the method adjusts the size of the search window. The size of the search window may be dependent upon information gathered about the data. Next, at step 760 , the method determines if it has converged upon the center of the probability distribution. If the mean shift method has converged, then the method is done. If the CAMSHIFT method has not converged then the method returns to step 730 where the mean shift method is performed using the new search window location with the new search window size is calculated.
[0041] An example of the continuously adaptive mean shift method in operation is presented in FIG. 8. Again, to simplify the explanation, the example is provided using a one dimension slice of a two dimensional probability distribution. However, the same principles apply for a two or more dimensional distribution. In the example of FIG. 8, the continuously adaptive mean shift method adjusts the search window to a size that is proportional square root of the zeroth moment. Specifically, the continuously adaptive mean shift method in the example of FIG. 8 in two dimensions adjusts the search window to have a width and height of:
w=h= 2 *{square root}{square root over (M 00 )}. (4)
[0042] wherein M 00 is the zeroth moment of the data within the search window. (See equation 1.) For N dimensional distributions where N ranges from 1 to infinity, each side of the search window would be set to
w = α i * M 00 1 N . ( 5 )
[0043] where α 1 . is a positive constant. However, other embodiments may use other methods of determining the search window size.
[0044] Referring to step 0 of FIG. 8, a three sample wide search window is placed at an initial location. After a first iteration of the method, the search window is moved to the left as illustrated in step 1 of FIG. 6. The search window was moved left since the mean location of the search window samples was left of the initial search window location. After a second iteration, the search window is again moved left as illustrated in step 2 since the mean location of the search window samples in step 1 is left of the center of the search window in step 1 . However, it should also be noted that the size of the search window increased since the amount of data in the search window has increased. After a third iteration, the center of the search window again moves left and the search window size again increases. It can be seen in the subsequent iterations that the adaptive mean shift method adjusts the window size as it converges upon the mean of the data. Referring to step 7 of FIG. 8, the continuously adaptive mean shift method converges upon the mean of the contiguous data. It has been found that the continuously adaptive mean shift method with a search window width and height set equal to 2*{square root}{square root over (M 00 )}. will typically find the center of the largest connected region of a probability distribution, a great benefit for tracking one of multiple confusable objects.
Head Tracking Using Continuously Adaptive Mean Shift
[0045] To provide an example usage of the continuously adaptive mean shift method, one specific embodiment of a head tracking system is provided. However, many variations exist. The example is provided with reference to FIG. 9, FIG. 10A and FIG. 10B.
[0046] To reduce the amount of data that needs to be processed, the head tracker uses a limited “calculation region” that defines the area that will be examined closely. Specifically, the calculation region is the area for which a probability distribution is calculated. Area outside of the calculation region is not operated upon. Referring to step 907 of FIG. 9, the head tracker initially sets the calculation region to include the entire video frame. The initial search window size and location is selected to capture a head that is substantially centered in the video frame. Again, the initial search window size can include the entire video frame. Thus, the present invention can be implemented without any initial search window size or search window location parameters that need to be determined.
[0047] Next, at step 914 , the flesh hue probability distribution is calculated in the calculation region. During the first iteration, the probability distribution is calculated for the entire video frame. The continuously adaptive mean shift method is applied by steps 921 , 935 , and 942 to locate the region with the highest probability density. At step 949 , the size and location of the search window are reported. This information can be used for tracking the head location and size. The size parameter can be used to determine a distance of the head from the camera.
[0048] At step 956 , the size and location of the search window are used to determine a new calculation region. The calculation region is the area 1030 centered around the search window 1020 as illustrated in FIG. 10A such that a flesh hue probability distribution will only be calculated for the area around the head. By using the size and location of the search window, the “lock” of the motion-tracker is reinforced on the object of interest. In the example of a head tracker, when a person is close to the camera as illustrated in FIG. 10B, the flesh probability distribution will be large and any movements they make will also be large in absolute number of pixels translated so the calculation region must be large. But when the person is far from the camera as illustrated in FIG. 10A, their flesh probability distribution will be small and even if the person moves quite fast the number of pixels that the person translates will be small since the person is so far from the camera, so the calculation region can be small. After determining the location of the new calculation region, the method returns to step 914 where the method calculates the probability distribution in the new calculation area. The method then proceeds to search for the area with the greatest probability density.
[0049] A Kickstart Method
[0050] To initially determine the size and location of the search window, other methods of object detection and tracking may be used. For example, in one embodiment, a motion difference is calculated for successive video frames. The center of the motion difference is then selected as the center of the search window since the center of the motion difference is likely to be a person in the image.
[0051] Search Window Sizing
[0052] In a digital embodiment such as digitized video images, the probability distributions are discrete. Since the methods of the present invention climb the gradient of a probability distribution, the minimum search window size must be greater than one in order to detect a gradient. Furthermore, in order to center the search window, the search window should be of odd size. Thus, for discrete distributions, the minimum window size is set at three. Also, as the method adapts the search window size, the size of the search window is rounded to the nearest odd number greater or equal to three in order to be able to center the search window. For tracking colored objects in video sequences, we adjust the search window size as described in equation 4.
[0053] Determining Orientation
[0054] After the probability distribution has been located by the search window, the orientation of the probability distribution can be determined. In the example of a flesh hue tracking system to locate a human head, the orientation of the head can be determined. To determine the probability distribution orientation, the second moment of the probability distribution is calculated. Equation 6 describes how a second moment is calculated.
[0055] Second moments are:
M 20 = ∑ x ∑ y x 2 I ( x , y ) ; M 02 = ∑ x ∑ y y 2 I ( x , y ) ( 6 )
[0056] After determining the second moments of the probability distribution, the orientation of the probability distribution (the angle of the head) can be determined.
[0057] Then the object orientation (major axis) is:
θ = arctan ( 2 ( M 11 M 00 - x c y c ) ( M 20 M 00 - x c 2 ) - ( M 02 M 00 - y c 2 ) ) 2 ( 7 )
[0058] In the embodiment of a head tracker, the orientation of the probability distribution is highly correlated with the orientation of the person's head.
[0059] The foregoing has described a method of tracking objects by tracking probability densities. It is contemplated that changes and modifications may be made by one of ordinary skill in the art, to the materials and arrangements of elements of the present invention without departing from the scope of the invention.
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A tracking method is disclosed. The method of the present invention tracks a object using a probability distribution of the desired object. The method operates by first calculating a mean location of a probability distribution within a search window. Next, the search window is centered on the calculated mean location. The steps of calculating a mean location and centering the search window may be performed until convergence. The search window may then be resized. Successive iterations of calculating a mean, centering on the mean, and resizing the search window track an object represented by the probability distribution. In one embodiment, a flesh hue probability distribution is generated from an input video image. The flesh hue probability distribution is used to track a human head within the video image.
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This application claims the benefit of U.S. patent application Ser. No. 60/318,794 filed on Sep. 13, 2001, incorporated herein by reference.
BACKGROUND OF THE INVENTION
The present invention is generally related to control and operation of power converter devices, and, more particularly, to circuits and techniques for parallel operation of power converters.
Switching-mode power converters are widely used in numerous applications to meet the needs of electronic systems. For example, in the telecom and networking industries, DC/DC converters convert a raw dc voltage (input), usually over a certain variation range, to a dc voltage (output) that meets a set of specifications.
DC/DC converters are commonly paralleled at their outputs either to provide higher output power to a load or to provide redundant operation in high reliability applications where the output must be maintained within specification in the event of a failure of a DC/DC converter. One of the main factors that contribute to effective operation of parallel DC/DC converters is the current sharing mechanism that is implemented in the parallel system. The purpose of this mechanism is to ensure equal distribution of current among the devices.
Various types of circuits for sharing a common load among a plurality of DC/DC converters are known. In a traditional current share scheme, each converter module has a current-share terminal, either at the output or at the input. When converters are in parallel operation, these current-share terminals are tied together. The signal at the current-share terminal tries to maintain an almost equal current in each module, which could be determined by a master-slave mechanism or an average type of mechanism. The master-slave technique may include, for example, a dedicated-master scheme where one module is selected as the master or an automatic-master where the system decides which converter will be chosen as the master depending on which converter has the largest output current.
Feedback loops exist in switching power converters to help the system maintain a constant output voltage. For parallel operation, inside each module, the actual current feedback signal is used to adjust its output voltage reference so that all modules will share the load current. However, if the output voltage reference and the current sharing terminal are located at different sides of the isolation boundary inside the converter, the current-sharing circuit becomes complex since the control signal has to be passed through the isolation boundary. This is especially problematic in standard converter modules, such as half-brick modules, quarter-brick modules, ⅛ th brick modules etc, where board space is limited.
Accordingly, it would be desirable to provide a simple and effective solution without sending a signal across the isolation boundary.
In addition, for protection and control needs, the output current or the main switch current of the converter needs to be reliably sensed. In power converters, a current sense transformer is usually used to sense the current information in the power switches or in transformer windings, for current mode control and for over-current protection. FIG. 1 shows a forward converter with a current sensing transformer T_sen. The main purpose of T_sen is to produce, from the primary current, a proportional secondary current that can easily be measured or used to control various circuits. The primary winding is connected in series with the source current to be measured, while the secondary winding is normally connected to a meter, relay, or a burden resistor to develop a low level voltage that is used for control purposes. Whenever a current sensing transformer is used, the proper reset of the transformer core under all operating conditions must be ensured, otherwise the saturation of the core could lead to a distorted current information and therefore the control loop and protection will not function properly. The resistance of the reset resistor R_reset is much higher than the resistance of the sensing resistor R_sen so that the small magnetizing current in the sensing transformer can generate enough voltage to reset the core during a fraction of the “OFF” period of the main power switch Q 1 .
This current sensing scheme assumes the current in Q 1 is always positive. However, in reality this current could be negative depending on the magnetizing current in the main transformer T and the output inductor current in Lo. This issue becomes more problematic in a dc/dc converter using synchronous rectification where there is a negative current in Lo under light load or during dynamic process during the “ON” period of the main power switch Q 1 . Due to the diode D_sen, the negative current reflected to the sensing transformer output will create a high voltage on the resistor R_reset, which in turn causes a high magnetizing current in the sense transformer T_sen. This magnetizing current causes false signal at Vsense, and can bringing the converter into malfunction. This high voltage could also quickly saturate the current sensing transformer core and cause the damage to the converter due to loss of sensed signal. Over-current protection is also important in any dc/dc converter. As the output current reaches a predetermined level, the converter should shut down or enter into a constant power mode to prevent damage to the converter and the loads that it powers.
Accordingly, a simple and reliable current sensing scheme, which also provides over-current protection is desired.
BRIEF SUMMARY OF THE INVENTION
Generally, the present invention fulfills the foregoing needs by providing in one aspect thereof a power distribution system including a plurality of power converter modules each having a current sharing signal terminal on an input side and power output terminals on an output side, the corresponding power output terminals of the several modules being connected together and adapted to power a common load; an interconnecting signal bus coupled across the current sharing signal terminals on the input side; a plurality of feedback circuits, each of which is associated with one of said modules, each feedback circuit including a comparator (output error amplifier) for comparing a feedback voltage on the output side with a reference voltage to provide an error signal to the input side; the error signal conditioned to provide a current command signal to said signal bus, wherein the signal bus provides a common current command signal to drive the power converter modules.
In a specific aspect thereof, the feedback circuits include isolation circuitry to electrically isolate the error signal from the input side in the form of an opto-isolator apparatus. The output error amplifier drives the input of the opto-isolator apparatus. Moreover, the error signal is conditioned by a first buffer (a first operational amplifier) to provide the current command signal to the signal bus. To operate as a master-slave scheme, a diode may be series coupled to the output of the first operational amplifier such that the highest current command signal of all power converter modules is provided to the signal bus.
In a further aspect thereof, a second buffer (a second operational amplifier) is provided to condition the common current command signal from the signal bus prior to driving the power converter module associated with the second buffer. The power converter module is driven by a pulse-width modulated (PWM) controller having the output of the second operational amplifier as an input thereto. The PWM controller may also include a ramp compensation signal input and a current sense input. In another aspect thereof, the second buffer is a compensator that compares the common current command signal from the signal bus with a sensed signal related to output current. The output of the compensator drives the power converter module associated therewith. In a further aspect thereof, the first operational amplifier compares the error signal with a second reference voltage to provide the current command signal provided to the signal bus, wherein the second reference voltage is generated from a bias voltage or a reference voltage from a pulse-width modulated (PWM) controller. Optionally, a time delay (e.g., an R-C circuit) is introduced to the second reference voltage.
The present invention also provides a current share circuit for power converters in parallel operation. The circuit includes an interconnecting signal bus coupled across current sharing signal terminals on an input side of said power converters; a plurality of feedback circuits, each of which is associated with one of said converters, each feedback circuit including a comparator for comparing a feedback voltage on an output side of the power converter with a reference voltage to provide an error signal to the input side; the error signal conditioned to provide a current command signal to said signal bus, wherein the signal bus provides a common current command signal to drive the power converters.
Moreover, a method for current sharing in parallel operated power converters is provided, the method including (a) interconnecting a signal bus across current sharing signal terminals on an input side of said power converters; (b) providing a plurality of feedback circuits, each of which is associated with one of said converters, each feedback circuit including (i) comparing a feedback voltage on an output side of the power converter with a reference voltage to provide an error signal to the input side; (ii) conditioning the error signal to provide a current command signal to said signal bus, and (iii) providing a common current command signal from the signal bus to drive the power converters.
In a further aspect thereof, a current sense circuit for a power converter is provided including a current sense transformer generating a current indicative of the current through the main switch of the power converter; and a transistor synchronized with the main power switch having a first port coupled to the current sense transformer for receiving a voltage that is indicative of the current through the main switch of the power converter and a second port for providing an output voltage across a sense resistor that is indicative of the current through the main switch.
The sensed current can be used for the over-current protection of a power converter. The over-current protection circuit includes a first diode to sample and hold the peak value of the current sense signal; and comparison circuitry capable of comparing said peak value with a reference voltage and developing an over-current protection signal in accordance therewith.
BRIEF DESCRIPTION OF THE DRAWINGS
The features and advantages of the present invention will become apparent from the following detailed description of the invention when read with the accompanying drawings in which:
FIG. 1 shows a forward converter with a current sensing transformer.
FIG. 2 is a functional block diagram of parallel modules with a current share scheme in accordance with the aspects of the present invention.
FIG. 3 shows a simplified circuit diagram of a forward converter.
FIG. 4 illustrates one exemplary circuit of a current share scheme for paralleling multiple modules in accordance with the aspects of the present invention.
FIG. 5 illustrates another exemplary circuit of a current share scheme for paralleling multiple modules in accordance with the aspects of the present invention.
FIG. 6 is a functional block diagram of parallel modules with another current share scheme in accordance with the aspects of the present invention.
FIG. 7 illustrates an exemplary circuit of a current share scheme including a time delay for paralleling multiple modules in accordance with the aspects of the present invention.
FIG. 8 shows a forward converter with a current sensing circuit in accordance with the aspects of the present invention.
FIG. 9 shows a circuit diagram of an over-current protection circuit in accordance with the aspects of the present invention.
FIG. 10 shows a circuit diagram of another over-current protection circuit in accordance with the aspects of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 2 shows the function blocks of two modules 12 a and 12 b in parallel. The power stages 14 a and 14 b shown are forward converters. This current-share scheme works for other topologies as well. It is important to note that the invention is not limited to paralleling just two converters 14 a and 14 b . Additional converters and associated components of appropriate topology can be connected in parallel if desired so as to divide the current supplied to the load among more than two DC/DC converters. For simplicity of discussion however, the drawings and the remainder of this description are limited to the case where only two forward converters 14 a and 14 b , are paralleled. From this description, it will be apparent to those skilled in the art how additional converters can be added in a similar manner. Each power stage may include a DC/DC converter and a respective control circuit. Multiple DC/DC converters may be connected in parallel to meet increased current demands of a load. With increased current demand, additional converters can be added as needed.
Turning to FIG. 3, a brief overview of the operation of forward converter 14 a is presented to facilitate an understanding of the present invention, the operation of forward converter 14 b being identical. In operation, a DC voltage input Vin 1 is connected to the primary winding of the power transformer T by a power switch Q 1 . A clamp circuit arrangement is also provided to limit the reset voltage. The power switch Q 1 is shunted by a series connection of a clamp capacitor Creset and a switch device Q 2 . The conducting intervals of Q 1 and Q 2 are mutually exclusive with certain time delay between them.
The secondary winding is connected to an output circuit through a synchronous rectifier circuit including rectifying devices SR 1 and SR 2 . With the power switch Q 1 conducting, the input voltage is applied across the primary winding. The secondary winding is oriented in polarity to respond to the primary voltage with a current flow through inductor Lo, the load connected to the output lead and back through the rectifier device SR 1 to the secondary winding. Continuity of the current flow in the inductor Lo when the power switch Q 1 is non-conducting is maintained by the current path provided by the conduction of the rectifier device SR 2 . An output filter capacitor Co shunts the output of the converter. The output of a PWM controller provides a PWM drive signal to switch Q 1 and switch Q 2 .
With reference to FIG. 2, forward converters 14 a and 14 b configured according to the present invention, are connected mutually in parallel at their output terminals Vo+ and Vo− across a common load (not shown). The respective input terminals Vin+ and Vin− of converters 14 a and 14 b are connected across a common DC source. “I_share 1 ” and “I_share 2 ” are the respective current share terminals 15 a and 15 b for parallel operation of multiple modules 12 a and 12 b . The respective I_share terminals 15 a and 15 b are connected via I_sharebus 17 .
Feedback loops are provided in each module to help the system maintain a constant output voltage. Referring to module 12 a , module 12 b being configured in the same manner, an output error amplifier 18 a compares the feedback output voltage Vo with a reference voltage Vo_ref so that the output of the error amplifier 18 a is a current command signal. This signal goes through an isolation block 20 a to the primary side where it is coupled to a first buffer 22 a . The output of buffer 22 a is a current command related signal available to its I_share terminal 15 a.
A conditioning circuit such as peak detect diode circuit can be also be included in buffer 22 a to allow the I_share terminal to pick the highest, the lowest or a weighted average of the current command related signals from all paralleled modules.
This common signal at the I_share terminal 15 a is then coupled to a second buffer 24 a in module 12 a (as is in all the paralleled modules). The output of the second buffer 24 a is conditioned so that it can serve as the current command signal I_comm to the PWM controller 16 a . Different PWM chips may require the command signal in different patterns. Since all the paralleled modules have the same signal at the inputs of their respective second buffers, their command signals should be essentially the same, so that their output currents will also be about the same. The buffers 22 a , 24 a can comprise a simple gain or contain certain poles and zeros in their transfer function.
An example circuit implementation of one exemplary embodiment of the current share scheme for paralleling multiple modules in accordance with the aspects of the present invention is shown in FIG. 4 . In this embodiment, isolation block comprises an optocoupler (Opto 20 ′) and the first and second buffers 22 ′, 24 ′ are operational amplifiers (Opam_ 1 and Opam_ 2 ). Z 1 -Z 9 are impedances that can be resistors, capacitors or the combination of both according to the design aspects of the particular circuit.
The output error amplifier 18 ′ compares the feedback output voltage Vo with a reference voltage Vo_ref to adjust its output and drive the input of Opto 20 ′. The polarity shown in the figure is such that when Vo is higher than the reference Vo_ref. the output of the error amplifier 18 ′ will move higher. With an increasing current in Opto 20 ′, the voltage across Z 2 will increase which leads to a decreasing “I_share” and increasing “I_comm”; “I_share” being the signal at the current share terminal for parallel operation of multiple modules and “I_comm” being the command signal to the following PWM controller 16 .
The polarity of the error amplifier block 18 ′ can be different based on different ways to implement error amplification as required by current control in different PWM controllers. For a different polarity, either the secondary or the primary connection of the Opto 20 ′ can be rearranged to accommodate the difference.
After the command signal goes through Opto 20 ′ to the primary side, it is coupled to Opam_ 1 (first buffer 22 ′). The output of Opam_ 1 (buffer 22 ′) is a current command related signal available to the module's I_share terminal 15 . The signal at the I_share terminal 15 , common to all modules in parallel, is then coupled to Opam_ 2 (buffer 24 ′). The output of Opam_ 2 (buffer 24 ′) in each module is conditioned so that it can serve as the current command signal to the PWM controller 16 . However, depending on the control logic of the PWM controller 16 , Opam_ 2 (buffer 24 ′) may not be needed and is, therefore, optional. The reference voltage for Opam_ 1 and Opam_ 2 (V_ref) can be generated from the V_bias or some other means such as the reference voltage from the PWM controller 16 as shown in FIGS. 2 and 6. In this example, a diode D_share makes the system a master-slave scheme with the highest I_share being used in all the paralleled modules.
Turning now to FIG. 5, another exemplary circuit of a current share scheme for paralleling multiple modules in accordance with the aspects of the present invention is shown. In this exemplary circuit, the circuit components are the same as in FIG. 4 except that a PWM controller TI UCC2809 is shown. For this PWM controller 16 ″, Opam_ 2 (buffer 24 ′) is used so that the correct logic of I_comm is fed into pin 1 of the PWM controller 16 . Since the voltage at the feedback pin (Pin 1 ) of UCC2809 is fixed to around 1V at the turn-off of the PWM signal, and the ramp compensation signal is also preprogrammed, the sum of the current command signal I_comm and the current sense signal I_sense have to be almost constant at the turn-off instant of gate drive signal. Therefore, modulating the current command signal I_comm through the current sharing circuit can directly control the current sense signal, and thus the output current of the converter module.
Turning now to FIG. 6, in another aspect of the invention, buffer 24 of FIG. 2 comprises a compensator 27 a in module 12 a ′, with module 12 b ′ configured the same. Compensator 27 a compares the signal at I_share terminal 15 a with a sensed signal related to the output current. The compensator 27 a may have a certain compensation function as required to control the output current in close-loop. The output V_con of the compensator 27 a can be used as a current command as in FIG. 4 or FIG. 5 . However, due to the closed loop control function of compensator 27 a , V_con can also be used directly to modulate the duty cycle, e.g., if a voltage-mode PWM chip is used.
Reference now will be made to FIG. 7 . In “hot-plug-in” applications, when a module is plugged in, it may go through a start-up process while other paralleled modules are already in operation. It is important that this process will not cause too much disturbance to the output voltage. For the plugged-in module in the initial start-up process, its Opto current initially will be low before the output error amplifier establishes its operating point. Therefore, the voltage across Z 2 will be low and I_share will be high. A high I_share will become the master signal commanding other modules in operation to boost the output current. As a result, the output voltage may have an overshoot spike. To avoid this undesired phenomenon, a time delay 28 can be introduced to the V_ref of Opam_ 1 so that I_share will not go high too quickly during the initial startup process. The delay can be implemented with a simple R-C as shown in FIG. 7 or other known means. This extra freedom could also help to improve the start-up performance of the single module operation. In the scheme shown in FIG. 6, similar function can be achieved by limiting the reference signal V_ref to the compensator 27 a during the startup (current walk-in).
Accordingly, the invention provides a simple and effective solution to the problems in the art without sending signal across the isolation boundary with the current-share terminal at the input side and the voltage reference and the output error amplifier at the output side. All the paralleled modules are forced to follow the same current reference signal feeding into the PWM controller in each module.
An advantage of the present invention is its simplicity. However, one drawback is the possible saturation of all but one of the output error amplifiers will lead to certain transients when the controlling unit (one with its voltage loop in control) is switched in/out of the system (N+1 redundancy). With known anti-saturation mechanisms, proper allocation of control loop gain, and other specific means, the transient performance is acceptable in many applications.
In another aspect of the invention, a method and circuit is provided for current sensing. With reference to FIG. 8, the circuit 30 shown replaces the diode D_sen of the prior art (FIG. 1) with a switch 32 (Q_sen) controlled to operate with the main switch Q 1 synchronously. An optional delay circuit, possibly consisting of a resistor, a capacitor, or a diode, can also be used to create certain delays between Q_sen's control signal and Q 1 's control signal, so that noise signals associated with the switching on and off of Q 1 can be reduced or excluded from the output of the current sense circuit. Switch 32 is shown as a MOSFET switch. The gate of switch 32 is connected to the gate of Q 1 directly. Alternately, the gate may be connected through some simple signal conditioning circuit such as a resistor, or a RC network so that the time difference between their gate signals can be used to optimize the performance, such as filtering out the spike of T_sen current at the turn-on of switch Q 1 , as known in the art. In this scheme, the switch 32 is controlled by the same gate signal (or a signal very close to the same gate signal if a signal conditioning circuit is used) of the main power switch Q 1 . Therefore, the sensed current, no matter whether it is positive or negative, will be able to go through R_sen when switch 32 is ON, avoiding the high voltage on R_reset when the switch current is negative.
The above-sensed current can also be used to generate an over-current protection signal as shown in the circuitry 34 of FIG. 9 . The sensed current information V_sen should have a waveform same as the current in the main switch Q 1 . This circuit 34 will react to the sensed peak current information. In many cases the contribution to V_sen from the magnetizing current of the power transformer is small enough comparing with the contribution from the current in the output filter inductor. In such cases, the protection set-point also well represents the output current. The diode D_peak will “sample and hold” the peak value of the current sense signal. Resistor R 1 is significantly smaller than R 2 so that the voltage on C 1 after a certain switching cycles will be close to the peak of V_sen. R 1 and C 1 are optional. R 1 can reduce the effect of the protection circuit on the current sense circuit, and also form a filter with C 1 to eliminate any high frequency components in the sensed signal due to either turn-on current spikes or other noises. R 2 is for discharging the voltage on C 1 with a discharging rate slow enough not affecting the accuracy of the protection set-point. With the proper selection of parameters R 1 , R 2 and C 1 , the voltage across C 1 can fairly accurately represent a parameter of the converter, such as the output inductor current. The voltage on C 1 will then be used to compare with a predefined voltage reference through an operational amplifier or a comparator whose output will change state as the sensed current information becomes greater than the predetermined value represented by Vref. The polarity of the two inputs to the OpAm or the Comparator is not labeled in the drawing and is determined by the need of the circuitry following it. The OCP signal can then be used to shut down the converter in various ways.
D_peak can also be implemented as a switch (e.g., MOSFET) controlled synchronously with the main switch. However, if it is implemented as a diode, its voltage drop is a function of temperature, and could take a significant portion of V_sen in practical use. To compensate this change for more accurate protection, another same type of diode can be added as shown in the circuitry 34 ′ of FIG. 10 . D_peak and D_match could be in one package, in close-by packages, or have certain thermal communication so their junction temperatures are not significantly different. The use of R 3 and R 4 is optional. They serve two purposes: (a) providing freedom to adjust the over-current set point without changing the V_sen magnitude that usually affects the control loop performance; (b) providing a bias current in D_match near the operating point of D_peak, so their voltage drops will be close under all conditions.
Depending on the requirement of the over-current protection, the output of the above circuitry can be used to either shut down the converter (option of latch or resume operation when the over-current condition is removed) or injecting a signal into the control loop so that the output voltage will decrease when the output current goes over the predetermined value—usually being referred to as constant power mode.
While the preferred embodiments of the present invention have been shown and described herein, it will be obvious that such embodiments are provided by way of example only. Numerous variations, changes and substitutions will occur to those of skill in the art without departing from the invention herein. Accordingly, it is intended that the invention be limited only by the spirit and scope of the appended claims.
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A power distribution system is provided including current sharing circuitry, current sensing and over-current protection. The system includes a plurality of power converter modules each having a current sharing signal terminal on an input side and power output terminals on an output side, the corresponding power output terminals of the several modules being connected together and adapted to power a common load; an interconnecting signal bus coupled across the current sharing signal terminals on the input side; a plurality of feedback circuits, each of which is associated with one of said modules, each feedback circuit including a comparator (error amplifier) for comparing a feedback voltage on the output side with a reference voltage to provide an error signal to the input side; the error signal conditioned to provide a current command signal to said signal bus, wherein the signal bus provides a common current command signal to drive the power converter modules.
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FIELD OF THE INVENTION
[0001] This invention concerns the field of paper manufacture and refers to an aqueous suspension for addition to cellulose fibre, paste, in which such suspension includes calcium sulphate plus at least one additive.
[0002] The addition of this aqueous suspension to the cellulose fibre paste during the paper preparation process causes a surprising increase in the opacifying capacity of calcium sulphate.
BACKGROUND OF THE INVENTION
[0003] In paper-making processes currently existing in the state of the art, different additives are normally added to the aqueous suspension of cellulose in order to give it the desired characteristics (physical and mechanical resistance values). Nevertheless, the amount of additives added in relation to the amount of cellulose may not exceed a certain threshold.
[0004] In the state of the art, the addition of calcium sulphate to the aqueous cellulose fibre suspension during the paper-making stage is known to give certain properties to the final product. The designation of calcium sulphate covers any compound that has the general formula of CaSO 4 nH 2 O, where n has a value ranging between 0 and 2 or higher).
[0005] These properties are generally related to greater physical and mechanical resistance of paper, lower energy consumption, better performance of the filler (added inorganic compounds such as additives), lower consumption of cellulose paste, etc.
[0006] Nevertheless, calcium sulphate has a low paper-opacifying capacity and, therefore, the addition of calcium sulphate to the cellulose fibre suspension during paper preparation, even at quantities above 30% by weight, does not sufficiently opacify the paper thus obtained to make it particularly suitable for printing. In other words, the maximum amount of calcium sulphate that can be added with respect to the amount of cellulose is not enough to give paper a sufficiently high degree of opacity.
[0007] When considering the high amount of paper used for printing and writing, in particular in publications, press uses, notebooks and books for school use and other similar purposes, it is evident that paper opacification is a significant problem.
[0008] The low opacifying capacity of paper containing calcium sulphate is the main reason that manufacturers of paper for printing and writing in general add substances such as titanium dioxide with greater opacifying capacity than calcium sulphate to the paste used to manufacture paper. Nevertheless these highly opacifying additives are costly and noticeably increase the cost of paper obtained in this way.
[0009] Hence, the need to find a less costly solution to the problem of paper opacification can be easily understood. Surprisingly, in this invention, the addition of small quantities of at least one additive to calcium sulphate prior to the addition thereof to the cellulose fibre solution for paper, manufacture has been found to significantly increase the opacifying capacity of this calcium sulphate. Suitable additives for this invention include: kaolin, calcium carbonate, talc, titanium dioxide, aluminium silicate, calcium silicate, other silicates and/or their mixtures, as described below.
DESCRIPTION OF THE INVENTION
[0010] This invention refers to an aqueous suspension for addition to the cellulose fibre paste used in paper-making, in which the suspension includes calcium sulphate and at least one additive Suitable additives for this invention are, for example: kaolin, calcium carbonate, talc, titanium dioxide, aluminium silicate, calcium silicate, other silicates and/or their mixtures. Due to the variety of compounds that show suitable behaviour in an aqueous suspension according to this invention, the additives indicated can be understood to be only examples of non-limiting additives.
[0011] This invention also refers to a process used to prepare this aqueous suspension that includes calcium sulphate and at least one additive.
[0012] This invention also refers to a process to obtain paper that includes the preparation of this aqueous suspension that contains calcium sulphate and at least one additive, and the addition of this Suspension to the aqueous cellulose fibre suspension used to manufacture paper.
[0013] In this invention, calcium sulphates with differing degrees of hydration can be used, except for natural calcium sulphate anhydrous. There are two kinds of calcium sulphates with n=0: natural anhydrous and artificial anhydrous. Natural calcium sulphate anhydrous, which is found in quarries mixed with calcium sulphate with n=2, cannot be used in a suspension according to this invention. In contrast, artificial calcium sulphate anhydrous, which comes from calcium sulphate dihydrate that has been heated to remove 2 moles of water, can be used in this invention, requiring simply more time and a higher stirring speed to obtain an aqueous suspension according to the invention.
[0014] Without intending to limit the scope of this invention in any way, it is postulated that when at least one of these additives is mixed with calcium sulphate in water, this additive is included in the crystalline structure of calcium sulphate modifying the percentage of reflected and/or refracted light rays and therefore modifying the opacifying capacity of this calcium sulphate.
[0015] This structural modification of calcium sulphate crystals does not occur if the additive is added in the presence of the aqueous cellulose fibre suspension. It is postulated that the cellulose rapidly attracts calcium sulphate, thereby preventing any possible transformation of the properties of calcium sulphate crystals.
[0016] The addition of additives of the kaolin, calcium carbonate, talc, titanium dioxide, aluminium silicate or calcium silicate type to the aqueous cellulose fibre suspension during paper-making is well known in the state of the art. Nevertheless, it is important to stress that in the state of the art, there is no description or suggestion that the combined use of calcium sulphate together with at least one additive prior to the addition to the cellulose fibre suspension would cause a significant increase in the opacifying capacity of calcium sulphate. This increase does not result simply from the sum of the opacifying capacities of calcium sulphate and the additive, but rather from a modification of the crystalline structure of calcium sulphate, which causes an opacifying effect that is surprisingly higher than expected.
[0017] In an aqueous suspension according to this invention, calcium sulphate and the additive(s) are found at a ratio by weight between 100:1 and 1:1, preferably between 50:1 and 2:1.
[0018] In an aqueous suspension according to this invention, the ratio between the mixture of calcium sulphate and the additive(s) with respect to water ranges between 0.1% and 80% by weight, preferably between 1% and 25% by weight. In an aqueous suspension according to this invention, the optimal pH value of this suspension ranges between 3 and 9, preferably between 4 and 8.
[0019] This invention also refers to a process used to prepare an aqueous suspension that includes calcium sulphate and at least one additive according to the invention. This process consists of; 1) mixing this calcium sulphate and at least one of these additives with water; and 2) homogenising the mixture by stirring vigorously.
[0020] In a preferred embodiment of this invention, this calcium sulphate and this additive are mixed together while still dry, before being mixed. with water. In another preferred embodiment of the invention, this calcium sulphate and this additive are added to water separately.
[0021] This invention also refers to a process used for paper-making, in which the process is characterised in that a previously prepared aqueous suspension of at least one additive and calcium sulphate is added to the cellulose fibre solution. This process includes the following stages: 1) Preparation of a suspension according to the invention as described above; 2) Preparation of a cellulose fibre suspension in water; 3) Addition of the suspension according to the invention to the cellulose fibre suspension in the paper circuit. In a paper-making process using an aqueous suspension according to this invention, this calcium sulphate and at least one of these additives is kept under suspension by stirring until the time the cellulose paste is added. The stirring time depends on the kind of calcium sulphate used and the kind of additive(s) and is, in general, equal to or greater than 30 minutes.
[0022] As an advantage, the paper-making process according to this invention allows highly opaque paper to be obtained at a low cost.
[0023] An illustrative, non-limiting example of the invention is given below.
EXAMPLES
[0024] The batch calcium sulphate used specifically in the following tests is CaSO 4 x0.3 H 2 O (i.e., n=0.3 moles). When this calcium sulphate is added along with at least ;one, additive, in water to create an aqueous suspension according to this, invention, this compound is hydrated to a greater or lesser extent, depending on the value of n.
[0025] In the tests described below, a stirring speed of 3000 rpm and. a stirring time of 30 minutes were used, with calcium sulphate hydrated with n=0.3.
[0026] Technical Characteristics of the Products Used in the Tests:
[0027] Kaolin
[0028] PARTICLE SIZE=88-90%<21i
[0029] Talc
[0030] PARTICLE SIZE=25%<2 μ, residue-free and filtered to 50 μ
[0031] CaCO 3
[0032] ANALYSIS:
[0033] CaCO 3 >99
[0034] SiO 2 0.4
[0035] MgO 0.3
[0036] Al 2 O 3 0.1
[0037] Fe 2 O 3 0.08
[0038] SO 4 <0.1
[0039] PARTICLE SIZE=particles with a size less than:)
[0040] 60 μ 99
[0041] 40 μ 95
[0042] 20 μ 83
[0043] 5 μ 38
Characteristics
[0044] WHITENESS FMX-Amber filter 88.6
[0045] FMY-Green filter 87.1
[0046] FMZ-Blue filter 80.6
[0047] Anastase Titanium Dioxide
[0048] TiO 2 min. 98.0%
[0049] Fe 2 O 3 max. 0.1%
[0050] SiO 2 max. 0.5%
[0051] SO 3 max. 0.5%
[0052] P 2 O 5 max. 0.55%
[0053] PARTICLE SIZE
[0054] Residue on sieve of mesh 325 (44 μm);<0.5%
[0055] Calcium Sulphate n=0.3
[0056] Sieve reject at 53 microns 0.39%
[0057] Whiteness Z % hunterlab. 923%
[0058] ASTM yellow index E313 2.1
[0059] Initial cure time 9 min
Example 1
Preparation of Fillers at a Concentration of 10% by Weight
[0060] Three different kinds of fillers were prepared:
[0061] a) Calcium sulphate dihydrate
[0062] 90% of saturated CaSO 4 water+10% of CaSO 4 .2 H 2 O=90% of saturated CaSO 4 water+(8.2% of CaSO 4 .0.3H 2 O+1.8% H 2 O)=91.8% of saturated CaSO 4 water+8.2% of CaSO 4 x0.3 H 2 O
[0063] b) Additive (talc, calcium carbonate, kaolin or titanium dioxide)
[0064] 90% desionised water+10% additive
[0065] c) Calcium sulphate+additive.
[0066] 90% saturated CaSO 4 water+9% CaSO 4 x2H 2 O+1% additive or additive mixture=90% water+(7.4% CaSO 4 x0.3H 2 O+1.6% H 2 O=9% CaSO 4 2H 2 O)+1% additive=91.6% water+7.4% CaSO 4 x0.3 H 2 O+1% additive
[0067] To prepare the suspensions, CaSO 4 and/or the additive are gradually added over the water while stirring at 3000 rpm, and stirring is continued for at least 30 minutes before the suspension is added to the fibre suspension.
Example 2
Preparation of Paper
[0068] 1—A cellulose dispersion at a concentration of 1±0.01% (dry) is prepared. A bleached sulphate cellulose paste is used as the starting material, as in the case of all tests.
[0069] a) In all tests where the filler Contains calcium sulphate, calcium sulphate-saturated water is used to prepare this dispersion. Calcium sulphate-saturated water has a conductivity of 1.42 mS.
[0070] b) In tests where the filler does not contain calcium sulphate, deionised water is used to prepare this dispersion.
[0071] The dispersion is prepared in a “Pulper” apparatus or laboratory disintegrator for 2 hours.
[0072] 2—Samples of the prepared solution are collected using a standard container to ensure that the same quantity of dispersed paste at 1±0.01% is collected at all times. This quantity is 37.478 g.
[0073] 3—A second dilution of the cellulose paste is made by homogenising the 37.478 g of paste at 1% with 400 g of water:
[0074] a) Calcium sulphate-saturated water in tests where the filler contains calcium sulphate.
[0075] b) Deionised water in all other cases.
[0076] The dilution is carried out in a magnetic laboratory stirrer apparatus at 1100 rpm for 40 sec.
[0077] 4—Immediately after the stirrer is turned on, one of the fillers prepared in example 1 is added.
[0078] Two different tests are conducted for each kind of filler: addition of 30% or 15% of filler, calculated with respect to the cellulose.
[0079] Addition of 30% calculated with respect to the cellulose: 1.124 g of filler at 10 are added.
[0080] 37.478 g of cellulose at 1%=0.37478 g of cellulose (dry).
[0081] 0.37478×30/100=0.1124 g filler (dry), i.e., 1.124 g of filler at 10%; which represents 23.1% of filler with respect to the total solids.
[0082] Addition of 15% calculated with respect to the cellulose: 0.562 g of filler at 10% are added.
[0083] 37.478 g of cellulose at 1%=0.37478 g of cellulose (dry).
[0084] 0.37478×15/100=0.0562 g filler (dry), i.e., 0.562 g of filler at 10%; which represents 11.55% of filler with respect to the total solids.
[0085] 5—After 40 sec., the stirrer is turned off and the dispersion is filtered through a Büchner funnel under vacuum conditions.
[0086] The filter used is a cellulose triacetate membrane of pore size of 0.2 microns, sufficiently small to prevent losses.
[0087] Once the dispersion is filtered, the filter+paper sheet is removed with Büchner tongs and the dispersion is placed in an oven at 80° C. with forced air circulation until the weight is constant.
[0088] 6—The dry paper sheet +filter is weighted and the opacity of the entire unit is checked in a photovolt apparatus.
[0089] Both the prepared sheet of paper and the filter have a diameter of 9.20 cm. The opacity of the unit is measured at 5 different points on the circumference: at the midpoint and at 4 points at a distance equally apart from each other that is equivalent to half the distance between the midpoint of the sheet and the circumference perimeter.
[0090] Once the 5 results have been obtained, the mean of all 5 results is computed. If any of the results vary more than 10% from the mean, the 5 results of this sheet are discarded.
[0091] To calculate the opacity of the paper prepared using the process according to the intention described above, the difference between the total opacity (of the sheet of paper+filter) and the filter opacity must be calculated.
[ Op ( P+F )]−( Op F )= Op P
[0092] Op(P+F)=opacity of paper+filter
[0093] Op F=opacity of the filter
[0094] Op P=opacity of the sheet of paper.
[0095] Results
[0096] A) From the Group of Additives
[0097] Two different tests are performed for each 5 additive (with 30% and 15% of filler with respect to cellulose).
PRODUCT OPAC. with 30% OPAC. with 15% Talc 8.76° 7.9° Calcium carbonate 12.25° 10.2° Calcium sulphate 14.4° 12.0° Kaolin 16.2° 13.0° TiO 2 19° 17.0°
[0098] B) Aqueous Suspension of Calcium Sulphate+Additive Added to the Cellulose Fibre Suspension.
OPAC. with OPAC. with Calcium sulphate + additive 30% 15% 10% calcium sulphate 14.4° 12° 9% calcium sulphate + 1% Talc 15.6° 14.3° 9% calcium sulphate + 1% 15.1° 13.6° Calcium carbonate 9% calcium sulphate + 1% 17.6° 17.0° kaolin 9% Calcium sulphate + 1% TiO 2 18.3° 17.4°
[0099] C) Calcium Sulphate and Additive Added Separately to the Cellulose Fibre Suspension
OPAC. with OPAC. with Calcium sulphate + additive 30% 15% 9% calcium sulphate + 1% talc 13.7° 11.5° 9% calcium sulphate + 1% CaO 3 14.3° 11.8° 9% calcium sulphate + 1% 14.7° 11.9° kaolin 9% calcium sulphate + 1% TiO 2 14.8° 12.5° 10% calcium sulphate 14.4° 12°
[0100] Discussion of the Results
[0101] The following table shows the increased opacifying capacity of calcium sulphate when this calcium sulphate is prepared and added in combination with one additive (in the case of 30% of fillers calculated with respect to dry cellulose).
OPACITY with 30% Increase with Prepared and added respect to calcium together sulphate only 10% calcium sulphate 14.4° 9% sulphate + 1% talc 15.6° 8.3% 9% sulphate + 1% CaO 3 15.1° 4.9% 9% sulphate + 1% kaolin 17.6° 22.2% 9% sulphate + 1% TiO 2 18.3° 27.1%
[0102] By comparing the results, the addition of calcium sulphate and one additive separately, to the fibre suspension is seen not to produce any particular increase in opacity, whereas if a previously prepared suspension of calcium sulphate and additive is added to the cellulose fibre suspension, a surprising increase in the opacity of calcium sulphate is observed.
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The aqueous suspension contains hydrated n calcium sulfate (CaSO 4 nH 2 O), the value of n ranging from 0 to 2 (0<n<2) and an additive. The method for preparing said aqueous suspension involves the following steps: a) mixing the calcium sulfate and at least one of said additives with water and b) homogenizing the mixture under strong agitation. The method for preparing the paper includes adding said aqueous suspension to the cellulose fiber suspension.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to an image forming apparatus, such as a printer, a copier, a fax machine.
[0003] 2. Description of the Related Art
[0004] A digital duplicating machine may have functions of a digital scanner and a digital printer, and a digital duplicating machine may even be formed by including both a digital scanner portion and digital printer portion. Digital scanners and digital printers have their own characteristic parameters, with which they are set to work at the best performance. For example, in a digital duplicating machine including a digital scanner portion and digital printer portion, the characteristic parameters of the digital scanner and digital printer are determined when they are fabricated in the factory and are usually stored in a non-volatile memory installed in the digital printer which usually works under sequential control.
[0005] Even when a digital scanner and a digital printer are fabricated separately, furthermore, even after the digital scanner and the digital printer are shipped, for example, when they are in distribution, it is still possible to realize a digital duplicating machine by just connecting the digital scanner to the digital printer. In, this case, because the digital scanner and the digital printer are fabricated separately, the characteristic parameters of the digital scanner and the digital printer are originally stored in their own non-volatile memories. In this case, because generally the digital scanner and the digital printer include built-in micro-computers to control their respective operations, the micro-computers may communicate with each other to realize the function of a duplicating machine.
[0006] However, when a digital scanner and a digital printer fabricated separately are connected later, the characteristic parameters of the digital scanner have to be modified to fit the overall performance of the digital duplicating machine. In this case, there arises a problem of management of the characteristic parameters, and this problem may make it difficult to realize the function of a digital duplicating machine.
SUMMARY OF THE INVENTION
[0007] Accordingly, it is a general object of the present invention to solve the above problem of the related art.
[0008] A first specific object of the present invention is to provide an image recording apparatus able to realize a function of a digital duplicating machine by connecting a digital scanning device to a digital printing device even when the digital scanning device and the digital printing device are in distribution.
[0009] A second specific object of the present invention is to provide an image recording apparatus able to ensure the performance of a digital scanning device and manage characteristic parameters of the digital scanning device from a digital printing device.
[0010] A third specific object of the present invention is to provide an image recording apparatus able to ensure the performance of a digital scanning device, manage characteristic parameters of the digital scanning device from a digital printing device, and maintain compatibility even when a different digital scanning device is connected to the digital printing device.
[0011] A fourth specific object of the present invention is to provide an image recording apparatus able to ensure the performance of a digital scanning device, and maintain compatibility even when the digital scanning device is newly connected or the digital scanning device is connected to a different digital printing device.
[0012] A fifth specific object of the present invention is to provide an image recording apparatus able to ensure the performance of a digital scanning device and eliminate the necessity of adjusting characteristic parameters of the digital scanning device even when the digital scanning device is newly connected.
[0013] To attain the above objects, according to a first aspect of the present invention, there is provided an image forming apparatus, comprising a digital printing device that prints an image according to image signals input thereto, the digital printing device including a first nonvolatile memory for storing first parameters that optimize performance thereof, and a digital scanning device, connectable to the digital printing device, that scans an image and converts the image into electric signals, the digital scanning device including a second nonvolatile memory for storing second parameters that optimize performance thereof, wherein the digital printing device includes control means for modifying the second parameters when the digital scanning device is connected to the digital printing device.
[0014] Preferably, the control means comprise reading means for reading the second parameters stored in the second nonvolatile memory of the digital scanning device when the digital scanning device is connected to the digital printing device, modification means for modifying the second parameters read by the reading means, and writing means for writing the modified second parameters to the second nonvolatile memory of the digital scanning device when the digital scanning device is connected to the digital printing device.
[0015] Preferably, the control means comprise reading means for reading the second parameters stored in the second nonvolatile memory of the digital scanning device when the digital scanning device is connected to the digital printing device, modification means for modifying the second parameters read by the reading means, and writing means for writing the modified second parameters to the first nonvolatile memory of the digital printing device and the second nonvolatile memory of the digital scanning device when the digital scanning device is connected to the digital printing device.
[0016] Preferably, the control means comprise reading means for reading the second parameters stored in the second nonvolatile memory of the digital scanning device when the digital scanning device is connected to the digital printing device, modification means for modifying the second parameters read by the reading means, and writing means for writing values equal to the modifications made by the modification means to the second nonvolatile memory of the digital scanning device when the digital scanning device is connected to the digital printing device.
[0017] Preferably, the control means comprise reading means for reading the second parameters stored in the second nonvolatile memory of the digital scanning device when the digital scanning device is connected to the digital printing device, modification means for modifying the second parameters read by the reading means, and writing means for writing values equal to the modifications made by the modification means to the first nonvolatile memory of the digital printing device and the second nonvolatile memory of the digital scanning device when the digital scanning device is connected to the digital printing device.
[0018] To attain the above objects, according to a second aspect of the present invention, there is provided a digital printing device that prints an image according to image signals input thereto, the digital printing device forming an image forming apparatus when connected with a digital scanning device that scans the image and converts the image into the image signals, the digital printing device including a first nonvolatile memory for storing first parameters that optimize performance thereof, and the digital scanning device including a second nonvolatile memory for storing second parameters that optimize performance thereof, the digital printing device comprising control means for modifying the second parameters when the digital scanning device is connected to the digital printing device.
[0019] These and other objects, features, and advantages of the present invention will become more apparent from the following detailed description of preferred embodiments given with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] [0020]FIG. 1 is a block diagram showing a hardware configuration of an image forming apparatus according to a first embodiment of the present invention;
[0021] [0021]FIGS. 2A and 2B are views of memory maps of the EEPROM 18 and NVRAM 25 of the image forming apparatus according to the first embodiment of the present invention;
[0022] [0022]FIG. 3 is a flow chart showing an example of the operation of the image forming apparatus according to the first embodiment of the present invention;
[0023] [0023]FIGS. 4A and 4B are views of memory maps of the EEPROM 18 and NVRAM 25 of an image forming apparatus according to a second embodiment of the present invention;
[0024] [0024]FIG. 5 is a flow chart showing an example of the operation of the image forming apparatus according to the second embodiment of the present invention;
[0025] [0025]FIG. 6 is a flow chart showing another example of the operation of the image forming apparatus according to the second embodiment of the present invention;
[0026] [0026]FIG. 7 is a flow chart showing an example of the operation of an image forming apparatus according to a third embodiment of the present invention;
[0027] [0027]FIGS. 8A and 8B are views of memory maps of the EEPROM 18 and NVRAM 25 of an image forming apparatus according to a fourth embodiment of the present invention;
[0028] [0028]FIG. 9 is a flow chart showing an example of the operation of the image forming apparatus according to the fourth embodiment of the present invention;
[0029] [0029]FIGS. 10A and 10B are views of memory maps of the EEPROM 18 and NVRAM 25 of an image forming apparatus according to a fifth embodiment of the present invention;
[0030] [0030]FIG. 11 is a flow chart showing an example of the operation of the image forming apparatus according to the fifth embodiment of the present invention;
[0031] [0031]FIGS. 12A and 12B are views of memory maps of the EEPROM 18 and NVRAM 25 of an image forming apparatus according to a sixth embodiment of the present invention; and
[0032] [0032]FIG. 13 is a flow chart showing an example of the operation of the image forming apparatus according to the sixth embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0033] Below, preferred embodiments of the present invention are explained with reference to the accompanying drawings.
[0034] In the following descriptions, as an example, the nonvolatile storage medium may be an NVRAM (NonVolatile Random Access Memory), which includes a power supply, or an EEPROM (Electrically Erasable Programmable Read-Only Memory), or an OTPROM (One Time Programmable Read-Only Memory), or a PROM (Programmable Read-Only Memory).
[0035] First Embodiment
[0036] [0036]FIG. 1 is a block diagram showing a hardware configuration of an image forming apparatus according to a first embodiment of the present invention.
[0037] The image forming apparatus according to the first embodiment of the present invention includes a digital scanner 1 and a digital printer 2 connected to each other, thus having the function of a digital duplicating machine. The digital scanner 1 has an EEPROM 18 , and the digital printer 2 has an NVRAM 25 , which are nonvolatile memories.
[0038] In the digital scanner 1 , a manuscript is placed on a glass window and is irradiated by a lamp 16 ; when a carriage holding the lamp 16 and an optical system moves, the manuscript is scanned in the sub scan direction; the light reflected from the manuscript or the light transmitted through the manuscript passes through the optical system, and is detected by a CCD 12 that acts as an image sensor; the light detected by the CCD 12 is converted into electrical signals in the CCD 12 , and from the image signals, the image on the manuscript is obtained by the digital scanner 1 . The image signals are amplified, combined, and are converted into digital signals (A/D conversion) in a signal processing unit 13 , and then are output to an image processing unit 26 of the digital printer 2 .
[0039] The controller 11 , which comprises an IC chip, controls all parts of the digital scanner 1 ; specifically, the controller 11 switches ON or OFF an inverter 15 that drives the lamp 16 , drives a motor 17 to move the carriage mentioned above, accepts detection signals from a sensor 14 that detects the movement of the carriage, and accesses the EEPROM 18 .
[0040] In the digital printer 2 , the main control section 21 has a CPU 22 that controls a not-illustrated engine of the digital printer 2 and the controller 11 of the digital scanner 1 . The CPU 22 operates according to the program stored in a ROM 23 ; it controls the digital printer 2 to work as a printer when the digital scanner 1 is not connected to the digital printer 2 , and when the digital scanner 1 is connected to the digital printer 2 , it controls all the components in the digital printer 2 and the digital scanner 1 so that the digital printer 2 and the digital scanner 1 together work as a digital duplicating machine.
[0041] The RAM 24 temporarily stores data generated when the CPU 22 is in operation, and the NVRAM 25 stores characteristic parameters of the digital printer 2 . The characteristic parameters of the digital scanner 1 are stored in the EEPROM 18 connected to the controller 11 . Those parameters are written to the digital scanner 1 and the digital printer 2 , respectively, when they are fabricated in the factory. The image processing unit 26 receives and processes the image signals from the signal processing unit 13 , and outputs the image signals to the engine of the digital printer 2 . The engine of the digital printer 2 records an image on a medium, such as paper, according to the image signals from the image processing unit 26 .
[0042] [0042]FIGS. 2A and 2B are views of memory maps of the EEPROM 18 and NVRAM 25 , respectively, of the image forming apparatus according to the first embodiment of the present invention.
[0043] As illustrated in FIG. 2A, in the EEPROM 18 , for example, a header 31 is allocated in a region of a few bytes located from the address 0000H, and a data region 32 is allocated next to the header 31 to store the characteristic parameters of the digital scanner 1 .
[0044] Similarly, as illustrated in FIG. 2B, in the NVRAM 25 , for example, a header 41 is allocated in a region of a few bytes located from the address 0000H, and a data region 43 is allocated next to the header 41 to store the characteristic parameters of the digital printer 2 .
[0045] When the digital scanner 1 is fabricated, the characteristic parameters of the digital scanner 1 are stored in the data region 32 , and the initial values of the characteristic parameters are stored in the header 31 of the EEPROM 18 .
[0046] Similarly, when the digital printer 2 is fabricated, the characteristic parameters of the digital printer 2 are stored in the data region 43 , and the initial values of the characteristic parameters are stored in the header 41 of the NVRAM 25 .
[0047] [0047]FIG. 3 is a flow chart showing an example of the operation of the image forming apparatus according to the first embodiment of the present invention. Specifically, FIG. 3 shows the procedure for adjusting values of the parameters of the digital scanner 1 when the digital scanner 1 is connected to the digital printer 2 as an option after the digital scanner 1 and the digital printer 2 are shipped and in distribution.
[0048] As illustrated in FIG. 3, in step S 31 , a user or a service person operates a panel on the digital printer 2 to select a mode for adjusting the values of the characteristic parameters of the digital scanner 1 . Upon that, the CPU 22 receives a signal from the panel indicating selection of the adjustment mode, and based on the signal, the CPU 22 displays a menu on the panel, allowing adjustment of the values of the characteristic parameters of the digital scanner 1 .
[0049] In step S 32 , on the panel, the user or the service person selects a parameter of the digital scanner 1 which is to be adjusted.
[0050] In step S 33 , the CPU 22 receives a signal from the panel indicating selection of the desired parameter, and based on the signal, the CPU 22 , via the controller 11 , reads the selected parameter from the data region 32 of the EEPROM 18 , in which the parameters of the digital scanner 1 are stored, and displays the value of the selected parameter on the panel.
[0051] In step S 34 , the user or the service person inputs a new value of the selected parameter of the digital scanner 1 on the panel.
[0052] In step S 35 , the CPU 22 stores the value of the selected parameter input from the panel in the RAM 24 temporarily.
[0053] In step S 36 , the user or the service person is required to confirm that the change of the value of the selected parameter will really be made.
[0054] In step S 37 , when it is confirmed that the change is to be made, the CPU 22 reads the value of parameter temporarily saved in the RAM 24 , and writes the value to the address of the selected parameter in the data region 32 .
[0055] In step S 38 , after all desired parameters are adjusted following the above steps S 31 through S 37 , the user or the service person is required to make confirmation again, and the adjustment of the characteristic parameters of the digital scanner 1 is completed after the confirmation.
[0056] In the above adjustments, when adjusting the values of the characteristic parameter of the digital scanner 1 , which is connected to the digital printer 2 to realize a digital duplicating machine after the digital scanner 1 and the digital printer 2 are shipped and in distribution, because the new values of the parameters are stored in the EEPROM 18 , which is a nonvolatile storage medium, the new values do not disappear even after the power is turned off, and thus the performance of the digital scanner 1 is ensured.
[0057] According to the present embodiment, because the digital printer 2 and the digital scanner 1 are equipped with nonvolatile memories (EEPROM 18 and NVRAM 25 ), therefore, even after the digital scanner 1 and the digital printer 2 are shipped and in distribution, the function of a digital duplicating machine can be realized by connecting the digital scanner 1 to the digital printer 2 .
[0058] Second Embodiment
[0059] The image forming apparatus of the present embodiment has the same configuration as that described in the first embodiment with reference to FIG. 1. That is, using the same numeral references as in the first embodiment for the same components, the image forming apparatus of the second embodiment includes a digital scanner 1 and a digital printer 2 connected to each other, thus having the function of a digital duplicating machine. The digital scanner 1 has an EEPROM 18 , and the digital printer 2 has an NVRAM 25 , which are nonvolatile memories.
[0060] The image forming apparatus of the present embodiment is different from that in the first embodiment in the aspect that one more data region is allocated in the NVRAM 25 of the digital printer 2 to store the characteristic parameters of the digital scanner 1 .
[0061] [0061]FIGS. 4A and 4B are views of memory maps of the EEPROM 18 and the NVRAM 25 , respectively, of the image forming apparatus according to the second embodiment of the present invention.
[0062] As illustrated in FIG. 4A, in the EEPROM 18 , for example, a header 31 is allocated in a region of a few bytes located from the address 0000H, and a data region 32 is allocated next to the header 31 to store the characteristic parameters of the digital scanner 1 .
[0063] Similarly, as illustrated in FIG. 4B, in the NVRAM 25 , for example, a header 41 is allocated in a region of a few bytes located from the address 0000H. A data region 42 is allocated next to the header 41 for storing the characteristic parameters of the digital scanner 1 . Furthermore, a data region 43 is allocated next to the data region 42 for storing the characteristic parameters of the digital printer 2 .
[0064] In the fabrication process of the digital scanner 1 , the characteristic parameters of the digital scanner 1 are stored in the data region 32 , and the initial values of the parameters are stored in the header 31 in the EEPROM 18 .
[0065] Similarly, in the fabrication process of the digital printer 2 , the characteristic parameters of the digital printer 2 are stored in the data region 43 , and the initial values of the parameters are stored in the header 41 in the NVRAM 25 . In the fabrication process of the digital printer 2 , the data region 42 contains only certain initial values.
[0066] [0066]FIG. 5 is a flow chart showing an example of the operation of the above image forming apparatus according to the present embodiment when power is turned on to start the image forming apparatus. One typical case as shown in FIG. 5 is the case in which the control section of the digital scanner 1 including the EEPROM 18 is exchanged, and thus, the characteristic parameters of the digital printer 2 have been written into the header 41 of the NVRAM 25 , but the data in the header 31 of the EEPROM 18 are still the initial values of the digital scanner 1 .
[0067] In step S 51 , when it is confirmed that the digital scanner 1 has been connected to the digital printer 2 , the CPU 22 reads data from the header 41 of the NVRAM 25 .
[0068] In step S 52 , the CPU 22 confirms whether the data read from the header 41 are the initial values of the parameters of the digital printer 2 .
[0069] If the data read from the header 41 are the initial values of the parameters of the digital printer 2 , the routine proceeds to step S 53 , otherwise, the routine proceeds to step S 57 .
[0070] In step S 53 , the CPU 22 , via the controller 11 , reads values of the characteristic parameters of the digital scanner 1 from the data region 32 in the EEPROM 18 , and saves the data to the RAM 24 .
[0071] In step S 54 , the CPU 22 writes the values of the characteristic parameters of the digital scanner 1 saved in the RAM 24 to the data region 42 of the NVRAM 25 .
[0072] In step S 55 , the CPU 22 writes the values of the characteristic parameters of the digital scanner 1 to the header 31 of the EEPROM 18 through the controller 11 .
[0073] In step S 56 , at the same time with the step S 55 , the CPU 22 also writes the values of the characteristic parameters of the digital printer 2 to the header 41 . After that, the routine is completed.
[0074] In step S 57 , if the data read from the header 41 are not the initial values of the parameters of the digital printer 2 , the CPU 22 reads data from the header 31 in the EEPROM 18 through the controller 11 .
[0075] In step S 58 , the CPU 22 confirms whether the data read from the header 31 are the initial values of the parameters of the digital scanner 1 . If they are, the routine proceeds to step S 53 , and the operations in steps S 53 through S 56 are executed as described above. Otherwise, the routine is completed.
[0076] By the above process, the characteristic parameters of the digital scanner 1 can be stored in the digital printer 2 in advance.
[0077] [0077]FIG. 6 is a flow chart showing another example of the operation of the image forming apparatus according to the present embodiment. Specifically, FIG. 6 shows the procedure for adjusting values of the parameters of the digital scanner 1 when the digital scanner 1 is connected to the digital printer 2 as an option after the digital scanner 1 and the digital printer 2 are shipped and in distribution.
[0078] As illustrated in FIG. 6, in step S 61 , a user or a service person operates a panel on the digital printer 2 to select a mode for adjusting the values of the characteristic parameters of the digital scanner 1 . Upon that, the CPU 22 receives a signal from the panel indicating selection of the adjustment mode, and based on the signal, the CPU 22 displays a menu on the panel, allowing adjustment of the values of the characteristic parameters of the digital scanner 1 .
[0079] In step S 62 , on the panel, the user or the service person selects a parameter of the digital scanner 1 which is to be adjusted.
[0080] In step S 63 , the CPU 22 receives a signal from the panel indicating selection of the desired parameter, and based on the signal, the CPU 22 , via the controller 11 , reads, the selected parameter from the data region 42 of the NVRAM 25 , in which the parameters of the digital scanner 1 are stored, and displays the value of the selected parameter on the panel.
[0081] In step S 64 , the user or the service person inputs a new value of the selected parameter of the digital scanner 1 on the panel.
[0082] In step S 65 , the CPU 22 stores the value of the selected parameter input from the panel to the RAM 24 temporarily.
[0083] In step S 66 , the user or the service person is required to confirm that the change of the value of the selected parameter will really be made.
[0084] In step S 67 , when it is confirmed that the change is to be made, the CPU 22 reads the value of parameter temporarily saved in the RAM 24 , and writes the value to the address of the selected parameter in the data region 42 .
[0085] In step S 68 , after all desired parameters are adjusted following the above steps S 61 through S 67 , the user or the service person is required to make confirmation again, and the adjustment of the characteristic parameters of the digital scanner 1 is completed after the confirmation.
[0086] Because of the above adjustments, when the digital printer 2 and the digital scanner 1 are connected to realize the function of a digital duplicating machine after the digital scanner 1 and the digital printer 2 are shipped and in distribution, it is possible to perform memory management for both the digital printer 2 and the digital scanner 1 on the digital printer 2 side.
[0087] According to the present embodiment, when a digital scanner 1 is newly connected to the digital printer 2 , because the data of the characteristic parameters in the EEPROM 18 of the digital scanner 1 can be stored in the NVRAM 25 of the digital printer 2 , memory management for the digital printer 2 and the digital scanner 1 can be performed on the side of the digital printer 2 . In addition, when modifying the values of the parameters, because the corrected values can also be stored in the NVRAM 25 of the digital printer 2 , the performance of the digital scanner 1 is ensured.
[0088] Third Embodiment
[0089] The image forming apparatus of the present embodiment has the same configuration as that described in the first embodiment with reference to FIG. 1. That is, using the same numeral references as in the first embodiment for the same components, the image forming apparatus of the present embodiment includes a digital scanner 1 and a digital printer 2 connected to each other, thus having the function of a digital duplicate machine. The digital scanner 1 has an EEPROM 18 , and the digital printer 2 has an NVRAM 25 , which are nonvolatile memories.
[0090] Furthermore, as illustrated in FIGS. 4A and 4B, a header 31 is allocated in the EEPROM 18 , and a data region 32 is allocated next for storing the characteristic parameters of the digital scanner 1 ; a header 41 is allocated in the NVRAM 25 , and a data region. 42 and a data region 43 are allocated in order for storing the characteristic parameters of the digital scanner 1 and the characteristic parameters of the digital printer 2 , respectively. Moreover, the characteristic parameters of the digital scanner 1 are stored into the data region 32 , and the initial values of the parameters are stored in the header 31 in the EEPROM 18 in the fabrication process of the digital scanner 1 ; and the characteristic parameters of the digital printer 2 are stored in the data region 43 , and the initial values of the parameters are stored in the header 41 in the NVRAM 25 in the fabrication process of the digital printer 2 . Further, the data region 42 contains certain initial values in fabrication.
[0091] [0091]FIG. 7 is a flow chart showing an example of the operation of the image forming apparatus according to the third embodiment of the present invention. Specifically, FIG. 7 shows the procedure for adjusting values of the parameters of the digital scanner 1 when the digital scanner 1 is connected to the digital printer 2 as an option after the digital scanner 1 and the digital printer 2 are shipped and in distribution.
[0092] As illustrated in FIG. 7, in step S 71 , a user or a service person operates a panel on the digital printer 2 to select a mode for adjusting the values of the characteristic parameters of the digital scanner 1 . Upon that, the CPU 22 receives a signal from the panel indicating selection of the adjustment mode, and based on the signal, the CPU 22 displays a menu on the panel, allowing adjustment of the values of the characteristic parameters of the digital scanner 1 .
[0093] In step S 72 , on the panel, the user or the service person selects a parameter of the digital scanner 1 which is to be adjusted.
[0094] In step S 73 , the CPU 22 receives a signal from the panel indicating selection of the desired parameter, and based on the signal, the CPU 22 , via the controller 11 , reads the selected parameter from the data region 42 of the NVRAM 25 , in which the parameters of the digital scanner 1 are stored, and displays the value of the selected parameter on the panel.
[0095] In step S 74 , the user or the service person inputs a new value of the selected parameter of the digital scanner 1 on the panel.
[0096] In step S 75 , the CPU 22 stores the value of the selected parameter input from the panel to the RAM 24 temporarily.
[0097] In step S 76 , the user or the service person is required to confirm that the change of the value of the selected parameter will really be made.
[0098] In step S 77 , when it is confirmed that the change is to be made, the CPU 22 reads the value of parameter temporarily saved in the RAM 24 , and writes the value to the address of the selected parameter in the data region 42 of the NVRAM 25 , and to the address of the parameter in the data region 32 of the EEPROM 18 .
[0099] In step S 78 , after all desired parameters are adjusted following the above steps S 71 through S 77 , the user or the service person is required to make confirmation again, and the adjustment of the characteristic parameters of the digital scanner 1 is completed after the confirmation.
[0100] Because of the above adjustments, when the digital printer 2 and the digital scanner 1 are connected to realize the function of a digital duplicating machine after the digital scanner 1 and the digital printer 2 are shipped and in distribution, it is possible to manage data stored in memories of both the digital printer 2 and the digital scanner 1 on the side of the digital printer 2 , and in addition, the adjusted parameters can also be stored in the digital scanner 1 . As a result, it is not necessary to adjust the characteristic parameters of the digital scanner 1 again even when the digital scanner 1 is connected to a different digital printer 2 .
[0101] According to the present embodiment, in a digital duplicating machine including the digital scanner 1 and the digital printer 2 which are connected to each other, when the values of the characteristic parameters of the digital scanner 1 are changed, the new values of the characteristic parameters are stored in both the EEPROM 18 of the digital scanner 1 and the NVRAM 25 of the digital printer 2 , and therefore, memory management can be performed from the side of the digital printer 2 , and the performance of the digital scanner 1 is ensured. Furthermore, compatibility of the digital scanner 1 is ensured even when a different digital scanner is connected to the digital printer 2 .
[0102] Fourth Embodiment
[0103] The image forming apparatus of the present embodiment has the same configuration as that described in the first embodiment with reference to FIG. 1. That is, using the same numeral references as in the first embodiment for the same components, the image forming apparatus of the present embodiment includes a digital scanner 1 and a digital printer 2 connected to each other, thus having the function of a digital duplicating machine. The digital scanner 1 has an EEPROM 18 , and the digital printer 2 has an NVRAM 25 , which are nonvolatile memories.
[0104] The image forming apparatus of the present embodiment is different from those of the previous embodiments in the aspect that corrections to the original values of the characteristic parameters of the digital scanner 1 are stored in the NVRAM 25 .
[0105] [0105]FIGS. 8A and 8B are views of memory maps of the EEPROM 18 and NVRAM 25 of the image forming apparatus according to the fourth embodiment of the present invention.
[0106] As illustrated in FIG. 8A, in the EEPROM 18 , for example, a header 31 is allocated in a region of a few bytes located from the address 0000H, and a data region 32 is allocated next to the header 31 to store the characteristic parameters of the digital scanner 1 .
[0107] Similarly, as illustrated in FIG. 8B, in the NVRAM 25 , for example, a header 41 is allocated in a region of a few bytes located from the address 0000H, and a data region 44 is allocated next to the header 41 to store the corrections to the original values of the characteristic parameters of the digital scanner 1 . Furthermore, a data region 43 is allocated next to the data region 44 for storing the characteristic parameters of the digital printer 2 .
[0108] In the fabrication process of the digital scanner 1 , the characteristic parameters of the digital scanner 1 are stored in the data region 32 , and the initial values of the parameters are stored in the header 31 in the EEPROM 18 .
[0109] Similarly, in the fabrication process of the digital printer 2 , the characteristic parameters of the digital printer 2 are stored in the data region 43 , and the initial values of the parameters are stored in the header 41 in the NVRAM 25 . The initial values of the data region 44 are zero.
[0110] [0110]FIG. 9 is a flow chart showing an example of the operation of the image forming apparatus according to the fourth embodiment of the present invention. Specifically, FIG. 9 shows the procedure for adjusting values of the parameters of the digital scanner 1 when the digital scanner 1 is connected to the digital printer 2 as an option after the digital scanner 1 and the digital printer 2 are shipped and in distribution.
[0111] As illustrated in FIG. 9, in step S 91 , a user or a service person operates a panel on the digital printer 2 to select a mode for adjusting the values of the characteristic parameters of the digital scanner 1 . Upon that, the CPU 22 receives a signal from the panel indicating selection of the adjustment mode, and based on the signal, the CPU 22 displays a menu on the panel, allowing adjustment of the values of the characteristic parameters of the digital scanner 1 .
[0112] In step S 92 , on the panel, the user or the service person selects a parameter of the digital scanner 1 which is to be adjusted.
[0113] In step S 93 , the CPU 22 receives a signal from the panel indicating selection of the desired parameter, and based on the signal, the CPU 22 , via the controller 11 , reads the selected parameter from the data region 32 of the EEPROM 18 , in which the parameters of the digital scanner 1 are stored. In addition, the CPU 22 reads the correction to the original value of the selected parameter from the data region 44 of the NVRAM 25 , and makes calculations using the original value of the selected parameter and the correction to the original value, and the result is used as the present value of the selected parameter. Then the CPU 22 displays the present value of the selected parameter on the panel.
[0114] Here, the calculation made by the CPU 22 may be the summation of the original value of the selected parameter stored in the EEPROM 18 and the correction to the original value of the selected parameter stored in NVRAM 25 , this sum giving the present value of the selected parameter.
[0115] In step S 94 , the user or the service person inputs a new value of the selected parameter of the digital scanner 1 on the panel.
[0116] In step S 95 , the CPU 22 calculates the difference between the new value of the selected parameter input from the panel and the value of the selected parameter stored in the EEPROM 18 , and stores the difference in the RAM 24 temporarily as the correction.
[0117] In step S 96 , the user or the service person is required to confirm that the change of the value of the selected parameter will really be made.
[0118] In step S 97 , when it is confirmed that the change is to be made, the CPU 22 reads the correction to the parameter temporarily saved in the RAM 24 , and writes the value of the correction to the corresponding address in the data region 44 of the NVRAM 25 .
[0119] In step S 98 , after all desired parameters are adjusted in the same way following the above steps S 91 through S 97 , the user or the service person is required to make confirmation again, and the adjustment of the characteristic parameters of the digital scanner 1 is completed after the confirmation.
[0120] Because of the above adjustments, when adjusting the characteristic parameters of the digital scanner 1 which is connected to the digital printer 2 to realize the function of a digital duplicating machine after the digital scanner 1 and the digital printer 2 are shipped and in distribution, it is not necessary to modify the original values of the characteristic parameters of the digital scanner 1 determined in the factory, but just store the corrections to the original values in the NVRAM 25 of the digital printer 2 . Therefore it is possible to maintain compatibility even when the digital scanner 1 is changed. Further, it is not necessary to adjust again the values of the characteristic parameters of the digital scanner 1 , and the values of the characteristic parameters determined previously based on the combination of the digital printer 2 and the former digital scanner 1 are still usable.
[0121] According to the present embodiment, in a digital duplicating machine including the digital scanner 1 and the digital printer 2 that are connected to each other, because only the corrections to the original values are stored in the NVRAM 25 of the digital printer 2 , the performance of the digital scanner 1 is ensured. Furthermore, because values of the characteristic parameters determined in the factory are stored in the EEPROM 18 of the digital scanner 1 , compatibility of the digital scanner 1 is ensured even when a different digital scanner is connected to the digital printer 2 .
[0122] Fifth Embodiment
[0123] The image forming apparatus of the present embodiment has the same configuration as that described in the first embodiment with reference to FIG. 1. That is, using the same numeral references as in the first embodiment for the same components, the image forming apparatus of the present embodiment includes a digital scanner 1 and a digital printer 2 connected to each other, thus having the function of a digital duplicating machine. The digital scanner 1 has an EEPROM 18 , and the digital printer 2 has an NVRAM 25 , which are nonvolatile memories.
[0124] However, the image forming apparatus of the present embodiment is different from those of the previous embodiments in the aspect that both the original values and the corrections to the original values of the characteristic parameters of the digital scanner 1 are stored in the NVRAM 25 .
[0125] [0125]FIGS. 10A and 10B are views of memory maps of the EEPROM 18 and NVRAM 25 , respectively, of the image forming apparatus according to the fifth embodiment of the present invention.
[0126] As illustrated in FIG. 10A, in the EEPROM 18 , for example, a header 31 is allocated in a region of a few bytes located from the address 0000H, and a data region 32 is allocated next to the header 31 to store the characteristic parameters of the digital scanner 1 .
[0127] Similarly, as illustrated in FIG. 10B, in the NVRAM 25 , for example, a header 41 is allocated in a region of a few bytes located from the address 0000H, and data regions 42 , 44 , and 43 are allocated next to the header 41 in order. The data regions 42 and 44 are used to store the original values and the corrections to the original values, respectively, of the characteristic parameters of the digital scanner 1 . The data region 43 is used to store the characteristic parameters of the digital printer 2 .
[0128] In the fabrication process of the digital scanner 1 , the characteristic parameters of the digital scanner 1 are stored in the data region 32 , and the initial values of the parameters are stored in the header 31 in the EEPROM 18 .
[0129] Similarly, in the fabrication process of the digital printer 2 , the characteristic parameters of the digital printer 2 are stored in the data region 43 , and the initial values of the parameters are stored in the header 41 in the NVRAM 25 . The initial values of the data region 44 are zero. In addition, the initial values of the characteristic parameters of the digital scanner 1 are stored in the data region 42 when the digital printer 2 is fabricated, and when the digital scanner 1 is connected to the digital printer 2 , data of the characteristic parameters of the digital scanner 1 stored in the data region 32 of the EEPROM 18 are transferred to the data region 42 , as described in the second embodiment.
[0130] [0130]FIG. 11 is a flow chart showing an example of the operation of the image forming apparatus according to the fifth embodiment of the present invention. Specifically, FIG. 11 shows the procedure for adjusting values of the parameters of the digital scanner 1 when the digital scanner 1 is connected to the digital printer 2 as an option after the digital scanner 1 and the digital printer 2 are shipped and in distribution.
[0131] As illustrated in FIG. 11, in step S 111 , a user or a service person operates a panel on the digital printer 2 to select a mode for adjusting the values of the characteristic parameters of the digital scanner 1 . Upon that, the CPU 22 receives a signal from the panel indicating selection of the adjustment mode, and based on the signal, the CPU 22 displays a menu on the panel, allowing adjustment of the values of the characteristic parameters of the digital scanner 1 .
[0132] In step S 112 , on the panel, the user or the service person selects a parameter of the digital scanner 1 which is to be adjusted.
[0133] In step S 113 , the CPU 22 receives a signal from the panel indicating selection of the desired parameter, and based on the signal, the CPU 22 reads the selected parameter from the data region 42 of the NVRAM 25 , in which the parameters of the digital scanner 1 are stored, and reads the correction to the original value of the selected parameter from the data region 44 of the NVRAM 25 . The CPU 22 makes calculations using the original value of the selected parameter and the correction to the original value, and the result is used as the present value of the selected parameter. Then the CPU 22 displays the present value of the selected parameter on the panel.
[0134] For example, the calculation made by the CPU 22 may be the summation of the original value of the selected parameter stored in the data region 42 and the correction to the original value of the selected parameter stored in the data region 44 of the NVRAM 25 , this sum giving the present value of the selected parameter.
[0135] In step S 114 , the user or the service person inputs a new value of the selected parameter of the digital scanner 1 on the panel.
[0136] In step S 115 , the CPU 22 calculates the difference between the new value of the selected parameter input from the panel and the value of the selected parameter stored in the data region 42 of the NVRAM 25 , and stores the difference in the RAM 24 temporarily as the correction.
[0137] In step S 116 , the user or the service person is required to confirm that the change of the value of the selected parameter will really be made.
[0138] In step S 117 , when it is confirmed that the change is to be made, the CPU 22 reads the correction to the parameter temporarily saved in the RAM 24 , and writes the value of the correction to the corresponding address in the data region 44 of the NVRAM 25 .
[0139] In step S 118 , after all desired parameters are adjusted in the same way following the above steps S 111 through S 117 , the user or the service person is required to make confirmation again, and the adjustment of the characteristic parameters of the digital scanner 1 is completed after the confirmation.
[0140] Because of the above adjustments, when the digital printer 2 and the digital scanner 1 are connected to realize the function of a digital duplicating machine, it is possible to perform memory management for both the digital printer 2 and the digital scanner 1 on the digital printer 2 side.
[0141] According to the present embodiment, in a digital duplicating machine including the digital scanner 1 and the digital printer 2 that are connected toh each other, when the characteristic parameters of the digital scanner 1 are modified, because only the corrections to the original values are stored in the NVRAM 25 of the digital printer 2 , the performance of the digital scanner 1 is ensured, and because values of the characteristic parameters determined in the factory are stored in the EEPROM 18 of the digital scanner 1 and the NVRAM 25 , compatibility of the digital scanner 1 is ensured even when the digital scanner is connected to a different digital printer 2 .
[0142] Sixth Embodiment
[0143] The image forming apparatus of the present embodiment has the same configuration as that described in the first embodiment with reference to FIG. 1. That is, using the same numeral references as in the first embodiment for the same components, the image forming apparatus of the present embodiment includes a digital scanner 1 and a digital printer 2 connected to each other, thus having the function of a digital duplicating machine. The digital scanner 1 has an EEPROM 18 , and the digital printer 2 has an NVRAM 25 , which are nonvolatile memories.
[0144] However, the image forming apparatus of the present embodiment is different from those of the previous embodiments in the aspect that the original values and the corrections to the original values of the characteristic parameters of the digital scanner 1 are stored in both the EEPROM 18 and the NVRAM 25 .
[0145] [0145]FIGS. 12A and 12B are views of memory maps of the EEPROM 18 and NVRAM 25 of the image forming apparatus according to the sixth embodiment of the present invention.
[0146] As illustrated in FIG. 12A, in the EEPROM 18 , for example, a header 31 is allocated in a region of a few bytes located from the address 0000H, and a data region 32 is allocated next to the header 31 to store the original values of the characteristic parameters of the digital scanner 1 . Furthermore, a data region 33 is allocated next to the data region 32 to store the corrections to the original values of the characteristic parameters of the digital scanner 1 .
[0147] Similarly, as illustrated in FIG. 12B, in the NVRAM 25 , for example, a header 41 is allocated in a region of a few bytes located from the address 0000H, and data regions 42 , 44 , and 43 are allocated next to the header 41 in order. The data regions 42 and 44 are used to store the original values and the corrections to the original values, respectively, of the characteristic parameters of the digital scanner 1 ; the data region 43 is used to store the characteristic parameters of the digital printer 2 .
[0148] In the fabrication process of the digital scanner 1 , the characteristic parameters of the digital scanner 1 are stored in the data region 32 , and the initial values of the parameters are stored in the header 31 in the EEPROM 18 . The initial values of the data region 33 are zero.
[0149] Similarly, in the fabrication process of the digital printer 2 , the characteristic parameters of the digital printer 2 are stored in the data region 43 , and the initial values of the parameters are stored in the header 41 in the NVRAM 25 . The initial values of the data region 44 are zero. In addition, the initial values of the characteristic parameters of the digital scanner 1 are stored in the data region 42 when the digital printer 2 is shipped, and when the digital scanner 1 is connected to the digital printer 2 , data of the characteristic parameters of the digital scanner 1 stored in the data region 32 of the EEPROM 18 are transferred to the data region 42 , as described in the second embodiment.
[0150] [0150]FIG. 13 is a flow chart showing an example of the operation of the image forming apparatus according to the fifth embodiment of the present invention. Specifically, FIG. 13 shows the procedure for adjusting values of the parameters of the digital scanner 1 when the digital scanner 1 is connected to the digital printer 2 as an option after the digital scanner 1 and the digital printer 2 are shipped and in distribution.
[0151] As illustrated in FIG. 13, in step S 131 , a user or a service person operates a panel on the digital printer 2 to select a mode for adjusting the values of the characteristic parameters of the digital scanner 1 . Upon that, the CPU 22 receives a signal from the panel indicating selection of the adjustment mode, and based on the signal, the CPU 22 displays a menu on the panel, allowing adjustment of the values of the characteristic parameters of the digital scanner 1 .
[0152] In step S 132 , on the panel, the user or the service person selects a parameter of the digital scanner 1 which is to be adjusted.
[0153] In step S 133 , the CPU 22 receives a signal from the panel indicating selection of the desired parameter, and based on the signal, the CPU 22 reads the selected parameter from the data region 42 of the NVRAM 25 , in which the parameters of the digital scanner 1 are stored, and reads the correction to the original value of the selected parameter from the data region 44 of the NVRAM 25 . The CPU 22 makes calculations using the original value of the selected parameter and the correction to the original value, and the result is used as the present value of the selected parameter. Then the CPU 22 displays the present value of the selected parameter on the panel.
[0154] For example, the calculation made by the CPU 22 may be the summation of the original value of the selected parameter stored in the data region 42 and the correction to the original value of the selected parameter stored in the data region 44 of the NVRAM 25 , this sum giving the present value of the selected parameter.
[0155] In step S 134 , the user or the service person inputs a new value of the selected parameter of the digital scanner 1 on the panel.
[0156] In step S 135 , the CPU 22 calculates the difference between the new value of the selected parameter input from the panel and the value of the selected parameter stored in the data region 42 of the NVRAM 25 , and temporarily stores the difference in the RAM 24 as the correction to the parameter.
[0157] In step S 136 , the user or the service person is required to confirm that the change of the value of the selected parameter will really be made.
[0158] In step S 137 , when it is confirmed that the change is to be made, the CPU 22 reads the correction to the parameter temporarily saved in the RAM 24 , and writes the value of the correction to the corresponding address in the data region 44 of the NVRAM 25 , and to the corresponding address in the data region 33 of the EEPROM 18 .
[0159] In step S 138 , after all desired parameters are adjusted in the same way following the above steps S 131 through S 137 , the user or the service person is required to make confirmation again, and the adjustment of the characteristic parameters of the digital scanner 1 is completed after the confirmation.
[0160] Because of the above adjustments, when the digital printer 2 and the digital scanner 1 are connected to realize the function of a digital duplicating machine, because the corrections to the characteristic parameters of the digital scanner 1 are stored in both the digital scanner 1 and the digital printer 2 , it is possible to maintain compatibility even when either the digital scanner 1 or the digital printer 2 is changed.
[0161] According to the present embodiment, when a digital scanner 1 is newly connected to the digital printer 2 , because the data of the characteristic parameters of the digital scanner 1 are stored in the NVRAM 25 of the digital printer 2 , memory management for the digital printer 2 and the digital scanner 1 can be performed on the side of the digital printer 2 . In addition, when the values of the parameters of the digital scanner 1 are modified, because the corrections to the original values can be stored in both the NVRAM 25 of the digital printer 2 and the EEPROM 18 of the digital scanner 1 , the performance of the digital scanner 1 is ensured. Furthermore, because values of the characteristic parameters of the digital scanner 1 determined in the factory are stored in the EEPROM 18 of the digital scanner 1 , compatibility of the digital scanner 1 is ensured even when the digital scanner is connected to a different digital printer 2 . In addition, new adjustment of the parameters of the digital scanner 1 is not needed even if a digital scanner 1 is newly connected to a digital printer 2 .
[0162] While the present invention has been described with reference to specific embodiments chosen for purpose of illustration, it should be apparent that the invention is not limited to these embodiments, but numerous modifications could be made thereto by those skilled in the art without departing from the basic concept and scope of the invention.
[0163] For example, the present invention is applicable to any kind of image forming apparatus, such as a fax machine as well as a digital printer, to which a digital scanner can be connected when necessary.
[0164] Summarizing the effect of the present invention, because the digital printing device and the digital scanning device are equipped with nonvolatile memories, the functions of a digital duplicating machine can be realized by connecting the digital scanning device to the digital printing device even when the devices are in distribution after their shipment.
[0165] In addition, because the data of the characteristic parameters of the digital scanning device are stored in the nonvolatile memory of the digital printing device, memory management for the two devices can be performed on the side of the digital printing device, and the performance of the digital scanning device is ensured. In addition, compatibility of the performance of the digital scanning device is ensured even when a different digital scanner is connected to the digital printer 2 .
[0166] In addition, compatibility of the performance of the digital scanning device is ensured even when a different digital scanning device is newly connected to a different digital printing device, or when the digital scanning device is connected to a different digital printing device.
[0167] Furthermore, it is not necessary to adjust values of the characteristic parameters of the digital scanning device, even when the digital scanning device is newly connected to the digital printing device.
[0168] This patent application is based on Japanese priority patent application No. 2002-193658 filed on Jul. 2, 2002, the entire contents of which are hereby incorporated by reference.
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There is provided an image forming apparatus including a digital printing device that prints an image according to image signals and a digital scanning device, connectable to the digital printing device, that scans an image and converts the image into electric signals. The digital printing device includes a first nonvolatile memory for storing first parameters that optimize performance of the digital printing device. The digital scanning device includes a second nonvolatile memory for storing second parameters that optimize performance of the digital scanning device. The digital printing device includes a section for modifying the second parameters when the digital scanning device is connected to the digital printing device.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to and the benefit of the filing date of PCT Application No. PCT/EP2007/006736, filed Jul. 30, 2007 and European Patent Application No. EP 06 425 539.1, filed Jul. 28, 2006, which are each hereby incorporated by reference in their entirety.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to reflective (mirror based) optics, and more particularly to multi-reflection optical systems and their fabrication.
[0003] A well known optical design for X-ray applications is the type I Wolter telescope. The optical configuration of type I Wolter telescopes consists of nested double-reflection mirrors operating at grazing incidence angles low enough to assure high reflectivity from the coating material, normally gold. In type I Wolter mirrors, the X-ray radiation from distant sources is first reflected by a parabolic surface and then by a hyperboloid, both with cylindrical symmetry around the optical axis.
[0004] More recently, a variation of the type I Wolter design already proposed for other applications, in which the parabolic surface is replaced by an ellipsoid, has found application for collecting the radiation at 13.5 nm emitted from a small hot plasma used as a source in Extreme Ultra-Violet (EUV) microlithography, currently considered a promising technology in the semiconductor industry for the next generation lithographic tools. Here, there is a performance requirement to provide a near constant radiation energy density or flux across an illuminated silicon wafer target at which an image is formed. The hot plasma in EUV lithography source is generated by an electric discharge (Discharge Produced Plasma or DPP source) or by a laser beam (Laser Produced Plasma or LPP source) on a target consisting of Lithium, Xenon, or Tin, the latter apparently being the most promising. The emission from the source is roughly isotropic and, in current DPP sources, is limited by the discharge electrodes to an angle of about 60° or more from the optical axis. EUV lithography systems are disclosed, for example, in US2004/0265712A1 entitled “Detecting Erosion In Collector Optics With Plasma Sources In Extreme Ultraviolet (EUV) Lithography Systems”, US2005/0016679A1 entitled “Plasma-based debris mitigation for extreme ultraviolet (EUV) light source” and US2005/0155624A1 entitled “Erosion mitigation for collector optics using electric and magnetic fields”.
[0005] The purpose of the collector in EUV sources is to transfer the largest possible amount of in-band power emitted from the plasma to the next optical stage, the illuminator, of the lithographic tool. The collector efficiency is defined as the ratio between the in-band power at the intermediate focus and the total in-band power radiated by the source in 2π sr. For a given maximum collection angle on the source side, the collector efficiency is mainly determined by the reflectivity of the coating on the optical surface of the mirrors.
[0006] A problem with known systems is that that collector efficiency is significantly lower than it might be since the reflectivity of the coating is not exploited in the most efficient way; any improvement in the collector efficiency is highly desirable.
[0007] A further problem is that, with the collector efficiencies available, there is imposed the need to develop extremely powerful sources, and to have high optical quality and stability in the collector.
[0008] A further problem is that, with the collector efficiencies available, the overall efficiency of the lithographic equipment may not be high enough to sustain high volume manufacturing and high wafer throughput.
[0009] A further problem is that the collector lifetime may be relatively short due to exposure to extremely powerful sources.
BRIEF DESCRIPTION OF THE INVENTION
[0010] The present invention seeks to address the aforementioned and other issues.
[0011] Various embodiments of the present invention find application in diverse optical systems, examples being collector optics for lithography, and telescope or imaging (e.g., X-ray) systems.
[0012] According to one aspect of various embodiments of the present invention there is provided a collector reflective optical system, in which radiation from a radiation source is directed to an image focus, comprising: one or more mirrors, the or each mirror being symmetric about an optical axis extending through the radiation source and the or each mirror having at least first and second reflective surfaces whereby, in use, radiation from the source undergoes successive grazing incidence reflections in an optical path at the first and second reflective surfaces; and wherein the at least first and second reflective surfaces are formed such that the angles of incidence of the successive grazing incidence reflections at the first and second reflective surfaces are substantially equal.
[0013] The angles of incidence of said successive grazing incidence reflections may be substantially equal for all rays incident on said reflective surfaces.
[0014] Each mirror may be formed as an electroformed monolithic component, and wherein the first and second reflective surfaces are each provided on a respective one of two contiguous sections of the mirror.
[0015] For each mirror, said at least first and second reflective surfaces may have figures, and positions and/or orientations relative to the optical axis whereby said angles of incidence are equal.
[0016] Moreover, in some embodiments for each mirror, the first reflective surface is nearest to the radiation source, and radiation from the second reflective surface is directed to the image focus on the optical axis; and wherein said first and second reflective surfaces are defined, for a given point of reflection at said reflective surfaces, by
[0000]
{
ρ
2
ρ
1
=
k
sin
-
4
(
θ
2
-
θ
1
4
)
ρ
1
-
ρ
2
=
2
c
cos
θ
2
-
cos
θ
1
cos
(
θ
1
-
θ
2
)
-
1
ρ
1
cos
θ
1
+
ρ
2
cos
θ
2
+
(
2
a
-
ρ
1
-
ρ
2
)
cos
(
θ
1
+
θ
2
2
)
=
2
c
[0017] where ρ 1 is the length from the source to the first reflective surface,
[0018] ρ 2 is the length from the image focus to the second reflective surface,
[0019] θ 1 is the angle between the optical axis and a line joining the source and a first point of reflection at the first reflective surface,
[0020] θ 2 is the angle between the optical axis and a line joining the image focus and a second point of reflection at the second reflective surface,
[0021] 2c is the length along the optical axis from the source to the image focus,
[0022] 2a is the constant length of the optical path, and
[0023] k is a constant.
[0024] The values of a and k may be determined by
[0000]
a
=
ρ
1
,
R
+
ρ
2
,
R
2
,
and
k
=
ρ
1
,
R
ρ
2
,
R
sin
4
(
θ
2
,
R
-
θ
1
,
R
4
)
[0000] where subscript “R” denotes values for the point of intersection R of the first and second reflective surfaces.
[0025] According to another aspect of various embodiments of the invention there is provided a collector optical system for EUV lithography, comprising the reflective optical system wherein radiation is collected from the radiation source.
[0026] According to another aspect of various embodiments of the invention there is provided an EUV lithography system comprising: a radiation source, for example a LPP source, the collector optical system; an optical condenser; and a reflective mask.
[0027] According to another aspect of various embodiments of the invention there is provided an imaging optical system for EUV or X-ray imaging, comprising the reflective optical system.
[0028] According to another aspect of various embodiments of the invention there is provided an EUV or X-ray imaging system, comprising: the imaging optical system; and an imaging device, for example a CCD array, disposed at the image focus.
[0029] According to another aspect of various embodiments of the invention there is provided an EUV or X-ray telescope system, comprising: the reflective optical system; wherein radiation from a source at infinity is reflected to the image focus.
[0030] In the EUV or X-ray telescope system, in some embodiments for each mirror, the first reflective surface is nearest to the radiation source, and radiation from the second reflective surface is directed to the image focus, and wherein the first and second reflective surfaces are defined, for a given point of reflection at said reflective surfaces, by
[0000]
{
ρ
1
+
ρ
3
cos
(
θ
2
/
2
)
=
2
c
-
ρ
2
cos
(
θ
2
)
ρ
1
+
ρ
3
=
2
a
-
ρ
2
[0031] where ρ 1 is the length from a reference plane to the first reflective surface,
[0032] ρ 2 is the length from the image focus to the second reflective surface,
[0033] ρ 3 is the length between the points of incidence at said first and second reflective surfaces,
[0034] θ 2 is the angle between the optical axis and a line joining the image focus and a second point of reflection at the second reflective surface,
[0035] 2c is the length along the optical axis from the source to the image focus,
[0036] 2a is the constant length of the optical path, and
[0037] k is a constant.
[0038] The values of a and k are more preferably determined by
[0000]
a
=
ρ
1
,
R
+
ρ
2
,
R
2
,
and
k
=
ρ
2
,
R
sin
4
(
θ
2
,
R
4
)
,
[0039] where subscript “R” denotes values for the point of intersection R of the first and second reflective surfaces.
[0040] According to another aspect of various embodiments of the invention there is provided an EUV or X-ray imaging system, comprising the EUV or X-ray telescope system, and an imaging device, for example a CCD array, disposed at the image focus.
[0041] In each of the aforementioned aspects of various embodiments of the invention, a plurality of minors may be provided in nested configuration.
[0042] Also, the two of more of the mirrors may each have a different geometry.
[0043] In addition, the mirrors may have mounted thereon, for example on the rear side thereof, one or more devices for the thermal management of the mirror, for example cooling lines, Peltier cells and temperature sensors.
[0044] The mirrors may have mounted thereon, for example on the rear side thereof, one or more devices for the mitigation of debris from the source, for example erosion detectors, solenoids and RF sources.
[0045] In accordance with various embodiments of the invention a two-reflection mirror for nested grazing incidence optics is provided, in which significantly improved overall reflectivity is achieved by making the two grazing incidence angles equal for each ray. The various embodiments of invention are applicable to non-imaging collector optics for Extreme Ultra-Violet microlithography where the radiation emitted from a hot plasma source needs to be collected and focused on the illuminator optics. The various embodiments of the invention are also described herein, embodied in a double-reflection mirror with equal reflection angles, for the case of an object at infinity, for use in X-ray applications.
BRIEF DESCRIPTION OF THE DRAWINGS
[0046] Embodiments of the invention will now be described in detail, by way of example, with reference to the accompanying drawings, in which:
[0047] FIG. 1 shows an example of a known EUV lithography system;
[0048] FIG. 2 shows the grazing incidence reflection in the collector optics of EUV lithography systems;
[0049] FIG. 3 depicts the conceptual optical layout of a known type I Wolter collector for EUV plasma sources;
[0050] FIG. 4 illustrates theoretical reflectivity of selected materials at 13.5 nm.
[0051] FIG. 5 shows geometry and conventions of the two-reflection mirror for EUV lithography applications, in accordance with one embodiment of the invention;
[0052] FIG. 6 shows the optical layout of a nested collector according to another embodiment of the invention;
[0053] FIG. 7 illustrates total reflectivity experienced by each ray as a function of the emission angle for the nested collector of FIG. 4 and for a type I Wolter design; and
[0054] FIG. 8 shows the geometry and conventions of the two-reflection mirror according to another embodiment of the invention, when the source focus is at infinity, for example in X-ray imaging applications.
DETAILED DESCRIPTION OF THE INVENTION
[0055] In the description and drawings, like numerals are used to designate like elements. Unless indicated otherwise, any individual design features and components may be used in combination with any other design features and components disclosed herein.
[0056] In the illustrations of optical elements or systems herein, unless indicated otherwise, cylindrical symmetry around the optical axis is assumed; and references to an “image focus” are references to an image focus or an intermediate focus.
[0057] In relation to the “substantially equal” grazing incidence angles in the fabricated mirrors, as used herein, this is to be interpreted as angles sufficiently similar as to result in enhanced collector efficiency, and more preferably significantly enhanced or maximized collector efficiency. While in no way limiting, it is to be interpreted as angles that differ by 10% or less, or by 5% or less, and even by 1% or less. The angles may be identical, but is not required.
[0058] Various embodiments of the invention may provide the collection efficiency that is improved and/or maximized. Various embodiments of the invention also may relax the effort in developing extremely powerful sources, improving the optical quality and stability of the collector output and increasing the collector lifetime. Various embodiments of the invention additionally may increase overall efficiency of the lithographic equipment, allowing higher wafer throughput.
[0059] FIG. 1 shows an example of a known EUV lithography system. The system 100 includes a laser 110 , a laser-produced plasma 120 , an optical condenser 130 , an optical collector 131 , an erosion detector 135 , a reflective mask 140 , a reduction optics 150 , and a wafer 160 . Alternatively, the laser 100 and the laser produced plasma 120 can be replaced with an electric discharge source 150 .
[0060] The laser 110 generates a laser beam to bombard a target material like liquid filament Xe or Sn. This produces the plasma 120 with a significant broadband extreme ultra-violet (EUV) radiation. The optical collector 131 collects the EUV radiation from the plasma. After the collector optics, the EUV light is delivered to the mask through a number of mirrors coated with EUV interference films or multilayer (ML) coating. The laser-produced plasma can be replaced with the electric discharge source 150 to generate the EUV light. The Xe or Sn is used in the electric discharge source 150 . The optical condenser 130 illuminates the reflective mask 140 with EUV radiation at 13-14 nm wavelengths. The collector optics 131 and condenser optics 130 may include a ML coating. The optical collectors 131 may be eroded over time for being exposed to the plasma 120 . The optical collectors 131 include circuitry or interface circuits to the erosion detector 135 . The erosion detector 135 detects if there is an erosion in the single-layer or ML coating of the collectors 131 . By monitoring the erosion in the ML coating continuously, severe erosion may be detected and replacement of eroded collectors may be performed in a timely fashion.
[0061] The reflective mask 140 has an absorber pattern across its surface. The pattern is imaged at 4:1 demagnification by the reduction optics 150 . The reduction optics 150 includes a number of mirrors such as mirrors 152 and 154 . These mirrors are aspherical with tight surface figures and roughness (e.g., less than 3 Angstroms). The wafer 160 is resist-coated and is imaged by the pattern on the reflective mask 140 . Typically, a step-and-scan exposure is performed, i.e., the reflective mask 140 and the wafer 160 are synchronously scanned. Using this technique, a resolution less than 50 nm is possible.
[0062] FIG. 2 shows the grazing incidence reflection in the collector optics of EUV lithography systems, i.e. in a sectional view within an exemplary EUV chamber. The light source, in this case a discharge produced plasma (DPP) source 205 , and collector mirrors 210 for collecting and directing the EUV light 215 for use in the lithography chamber 105 are inside the EUV chamber. The collector mirrors 210 may have a nominally conical/cylindrical or elliptical structure.
[0063] Tungsten (W) or other refractory metals or alloys that are resistant to plasma erosion may be used for components in the EUV source. However, plasma-erosion may still occur, and the debris produced by the erosion may be deposited on the collector mirrors 210 . Debris may be produced from other sources, e.g., the walls of the chamber. Debris particles may coat the collector mirrors, resulting in a loss of reflectivity. Fast atoms produced by the electric discharge (e.g., Xe, Li, Sn, or In) may sputter away part of the collector mirror surfaces, further reducing reflectivity.
[0064] In certain circumstances, a magnetic field is created around the collector mirrors to deflect charged particles and/or highly energetic ions 220 and thereby reduce erosion. A magnetic field may be generated using a solenoid structure. This magnetic field may be used to generate Lorentz force when there is a charged particle traveling perpendicular or at certain other angles with respect to the magnetic field direction. By applying high current (I) and many loops around the ferromagnetic tube, a high magnetic field can be generated.
[0065] FIG. 3 depicts the conceptual optical layout of a known type I Wolter collector for EUV plasma sources. The purpose of the collector in EUV sources is to transfer the largest possible amount of in-band power emitted from the plasma to the next optical stage, the illuminator ( 130 ; FIG. 1 ), of the lithographic tool.
[0066] With reference to FIG. 3 , although many more nested mirrors in the collector optical system 300 may be illustrated, only two ( 302 , 304 ) are shown. The radiation from the source 306 is first reflected by the hyperbolic surfaces 308 , 310 , then reflected by the elliptical surfaces 312 , 314 , and finally focused to an image or intermediate focus 316 on the optical axis 320 . As in the type I Wolter telescope mentioned above, the elliptical ( 312 , 314 ) and the hyperbolic ( 308 , 310 ) surfaces share a common focus 318 . For each of the mirrors 302 , 304 , etc. the different sections on which the surfaces 308 , 312 are disposed may be integral, or may be fixed or mounted together.
[0067] The output optical specification of the collector 300 , in terms of numerical aperture and etendue, must match the input optical requirements for the illuminator ( 130 ; FIG. 1 ). The collector 300 is designed to have maximum possible efficiency, while matching the optical specification of the illuminator ( 130 ; FIG. 1 ) on one side and withstanding the thermal load and the debris from the plasma source 306 on the other side. Indeed, the power requirement for in-band radiation at the intermediate focus 316 has been seen to increase from the original 115 W towards 180 W and more, due to the expected increase in exposure dose required to achieve the desired resolution and line-width roughness of the pattern transferred onto the wafer ( 160 ; FIG. 1 ). Since the maximum conversion efficiency of both DPP and LPP sources is limited to a few percent, and since the reflectivity of normal incidence mirrors in the illuminator 130 and the projection optics box can not exceed about 70%, for each of the 6-8 mirrors or more along the optical path to the plane of the wafer 160 , the collector 300 must withstand thermal loads in the range of several kilowatts. Deformations induced by such high thermal loads on the thin metal shell of which the mirrors 302 , 304 are made may jeopardize the stability and the quality of the output beam of the collector 300 even in presence of integrated cooling systems on the back surface of the mirrors.
[0068] It is apparent from the foregoing that any improvement in the collector efficiency has benefits for relaxing the need for developing extremely powerful sources, for increasing the wafer throughput of the lithographic equipment, and for improving the optical quality and stability of the collector output, as well as the benefit of increasing the collector lifetime.
[0069] FIG. 4 illustrates theoretical reflectivity of selected materials at 13.5 nm, i.e. some example of the dependence of the reflectivity on the grazing incidence angle for some selected materials at a wavelength of 13.5 nm. For a given maximum collection angle on the source side, the collector efficiency is mainly determined by the reflectivity of the coating on the optical surfaces 308 - 314 of the mirrors 302 , 304 . Since each ray experiences two reflections, the overall reflectivity is given by the product of the reflectivity of each of the two reflections.
[0070] FIG. 5 shows geometry and conventions of the two-reflection mirror 302 for EUV lithography applications, in accordance with one embodiment of the invention. Although many more nested mirrors in the collector optical system may be illustrated, only one ( 302 ) is shown. The design according to various embodiments of the invention is based on the discovery that the overall reflectivity is maximized when, for all rays, the two grazing incidence angles, and thus the reflectivity of the two reflections, are equal, at least for the kind of dependence on the grazing incidence angle shown in FIG. 4 . This condition cannot be satisfied for all rays in a type I Wolter design. Indeed, in the latter, for each mirror, the two grazing incidence angles can be made equal for one ray at most.
[0071] In accordance with various embodiments of the invention, double-reflection collector mirrors 302 , 304 are provided, in which the above condition (equal grazing incidence angle) is satisfied for all rays collected by each mirror 302 , 304 . A very brief theoretical treatment and the description of the design is given hereinafter, as is a comparison of the expected efficiency of a nested collector 300 according to embodiments of the invention to the efficiency of type I Wolter collector. Although Abbe's condition is not satisfied in the collector according to an embodiment of the invention, coma aberration is of concern only to the extent it affects the collector efficiency. Due the finite size of the plasma source and possibly the shape errors of the collector mirrors, the relative contribution of coma aberration is considered negligible.
Mirror Surface Shapes
[0072] Various embodiments of the present invention employ, in the reflective surfaces of the mirrors, certain shapes/geometries in order to enhance performance; and in order that the mathematical definitions of these geometries may be better understood, the parameters and notation used in those representations will be briefly addressed below.
[0073] In the geometry shown in FIG. 5 , a ray emitted from the object or source focus S (i.e. plasma source 306 ) is reflected at point P on the first surface 308 , reflected at point Q on the second surface 312 and finally focused to the image or intermediate focus IF ( 316 ). Symmetry around the optical axis 320 is assumed. The positions of the source 306 and the image focus 316 define the vector 2c=IF−S of length 2c. The ray path is described by the three adjacent vectors ρ 1 u 1 =P−S, p 2 u 2 =IF−Q, and ρ 3 u 3 =Q−P of length ρ 1 , ρ 2 , and ρ 3 , respectively. The direction of each vector is defined by the unit vectors u 1 , u 2 , and u 3 forming angles θ 1 , θ 2 , and θ 3 measured counterclockwise with respect to the optical axis 320 . If three vectors ρ 1 u 1 , ρ 2 u 2 , and ρ 3 u 3 are assigned as functions of a parameter t, the geometry of the cross sections of the two surfaces 308 , 312 is defined with respect to S by the tips of the vectors ρ 1 u 1 and ρ 1 u 1 +ρ 3 u 3 .
[0074] In accordance with embodiments of the invention, the three vectors p 1 u 1 , p 2 u 2 , and p 3 u 3 satisfy the following relation
[0000] ρ 1 u 1 +ρ 2 u 2 +ρ 3 u 3 =2 c. (1)
[0075] In addition, in order for a spherical wave emitted from the source S ( 306 ) and reflected by the two surfaces 308 , 312 to be focused to the image focus IF ( 316 ), the optical path is the same for all the rays. In accordance with embodiments of the invention, if 2a is the constant length of the optical path, then
[0000] ρ 1 +ρ 2 +ρ 3 =2 a. (2)
[0076] Finally, using the reflection conditions at point P and Q (the points of reflection at the surfaces 308 and 312 , respectively) and the fact that, in accordance with embodiments of the invention, the two grazing incidence angles ψ 13 =(θ 1 −θ 3 )/2ψ 23 =(θ 3 −θ 2 )/2 are equal, i.e.
[0000] θ 1 −θ 3 =θ 3 −θ 2
[0000] enables the geometry of the mirrors (reflective surfaces) in accordance with embodiments of the invention, to be defined. More specifically, the following system is employed in accordance with embodiments of the invention.
[0000]
{
ρ
2
ρ
1
=
k
sin
-
4
(
θ
2
-
θ
1
4
)
ρ
1
-
ρ
2
=
2
c
cos
θ
2
-
cos
θ
1
cos
(
θ
1
-
θ
2
)
-
1
ρ
1
cos
θ
1
+
ρ
2
cos
θ
2
+
(
2
a
-
ρ
1
-
ρ
2
)
cos
(
θ
1
+
θ
2
2
)
=
2
c
(
4
)
[0077] If θ 1 , a, c, k are given, these are 3 equations in 3 unknowns ρ 1 , ρ 2 and θ 2 that can be solved numerically. The resulting profile (mirror figure or geometry) is then rotated around the optical axis 320 to obtain the axial symmetric two-surfaces mirror 302 . The surfaces 308 , 312 defined by (4) cannot be described by second order algebraic equations. In particular, these surfaces 308 , 312 are not generated by conic sections and do not have a common focus, as happens in two-reflection systems consisting of ellipsoids and/or hyperboloids.
[0078] The values θ 1,R and |θ 2,R | of the angles θ 1 and ∥θ 2 | at the intersection point R are the minimum angles at both the source 306 and the image focus 316 . Since ρ 3 =0 at R, assuming that c is assigned, the length ρ 1,R and ρ 2,R are known and the constants a and k are determined by relation (2) and (4a)
[0000]
a
=
ρ
1
,
R
+
ρ
2
,
R
2
,
(
5
)
k
=
ρ
1
,
R
ρ
2
,
R
sin
4
(
θ
2
,
R
-
θ
1
,
R
4
)
.
(
6
)
[0079] When θ 1 is allowed increase from its minimum value θ 1,R , relations (4) give the shape of both surfaces 308 , 312 of the mirror 302 . The maximum value of θ 1 is arbitrary to a certain extent. A convenient choice is such that the minimum distance of the mirror 302 from the source 306 is some prescribed value ρ 1 so that a spherical region of radius ρ 1 around the source 306 is left free for the hardware required to mitigate the debris from the plasma source 306 . Alternatively, in order to ease the mounting of the mirror on a common supporting structure, the maximum value for θ 1 can be is chosen such that all the mirrors end at the same horizontal coordinate on side of the image focus 316 .
[0080] The figures/geometries of the outer mirrors 304 , etc. (see FIG. 6 ), are calculated iteratively as follows. The vertex R′ of the second mirror 304 ( FIG. 6 ) is defined by the intersection of the rays through points A and B. These rays also define the minimum values θ 1,R′ and θ 2,R′ of the angles θ 1 and |θ 2 | and the corresponding length of ρ 1,R′ and ρ 2,R′ . The above procedure can then be applied to calculate the new constant values a′ and k′ from (5) and (6) and the mirror shape from (4). The process can then be iterated to cover the desired numerical aperture with a proper number of nested mirrors.
[0081] FIG. 6 shows the optical layout of a nested collector 300 according to another embodiment of the invention. This is the same as the above-described embodiment, except as described hereinafter. The nested collector 300 consists of 15 double-reflection mirrors ( 302 , 304 , etc.) with a thickness of 2 mm. In this case, there is a focal length 2c of 1500 mm, a minimum distance ρ 1 between the optics 300 and the source focus 306 of 110 mm and a minimum and maximum angles of the radiation at the intermediate focus 316 of 1.5° and 8°, respectively. The corresponding minimum and maximum collected angles are 9.2° and 86.8°, equivalent to 5.3 sr (taking into account the obscurations from the mirror thickness). As mentioned hereinbefore, the collection efficiency of the collector is defined as the ratio between the power at the image or intermediate focus and the power emitted from the source in 2π sr. For an isotropic point source, the collection efficiency of each mirror 302 , 304 , etc. is given by
[0000]
η
=
∫
θ
1
,
R
θ
1
,
A
R
(
ψ
13
)
R
(
ψ
23
)
sin
θ
1
θ
1
=
∫
θ
1
,
R
θ
1
,
A
R
2
(
θ
1
-
θ
2
(
θ
1
)
4
)
sin
θ
1
θ
1
,
(
7
)
[0000] where R(ψ) is the mirror reflectivity at the grazing incidence angle ψ. Assuming a reflective coating of Ruthenium with theoretical reflectivity, the total collection efficiency for the collector in FIG. 6 is 50.9%. This value should be compared with the calculated efficiency of 40.1% for a reference collector design based on a type I Wolter configuration matching the same boundary conditions in terms of focal length, angles at the intermediate focus and maximum collected angle.
[0082] In accordance with embodiments of the invention, the manufacturing process for fabrication of each of the nested grazing incidence mirrors 302 (as well as the outer mirrors 304 , etc.; see FIG. 6 ), of the assembly of nested mirrors as a whole, is based on electroforming, whereby the mirror 302 , 304 , etc. is obtained by galvanic replication from a negative master (not shown). In this case, it is appropriate to extend the two sections of the mirror providing the two reflecting surfaces 308 , 312 until they join at a given point (R). In this way, the two sections of the mirror are manufactured in a monolithic structure, thus avoiding the need for further relative alignment. Techniques for the manufacture of mirrors by electroforming are disclosed in, for example, EP-A-1329040, entitled “Telescope Mirror For High Bandwidth Free Space Optical Data Transmission” and WO2005/054547, entitled “Fabrication Of Cooling And Heat Transfer Systems By Electroforming”.
[0083] FIG. 7 illustrates total reflectivity experienced by each ray as a function of the emission angle for the nested collector 300 of FIG. 6 and for a type I Wolter design. The nested collector 300 according to embodiments of the invention is more effective than the type I Wolter design, at least at large emission angles. As the inner mirrors collect a small angular range, the gain in reflectivity at lower emission angles is more limited.
[0084] FIG. 8 shows the geometry and conventions of the two-reflection mirror according to another embodiment of the invention, when the source focus is at infinity, for example in EUV or X-ray imaging applications. The design is similar to the above-described embodiment, and so will be briefly discussed. In this case u 1 is parallel to the optical axis 320 and θ 1 =0, as shown in FIG. 8 . Only the projection of equation (1) on the optical axis 320 is applicable,
[0000] ρ 1 +ρ 2 u 1 ·u 2 +ρ 3 u 1 ·u 3 =2 c. (8)
[0085] Instead, equation (2) is still valid.
[0086] In accordance with embodiments of the invention, with the two grazing incidence angles ψ 13 =θ 3 /2 and ψ 23 =(θ 3 −θ 2 )/2 being equal, gives θ 3 =θ 2 /2. Using the reflection conditions at point P and Q in FIG. 8 , with θ 2 is chosen as the independent variable, in accordance with embodiments of the invention, the geometries of the reflective surfaces are defined by
[0000]
{
ρ
1
+
ρ
3
cos
(
θ
2
/
2
)
=
2
c
-
ρ
2
cos
(
θ
2
)
ρ
1
+
ρ
3
=
2
a
-
ρ
2
(
9
)
[0087] As before, with c assigned, the constants a and k are determined in accordance with embodiments of the invention, once the minimum value |θ 2,R | of the angle of |θ 2 | at point R is given, by
[0000]
a
=
ρ
1
,
R
+
ρ
2
,
R
2
,
(
10
)
k
=
ρ
2
,
R
sin
4
(
θ
2
,
R
4
)
.
(
11
)
[0088] The process for the determination of the first 302 and subsequent (not shown) mirrors is then identical to that described for the collector 300 in the embodiment of FIG. 5 .
[0089] In contrast with embodiments of the present invention, in double-reflection conical mirrors for X-ray telescopes, axial rays do not come to a point geometric focus and the optics is not corrected for on-axis spherical aberration.
[0090] The design of double-reflection mirrors 302 , 304 , etc. according to embodiments of the invention, with equal grazing incidence angles, is effective in increasing the efficiency of collectors for EUV microlithography, at least at large emission angles. The increasing demand for high power level needed for high volume manufacturing tools requires enhancing the performance of the subsystems to the physical limits. For collectors, this implies, among others, increasing the collected solid angle and improving the overall reflectivity. To this end, the collector optical systems according to the present invention have a collection efficiency 27% greater than a type I Wolter configuration for the selected reference specifications set out herein.
[0091] While the invention has been described in terms of various specific embodiments, those skilled in the art will recognize that the invention can be practiced with modification within the spirit and scope of the claims.
|
A reflective optical system, in which radiation from a radiation source is directed to an image focus or intermediate focus, including one or more mirrors (symmetric about the optical axis). Each mirror has at least first and second reflective surfaces, whereby radiation from the source undergoes successive grazing incidence reflections in an optical path at first and second reflective surfaces. The first and second reflective surfaces are formed such that the angles of incidence of the successive grazing incidence reflections at the first and second reflective surfaces are substantially equal. Each mirror may be formed as an electroformed monolithic component, wherein the first and second reflective surfaces are each provided on a respective one of two contiguous sections of the mirror. The reflective optical system may be embodied in a collector optical system for EUV lithography, or in an EUV or X-ray telescope or imaging optical system.
| 6
|
[0001] This application is a continuation of PCT International Application No. PCT/US2008/009986, filed Aug. 22, 2008, which claims the benefit of U.S. Provisional Application Ser. No. 60/965,762 filed on Aug. 22, 2007; U.S. Provisional Application Ser. No. 60/965, 732 filed on Aug. 22, 2007, U.S. Provisional Application Ser. No. 60/965, 746 filed on Aug. 22, 2007 and U.S. Provisional Application Ser. No. 60/993,113 filed on Sep. 10, 2007, all of which applications are incorporated herein by reference in their entirety.
STATEMENT REGARDING FEDERALLY-SPONSORED RESEARCH
[0002] The present invention was supported by grants from the National Institute of Health (NCRR/NIH), grant number P40-RR-017688. The U.S. Government may have certain rights to the present invention.
FIELD OF INVENTION
[0003] The present invention relates to animal studies and more particularly to systems, devices and apparatuses that are utilized during such studies in connection with feeding and studying animals. Such systems, apparatuses, and devices include for example, animal enclosures, sound attenuation chambers, olfactory discrimination systems and water feeders for animals within an animal enclosure.
BACKGROUND OF THE INVENTION
[0004] In general there are a number of areas in which animals, such as mice and rats, are used in connection with experimentation. Some examples include animal behavioral studies, clinical studies such as those to evaluate the effect and toxicity of new medicines, and carcinogenetic studies. The value of research using lab animals hinges on the ability to carry out the experiments in a tightly controlled environment. Diet, caging materials (e.g., cages and water bottles), and other environmental variables have the potential to create serious disruptions in animal studies.
[0005] In regards to animal enclosures, particularly those used in connection with animal behavioral studies, the enclosure is typically designed and constructed for a given application or one test scenario or one series of tests. Consequently, the enclosures tend to be expensive, generally difficult to modify after they are constructed, so they are not easily adaptable to other uses. In addition, such enclosures are typically designed for the size of the animal to be used for the particular test phase. Thus, there continues to be a need to develop animal enclosures that can be easily modified or adaptable for different uses as well as being of a design that allows the design to be scaled to the size of the animal for the intended use.
[0006] In animal testing, some animals show a particular sensitivity to ambient noise which can disrupt the testing program or provide a confounding factor(s). When one is working in a crowded laboratory or other such space, with multiple experiments and multiple animals, it can be extremely difficult to achieve conditions where the test animal(s) are not exposed to such external or ambient sounds/noise. Consequently, the animal may be located in a chamber that is configured to attenuate ambient noise. Also, as with the animal enclosures, conventional chambers are generally constructed for the intended test protocol and test animal. Thus, there continues to be a need for improvement to such chambers to improve on sound attenuation while not comprising the need for breathable air and for chambers that are easily designable and constructed for different size test animals.
[0007] Many tasks used in animal behavioral testing require complicated training procedures to teach the animal to perform responses that they are unfamiliar with. This training is a time consuming aspect of certain types of experiments and is often not of particular interest to the researcher in and of itself. One such type of experiments utilizes the natural propensity of rodents to investigate novel aspects of their environment using their sense of smell. In such, experiments, a rodent is exposed to the smell of a gas or the like having a particular odor or smell, which is then required to make a discrete behavioral response to such exposure. Conventional systems yield measures of behavior that are such as to be somewhat ambiguous. Also, conventional systems are cumbersome, not fully automated and have practical limits on the number of scents or smells limits that can be delivered and the speed on which such scents can be delivered and changed from one scent to another, as well as the adaptability of such systems to be easily modified to deliver other or different scents. Thus, there is a continuing need to develop olfactory types of system that take such advantage of the natural propensity of rodents to investigate novel aspects of their environment using their sense of smell which can provide measures of behavior that are less ambiguous than the measures yielded by conventional systems and which overcome all or most of the above-described shortcomings.
[0008] As indicated above, as part of animal experiments, it is frequently necessary to measure the amount of fluid (e.g., water) that an animal (e.g., mouse or rat) consumes over a short duration or the duration of the test protocol. Conventional products on the market, are not necessarily leak-proof which can lead to an over-estimation of the amount of fluid that was consumed. Also, such conventional products must be moved or disconnected from the enclosure and also can require that the product be turned over in order for the technician to be able to read or determine the amount of fluid that has been consumed by the animal. Thus, there continues to be a need for apparatuses or devices for delivering water that further minimize if not eliminate leakage thereby providing a device capable of making more accurate measurements of fluid consumption as well as devices that allow such measurements to be made without having to handle the device.
[0009] Some examples of prior art animal enclosures or cage systems are found in U.S. Pat. Nos. 3,397,676; 5,003,922 and 6,308,660. A cage for breeding experimental animals and a ventilation apparatus for a cage rack system is found in PCT Publication No. WO/02/1153. The PheComp system of Panlab is a conventional system that is configured for use in studying the compulsive food and drink behaviors in rodents.
[0010] It thus would be desirable to provide new systems, apparatuses and devices, as well as methods related thereto, for the care of experimental animals and testing or study of such experimental animals. It would be particularly desirable to provide an animal enclosure that can be easily modified or adapted for different uses as well as being of a design that allows the design to be scaled to the size of the animal in comparison to prior art devices. It would be particularly desirable to provide a sound attenuation chamber that improves on sound attenuation while not comprising the need for breathable air and for chambers that are easily designable and constructed for different size test animals in comparison to prior art chambers. It would be particularly desirable to provide an olfactory discrimination system that takes advantage of the natural propensity of rodents to investigate novel aspects of their environment using their sense of smell and which can provide measures of behavior that are less ambiguous than the measures yielded by prior art systems as well as overcoming a number of shortcomings of such prior art systems. It would be particularly desirable to provide an animal water delivery device or apparatus that is capable of making more accurate measurements of fluid consumption as compared to prior art devices as well as minimizing or eliminating the need to handle the device to make such measurements as is required with prior art devices. Such collection systems, apparatuses and devices preferably would be less costly than prior art devices and such methods would not require highly skilled users to utilize the device.
SUMMARY OF THE INVENTION
[0011] The present invention features various device, apparatuses and systems for use in connection with animal studies or experimentation as well as methods related thereto. Such devices, apparatuses and systems include a scalable animal enclosure that is easily customized for a given application; a scalable and easily customizable sound attenuation chamber that can be used with such an animal enclosure; an olfactory discrimination system which can quickly delivery an odor to an animal while minimizing the potential for ambient contamination and a leak-free water delivery device that provides a mechanism for the experimenter to determine water consumption without handling the device.
[0012] According to one aspect of the present invention, there is featured a scalable animal enclosure that includes a frame made up of a plurality of scalable frame members that are interconnected to each other and a plurality of wall members. Each of the plurality of scalable frame members include a connecting mechanism configured so as to releasably secure an end portion of an adjacent wall member. Each wall member is secured to an adjacent pair of wall members so as to thereby form a wall of the animal enclosure.
[0013] According to another aspect of the present invention there is featured, a sound attenuation chamber that includes a frame having a plurality of scalable frame members that are interconnected to each other; and a plurality of panel members. Each of the plurality of scalable frame members includes a connecting mechanism that is configured so as to secure an end portion of a panel member. Also, each of the plurality of panel members is configured so as to include a plurality of layers of materials having different densities that when attached to each other creates a panel that attenuates sound external to the chamber. In further embodiments, each of the plurality of panels is configured to include at least three layers of material, the density of each layer being different from the other layers.
[0014] According to another aspect of the present invention, there is featured an olfactory discrimination system for selectively exposing an animal to one of a plurality of odors at a time. Such a system includes an odor delivery subsystem. Such an odor delivery sub-system includes a plurality of bottles, each containing a material(s) for generating an odor and a delivery device that is configured to selectively deliver a specific odor from one of the plurality of bottles to the animal. The delivery device includes a delivery line and a bypass line that is operably coupled to the delivery line. The delivery device also is configured so that the bypass line is selectively coupled to a vacuum source so flow of the odor through the delivery line occurs when the bypass line is fluidly coupled to the vacuum source and so the odor is delivered to the animal from the delivery line when the bypass line is fluidly de-coupled from the vacuum source.
[0015] In further embodiments, such an olfactory discrimination system further includes a means for providing a continuous source of gas, where the continuous gas source means is fluidly coupled to the delivery line. Also the delivery device is further configured so that the continuous gas source means is coupled to the delivery line when the bypass line is open, when flow of odor through the delivery line occurs and when the odor is being delivered to the animal, and so that the gas continues to flow through the delivery line after flow of the odor to the animal is discontinued. In yet further embodiment, such an olfactory discrimination system includes N bottles. where N is an integer greater than 2 and in more specific embodiments, N is 16.
[0016] In yet further embodiments, such an olfactory discrimination system further includes a fluid delivery subsystem. Such a fluid delivery sub-system includes a plurality of bottles, each containing a different fluid; and a fluid delivery device configured to selectively deliver a specific fluid from one of the plurality of bottles to a watering device for the animal. Such a delivery device includes a plurality of delivery lines one for each bottle, a plurality of control devices one of said plurality of control devices being operably coupled to a respective one of the delivery lines, and a controller operably coupled to each of the control devices and which is configured so as to cause the respective control device, corresponding to the bottle having the fluid to be delivered, to operate so as to allow the fluid to flow from the bottle to the watering device.
[0017] According to another aspect of the present invention there is featured an apparatus for measuring the water consumed by an animal over time; such an apparatus includes a watering device; an indexed storage device configured to store a fluid and to include gradations representative of an amount of fluid therein; and a means for fluidly coupling the watering device to the indexed storage device. In further embodiments, the means for fluidly coupling includes an adaptor configured to couple with an end of the watering device and an end of the indexed storage device.
[0018] In yet further embodiments, the measuring apparatus further includes a quick disconnect including a first part and a second part that are selectively fluidly coupled and de-coupled from each other, and the means for coupling includes an adapter configured to selectively couple with an end of the watering device and one of an end of the first part or second part.
[0019] According to another aspect of the present invention, there is featured a method for determining an amount of fluid consumed by an animal comprising the steps of providing a watering apparatus including an indexed storage device configured to store a fluid and to include gradations representative of an amount of fluid in therein; and visually observing the indexed storage device and determining therefrom an amount of fluid consumed by the animal. In further embodiments, such visually observing does not involve the touching or the manipulating of the indexed storage device by a user.
[0020] There also is featured a method for selectively exposing an animal to one of a plurality of odors at a time, including the step of providing an odor delivery subsystem. Such a odor delivery sub-system includes a plurality of bottles, each containing a material(s) for generating an odor, a delivery device configured to selectively deliver a specific odor from one of the plurality of bottles to the animal, and the delivery device including a delivery line and a bypass line operably coupled to the delivery line. Such a method also includes coupling the bypass line to a vacuum source so flow of the odor through the delivery line occurs, and decoupling the bypass line from the vacuum source so the odor is delivered to the animal from the delivery line when the bypass line is fluidly de-coupled from the vacuum source.
[0021] In further embodiments, such a method includes providing a fluid delivery subsystem that includes a plurality of bottles, each containing a different fluid and a fluid delivery device configured to selectively deliver a specific fluid from one of the plurality of bottles to a watering device for the animal. Such a method also includes operating the fluid delivery device so that the fluid in the bottle having the fluid to be delivered flows from the bottle to the animal watering device.
[0022] Also featured is a method for making a sound attenuation chamber comprising the steps of creating a frame from a plurality of scalable frame members that are interconnected to each other; providing a plurality of panel members, each of the plurality of panel members is configured so as to include a plurality of layers of materials having different densities that when attached to each other creates a panel that attenuates sound external to the chamber; and connecting each of the plurality of frame members to adjacent pairs of scalable frame members so as to form at least five walls of the chamber.
[0023] Other aspects and embodiments of the invention are discussed below.
BRIEF DESCRIPTION OF THE DRAWING
[0024] For a fuller understanding of the nature and desired objects of the present invention, reference is made to the following detailed description taken in conjunction with the accompanying drawing figures wherein like reference character denote corresponding parts throughout the several views and wherein:
[0025] FIGS. 1( a ), 1 ( b ) are axonometric views of illustrative embodiments of a scalable animal enclosure according to the present invention;
[0026] FIG. 2 is another, enlarged axonometric view of the scalable animal enclosure of FIG. 1( b );
[0027] FIG. 3 is another, enlarged axonometric view of the scalable animal enclosure of FIG. 1( a );
[0028] FIG. 4 is a top of a scalable animal enclosure according to another illustrative embodiment of the present invention;
[0029] FIG. 5 is an illustrative view showing a stacked arrangement of a multiplicity of sound attenuation chambers according to the present invention;
[0030] FIG. 6 is a cross-sectional view of a corner portion of the sound attenuation chamber of FIG. 5 ;
[0031] FIG. 7 is a illustrative view showing the door and door sealing arrangement of the sound attenuation chamber of FIG. 5 ;
[0032] FIG. 8( a ) is an illustrative view of a back wall of the sound attenuation chamber of FIG. 5 , showing a portion of the air ventilation system;
[0033] FIG. 8( b ) is an enlarged view of a portion of FIG. 8( a ) showing the baffles;
[0034] FIG. 9 is another illustrative view of the back wall of the sound attenuation chamber of FIG. 5 , showing another portion of the air ventilation system;
[0035] FIG. 10 is a partial view of a corner portion in the top or bottom surface of the sound attenuation chamber of FIG. 5 , showing a feature by which the sound attenuation chamber can be stacked;
[0036] FIG. 11 is another illustrative view of the stacked arrangement shown in FIG. 5 , but with the doors opened;
[0037] FIGS. 12( a ),( b ) include an illustrative front view ( FIG. 12( a )) and an illustrative back view ( FIG. 12( a )) of an olfactory discrimination system according to the present invention;
[0038] FIG. 13 is an illustrative front view of the olfactory discrimination system of FIG. 12 with the doors to the sound attenuation chambers opened;
[0039] FIG. 14 is an illustrative view of the interior of an opened sound attenuation chamber also showing the animal enclosure disposed therein;
[0040] FIG. 15( a ) is an illustrative front view of a portion of the olfactory discrimination system of FIG. 12 showing the fluid storage and the flow control valves/meters that meter flow of the odor being delivered to the animal;
[0041] FIG. 15( b ) is an enlarged view of FIG. 15( a ) showing the fluid storage;
[0042] FIG. 16 is an illustrative back view of a portion of the olfactory discrimination system of FIG. 12 showing a portion of the sub-system for delivering the odor to the animal;
[0043] FIG. 17 is an illustrative view within the olfactory discrimination system of FIG. 12 showing a view of another portion of the sub-system for delivering the odor to the animal;
[0044] FIG. 18 is an illustrative view within the olfactory discrimination system of FIG. 12 showing a side view of a portion of the subsystem for delivering fluid to the animal;
[0045] FIG. 19 is an illustrative view of the individual fluid storage bottles of FIG. 15( b );
[0046] FIG. 20 is an illustrative view showing the fluid storage bottles connected to the inlets;
[0047] FIG. 21 is another of the bottle inlets but with the fluid storage bottles disconnected from the inlets;
[0048] FIG. 22 is a schematic block diagram view of the odor delivery sub-system;
[0049] FIG. 23 is a schematic block diagram view of the fluid delivery sub-system;
[0050] FIG. 24 is a illustrative view of a customized animal enclosure showing a side wall member configured with the animal nose poke and the fluid well area;
[0051] FIG. 25 is an illustrative view showing interconnections between the odor and fluid delivery sub-systems and the related features of the animal nose poke and the fluid well area;
[0052] FIGS. 26( a )-( b ) are various illustrative elevation views of a part of a capillary licker according to embodiments of the present invention;
[0053] FIG. 26( c ) is an illustrative view of a part of a capillary licker according to other embodiments of the present invention;
[0054] FIG. 26( d ) is an illustrative view of a valve assembly portion of a capillary licker according to the present invention;
[0055] FIG. 27 is an illustrative view of a capillary licker according to the present invention;
[0056] FIG. 28 is partial illustrative view of a disassembled capillary licker according another embodiment of the present invention;
[0057] FIG. 29 is a schematic block view of the flow control valve/meter station on the front side of the olfactory discrimination device; and
[0058] FIG. 30 is an illustrative view of an exemplary odor cartridge.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0059] Referring now to the various figures of the drawing wherein like reference characters refer to like parts, there is shown in FIGS. 1( a ), 1 ( b ) axonometric views of illustrative embodiments of a scalable animal enclosure 100 a,b according to the present invention. Also, there is shown in FIG. 2 an enlarged axonometric view of the scalable animal enclosure 100 b of FIG. 1( b ) and in FIG. 3 another, enlarged axonometric view of the scalable animal enclosure 100 a of FIG. 1( a ). There is shown in FIG. 4 a top view of yet another scalable animal enclosure 100 c.
[0060] In the following discussion, when reference is made to a specific animal enclosure or a part of an animal enclosure that is specific to one of the illustrated animal enclosures, the reference numeral includes a numeric character and an alpha character (e.g., 100 a,b , 110 a,b ). When reference is being made generally to any animal enclosure of the present invention or generally to a common but slightly different feature (e.g., base 110 a,b ) of the illustrated animal enclosure, then reference may be made to only the numeric character that is in common (e.g., base 110 ).
[0061] As can be seen from the following discussion, the animal enclosures 100 a,b,c shown in these figures illustrate the adaptability or flexibility of the animal enclosure to be assembled so as to carry out any of a number of functions as well as the ease by which such an animal enclosure is scalable during the process of making and assembling such an animal enclosure of the present invention. Also, as hereinafter described in connection with another aspect of the present invention, such animal enclosures 100 are usually placed inside of a sound attenuation chamber, such as that described herein, or other enclosure in order to run experiments.
[0062] As shown in FIG. 1( a ) and FIG. 3 , an animal enclosure 100 a according to one illustrative embodiment of the present invention includes a base member 110 a ; side wall members 120 a ; a front wall member 130 ; and a plurality of vertical fixed frame members 140 . As shown in FIG. 1( b ) and FIG. 2 , an animal enclosure 100 b according to another illustrative embodiment of the present invention includes a base member 110 b ; side wall members 120 b ; a front wall member 130 ; and a plurality of vertical fixed frame members 140 . As shown in FIG. 4 , an animal enclosure 100 c according to another illustrative embodiment, includes a base member 110 b ; side wall members 120 b ; a front wall member 130 ; and a plurality of vertical fixed frame members 140 , where one or more sides 102 of the animal enclosure 100 c includes a plurality of side wall members.
[0063] The scalable animal enclosure 100 is particularly useful for experiments involving laboratory mice or other small laboratory animals. In one illustrative embodiment, the base member 110 includes a first base member 112 having a configuration that is appropriate for the intended use and also is constructed of a material suitable for the intended use. In particular embodiments, the first base member 112 is constructed from a plastic material. In addition, the shape of the first base member and its size is configurable to fit the intended use and can be in the shape of a rectangle, square circle, pentagon, hexagon, octagon and the like. In more specific embodiments, the shape of the first base member 112 is arranged to compliment the shape of the structure that extends vertically upwardly and is defined by the side wall members 120 the front wall member 130 and the vertical fixed frame members 140 .
[0064] The first base member 112 is configurable with a through opening 115 that is located in a central portion of the first base member and being within the interior of the animal disclosure as defined by the side wall members 120 and the front wall member 130 . The animal enclosure is further configurable so that a perforated member 114 , such as a perforated plastic sheet 114 b or a perforated metal sheet 114 b , is disposed so as to extend over and beyond the boundaries of the centrally located through opening 115 so as thereby extend over the opening. In further embodiments, a plurality of rods 116 (metal or plastic) are arranged so as to extend across the centrally located through opening 115 and in more specific embodiments extend between the axially extending walls of the centrally located through opening. Alternatively, a sheet like member including such rods is provided which sheet like member is disposed so as to extend over and beyond the boundaries of the centrally located through opening 115 so as to extend over the opening. In further embodiments, the rods are arranged to provide a mesh like structure.
[0065] The perforated sheet members and rod structures described above, provide a support surface for the animal when it is located within the animal enclosure 100 , to walk or rest upon. These members or structures also provide a mechanism that allows animal waste to fall through to a collection device (not shown) as is known in the art (e.g., a removable urine pan) that is located below the centrally located through opening 115 in the base member 110 . The foregoing structures are illustrative and shall not be limiting as its is within the scope of the present invention for any structure or combination with the first base member as is known to those skilled in the to be utilized to form such a removable or fixed support structure or floor that is appropriate for the intended use.
[0066] The structure that extends upwardly from the base member 110 , defines the outer vertical boundaries of the sides 102 , or the enclosure or compartment in which the animal is located. This upwardly extending structure includes the side wall members 120 (which includes the back wall member), the front wall member 130 and the vertical frame members 140 . An end 144 a of each vertical frame member 140 is secured to the base member 110 so that the frame members are generally in fixed relation to the base member. Such securing can be accomplished using any of a number of means known to those skilled in the art including mechanical attachments (screws, bolts, nuts and adhesives).
[0067] In particular embodiments, the side wall members 120 a,b are removably secured to each frame member 140 that abuts an end of a given side wall member. Thereby also securing the side walls in fixed relation to the base member 110 . In further embodiments, the side walls are secured so that a bottom edge of the side walls abut the base member 110 or are spaced a distance from the base member such as to provide for ventilation.
[0068] In more specific embodiments, the frame members 140 are configured so as to include at least one slot 142 that extends vertically, preferably two such vertically extending slots, in which is slidably received a vertically extending end of a side wall member 120 a,b . The slots 142 in the frame members 140 provide a mechanism by which the wall members 120 a,b can be easily removed or replaced after the animal enclosure is assembled so as to allow one or more wall members that have been modified or customized for a given testing or experimental sequence to be inserted between adjacent frame members 140 . For example, and as illustration, the side wall members 120 are configurable so as to be opaque 121 b , clear 121 c (e.g., to allow a camera or researcher to see through), a custom wall 121 a with necessary scientific equipment (e.g., electronic components, fiber optics, lights, etc.), or a combination of the above as dictated by the needs and intents of the experiment to be performed.
[0069] Because of this flexibility, an animal enclosure 100 of the present invention can be modified as and when needed to fit the needs for multiple research purposes, which is in contrast to conventional animal enclosures that do not have such flexibility. As animal enclosures 100 are easily modified to fit different research purposes, research cost are reduced as compared to research where a one-off animal enclosure is used. Also, if a customized side wall member is not available for a given experiment, a customized wall member can be made for the given experiment and then used in combination with an existing animal enclosure, which again will lead to reduced costs as compared to the cost of an animal enclosure that is suitable only a given experiment.
[0070] In further embodiments, the frame members 140 further include one or more slots 142 or other structural feature (e.g., threaded aperture) that can serve as an attachment point for devices, or other equipment/structure that is mounted to the exterior surfaces of the animal enclosure, more specifically to one or more of the frame members 140 thereof.
[0071] The number of frame members 140 are defined by the general shape of the structure extending upwardly from the first base member 112 , the size of the enclosure 100 and the number of side wall members 120 being used to define a side of the enclosure. In particular embodiments, each animal enclosure 100 includes a plurality of frame members 140 , four or more frame members 140 , and in illustrative embodiments, four frame members per animal enclosure.
[0072] In further embodiments, and with particular reference to FIG. 4 , an animal enclosure 100 of the present invention is configurable so that one or more sides 102 thereof, more particularly two sides, of the animal enclosure are arranged to include a plurality of side wall members 120 c and one or more frame members 140 that are located between the frame members 140 disposed at intersections or corners of sides (including back and front walls). The one or more frame members being provided to couple each adjacent pair of side wall members 120 c and also being coupled to the base member 110 c including a perforated member 114 c . The side wall members 120 c are configurable so as to span the same lateral distance or as illustrated in FIG. 4 , the side wall members are configurable so that each extend laterally a different amount (i.e., side wall members can have different widths).
[0073] In illustrative embodiments, the frame members 140 comprise four bars of 1″×1″ 80/20 T-slotted extruded aluminum, each bar forming a frame member for the animal enclosure. The slots in each of the frame members removably (e.g., slidably) receive the vertical extending sides of a side wall member 120 as described above.
[0074] The front wall member 130 of each animal enclosure 100 in particular embodiments is configured as the door for the animal enclosure that is releasably secured to the frame members 140 adjacent to the front wall or other structure of the animal enclosure (e.g., the top member 150 ) using any of a number of mechanisms or techniques known to those skilled in the art. In illustrative embodiments, the present invention utilizes a magnetic latch to secure the front wall 130 to the adjacent frame members 140 .
[0075] In more particular illustrative embodiments, the vertical edges of the front wall member 130 include a metal surround, such as for example, a stainless steel U-channel frame 132 and magnets 160 are located in the slots 142 on opposing sides of the adjacent frame members 140 which create a magnetic field sufficient in strength to keep the animal inside the animal enclosure from pushing the front wall member open. In illustrative embodiments, the magnets 160 comprise two rare earth magnets and a neodymium magnet underneath each rare magnet.
[0076] In further embodiments, the animal enclosures 100 a,b also can include a top member 150 a,b . The top member 150 is secured to the frame members 140 using any of a number of means known to those skilled in the art. In illustrative embodiments the top member is secured mechanically to the frame members 140 using a threaded member (not shown) secured to the frame member and a nut 152 .
[0077] As shown in FIG. 1( b ), the top member 150 also is configurable so as to include one or more through apertures 154 . As shown more clearly in FIG. 1( a ), the top member 150 also is configurable so as to include a fixed part 156 a and a removable part 156 b , where the removable part 156 b is removable secured to the fixed part 156 by screws (not shown) and nuts 157 .
[0078] It should be recognized that when an animal enclosure 100 of the present invention is being initially constructed, the constructor adjusts the lengths of the frame members 140 and the heights and widths of the side wall members 120 and the front wall member 130 so as to create an enclosure that is appropriately sized for the animal. Also, the base member 110 size and shape can be easily determined from the design and size of the enclosure formed when the frame members 140 , and side wall members 120 and front wall 130 are assembled and arranged on the surface of the base member. Thus, it can be seen that the basic structure being defined by these features of the animal enclosure of the present invention are easily scalable so as to construct animal enclosures for animals of different sizes and physical capabilities. As also indicated above, because side wall members of the present invention are easily removable and/or customizable, the constructor or a user in the field can easily replace one side wall member with another side wall member having different characteristics without requiring the disassembly of the entire animal enclosure. As discussed hereinafter, such an animal enclosure 100 is usable in combination with a sound attenuation chamber 200 of the present invention.
[0079] When working with mice or rats, many experiments require conditions under which the animals are not exposed to external sounds that may act as confounding factors. When working in a crowded laboratory, with multiple experiments and multiple animals, it can be extremely difficult to achieve such conditions. Referring now to FIGS. 5-11 there are shown various views of a sound attenuation chamber 200 according to the present invention which advantageously provides a sufficiently large environment to run complex animal experiments yet are also able to block out a vast majority of the ambient noise.
[0080] Referring now to FIG. 5 , there is shown an illustrative view of a stacked arrangement of a multiplicity of sound attenuation chambers 200 according to the present invention. The sound attenuation chambers 200 of the present invention are configurable so as to take full advantage of available lab space. As shown in FIG. 5 , the structure of such a sound attenuation chamber allows a large number of test systems enclosed in such chamber to be fully operational in close proximity, providing for economy of space and efficient use of personnel. Further, test systems within such a chamber can be easily re-configured within allocated space depending on demand and usage. Furthermore, all the walls 202 a - e , 204 , including the door 204 , are modular, allowing them to be easily customized and/or replaced.
[0081] Each sound attenuation chamber 200 is a relatively large, scalable enclosure including six walls 202 a - e , 204 , one of which acts as the door 204 for the sound attenuation chamber, and a plurality of frame members 220 that are configured and arranged to form a supporting frame to which the walls and door are attached.
[0082] As shown more clearly in FIG. 6 , each of the walls 202 a - 3 , 204 includes three or more layers 210 a - c where at least three of the layers are composed of materials that have densities that vary from each other. In particular embodiments, the walls 202 a - e exclusive of the door 204 are composed of three layers and the door is composed of four layers. It should be recognized that the walls and door 202 a - e , 204 are configurable so as to include any number of layers of sound attenuating materials so as to achieve a desired level of sound attenuation.
[0083] In illustrative embodiments, the walls 202 a - e (excluding the door) are made of three layers of sound attenuating plastic sheets; more specifically an external or outer layer 210 a of PVC Type I, a middle layer 210 b of a water-resistant sound absorbing sheet (e.g., compressed, corrosion-resistant polypropylene beads), and an internal or inner layer 210 c of expanded rigid PVC. In more particular illustrative embodiments, the walls 2020 a - e are made from three materials: 1/16″ thick PVC Type I grey sheet, 0.236″ thick white expanded PVC sheet, and 1″ thick water-resistant sound absorbing sheet (polypropylene foam). The sheets are secure together using an adhesive material (e.g., 3M Aerosol Adhesive High Strength 90 ) with the Type I PVC on the outside, the polypropylene foam in the middle, and expanded PVC on the inside.
[0084] Once the walls 202 a - e are prepared (e.g., adhesive has dried), the wall pieces are then configured for mating with the frame members 220 . For example, the walls 202 a - e are edged on all four sides (for example, using a table saw) so as to create a slight protrusion that extends from the middle layer 210 b of polypropylene foam. Also, for example, the inside of the wall or the inner layer 202 c (expanded PVC portion) is also edged on the table saw to a roughly 45 degree angle so as to allow the walls to internally overhang the frame members 220 slightly yet fit firmly together inside of the box. This thereby further limits if not prevents ambient noise from entering the box through the material making up the frame members 220 . An inner layer 210 c of expanded PVC is particularly advantageous because this material is nonporous and easily cleaned with standard laboratory products.
[0085] As to the remaining wall that forms the door 204 for the sound attenuation chamber 200 , in illustrative embodiments the door is composed of four layers 212 a - d and at least three of the layers are composed of materials having different densities. In more particular illustrative embodiments, the first layer 212 a is composed of a material having a first density, the second and third layers 212 b,c are composed of a material having a second density that is different than the density of the first layer and the fourth layer 212 d is composed of a material having a third density that is different than the density of the first through third layers. In yet further illustrative embodiments, the external or first layer 212 a is an external PVC Type I sheet, the second and third layers 212 b,c are sheets of polypropylene foam, and the fourth layer 212 d is a sheet of internal expanded PVC. For the door, the second layer 212 b is configured for mating with the corresponding frame member 220 . For example, the second layer 212 b is further processed so as to create a slight protrusion that extends from the second layer of polypropylene foam that engages with the frame member 220 . The door 204 is otherwise manufactured or assembled as described above.
[0086] In further embodiments, after the rear wall 202 is assembled (as described above), the rear wall is further processed to create a ventilation pathway 230 so that air can flow from the exterior of the sound attenuation chamber 200 to the interior thereof. In more particular embodiments, and as shown more clearly in FIGS. 8( a ),( b ), the rear wall 202 e from the side that would be external, is processed or machined so as to create a pathway 230 including a series of baffles 232 . The series of baffles 232 allow air to pass laterally through the wall without compromising the sound attenuation properties of the chamber 200 . As shown more clearly in FIG. 9 , the baffles 232 are covered with an external piece 234 , such as individual piece of Type I PVC. This external piece 234 includes one opening 236 a with an attached fan 238 so air will move into the box. After the external piece 234 is attached, two other small circular openings on the inside and outside of the sound attenuation chamber 200 are provided and a mini-louver 237 is pressed into each of these openings to help muffle sound further.
[0087] The ventilation fan 238 allows an animal to stay in the sound attenuation chamber 200 for longer periods of time as compared to conventional sound attenuation chambers. Also the rear wall 202 e is unique as compared to other conventional devices, in that there is not a direct opening between the inside and outside of the chamber. In the present invention, the ventilation or air coming from the outside externally must past laterally through a series of baffles in the middle layer of the rear wall. This allows the animal to remain properly ventilated while still maintaining the sound attenuation properties of the chamber.
[0088] The rear wall 202 e also can be configured with one or more slots or openings to allow cables 204 (e.g., monitoring cables, control cables, power cables) to pass through from the outside to the interior of the sound attenuation chamber 200 . These slots or openings 250 are then closed or sealed by inserting pieces 252 of polypropylene foam that is configured to expand to form a seal when inserted therein.
[0089] The sound attenuation chamber further includes a frame that is made up of the frame members 220 that are secured to each other to form the frame. The frame support members 220 are secured to each other using any of a number of techniques known to those skilled in the art and otherwise appropriate for the intended use. In more particular embodiments, the frame members 220 are secured to each other mechanically. The frame members 220 preferably are made from a material having sufficient strength so that sound attenuation chambers 200 can be stacked one upon each other and otherwise can support the walls and other loads that can occur during use of the sound attenuation chamber.
[0090] For example, as shown in FIG. 11 the sound attenuation chamber 200 can be configured so it includes a sliding drawer on which would be disposed an animal enclosure such as that described herein. Thus, the materials and structure of the frame members 220 when assembled and secured to each other would provide sufficient strength so as to support the drawer when it is extended outside of the chamber 200 .
[0091] In further embodiments, and as shown more clearly in FIG. 10 , the frame members when assembled together include a mechanism by which the sound attenuation chambers can be stacked upon each other and so as to prevent lateral movement of an upper chamber. In more specific illustrative embodiments, one or more apertures 240 are provided in the frame formed from the frame members 220 , for example at each corner of the bottom and top surface of the chamber. A rod is inserted therein to prevent lateral movement of the upper chamber with respect to the lower chamber.
[0092] The layers wall forming the door further includes a surrounding frame work of frame members 220 that are joined to reach other to provide a supporting structure for the door. The door frame is hingeably coupled to the adjacent frame members 220 of the sides of the sound attenuation chamber 200 so that the door can be opened and closed. The door also includes a mechanism for keeping the door 200 shut, such as for example a magnetic latch as is known to those skilled in the art and a fixture (e.g., handle) that a user can grasp to open and close the door.
[0093] In further embodiments, the structure forming the sound attenuation chamber 200 after it has been fully assembled (e.g., with the frame and walls in place), is further configured so as to implement further measures to further attenuate sound transmission. All of the corners and edges (except those of the door) are covered with a silicon sealant 260 to further seal each box from external sound. Also, strips 262 of soft silicone foam rubber are placed on the exposed 45 degree edges of the wall panels that will meet with the door and/or on the exposed inside surface of the door frame 205 . This allows the door to form a complete seal and preserves the sound attenuation properties of the box. Further, a sealing member 264 made of a resilient material such as santoprene foam rubber cord is pressed into slots provided in the inside edge of the surrounding door framework (e.g., the T-slots of the 80/20 aluminum extrusion) opposing the inside edge of the door so as to provide a further seal for the door.
[0094] In view of the foregoing it can be seen that the dimensions of a sound attenuation chamber 200 of the present invention are highly customizable, and may be scaled up or down to meet a researcher's experimental needs. In more particular illustrative embodiments, the frame members 220 making up the frame of the chamber are composed of cut-to-length pieces of 1″×1″ T-Slotted Aluminum Extrusion made by 80/20, Inc. The pieces are tapped with ¼″×20 holes in both ends so that the frame members form the frame (e.g., a frame having a cube formation) using 10 Series Square Tricorner Connectors (made by 80/20, Inc.) as the corner pieces. Four of such pieces also are assembled in a similar manner into a square formation to form the outer perimeter of the door 204 . The door 204 is attached to the main box that makes up a part of the sound attenuation chamber 200 using 80/20 10 Series Heavy Duty Hinges. Also provided are an 80/20 Magnetic Door Catch to keep the door in place or closed and small plastic door handle that makes for easier opening. In yet further embodiments, the T-slots of the upper pieces of aluminum extrusion may be filled in with a T-slot cover, also made by 80/20. This may make the boxes easier to clean, especially if they are stacked.
[0095] Although the sound attenuation chambers 200 may not be considered as being completely sound-proof, the chambers are nonetheless capable of canceling out a vast majority of external or ambient noise. This makes the chambers 200 particularly useful for carrying out experiments with animals that are sensitive to sound (e.g., mice). In further embodiments, the walls are also constructed so as to be water proof, thereby preserving the sound attenuation properties despite potential spills of animal urine or laboratory solutions. Also, as compared to similar devices on the market, a sound attenuation chamber 200 of the present invention offers sound attenuation capabilities and customizability, yet are still relatively inexpensive.
[0096] Many tasks used in animal behavioral testing require complicated training procedures to teach the animal to perform responses that they are unfamiliar with. This training is a time consuming aspect of certain types of experiments and is often not of particular interest to the researcher in and of itself. One such type of experiments utilizes the natural propensity of rodents to investigate novel aspects of their environment using their sense of smell. In such, experiments, a rodent is exposed to the smell of a gas or the like having a particular odor or smell which is then required to make a discrete behavioral response to such exposure. Referring now to FIGS. 12-21 , 24 - 25 and 29 - 30 there are shown various views of an olfactory discrimination system 400 according to another aspect of the present invention. Referring also to FIGS. 22-23 , there are shown schematic block diagram views of the sub-systems that deliver the smell and fluid to the rodent.
[0097] While the olfactory discrimination system 400 of the present invention is shown in use with a sound attenuation chamber 200 and an animal enclosure 100 described herein that are further configured or customized for performance of the function to be carried out in this type of experiment, this shall not be considered as limiting. It is within the scope of the present invention for the olfactory discrimination system and elements as described herein be adapted for use with any of number of other conventional devices.
[0098] In the illustrated embodiment, the olfactory discrimination system 400 of the present invention includes a plurality of sound attenuation chambers 200 a in which is disposed an animal enclosure 100 d ; an odor delivery subsystem 500 , a fluid delivery subsystem 600 , all of which are mounted in a rack 402 . For purposes of facilitating viewing by the user as well as access, the flow control valves/meters 532 a - t of the odor delivery subsystem 500 and the fluid storage bottles 610 of the fluid delivery subsystem 600 are located on the front side of the olfactory discrimination system 400 . Also, for access purposes, major portions of the odor delivery subsystem 500 are located so as to be accessed from the back side of the olfactory discrimination system 400 . As also described herein, the odor cartridge 580 of the odor delivery sub-system 500 is designed so it can be removed as a unit thereby facilitating use, modification and operation of the olfactory discrimination system 400 .
[0099] The animal enclosures 100 d used for such testing are individually housed within specially designed sound attenuating chambers 200 a , and feature a modular construction that allows the experimenter to easily modify the animal enclosure and/or sound attenuation chamber 200 a beyond that shown to assess spatial discrimination (e.g., multiple wells, multiple locations), working memory (e.g., multiple odors; match and non-match to sample), and spatial working memory (e.g., multiple odors and wells). The olfactory discrimination system 400 described herein is used to screen for motor reaction time and signal detection.
[0100] The animal enclosure 100 d used in this experiment is further customized as follows. The rear wall 120 ar and the door 130 d , of the enclosure are made of a clear material (e.g., clear plastic material). The clear rear wall 120 ar allows a small camera 190 , such as small bullet camera, to see into the interior of the enclosure 100 d . The camera 190 is coupled to external monitoring equipment, thereby allowing a researcher to observe behavior of the animal (e.g., mouse) in the enclosure 100 d . The left wall 120 a 1 is made of an opaque plastic.
[0101] The roof or top 150 d of the animal enclosure includes a removable circular plastic sheet such as that also shown in FIG. 3 , that is held in place with “pop-in” connectors, thus allowing the ceiling to be moved or removed with minimal effort. The right wall 120 art of the enclosure is customized so as to include a nose poke system as described hereinafter that forms a part of both the odor delivery system 500 and the fluid delivery system 600 .
[0102] The nose poke system includes the odor structure 570 that includes an odor port 572 and an animal detection apparatus 574 that detects the presence of the animal 2 (e.g., the nose of a mouse) in the odor port. In illustrative embodiments, the structure of the odor structure is made in part from polycarbonate plastic. In an illustrative embodiment, the animal detection apparatus 574 , embodies an infrared beam break system to detect when a mouse puts its nose inside the odor port 572 . Such an infrared beam break system typically includes an IR light emitting diode and a corresponding IR light detector located in the odor port so that a signal is generated when the light beam is broken by the entry of an animal body part into the odor port. As is described hereinafter, the odor port 572 is connected via tubing to the odor bottles 510 outside of the sound attenuation chamber 200 a . This provides a mechanism whereby odor is pulled from one of the odor bottles 510 into the odor port 572 within the animal enclosure 100 d , and then vacuumed back out as short as a fraction of a second later as described further herein.
[0103] Above the odor port is located a fluid well structure 620 , including a well 622 for receiving liquid, that is fluidly coupled to fluid bottles 610 that allow a fluid such as water, sucrose, quinine, or conceivably any other low viscosity liquid to be pulled into the well residing in the animal enclosure 100 d , allow the animal to taste or drink it, and then drained away via a drain line 630 . A guard 192 is provided above the fluid well (e.g., a aluminum guard bent at a high angle) to prevent the animal from climbing on the fluid well.
[0104] The sound attenuation chamber 200 as described herein is further modified as described hereinafter for this application. In this application one of the walls 202 c forming the roof or top of the sound attenuation chamber 200 a is arranged so as to include an attachment 290 for a screw-based light bulb in order to provide light for the animal when the experiment is running. Also, attached to the rear wall 202 e is a Coulbourn ECB board 292 , which is used for the optics system. This ECB board 292 can be used with a variety of other Coulbourn products, allowing a researcher to customize the chamber or animal enclosure further to meet his or her needs for a given experiment.
[0105] The right wall 202 a of the sound attenuation chamber 200 a includes a plurality of holes, more specifically seven holes through which tubing corresponding to various lines of the odor delivery sub-system 500 and the fluid delivery sub-system 600 are passed (e.g., drilled ⅛″ round holes arranged roughly in a pattern like that of an “I” beam). As described herein, this tubing provides a mechanism that allows the animal enclosure and functionalities thereof to couple with the odor, volume, and concentration controls on the outside of the sound attenuation chamber 200 a.
[0106] Now referring to the schematic block diagram of FIG. 22 and FIGS. 16-17 , 24 - 25 and 29 - 30 , the olfactory odor delivery subsystem 500 of the present invention is discussed in more detail. Such a subsystem 400 includes a plurality of gas cartridges or bottles 510 each partially filled with whatever chemicals the researcher chooses for creating or otherwise providing an odor. In particularly illustrative embodiments, there are provided sixteen 9.5 dram bottles. In further embodiments and as described in further detail herein, a pressure source 502 is fluidly coupled to each bottle 510 to assist with flow of the odor from the bottle to the odor port.
[0107] As shown more clearly in FIG. 30 , the bottles 510 are arranged so as to be sandwiched between two pieces 501 a,b , more specifically two pieces of polycarbonate. The lower piece 501 b is machined so as to provide sixteen small circular indentations in which the bottles 510 rest, and a Buna-N 0-ring is placed within each indentation to allow the odor bottle assembly or odor assembly 580 to be compressed and sealed without the bottles breaking. The upper piece 501 a is machined so that there are two small threaded thru-holes 503 above each bottle 510 . Sixteen rings, each the size of a bottle top, is machined into the underside of the upper piece 501 a around each duo of holes 503 and a Buna-N ring is fitted into each, allowing for each bottle to form an airtight seal with the upper piece. There are also attachment points for the solenoid valves 512 , polycarbonate standoffs, and long attachment screws.
[0108] The assemblage of the foregoing parts along with other structure described herein, forms an odor cartridge 580 that is configured so as to be easily removed from the odor delivery sub-system 500 and easily replaced with another such odor cartridge whose bottles can contain different scents or odors from the cartridge being replaced. Thus, it is within the scope of the present invention, for a plurality of such odor cartridges 580 to be available for use with the olfactory discrimination system 400 .
[0109] Each odor cartridge 580 is built using eight standoffs (e.g., to ensure the proper height and to keep it stable when the upper and lower bottom pieces 501 a,b are compressed) and four long screws that run from the upper piece to the lower piece so as to allow these pieces to form an airtight seal around the bottles. In further embodiments, a smaller intermediary piece 501 c with holes for each bottle 510 rests on nuts attached to the long screws. This intermediary piece 501 c is placed roughly halfway between the upper and lower pieces 501 a,b and is used to keep the bottles arranged in the proper configuration relative to one another.
[0110] The two small threaded thru-holes 503 above each bottle 510 are each filled with screw-in barb fittings. One barbed fitting for each bottle is connected to a Twintec “BH” Series socket piece 505 a via a short length of polyurethane tubing. The other barbed fitting is connected using polyurethane tubing to a solenoid valve 512 , one for each bottle 510 , which all run via more polyurethane tubing to a central hub piece 520 that functions as a distribution manifold. A single tube 540 runs from the hub piece 520 through a wall of the sound attenuation chamber 200 a and is coupled to the delivery line 542 that feeds the odor port 572 . Thus, when the solenoid 512 for a corresponding bottle 510 is activated, the odor is eventually pulled from the corresponding bottle into the odor port within the animal enclosure 100 d , which is described further herein.
[0111] One-way check valves 516 are located in the tubing between each solenoid valve and the hub piece 520 , thus preventing odor from flowing backward from one bottle into another. Each of the solenoid valves 512 is electronically controlled by a computer 410 (e.g., a Coulbourn computer system) and the activation of the solenoids can be customized (e.g., opening times) to meet a researcher's needs.
[0112] The aforementioned Twintec “BH” Series socket piece 505 a on the odor cartridge attaches to a matching screw-in plug piece 505 b . This connection allows the odor cartridge 580 to be moved and switched with minimal effort. The matching plug piece 505 b is attached via polyurethane tubing to a series of Minimaster flow control valves/meters 532 a - p , one for each bottle 510 , that allow for controlling and monitoring air flow through each bottle of the odor cartridge 580 .
[0113] In more particular embodiments, air from the pressure source 502 is provided to an overall pressure air flow control valve/meter 532 s via one airline 515 a , that can be used to control the flow rate of air to the always on air-odor mixture control valve/meter 532 q and it also can be used to provide an indication of the overall flow rate. The always on air-odor mixture control valve/meter 532 q provides an air output to each of the bottle flow control/meter valves 532 a - p via a second air line 515 b and an air output that feeds to one of the input connections of the central hub piece 520 via a third airline 515 c . In illustrative embodiments, the control valve/meter described herein are Minimaster flow meters that can be adjusted to control the material (e.g., air/, air/odor mixture) flowing there through.
[0114] Each of the bottle flow control/meter valves 532 a - p is fluidly connected or coupled to a corresponding one of the bottles 510 through the Twintec “BH” Series socket piece connection 505 a,b and through one of the two small thru-holes 503 above the corresponding bottle that forms in combination with tubing a fourth airline 515 d . In further embodiments, a check valve 516 is located in the fourth air line 515 d to forestall contamination by preventing reverse flow.
[0115] In operation, when odor is desired to be provided to the odor port 572 , a solenoid valve 512 located in a respective bottle discharge line 514 for a corresponding bottle is opened, whereby an odor/air mixture flows from the bottle (i.e., out through the other of the two small thru-holes 503 above the corresponding bottle) through the respective discharge 514 and check valve 516 to another one of the input connection of the central hub 520 . As there are sixteen bottles 510 and bottle flow control/meter valves 532 a - p (see e.g., FIG. 29 ) in the illustrated embodiment, the central hub 520 is configured so to include enough input connections to couple with each respective bottle discharge line 514 and the air line 515 e from the always on air-odor mixture control valve/meter 532 q.
[0116] The always on air-odor mixture control valve/meter 532 q is configured to carry out at least two functions. When a solenoid valve 512 for a desired bottle 510 is opened to allow an odor/air mixture to flow through a respective bottle discharge line 514 , the air coming from the always on air-odor mixture control valve/meter 532 q is used to further control the density, concentration or strength of the odor/air mixture flowing through the respective discharge line concentration which would be received in the odor port 272 . In other words, the air coming from the always on air-odor mixture control valve/meter 532 q mixes the odor/air mixture flowing through the respective discharge line 514 (e.g., in the central hub 520 ) and this mixture flows through the hub discharge line 540 .
[0117] When the open solenoid 512 is thereafter closed, the air flowing from the always on air-odor mixture control valve/meter 532 q continues to flow which, in combination with the bypass line 544 and/or the always on vacuum line 550 causes any odor/air mixture remaining in the downstream discharge pathway including down stream tubing and functionalities (e.g., central hub 520 ) to be flushed or cleansed therefrom. Thus, the odor delivery system automatically cleans itself following an odor discharge without requiring action by the experimenter (e.g., self-cleaning).
[0118] As indicated above, the odor delivery sub-system includes an always on vacuum line 550 . The always on vacuum line is continuously, fluidly coupled the odor port 572 and to a vacuum source 551 via a vacuum exhaust port control valve/meter 532 r so as to control the level of vacuum or suction being developed on the odor port 572 . In particular illustrative embodiments, the vacuum being developed is controlled so that a positive pressure condition exists within the animal enclosure and within the sound attenuation chamber 200 a.
[0119] The odor delivery sub-system also includes a bypass line 544 that is fluidly coupled at one end to the delivery line 542 and the hub discharge line 540 and at the other end to a vacuum source that is preferably located in a room remote from the room in which testing is being done. The bypass line 544 is configured to include a bypass line control valve/meter 532 t and an odor exhaust bypass solenoid 545 that selectively couples and decouples the bypass line to the vacuum source.
[0120] In further embodiments of the present invention, each of the solenoids 512 , 545 are controlled by a computer 410 ( FIG. 23 ) such as a Coulbourn computer system. The computer controls the solenoids so that the solenoid 512 corresponding to the odor to be delivered to the odor port 572 is opened and remains open for the desired duration of time and that the odor exhaust bypass solenoid is controlled as described hereinafter to facilitate drawing the odor/air mixture to the odor port and thereafter closed so the so-drawn odor/air mixture is drawn into the odor port 572 so that it can be sensed by the animal.
[0121] It should be noted while a single bottle pathway of a odor cartridge 500 is illustrated in FIG. 22 for clarity; this shall not be considered a limitation as it is within the scope of the present invention for the odor cartridge to be configured so as to include “N” such bottle pathways, where “N” is an integer greater than one and in specific illustrative embodiments N=16. This also shall not be considered a limitation as N is adjustable to fit the intended uses and functions of the olfactory discrimination system such as how many different odors that can be selected to be tested at any one time. Thus, N can be greater than 16 as well as being less than sixteen.
[0122] Now referring to the schematic block diagram of FIG. 23 and FIGS. 18-21 , and 24 - 25 , the fluid delivery sub-system 600 of the present invention is discussed in more detail. The fluid delivery sub-system 600 , more specifically functionalities thereof, are also controlled by the computer (e.g., a Coulbourn computer system). The fluid reservoirs are stored in bottles 610 (e.g., customized 9.5 dram bottles), each with a female quick-disconnect shutoff fitting 611 , which allows the bottles to be moved and replaced without spillage. These fittings 611 are able to connect to their equivalent male fittings 613 attached to a mounting bracket 640 (e.g., aluminum mounting bracket. In illustrative embodiments, the bracket 640 holds up to three bottles at once. As indicated herein, it is within the scope of the present invention to expand the number of bottles available.
[0123] Three valves 650 (e.g., 075P Series Pinch Valves from Western Analytical) also are attached to this bracket 640 , one for each bottle 610 . When the valves 650 are activated by the computer 410 , the valves release the 1/16″ tubing 614 a - c running through them, thereby allowing fluid to drain via gravity from the fluid reservoir or bottle 610 , through the side wall of the sound attenuating chamber 200 a and thence into the well 622 inside of the animal enclosure 100 d . Another valve 632 acts as a control for the central drain line 630 located in the animal enclosure. It is within the scope of the present invention for the bottles be under pressure or a pump be provided to facilitate the flow of the fluid from the bottle to the well 622 . It also is within the scope of the present invention for a pump or a suction source be fluidly coupled to the drain line 630 to facilitate draining of fluid from the well 622 .
[0124] The olfactory discrimination system 400 of the present invention features modular construction on several levels allowing for future adaptations and functions. Individual units of the system can be moved/removed to allow for different configurations to suit the researchers needs. For example, a unit can be removed from the system and set up on a bench top to allow for electrophysiological recording. Additionally, the walls of the animal enclosure chamber can be removed and replaced to meet different experimental demands. For example, multiple odor ports and/or fluid reward delivery wells can be inserted in the enclosure to add a spatial component to research protocols.
[0125] The use or operation of the olfactory discrimination system of the present invention can be understood from reference to the following discussion and with reference to above-identified figures. Sixteen odors provide in bottles 510 are sealed in interchangeable cartridges 580 allowing for the delivery of any possible combination of odorants. Solenoid valves 512 , 545 on the system control the odor/air mixture allowing for the delivery of different concentrations of odorants. The odor/air mixture delivery is nearly instantaneous due to the bypass line 554 .
[0126] During an experiment, the experimenter selects an odor from one of bottles 510 to present to the animal. That odor is then fed via the hub discharge line 540 from the hub piece 520 into the bypass line 544 directly under the odor port 572 . Delivery of the odor delivery is then accomplished by turning off the bypass line 544 (i.e., closing the odor exhaust bypass solenoid 545 ) thereby forcing the odor/air mixture via the delivery line 542 into the odor port 572 . The delivered odor/air mixture is pulled into and thence out of the odor port 572 by the top vacuum line 550 that is operably coupled to the top of the odor port. As the odor delivery sub-system 500 can deliver odors in a time-sensitive manner, experimenters can deliver multiple short-duration puffs of different odors which can be incorporated into a working memory task. Because conventional systems do not incorporate such an odor bypass feature, they are not certain to deliver odor in a time-sensitive manner and thus cannot assess working memory.
[0127] The odor is localized to the odor port 572 due to a combination of several features. Additional valves control the overall flow of air/odor mixture into the port and the overall vacuum flow of air/odor mixture out of the port. In concert with the integrated sound attenuation chamber 200 a that are specially designed and sealed (also attenuate sound) and specifically calibrated ventilation fans, the odor delivery sub-system 500 of the present invention ensures that odor should not escape the odor port into the animal enclosure. Thus, pollution of the animal enclosure is thereby avoided.
[0128] Also, the vacuum lines 544 , 550 run out of the testing room to a vacuum source that is located remote from the testing room and is ultimately pumped out of the building. This ensures that the odor leaving the system does not escape into the testing room. Because conventional systems do not incorporate these aspects, these other systems cannot assure that odorant is not contaminating the testing area and thus also the animal enclosure; and therefore one cannot be sure that the animal is only sampling the odor selected by the experimenter in a time-sensitive manner nor can they be sure that other animals in the testing room are not sampling waste odors.
[0129] As to the fluid delivery sub-system 600 , this sub-system can deliver a precise amount of up to three different fluids at any time. This feature is expandable to six fluids and is not available on any conventional system. The fluids are delivered from easy-to-load quick-change bottles 610 and the entire sub-system is self-cleaning (also a feature not found on conventional systems).
[0130] Referring now to FIGS. 26-28 there are shown various views of capillary lickers 700 or components thereof according to another aspect of the present invention. Such a capillary licker 700 can be used in combination with the any of the animal enclosures 100 a - d described herein as well as with any of a number of other such enclosures known to those skilled in the art. Such a capillary licker also can be used in combination with the sound attenuation chamber 200 and/or olfactory discrimination system 400 as described herein.
[0131] In illustrative embodiments, a capillary licker 700 according to the present invention includes a water valve 710 (e.g., Lixit L-130 Water Valve), an adaptor piece 720 , a disconnect piece 730 (e.g., Air Logic Miniature Quick Disconnect, ⅛″) and an indexed storage device 740 a - c (e.g., volumetric serological pipet). In further embodiments, such a capillary licker 700 is configurable to include tubing (e.g., ⅛″ ID polyurethane tubing) to interconnect the valve assembly and the pipet. In the present invention, the adapter piece is used to attach the water valve 710 to the disconnect piece 730 , more specifically either the male part of disconnect piece (hereinafter male disconnect piece 730 a ) or the female part of disconnect piece (hereinafter female disconnect piece 730 b ) so as to thereby create a leak-proof system.
[0132] The following is an illustrative description of making such an adapter piece 720 for use in a particular application. It should be recognized that it is well within the skill of those in the art to adapt the following for use in making different size adapters pieces for connection with water valves or disconnects having different end connection details.
[0133] An adaptor piece 720 for interconnecting a Lixit L-130 Water Valve to an Air Logic Miniature Quick Disconnect, ⅛″ is built using a ½″ diameter piece of polyetherimide (Ultem) rod, cut to 0.845″ in length. One end is drilled and tapped with a ⅛×27 NPT pipe tap to a depth of 0.590″. The opposite end is drilled and tapped with a 10×32 tap so that it opens into the opposite end. The end with the 10×32 hole is tapered down starting 0.255″ from the edge. The diameter of the end with the 10×32 hole should be tapered down to a diameter of 0.356″.
[0134] The Lixit L-130 Water Valve 710 is then screwed into the ⅛×27 NPT end of the so constructed adapter piece 720 and the female Air Logic Miniature Quick Disconnect 730 b is screwed into the 10×32 end of the adapter piece. As shown in FIGS. 26( c ) and 27 , a piece of tubing 750 (e.g., polyurethane tubing) can be attached the barbed end of the male quick disconnect 730 a , and this tubing is attached to the pipet 740 ( c ). As shown in FIGS. 26( a ), 26 ( b ) and 28 , the outlet end of the indexed storage device 740 ( a ),( b ) can be of such a design that it can be coupled to the male disconnect piece 730 a and thus tubing is not involved in the construction of these capillary lickers 700 ( a ),( b ).
[0135] The use of the capillary licker 700 of the present invention can be understood from the following discussion and with reference to the foregoing discussion and the referenced drawing figures. The indexed storage device 740 is located within an animal enclosure such as that described herein. The researcher fills the indexed storage device 740 with a desired quantity of liquid before or after the storage device is located within the animal enclosure. The animal drinks the fluid using the Lixit water valve over the course of an experiment. The researcher reads how much fluid has been consumed by examining the level of water versus the indexed markings on the storage device 740 (e.g., markings on a volumetric pipet).
[0136] As illustrated in FIGS. 26( a )-( c ), the indexed storage device 740 can be of any size that is suitable for the intended use and experiment. More specifically, the capillary licker 700 of the present invention is such that it is easily configurable to use any one of a number of multiple different sizes of storage devices or pipets, thus allowing researchers to run experiments longer, with larger animals, or with more available fluid.
[0137] Although a preferred embodiment of the invention has been described using specific terms, such description is for illustrative purposes only, and it is to be understood that changes and variations may be made without departing from the spirit or scope of the following claims.
INCORPORATION BY REFERENCE
[0138] All patents, published patent applications and other references disclosed herein are hereby expressly incorporated by reference in their entireties by reference.
EQUIVALENTS
[0139] Those skilled in the art will recognize, or be able to ascertain using no more than routine experimentation, many equivalents of the specific embodiments of the invention described herein. Such equivalents are intended to be encompassed by the following claims.
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Featured are various devices, apparatuses and systems for use in connection with animal studies or experimentation as well as methods related thereto. Such devices, apparatuses and systems include a scalable animal enclosure that is easily customized for a given application; a scalable and easily customizable sound attenuation chamber that can be used with such an animal enclosure; an olfactory discrimination system which can quickly delivery an odor to an animal while minimizing the potential for ambient contamination and a leak-free water delivery apparatus that provides a mechanism for the experimenter to determine water consumption without handling the device.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit under 35 U.S.C.§ 119(e) of U.S. Provisional Patent Application No. 60/376,073 filed Apr. 29, 2002, entitled Torque Converter Clutch Regulator Valve and Method of Installation.
BACKGROUND OF INVENTION
[0002] The present invention relates to the field of hydraulic circuits within automatic transmission systems and, more particularly, to a replacement torque converter clutch (hereinafter “TCC”) regulator valve that reduces fluid pressure loss to the torque converter apply and release circuits, which actuate the torque converter clutch.
[0003] The General Motors 4L60-E (hereinafter “GM”) transmission and other similar GM transmissions are equipped with mechanisms to “lockup” their torque converters to varying degrees under certain operating conditions. The purpose of the lockup converter is to provide for direct drive when the vehicle is cruising at higher speeds. Since there is always some slippage in the fluid coupling of a torque converter, some power is lost and fuel economy suffers. By providing a direct mechanical coupling through the transmission at high engine speeds, the lockup converter improves fuel economy.
[0004] This is accomplished by an electronic/hydraulic torque converter clutch system, which utilizes a lockup piston within the torque converter housing. The lockup piston has friction material on its forward surface. When the vehicle is at cruising speed and lockup is desired, an electric solenoid is energized which opens the torque converter clutch (hereinafter “TCC”) regulator valve. This allows fluid pressure to act upon the lockup piston, which is forced against a machined surface on the converter cover. Thus, the lockup piston and the converter cover are locked together and act as a single unit similar to a manual transmission clutch. When lockup is no longer required, a port opens that allows the pressurized fluid to exhaust. The lockup piston then moves away from the torque converter housing re-establishing the fluid coupling.
[0005] Early 4L60E transmissions utilized 2 nd gear clutch fluid, which was essentially line pressure applied via an orifice, to actuate the TCC regulator valve. In this version of the transmission, the TCC regulator valve and the isolator valve were combined into one valve. In later versions lockup in the electronic torque converter clutch system was controlled by a pulse width modulated torque converter clutch (hereinafter “PWM TCC”) solenoid that provides an output or control pressure in response to the duty cycle imposed on the solenoid coil.
[0006] In 1993 General Motors converted to the PWM actuated TCC regulator valve and divided it into two separate valves, namely the regulator apply valve and the isolator valve. Thus, in the PWM versions (1993-1997) of the 4L60E torque converter, there are actually two converter solenoids being employed in the system. The PWM TCC solenoid sends automatic transmission fluid (hereinafter “ATF”) to the isolator valve. Since the PWM TCC solenoid is duty-cycling the isolator valve, it oscillates continuously within the valve body. The regulator apply valve receives line pressure and regulates it to a lesser pressure, which is known as converter apply pressure. Converter apply pressure is not actually sent to the torque converter, but to the TCC apply valve. The TCC apply valve is actuated by the TCC solenoid. This solenoid is simply an On/Off type solenoid and not a PWM type. It is the TCC apply valve that actually directs ATF to the torque converter.
[0007] In 1998 General Motors went to the “EC3” style torque converter. This design allows the torque converter to continuously slip from 2 nd gear upward without ever locking up completely. This design was intended to improve fuel economy and converter control. The regulator apply and isolator valves were changed only slightly and function exactly the same as the 1993-1997 PWM version.
[0008] A disadvantage associated with these systems is the pulsating flow generated by the pulse width modulated TCC isolator valve as it cycles between its open and closed positions. The isolator valve imparts some of this pulsating movement to the regulator apply valve. These pulsations cause wear within the valve body resulting in hydraulic fluid leakage and incorrect pressure responses. As a result vehicles with a 4L60E transmission often have insufficient TCC apply pressure causing uncontrolled clutch slippage, which overheats the converter and generates TCC slip codes requiring service work. These complaints can often be caused by ATF leakage past the TCC regulator valve resulting in reduced converter apply pressure.
[0009] There are known prior art patents that are available in the field and their discussion follows. One example is U.S. Pat. No. 4,271,939 to Iwanga et al. (hereinafter “939 patent”), which discloses a hydraulic control system for a torque converter for ensuring release of the lock-up condition of the torque converter. This is accomplished by providing a flow restrictor in the hydraulic working fluid supply passage for the torque converter to make the flow resistance of the passage equal to or larger than the flow resistance of the hydraulic working fluid supply passage for the lock-up control chamber. In this control system a first or feed passageway communicates with a source of pressurized fluid and with a torque converter chamber, a second or discharge passageway communicates with the torque converter chamber and a third passageway communicates with a lock-up control or clutch chamber of the lockup clutch. A lockup control valve communicates with the same source of pressurized fluid and with the third passageway. The first passageway is provided with the flow restrictor. With the provision of the flow restrictor, the disengagement of the lockup clutch will be assured upon pressurization of the third passageway.
[0010] Another example is U.S. Pat. No. 4,618,036 to Ideta (hereinafter “036 patent”), which discloses a hydraulic control system for the lockup clutch of a torque converter wherein release of a lockup clutch is ensured even when the discharge flow rate of the pump is low. This control system comprises a pump driven by an engine to discharge fluid, a torque converter having a lockup clutch with a lockup clutch piston movable to a clutch released position when fluid pressure within a lockup release chamber is higher than fluid pressure within a working chamber in the torque converter cavity, a line pressure regulator valve and an orifice, which provides a restricted flow communication between the torque converter and the pump even when line pressure generated by the line pressure regulator valve is lower than a predetermined value. The Ideta ('036) patent utilizes cutouts 20 formed on the land 32 d of the first spool 32 ( FIG. 1 ) on the line pressure regulator valve to permit a sufficient flow of hydraulic fluid via oil conduit 62 to torque converter 10 at low speed operation to ensure the release of the lockup clutch.
[0011] While these patents relate generally to hydraulic control systems for torque converters, they do not disclose improving hydraulic control over the torque converter clutch apply circuit or a related method for restoring the hydraulic integrity of such circuits by use of a replacement valve mechanism.
[0012] Pending U.S. patent application Ser. No. 09/939,372 to Stafford discloses an actuator feed limit valve (hereinafter “AFL”) assembly comprising a replacement hydraulic valve mechanism for installation within the original equipment valve body of an automatic transmission. The AFL valve directs line pressure into the actuator feed limit circuit, which feeds the shift solenoids, pressure control solenoid and other hydraulically actuated components of the transmission. This valve mechanism utilizes a full contact valve sleeve having inlet and exhaust ports disposed about its circumference, which substantially reduces side loading, bore wear, and AFL fluid circuit leakage. However, this patent application does not disclose the structural improvements and technical advantages of the present invention.
SUMMARY OF THE INVENTION
[0013] Accordingly, the present invention is a replacement TCC regulator valve assembly for the GM 4L60-E transmissions comprised of two separate valves, namely a regulator apply valve and an isolator valve, which is designed to increase fluid pressure within the torque converter apply circuit and to restore the hydraulic integrity thereof.
[0014] In one embodiment the replacement TCC regulator valve assembly employs a wear-resistant regulator apply valve sleeve, which has been added to provide full support to the regulator apply valve to prevent side loading (i.e. lateral movement) in operation. The control lands or so-called spools on the regulator apply valve have been reduced in diameter area by up to 10% in comparison to the original equipment valve, which reduces the balance circuit apply surface on the end face of the apply valve. Thus, the overall effect is to increase the influence of the PWM TCC solenoid on valve operation resulting in increased line pressure flow to the converter apply circuit for transmissions having such PWM converter systems.
[0015] In addition, the axial length of the replacement isolator valve has been increased in comparison to the original equipment valve to reside in contact with the unworn portions of the mating bore in the valve body to ensure accurate operation. Annular lubrication grooves have also been added to the present isolator valve for better valve centering to improve performance.
[0016] In an alternative embodiment, an optional isolator valve sleeve is added to the present TCC regulator valve assembly for instances wherein the OEM isolator valve bore has extreme wear that cannot be corrected solely by the installation of a replacement isolator valve.
[0017] There has thus been outlined, rather broadly, the important features of the invention in order that the detailed description thereof that follows may be better understood, and in order that the present contribution to the art may be better appreciated. There are additional features of the invention that will be described hereinafter and which will form the subject matter of the claims appended hereto.
[0018] Other features and technical advantages of the present invention will become apparent from a study of the following description and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The novel features of the present invention are set forth in the appended claims. The invention itself, however, as well as other features and advantages thereof will be best understood by reference to the following detailed description of an illustrative embodiment when read in conjunction with the accompanying figures, wherein:
[0020] FIG. 1A is a longitudinal cross-section of a TCC regulator valve assembly disposed within the valve body of a GM transmission and labeled Prior Art;
[0021] FIG. 1B is a longitudinal cross-section of another embodiment of a prior art TCC regulator valve assembly disposed within the valve body of a GM transmission labeled Prior Art;
[0022] FIG. 2A is a longitudinal cross-section of a reaming tool within the valve body for resizing the bore prior to installation of a remanufactured TCC regulator valve assembly labeled Prior Art and shown in FIG. 2B ;
[0023] FIG. 2B is a longitudinal cross-section of a remanufactured TCC regulator valve labeled Prior Art;
[0024] FIG. 3A is a longitudinal cross-section of the replacement TCC regulator valve assembly of the present invention shown in the closed position;
[0025] FIG. 3B is a longitudinal cross-section of the replacement TCC regulator valve of FIG. 3A shown in the open position;
[0026] FIG. 4 is a side elevational view of the modified regulator apply valve of the present invention;
[0027] FIG. 5 is a longitudinal cross-section of the regulator apply valve sleeve of the present invention;
[0028] FIG. 6 is a longitudinal cross-section of the modified isolator valve of the present invention;
[0029] FIG. 7 is a longitudinal cross-section of a reaming tool of the present invention within the valve body for resizing a first axial section of the bore prior to installation of the present TCC regulator valve assembly shown in FIGS. 3A and 3B ;
[0030] FIG. 8 is a longitudinal cross-section of another embodiment of the replacement TCC regulator valve assembly including an isolator valve sleeve; and
[0031] FIG. 9 is a longitudinal cross-section of an alternative reaming tool of the present invention for resizing a second axial section of the bore prior to the installation of the replacement TCC regulator valve assembly including the isolator valve sleeve shown in FIG. 8 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0032] Prior to describing the present invention in detail it may be beneficial to review the structure and function of a TCC regulator valve of the prior art. With reference to the drawings there is shown therein such a TCC regulator valve of the prior art, indicated generally at 100 and illustrated in FIG. 1A . The prior art TCC regulator valve 100 made available in some GM vehicles from 1993 to 1997 is comprised of a regulator apply valve 102 , an isolator valve 105 , and an isolator valve spring 106 arranged within the valve body 110 .
[0033] FIG. 1B illustrates another prior art TCC regulator valve, indicated generally at 200 , which was made available on GM vehicles in 1998. The TCC regulator valve 200 is similarly constructed for installation in the valve body 110 with the exception of the isolator valve 105 ′ wherein the configuration has been modified.
[0034] Still referring to FIG. 1B these components are arranged in coaxial relation as shown within a mating bore 111 and are captured in the valve body 110 by an end plug 115 , which is secured by a retaining clip 117 . The valve body 110 includes ATF exhaust ports 107 , 108 , a PWM TCC solenoid circuit as at 112 for receiving pressurized ATF, a line pressure port 113 for counteracting fluid pressure delivered via the PWM TCC solenoid port 112 , a TCC apply circuit as at 114 for sending pressurized ATF to the TCC apply valve (not shown), and a TCC apply balance port 116 .
[0035] In the early prior art designs the isolator valves 105 , 105 ′ ( FIGS. 1A and 1B ) are fabricated from steel. Valves 105 , 105 ′ continuously oscillate within the bore 111 of the aluminum valve body 110 as the PWM TCC solenoid cycles to provide smooth converter clutch engagement. Such oscillating movement wears the bore 111 at locations adjacent the isolator valves 105 , 105 ′ allowing PWM TCC solenoid pressure to leak past the isolator valves 105 , 105 ′ to exhaust. The regulator apply valve 102 also wears the bore 111 allowing converter apply pressure leakage, which eventually causes unwanted clutch slippage and overheating of the torque converter.
[0036] It is known in the prior art to ream the bore 111 oversize by the use of a suitable reaming tool 150 as shown in FIG. 2A to resurface the bore and to replace the original equipment manufacture (hereinafter “OEM”) valves 102 , 105 with oversize valves 102 ′, 105 ′ as seen in FIG. 2B . However, using this repair technique and the resulting remanufactured TCC regulator valve assembly 300 ( FIG. 2B ) has proven to be unsatisfactory and has resulted in very early wear problems in such remanufactured units. Thus, the present invention has been developed to resolve these problems and will now be described.
[0037] Referring to FIGS. 3A and 3B there is shown a replacement TCC regulator valve assembly in accordance with the present invention, indicated generally at 10 . The present TCC regulator valve assembly 10 includes a replacement regulator apply valve, indicated generally at 20 , a new regulator apply valve sleeve, indicated generally at 15 , and a replacement isolator valve, indicated generally at 25 . The OEM isolator valve spring 106 and the OEM retaining clip 117 may be reused in the present invention. The OEM end plug 115 is effectively integrated into the present sleeve 15 and, thus, the OEM plug 115 may be discarded.
[0038] Referring to FIG. 4 the present regulator apply valve 20 is illustrated. This spool-type valve 20 includes a pair of control diameters or lands 42 , 45 interconnected by a stem portion 43 , which may include a peripheral groove formed thereon (not shown) for identification purposes. A spring locating diameter 40 is formed coaxially with land 42 and functions to guide the spring 106 against the end face of land 42 .
[0039] Land 42 also includes an annular, lubrication groove 24 that fills with ATF during operation. This provides an even film of lubrication about land 42 , which resists side loading and uneven wear within the mating bore 111 . The end face 45 a of land 45 in combination with the end face 46 a of the chamfered contact diameter 46 defines a reaction surface (i e. balance apply surface) for pressurized ATF entering the balance apply port at 116 ( FIGS. 3A and 3B ).
[0040] Lands 42 , 45 function to control the flow of line pressure as at 113 to the TCC apply circuit 114 as hereinafter described. In the present invention the outside diameters of lands 42 , 45 have been reduced by up to 10% in comparison to the OEM apply valve 102 to reduce the balance apply surface 45 a , 46 a (as defined hereinabove) rendering the present regulator apply valve 20 less responsive to balance apply pressure via circuit 116 and, accordingly, more responsive to pulse width modulated (PWM) solenoid control via circuit 112 . This results in an increased flow of ATF from line pressure circuit 113 to converter apply circuit 114 and higher converter apply pressure in operation.
[0041] In the preferred embodiment the regulator apply valve 20 is fabricated from aluminum material per 6262-T8/T9 or 6061-T6 and is hard anodized per MIL-A-8625, Type III, Class 2 to provide an optimal coefficient of friction with the mating valve sleeve 15 .
[0042] As more clearly shown in FIG. 5 , sleeve 15 is a generally cylindrical construction having a longitudinal bore 14 of sufficient size to allow valve 20 to oscillate therein. Sleeve 15 includes a plurality of inlet ports 16 and a plurality of outlet ports 18 formed within annular grooves 45 at predetermined locations in fluid communication with the line pressure port 113 and the TCC apply circuit 114 respectively ( FIG. 3B ). Sleeve 15 includes at least one TCC balance apply orifice 19 formed within the annular groove 40 ( FIG. 5 ) at a predetermined location in fluid communication with the TCC balance apply circuit 116 . The sleeve 15 may also include a plurality of exhaust ports 17 formed at a distal end thereof in proximity to exhaust port 108 .
[0043] An annular groove 21 is formed at one end of the sleeve 15 for receiving the OEM retaining clip 117 . Once the valve sleeve 15 is placed within the valve body 110 , the retaining clip 117 is installed within the annular groove 21 to secure the sleeve 15 and the entire TCC regulator valve assembly 10 within the valve body 110 . Thus, it will be appreciated that the primary feature (i.e. groove 21 ) and the function (i.e. valve containment) of the prior art end plug 115 ( FIG. 1A ) are effectively integrated into the present regulator apply valve sleeve 15 .
[0044] In one embodiment the sleeve 15 is fabricated from a high grade 4032-T6/T651/T86 aluminum to provide an optimal working surface for contact with the hard anodized regulator apply valve 20 and increased service longevity in comparison to the OEM design. The present sleeve 15 functions to restore the hydraulic integrity of the TCC apply circuit 114 and to provide full support to the regulator apply valve 20 within the sleeve 15 thereby eliminating the side-loading problem inherent in the OEM design.
[0045] Referring to FIG. 6 there is shown a replacement isolator valve in accordance with the present invention, indicated generally at 25 . Isolator valve 25 is a generally cylindrical construction fabricated from low carbon steel and case hardened to a predetermined case depth to resist wear. Isolator valve 25 includes a plurality of annular grooves 50 formed thereon, which function to center the valve 25 within the bore 111 by filling with ATF during operation and to distribute hydraulic pressure across the surface of the valve to prevent side-loading. In the embodiment shown four annular grooves 50 are formed in parallel relation at regular intervals on the outside diameter of the valve 25 .
[0046] The replacement isolator valve 25 has an increased axial length that is approximately 0.560 inches longer than the OEM isolator valves 105 , 105 ′, 105 ″ ( FIGS. 1A, 1B , and 2 B), and yet retains adequate clearance and proper function within its mating bore 111 in the OEM valve body 110 . The increased axial length allows the isolator valve 25 to ride in the unworn portions of the valve body 111 in the area adjacent exhaust port 107 ( FIG. 3B ) ensuring concentric operation of the isolator valve 25 in combination with the regulator apply valve 20 .
[0047] The isolator valve 25 includes a spring recess 27 integrally formed therein at a proximal end thereof to receive spring 106 . The isolator valve 25 may also include an axial protuberance 29 formed on a distal end thereof. The protuberance 29 permits ATF entering the PWM TCC solenoid port 112 to flow evenly around protuberance 29 to the actuating surface 25 a of the valve 25 . The protuberance 29 also prevents the end face of the valve 25 from striking against the inside of the valve body 110 as at 130 ( FIG. 3A ), which would disrupt ATF flow resulting in pressure loss within the converter apply circuit 114 .
[0048] To install the present TCC regulator valve assembly 10 , the retaining clip 117 , end plug 115 , regulator apply valve 102 , spring 106 , and either isolator valve 105 or 105 ′ of the prior art are removed from the valve body bore 111 . The OEM clip 117 and spring 106 are retained for reuse. Using a reaming tool 150 ′ such as Sonnax reamer (77754-R2) the bore 111 is enlarged to a sufficient size to accommodate the valve sleeve 15 as illustrated in FIG. 7 . Reamer 150 ′ includes a cutting diameter 152 , which is piloted by a guide diameter 154 that locates in a distal end (i.e. second axial section) of the bore 111 to ensure that the sleeve 15 will be concentric to the isolator valve 25 once installation is complete. After removal of any debris and burrs from the resized proximal end (i.e. first axial section) of bore 111 and applying lubrication, the present TCC regulator valve assembly 10 is installed as shown in FIGS. 3A and 3B .
[0049] In some instances the distal end of the bore 111 wherein the isolator valve 25 resides has such extreme wear that even the present modified isolator valve 25 will not prevent excessive oil loss. In this circumstance another embodiment of the TCC regulator valve assembly 10 ′ is provided as shown in FIG. 8 . In this embodiment an isolator valve sleeve, indicated generally at 60 , is utilized to remedy the leakage problem and to restore hydraulic integrity to the present valve assembly 10 ′.
[0050] The isolator valve sleeve 60 is a generally cylindrical construction, which is also fabricated from a high grade 4032-T6/T651/T86 aluminum and includes an internal bore 62 of a sufficient size to permit the oscillating movement of the present Isolator Valve 25 as described hereinabove. Sleeve 60 is provided with a plurality of inlet ports 16 ′ and a plurality of outlet ports 18 ′ formed at 90 degree intervals within annular grooves 49 ′ at predetermined locations in fluid communication with the PWM TCC solenoid circuit 112 and exhaust port 107 respectively in a manner similar to the regulator valve sleeve 15 ( FIG. 5 ).
[0051] The present sleeve 60 functions to restore the hydraulic integrity of the TCC solenoid circuit 112 and to provide full support to the isolator valve 25 within the sleeve 60 thereby eliminating side-loading and the excessive wear problems inherent in the OEM and remanufactured OEM designs described hereinabove. In all other respects the TCC regulator valve assembly 10 ′ including the isolator valve sleeve 60 operates in substantially the same manner as the TCC regulator valve 10 as described hereinabove.
[0052] In order to install the TCC regulator valve assembly 10 ′ an alternate reaming tool 150 ″ such as Sonnax reamer (77754-RM5) is utilized to enlarge the distal end (i.e. second axial section) 111 b of the bore 111 to a sufficient size to accommodate the valve sleeve 60 as illustrated in FIG. 9 . After removal of any debris and burrs from the resized distal end 111 b of the bore 111 and applying lubrication, the present regulator valve assembly 10 ′ is installed as shown in FIG. 8 .
[0053] In operation the output pressure from the PWM TCC solenoid in the high duty cycle enters the TCC regulator valves 10 , 10 ′ via the PWM TCC solenoid circuit 112 , which strokes the isolator valve 25 (i.e. to the right) from the closed position shown in FIG. 3A to the open position shown in FIG. 3B . It can be seen that the proximal end of the isolator valve 25 surrounding spring recess 27 resides in an unworn portion of the bore 111 b ( FIG. 3B ) adjacent the exhaust port 107 , which would not have been traversed by any of the OEM isolator valves 105 , 105 ′, 105 ″ due to their shorter axial length.
[0054] Simultaneously, the regulator apply valve 20 is also stroked opening the TCC apply circuit 114 to line pressure via line port 113 ( FIG. 3B ). As the apply valve 20 oscillates within the sleeve 15 , the groove 24 functions to distribute pressure across the circumference of land 42 eliminating side loading of the valve 20 within sleeve 15 . It can be seen that sleeve 15 extends partially over exhaust port 108 ( FIG. 3B ). This protects that portion of the bore 111 a that is susceptible to wear in the OEM design due to repeated oscillation and causes ATF/pressure leakage in the prior art regulator apply valves 102 , 102 ′.
[0055] As the PWM TCC solenoid cycles and returns to a lower percentage duty cycle, the hydraulic pressure in the PWM TCC solenoid circuit 112 is depleted. The isolator spring 106 then forces the Isolator Valve 25 back to the closed position with the assistance of fluid pressure entering the balance apply circuit at 116 and the solenoid cycle is repeated.
[0056] Although not specifically illustrated in the drawings, it should be understood that additional equipment and structural components will be provided as necessary and that all of the components described above are arranged and supported in an appropriate fashion to form a complete and operative torque converter clutch regulator valve assembly and method of installation incorporating features of the present invention.
[0057] Moreover, although illustrative embodiments of the invention have been described, a latitude of modification, change, and substitution is intended in the foregoing disclosure, and in certain instances some features of the invention will be employed without a corresponding use of other features. Accordingly, it is appropriate that the appended claims be construed broadly and in a manner consistent with the scope of invention.
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A replacement torque converter clutch regulator valve assembly for use within an automatic transmission including two cooperating valves, namely a regulator apply valve and an isolator valve, disposed in fluid communication with a line pressure circuit and a torque converter clutch apply circuit is disclosed. In one embodiment the regulator apply valve employs a regulator apply valve sleeve, which provides support to the regulator apply valve to prevent side loading. Modified control lands on the regulator apply valve have a reduced cross-sectional area calculated to increase the influence of the pulse width modulated solenoid, which provides an output pressure in response to the duty cycle imposed on the solenoid coil in pulse width modulated converter systems. In an alternative embodiment an isolator valve sleeve is utilized for instances wherein the isolator valve bore has extreme wear that cannot be corrected solely by the installation of the replacement isolator valve.
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CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims priority from Japanese Patent Application No. 2007-163768 filed Jun. 21, 2007. The entire content of this priority application is incorporated herein by reference.
TECHNICAL FIELD
[0002] The invention relates to an image processing apparatus, an image processing method, and an image processing program and, more particularly, to an image processing apparatus, an image processing method, and an image processing program allowing a user to readily visually confirm a result of determined image process and having good operability.
BACKGROUND
[0003] Image processing apparatuses capable of applying various image processes such as color tone correction or rotation to image data taken by an electronic camera, for example, are well known in the art. Such image processing apparatuses display thumbnail images which are reduced images on the screen thereof so as to allow a user to confirm a plurality of input image data at sight. One such image processing apparatus disclosed in Japanese Patent Application Publication No. 2000-215322 applies predetermined image process to a thumbnail image that has been selected as image data to be processed by a user and displays a result of the image process on the screen thereof.
SUMMARY
[0004] However, in most cases, the user determines, through a trial and error process, which image process is to be applied to respective image data. Thus, the conventional arts disclosed in Japanese Patent Application Publication No. 2000-215322 make user operation cumbersome and complicated.
[0005] In order to attain the above and other objects, the invention provides an image processing apparatus. The image processing apparatus includes a display, a retrieving unit, a process display unit, a process receiving unit, a process storing unit, a thumbnail display unit, and a thumbnail designating unit. The retrieving unit retrieves image data. The process display unit displays on the display a plurality of candidate image processes to be performed on the image data. The process receiving unit receives an instruction indicating a selected image process selected from among the plurality of candidate image processes. The process storing unit stores the selected image process. The thumbnail display unit displays a thumbnail image corresponding to the image data on the display. The thumbnail designating unit designates a thumbnail image. The thumbnail display unit displays a processed thumbnail image that represents a result of the selected process performed on the image data corresponding to the designated thumbnail image.
[0006] According to another aspects, the invention provides an image processing method. The image processing method includes retrieving image data, displaying a plurality of candidate image processes to be performed on the image data, receiving an instruction indicating a selected image process selected from among the plurality of candidate image processes, storing the selected image process, displaying a thumbnail image corresponding to the image data, and designating a thumbnail image. The thumbnail displaying step displays a processed thumbnail image that represents a result of the selected process performed on the image data corresponding to the designated thumbnail image.
[0007] According to another aspects, the invention provides a computer-readable storage medium storing a set of program instructions executable on an image processing apparatus. The program instructions includes retrieving image data, displaying a plurality of candidate image processes to be performed on the image data, receiving an instruction indicating a selected image process selected from among the plurality of candidate image processes, storing the selected image process, displaying a thumbnail image corresponding to the image data, and designating a thumbnail image. The thumbnail displaying step displays a processed thumbnail image that represents a result of the selected process performed on the image data corresponding to the designated thumbnail image.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] Embodiments in accordance with the invention will be described in detail with reference to the following figures wherein:
[0009] FIG. 1 is a perspective view showing the outer structure of a multifunction peripheral according to an embodiment;
[0010] FIG. 2 is a block diagram showing an electrical configuration of the multifunction peripheral;
[0011] FIG. 3( a ) is a view showing an example of a display screen of a touch panel displaying thumbnail images;
[0012] FIG. 3( b ) is a view showing an example of the display screen of the touch panel displaying image process keys;
[0013] FIG. 3( c ) shows a storage content of a position information storage area when the thumbnail images are displayed on the touch panel;
[0014] FIG. 3( d ) shows a storage content of the position information storage area when the image process keys are displayed on the touch panel;
[0015] FIG. 4 is a view schematically showing a configuration of a determined image process storage area;
[0016] FIG. 5 is a flowchart showing a thumbnail image display process executed by the multifunction peripheral;
[0017] FIG. 6( a ) shows an example of the display screen of the touch panel displaying the image process keys when an image process key is touched by a user;
[0018] FIG. 6( b ) shows an example of a display screen of the touch panel when a determination key is touched by the user;
[0019] FIG. 6( c ) shows an example of the display screen of the touch panel when the steps S 12 is executed;
[0020] FIG. 6( d ) is a view showing an example of the display screen of the touch panel on which a thumbnail image that has been touched by the user is replaced with a thumbnail image representing a result of an image process result “sepia”;
[0021] FIG. 6( e ) is a view showing an example of the display screen of the touch panel where the selected thumbnail image representing the result of the image process “sepia” is replaced with a thumbnail image representing a result obtained by canceling the image process “sepia”;
[0022] FIG. 6( f ) is a view showing an example of the display screen which displays a message in a dialogue area;
[0023] FIG. 7( a ) is a view showing an example of the display screen of the touch panel when two image processes “sepia” and “left-handed rotation” have been determined;
[0024] FIG. 7( b ) is a view showing an example of the display screen of the touch panel showing a result of the image process when two image processes “sepia” and “left-handed rotation” are simultaneously applied to the thumbnail image;
[0025] FIG. 7( c ) is a view showing an example of the display screen of the touch panel in the multifunction peripheral according to a second embodiment; and
[0026] FIG. 8 is a flowchart showing a part of thumbnail image display process performed in the multifunction peripheral according to the second embodiment.
DETAILED DESCRIPTION
[0027] A first embodiment of the invention will be described while referring to the accompanying drawings. FIG. 1 is a perspective view showing the outer structure of a multifunction peripheral (MFP) 1 according to the embodiment. As shown in FIG. 1 , the multifunction peripheral 1 is integrally configured of a printer 2 disposed on the bottom, a scanner 3 disposed on the top, and a control panel 4 provided on the front surface of the scanner 3 . The multifunction peripheral 1 implements a copier function, and a facsimile function, a printer function to record (print) image based on data received from external devices such as a personal computer (PC) on a recording sheet.
[0028] The multifunction peripheral 1 includes a connection panel 70 below the control panel 4 . The connection panel 70 has a USB terminal 71 on the left end side thereof. The USB terminal 71 is a connector terminal for communicably connecting the multifunction peripheral 1 to an external device through a USB connection. The connection panel 70 has a slot portion 72 on the right end side thereof. The slot portion 72 includes a plurality of card slots into which a memory card (card-type memory) can be inserted. When a memory card is inserted into one of the card slots, image data is read out by a controller 20 (see FIG. 2 ) to be described later from the inserted memory card.
[0029] The control panel 4 is provided on the front side of the multifunction peripheral 1 . The control panel 4 is used for a user to operate the printer 2 or the scanner 3 . The control panel 4 includes various operation keys 40 and a touch panel 41 . The user can input a desired instruction by using the control panel 4 . When a prescribed instruction is input to the multifunction peripheral 1 , the operation of the multifunction peripheral 1 is controlled by the controller 20 (see FIG. 2 ) based on the input information.
[0030] The touch panel 41 has a screen on which various images are displayed and detects a contact of an indicator 42 (see FIGS. 3( a ) to 3 ( d )) such as a finger or a pen with the screen. The user brings the indicator 42 into contact (touch) with information displayed on the touch panel 41 so as to input his or her desired instruction.
[0031] An electrical configuration of the multifunction peripheral 1 according to the embodiment will next be described with reference to FIG. 2 . FIG. 2 is a block diagram showing the electrical configuration of the multifunction peripheral 1 . The multifunction peripheral 1 includes a parallel interface (I/F) 29 and the USB terminal 71 . The parallel interface 29 is an interface connectable to a PC via a cable. The USB terminal 71 is connectable to a digital camera. The slot portion 72 can detachably mount an external medium (e.g., storage medium such as a memory card or hard disk). With this configuration, image data can be input from the PC, the digital camera, and the external medium to the multifunction peripheral 1 . The connection configuration between the multifunction peripheral 1 and the abovementioned devices (PC, digital camera, external medium) is not limited to this. For example, the multifunction peripheral 1 may be connected to the abovementioned devices via a not shown network I/F.
[0032] The controller 20 functions to control the overall operations of the multifunction peripheral 1 , including the printer 2 , the scanner 3 , and the control panel 4 (see FIG. 1 ). The controller 20 is configured of a microcomputer primarily including a central process unit (CPU) 21 , a read-only memory (ROM) 22 , a random access memory (RAM) 23 , and an electrically erasable and programmable ROM (EEPROM) 24 , which is a rewritable, nonvolatile storage device. The controller 20 is connected to an application specific integrated circuit (ASIC) 26 via a bus 25 .
[0033] The CPU 21 is a central process unit for controlling the entire operation of the multifunction peripheral 1 . The ROM 22 stores various control programs executed by the CPU 21 and fixed values used when the programs are executed. The ROM 22 stores a thumbnail image display program 221 serving as an image process program. A thumbnail image display process to be described later using FIG. 5 is executed by the thumbnail image display program 221 .
[0034] The RAM 23 is a rewritable memory used as a memory area for temporarily storing various data or working area when the CPU 21 executes the above program. The RAM 23 has a load area for storing the program which is instructed to be loaded upon activation of the multifunction peripheral 1 .
[0035] The RAM 23 further has an image file temporary storage area 230 , an image process type storage area 231 , a position information storage area 232 , a selected image storage area 233 , and a determined image process storage area 234 .
[0036] The image file temporary storage area 230 is an area for storing an image file read out from a memory card (not shown) inserted into the slot portion 72 . In the embodiment, the image file to be stored in the image file temporary storage area 230 is, for example, JPEG image data which has original image data and thumbnail data that is for displaying the image file (the original image) in a reduced size as additional information.
[0037] With reference to FIG. 3( a ), thumbnail images 411 which are displayed on the touch panel 41 based on the thumbnail data added to respective image files will be described below. FIG. 3( a ) is a view showing an example of a display screen of the touch panel 41 displaying the thumbnail images 411 . Since each of the thumbnail images 411 is a reduced sample image corresponding to each image file read in the image file temporary storage area 230 , a large number of thumbnail images 411 can be arranged in a matrix on the touch panel 41 , as shown in FIG. 3( a ). In FIG. 3( a ), 12 thumbnail images 411 are arranged in a 3×4 matrix.
[0038] In the embodiment, the display area of the touch panel 41 is divided into a selection area 413 and a dialogue area 414 . The thumbnail images 411 are displayed in the selection area 413 , while a message to the user and operation keys 412 are displayed in the dialogue area 414 . In the example of FIG. 3( a ), a determination key 4121 and a cancel key 4122 are displayed as the operation keys 412 . The user touches one of the operation keys 412 to thereby make a desired input operation. In the embodiment, the images, such as the determination key 4121 and the cancel key 4122 , which are displayed in the dialogue area 414 and which are touched by the user for input of a specific instruction are collectively referred to as operation keys 412 .
[0039] Returning to FIG. 2 , the image process type storage area 231 is an area for storing image process that has been selected from among the image process that the multifunction peripheral 1 can execute. The multifunction peripheral 1 can apply a plurality of kinds of image process to the image file stored in the image process type storage area 231 . The image process that the multifunction peripheral 1 can execute includes, for example, “right-handed rotation” that rotates an image in the right-handed direction, “left-handed rotation” that rotates an image in the left-handed direction, “sepia” that corrects the tone of an image into sepia tone, “order specification” that creates order information to images, “frameless” that eliminates a margin portion of an image, “red eye correction” that removes red eye from an image, “monochrome” that converts a color image into a monochrome one, “date stamping” that stamps date onto an image, “framed” that provides a predetermined margin portion on an image, and “exposure compensation” that compensates the brightness of an image.
[0040] With reference to FIG. 3( b ), image process keys 415 will be described below. FIG. 3( b ) is a view showing an example of a display screen of the touch panel 41 displaying the image process keys 415 . The image process keys 415 are displayed on the touch panel 41 so as to allow the user to designate the image process to be applied. As shown in FIG. 3( b ), the image process keys 415 are arranged in a matrix. The image process keys 415 one-to-one correspond to a plurality of image process that the multifunction peripheral 1 can execute. The user selects a given image process key 415 from among the plurality of image process keys displayed on the touch panel 41 and brings the indicator 42 , such as a finger, into contact (touch) with the selected image process key 415 displayed on the touch panel 41 so as to instruct image process corresponding to the selected image process key 415 . In other words, as shown in FIGS. 3( a ) and 3 ( b ), the selection area 413 has 3×4 divided areas that are obtained by dividing the selection are 413 into 3 rows and 4 columns. As shown in FIG. 3( a ), each of 3×4 areas displays the thumbnail image 411 . As shown in FIG. 3( b ), each of 3×4 areas displays the image process key 415 .
[0041] The image process key 415 touched by the user is lit up like the image process key 415 of “sepia” shown in FIG. 3( b ), so as to be distinguished from other image process keys 415 . As a result, even if the user touches a wrong key, he or she can quickly recognize the operation error.
[0042] The selected image processes are stored in the image process type storage area 231 when the user touches, so as to determine the selected image processes, the determination key 4121 displayed as the operation key 412 on the touch panel 41 in which one or a plurality of image processes are selected.
[0043] Returning to FIG. 2 , the position information storage area 232 is an area for storing a correspondence between image (for example, the thumbnail image) displayed on the touch panel 41 and position information of the image.
[0044] FIGS. 3( c ) and 3 ( d ) are views each schematically showing a configuration of the position information storage area 232 . FIG. 3( c ) shows the storage content of the position information storage area 232 when the thumbnail images 411 are displayed on the touch panel 41 , and FIG. 3( d ) shows the storage content of the position information storage area 232 when the image process keys 415 are displayed on the touch panel 41 .
[0045] As shown in FIGS. 3( c ) and 3 ( d ), the position information storage area 232 stores a coordinate serving as position information indicating the position of each rectangular area that is obtained by divining the display area of the touch panel 41 into, for example, a 3×6 matrix (3 rows and 6 columns).
[0046] The coordinate stored in the position information storage area 232 is represented by an x-coordinate and a y-coordinate in a coordinate system where the observer's lower right of the touch panel 41 is set as the origin, a horizontal direction is set as an x-axis, and a vertical direction is set as a y-axis. In FIG. 3( c ), a coordinate in which x-coordinate is i and y-coordinate is j is represented as XiYj where i and j are natural numbers. The touch panel 41 detects a contact of the indicator 42 therewith based on, e.g., a pressure applied thereto and outputs a coordinate of the position at which the contact is detected.
[0047] Further, when the thumbnail images 411 are displayed on the touch panel 41 as shown in FIG. 3( a ), image file names (P 1 , P 2 , . . . ) of the thumbnail images 411 displayed at their respective coordinates are stored in the position information storage area 232 in association with the respective coordinates, as shown in FIG. 3( c ).
[0048] Further, when the image process keys 415 are displayed on the touch panel 41 as shown in FIG. 3( b ), image process names corresponding to the image process keys 415 displayed at their respective coordinates are stored, in place of the abovementioned image file name, in the position information storage area 232 in association with the respective coordinates, as shown in FIG. 3( d ).
[0049] Thus, by referring to the position information storage area 232 based on the coordinate corresponding to the contact position output by the touch panel 41 , the thumbnail image 411 or the image process selected by the user can be identified.
[0050] For example, as shown in FIG. 3 ( d ), the image process name “right-handed rotation” is associated with a coordinate X3Y2 on the position information storage area 232 , so that when the user touches the “right-handed rotation” key displayed at the coordinate X3Y2, the CPU 21 determines that the user instructs to select “right-handed rotation” based on the coordinate.
[0051] Returning to FIG. 2 , the selected image storage area 233 is an area for storing information indicating whether each of the thumbnail images 411 displayed on the touch panel 41 is a selected thumbnail image which has been selected by the user or a non-selected thumbnail image which has not been selected by the user. Details of the “selected thumbnail image” and “non-selected thumbnail image” will be described later with reference to FIG. 5 .
[0052] The determined image process storage area 234 is an area for storing information (attribute information) indicating the image process which has been determined to be applied to each image file stored in the image file temporary storage area 230 .
[0053] FIG. 4 is a view schematically showing a configuration of the determined image process storage area 234 . When the user determines, by using the touch panel 41 , an image process and an image file to which the determined image process is to be applied, the determined image process is stored as attribute information of the determined image file. For example, since, as shown in FIG. 4 , an image files P 1 is associated with “sepia” as the attribute information in the determined image process storage area 234 , the image process “sepia” are applied to the image file P 1 . Further, since image file P 2 is associated with the “sepia” and “right-handed rotation” as the attribute information in the determined image process storage area 234 , the image processes “sepia” and “right-handed rotation” are applied to the image file P 2 .
[0054] Returning to FIG. 2 , the ASIC 26 will be described below. The ASIC 26 is connected to the controller 20 via the bus 25 . A panel gate array (panel GA) 27 for controlling the operation keys 40 used for the user to input his or her desired instruction to the multifunction peripheral 1 is connected to the ASIC 26 . The panel gate array 27 detects a depression (input operation) of a operation key 40 and outputs a prescribed code signal. Each of operation keys 40 is assigned to a respective code signal (key code). Upon receiving a prescribed key code from the panel gate array 27 , the CPU 21 performs requested control process according to a prescribed key process table.
[0055] A touch panel controller 28 is connected to the ASIC 26 . The touch panel controller 28 is for controlling the display screen of the touch panel 41 . The touch panel controller 28 displays, under the control of the CPU 21 , an image corresponding to data received from a connected external device or a memory card inserted into the slot portion 72 .
[0056] Further, an NCU (Network Control Unit) 31 is connected to the ASIC 26 . The NCU 31 is connected to a general public line (not shown) so as to realize a facsimile function. In addition, a modem 32 is connected, via the NCU 31 to the ASIC 26 .
[0057] Next, with reference to FIG. 5 and FIGS. 6( a ) to 6 ( f ), the thumbnail image display process will be described. The thumbnail image display process is executed in the multifunction peripheral 1 having the configuration described above. FIG. 5 is a flowchart showing the thumbnail image display process executed by the multifunction peripheral 1 , and FIGS. 6( a ) to 6 ( f ) are views showing the transition of the display of the touch panel 41 . In the following, the flowchart of FIG. 5 will be described with appropriate reference to FIGS. 6( a ) to 6 ( f ).
[0058] The thumbnail image display process is executed when a memory card is inserted into the slot portion 72 by the user to cause image files stored in the memory card is loaded into the image file temporary storage area 230 (see FIG. 2 ). When the cancel key 4124 is touched by the user during execution of the thumbnail image display process, this thumbnail image display process is ended.
[0059] First, in S 2 the CPU 21 controls the touch panel 41 to display m image process keys 415 (see FIG. 3( b )) in the selection area 413 . The “m” is a predetermined natural number equal to or more than 2. When the number of image processes to be displayed as choices exceeds the “m”, i.e., when the image process keys 415 corresponding to all the image processes cannot be displayed, a cursor key (not shown) may be used to scroll up and down the image process keys 415 . FIG. 6( a ) shows an example of the touch panel 41 displaying the image process keys 415 to change the image processes keys 415 . In this example, 12 image process keys 415 are displayed.
[0060] Returning to FIG. 5 , and description will now be continued. In S 4 the CPU 21 determines whether or not any of image process key 415 has been touched. Concretely, the CPU 21 detects a contact of the indicator 42 with the touch panel 41 , and determines whether or not the x-coordinate of the contact position falls between 0 and 3.
[0061] When there is a touch on the given image process key 415 (S 4 : Yes), that is, the CPU 21 detects a contact of the indicator 42 with the touch panel 41 , and determines that the x-coordinate of the contact position falls between 0 and 3, in S 6 the CPU 21 light up the touched image process key 415 . Then, in S 8 the CPU 21 determines whether or not the determination key 4121 displayed at a coordinate (4,0) has been touched. When the determination key 4121 has not been touched (S 8 : No), the CPU 21 returns to S 4 , and repeats steps S 4 and subsequent process. Accordingly, when another image process key 415 is touched (S 4 : Yes), the CPU 21 light up the touched image process key 415 . When any of the image process keys 415 have not been touched (S 4 : No), the CPU 21 skips S 6 and proceeds to S 8 .
[0062] When the user has selects all the desired image process, and touches the determination key 4121 in a state where at least one image process key 415 is lit up (S 8 : Yes), in S 10 the CPU 21 stores, in the image process type storage area 231 , each image process corresponding to the lit up image process key 415 , that is, image process selected by the user.
[0063] FIG. 6( b ) shows an example of a display screen of the touch panel 41 when the determination key 4121 is touched by the user. As shown in FIG. 6( b ), the user selects a given image process (in this example, “sepia”) and touches the determination key 4121 to thereby determine any of the plurality of image processes that can be executed by the multifunction peripheral 1 .
[0064] Returning to FIG. 5 , in S 12 the CPU 21 switches the display in the selection area 413 on the touch panel 41 from the m image process keys 415 , to m thumbnail images 411 .
[0065] When the number of the image files that have been loaded is less than m, thumbnail images 411 corresponding to all the loaded image files are displayed on the touch panel 41 . When the number of the image files that have been loaded exceeds the “m”, i.e., when thumbnail images 411 corresponding to all the image files cannot be displayed, a cursor key (not shown), for example, may be used to scroll up and down the thumbnail images 411 to change the thumbnail images 411 .
[0066] FIG. 6( c ) shows an example of a display screen of the touch panel 41 when the process of S 12 is executed. As shown in FIG. 6( c ), when the thumbnail images 411 are displayed, a message, such as “sepia is being applied” is displayed so as to allow the user to confirm the image process that has been determined is displayed in the dialogue area 414 . Thus, the user can select the thumbnail image while visually confirming the image process to be applied.
[0067] Returning to FIG. 5 , in S 14 the CPU 21 determines whether or not any of thumbnail images 411 displayed on the touch panel 41 has been touched. That is, the touch panel 41 detects the thumbnail image 411 is touched, and then the CPU 21 receives the selection instruction to select the thumbnail image 411 based on the detection of the touch panel 41 .
[0068] When the CPU 21 determines that the thumbnail image 411 has been touched by the user (S 14 : Yes), in S 16 the CPU 21 refers the selected image storage area 233 that stores information indicating whether each of the thumbnail images 411 is the selected thumbnail image or non-selected thumbnail image. Accordingly, the CPU 21 determines whether or not the touched thumbnail image 411 is the selected thumbnail image that has been selected by the user.
[0069] In the initial state, since no selected thumbnail image is displayed on the touch panel 41 , the touched thumbnail image 411 is determined not to be the selected thumbnail image (S 16 : No). Thus, this case (S 16 : No) will be described. In this case, in S 22 the CPU 21 lights up the touched thumbnail image and replaces the touched thumbnail with a thumbnail image representing a result of the image process stored, in association with the touched image, in the image process type storage area 231 .
[0070] Then, in S 26 the CPU 21 stores information indicating that the touched thumbnail image is the selected thumbnail image in the selected image storage area 233 , and the CPU 21 proceeds to S 28 . In the description, the thumbnail image 411 touched by the user and representing a result of the image process stored in the image process type storage area 231 is referred to as “selected thumbnail image” and thumbnail image that has not been touched by the user, that is, thumbnail image which is not the “selected thumbnail image” is referred to as “non-selected thumbnail image”.
[0071] FIG. 6( d ) is a view showing an example of a display screen on which the thumbnail image that has been touched by the user is replaced, in the step S 22 , with a thumbnail image representing the image process result. As shown in FIG. 6( d ), when the user instruct to select the thumbnail image 411 , the selected thumbnail image 411 is replaced with a thumbnail image 411 representing a result of the image process (in this case, “sepia” process) that has been previously determined, on the image data corresponding to the selected thumbnail image 411 . With this configuration, the user can visually confirm a result of the image process in a moment only by touching the thumbnail image 411 . Since the thumbnail images other than the thumbnail image that has been touched by the user are displayed without modification at the same positions. Accordingly, the user can visually confirm a relationship between the thumbnail image representing the image process result and other thumbnail images to thereby determine, in a comprehensive manner, the influence exerted by the image process.
[0072] In the embodiment, the image process stored in the image process type storage area 231 is applied to the thumbnail data added to each image file to obtain thumbnail data that has been subjected to the image process. A thumbnail image (e.g., thumbnail image subjected to image process “sepia”) representing the process result is displayed based on the obtained thumbnail data. Alternatively, the image process stored in the image process type storage area 231 may be applied to an image file which is the original data of the thumbnail image 411 to obtain an image file that has been subjected to the image process. In this case, thumbnail data is created from the obtained image file. A thumbnail image representing the image process result is displayed based on the created thumbnail data.
[0073] Returning to FIG. 5 , in S 28 the CPU 21 determines whether or not the determination key 4121 displayed at the coordinate (4,0) has been touched. When the determination key 4121 has not been touched (S 28 : No), the CPU 21 returns to S 14 , where the determination process is repeated. That is, every time a thumbnail image 411 is touched (S 14 : Yes), in S 16 the CPU 21 determines whether the touched thumbnail image is the selected thumbnail image. When the touched thumbnail image 411 is not the selected thumbnail image (S 16 : NO), in S 22 the CPU 21 replaces the touched thumbnail image with a thumbnail image representing a result of the image process stored, in association with the touched image, in the image process type storage area 231 .
[0074] Thus, the user can visually confirm the result of the image process that has been determined to be applied to the touched thumbnail image 411 in a moment only by a simple operation of only touching the thumbnail image 411 . Further, every time a thumbnail image 411 is touched by the user, the touched thumbnail image 411 is substituted with a thumbnail image 411 representing a result of the image process, so that only a small number of operation is required even in the case where results of the image process applied to a large number of thumbnail images 411 are required to be confirmed, resulting in good operability.
[0075] Next, a case (S 16 : Yes) where the thumbnail image 411 that has been touched by the user is determined to be the selected thumbnail image will be described. As described above, the selected thumbnail image is displayed in a state showing a result when the image process, that is stored in the image process type storage area 231 , is performed on the image data corresponding to the selected thumbnail image. Thus, when such a selected thumbnail image is touched, in S 18 the CPU 21 replaces the touched thumbnail image with a thumbnail image 411 representing a result of process obtained by canceling the image process stored in the image process type storage area 231 , i.e., most recently determined image process. In other words, the CPU 21 replaces the touched thumbnail image representing the result of the image process performed on the image data, with the thumbnail image 411 representing the image data without performing the image process stored in the image process type storage area 231 when the selected thumbnail image is touched by the user. In S 20 the CPU 21 stores the thumbnail image that has been touched by the user in the selected image storage area 233 as the non-selected thumbnail image.
[0076] FIG. 6( e ) is a view showing an example of a state where one selected thumbnail image representing a result of the image process “sepia” is replaced with a thumbnail image 411 representing a process result obtained by canceling the image process “sepia” when the user touches the selected thumbnail image. As shown in FIG. 6( e ), a simple operation of touching the selected thumbnail image allows the user to confirm a result of image process obtained by canceling the image process stored in the image process type storage area 231 . As a result, the user can adequately determine whether or not the intended image process is applied to image data corresponding to the thumbnail image.
[0077] Returning to FIG. 5 , in S 28 the CPU 21 determines whether or not the determination key 4121 displayed at the coordinate (4,0) has been touched by the user. When the CPU 212 determines that the determination key 4121 has not been touched (S 28 : No), the CPU 21 returns to S 14 , and the step S 14 and subsequent steps are repeated.
[0078] When the CPU 21 determines that the determination key 4121 displayed at the coordinate (4,0) is touched in the above repetition (S 28 : Yes), in S 30 the CPU 21 stores, during the determined image process storage area 234 (see FIG. 4 ), the image process that is stored in the image process type storage area 231 as attribute information of an image file corresponding to the selected thumbnail image. According to the attributed information, the image process determined by the user is executed for respective image files.
[0079] Subsequently, in S 32 the CPU 21 controls the touch panel 41 to display, in the dialogue area 414 , a message inquiring whether or not there is subsequent process.
[0080] FIG. 6( f ) is a view showing an example of a state where the message is displayed in the dialogue area 414 by the process of S 32 . As shown in FIG. 6( f ), two operation keys 412 of “Yes” ( 4122 ) and “No” ( 4121 ) are displayed in the dialogue area 414 so as to allow the user to input his or her answer to the message.
[0081] Returning to FIG. 5 , when the CPU 21 determines that the operation key 412 of “No” has been touched (S 34 : No), the CPU 21 ends the process.
[0082] When the CPU 21 determines that the operation key 412 of “Yes” has been touched (S 34 : Yes), in S 36 the CPU clears the image process type storage area 231 . In S 38 the CPU 21 stores, in the selected image storage area 233 , all the thumbnail images as the non-selected thumbnail images. Subsequently, the CPU 212 returns to S 2 , where the CPU 21 switches the display in the selection area 413 on the touch panel 41 from the screen displaying thumbnail images 411 to the screen displaying the image process keys 415 , and subsequent steps are repeated.
[0083] According to the above procedure, when the user newly determines his or her desired image process, the newly determined image process is stored in the image process type storage area 231 (see FIG. 2 ). That is, only the image process that has most recently been determined is always stored in the image process type storage area 231 . Then, by repeating the same operation procedure, a result of the newly determined image process for a given thumbnail image 411 can be confirmed. Thus, with a simple operation, a result of various types of image process can visually be confirmed.
[0084] When in S 14 a new image process is selected and determined, the thumbnail images 411 are displayed on the touch panel 41 . At this time, if determined image process corresponding to some thumbnail image 411 is stored in the determined image process storage area 234 as the attribute information, this thumbnail image 411 is displayed in a state showing a result of image process on the image file corresponding to this thumbnail image 411 . This allows the user to consider whether or not to add another image process while visually confirming the result of the determined image process by the thumbnail images 411 .
[0085] FIGS. 7( a ) to 7 ( c ) are views showing an example of a display screen of the touch panel 41 when two or more image process have been determined in the process from S 4 to S 10 . As shown in FIG. 7( a ), when the determination key 4121 is touched with the “left-handed rotation” and “sepia” selected, the “left-handed rotation” and “sepia” are simultaneously applied to the touched thumbnail image 411 as shown in FIG. 7( b ). As described above, even in the case where a plurality of image process are selected and determined, the user can visually confirm in a moment a result of the applied image process.
[0086] Further, in the operation procedure according to the embodiment, as shown in FIG. 7( a ), the image process keys 415 are first displayed on the touch panel 41 . When some image process is selected and the determination key 4121 is touched, the image process keys 415 are disappeared from the touch panel 41 . Then, as shown in FIG. 7( b ), the thumbnail images 411 are displayed on the touch panel 41 . This configuration effectively utilizes a limited space of the touch panel 41 , thereby largely displays the thumbnail images 411 and image process keys 415 in an easy to view manner. Further, the image process keys 415 and thumbnail images 411 are both displayed at the same area (in the selection area 413 ), so that the user needs only to pay attention to the selection area 413 , resulting in good visibility.
[0087] Further, in the embodiment, the image process keys 415 are displayed in the selection area 413 on the touch panel 41 in a 3×4 matrix (3 rows and 4 columns), and the thumbnail images 411 are displayed in a 3×4 matrix (3 rows and 4 columns) as well. That is, the image process keys 415 and thumbnail images 411 are arranged in the same layout. Thus, even in the case where the display is switched from process keys 415 to thumbnail images 411 , or conversely, where the display is switched from the thumbnail images 411 to image process keys 415 , the user needs only to pay attention to a change in the same area, resulting in good visibility. Further, the user needs only to pay attention to the operation in the same area, resulting in good operability. Thus, the user can continue performing operation without experiencing discomfort even when the display state is switched.
[0088] Next, with reference to FIG. 7( c ) and FIG. 8 , a control process performed by the multifunction peripheral 1 according to a second embodiment will be described. In the multifunction peripheral 1 according to the second embodiment, thumbnail images before and after image process corresponding to a touched thumbnail image are displayed side-by-side. In the second embodiment, the same reference numerals as the first embodiment are given to the parts which are common to the first embodiment, and the overlapped description is omitted.
[0089] FIG. 8 is a flowchart showing a part of thumbnail image display process performed in the multifunction peripheral 1 according to the second embodiment. The thumbnail image display process according to the second embodiment differs from that of the first embodiment in that steps from S 140 to S 280 shown in FIG. 8 are executed in place of the steps from S 14 to S 28 in the flowchart shown in FIG. 5 .
[0090] The flowchart shown in FIG. 8 shows the process after S 12 of FIG. 5 , that is, after the user selects and determines an image process, and the thumbnail images 411 are displayed in the selection area 413 on the touch panel 41 .
[0091] First, in 5140 the CPU 21 determines whether or not the thumbnail image 411 displayed on the touch panel 41 has been touched. When the CPU 21 determines that the thumbnail image 411 has been touched by the user (S 140 : Yes), in S 150 the CPU 21 determines whether or not the touched thumbnail image 411 is the selected thumbnail image. When the CPU 21 determines that the touched thumbnail image 411 is the selected thumbnail image (S 150 : Yes), the CPU 21 returns to S 140 and the steps S 140 and subsequent steps are repeated.
[0092] On the other hand, when the CPU 21 determines that the touched thumbnail image is not the selected thumbnail image (S 150 : No), in S 160 the CPU 21 lights up the touched thumbnail image 411 . The CPU 21 controls the touch panel 41 to display, at a coordinate (4,0) in the dialogue area 414 , a processed thumbnail image 416 (see FIG. 7( c )) that representing a result after the image process, which is stored in the image process type storage area 231 is performed on the image data corresponding to the touched thumbnail image 411 .
[0093] In S 180 the CPU 21 controls the touch panel 41 to display, at a coordinate (5,0) in the dialogue area 414 , an unprocessed thumbnail image 417 representing the image before image process is performed, that is, the thumbnail image at the time when the thumbnail image 411 is touched by the user, or the same thumbnail image as the touched thumbnail image 411 .
[0094] FIG. 7( c ) is a view showing an example of a display screen of the touch panel 41 in the multifunction peripheral 1 according to the second embodiment. As shown in FIG. 7( c ), when one thumbnail image 411 is touched, the processed thumbnail image 416 and the unprocessed thumbnail image 417 , which correspond to the touched thumbnail image 411 , are displayed in the dialogue area 414 . As can be seen from FIG. 7( c ), the processed thumbnail image 416 and the unprocessed thumbnail image 417 have the same size and are arranged side-by-side in the dialogue area 414 . In other words, the processed thumbnail image 416 and the unprocessed thumbnail image 417 have the same reduction ratio to an image size of the original image data. With this configuration, the user easily compares the two thumbnail images to thereby adequately determine whether or not to apply the image process. Further, as described later, the processed thumbnail image 416 and the unprocessed thumbnail image 417 function also as the operation key 412 .
[0095] Returning to FIG. 8 , in S 190 the CPU 21 determines whether or not the unprocessed thumbnail image 417 has been touched. When the unprocessed thumbnail image 417 has been touched (S 190 : Yes), in S 200 the CPU 21 erases the processed thumbnail image 416 and the unprocessed thumbnail image 417 , instead, displays the operation key 412 such as the determination key 4121 and cancel key 4122 , and a massage inquiring whether or not the current image process is determined. Subsequently, in S 280 the CPU 21 determines whether or not the determination key 4121 displayed at the coordinate (4,0) has been touched by the user. When the CPU makes a positive determination, that is, the CPU 21 determines that the determination key 4121 at the coordinate (4, 0) has been touched (S 280 : Yes), the CPU 21 proceeds to S 30 of the flowchart shown in FIG. 5 . When the CPU 21 makes a negative determination, that is, the CPU 21 determines that the determination key 4121 at the coordinate (4, 0) has not been touched, the CPU 21 returns to S 140 .
[0096] On the other hand, when the CPU 21 determines that the unprocessed thumbnail image 417 displayed in the dialogue area 414 has not been touched (S 190 : No), in S 210 the CPU 21 determines whether or not the processed thumbnail image 416 in the dialogue area 414 has been touched. When the CPU 21 determines that the processed thumbnail image 416 has been touched (S 210 : Yes), the CPU 21 controls the touch panel 41 to replace the touched thumbnail image 411 in the selection area 413 with the unprocessed thumbnail image 417 . Subsequently, in S 230 the CPU 21 stores the replaced thumbnail image 411 as the selected thumbnail image in the selected image storage area 233 , and the CPU 21 proceeds to S 200 .
[0097] When the CPU 21 determines that the unprocessed thumbnail image 417 displayed in the dialogue area 414 has not been touched (S 190 : No), and when the CPU determines that the processed thumbnail image 416 displayed in the dialogue area 414 has not been touched (S 210 : No), the CPU 21 proceeds to S 200 .
[0098] In the multifunction peripheral 1 according to the second embodiment, the processed thumbnail image 416 and the unprocessed thumbnail image 417 are simultaneously displayed. This allows the user to adequately determine whether or not to apply the image process to image data corresponding to the processed thumbnail image 416 and the unprocessed thumbnail image 417 .
[0099] While the invention has been described in detail with reference to the above embodiments thereof, it would be apparent to those skilled in the art that various changes and modifications may be made therein without departing from the spirit of the invention.
[0100] For example, although the touch panel 41 provided in the multifunction peripheral 1 is configured to detect a contact of the indicator therewith in the above embodiments, the invention may be applied to case where a touch panel configured to detect proximity of the indicator thereto.
[0101] Further, in the above embodiments, image files stored in the memory card are loaded into the image file temporary storage area 230 (see FIG. 2 ), and the thumbnail images 411 in the respective image files are displayed on the touch panel 41 . Alternatively, the invention may suitably be applied to a configuration in which thumbnail data is created from image data scanned by the scanner 3 and thumbnail images corresponding to the created image data are displayed on the touch panel 41 . Or, the invention may also be applied to a configuration in which thumbnail images in respective image files received from an external device are displayed on the touch panel 41 .
[0102] Further, in the first embodiment, when the touched thumbnail image 411 is the selected thumbnail image, that is, an image representing a result of the image process that has already been selected (S 16 : Yes), in S 18 the touched thumbnail image 411 is replaced with a thumbnail image 411 representing a result of process obtained by canceling the most recently selected image process. Alternatively, when the user touches again the selected thumbnail image, the thumbnail image 411 is replaced with an image representing a result when the image process is applied to the image data once again. For example, when the selected thumbnail image shows a result of the image process “right-handed rotation” that is stored in the image process type storage area 231 , the currently displayed thumbnail image 411 represents a state where the “right-handed rotation” image process has already been performed on the image data. When the user further touches this selected thumbnail image again, the current thumbnail image 411 (selected thumbnail image) may be replaced with a thumbnail image 411 representing a state where the additional “right-handed rotation” image process has been performed on the image data.
[0103] Further, in the thumbnail image display process according to the first embodiment, when a touched thumbnail image is a selected thumbnail image (S 16 : Yes), in S 18 the touched thumbnail image is replaced with a thumbnail image representing a result of process obtained by canceling only the most recently selected image process. Alternatively, the touched thumbnail image may be replaced with a thumbnail image representing a result of process obtained by canceling all the selected image process.
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An image processing apparatus includes a display, a retrieving unit, a process display unit, a process receiving unit, a process storing unit, a thumbnail display unit, and a thumbnail designating unit. The retrieving unit retrieves image data. The process display unit displays on the display a plurality of candidate image processes to be performed on the image data. The process receiving unit receives an instruction indicating a selected image process selected from among the plurality of candidate image processes. The process storing unit stores the selected image process. The thumbnail display unit displays a thumbnail image corresponding to the image data on the display. The thumbnail designating unit designates a thumbnail image. The thumbnail display unit displays a processed thumbnail image that represents a result of the selected process performed on the image data corresponding to the designated thumbnail image.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation application of U.S. patent application Ser. No. 10/494,405, filed Oct. 26, 2004, which is the U.S. National Phase application of PCT International Application No. PCT/GB02/04724, filed Oct. 18, 2002, and claims priority of British Application No. 0126346.6, filed Nov. 2, 2001, all of which are incorporated herein by reference.
FIELD OF THE INVENTION
The present invention concerns improvements in materials handling, more especially it concerns improvements in the sampling, and eventual analysis or assay, of variable feedstocks.
BACKGROUND OF THE INVENTION
Many processes involve the sampling of bulk variable feedstocks, and this has especial importance where the feedstock contains one or more high value components. For example, in the recycle and refining of waste catalysts, or other wastes containing materials such as the platinum group metals, silver and gold, the refining organisation needs to determine levels of such metals in the bulk material to assess the value of metals to be credited to the owner of the bulk material. There is a need for improved sampling methods and, accordingly, for improved metal assays.
SUMMARY OF THE INVENTION
The bulk materials acting as feedstocks in the present invention may be in any non-gaseous form, for example liquid, such as waste homogeneous catalyst, solid or slurry. If the feedstock is a solid, such as a filter cake or other solid form, it is necessary to break up the solid, by for example crushing or milling so that the bulk is dispersible. Desirably, the particle size of solids is less than 500 μm, preferably less than 100 μm, bearing in mind the need to obtain suspension as a homogeneous slurry.
The present invention accordingly provides a method of refining comprising receiving a bulk sample of unknown composition, sampling the bulk sample to yield a reduced volume sample, assaying said reduced volume sample for one or more desired components, calculating the content of one or more desired components in the bulk sample, and passing the remaining bulk sample to a refining process; wherein sampling of the bulk sample comprises dispersing the bulk sample in a liquid, stirring the resulting dispersion in a mixing tank, continuously withdrawing from the bottom section of the tank a portion of the dispersion and recycling it via a recycle loop to the upper portion of the tank such that a substantially homogeneous dispersion is obtained in at least the recycle loop, and taking a representative sample of dispersion from the recycle loop. If necessary, the reduced volume sample may be subsequently sub-divided and representative sub-division samples are assayed or analysed for key components in conventional manner.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described by way of example only and with reference to the accompanying drawings in which;
FIG. 1 shows a schematic representation of apparatus for carrying out sampling according to the invention; and,
FIG. 2 is a graph comparing metal values for a range of samples evaluated using the method of the present invention with those obtained using conventional pyrolysis.
DETAILED DESCRIPTION OF THE INVENTION
Preferably, the refining process is a supercritical water oxidation process as described in WO 01/83834. For technical reasons, conventional refining techniques do not sample and assay the bulk sample, but only sample and assay after one or more preliminary concentration or refining steps. Accordingly, the present invention represents a significant departure from the state of the art, and is believed to offer advantages in speed of processing, and hence significantly reduce the cost of financing “work in progress”.
The method of sampling according to the invention desirably uses a conical-ended stirred mixing tank, fitted with a pipe at the apex of the cone. Other tank shapes may, however, be used, for example a hemispherical, frusto-conical or similar section base. The recycle of dispersion is to the upper section of the tank, and may be made to any one or more points in said upper section. Conveniently, a single recycle point is approximately half-way along a radius of the tank.
Suitable mixing speeds, impeller shapes, recycle line diameters and recycle rates may vary according to the volume of the mixing tank and volume of the sample dispersion, and may be established by routine experiment. The aim is, of course, to ensure that the representative sample taken from the recycle loop is truly representative and this is essentially achieved by ensuring that the dispersion is homogenised.
Particularly preferred bulk sample feedstocks are spent catalysts, especially those comprising a platinum group metal carried on a carbon support. Such spent catalysts generally contain considerable quantities of organic solvent. However, since these are often regarded as wastes, they may be contaminated with a variety of organic (e.g. paper, cloth etc.) or inorganic (e.g. nuts and bolts etc.) matter. Such contaminating matter is desirably screened out.
Suitable liquid or slurry samplers are commercially available for use in the recycle loop. The volume taken is not especially important.
The methods used for assay or further analysis are conventional and form no part of this invention. Similarly, refining methods may be conventional or the supercritical water method of WO 01/83834.
Depending upon the nature of the bulk sample and especially the nature of solvents or residues associated with the values in the bulk sample, an additive to improve dispersion in the liquid may be required. The liquid is advantageously water, and conventional and commercially available surfactants may be used if the bulk sample is essentially non-polar. Initial tests on bulk samples which have a polar character indicate that certain surfactants, e.g. “Quadralene”™ (used for glassware washing machines) may be advantageously used.
Suitable concentrations of bulk sample in the liquid are from 10-15 wt %. Conveniently, the bulk sample, crushed or milled if necessary, is added, together with an appropriate surfactant, to the tank already charged with water, mixing is begun and the recycle initiated.
With reference to FIG. 1 , apparatus for carrying out the invention includes a mixing tank, 1 . In proving trials, a steel tank of 600 liter capacity, with a conical bottom, has been used. A conventional axial impeller, 2 , is fitted in tank 1 , to mix the contents. A recycle line, 3 , of 19 mm internal diameter is attached to the conical base of tank 1 .
The recycle line is connected to a pump, 4 , before being returned to the upper section of tank 1 . The pump has been operated at 4400 l/hr. Fitted downstream of the pump is a commercial liquid/slurry sampler “Isolock”™ 5 , which collects a sample volume of 500 ml.
The recycle line may include a line, 6 , to allow the contents of the tank to be emptied or further processed.
The charge of bulk sample is conveniently received in a bulk container, 7 , fitted with a pump, 8 , for water, wash water and/or surfactant. The bulk sample is fed to a screen, 9 , to remove gross contaminants; a screen size of 3-10 mm size is generally appropriate for spent carbon-based catalyst.
The sample is suitably passed to an assay laboratory, where it is resuspended and kept agitated. Sub-samples may be taken by using tube sampling. It is generally good practice to take a number of samples, some of which may be retained as a reference sample, to minimise the opportunity for process variability.
For example, where the bulk sample consists essentially of spent carbon-supported catalyst with organic solvent, it is preferred to oxidise all organic/carbonaceous material to CO 2 , using a mixture of sulphuric and nitric acids. The residual precious metal can then be dissolved in a pre-set volume of aqua regia and analysed, for example using Inductively Coupled Plasma Emission Spectroscopy against standard solutions of known platinum group metal content.
EXAMPLE
Fifty-one catalyst samples were evaluated using the method of the invention. The samples were sourced from a wide range of used and unused materials with a range of physical properties and impurities. Results are shown in Table 1. Recovery is measured as the ratio (expressed as a percentage) between the amount of metal evaluated in each sample using the method of the invention and that evaluated by conventional pyrolysis. Excellent agreement was found between the two methods indicating that method of the invention provides an accurate and reliable measure of total metal content. The results of Table 1 are illustrated graphically in FIG. 2 , with a line of unit gradient for reference.
It will be appreciated by the skilled person, that the method and apparatus as described may be varied in many ways. The invention includes all novel items and novel combinations and equivalents thereof. The skilled person may readily adapt the description herein in order to optimise the invention for particular circumstances.
TABLE 1
Sample No.
Recovery/%
1
100.6
2
100.7
3
96.3
4
98.5
5
103.5
6
180.4
7
128.6
8
99.5
9
94.2
10
106.7
11
101.0
12
96.7
13
94.5
14
94.7
15
99.8
16
96.3
17
101.4
18
102.0
19
96.6
20
103.6
21
94.0
22
100.0
23
94.9
24
92.4
25
191.1
26
98.6
27
95.0
28
103.2
29
92.6
30
67.6
31
99.0
32
105.2
33
104.5
34
39.9
35
92.3
36
100.7
37
96.2
38
95.6
39
104.7
40
105.7
41
106.7
42
96.7
43
104.9
44
101.8
45
94.3
46
109.1
47
103.3
48
105.3
49
118.4
50
92.1
51
97.0
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A bulk sample is fed with a liquid into a mixing tank ( 1 ) where it is stirred to form a dispersion. A proportion of the dispersion is recycled from the bottom of the tank through a line to the top of the tank so that at least the dispersion in the recycle loop ( 3 ) is substantially homogeneous, and a representative sample of the dispersion is taken from the recycle loop, e.g. using a slurry sampler ( 5 ).
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FIELD OF THE INVENTION
The present invention relates to a break-over photodiode.
BACKGROUND INFORMATION
German Patent No. 44 17 164 describes a break-over photodiode that can be stacked with a plurality of additional break-over photodiodes. This stack represents a light-sensitive high-voltage switch. Each break-over photodiode of this stack has a light-sensitive region illuminated by light-emitting elements so that at a predefined time, for example, in an ignition voltage distributor of a car at the time of the ignition of the cylinder pertaining to the light-sensitive high-voltage switch, the break-over photodiode switches through. With the disclosed design of the individual break-over photodiodes, light sensitivity to lateral illumination is a critical parameter, as is the minimum required light flux for triggering the break-over photodiode, which should be reduced. Furthermore, it is desirable to ensure that the break-over photodiode, in particular a stack of break-over photodiodes, will not switch through in an undesirable manner as a result of parasitic or displacement currents.
SUMMARY OF THE INVENTION
The arrangement according to the present invention has the advantage of an increased light sensitivity in an edge region that can be laterally illuminated. Thus, the break-over photodiode can be triggered through lateral illumination even when voltages that are low in comparison to the break-over voltage are applied.
By selecting the thickness of an n - layer in an appropriate manner, a higher current amplification can be achieved within the break-over photodiode than at its edges. This has proven to be advantageous for a homogeneous current distribution when the break-over photodiode switches through. Thus, a concentration of higher currents in the edge region of the break-over photodiode due to the high field intensities prevailing there can be counteracted.
It is further advantageous to dimension an edge-gate-cathode resistivity formed by a p region located between the n - region and the edge emitter so that a break-over of the break-over photodiode occurs without the central region being illuminated. The break-over photodiode has a high break-over current in such case, which protects the diode from unintentional switching due to parasitic currents and/or cut-off currents. Such advantage is particularly important in the case of small chip surfaces or when no other methods for protecting the break-over photodiode from undesired switching are available.
Designing a rand emitter located in the edge region with a greater thickness than that of an emitter located in the central area and/or selecting the doping profile of the edge emitters and internal emitter in an appropriate manner is a simple way of making an edge-gate-cathode resistivity greater than a center-gate-cathode resistivity located in the central area.
In order to design the edge-gate-cathode resistivity to be greater than the center-gate-cathode resistivity, the gate can be dimensioned appropriately in the edge region or the central region. This provides another advantage of a larger effective base width of an npn partial transistor in the edge region, and prevents the current from being excessively amplified in the edge-region.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a conventional break-over photodiode for lateral illumination.
FIG. 2 shows a break-over photodiode with an avalanche geometry.
FIG. 3 shows a break-over photodiode with a punch-through geometry.
FIG. 4 shows a first embodiment according to the present invention.
FIG. 5 shows a second embodiment according to the present invention.
DETAILED DESCRIPTION
FIG. 1 shows a conventional break-over photodiode 100, provided for lateral illumination 9 in an edge region 110. Henceforward, the symbols for a break-over photodiode designed as a pnpn thyristor will be used for all figures. Replacing "p" with "n" and "anode" with "cathode," the corresponding description of an npnp thyristor design is obtained.
A p region 2 connected to an anode metal plating 1 is followed by an n - region 3, into which a gate 4, configured as a p region, is embedded. An edge emitter 5a is in turn embedded into the edge region 110 of gate 4 as an n region. An internal emitter 5b, consisting of a plurality of adjacent n regions, is embedded into central region 120 of gate 4. Edge emitter 5a, internal emitter 5b, and gate 4 are short-circuited via a cathode metal plating 6. An n + region 8 is embedded on the edges facing away from p region 2 of n - region 3. The area of break-over photodiode 100 that is not covered by cathode metal plating 6 is sealed with a silicon oxide layer 7. p region 2, n - region 3, and gate 4 form a pnp partial transistor, and emitter regions 5a,b, gate 4, and n region 3 form an npn partial transistor. This is the conventional design of a pnpn thyristor, which switches through from a break-over voltage applied between anode metal plating 1 and cathode metal plating 6 in the direction of flow. Alternatively, break-over photodiode 100 can also be triggered under this break-over voltage by lateral light incidence 9. n + region 8 serves as a "channel stop." It limits a space charge region formed before break-over photodiode 100 switches through and thus suppresses surface effects. Silicon oxide layer 7 serves as a protection and electrical insulation. The short circuit between edge emitter 5a, internal emitter 5b, and gate 4 through cathode metal plating 6 reduces the light sensitivity of break-over photodiode 100 to lateral illumination 9 (the minimum required light flux for triggering break-over photodiode 100 below the break-over voltage is set high), but it is required, among other things, that the high sturdiness requirements for break-over photodiode 100 be satisfied with quick voltage changes.
The triggering mechanism of thyristors, configured as break-over photodiodes are discussed in detail below. When a voltage is applied between anode and cathode, the pn junction between gate 4 and n region 3 is blocked. This blockage can be overcome by a build-up of a voltage differential greater than 0.6 V (for silicon at room temperature) between emitter regions 5a,b and gate 4, since then the npn transistor formed by emitter regions 5a,b, gate 4, and n region 3 becomes conducting. Since emitter region 5a,b and gate 4 are short-circuited via the cathode metal plating 6, a sufficient voltage differential can build up between the emitter regions 5a,b and the gate 4 only if a sufficiently high current flows through the p region that forms gate 4. The intensity of the sufficient current depends on the layer resistivity of gate 4 under the emitter region. In edge region 110, an edge-gate-cathode resistivity R -- rand is formed basically by the p region located under edge emitter 5a. In the central region 120, a center-gate-cathode resistivity R -- mitte is basically formed by the p region located under the internal emitter. The magnitude of these resistivities R -- rand and R -- mitte define the current required for triggering the break-over photodiode. Since a photoelectric current is generated by illuminating the edge region 110, the resistivity R -- rand is critical for triggering the break-over photodiode by illuminating i. The greater the resistivity R -- rand, the easier it is to trigger the break-over photodiode by illuminating it. The break-over photodiode can, however, also be triggered without illuminating it if the parasitic currents and/or cut-off currents exceed a certain value. Normally parasitic currents are currents generated as a result of dynamic effects, for example, when a voltage is applied between anode and cathode due to parasitic capacitances or pn junction capacitances. In order to trigger the diode with such currents ("parasitic currents," short for "parasitic and/or cut-off currents"), it is important to determine whether the diode has an avalanche geometry or a punch-through geometry.
FIG. 2 shows a break-over photodiode with an avalanche geometry. This geometry is defined by the fact that break-over of the diode occurs through the avalanche effect, i.e., due to high field intensities. Such high field intensities arise at the high curvatures of space charge region 20 located in edge zone 110 for the geometry illustrated in FIG. 2. Therefore, the parasitic currents flow predominantly in edge zone 110 as illustrated in FIG. 2 through current paths 21. Therefore, in order to trigger this diode by parasitic currents, resistivity R -- rand is also critical, since an increase in R -- rand (which is required for high light sensitivity) also results in an increase in the sensitivity to triggering by parasitic currents. Thus, a high sensitivity to light coupled with a high degree of safety against undesired switching due to parasitic currents is difficult to achieve in such break-over photodiodes.
FIG. 3 shows the case of a break-over photodiode with punch-through geometry, where, contrary to the avalanche geometry, the difference in current amplification of the pnp partial transistor between the edge and central zones is significant. A space charge region 30 approaches p region 2 shortly before switching so that an effective base width, given by the distance of space charge region 30 from p region 2, becomes extremely small. For this to occur, n region 3 must be sufficiently thin. This results in high current amplification even of the currents flowing prior to switching in the central zone of the break-over photodiode. Therefore, despite the high field intensities in the curved area of space charge region 30, most of the parasitic currents flow along current paths 31, which are concentrated in central zone 120 of the break-over photodiode. If the voltage applied between anode and cathode metal plating 1 and 6, respectively (without illumination) is increased until it reaches the "break-over voltage," the voltage that drops at the layer resistivity of gate 4 (described with the explanation to FIG. 1) reaches a certain value (for silicon approximately 0.6 V at room temperature), which results in the break-over photodiode switching through. In the punch-through geometry described above, this voltage drop is first achieved through the currents flowing before switching-through takes place in central area 120 of break-over photodiode 100. Triggering in punch-through geometry through parasitic currents is therefore determined by R -- mitte, as long as the difference between R -- rand and R -- mitte is not so great that the low intensity of the parasitic currents on the edge is overcompensated for by a very large resistivity R -- rand.
Lateral illumination 9 produces charge carriers, which become insulated in the space charge region of edge zone 110. In such case, holes flow to gate 4 and form a current that causes a voltage drop at the layer resistivity of gate 4 in edge zone 110. The punch-through geometry allows reaching a certain voltage drop at gate 4 to be set separately as a condition for the break-over photodiode to switch through, triggered by illumination below the break-over voltage, as well as for switching through to occur as a result of the break-over voltage being reached (without illumination). Also measures other than the use of punch-through geometry are conceivable, of course, which prevent intense parasitic currents from flowing in the edge zone.
R -- rand is critical for triggering as a result of lateral illumination 9 below the break-over voltage, since the light-induced current, which is to deliver the voltage drop required for break-over at the R -- rand (e.g., 0.6 V for silicon at room temperature) only flows in the edge zone (110). The edge zone (110) can have a symmetrical design, so that the break-over photodiode can be illuminated laterally from either side.
On the other hand, current paths 31 of the currents that flow even without illumination prior to reaching the break-over voltage are concentrated in central area 120. They are responsible for the voltage drop required for break-over at R -- mitte. If this voltage drop reaches 0.6 V (for silicon at room temperature), the voltage applied between cathode metal plating (1) and anode metal plating (6) has reached the break-over voltage value and the break-over photodiode switches through.
FIG. 4 shows a first embodiment 210 of a break-over photodiode 100 according to the present invention with thick edge emitter 5a'. Edge emitter 5a' in edge zone 110, which is thick compared to the internal emitter 5b in the central area 120, ensures high layer resistivity of gate 4, and thus a high R -- rand, in the edge zone where charge carriers are produced through lateral illumination 9, due to the small cross section in the lateral direction under edge emitter 5a'. Thus, the minimum light flux required for reaching the triggering condition (a voltage drop of, for example, 0.6 V for silicon at room temperature) is reduced.
FIG. 5 shows a second embodiment 310 of break-over photodiode 100 according to the present invention with a gate 50, which is thinner in edge zone 110 than in central zone 120. As in the case of first embodiment 210, here as well the layer resistivity of the gate in the edge zone and R -- rand is greater than in the central area before the break-over photodiode switches through. Also in this case, increased light sensitivity is obtained to lateral illumination. If a break-over of break-over photodiode 210 or 310 occurs without illumination in the central area 120, in order to ensure a high break-over current, R -- rand must also be selected so that the triggering condition (voltage drop of approx. 0.6 V for silicon at room temperature) is not attained in edge zone 110 of gate 4 first due to the currents flowing before break-over photodiode 210 or 310 switches through, despite the greater current amplification of the pnp partial transistor in central area 120. Thus, the diodes shown in FIGS. 4 and 5, which otherwise have punch-through geometry or other means limiting a considerable portion of the parasitic currents to the central zone, can be triggered with a low light flux and are well-protected from unintended triggering, since parasitic currents flow mainly in the central area.
In embodiments of the photodiodes 210 and 310 according to the present invention, an increased edge-gate-cathode resistivity R--rand can optionally be achieved by a suitable doping profile of gate 4 in the edge and central zones. A combination of a suitable choice of emitter thickness, gate thickness, and doping profile in the edge and central zones is also conceivable.
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A break-over photodiode, designed as a light-sensitive thyristor, can be stacked using a series connection with a plurality of break-over photodiodes, such stacking representing a high-voltage break-over diode. The break-over photodiode can be triggered by lateral illumination in an edge zone, and includes a gate-layer resistivity under the emitter which is greater in an edge zone of the break-over photodiode than in the central zone of the break-over photodiode. The light sensitivity of the laterally illuminatable break-over photodiode is increased by a greater gate-layer resistivity in the edge zone as compared to the central zone.
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BACKGROUND OF THE INVENTION
The present invention relates in general to amusement rides, and, more particularly, to amusement rides in which the riders are subjected to a movement in multiple directions.
Amusement rides are popular forms of entertainment for individuals of all ages. The excitement experienced by riders is often directly related to the ability of the ride to subject the riders to various disorienting motions. For example, the standard ferris wheel is designed so that the riders travel in a circular path about the horizontal rotational axis of the ferris wheel. The riders, however, are generally maintained in an upright position as the ferris wheel rotates and are thus subjected to movement in only a single dimension. Other more complex rides have been designed which subject the riders to movement in two and three dimensions. As one example, a ferris wheel type ride has been developed in which the passenger cars rotate about an axis which is tangential to the circular path of the ferris wheel. This additional dimension of movement increases the disorientation and excitement experienced by the riders.
As riders become accustomed to the range of motions provided by conventional rides, more challenging rides must be developed. A need has thus developed for an amusement ride which subjects riders to movement in multiple dimensions to maintain the high level of thrills sought by many riders.
SUMMARY OF THE INVENTION
It is a primary object of this invention to provide an amusement ride which subjects passengers to movement in multiple dimensions so that greater excitement can be achieved by the disorienting effect of such movement.
To accomplish these and other related objects of the invention, in one aspect the invention is related to an amusement ride comprising: a base; a boom coupled with the base at one end and moveable at the other end from a lowered position to an elevated position; a rotatable top mounted at said other end of the boom, said top being mounted for tilting movement when said boom is in said elevated position; a drive mechanism for causing rotation of said top; a tilting mechanism for cause said tilting of the top; and a plurality of passenger seats mounted at circumferentially spaced apart positions on said top and rotatable with said top in a closed loop, each of said passenger seats being mounted for rotation about axes which are tangential to the loop. Normally, the loop will be circular and the seats are mounted for forward and backward rotation under the influence of inertial and centrifugal forces during operation of the ride.
In another aspect, the invention is related to a method of operating the ride, comprising the steps of rotating the top, raising the boom to elevate the top, tilting the top while elevated and rotating under conditions sufficient to cause the passenger seats to rotate forwardly and backwardly about an axis which is tangential to the rotational path that the seats are carried through by rotation of the top. At the end of the ride sequence, the boom can be lowered while the top is tilted and is still rotating. The top is then stopped from rotating to allow the passengers to disembark from the seats. Optionally, the seats can be locked against forward and backward rotation until the boom has been raised. In order to return the seats to the correct attitude at the end of the ride sequence, the rotational speed of the top can be increased to return the seats to an outward facing orientation. The locking mechanism can then be engaged to prevent forward and backward rotation or pivoting of the seats.
BRIEF DESCRIPTION OF THE DRAWINGS
In the accompanying drawings which form a part of the specification and are to be read in conjunction therewith and in which like reference numerals are used to indicate like parts in the various views:
FIG. 1 is a perspective view of an amusement ride of the present invention shown in an operating position;
FIG. 2 is a top plan view of the amusement ride in a loading position, the ride being shown on a reduced scale from that used in FIG. 1;
FIG. 3 is a side elevation view of the amusement ride taken in vertical section along line 3--3 of FIG. 1 in the direction of the arrows, phantom lines being used to show the loading position and an intermediate position of the ride;
FIG. 4 is an enlarged side elevation view of the ride showing the boom and its operating mechanisms and a fragmentary portion of the rotatable top;
FIG. 5 is a slightly enlarged side elevation view of a passenger seat mounted on an end of a sweep arm, portions of the seat being broken away to illustrate internal components and phantom lines being used to showing the released position for the passenger restraints;
FIG. 6 is a side elevation view of the passenger seat taken in vertical section along line 6--6 of FIG. 1 in the direction of the arrows;
FIG. 7 is a fragmentary top plan view of the end portion of one of the sweep arms showing the braking mechanism used to lock a passenger seat against rotation during passenger loading and unloading;
FIG. 8 is a side elevation view of the sweep arm shown in FIG. 6, portions being broken away to illustrate component parts of the braking mechanism;
FIG. 9 is a top plan view showing one of the passenger seats and fragmental portions of the associated sweep arms;
FIG. 10 is a back elevation view of one of the passenger seats taken in vertical section along line 10--10 of FIG. 5 in the direction of the arrows to show the operating mechanisms for the passenger restraints;
FIG. 11 is an enlarged side elevation view of one of the sweep arms taken within the circle designated by numeral 11 in FIG. 8 and showing further details of the braking mechanism which is shown in a retracted position;
FIG. 12 is a side elevation view similar to that shown in FIG. 11 but showing the braking mechanism in an engaged position; and
FIG. 13 is an end elevation view of the sweep arm taken in vertical section along line 13--13 of FIG. 12 in the direction of the arrows, and showing further details of the braking mechanism.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings in greater detail and initially to FIG. 1, an amusement ride constructed in accordance with the present invention is represented generally by the numeral 20. Ride 20 comprises a top 22 mounted for both rotating and tilting movement and carrying a plurality of circumferentially spaced passenger seats 24. The ride 20 includes a suitable base 26 which can be permanently installed at an amusement park or can be constructed for ready disassembly if the ride 20 is intended to be transported, between various site locations. A circular loading platform 28 and ramps 30 are provided for loading and offloading passengers and a control booth 32 is positioned to allow the ride operator to control the ride 20 while visually observing its operation. Fencing 34 is also provided to restrict access to the ride 20 and for forming passenger lines.
Turning additionally to FIGS. 2-4, the top 22 comprises a central hub 36 and a plurality of sweep arms 38 which extend radially from the hub 36 in a spoke-like fashion and carry the passenger seats 24. Each passenger seat 24 is positioned in an outwardly facing direction between the end portions of adjacent sweep arms 38. The passenger seats 24 are rotatably coupled to the sweep arms 24 using roller bearings 40 which permit 360° rotation of the seats in both forward and backward directions as indicated by the arrows in FIG. 4.
The sweep arms 38 are constructed from suitably rigid materials having sufficient strength to support the passenger load carried by the seats 24. The number of, and spacing between, adjacent sweep arms 38 is determined by the desired number and width of passenger seats 24. The length of the sweep arms 38 can also be varied as desired to provide the selected diameter for the top 22.
The hub 36 is rotatably driven by a gear 42 fixed below the hub. The gear 42 is in turn driven by a drive gear 44 carried on a shaft of an electric drive motor 46. It is to be understood that other drive mechanisms, including indirect drives, can be utilized if desired to achieve rotation of the top 22.
An elongated boom 48 is used to raise and lower the top 22 during operation of the ride 20. The boom 48 comprises a pair of spaced apart, parallel box beams 49 which are connected together by cross-braces 50 positioned along the length of the beams 49. The boom 48 is pivotally mounted at one end to a stanchion 51 on base 26 and is pivotally connected at the other end to a tilt head 52 which forms a portion of and allows tilting of top 22. A hydraulic lift cylinder 54 is used to move the boom 48 between elevated and lowered positions. The lift cylinder 54 is pivotally mounted at one end to a stanchion 55 on the base 26 and at the other end with an intermediate portion of boom 48. Extension and retract of the lift cylinder 54 piston thus causes pivoting of boom 48 about a pivot axis 56.
The tilt head 52 is pivotally carried on the end of boom 48 opposite from the pivot axis 56. The tilt head 52 is constructed to connect the hub 36 to the end of the boom 48 in a manner which allows tilting movement of the hub and associated sweep arms 38 and passenger seats 24. The tilt head 52 is pivotally mounted to the boom 48 by a pivot pin 58 and bearings 60. The bearings 60 in turn are carried by brackets 62 which are mounted to the cross-brace 50 positioned at the end of boom 48.
Tilting movement of the tilt head 52 is controlled by a pair of double-acting leveling cylinders 64 which extend between the boom 48 and the tilt head 52. The leveling cylinders 64 operate to maintain the top 22 in a horizontal attitude while the boom 48 is being moved between its lowered and elevated positions. Once the boom 48 reaches its elevated positions, the leveling cylinders 64 are operated to tilt the top 22 to the desired angle with respect to the horizontal.
The leveling cylinders 64 are hydraulically connected to a slave cylinder 66 which extends between a stanchion 67 on the base 26 and the boom 48 near pivot axis 56. The hydraulic volume of the single slave cylinder 66 corresponds to the combined volume of the leveling cylinders 64 so that extension of the piston in the slave cylinder causes a corresponding extension of both leveling cylinder pistons. As a result of this operational connection between the slave cylinder 66 and leveling cylinders 64, angular displacement of the boom causes an opposite and corresponding angular displacement of the top 22, thereby maintaining the top 22 in a horizontal attitude during raising and lowering of the boom 48. Once the boom reaches its elevated operating position, the pistons in the leveling cylinders 64 may be retracted by opening a bypass valve (not shown) so that the top 22 can be tilted to a desired angle in relation to the horizontal.
Turning now to FIGS. 5-6 and 9-10, the passenger seat 24 will be described in more detail. Seat 24 faces radially outward during loading and unloading of passengers and is generally open at the front and top. The seat is sized to accommodate two passengers seated in side by side relationship and includes a pair of padded over-the-shoulder safety restraints 68, each of which is operable by an associated cylinder 70. A leg restraint 72 is also provided for each passenger in seat 24 and is manually operable by the ride operator. For appearance purposes, the cylinders 70 are preferably located interiorly of an outer shell 74 of seat 24.
The passenger seat 24 is mounted for forward and backward rotation by spindles 76 which extend from both sides of the seat and are received within the roller bearings 40 mounted in the ends of the sweep arms 38. The seats 24 are not powered for rotation but instead rotate as a result of inertial and centrifugal forces acting on the seat during operation of the ride 20. In order to achieve this rotation of the seats, it has been found that a center of gravity (designated by the numeral 75 in FIG. 5) of the unoccupied seats normally should be offset from the rotation axis of spindles 76. The positioning of the rotation axis in relation to the center of gravity should also be selected while giving consideration to the factors which affect the inertial and centrifugal forces exerted on the seat during operation of the ride. Among these factors are the radial distance of the seats 24 from the rotation axis of hub 36, the angle at which the top 22 is tilted from the horizontal, and the rotational speed of the top 22. While no mathematical formula has been determined for correlating these various factors, it has been found through experimentation with a top 22 having a 30 ft. diameter and rotating at 10.5 rpm, that optimum rotation of the seats 24 can be obtained by placing the center of gravity of the unoccupied seats 1.63 inches below and 2.5 inches radially outward from the pivot axis at spindles 76 and by tilting the operating top 22 at approximately 70° from the horizontal. In general, the top 22 should be tilted at an angle within the range of 45° to 80° from the horizontal, and more preferably from 55° to 75° from the horizontal to achieve seat rotation regardless of the diameter of the top 22.
Turning more specifically to FIGS. 7-8 and 11-13, a plurality of locking mechanisms 78 prevent rotation of the seats 24 during loading and unloading of the passengers and at selected times during the operation of ride 20. Each locking mechanism 78 includes an electric actuator 80 mounted within an associated sweep arm 38 and having a radially extendable and retractable arm 82. The arm 82 is connected by a radially adjustable clevis 83 to a slide block 84 which moves radially within V-shaped guide surfaces 86 presented by upper and lower guides 88. The slide block 84 has a cutout which forms a wide slot 90 which is shaped to capture a complementally shaped portion of a locking block 92 which is fixed to and rotatable with seat spindle 76. The locking block 92 is joined to the spindle by splines 94 and is held in place by a nut (not shown) threaded onto the associated end of the spindle 76.
As is best illustrated sequentially in FIGS. 11 and 12, retraction of the actuator arm 82 causes the slide block 84 to be removed from engagement with the locking block 92 carried on seat spindle 76. This disengagement permits the seat spindle 76 to rotate within the associated bearings as the associated seat 24 is subjected to centrifugal and inertial forces during operation of the ride 20. When rotation of the seat 24 is to again be stopped, the actuator arm 82 is extended to bring the slide block 84 back into engagement with the locking block 92.
It is important that the slide block 84 be able to initially capture the locking block 92 even while the seat 24 is pivoting back and forth. To accomplish this objective, the forward end of the slot 90 formed in the slide block 84 is of a greater dimension than the receiving end of the locking block 92. This allows the seat and locking block 92 to be pivoting through a preselected range of motion as the slide block 84 is advancing into engagement with the locking block 92. The narrowing guide surfaces 96 of the slot 90 then contact the complementally shaped guide surfaces 98 on the locking block 92 to progressively restrict the pivoting freedom of the seat 24 and locking block. When the actuator arm 82 is fully extended, the contacting guide surfaces 96 and 98 lock the seat 24 in the desired attitude and prevent pivoting movement of the seat 24.
In order to ensure that the slide block 84 does not advance while the locking block 92 is rotating or is pivoting beyond the preselected range of movement, the top 22 is returned to a horizontal position and rotated at a sufficient speed so that the centrifugal and inertial forces acting on the seat 24 return the seat to the outward facing position and prevent forward and backward rotation of the seat 24.
The operation of ride 20 commences by rotating the top 22 using electric motor 46 after the passengers have been loaded into seats 24. Normally, rotation of top 22 will begin while the boom 48 is still in the lowered position but it will be appreciated that rotation can be delayed until the top is raised. The locking mechanism 78 is also normally engaged to prevent backward and forward rotation of seats 24 about the tangential pivot axis. The lift cylinder 54 is then extended to raise the spinning top 22 upwardly. The top 22 is maintained in a horizontal attitude during lifting of boom 48 by the interconnection between the slave cylinder 66 and leveling cylinders 64. As the boom 48 elevates, the slave cylinder 66 extends and cause a corresponding extension of leveling cylinders 64. Extension of leveling cylinders 64, in turn, causes pivoting of the tilt head 52 to maintain the top 22 in the desired horizontal position.
Once the boom 48 is fully elevated, the leveling cylinders 64 are retracted to cause tilting of the top 22 from the horizontal position to a desired angle in relation to the horizontal. It will be appreciated that this tilting can also begin while the boom is being elevated. The seat locking mechanisms 78 are also released so that the seats 24 are free to pivot and then rotate forwardly and backwardly about their tangential pivot axes. This rotation of the seats 24 results from the centrifugal and inertial forces which are exerted on the seats during rotation and tilting of the top 22. It will be appreciated that the forces acting on the seats will varying depending on the rotational speed of the top and the angle at which the top is positioned. Release of the locking mechanisms 78 normally occurs after the boom 48 is raised but can occur earlier if desired.
The tilt angle of the top 22 may be varied during operation of the ride 20 or it may remain at a preselected angle. It can be seen that during operation of ride 20, passengers are subjected to motion in three dimensions as the top 22 rotates and tilts and the seats 24 rotate about axes tangential to the circular path they are carried through by the rotating top 22. This combination of motions and the planes that the passengers are carried through are particularly disorienting and thrilling even to seasoned passengers.
As the ride sequence is ending, the boom 48 is lowered while the top 22 is rotating and, preferably, while the top 22 is tilted at an angle to the horizontal. The hydraulic interconnection between the slave cylinder 66 and the leveling cylinders 64 is designed so that the leveling cylinders 64 remain retracted as the slave cylinder 66 retracts during lower of boom 48. This interconnection ensures that the top 22 is in a horizontal position when the boom 48 is fully lowered, thereby preventing contact between the top 22 and surrounding loading platform 28.
In order to return the seats 24 to the upright, outwardly facing position at the end of the ride sequence, the top 22 is run through a spin-out cycle which subjects the seats 24 to sufficient centrifugal and inertial forces to orient the seats in the desired position. The locking mechanism 78 is then engaged to prevent rocking movement of the seats. The spinning of the top 22 is then stopped and the passengers are free to leave seats 24 once the restraints 68 and 72 are released.
The sequencing and operation of the ride 20 is automatically controlled by a suitable controller (not shown) of various types know to those of ordinary skill in the art.
From the foregoing, it will be seen that this invention is one well adapted to attain all the ends and objects hereinabove set forth together with other advantages which are obvious and which are inherent to the structure.
It will be understood that certain features and subcombinations are of utility and may be employed without reference to other features and subcombinations. This is contemplated by and is within the scope of the claims.
Since many possible embodiments may be made of the invention without departing from the scope thereof, it is to be understood that all matter herein set forth or shown in the accompanying drawings is to be interpreted as illustrative and not in a limiting sense.
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An amusement ride is provided in which passengers can be simultaneous subjected to three different types of movement. A circular motion is provided by the circular rotation of the head which mounts the passenger seats. A tilting motion is provided by mounting the head for tilting movement as it rotates in the circular path. The third type of motion is provided by mounting the passenger seats so that they rotate about an axis tangential to the circular path in which they travel.
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CROSS-REFERENCE TO RELATED APPLICATION
A. 35 U.S.C. Sections 120, 121 and 365(c)
This application is a divisional/continuation of copending application:
application Ser. No. 09/309,947 filed on May 11, 1999, now U.S. Pat. No. 6,316,214.
This application claims priority benefit from copending U.S. Provisional Application Ser. No. 60/085,024, filed May 11, 1998, the disclosure of which is hereby incorporated herein by reference.
BACKGROUND OF THE INVENTION
The ecteinascidins (herein abbreviated Et or Et's) are exceedingly potent antitumor agents isolated from the marine tunicate Ecteinascidia turbinata . In particular, Et's 729, 743 and 722 have demonstrated promising efficacy in vivo, including activity against P388 murine leukemia, B16 melanoma, Lewis lung carcinoma, and several human tumor xenograft models in mice.
The isolation and characterization of natural Et 743 is taught in U.S. Pat. No. 5,089,273 which is hereby incorporated herein by reference. The preparation of synthetic Et 743 is taught in U.S. Pat. No. 5,721,362, which is hereby incorporated herein by reference.
The antitumor activities of ecteinascidin compounds, particularly Et 729 and Et 743 are well documented in the scientific literature. See for example, Goldwasser et al., Proceedings of the American Association for Cancer Research, 39: 598 (1998); Kuffel et al., Proceedings of the American Association for Cancer Research, 38: 596 (1997); Moore et al., Proceedings of the American Association for Cancer Research, 38: 314 (1997); Mirsalis et al., Proceedings of the American Association for Cancer Research, 38: 309 (1997); Reid et al., Cancer Chemotherapy and Pharmacology, 38: 329-334 (1996); Faircloth et al., European Journal of Cancer, 32A, Supp. 1, pp. S5 (1996); Garcia-Rocha et al., British Journal of Cancer, 73: 875-883 (1996); Eckhardt et al., Proceedings of the American Association for Cancer Research, 37: 409 (1996); Hendriks et al., Proceedings of the American Association for Cancer Research, 37: 389 (1996); the disclosures of which are hereby incorporated herein by reference.
Ecteinascidin 743 (Et 743) has the following structure:
In view of the impressive antitumor activities of this class of compounds, the search continues for related structures that may possess equal or higher levels of antitumor activity. The present invention, which is directed to the isolation and characterization of natural metabolites of Et 743, is a result of these continued studies.
SUMMARY OF THE INVENTION
The purification and structure elucidation of several products of the metabolism of Et 743 by human cytochrome CYP3A4 have been accomplished. These compounds are abbreviated herein as “ETM” followed by a numeric value which represents the approximate molecular weight.
For example, ETM 305 and ETM 775 were isolated from a metabolic mixture obtained from a biochemical study performed by the Analytical Chemistry Department at PharmaMar, Spain. A similar metabolic study carried out by the Mayo Clinic led to the identification of ETM 204. The structures of these ecteinascidin metabolites are as follows:
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention may be better understood by reference to the drawings accompanying this specification, wherein:
FIG. 1 is the 1 H NMR spectrum (500 MHz) of ETM-SiOH-1 (non-polar impurity) in CDCl 3 ;
FIG. 2 is the HPLC chromatogram of ETM-SiOH-4 (ETM 775);
FIG. 3 is the HPLC chromatogram of ETM-SiOH-3 (ETM 305);
FIG. 4 is the HPLC chromatogram of ETM-SiOH-2 (trace metabolites);
FIG. 5 is the LRFAB mass spectrum of ETM 305 in M.B. (magic bullet 4 );
FIG. 6 is the ESI mass spectrum of ETM 305;
FIG. 7 is the 1 H NMR spectrum (750 MHz) of ETM 305 in CD 3 OD;
FIG. 8 is the FAB/MS/MS spectrum of ETM 305;
FIG. 9 is the UV spectrum of ETM 305;
FIG. 10 is the UV spectrum of ETM;
FIG. 11 is the LRFAB mass spectrum of ETM 775 in M.B.;
FIG. 12 is the ESI mass spectrum of ETM 775 (positive mode);
FIG. 13 is the ESI mass spectrum of ETM 775 (negative mode);
FIG. 14 is the FAB/MS/MS spectrum of ETM 775 (m/z 138-302);
FIG. 15 is the FAB/MS/MS spectrum of ETM 775 (m/z 440-620);
FIG. 16 is the 1 H NMR spectrum (750 MHz) of ETM 775 in CD 3 OD;
FIG. 17 is the UV spectrum of ETM 775;
FIG. 18 is the HPLC choromatogram of ETM 305;
FIG. 19 is the UV spectrum of ETM 305;
FIG. 20 is the ESI mass spectrum of ETM 305;
FIG. 21 is the ESI mass spectrum of ETM 204;
FIG. 22 is the 1 H NMR spectrum (500 MHz) of ETM 204 in CD 3 OD; and
FIG. 23 is the ESI/MS/MS spectrum of ETM 204.
DETAILED DESCRIPTION OF THE INVENTION
I. Et 743 Metabolic Study
A. Preparation of Metabolic Mixture—ETM:
Et-743 (50 μM) was incubated with 0.4 mg/ml of human lymphoblast-expressed CYP3A4 isoform (Gentest Corporation, Woburn, Mass.) in 0.1 M Tris-HCl buffer (pH 7.4) containing an NADPH generating system (0.4 mM NADP + , 25 mM glucose-6-phosphate, 0.5 U/ml glucose-6-phosphate dehydrogenase and 3.3 mM magnesium chloride). After four (4) hours at 37° C., the reaction was stopped with ice cold acetonitrile and the solids removed by centrifugation (12,000 g, 4 min.). Supernatants were analyzed by HPLC.
B. Purification of ETM 305 and ETM 775
2.6 mg of ETM (generated as in A, above) was dissolved in a small amount of CHCl 3 and loaded into a silica gel column (8×100 mm glass column filled with a silica gel/CHCl 3 slurry). First, the column was eluted with CHCl 3 followed by CHCl 3 /MeOH mixtures (98, 96, 94, 92 and 90%). A total of ten test tubes were collected (3 mL each) and combined on the basis of TLC to yield four fractions (Table 1). The less polar and non-cytotoxic fraction (ETM-SiOH-1, 2 mg) consisted of a lipid not structurally related to Et 743 as revealed by the 1 H NMR spectrum (FIG. 1 ).
The remaining cytotoxic fractions were further purified by HPLC (Phenomenex-Ultracarb ODS, 10 μm, 10×150 mm, 3:1 MeOH/H 2 O 0.02 M NaCl, 1 mL/min., Da Detection: 210, 220, 254 and 280 nm). The most polar fraction (ETM-SiOH-4, 0.2 mg) yield 0. 1 mg of ETM 775 (FIG. 2 ). ETM-SiOH-3 yield 0.3 mg of ETM 305 (FIG. 3 ), and ETM-SiOH-2 consisted of a complex mixture of trace metabolites (FIG. 4 ).
TABLE 1 ETM-SiOH fractions: R f , weight and cytoxic activity. L1210 growth inhibition (%) ID# Test tube # R f a Weight at 500 ng/mL ETM-SiOH 1 1 0.9 2.0 mg 0 ETM-SiOH 2 2 0.5, 0.7 0.3 mg 80 b ETM-SiOH 3 4-5 0.5 0.4 mg 30 ETM-SiOH 4 6 0.3 0.2 mg 3 a Silica gel TLC using 9:1 CHCl 3 /MeOH as mobile phase. b 30% inhibition at 250 ng.
C. The Structure of ETM 305.
ETM 305 (IC 50 0.2 μm/mL vs L1210 cells) showed a molecular ion at 306.0977 by HRFAB/MS (FIG. 5 ). This data is in agreement with the molecular formula C 15 H 16 NO 6 (Δ 0.1 mmu). ESI/MS analysis confirmed the molecular weight of ETM 305 (FIG. 6 ); a molecular ion at m/z 306 was observed together with its sodium adduct (m/z 328). The 1 H NMR spectrum of ETM 305 ( FIG. 7 ) was very important for the structural assignment. Resonances at δ 2.04, 2.28 and 6.09 were almost identical to those of Me-6 (δ 2.03), —OCOCH 3 (δ 2.29) and the dioxy-methylene protons (δ 6.11 and 6.01) in Et 743, 1 respectively.
In addition, it was observed resonances corresponding to a —CH═CH—NHCHO unit (δ 7.09, d, 1H, J=15 Hz; δ 6.19, d, 1H, J=15 Hz; δ 8.04, s, 1H), 2 an additional methyl group (δ 2.52, s, 3H). The chemical shift of this methyl group match pretty well wit that of the methyl group on acetophenone 3 (δ 2.55). It is interesting to note that the 1 H NMR spectrum of ETM 305 consisted of two sets of resonances (4:1 ratio) due to rotational conformers around the —NH—CHO bond The 1 H NMR data together with the MS data suggested that ETM 305 had the B-unit aromatic ring system of Et 743 attached to a vinyl-formamide unit and to a methyl ketone as shown in Scheme 1. FAB/MS/MS on m/z 306 supported the proposed structure (FIG. 8 ).
D. The Structure of ETM 775.
ETM 775 (IC 50 0.2 μg/mL vs L1210 cells) showed a molecular ion at 776.2489 by HRFAB/MS (FIG. 11 ). This data is in agreement with the molecular formula C 39 H 42 N 3 O 12 S (Δ 0.0 mmu) which indicated that ETM 775 is an oxidation product of Et 743. Both, positive and negative mode ESI/MS spectra confirmed the molecular weight of ETM 775 (FIGS. 12 and 13 ). Because of the limited amount of ETM 775, the structural assignment was carried out mainly by interpretation of its mass spectral data. FABMS/MS on M+H of ETM 775 (m/z 776) was critical in assigning the location of the extra oxygen was located on N-2 in the form of an N-oxide as revealed by peaks at m/z 276 and 260 (276 -oxygen). A fragment ion at m/z 232, not observed in Et 743, suggested that the carbinol amine oxygen was oxidized to the amide (Scheme 3). The structures of the A- and C-units in ETM 775 remained intact as revealed by the presence of the characteristic mass spectral peaks at m/z 204 (A-unit), and m/z 224 and 250 (C-unit). 1 Both, the 750 750 Mhz 1 H NMR ( FIG. 16 ) and the UV ( FIG. 17 ) spectra resembled those of Et 743. 1
II. Et 743—Mayo Metabolic Study
A. M1 Metabolite (ETM 305).
The ETM sample was filtered through a C18 sep-pack and the eluant (3:1 MeOH/H 2 O) concentrated under a nitrogen stream. Purification of the resulting residue by HPLC (same conditions as described above) revealed the presence of a compound with a retention time identical to that of ETM 305 (FIG. 18 ). Both, the UV ( FIG. 19 ) and ESI/MS ( FIG. 20 ) spectra of M1 were identical to that of ETM 305. Thus, it was concluded that the M1 metabolite had the same chemical structure as ETM 305.
B. M2 Metabolite (ETM 204).
The provided sample was filtered through a C18 sep-pack and the eluant (3:1 MeOH/H 2 O) concentrated under a nitrogen stream and the resulting residue analyzed by FAB/MS, ESI/MS and 1 H NMR.
C. The Structure of ETM 204 (M2).
ETM 204 showed a molecular ion at 204.1024 by HRFAB/MS. This data is in agreement with the molecular formula C 12 H 14 NO 2 (Δ 0.0 mmu). ESI/MS analysis confirmed the molecular weight as 204 (FIG. 21 ). The molecular formula matched with the molecular formula of the a-unit in Et 743. Thus, the chemical structure of ETM 204 was proposed to be the aromatic ammonium salt derivative shown in Scheme 3. This simple compound (as well as the other metabolites) can easily be monitored to assay the breakdown of Et 743 in vivo.
A 1 H NMR spectrum ( FIG. 22 ) of ETM 204 showed resonances that supported the proposed structure: four aromatics signals (δ9.2, s; δ 7.8, d, J=5 Hz, and δ 6.8, s) and three methyl singlets (δ 4.2, δ3.9 and δ 2.4) The ESI/MS/MS of ETM 204 ( FIG. 23 ) showed a prominent peak ion at 189 corresponding to the apparent loss of the N-methyl group (204-CH 3 ).
Biological Studies of ETM-305 and ETM-775:
Compounds ETM-305 and ETM-775 have been assayed employing standard protocols for the following tumor cell lines; P-388 (murine leukemia); A-549 (human lung carcinoma); HT-29 (human colon adenocarcinoma); and MEL-28 (human malignant melanoma). See, for example, Bergeron et al., Biochem. Biophys. Res. Comm., 1984, 121 (3) 848-854 and Schroeder et al., J. Med. Chem., 1981, 24 1078-1083. These results are shown below in Table 2:
TABLE 2 Cell Line & Activity IC 50 (μg/ml) Compound: P-388 A-549 HT-29 MEL-28 ETM-305 0.5 0.5 0.5 0.25 ETM-775 0.01 0.01 0.01 0.01
Methods of Treatment
The present invention includes bioactive compounds, and accordingly, an embodiment of the present invention is directed to methods of treatment using such compounds. As described above, the compounds of the present invention have exhibited in vitro cytoxicity against tumor cell lines. It is anticipated that these in vitro activities will likewise extend to in vivo utility.
These compounds have been isolated in substantially pure form, i.e., at a purity level sufficient to allow physical and biological characterization thereof. These compounds have been found to possess specific antitumor activities and as such they will be useful as medicinal agents in mammals, particularly in humans. thus, another aspect of the present invention concerns pharmaceutical compositions containing the active compounds identified herein and methods of treatment employment such pharmaceutical compositions.
As described above, the active compounds of the present invention exhibit antitumor activity. thus, the present invention also provides a method of treating any mammal affected by a malignant tumor sensitive to these compounds, which comprises administering to the affected individual a therapeutically effective amount of an active compound or mixture of compounds, or pharmaceutical compositions thereof. The present invention also relates to pharmaceutical preparations, which contain as active ingredient one or more of the compounds of this invention, as well as the processes for its preparation.
Example of pharmaceutical compositions include any solid (tablets, pills, capsules, granules, etc.) or liquid (solutions, suspensions of emulsions) with suitable composition or oral, topical or parenteral administration, and they may contained the pure compound or in combination with any carrier of other pharmacologically active compounds. These compositions may need to be sterile when administered parenterally.
The terms “unit dose” as it pertains to the present invention refers to physically discrete units suitable as unitary dosages for animals, each unit containing a predetermined quantity of active material calculated to produce the desired antitumor effect in association with the required diluent; i.e., carrier, or vehicle. The specifications for the novel unit dose of this invention are dictated by and are directly dependent on (a) the unique characteristics of the active material and the particular antitumor effect to be achieved, and (b) the limitations inherent in the art of compounding such active material for antitumor use in animals.
Unit dosage forms are typically prepared from the frozen or dried active compound (or salts thereof by dispersement in a physiologically tolerable (i.e., acceptable) diluent or vehicle such as water, saline or phosphate-buffered saline to form an aqueous composition. Such diluents are well known in the art and are discussed, for example, in Remington's Pharmaceutical Sciences, 16th Ed., Mack Publishing Company, Easton, Pa. (1980) at pages 1465-1467.
Dosage forms can also include an adjuvant as part of the diluent. Adjuvants such as complete Freund's adjuvant (CFA), incomplete Freund's adjuvant (IFA) and alum are materials well known in the art, and are available commercially from several sources.
The quantity of active compound to be administered depends, inter alia, on the animal species to be treated, the subject animal's size, the size of the tumor (if known), the type of tumor (e.g., solid) present, and the capacity of the subject to utilize the active compound. Precise amounts of active compound required to be administered depend on the judgment of the practitioner and are peculiar to each individual, particularly where humans are the treated animals. Dosage ranges, however, can be characterized by a therapeutically effective blood concentration and can range from a concentration of from about 0.01 μM to about 100 μM, preferably about 0.1 μM to 10 μM.
Suitable regimes for initial administration and booster injections are also variable, but are typified by an initial administration followed by repeated doses at one or more hour intervals by a subsequent injection or other administration. Alternatively, continuous intravenous infusion sufficient to maintain a therapeutically effective concentration in the blood are contemplated.
REFERENCES
The following background references are provided to assist the reader in understanding this invention. To the extent necessary, the contents are hereby incorporated herein by reference.
1. A) Rinehart et al., J. Org. Chem. 1990, 55, 4512. B) Rinehart et al., J. Am. Chem. Soc., 1996, 118 9017. 2. Herbert et al., J. Chem. Soc. Perkin Trans. I, 1987, 1593. 3. Pretsch et al. Tables of Spectral Data for Structure Determination of Organic Compounds ; Springer-Verla: Berlin, 1989; p. H125. 4. Rinehart et al., Biochem. Res. Commun., 1984, 124, 350.
The present invention has been described in detail, including the preferred embodiments thereof. However, it will be appreciated that those skilled in the art, upon consideration of the present disclosure, may make modifications and/or improvements on this invention and still be within the scope and spirit of this invention.
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The purification and structure elucidation of several products of the metabolism of Et 743 by human cytochrome CYP3A4 have been accomplished. These compounds are abbreviated herein as “ETM” followed by a numeric value which represents the approximate molecular weight. Three compounds have been identified to date, namely ETM 305, ETM 775 and ETM 204. The structures of these ecteinascidin metabolites are as follows:
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. provisional application 61/222,075, filed Jun. 30, 2009, which is incorporated by reference herein in its entirety.
STATEMENT REGARDING GOVERNMENT FUNDING FOR RESEARCH AND DEVELOPMENT
[0002] This invention was made with United States government support awarded by the following agencies: NIH A1063326. The United States government has certain rights in this invention.
BACKGROUND OF THE INVENTION
[0003] Quorum sensing (QS) is a process by which bacteria assess their population density through a language of low molecular weight signalling molecules (autoinducers). Gram-negative bacteria commonly use N-acylated homoserine lactones (AHLs) as their primary autoinducers and their respective receptors (R proteins) for QS. Assessing population density allows for the modulation of gene expression levels required for group behaviour. Genes regulated by QS in Pseudomonas aeruginosa include virulence factor production and biofilm production. [Geske, G. D.; O'Neill, J. C.; Miller, D. M.; Mattmann, M. E.; Blackwell, H. E., Modulation of Bacterial Quorum Sensing: Systematic Evaluation of N-Acylated Homoserine Lactones in Multiple Species and New Insights into Their Mechanism of Action. J. Am. Chem. Soc. 2007, 129, 13613-13625.]
[0004] At high cell densities, bacteria use this chemical signaling process to switch from a nomadic existence to that of multicellular community. This lifestyle switch is significant, as numerous pathogenic bacteria use quorum sensing to turn on virulence pathways and form drug-impervious communities called biofilms that are the basis of myriad chronic infections. Over 80% of bacterial infections in humans involve the formation of biofilms, as exemplified in lung infections by Pseudomonas aeruginosa, which is the primary cause of morbidity in cystic fibrosis patients. The treatment of infections by pathogens that form biofilms costs over $1 billion/year in the US alone. Biofilms are dense extracellular polymeric matrices in which the bacteria embed themselves. Biofilms allow bacteria to create a microenviroment that attaches the bacteria to the host surface and which contains excreted enzymes and other factors allowing the bacteria to evade host immune responses including antibodies and cellular immune responses. Such biofilms can also exclude antibiotics. Further, biofilms can be extremely resistant to removal and disinfection. For individuals suffering from cystic fibrosis, the formation of biofilms by P. aeruginosa is eventually fatal. Other bacteria also respond to quorum sensing signals by producing biofilms. Biofilms are inherent in dental plaques, and are found on surgical instruments, food processing and agriculture equipment and water treatment and power generating machinery and equipment.
[0005] Gram-negative bacteria represent numerous relevant pathogens using quorum-sensing pathways. Besides P. aeruginosa, other quorum sensing bacteria include: Aeromonas hydrophila, A. salmonicida, Agrobacterium tumefaciens, Burkholderia cepacia, Chromobacterium violaceum, Enterobacter agglomeran, Erwinia carotovora, E. chrysanthemi, Escherichia coli, Nitrosomas europaea, Obesumbacterium proteus, Pantoea stewartii, Pseudomonas aureofaciens, P. syringae, Ralstonia solanacearum, Rhisobium etli, R. leguminosarum, Rhodobacter sphaeroides, Serratia liguefaciens, S. marcescens, Vibrio anguillarum, V. fischeri, V. cholerae, Xenorhabdus nematophilus, Yersinia enterocolitica, Y. pestis, Y. pseudotuberculosis, Y. medievalis, and Y. ruckeri. Studies on the above listed bacteria indicate that, while the Al is generally an AHL compound, the genes affected as well as the phenotypes resulting from induction of the promoter differ according to the particular life cycle of each bacterium. Further, quorum sensing stimulation typically results in altered expression of multiple genes.
[0006] P. aeruginosa is an opportunistic pathogen that causes severe, often fatal, infections in burn victims and cystic fibrosis patients and is therefore of direct and profound biomedical importance. P. aeruginosa uses 3-oxo-dodecanoyal homoserine lactone (OdDHL) as its autoinducer (Compound A):
[0000]
[0000] While successful modifications to the acyl tail region of autoinducers have been made, modifications to the AHL head group have met limited success. Modifications to the head group are important because the lactone ring is prone to hydrolysis at pH 7 and higher. [Glansdorp, F. G.; Thomas, G. L.; Lee, J. K.; Dutton, J. M.; Salmond, G. P. C.; Welch, M.; Spring, D. R., Synthesis and stability of small molecule probes for Pseudomonas aeruginosa quorum sensing modulation. Org. Biomol. Chem. 2004, 2, 3329-3336.] This work relates to non-homoserine lactone-based autoinducer analogs for QS modulation and provides a better understanding of the structural and electronic requirements of the autoinducer's head group. Certain of the compounds of this invention are designed as autoinducer analogs for QS modulation in P. aeruginosa.
[0007] Previous work in the field of P. aeruginosa QS modulators showed that many active non-lactone structures are highly conjugated and retain some form of the acyl chain, suggesting that a region of hydrophobicity in the acyl tail region is critical. [Muh, U.; Schuster, M.; Heim, R.; Singh, A.; Olson, E.; Greenberg, E. P., Novel Pseudomonas aeruginosa Quorum-Sensing Inhibitors Identified in an Ultra-High-Throughput Screen. Antimicrob. Agents Chemother. 2006, 50, 3674-3679; Muh, U.; Hare, B. L.; Duerkop, B. A.; Schuster, M.; Hanzelka, B. L.; Heim, R.; Olson, E. R.; Greenberg, E. P., A Structurally Unrelated Mimic of a Pseudomonas aeruginosa acyl-homoserine lactone quorum sensing signal. Proc. Natl. Acad. Sci. U.S.A. 2006, 103, 16948-16952; Lee, L. Y. W.; Hupfield, T.; Nicholson, R. L.; Hodgkinson, J. T.; Su, X.; Thomas, G. L.; Salmond, P. C.; Welch, M.; Spring, D. R., 2-Methoxycyclopentyl analogues of a Pseudomonas aeruginosa quorum sensing modulator. Molecular BioSystems 2008, 4, 505-507; Eberhard, A.; Widrig, C. A.; MaBath, P.; Schineller, J. B., Analogs of the autoinducer of bioluminescence in Vibrio fischeri. Arch. Microbiol. 1986, 146, 35-40; Rasmussen, T. B.; Givskov, M., Quorum sensing inhibitors: a bargain of effects. Microbiology 2006, 152, 895-904; Hjelmgaard, T.; Persson, T.; Rasmussen, T. B.; Givskov, M.; Nielsen, J., Synthesis of Furanone-based natural product analogues with quorum sensing antagonist activity. Bioorg. Med. Chem. 2003, 11, 3261-3271; Smith, K. M.; Bu, Y.; Suga, H., Induction and Inhibition of Pseudomonas aeruginosa quorum sensing by synthetic autoinducer analogs. Chem. Biol. 2003, 10, 81-89; Schaefer, A. L.; Hanzelka, B. L.; Eberhard, A.; Greenberg, E. P., Quorum sensing in Vibrio fischeri: Probing autoinducer-LuxR interactions with autoinducer analogs. J.Bacteriol. 1996, 178, 2897-2901; Passador, L.; Tucker, K. D.; Guertin, K. R.; Journet, M. P.; Kende, A. S.; Iglewski, B. H., Functional analysis of the Pseudomonas aeruginosa Autoinducer PAI. J. Bacteriol. 1996, 178, 5995-6000; Smith, K. M.; Bu, Y.; Suga, H., Library Screening for Synthetic Agonists and Antagonists of a Pseudomonas aeruginosa autoinducer. Chem. Biol. 2003, 10, 563-571; Ishida, T.; Ikeda, T.; Takiguchi, N.; Kuroda, A.; Ohtake, H.; Kato, J., Inhibition of quorum sensing in Pseudomonas aeruginosa by N-acyl cyclopentylamides. Appl. Environ. Microbiol. 2007, 73, 3183-3188; Fletcher, M. P.; Diggle, S. P.; Crusz, S. A.; Chhabra, S. R.; Camara, M.; Williams, P., A dual biosensor for 2-alkyl-4-quinolone quorum sensing signal molecules. Environ. Microbiol. 2007, 9, 2683-2693; Kim, C.; Kim, J.; Park, H. Y.; Park, H. J.; Lee, J. H.; Kim, C. K.; Yoon, J., Furanone derivatives as quorum sensing antagonists of Pseudomonas aeruginosa. Appl. Microbiol. Biotechnol. 2008, 80, 37-47; Estephane, J.; Dauvergne, J.; Soulere, L.; Reverchon, S.; Queneau, Y.; Doutheau, A., N-Acyl-3-amino-5H-furanone derivatives as new inhibitors of LuxR-dependent quorum sensing: Synthesis, biological evaluation and binding mode study. Bioorg. Med. Chem. Lett. 2008, 18, 4321-4324.]
[0008] Furthermore, a close examination of the crystal structure of the N-terminal domain of LasR reveals a hydrogen bond between the 3-oxo carbonyl in the acyl tail of OdDHL and a water molecule present in the LasR binding site [Bottomley, M. J.; Muraglia, E.; Bazzo, R.; Carfi, A., Molecular insights into quorum sensing in the human pathogen Pseudomonas aeruginosa from the structure of the virulence regulator LasR bound to its autoinducer. J. Biol. Chem. 2007, 282, 13592-13600.]
[0009] Published US application US2006/0178430, published Aug. 10, 2006 and International published application WO 2008/116029, published Sep. 25, 2008 relate to quorum sensing compounds and their uses. These documents are incorporated by reference in their entirety herein for their description of the state of the art and for additional methods of synthesis, methods of testing, and methods of application of quorum sensing compounds.
[0010] Janssens, J. C. A. et al. (2007) Applied Environ. Microbiol. 73(2) 535-544 reports that certain N-acyl homoserine lactones including certain thiolactones are strong activators of SdiA, the Salmonella enterica Serovar Typhimurium LuxR homologues.
[0011] Published PCT application WO2002/052949 relates to the use of autoinducer compounds as additives to animal feeds for improving animal performance.
SUMMARY OF THE INVENTION
[0012] The invention provides a compound of formula I:
[0000] A-[Z] n -L1-[Y] q —W—[V] m -L2-HG
[0000] or a pharmaceutically acceptable salt or ester thereof
where: W is —NH— or
[0000]
[0000] Y is —CO—, —CO—CH 2 —CO—, —NH—CO—, —CO—CH 2 —C(Y1)-, —SO 2 —, where Y1 is —OH, —SH, —NH 2 or —F;
q is 1 or 0 to indicate the presence or absence, respectively of Y; L1 and L2, independently, are —[CH 2 ] p1 — and —[CH 2 ] p2 —, where p1 and p2, independently, are 0 or integers ranging from 1-10 and one or more of the carbons of L1 or L2 can be substituted with one or two non-hydrogen substituents; V is
[0000]
[0000] where R N is an alkyl group having 1-3 carbon atoms;
m is 1 or 0 to indicate, respectively, the presence or absence of the V group; Z is —CO—, —O—CO—, —CO—O—, —NH—CO—,—CO—NH—, —NH—CO—NH—, —O—, —S—, or —NH 2 —, n is 1 or 0 to indicate, respectively, the presence of absence of the Z group; A is an aryl or heteroaryl group having one or two 5- or 6-member rings with 1-3 heteroatoms in a ring, a C 5 -C 8 cycloalkyl group, a C 5 -C 8 cycloalkenyl group, a heterocyclic group having one or two 5 to 8-member rings with 1-3 heteroatoms in a ring, a branched or unbranched C 1 -C 12 acyclic aliphatic group, all of which groups can have one or more non-hydrogen substituents selected from the group consisting of halogen, nitro, hydroxyl, nitrile, azide, —R, —OR, —COOR, —OCOR, —COR, —OCOOR, —CON(R) 2 , —OCON(R) 2 , —N(R) 2 , —SR, —SO 2 R, —SOR, and —SO 2 N(R) 2 , wherein each R is independently selected from the group consisting of hydrogen, an amine group, a substituted or unsubstituted unbranched C 1 -C 12 acyclic aliphatic group, a substituted or unsubstituted branched C 1 -C 12 acyclic aliphatic group, a substituted or unsubstituted C 3 -C 8 cycloalkyl group, a substituted or unsubstituted C 3 -C 8 cycloalkenyl group, a fluorinated C 1 -C 12 alkyl group, a substituted or unsubstituted aryl group, a substituted or unsubstituted heterocyclic group, and a protecting group; additionally, two R groups in the same substituent, optionally form a 4-8 member ring; and HG is a head group selected from an aryl or heteroaryl group having one or two 5- or 6-member rings with 1-3 heteroatoms in a ring; a C 5 -C 8 cycloalkyl group; a C 5 -C 8 cycloalkenyl group; a heterocyclic group having one or two 5 to 8-member rings with 1-3 heteroatoms in a ring; an alkyl group having 1-3 carbon atoms substituted with two aryl or heteroaryl groups; a cyclic lactone, lactam, thiolactone or ketone group having a 4-8 member ring, or an ester group R E —CO—CO—, where R E is an optionally substituted alkyl group having 1-6 carbon atoms; all of which groups can have one or more non-hydrogen substituents selected from the group consisting of halogen, nitro, hydroxyl, nitrile, azide, —R, —OR, —COOR, —OCOR, —COR, —OCOOR, —CON(R) 2 , —OCON(R) 2 , —N(R) 2 , —SR, —SO 2 R, —SOR, and —SO 2 N(R) 2 , wherein each R is independently selected from the group consisting of hydrogen, an amine group, a substituted or unsubstituted unbranched C 1 -C 12 acyclic aliphatic group, a substituted or unsubstituted branched C 1 -C 12 acyclic aliphatic group, a substituted or unsubstituted C 3 -C 8 cycloalkyl group, a substituted or unsubstituted C 3 -C 8 cycloalkenyl group, a fluorinated C 1 -C 12 alkyl group, a substituted or unsubstituted aryl group, a substituted or unsubstituted heterocyclic group, and a protecting group; additionally, two R groups on the same substituent optionally form a 4-8 member ring.
[0021] In specific embodiments, n is 0. In specific embodiments, m is 0. In specific embodiments, n is 0 and m is 0. In specific embodiments, n is 0 and q is 1. In specific embodiments, n is 0, m is 0 and q is 1. In specific embodiments, n is 0, m is 1 and q is 1. In specific embodiments, n is 1, m is 1 and q is 1.
[0022] In a specific embodiment, W is —NH—.
[0023] In an embodiment, HG is a group having formula:
[0000]
[0000] where r is an integer ranging from 1-4, G is —O—, —S—, —NH— or —CH 2 —; R′ is hydrogen or a 1-6 carbon aliphatic group, particularly an alkyl group, and X represents optional substitution with one or more non-hydrogen substituents on one or more ring carbons. In specific embodiments, r is 1 or 2, the ring is unsubstituted and R′ is H.
[0024] In a specific embodiment, G is —S—. In a specific embodiment, G is —S— and r is 1. In a specific embodiment, G is —S—, r is 1 and R′ is an alkyl group.
[0025] In a specific embodiment, G is —S—, r is 1 and R′ is an alkyl group. X represents 1, or 2 substituents on the ring.
[0026] In an embodiment, HG is a group other than a ketone, lactone, or lactam group, when W is —NH—.
[0027] In an embodiment, HG is selected from an optionally substituted phenyl, naphthyl, cyclohexyl, cyclohexenyl, cyclopentyl, pyridyl, piperidyl, furyl, thienyl, pyrroyl, or
[0000]
[0000] where r is an integer ranging from 1-4, R′ is hydrogen or a 1-6 carbon aliphatic group, particularly an alkyl group, and X represents optional substitution with one or more non-hydrogen substituents on one or more ring carbons. In specific embodiments, r is 1, the ring is unsubstituted and R′ is H. In specific embodiments, r is 1, and R′ is an alkyl group, particularly a methyl group. In specific embodiments, r is 1, R′ is an alkyl group, particularly a methyl group and X represents 1, or 2 substituents on the ring.
[0028] In specific embodiments, when HG is an unsubstituted thiolactone ring (where G is S and all X and R′ are hydrogen) and W is —NH—, A is a group other than an unsubstituted alkyl group or a halogenated alkyl group. In specific embodiments, when HG is an unsubstituted thiolactone ring (where G is S and all X and R′ are hydrogen); W is —NH—, q is 1 and Y is —COCH 2 —CO—, A is a group other than an unsubstituted alkyl group or a halogenated alkyl group. In specific embodiments, when HG is an unsubstituted thiolactone ring (where G is S and all X and R′ are hydrogen); W is —NH—; m, n, p1 and p2 are all 0; q is 1 and Y is —CO—CH 2 —CO—, A is a group other than an unsubstituted alkyl group or a halogenated alkyl group.
[0029] In specific embodiments, HG is a group as illustrated in FIG. 1-1 , or 1 - 2 , where X, X1 and X2, represent optional substitution with one or more non-hydrogen substituents on one or more ring carbons. In these FIG. X, X1 and X2 represents optional substitution with one or more non-hydrogen substituents on one or more ring carbons, RA is H or an alkyl group, particularly one having 1-3 carbon atoms. In more specific embodiments, HG is selected from groups HG1, HG4, HG7, HG8, HG10, HG11, or HG12. In other specific embodiments, HG is selected from groups HG2, HG3, HG14, HG15, HG17, HG18 or HG21. In specific embodiments, HG is a group of any of FIG. 2-1 , 2 - 2 , or 2 - 3 . In these FIG. X, X1-X5 represents optional substitution with one or more non-hydrogen substituents on one or more ring carbons and R′ is an alkyl group having 1-6 or 1-3 carbon atoms.
[0030] In specific embodiments HG is an ester group RE-O—CO—, where RE is an unsubstituted alkyl group having 1-6 carbon atoms; an alkyl group substituted with one or more halogens, particularly fluorines; a phenyl group or optionally substituted phenyl group, particular a phenyl group substituted with one or more halogens, particularly fluorine, one or more nitro groups, one or more alkoxy groups (including 1C-3C alkoxy groups), or one or more trifluoromethyl groups. In specific embodiments, RE is methyl, ethyl, propyl or butyl groups. In more specific embodiments, RE is a methyl or ethyl group. In specific embodiments when HG is an ester group L2 is —CH(CH 3 )—.
[0031] In specific embodiments, HG is a group as illustrated in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 , and A is a branched or unbranched aliphatic group having 1-12 carbon atoms and more specifically is an alkyl or alkenyl group having 1-12 carbon atoms. In specific embodiments HG is a group as illustrated in FIG. 2-1 , 2 - 2 , or 2 - 3 .
[0032] In specific embodiments, A is a group as in FIG. 3 , where X represents optional substitution with one or more non-hydrogen substituents on one or more ring carbons or on a specific ring carbon, R′ is an alkyl group, particularly one having 1-6 or 1-3 carbon atoms. In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 1 - 3 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a group in FIG. 3 . In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 1 - 3 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a group in FIG. 3 and
[0033] W is
[0000]
[0034] In specific embodiments, A is one of A1-A13 ( FIG. 3-1 ). In specific embodiments, A is one of A1-A13 ( FIG. 3-1 ) and n is 0. In specific embodiments, A is one of A1-A13 ( FIG. 3-1 ), n is 0, q is 1 and Y is —CO— or —CO—CH 2 —CO—. In specific embodiments, A is one of A1-A13 ( FIG. 3-1 ), n is 0, q is 1, Y is —CO— or —CO—CH 2 —CO—, and W is —NH—. In specific embodiments, A is one of A1-A13 ( FIG. 3-1 ), n is 0, q is 1, Y is —CO— or —CO—CH 2 —CO—, and W is
[0000]
[0000] In specific embodiments, A is one of A1-A13 ( FIG. 3 ), n is 0, q is 1, Y is —CO— or —CO—CH 2 —CO—, W is —NH— and m is 0. In specific embodiments, A is one of A1-A13 ( FIG. 3 ), n is 0, q is 1, Y is —CO— or —CO—CH 2 —CO—, W is —NH— and m is 1.
[0035] In specific embodiments, A is a branched or straight chain alkyl or alkenyl group. In specific embodiments, A is a branched or straight chain alkyl or alkenyl and n is 0. In specific embodiments, A is a branched or straight chain alkyl or alkenyl, n is 0, q is 1 and Y is —CO— or —CO—CH 2 —CO—. In specific embodiments, A is a branched or straight chain alkyl or alkenyl, n is 0, q is 1, Y is —CO— or —CO—CH 2 —CO— and W is —NH—. In specific embodiments, A is a branched or straight chain alkyl or alkenyl, n is 0, q is 1, Y is —CO— or —CO—CH 2 —CO—, and W is
[0000]
[0036] In specific embodiments, A is a branched or straight chain alkyl or alkenyl, n is 0, q is 1, Y is —CO— or —CO—CH 2 —CO—, W is —NH— and m is 0. In specific embodiments, A is a branched or straight chain alkyl or alkenyl n is 0, q is 1, Y is —CO— or —CO—CH 2 —CO—, W is —NH— and m is 1.
[0037] In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 and W is NH and m is 1. In specific embodiments, HG is a group as in FIG. 1 - 1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 , L1 is —CH 2 — or —CH 2 —CH 2 —, L2 is —(CH 2 )0-1- and q is 1. In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 , L1 is —CH 2 — or —CH 2 —CH 2 —, L2 is —(CH 2 ) 0-1 — and q is 1 and Y is —CO— or —CO—CH 2 —CO—. In specific embodiments, HG is a group as in FIGS. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 , and L1 is —CH 2 — or —CH 2 —CH 2 —, L2 is —(CH 2 ) 0-1 — and q is 1 and Y is —CO—.
[0038] In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a branched or straight chain alkyl or alkenyl and W is —NH— and m is 1. In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a branched or straight chain alkyl or alkenyl, L1 is —CH 2 — or —CH 2 —CH 2 —, L2 is —(CH 2 ) 0-1 — and q is 1. In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a branched or straight chain alkyl or alkenyl, L1 is —CH 2 — or —CH 2 —CH 2 —, L2 is —(CH 2 ) 0-1 — and q is 1 and Y is —CO— or —CO—CH 2 —CO—. In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a branched or straight chain alkyl or alkenyl, and L1 is —CH 2 — or —CH 2 —CH 2 -L2 is —(CH 2 ) 0-1 — and q is 1 and Y is —CO—.
[0039] In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a group in FIG. 3-1 and W is NH and m is 1. In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a group in FIG. 3 , L1 is —CH 2 — or —CH 2 —CH 2 —, L2 is —(CH 2 ) 0-1 — and q is 1. In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a group in FIG. 3 , L1 is —CH 2 — or —CH 2 —CH 2 —, L2 is —(CH 2 ) 0-1 — and q is 1 and Y is —CO— or —CO—CH 2 —CO—. In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 , or 2-3 and A is a group in FIG. 3 , with the exception that A is not the same group as HG and L1 is —CH 2 — or —CH 2 —CH 2 —, L2 is —(CH 2 ) 0-1 — and q is 1 and Y is —CO—.
[0040] In specific embodiments, HG is a group as in FIG. 1-1 , 1 - 2 , 1 - 3 , 2 - 1 , 2 - 2 , or 2 - 3 and A is a group in FIG. 3-1 with the exception that A is not the same group as HG.
[0041] In specific embodiments, HG is P1-P50. In specific embodiments, HG is P1-P50 and L2 is —(CH 2 ) 0-2 — and may be substituted on one carbon with an alkyl group having 1-3 carbon atoms. In specific embodiments, HG is P1-P50; L2 is —(CH 2 ) 0-2 — and is optionally substituted on one carbon with an alkyl group having 1-3 carbon atoms, and m is 0. In specific embodiments, HG is P1-P50; L2 is —(CH 2 ) 0-2 — and may be substituted on one carbon with an alkyl group having 1-3 carbon atoms, and m is 1. In specific embodiments, HG is P1-P50; L2 is —(CH 2 ) 0-2 — and may be substituted on one carbon with an alkyl group having 1-3 carbon atoms, and m is 1 and W is NH. In specific embodiments, HG is P1-P50; L2 is —(CH 2 ) 0-2 — and may be substituted on one carbon with an alkyl group having 1-3 carbon atoms, and m is 1, W is NH and q is 1. In specific embodiments, HG is P1-P50; L2 is —(CH 2 ) 0-2 — and may be substituted on one carbon with an alkyl group having 1-3 carbon atoms, and m is 1, W is —NH—, q is 1 and Y is —CO— or —CO—CH 2 —CO—. In specific embodiments HG is P1-P50 and L1 is —(CH2)0-2-. In specific embodiments HG is P1-P50 and n is 0.
[0042] HG groups may be unsubstituted. HG groups may be substituted. Optional substitution on HG groups includes substitution with one or more non-hydrogen substituents selected from the group consisting of halogen, nitro, hydroxyl, nitrile, azide, —R, —OR, —COOR, —OCOR, —COR, —OCOOR, —CON(R) 2 , —OCON(R) 2 , —N(R) 2 , —SR, —SO 2 R, —SOR, —SO 2 N(R) 2 , wherein each R is independently selected from the group consisting of hydrogen, an amine group, a substituted or unsubstituted unbranched C1-C12 acyclic aliphatic group, a substituted or unsubstituted branched C1-C12 acyclic aliphatic group, a substituted or unsubstituted C3-C8 cycloalkyl group, a substituted or unsubstituted C3-C8 cycloalkenyl group, a fluorinated C1-C12 alkyl group, a substituted or unsubstituted aryl group, a substituted or unsubstituted heterocyclic group, and a protecting group, where two R groups on the same substituent optionally form a 4-8 member ring (carbon ring or a carbon ring with 1-3 heteroatom ring members); additionally, two X, X1 or X2 groups, particularly two such groups on adjacent ring positions can form a 4-8 member ring. Specific substituents include among others optionally substituted alkyl groups having 1-3 carbon atoms.
[0043] In specific embodiments, X, X1 or X2 represent one or more halogens, nitro, azide, nitrile, alkyl groups particularly those having 1-3 carbon atoms, —OR, —COOR, —SO 2 —R, —SR, or —N(R) 2 , particularly where R is hydrogen or an alkyl group having 1-3 carbon atoms.
[0044] In specific embodiments, one or more carbons of L1 can be substituted with an alkyl group having 1-3 carbon atoms, a hydroxyl or amine group or a halogen, particularly a fluorine. In a more specific embodiment one carbon of L1 can be substituted with one non-hydrogen substituent. In a specific embodiment L1 is —CH(R′)— where R′ is an alkyl group. In a specific embodiment L1 is —(CF 2 ) p1 —.
[0045] In specific embodiments, one or more carbons of L2 can be substituted with an alkyl group having 1-3 carbon atoms, a hydroxyl or amine group or a halogen, particularly a fluorine. In a more specific embodiment one carbon of L2 can be substituted with one non-hydrogen substituent. In a specific embodiment L2 is —CH(R′)— where R′ is an alkyl group. . In a specific embodiment L2 is —(CF 2 ) p1 —.
[0046] The invention also provides a compound of formula II:
[0000]
[0047] or a pharmaceutically acceptable salt or ester thereof
[0048] where variables are defined as for formula I. In an embodiment, q is 0. In an embodiment q is 1. In an embodiment, q is 1 and Y is and Y is —CO—, —CO—CH 2 —CO— or —CO—CH 2 —C(Y1)-.
[0049] In embodiments of formula II, A is a branched or unbranched C1-C12 acyclic aliphatic group. More specifically A is a branched or unbranched alkyl or alkenyl group having 1-15 carbon atoms. In more specific embodiments of formula II where A is a branched or unbranched C1-C12 acyclic aliphatic group, n is 0, q is 0 and L1 is —(CH 2 ) p1 —, where p1 is 0-6. In additional specific embodiments of formula II where A is a branched or unbranched C1-C12 acyclic aliphatic group, n is 0, q is 1, Y is —CO— or —CO—CH 2 —C(Y1)-, L1 is —(CH 2 ) p1 —, where p1 is 0-6. In more specific embodiments, A is a branched or unbranched alkyl group having 1-12 carbon atoms.
[0050] In embodiments of formula II, A is an optionally substituted aryl group. In more specific embodiments, q is 0, L1 is —(CH 2 ) p — where p is 0-6 and A is an optionally substituted aryl group, particularly an optionally substituted phenyl, biphenyl or naphthyl group. In additional specific embodiments, q is 0, L1 is —(CH 2 ) p —, where p is 1-3, and A is an optionally substituted aryl group, particularly an optionally substituted phenyl, biphenyl or naphthyl group. In additional embodiments, the phenyl, biphenyl or naphthyl group is unsubstituted or substituted with one or more halide, nitro, hydroxyl, nitrile, azide, —OR, —N(R) 2 , —SR, or —SO 2 R groups, where R is an alkyl group having 1-3 carbon atoms.
[0051] In embodiments of formula II, HG is an optionally substituted phenyl, naphthyl, cyclopentyl, cyclohexyl, cyclohexenyl, furyl, or group having formula:
[0000]
[0000] where variables are as defined above and in specific embodiments, r is 1 or 2. In additional embodiments, the ring is unsubstituted and R′ is hydrogen. In additional embodiments, R′ is an alkyl group having 1-3 carbon atoms. In additional embodiments, the ring carries 1-3 substituents, particularly optionally substituted alkyl groups having 1-3 carbon atoms. Preferred optional substitution for phenyl, naphthyl, cyclopentyl, cyclohexyl, or cyclohexenyl HG groups is one or more halogen, nitro, or alkoxy (having 1-3 carbon atoms). In specific embodiments, HG is:
[0000]
[0000] where r, X and R′ are as defined above. In specific embodiments, r is 1. IN specific embodiments, R′ is H. In specific embodiments, R′ is optionally substituted C1-C3 alkyl. In specific embodiments, X is 1-3 substituents on the ring. In specific embodiments, r is 1 and X is 1 or 2 substituents on the ring. In specific embodiments, X is 1 or 2 optionally substituted alkyl groups having 1-3 carbon atoms.
[0052] Compounds of this invention can be optically active, racemic, enantiomerically pure or mixtures of enantiomers. HG may have optically active carbons and may exist as enantiomeric pairs. For example, HG of formula:
[0000]
[0000] can be in the enantiomeric forms:
[0000]
[0000] Note that carbons in the HG ring other than that shown may be optically active dependent upon X substitution.
[0053] The invention also provides a compound of formula III:
[0000] A-[Z] n -L1-[Y] q —NH—[V] m -L2-HG
[0000] or a pharmaceutically acceptable salt or ester thereof,
where variables are defined as for formula I. In specific embodiments of formula III, m is 0. In other specific embodiments, n is 0. In other specific embodiments, m and n are both 0. In specific embodiments, m is 0 and q is 1. In more specific embodiments, m is 0, q is 1 and Y is —CO—, —CO—CH 2 —CO— or —CO—CH 2 —C(Y1)-. In more specific embodiments, m is 0, q is 1 and Y is —CO—, —CO—CH 2 —CO— or —CO—CH 2 —C(Y1)-, and A is an optionally substituted aryl group, particularly an optionally substituted phenyl group. In more specific embodiments, m is 0, q is 1 and Y is —CO—, —CO—CH 2 —CO— or —CO—CH 2 —C(Y1)-, and A is an optionally substituted branched or unbranched C 1 -C 12 acyclic aliphatic group. In specific embodiments HG is a group of any of FIG. 1-1 , 1 - 2 , 1 - 3 , 2 - 1 , 2 - 2 or 2 - 3 . In specific embodiments, HG is:
[0000]
[0000] where r, X and R′ are as defined above. In specific embodiments, r is 1. In specific embodiments, R′ is H. In specific embodiments, R′ is optionally substituted C1-C3 alkyl. In specific embodiments, X is 1-3 substituents on the ring. In specific embodiments, r is 1 and X is 1 or 2 substituents on the ring. In specific embodiments, X is 1 or 2 optionally substituted alkyl groups having 1-3 carbon atoms.
[0055] The invention also provides a compound of formula IV:
[0000]
[0000] or a pharmaceutically acceptable salt or ester thereof,
where variables are defined as for formula I. In specific embodiments, R N is hydrogen. In specific embodiments, q is 1 and Y is —CO—, —CO—CH 2 —CO— or —CO—CH 2 —C(Y1)-. In specific embodiments, HG is an optionally substituted aryl group, particularly an optionally substituted phenyl group. In specific embodiments, A is A is an optionally substituted aryl group, particularly an optionally substituted phenyl group. In specific embodiments, A is an optionally substituted branched or unbranched C 1 -C 12 acyclic aliphatic group, particularly an optionally substituted branched or unbranched alkyl or alkenyl group having 1 to 12 carbon atoms. In specific embodiments HG is a group of any of FIG. 1-1 , 1 - 2 , 2 - 1 , 2 - 2 or 2 - 3 . In specific embodiments, HG is:
[0000]
[0000] where r, X and R′ are as defined above. In specific embodiments, r is 1. IN specific embodiments, R′ is H. In specific embodiments, R′ is optionally substituted C1-C3 alkyl. In specific embodiments, X is 1-3 substituents on the ring. In specific embodiments, r is 1 and X is 1 or 2 substituents on the ring. In specific embodiments, X is 1 or 2 optionally substituted alkyl groups having 1-3 carbon atoms.
[0057] The invention also provides a compound of formula V:
[0000]
[0000] or a pharmaceutically acceptable salt or ester thereof, where variables are defined as for formula I. In specific embodiments, R E is an unsubstituted alkyl group having 1-6 carbon atoms. In specific embodiments, R E is methyl or ethyl. In specific embodiments, A is a branched or straight-chain aliphatic group having 1-12 carbon atoms. In specific embodiments, A is a branched or straight-chain alkyl group having 1-12 carbon atoms. In specific embodiments, A is an optionally substituted phenyl group. In specific embodiments, A is a phenyl group substituted with one or more halogens, nitro groups, alkoxy groups having 1-3 carbon atoms, or one or more trifluoroethyl groups. In specific embodiments W is —NH—. In specific embodiments L1 and L2 are independently either —CH 2 — or —CH 2 —CH 2 —. In a specific embodiment L2 is —CH(CH 3 )—. In specific embodiments, Y is —CO—, —CO—CH 2 —CO—, —NH—CO—, —CO—CH 2 —C(Y1)-. In specific embodiments, Y is —CO—, or —CO—CH 2 —CO. In specific embodiments, q is 1. In specific embodiments, n is 0. In specific embodiments, m is 0. In specific embodiments, n and m are 0 and q is 1. In specific embodiments Y is —CO— or —CO—CH 2 —CO—.
[0058] The invention also provides a compound of formula VI:
[0000]
[0000] where R F is an optionally substituted a branched or unbranched C 1 -C 12 acyclic aliphatic group, L2, V and m are as defined above, f is 0 or 1 to show the absence of presence of the CO group, and HG is a head group as defined in formula I. In specific embodiments, m is 0. In specific embodiments m is 1. In specific embodiments L2 is —CH 2 — or —CH 2 —CH 2 —. In specific embodiments, HG can be any group as in FIG. 1-1 , 1 - 2 or 1 - 3 . In other specific embodiments, HG is an optionally substituted phenyl group. In specific embodiments, L2 is —CH 2 — and HG is an optionally substituted phenyl group. In specific embodiments, m is 1, L2 is —CH 2 — and HG is an optionally substituted phenyl group. In specific embodiments, m is 0, L2 is —CH 2 — and HG is an optionally substituted phenyl group. In specific embodiments R F is a branched or straight-chain alkyl group. In specific embodiments R E is a branched or straight-chain alkenyl group having one or two double bonds. In specific embodiments, f is 1 and m is 0. In specific embodiments, f is 0 and m is 0. In specific embodiments, f and m are both 1. In specific embodiments, f is 0 and m is 1. In specific embodiments, HG is a phenyl group substituted with 1 to 5 halogens, particularly bromine, chlorine or fluorine. In specific embodiments, HG is a phenyl group substituted with 1 to 5 fluorines. In specific embodiments, HG is a phenyl group substituted with 1 or 2 alkoxy groups having 1-3 carbon atoms. In specific embodiments, HG is a phenyl group substituted with 1-3 nitro groups. In specific embodiments, HG is a furyl group, particularly a 1-furyl group. In specific embodiments, m is 1, f is 1, L2 is —CH 2 — or —CH 2 —CH 2 — and HG is selected from HG groups of FIG. 1-1 , 1 - 2 , 1 - 3 , 2 - 1 , 2 - 2 , 2 - 3 or 2 - 4 . In specific embodiments, m is 1, f is 0, L2 is —CH 2 — or —CH 2 —CH 2 — and HG is selected from HG groups of 1-1, 1-2, 1-3, 2-1, 2-2, 2-3 or 2-4. In specific embodiments, m is 0, L2 is —CH 2 — or —CH 2 —CH 2 — and HG is selected from HG groups of FIG. 1-1 , 1 - 2 , 1 - 3 , 2 - 1 , 2 - 2 or 2 - 3 . In specific embodiments, m is 0, f is 1, L2 is —CH 2 — or —CH 2 —CH 2 — and HG is selected from HG groups of FIG. 11-1 , 1 - 2 , 1 - 3 , 2 - 1 , 2 - 2 , 2 - 3 or 2 - 4 . In specific embodiments, m is 0, f is 0, L2 is —CH 2 — or —CH 2 —CH 2 — and HG is selected from HG groups of FIG. 1-1 , 1 - 2 , 1 - 3 , 2 - 1 , 2 - 2 , 2 - 3 or 2 - 4 . In specific embodiments, HG is:
[0000]
[0000] where r, X and R′ are as defined above. In specific embodiments, r is 1. In specific embodiments, R′ is H. In specific embodiments, R′ is optionally substituted C1-C3 alkyl. In specific embodiments, X is 1-3 substituents on the ring. In specific embodiments, r is 1 and X is 1 or 2 substituents on the ring. In specific embodiments, X is 1 or 2 optionally substituted alkyl groups having 1-3 carbon atoms.
[0059] The present invention provides compounds and methods for modulation of quorum sensing of bacteria. In an embodiment, the compounds of the present invention are able to act as replacements for naturally occurring bacterial quorum sensing ligands in a ligand-protein binding system; that is, they imitate the effect of natural ligands and produce an agonistic effect. In another embodiment, the compounds of the present invention are able to act in a manner which disturbs or inhibits the naturally occurring ligand-protein binding system in quorum sensing bacteria; that is, they produce an antagonistic effect. The present invention also provides methods of increasing or reducing the virulence of quorum sensing bacteria. In one aspect, the method comprises contacting a bacterium with an effective amount of a compound of the present invention. In another aspect, the method comprises contacting a bacterium with a therapeutically effective amount of a pharmaceutically acceptable salt or ester of the compounds of the present invention. In yet another aspect, the method comprises contacting a bacterium with a precursor which can form an effective amount of a compound of the present invention.
[0060] The present invention provides compositions for modulation of quorum sensing of bacteria which comprises one or more compounds of this invention, particularly one or more compounds of formulas I to VI herein. The compositions herein can further comprise an appropriate carrier, particularly a pharmaceutically acceptable carrier for therapeutic applications. In applications herein, one or more compounds of the invention can be compounds with one or more antibacterial compounds.
[0061] In an embodiment, the methods of the present invention can be used for disrupting a biofilm formed by a quorum sensing bacterium. A method of the present invention for disrupting a biofilm comprises contacting the biofilm with an effective amount of a compound of the present invention. In an embodiment, the methods of the present invention can be used to diminish or inhibit biofilm production. Alternatively, the methods of the present invention can be used for causing a quorum sensing bacterium to initiate or enhance biofilm production. Initiation or enhancement of biofilm formation of beneficial bacteria (those, for example, that provide a health benefit or are used in production of a valuable product) can facilitate or enhance such a health benefit or can be used to enhance or improve production of desirable valuable products. In a specific embodiment, compounds which activate quorum sensing of beneficial gut bacterial can provide a probiotic effect.
[0062] In an embodiment, the methods of the present invention can be used for inhibiting or diminishing the symbiotic behavior of a quorum sensing bacteria. In another embodiment, the methods of the present invention can be used for stimulating, initiating, or enhancing the symbiotic behavior of a quorum sensing bacteria.
[0063] In another embodiment of the methods, the compounds of the present invention can be administered to a subject to initiate modulation of quorum sensing of bacteria. In an embodiment, the administration of an effective amount of a compound of the present invention to a subject can initiate or enhance the symbiotic behavior of quorum sensing bacteria in the subject. In an embodiment, the administration of an effective amount of a compound of the present invention to a subject can disrupt a biofilm of quorum sensing bacteria in the subject. In an embodiment, the administration of an effective amount of a compound of the present invention to a subject can initiate or enhance the symbiotic behavior of a target species or a selected strain of a target species of quorum sensing bacteria in the subject. In an embodiment, the administration of an effective amount of a compound of the present invention to a subject can regulate the virulence of quorum sensing bacteria in the subject. In an embodiment, the administration of an effective amount of a compound of the present invention to a subject can regulate the virulence of a target species or a selected strain of a target species of quorum sensing bacteria in the subject.
[0064] The methods of the present invention also provide for regulation of the level of virulence of quorum sensing bacteria. In an embodiment, one or more compounds of the present invention is brought into contact with a quorum sensing bacteria to selectively regulate the virulence of the bacteria. In an embodiment, a mixture of the compounds of the present invention is brought into contact with a quorum sensing bacteria to selectively regulate the virulence of the bacteria. The amount of each compound in the mixture is that amount effective to achieve a desired effect on regulation of virulence. The methods of the present invention also provide for regulation of the production of a biofilm by quorum sensing bacteria. In an embodiment, one or more compounds of the present invention is brought into contact with a quorum sensing bacteria or bacterial biofilm to selectively regulate the biofilm production by the bacteria. In an embodiment, a mixture of the compounds of the present invention is brought into contact with a quorum sensing bacteria or bacterial biofilm to selectively regulate the biofilm production by the bacteria. The amount of each compound in the mixture is that amount effective for desired regulation of biofilm formation.
[0065] The methods of the present invention also provide for regulation of the virulence, biofilm production, or symbiotic behavior of a quorum sensing bacteria by contacting the bacteria with a photoactive compound and illuminating the bacteria and photoactive compound. In an embodiment, illuminating a photoactive compound of the present invention can change the agonistic or antagonistic behavior of the compound.
[0066] In an embodiment, the present invention provides a surface coating or polymer having incorporated therein a compound of the present invention. The amount of compound or polymer in the surface coating is that sufficient to provide antimicrobial or antifouling effect. In an embodiment, the compounds of the present invention are useful as an antimicrobial and/or antifouling agent. Compounds of the present invention are further useful in a medical, scientific, and/or biological application. In one aspect, the present invention provides a composition comprising one or more compounds of the present invention and a carrier or diluent. In a preferred embodiment, the carrier or diluent comprises a liquid. Such a liquid may comprises an aqueous solvent or a non-aqueous solvent. An exemplary solvent comprises one or more organic solvents. The carrier or diluent may also comprise an ionic liquid. In an embodiment of this aspect, the composition comprises an organic or inorganic polymeric substance. The polymeric substance may comprise one or more compounds of the present invention, admixed with a polymer, bound to a polymer, or adsorbed on to a polymer. In an exemplary embodiment of this aspect, the composition is in the form of a solution or suspension of said at least one compounds of the present invention, preferably in an aerosol or powder formulation.
[0067] In an embodiment of this aspect, the composition is formulated as a disinfectant or cleaning formulation. In another embodiment, the composition is in the form of a powder, a solution, a suspension, a dispersion, an emulsion, or a gel. In an exemplary embodiment, the composition is in the form of a pharmaceutical composition comprising a pharmaceutically acceptable carrier, diluent, and/or excipient and one or more compounds of the present invention. The composition may be in a form suitable for parenteral or non-parenteral administration. A preferred composition may be formulated for topical, intradermal, intramuscular, intraperitoneal, intravenous, subcutaneous, intranasal, epidural, ophthalmic, or oral administration. In an embodiment of this aspect the composition is formulated for administration by infusion or bolus injection, absorption through epithelial or mucocutanous linings and may be administered together with other biologically active agents. In an embodiment, the composition may further be formulated for use in an inhaler or nebulizer.
[0068] In another aspect, the present invention provides a method of treating an infection in a human or animal subject, the method comprising administration to the subject of an effective amount of one or more compounds of the present invention. In an embodiment, the treatment is therapeutic or prophylactic. In an embodiment, the method further comprises administering one or more pharmaceutically acceptable antibacterial compounds to the subject, prior to, at the same time as or after administration of the one or more compounds of this invention.
[0069] In a related embodiment, the present invention provides a method of treating an infection or condition in a subject that is characterized by biofilm formation, the method comprising administering one or more compounds of the present invention. In an embodiment, the method further comprises administering one or more pharmaceutically acceptable antibacterial compounds to the subject, prior to, at the same time as or after administration of the one or more compounds of this invention. In an embodiment, the condition is cystic fibrosis. In an embodiment, the condition is dental caries, periodonitis, otitis media, muscular skeletal infections, necrotizing fasciitis, biliary tract infection, osteomyelitis, bacterial prostatitis, native valve endocarditis, cystic fibrosis pneumonia, or meloidosis. In an embodiment, the condition is a nosocomial infection; preferably the infection is ICU pneumonia or an infection associated with sutures, exit sites, arteriovenous sites, scleral buckles, contact lenses, urinary catheter cystitis, peritoneal dialysis (CAPD) peritonitis, IUDs, endotracheal tubes, Hickman catheters, central venous catheters, mechanical heart valves, vascular grafts, biliary stent blockage, orthopedic devices, or penile prostheses. In an embodiment, the infection is a skin infection, a burn infection, or a wound infection. According to this aspect, the subject may preferably be an immunocompromised individual.
[0070] The present invention further provides a method for treating or preventing biofilm formation on a surface, the method comprising contacting said surface with one or more compounds in an amount effective for affecting biofilm formation of the present invention. In an embodiment, the method further comprises contacting the surface with one or more antibacterial compounds appropriate for the application, prior to, at the same time as or after contact with the one or more compounds of this invention. In an embodiment, the surface is a non-biological surface. In an embodiment, the surface is a natural surface. In an embodiment, the surface is a surface of a plant, seed, wood, fiber or hair. In an embodiment, the surface is a biological surface; preferably the surface is a surface of a tissue, membrane, or skin. In an embodiment, the surface is a hard surface; preferably the surface comprises a metal, an organic polymer, an inorganic polymer, a natural elastomer, a synthetic elastomer, glass, wood, paper, concrete, rock, marble, gypsum, or ceramic. In an embodiment, the said surface is coated or wherein the surface is a coating; in a preferred embodiment, the coating comprises enamel, varnish, or paint.
[0071] In an embodiment of this aspect, the surface is a soft surface, and may be the surface of a fiber comprising a yarn, a textile, a vegetable fiber, or rock wool. In another embodiment, the surface is a porous surface. In an embodiment, the surface is a surface of process equipment or components of cooling equipment. In a preferred embodiment, the process equipment is or is a component of a cooling tower, a water treatment plant, a dairy processing plant, a food processing plant, a chemical process plant, or a pharmaceutical process plant. In a preferred embodiment the surface is that of a filter or a membrane filter.
[0072] In an embodiment of this aspect, the surface is a surface of a toilet bowl, a bathtub, a drain, a high-chair, a counter top, a vegetable, a meat processing room, a butcher shop, food preparation areas, an air duct, an air-conditioner, a carpet, paper or woven product treatment, a diaper, personal hygiene products and a washing machine. In another embodiment, the surface is an industrial surface or a medical surface; preferably the surface is a surface in a hospital, a veterinary hospital, a mortuary, or a funeral parlor.
[0073] In another aspect, the compounds of the present invention are useful as a component of a dentifrice, a mouthwash, or a composition for the treatment of dental caries; for treatment of acne; or for cleaning and/or disinfecting contact lenses. The compounds of the present invention are further useful for incorporation into the surface of a medical device or an implant device. Preferably the implant device is an artificial heart valve, hip joint, an indwelling catheter, pacemaker, or surgical pin. The compounds of the present invention are further useful as an antifouling coating. The present invention further provides an optical lens, wherein at least a part of a surface of the lens is associated with one or more compounds of the present invention. Preferably, the optical lens is a contact lens.
[0074] In another aspect, the present invention provides a biofilm removing or inhibiting composition comprising one or more compounds of the present invention in an amount effective for removing or inhibiting biofilm formation and a vehicle or carrier, wherein the amount of the mixture is effective to remove or disrupt a bacterial biofilm or inhibit normal biofilm formation. An embodiment of this aspect may further comprise a surfactant selected from the group consisting of an anionic surfactant, a nonionic surfactant, an amphoteric surfactant, a biological surfactant, and any combination of these; or a compound selected from the group consisting of an antibacterial which includes among others a biocide, a fungicide, an antibiotic, and any combination of these.
[0075] In another aspect, the present invention provides a method of removing a biofilm from a surface, the method comprising the step of administering a cleaning-effective amount of one or more compounds of the present invention to a biofilm-containing surface. A preferred method of this aspect comprises the step of administering an effective amount of one or more compounds of the present invention to the surface, wherein the amount is effective to prevent biofilm formation. Such a surface may be a hard or rigid surface or a surface selected from the group consisting of glazed ceramic, porcelain, glass, metal, wood, chrome, plastic, vinyl, composite materials (such as Formica® (Formica Corporation, Cincinnatti, Ohio), and the surface of a drainpipe. In an embodiment, the surface is a soft or flexible surface, or the surface is selected from the group consisting of a shower curtain or liner, upholstery, laundry, clothing, and carpeting. In an embodiment, the surface is a biological surface and the effective amount is a therapeutically effective amount for application to the biological surface for inhibiting biofilm formation. The compounds of the present invention are useful in particular, for removing or disrupting a biofilm produced by a bacterium of the class Pseudomonas, a bacterium is of the species Pseudomonas aeruginosa, or an organism selected from the group consisting of bacteria, algae, fungi and protozoa. In a specific aspect, this method further comprises a step of applying or administering to a biofilm-containing surface an antibacterial compound before, at the same time as or after applying or administering the one or more compounds of this invention.
[0076] In another aspect, the invention provides a medicament for treating an infection or for disruption of a biofilm which comprises one or more of the compounds of this invention e.g., those of formulas I-VI, and a method for making a medicament which comprises one or more of the compounds of this invention. In particular, the method comprises the step of combining one or more compounds of this invention with a pharmaceutically acceptable carrier to form a pharmaceutical composition for treatment of infection and/or biofilm formation. In another particular embodiment, the method further comprises combining an antibacterial compound appropriate for the application to a medicament along with one or more compounds of this invention.
[0077] Without wishing to be bound by any particular theory, there can be discussion herein of beliefs or understandings of underlying principles relating to the invention. It is recognized that regardless of the ultimate correctness of any mechanistic explanation or hypothesis, an embodiment of the invention can nonetheless be operative and useful.
BRIEF DESCRIPTION OF THE FIGURES
[0078] FIG. 1 (2 pages) illustrates exemplary HG groups.
[0079] FIG. 2 (3 pages) illustrates exemplary HG groups.
[0080] FIG. 3 illustrates exemplary A groups.
[0081] FIG. 4 provides structures (and reference numbers) of exemplary non-homoserine lactone based autoinducer analogs synthesized by the method highlighted in Scheme 1.
[0082] FIG. 5A is a bar graph showing the results of agonism assay for initial heterocyclic and carbocyclic library (Scheme 1) shown as a percent of the positive control. The black bars are DH5α (pJN105L+pSC11) and the grey bars are PA01 MW1 (pUM15). Agonism positive control=activity of the reporter strain at full turn on for the strain. Full turn on for each strain: DH5α (pJN105L+pSC11)—100 nM OdDHL; PA01 MW1 (pUM15)—100 μM OdDHL. Negative control (Neg)=bacteria in the absence of natural and synthetic ligand. Error bars=standard deviation of the mean of triplicate samples.
[0083] FIG. 5B is a bar graph showing the results of agonism assay for initial heterocyclic and carbocyclic library (Scheme 1) shown as a percent of the positive control. Antagonism positive control (Pos)=activity of the reporter strain in the absence of synthetic ligand at the EC50 value for the strain. Strain EC50 values: DH5α (pJN105L+pSC11)—10 nM OdDHL; PA01 MW1 (pUM15)—1 μM OdDHL. Negative control (Neg)=bacteria in the absence of natural and synthetic ligand. Error bars=standard deviation of the mean of triplicate samples.
[0084] FIG. 6 provides structures (with reference numbers) of the racemic thiolactone library prepared as illustrated in Scheme 2.
[0085] FIGS. 7A and 7B are bar grafts presenting results of agonism (7A) and antagonism (7B) assays for the racemic thiolactone library ( FIG. 6 ). The biological testing conditions were the same as described in FIGS. 5A and 5B , respectively.
[0086] FIG. 8 provides structures (with reference numbers) of the enantiopure thiolactone library and EDC couplings.
[0087] FIGS. 9A-9H are bar grafts comparing agonism and antagonism of the racemic and enantiopure compounds of Libraries of FIG. 6 and FIG. 8 . All synthetic ligands were tested at 10 μM using standard methods described in FIGS. 5A and 5B .
[0088] FIGS. 10A and B are graphs comparing the functional half-lives of autoinducers as described in Example 4.
[0089] FIG. 11 provides structures(with reference numbers) of compounds having glycine ethyl ester structures.
[0090] FIGS. 12A and 12B are bar graphs with results of activity assays of the glycine ethyl ester library (for agonism 12A and antagonism 12 B) according to the assay conditions described in FIGS. 5A and 5B .
[0091] FIG. 13 provides structures (with reference numbers) of an exemplary library having cyclopentyl amine head groups.
[0092] FIG. 14 provides structures (with reference numbers) of an exemplary library having aniline head groups.
[0093] FIGS. 15A and 15B are bar graphs with results of activity assays of the compounds of FIGS. 13 and 14 (for agonism 15A and antagonism 15 B) according to the assay conditions described in FIGS. 5A and 5B .
DETAILED DESCRIPTION OF THE INVENTION
[0094] Unless defined otherwise, all technical and scientific terms used herein have the broadest meanings as commonly understood by one of ordinary skill in the art to which this invention pertains. In addition, hereinafter, the following definitions apply:
[0095] Quorum sensing assays conducted as described herein can be used to assess whether or no a given compound of the invention is a quorum sensing agonist or antagonist of a given bacterium, particularly a given Gram-Negative bacterium. It will be appreciated by one of ordinary skill in the art that assays other than those described herein can be employed to assess activation of or inhibition of biofilm formation as well as the effect of compounds of this invention on bacterial growth.
[0096] As defined herein, “contacting” means that a compound of the present invention is provided such that it is capable of making physical contact with another element, such as a microorganism, a microbial culture, a biofilm, or a substrate. In another embodiment, the term “contacting” means that a compound of the present invention is introduced into a subject receiving treatment, and the compound is allowed to come in contact in vivo.
[0097] Compounds of this invention that disrupt bacterial quorum sensing and biofilm formation can be used in combination with antimicrobial and antibacterial compounds (other than compounds which inhibit quorum sensing). The terms antimicrobial and antibacterial are employed broadly herein to refer to any compound that exhibits a growing inhibition activity on a microorganism or bacterium, respectively. A subset of such antimicrobial and antibacterial compounds are pharmaceutically acceptable for use in the treatment of humans and animals. A subset of antimicrobial and antibacterial compounds are biocides. A subset of antimicrobial and antibacterial compounds are antibiotics. In specific embodiments, compounds of the invention which are inhibitors or quorum sensing and biofilm formation are used to augment or facilitate the action of convention antibiotic treatment. The invention provides methods in which contact with or treatment with one or more quorum sensing compounds of the invention which inhibit quorum sensing is combined with contract with or treatment with one or more antimicrobial or antibacterial compounds. The invention provides methods in which contact with or treatment with one or more quorum sensing compounds of the invention which inhibit quorum sensing is combined with contract with or treatment with one or more antibiotics. Antibiotics include among others beta-lactam antibiotics, cephaosporins, clavulanic acid and derivatives thereof, aminoglycosides, tetracyclines, macrolide antibiotics.
[0098] Quorum sensing inhibitors of the invention can also generally be combined with antimicrobial agents, including antifungal agents, and antiviral agents.
[0099] In some cases, combination of one or more quorum sensing inhibitor of this invention with one or more antibacterial compound, antimicrobial compound or antiviral agent can enhance the activity of one or more antibacterial compound, antimicrobial compound or antiviral agent. In some case the combination of one or more quorum sensing inhibitor with one or more antibacterial compound, antimicrobial compound or antiviral agent synergizes the activity of the one or more antibacterial compound, antimicrobial compound or antiviral agent.
[0100] One or more quorum sensing inhibitor compounds of this invention can be combined with one or more antibacterial compounds, one or more antimicrobial compounds, one or more antiviral compounds and more specifically one or more antibiotics in pharmaceutically acceptable compositions useful for treatment of infections. Such pharmaceutical compositions typically further comprise a pharmaceutically acceptable carrier. Such combination compositions and medicaments can be employed for treatment of infection.
[0101] Contact with or treatment employing one or more quorum sensing inhibitor compounds of this invention can be combined with contact with or treatment with one or more antibacterial compounds, one or more antimicrobial compounds, one or more antiviral compounds and more specifically one or more antibiotics. In this case, contact or treatment is with one or more separate pharmaceutical composition which may be put in contact with the area to be treated (e.g., applied to a surface, including a biological surface) or administered to a subject at the same time or at different times. The quorum sensing inhibitor can be applied or administered before, after or at the same time as the antibacterial compound, antimicrobial compound or antiviral compound is applied or administered.
[0102] Aliphatic groups include straight chain, branched, and cyclic groups having a carbon backbone having from 1 to 30 carbon atoms. Aliphatic groups include alkyl groups, alkenyl groups, alkynyl groups, and aryl groups. Aliphatic groups are optionally substituted with one or more non-hydrogen substituents. Substituted aliphatic groups include among others those which are substituted with aryl groups, which in turn can be optionally substituted. Substituted aliphatic groups include fully halogenated or semihalogenated aliphatic groups, such as aliphatic groups having one or more hydrogens replaced with one or more fluorine atoms, chlorine atoms, bromine atoms and/or iodine atoms. Substituted aliphatic groups include fully fluorinated or semifluorinated aliphatic groups, such as aliphatic groups having one or more hydrogens replaced with one or more fluorine atoms. Aliphatic groups are optionally substituted with one or more protecting groups.
[0103] Alkyl groups include straight-chain, branched and cyclic alkyl groups. Alkyl groups include those having from 1 to 30 carbon atoms. Alkyl groups include small alkyl groups having 1 to 3 carbon atoms. Alkyl groups include medium length alkyl groups having from 4-10 carbon atoms. Alkyl groups include long alkyl groups having more than 10 carbon atoms, particularly those having 10-30 carbon atoms. Cyclic alkyl groups include those having one or more rings. Cyclic alkyl groups include those having a 3-, 4-, 5-, 6-, 7-, 8-, 9- or 10-member carbon ring and particularly those having a 3-, 4-, 5-, 6-, 7-, or 8-member ring. The carbon rings in cyclic alkyl groups can also carry aliphatic groups. Cyclic alkyl groups can include bicyclic and tricyclic alkyl groups. Alkyl groups are optionally substituted with one or more non-hydrogen substituents. Substituted alkyl groups include among others those which are substituted with aliphatic groups, which in turn can be optionally substituted. Specific alkyl groups include methyl, ethyl, n-propyl, iso-propyl, cyclopropyl, n-butyl, s-butyl, t-butyl, cyclobutyl, n-pentyl, branched-pentyl, cyclopentyl, n-hexyl, branched hexyl, and cyclohexyl groups, all of which are optionally substituted. Substituted alkyl groups include fully halogenated or semihalogenated alkyl groups, such as alkyl groups having one or more hydrogens replaced with one or more fluorine atoms, chlorine atoms, bromine atoms and/or iodine atoms. Substituted alkyl groups include fully fluorinated or semifluorinated alkyl groups, such as alkyl groups having one or more hydrogens replaced with one or more fluorine atoms.
[0104] An alkoxy group is an alkyl group, as broadly discussed above, linked to oxygen and can be represented by the formula R—O—.
[0105] Alkenyl groups include straight-chain, branched and cyclic alkenyl groups. Alkenyl groups include those having 1, 2 or more double bonds and those in which two or more of the double bonds are conjugated double bonds. Alkenyl groups include those having from 2 to 20 carbon atoms. Alkenyl groups include small alkenyl groups having 2 to 3 carbon atoms. Alkenyl groups include medium length alkenyl groups having from 4-10 carbon atoms. Alkenyl groups include long alkenyl groups having more than 10 carbon atoms, particularly those having 10-20 carbon atoms. Cyclic alkenyl groups include those having one or more rings. Cyclic alkenyl groups include those in which a double bond is in the ring or in an alkenyl group attached to a ring. Cyclic alkenyl groups include those having a 3-, 4-, 5-, 6-, 7-, 8-, 9- or 10-member carbon ring and particularly those having a 3-, 4-, 5-, 6- or 7-member ring. The carbon rings in cyclic alkenyl groups can also carry aliphatic groups. Cyclic alkenyl groups can include bicyclic and tricyclic aliphatic groups. Alkenyl groups are optionally substituted with one or more non-hydrogen substituents. Substituted alkenyl groups include among others those which are substituted with aliphatic groups, which groups in turn can be optionally substituted. Specific alkenyl groups include ethenyl, prop-1-enyl, prop-2-enyl, cycloprop-1-enyl, but-1-enyl, but-2-enyl, cyclobut-1-enyl, cyclobut-2-enyl, pent-1-enyl, pent-2-enyl, branched pentenyl, cyclopent-1-enyl, hex-1-enyl, branched hexenyl, cyclohexenyl, all of which are optionally substituted. Substituted alkenyl groups include fully halogenated or semihalogenated alkenyl groups, such as alkenyl groups having one or more hydrogens replaced with one or more fluorine atoms, chlorine atoms, bromine atoms and/or iodine atoms. Substituted alkenyl groups include fully fluorinated or semifluorinated alkenyl groups, such as alkenyl groups having one or more hydrogens replaced with one or more fluorine atoms.
[0106] Alkynyl groups include straight-chain, branched and cyclic alkynyl groups. Alkynyl groups include those having 1, 2 or more triple bonds and those in which two or more of the triple bonds are conjugated triple bonds. Alkynyl groups include those having from 2 to 20 carbon atoms. Alkynyl groups include small alkynyl groups having 2 to 3 carbon atoms. Alkynyl groups include medium length alkynyl groups having from 4-10 carbon atoms. Alkynyl groups include long alkynyl groups having more than 10 carbon atoms, particularly those having 10-20 carbon atoms. Cyclic alkynyl groups include those having one or more rings. Cyclic alkynyl groups include those in which a triple bond is in the ring or in an alkynyl group attached to a ring. Cyclic alkynyl groups include those having a 3-, 4-, 5-, 6-, 7-, 8-, 9- or 10-member carbon ring and particularly those having a 3-, 4-, 5-, 6- or 7-member ring. The carbon rings in cyclic alkynyl groups can also carry aliphatic groups. Cyclic alkynyl groups can include bicyclic and tricyclic aliphatic groups. Alkynyl groups are optionally substituted with one or more non-hydrogen substituents. Substituted alkynyl groups include among others those which are substituted with alkyl or aryl groups, which groups in turn can be optionally substituted. Alkynyl groups include acetyl, methylacetyl, 1-pentynyl, and 2-pentynyl, all of which are optionally substituted. Substituted alkynyl groups include fully halogenated or semihalogenated alkynyl groups, such as alkynyl groups having one or more hydrogens replaced with one or more fluorine atoms, chlorine atoms, bromine atoms and/or iodine atoms. Substituted alkynyl groups include fully fluorinated or semifluorinated alkynyl groups, such as alkynyl groups having one or more hydrogens replaced with one or more fluorine atoms.
[0107] Aryl groups include groups having one or more 5- or 6-member aromatic or heteroaromatic rings. Aryl groups can contain one or more fused aromatic rings. Heteroaromatic rings can include one or more N, O, or S atoms in the ring. Heteroaromatic rings can include those with one, two or three N, those with one or two O, and those with one or two S, or combinations of one or two or three N, O or S. Aryl groups are optionally substituted with one or more non-hydrogen substituents. Substituted aryl groups include among others those which are substituted with alkyl or alkenyl groups, which groups in turn can be optionally substituted. Specific aryl groups include phenyl groups, biphenyl groups, pyridinyl groups, and naphthyl groups, all of which are optionally substituted. Substituted aryl groups include fully halogenated or semihalogenated aryl groups, such as aryl groups having one or more hydrogens replaced with one or more fluorine atoms, chlorine atoms, bromine atoms and/or iodine atoms. Substituted aryl groups include fully fluorinated or semifluorinated aryl groups, such as aryl groups having one or more hydrogens replaced with one or more fluorine atoms. The term heteroaryl is used for aryl groups having one or more heteroaromatic rings. Aryl groups include those that are not heteroaryl groups.
[0108] Arylalkyl groups are alkyl groups substituted with one or more aryl groups wherein the alkyl groups optionally carry additional substituents and the aryl groups are optionally substituted. Specific alkylaryl groups are phenyl-substituted alkyl groups, e.g., phenylmethyl groups. Alkylaryl groups are alternatively described as aryl groups substituted with one or more alkyl groups wherein the alkyl groups optionally carry additional substituents and the aryl groups are optionally substituted. Specific alkylaryl groups are alkyl-substituted phenyl groups such as methylphenyl. Substituted arylalkyl groups include fully halogenated or semihalogenated arylalkyl groups, such as arylalkyl groups having one or more alkyl and/or aryl having one or more hydrogens replaced with one or more fluorine atoms, chlorine atoms, bromine atoms and/or iodine atoms.
[0109] The term “heterocyclic or heterocyclyl” generically refers to a monoradical that contains at least one ring of atoms, which may be a saturated, unsaturated wherein one or more carbons of the ring are replaced with a heteroatom (a non-carbon atom) To satisfy valence the heteroatom may be bonded to H or a substituent groups. Ring carbons may be replaced with —O—, —S—, —NR—, —N═ among others. More specifically heterocyclic groups can contain one or two 4-6 member rings wherein two rings may be fused. In specific embodiments, one or two rings of the heterocyclic group can contain one, two or three heteroatoms, particularly —O—, —S—, —NR— or —N═ and combinations of such heteroatoms.
[0110] Protecting groups are groups substituted onto an aliphatic hydrocarbon for protection of one or more substituents, for example protection of alcohols, amines, carbonyls, and/or carboxylic acids. Protecting groups include, but are not limited to, acetyl groups, MEM groups, MOM groups, PMB groups, Piv groups, THP groups, TMS groups, TBDMS groups, TIPS groups, methyl ethers, Cbz groups, BOC groups, FMOC groups, benzyl groups, PMP groups, acetal groups, ketal groups, acylal groups, dithiane groups, methyl esters, benzyl esters, t-butyl esters, and silyl esters. These and other protecting groups known in the art of organic synthesis may be optionally used as a substituent of an aliphatic group.
[0111] Optional substitution of aliphatic groups includes substitution with one or more aliphatic groups, wherein the aliphatic groups are optionally substituted.
[0112] Optional substituents for aliphatic groups include among others: —R, —COOR, —COR, —CON(R)2, —OCON(R)2, —N(R)2, —SR, —SO2R, —SOR, —OCOOR, —SO2N(R)2, and —OR; wherein R is selected from the group consisting of, a hydrogen, a halogen, an amine group, a substituted or unsubstituted unbranched C1-C12 acyclic aliphatic group, a substituted or unsubstituted branched C1-C12 acyclic aliphatic group, a substituted or unsubstituted C3-C8 cycloalkyl group, a substituted or unsubstituted C3-C8 cycloalkenyl group, a fluorinated C1-C12 alkyl group, a substituted or unsubstituted aryl group, a substituted or unsubstituted heterocycle, a substituted or unsubstituted C1-C12 alkoxy group, a fluorinated C1-C12 alkoxy group, a hydroxyl group, a nitrile group, an azide group, a nitro group, an acyl group, a thiol group, a protecting group, —COOR, —COR, —CON(R)2, —OCON(R)2, —N(R)2, —SR, —SO2R, —SOR, —OCOOR, —SO2N(R)2, and —OR; additionally, R and R can form a ring;.
[0113] Specific substituted alkyl groups include haloalkyl groups, particularly trihalomethyl groups and specifically trifluoromethyl groups. Specific substituted aryl groups include mono-, di-, tri, tetra- and pentahalo-substituted phenyl groups; mono-, di-, tri-, tetra-, penta-, hexa-, and hepta-halo-substituted naphthalene groups; 3- or 4-halo-substituted phenyl groups, 3- or 4-alkyl-substituted phenyl groups, 3- or 4-alkoxy-substituted phenyl groups, 3- or 4-RCO-substituted phenyl, 5- or 6-halo-substituted naphthalene groups. More specifically, substituted aryl groups include acetylphenyl groups, particularly 4-acetylphenyl groups; fluorophenyl groups, particularly 3-fluorophenyl and 4-fluorophenyl groups; chlorophenyl groups, particularly 3-chlorophenyl and 4-chlorophenyl groups; methylphenyl groups, particularly 4-methylphenyl groups, and methoxyphenyl groups, particularly 4-methoxyphenyl groups.
[0114] As to any of the above groups which contain one or more substituents, it is understood, that such groups do not contain any substitution or substitution patterns which are sterically impractical and/or synthetically non-feasible. In addition, the compounds of this invention include all stereochemical isomers arising from the substitution of these compounds.
[0115] The term “effective amount” is used generically herein to refer to the amount of a given compound or in case of a mixture the combined amount of mixture components that provides a measureable effect for a listed function. For example, in certain aspects of the invention, a compound of the invention is contacted with an element in order to disrupt a biofilm and in this case, the effective amount or combined effective amount of the compound or compounds is that amount that shows a measurable disruption of a biofilm. The effective amount will vary dependent upon the stated function, the environment or element being contacted, the organism forming the biofilm or which is to be contacted, the state of development of the biofilm, among other conditions of the use of the compound. It will be understood by one of ordinary skill in the art, that for a given application, the effective amount can be determined by application of routine experimentation and without undue experimentation by methods that are described herein or that are known in the art.
[0116] The term “therapeutically effective amount” is used generically herein to refer to the amount of a given compound or in case of a mixture the combined amount of a mixture of components when administered to the individual (including a human, or non-human animal) that provides a measureable therapeutic effect for a listed disease, disorder or condition to at least partially ameliorate a symptom of such disease, disorder or condition. The present invention provides methods of treating disorders, diseases conditions and symptoms in a human or non-human animal and particularly in a human, by administering to an individual in need of treatment or prophylaxis, a therapeutically effective amount of one or more compounds of this invention to the individual in need thereof. The result of treatment can be partially or completely alleviating, inhibiting, preventing, ameliorating and/or relieving the disorder, condition or one or more symptoms thereof. As is understood in the art, the therapeutically effective amount of a given compound will depend at least in part upon, the mode of administration, any carrier or vehicle (e.g., solution, emulsion, etc.) employed, the extent of damage and the specific individual (human or non-human) to whom the compound is to be administered (age, weight, condition, sex, etc.). The dosage requirements needed to achieve the “therapeutically effective amount” vary with the particular compositions employed, the route of administration, the severity of the symptoms presented and the particular subject being treated. Based on the results obtained in standard pharmacological test procedures, projected daily dosages of active compound can be determined as is understood in the art.
[0117] Administration is intended to encompass administration of a compound, pharmaceutically acceptable salt, solvate or ester thereof alone or in a pharmaceutically acceptable carrier thereof or administration of a prodrug derivative or analog of a compound of this invention which will form an equivalent amount of the active compound or substance within the body. An individual in need of treatment or prophylaxis includes those who have been diagnosed to have a given disorder or condition and to those who are suspected, for example, as a consequence of the display of certain symptoms, of having such disorders or conditions.
[0118] Compounds of this invention can be employed in unit dosage form, e.g. as tablets or capsules. In such form, the active compound or more typically a pharmaceutical composition containing the active compound is sub-divided in unit dose containing appropriate quantities of the active compound; the unit dosage forms can be packaged compositions, for example, packaged powders, vials, ampules, pre-filled syringes or sachets containing liquids. The unit dosage form can be, for example, a capsule or tablet itself, or it can be the appropriate number of any such compositions in package form.
[0119] The dosage can vary within wide limits and as is understood in the art will have to be adjusted to the individual requirements in each particular case. By way of general guidance, the daily oral dosage can vary from about 0.01 mg to 1000 mg, 0.1 mg to 100 mg, or 10 mg to 500 mg per day of a compound of formulas herein or of the corresponding amount of a pharmaceutically acceptable salt thereof. The daily dose may be administered as single dose or in divided doses and, in addition, the upper limit can also be exceeded when this is found to be indicated.
[0120] Any suitable form of administration can be employed in the method herein. The compounds of this invention can, for example, be administered in oral dosage forms including tablets, capsules, pills, powders, granules, elixirs, tinctures, suspensions, syrups and emulsions. Oral dosage forms may include sustained release or timed release formulations. The compounds of this invention may also be administered topically, intravenously, intraperitoneally, subcutaneously, or intramuscularly, all using dosage forms well known to those of ordinary skill in the pharmaceutical arts.
[0121] Compounds of this invention can also be administered in intranasal form by topical use of suitable intranasal vehicles. For intranasal or intrabronchial inhalation or insulation, the compounds of this invention may be formulated into an aqueous or partially aqueous solution, which can then be utilized in the form of an aerosol. Administration includes any form of administration that is known in the art and is intended to encompass administration in any appropriate dosage form and further is intended to encompass administration of a compound, alone or in a pharmaceutically acceptable carrier. Pharmaceutical carriers are selected as is known in the art based on the chosen route of administration and standard pharmaceutical practice.
[0122] The compounds of this invention can also be administered to the eye, preferably as a topical ophthalmic formulation. The compounds of this invention can also be combined with a preservative and an appropriate vehicle such as mineral oil or liquid lanolin to provide an ophthalmic ointment. The compounds of this invention may be administered rectally or vaginally in the form of a conventional suppository. The compounds of this invention may also be administered transdermally through the use of a transdermal patch containing the active compound and a carrier that is inert to the active compound, is non toxic to the skin, and allows delivery of the agent for systemic absorption into the blood stream via the skin.
[0123] The compounds of the invention may be administered employing an occlusive device. A variety of occlusive devices can be used to release an ingredient into the blood stream such as a semipermeable membrane covering a reservoir containing the active ingredient with or without a carrier, or a matrix containing the active ingredient. Other occlusive devices are known in the literature.
[0124] Pharmaceutical compositions and medicaments of this invention comprise one or more compounds in combination with a pharmaceutically acceptable carrier, excipient, or diluent. Such compositions and medicaments are prepared in accordance with acceptable pharmaceutical procedures, such as, for example, those described in Remington's Pharmaceutical Sciences, 17th edition, ed. Alfonoso R. Gennaro, Mack Publishing Company, Easton, Pa. (1985), which is incorporated herein by reference in its entirety. The invention also encompasses method for making a medicament employing one or more compounds of this invention which exhibit a therapeutic effect.
[0125] Pharmaceutically acceptable carriers are those carriers that are compatible with the other ingredients in the formulation and are biologically acceptable. Carriers can be solid or liquid. Solid carriers can include one or more substances that can also act as flavoring agents, lubricants, solubilizers, suspending agents, fillers, glidants, compression aids, binders, tablet-disintegrating agents, or encapsulating materials. Liquid carriers can be used in preparing solutions, suspensions, emulsions, syrups and elixirs. The active ingredient can be dissolved or suspended in a pharmaceutically acceptable liquid carrier such as water (of appropriate purity, e.g., pyrogen-free, sterile, etc.), an organic solvent, a mixture of both, or a pharmaceutically acceptable oil or fat. The liquid carrier can contain other suitable pharmaceutical additives such as, for example, solubilizers, emulsifiers, buffers, preservatives, sweeteners, flavoring agents, suspending agents, thickening agents, colors, viscosity regulators, stabilizers or osmo-regulators. Compositions for oral administration can be in either liquid or solid form.
[0126] Suitable solid carriers include, for example, calcium phosphate, magnesium stearate, talc, sugars, lactose, dextrin, starch, gelatin, cellulose, methyl cellulose, sodium carboxymethyl cellulose, polyvinylpyrrolidine, low melting waxes and ion exchange resins. Suitable examples of liquid carriers for oral and parenteral administration include water of appropriate purity, aqueous solutions (particularly containing additives, e.g. cellulose derivatives, sodium carboxymethyl cellulose solution), alcohols (including monohydric alcohols and polyhydric alcohols e.g. glycols) and their derivatives, and oils. For parenteral administration, the carrier can also be an oily ester such as ethyl oleate and isopropyl myristate. Sterile liquid carriers are used in sterile liquid form compositions for parenteral administration. The liquid carrier for pressurized compositions can be halogenated hydrocarbon or other pharmaceutically acceptable propellant. Liquid pharmaceutical compositions that are sterile solutions or suspensions can be administered by, for example, intramuscular, intraperitoneal or subcutaneous injection. Sterile solutions can also be administered intravenously. Compositions for oral administration can be in either liquid or solid form. The carrier can also be in the form of creams and ointments, pastes, and gels. The creams and ointments can be viscous liquid or semisolid emulsions of either the oil-in-water or water-in-oil type. Pastes comprised of absorptive powders dispersed in petroleum or hydrophilic petroleum containing the active ingredient can also be suitable.
[0127] The term “pharmaceutically acceptable salts” refers to those salts which retain the biological effectiveness and properties of the free bases or free acids, which are not biologically or otherwise undesirable. The salts are formed with inorganic acids such as hydrochloric acid, hydrobromic acid, sulfuric acid, nitric acid, phosphoric acid and the like, preferably hydrochloric acid, and organic acids such as acetic acid, propionic acid, glycolic acid, pyruvic acid, oxylic acid, maleic acid, malonic acid, succinic acid, fumaric acid, tartaric acid, citric acid, benzoic acid, cinnamic acid, mandelic acid, methanesulfonic acid, ethanesulfonic acid, p-toluenesulfonic acid, salicylic acid, N-acetylcystein and the like.
[0128] In addition these salts may be prepared from addition of an inorganic base or an organic base to the free acid. Salts derived from an inorganic base include, but are not limited to, the sodium, potassium, lithium, ammonium, calcium, magnesium salts and the like. Salts derived from organic bases include, but are not limited to salts of primary, secondary, and tertiary amines, substituted amines including naturally occurring substituted amines, cyclic amines and basic ion exchange resins, such as isopropylamine, trimethylamine, diethylamine, triethylamine, tripropylamine, ethanolamine, lysine, arginine,N-ethylpiperidine, piperidine, polyimine resins and the like. Compounds of formula I can also be present in the form of zwitterions.
[0129] Pharmaceutically acceptable salts comprise pharmaceutically-acceptable anions and/or cations. Pharmaceutically-acceptable cations include among others, alkali metal cations (e.g., Li+, Na+, K+), alkaline earth metal cations (e.g., Ca2+, Mg2+), non-toxic heavy metal cations and ammonium (NH4+) and substituted ammonium (N(R′)4+, where R′ is hydrogen, alkyl, or substituted alkyl, i.e., including, methyl, ethyl, or hydroxyethyl, specifically, trimethyl ammonium, triethyl ammonium, and triethanol ammonium cations). Pharmaceutically-acceptable anions include among other halides (e.g., Cl—, Br—), sulfate, acetates (e.g., acetate, trifluoroacetate), ascorbates, aspartates, benzoates, citrates, and lactate.
[0130] Compounds of the invention can have prodrug forms. Prodrugs of the compounds of the invention are useful in the methods of this invention. Any compound that will be converted in vivo to provide a biologically, pharmaceutically or therapeutically active form of a compound of the invention is a prodrug. Various examples and forms of prodrugs are well known in the art. Examples of prodrugs are found, inter alia, in Design of Prodrugs, edited by H. Bundgaard, (Elsevier, 1985), Methods in Enzymology, Vol. 42, at pp. 309-396, edited by K. Widder, et. al. (Academic Press, 1985); A Textbook of Drug Design and Development, edited by Krosgaard-Larsen and H. Bundgaard, Chapter 5, “Design and Application of Prodrugs,” by H. Bundgaard, at pp. 113-191, 1991); H. Bundgaard, Advanced Drug Delivery Reviews, Vol. 8, p. 1-38 (1992); H. Bundgaard, et al., Journal of Pharmaceutical Sciences, Vol. 77, p. 285 (1988); and Nogrady (1985) Medicinal Chemistry A Biochemical Approach, Oxford University Press, New York, pages 388-392).
[0131] The invention expressly includes pharmaceutically usable solvates of compounds according to formulas herein. The compounds of formula I can be solvated, e.g. hydrated. The solvation can occur in the course of the manufacturing process or can take place, e.g. as a consequence of hygroscopic properties of an initially anhydrous compound of formulas herein (hydration).
[0132] In specific embodiments herein, compounds 2, 13, 18E, 20E, 23E, 25E 30E, 32, 33, 34, 35, 36, 37, 38, 39 are particularly useful for disruption of bacterial quorum sensing and biofilm disruption, particularly in E. coli, V. fischeri and/or A. tumefaciens.
[0133] In specific embodiments herein, compounds 3, and 19E are particularly useful for activation of bacterial quorum sensing and biofilm formation, particularly in E. coli, V. fischeri and/or P.aeruginosa.
[0134] In specific embodiments herein, compounds 2, 13, 18E, 30E, 32, 33, 34, 35, 36, 37 are particularly useful for disruption of bacterial quorum sensing and biofilm disruption in E. coli. In specific embodiments, compounds 1E, 18E, 20E, 22E, 23E, 25E, 26E, 27E, 28E, 30E, 33, 34, 36, 38 and 39 are particularly useful for disruption of bacterial quorum sensing and biofilm disruption in V. fischeri. In specific embodiments herein, compounds 1E, 26E, 27E, and 30E are particularly useful for disruption of bacterial quorum sensing and biofilm formation, particularly in A. tumefaciens.
[0135] In specific embodiments herein, compounds 3, 14, 16, 17, 1E, 19E, 22E, 26E, 27E, 28E, and 31 are particularly useful for activation of bacterial quorum sensing and biofilm formation in E. coli. In specific embodiments herein compound 24E is particularly useful for activation of bacterial quorum sensing and biofilm formation in A. tumefaciens. In specific embodiments herein compound 19E is particularly useful for activation of bacterial quorum sensing and biofilm formation in V. fischeri. In specific embodiments herein compounds 3 and 1E are particularly useful for activation of bacterial quorum sensing and biofilm formation in P. aeruginosa.
[0136] In specific embodiments herein compounds of the formulas herein which exhibit 20% or more inhibition in quorum sensing antagonism assays as described in the examples herein are particularly useful for disruption of bacterial quorum sensing and bacterial biofilm formation. In specific embodiments herein compounds of the formulas herein which exhibit 50% or more inhibition in quorum sensing antagonism assays as described in the examples herein are particularly useful for disruption of bacterial quorum sensing and bacterial biofilm formation. In specific embodiments herein compounds of the formulas herein which exhibit 75% or more inhibition in quorum sensing antagonism assays as described in the examples herein are particularly useful for disruption of bacterial quorum sensing and bacterial biofilm formation.
[0137] In specific embodiments herein compounds of the formulas herein which exhibit 20% or more activation in quorum sensing agonism assays as described in the examples herein are particularly useful for activation of bacterial quorum sensing and bacterial biofilm formation. In specific embodiments herein compounds of the formulas herein which exhibit 50% or more activation in quorum sensing agonism assays as described in the examples herein are particularly useful for activation of bacterial quorum sensing and bacterial biofilm formation. In specific embodiments herein compounds of the formulas herein which exhibit 75% or more activation in quorum sensing agonism assays as described in the examples herein are particularly useful for activation of bacterial quorum sensing and bacterial biofilm formation.
[0138] Compounds of this invention are additionally useful as tools for use in research in the study of quorum sensing in bacteria.
[0139] Well-known methods for assessment of drugability can be used to further assess active compounds of the invention for application to given therapeutic application. The term “drugability” relates to pharmaceutical properties of a prospective drug for administration, distribution, metabolism and excretion. Drugability is assessed in various ways in the art. For example, the “Lipinski Rule of 5” for determining drug-like characteristics in a molecule related to in vivo absorption and permeability can be applied (C. A. Lipinski, F. Lombardo, B. W. Dominy, P. J. Feeney, Experimental and computational approaches to estimate solubility and permeability in drug discovery and development settings, Adv. Drug Del. Rev., 2001, 46, 3-26 and Arup K. Ghose, Vellarkad N. Viswanadhan, and John J. Wendoloski, A Knowledge-Based Approach in Designing Combinatorial or Medicinal Chemistry Libraries for Drug Discovery, J. Combin. Chem., 1999, 1, 55-68.) In general a preferred drug for oral administration exhibits no more than one violation of the following rules:
[0140] (1) Not more than 5 hydrogen bond donors (e.g., nitrogen or oxygen atoms with one or more hydrogens);
[0141] (2) Not more than 10 hydrogen bond acceptors (e.g., nitrogen or oxygen atoms);
[0142] (3) Molecular weight under 500 g/mol and more preferably between 160 and 480; and
[0143] (4) log P less than 5 and more preferably between −0.4 to +5.6 and yet more preferably −1<log P<2.
[0144] Compounds of this invention preferred for therapeutic application include those that do not violate one or more of 1-4 above.
[0145] Compounds of this invention preferred for therapeutic application include those having log P less than 5 and more preferably between −0.4 to +5.6 and yet more preferably −1<log P<2.
[0146] The compounds of this invention may contain one or more chiral centers. Accordingly, this invention is intended to include racemic mixtures, diasteromers, enantiomers and mixture enriched in one or more steroisomer. The scope of the invention as described and claimed encompasses the racemic forms of the compounds as well as the individual enantiomers and non-racemic mixtures thereof.
[0147] It is understood that this invention is not limited to the particular methodology, protocols, cell lines, and reagents described, as these may vary. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention which will be limited only by the appended claims.
[0148] It must be noted that as used herein and in the appended claims, the singular forms “a”, “an”, and “the” include plural reference unless the context clearly dictates otherwise. Thus, for example, reference to “a cell” includes a plurality of such cells and equivalents thereof known to those skilled in the art, and so forth. As well, the terms “a” (or “an”), “one or more” and “at least one” can be used interchangeably herein.
[0149] As used herein, the term “treating” includes preventative as well as disorder remittent treatment. As used herein, the terms “reducing”, “suppressing” and “inhibiting” have their commonly understood meaning of lessening or decreasing.
[0150] In certain embodiments, the present invention encompasses administering the compounds useful in the present invention to a patient or subject. A “patient” or “subject”, used equivalently herein, refers to an animal. In particular, an animal refers to a mammal, preferably a human. The subject either: (1) has a condition remediable or treatable by administration of a compound of the invention; or (2) is susceptible to a condition that is preventable by administering a compound of this invention.
[0151] Unless defined otherwise, all technical and scientific terms used herein have the same meanings as commonly understood by one of ordinary skill in the art to which this invention belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are now described. All publications mentioned herein are incorporated herein by reference for the purpose of describing and disclosing the chemicals, cell lines, vectors, animals, instruments, statistical analysis and methodologies which are reported in the publications which might be used in connection with the invention. Nothing herein is to be construed as an admission that the invention is not entitled to antedate such disclosure by virtue of prior invention.
[0152] The invention includes compounds of formula I which exhibit activity as antagonist of quorum sensing in bacteria, particularly specific bacteria disclosed herein. The invention also includes compounds of formula I which exhibit activity as agonist of quorum sensing in bacteria, particularly specific bacteria disclosed herein.
[0153] In an embodiment, compounds of formula I have activity as an agonist or antagonist of native quorum sensing compounds. In an embodiment, compounds of formula I can be used to selectively adjust the virulence, biofilm production, or symbiotic behavior of a quorum sensing bacteria. In an embodiment, compounds of formula I can be administered to a subject to initiate an immune response towards a quorum sensing bacteria.
[0154] In an embodiment, certain compounds are preferred for selectively adjusting the virulence, biofilm production, or symbiotic behavior of a particular species or strain of a particular species of quorum sensing bacteria. In an embodiment, preselected mixtures of L- and D-isomers of compounds of the present invention can be used to selectively adjust the virulence, biofilm production, or symbiotic behavior of a particular species or strain of a particular species of quorum sensing bacteria.
[0155] In an embodiment, the compounds of the present invention are useful as a combinatorial library comprising a preselected mixture of two or more compounds of the present invention. In an embodiment, the two or more compounds can each be used to separately selectively adjust the virulence, biofilm production, or symbiotic behavior of a particular species or strain of a particular species of quorum sensing bacteria.
[0156] When a group of substituents is disclosed herein, it is understood that all individual members of those groups and all subgroups, including any isomers and enantiomers of the group members, and classes of compounds that can be formed using the substituents are disclosed separately. When a Markush group or other grouping is used herein, all individual members of the group and all combinations and subcombinations possible of the group are intended to be individually included in the disclosure. When a compound is described herein such that a particular isomer or enantiomer of the compound is not specified, for example, in a formula or in a chemical name, that description is intended to include each isomer and enantiomer of the compound described individually or in any combination. When an atom is described herein, including in a composition, any isotope of such atom is intended to be included. Specific names of compounds are intended to be exemplary, as it is known that one of ordinary skill in the art can name the same compounds differently. Every formulation or combination of components described or exemplified herein can be used to practice the invention, unless otherwise stated. Whenever a range is given in the specification, for example, a temperature range, a time range, or a composition range, all intermediate ranges and subranges, as well as all individual values included in the ranges given are intended to be included in the disclosure.
[0157] All patents and publications mentioned in the specification are indicative of the levels of skill of those skilled in the art to which the invention pertains. References cited herein are incorporated by reference herein in their entirety to indicate the state of the art, in some cases as of their filing date, and it is intended that this information can be employed herein, if needed, to exclude (for example, to disclaim) specific embodiments that are in the prior art. For example, when a compound is claimed, it should be understood that compounds known in the prior art, including certain compounds disclosed in the references disclosed herein (particularly in referenced patent documents), are not intended to be included in the claim.
[0158] The invention has been described with reference to various specific and preferred embodiments and techniques. However, it should be understood that many variations and modifications may be made while remaining within the spirit and scope of the invention. It will be apparent to one of ordinary skill in the art that methods, devices, device elements, materials, procedures and techniques other than those specifically described herein can be applied to the practice of the invention as broadly disclosed herein without resort to undue experimentation. All art-known functional equivalents of methods, devices, device elements, materials, procedures and techniques described herein are intended to be encompassed by this invention. Whenever a range is disclosed, all subranges and individual values are intended to be encompassed. This invention is not to be limited by the embodiments disclosed, including any shown in the drawings or exemplified in the specification, which are given by way of example or illustration and not of limitation.
[0159] 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, but it is recognized that various modifications are possible within the scope of the invention claimed. Thus, it should be understood that although the present invention has been specifically disclosed by preferred embodiments, exemplary embodiments and optional features, modification and variation of the concepts herein disclosed may be resorted to by those skilled in the art, and that such modifications and variations are considered to be within the scope of this invention as defined by the appended claims. The specific embodiments provided herein are examples of useful embodiments of the present invention and it will be apparent to one skilled in the art that the present invention may be carried out using a large number of variations of the devices, device components, methods steps set forth in the present description. As will be obvious to one of skill in the art, methods and devices useful for the present methods can include a large number of optional composition and processing elements and steps.
[0160] Many of the molecules disclosed herein contain one or more ionizable groups [groups from which a proton can be removed (e.g., —COOH) or added (e.g., amines) or which can be quaternized (e.g., amines)]. All possible ionic forms of such molecules and salts thereof are intended to be included individually in the disclosure herein. With regard to salts of the compounds herein, one of ordinary skill in the art can select from among a wide variety of available counterions those that are appropriate for preparation of salts of this invention for a given application. In specific applications, the selection of a given anion or cation for preparation of a salt may result in increased or decreased solubility of that salt.
[0161] Every formulation or combination of components described or exemplified herein can be used to practice the invention, unless otherwise stated.
[0162] Whenever a range is given in the specification, for example, a temperature range, a time range, or a composition or concentration range, all intermediate ranges and subranges, as well as all individual values included in the ranges given are intended to be included in the disclosure. It will be understood that any subranges or individual values in a range or subrange that are included in the description herein can be excluded from the claims herein.
[0163] All patents and publications mentioned in the specification are indicative of the levels of skill of those skilled in the art to which the invention pertains. References cited herein are incorporated by reference herein in their entirety to indicate the state of the art as of their publication or filing date and it is intended that this information can be employed herein, if needed, to exclude specific embodiments that are in the prior art. For example, when composition of matter are claimed, it should be understood that compounds known and available in the art prior to Applicant's invention, including compounds for which an enabling disclosure is provided in the references cited herein, are not intended to be included in the composition of matter claims herein.
[0164] As used herein, “comprising” is synonymous with “including,” “containing,” or “characterized by,” and is inclusive or open-ended and does not exclude additional, unrecited elements or method steps. As used herein, “consisting of excludes any element, step, or ingredient not specified in the claim element. As used herein, “consisting essentially of does not exclude materials or steps that do not materially affect the basic and novel characteristics of the claim. In each instance herein any of the terms “comprising”, “consisting essentially of and “consisting of may be replaced with either of the other terms. The invention illustratively described herein suitably may be practiced in the absence of any element or elements, limitation or limitations which is not specifically disclosed herein.
[0165] One of ordinary skill in the art will appreciate that starting materials, biological materials, reagents, synthetic methods, purification methods, analytical methods, assay methods, and biological methods other than those specifically exemplified can be employed in the practice of the invention without resort to undue experimentation. All art-known functional equivalents, of any such materials and methods are intended to be included in this invention. The terms and expressions which have been employed are used as terms of description and not of limitation, and there is no intention that in the use of such terms and expressions of excluding any equivalents of the features shown and described or portions thereof, but it is recognized that various modifications are possible within the scope of the invention claimed. Thus, it should be understood that although the present invention has been specifically disclosed by preferred embodiments and optional features, modification and variation of the concepts herein disclosed may be resorted to by those skilled in the art, and that such modifications and variations are considered to be within the scope of this invention as defined by the appended claims.
[0166] The invention is further illustrated by the following non-limiting examples.
The Examples
Example 1
[0167] Heterocycles and carbocycles were chosen as head groups for a library ( FIG. 4 ) in order to probe the orientation and electronics necessary for a positive binding interaction with Trp60, shown to be an important residue in the N-terminal domain of the LasR crystal structure. Fluorine was chosen as a lactone carbonyl mimic due to its ability to accept hydrogen bonds. Multiple fluorine aromatic substitutions were examined to determine if Trp60 could hydrogen bond to multiple atoms given the correct spatial orientation. Non-hydrogen bonding oxygen-containing moieties were chosen to examine the effects of non-hydrogen bonding electrostatic interactions. The library also contained carbocycles to explore the necessity of the Trp60 binding interaction. A thiolactone analog shown to be active in previous experiments was chosen to serve as a control compound for our bacterial strains. [Passador, L.; Tucker, K. D.; Guertin, K. R.; Journet, M. P.; Kende, A. S.; Iglewski, B. H., Functional analysis of the Pseudomonas aeruginosa Autoinducer PAI. J. Bacteriol. 1996, 178, 5995-6000.] The glycine ethyl ester and the alanine methyl ester were chosen to explore the effects of variations on synthetic ring-opened forms of the lactone unavailable to nature.
[0168] Based upon this design strategy, a 17 member non-lactone based library ( FIG. 4 ) was synthesized using solution-phase chemistry. To facilitate the ease of synthesis, a Meldrum's Acid derivative was used as a common intermediate. Reacting Meldrum's Acid with decanoyl chloride afforded the Meldrum's Acid derivative, which was refluxed with the desired amines to form the initial library (Scheme 1).
[0169] Scheme 1 is a general synthetic method for producing 3-oxo-dodecanoyal derivatives of the natural autoinducer for P. aeruginosa. DMAP=dimethyl amino pyridine. TEA=triethyl amine. R can, for example, be a unsubstituted or substituted heterocycle or carbocycle:
[0000]
[0000] This method can be employed for synthesis of various compounds herein by choice of starting materials and routine adaptation of methods disclosed herein or of methods that are well-known in the art. This method can be used for synthesis of compounds, where R is various substituted and unsubstituted heterocyclic rings, in particular, where R is a ring substituted thiolactone group. Appropriate starting materials for making ring-substituted compounds of this inventions are readily available either form commercial sources or by known synthetic methods. Additional references which provide details useful in the synthesis of thiolactones of this invention include among others U.S. Pat. Nos. 3,840,534 and 3,926,965 and Krasncv et al. (1999) Russian J. Org. Chem. 35(4):572-577.
[0170] The initial library was tested for LasR agonistic and antagonistic activity in two strains: Escherichia coli DH5α (pJN105L+pSC11) [Lee, J. H.; Lequette, Y.; Greenberg, E. P., Activity of purified QscR, a Pseudomonas aeruginosa orphan quorum-sensing transcription factor. Mol. Microbiol. 2006, 59 (2), 602-609] and P. aeruginosa PA01 MW1 (pUM15) [Muh, U.; Schuster, M.; Heim, R.; Singh, A.; Olson, E.; Greenberg, E. P., Novel Pseudomonas aeruginosa Quorum-Sensing Inhibitors Identified in an Ultra-High-Throughput Screen. Antimicrob. Agents Chemother. 2006, 50, 3674-3679] ( FIGS. 5A and 5B). Both strains allow for synthetic autoinducer mimic evaluation and contain a reporter gene that allows for a quantitative readout of QS activity. DH5α (pJN105L+pSC11) is a heterologous β-galactosidase E. coli reporter strain containing a plasmid for the P. aeruginosa LasR gene. The PA01 MW1 (pUM15) strain uses the natural P. aeruginosa background containing a Lasl deletion and the gene for yellow fluorescent protein (YFP) under the control of the Lasl promoter to evaluate the LasI/R activity. Since the PA01 MW1 (pUM15) strain evaluates LasR in the natural P. aeruginosa background, in contrast to the heterologous E. coli strain, an improved idea of the interplay between the isolated LasI/R system and the combination of LasI/R with other QS subsystems such as QscR can be determined. Furthermore, additional nuances of the natural system such as compound permeability are incorporated in assays using the PA01 MW1 (pUM15) strain.
[0171] The initial library was also tested in Vibrio fischeri ESI 114 (Δ-Luxl) [Lupp, C.; Urbanowski, M.; Greenberg, E. P.; Ruby, E. G., The Vibrio fischeri quorum-sensing systems ain and lux sequentially induce luminescence gene expression and are important for persistence in the squid host. Mol. Microbiol. 2003, 50 (1), 319-331] and Agrobacterium tumefaciens WCF (pCF372). [Zhu, J.; Beaber, J. W.; More, M. I.; Fuqua, C.; Eberhard, A.; Winans, S. C., Analogs of the autoinducer 3-oxooctanoyl-homoserine lactone strongly inhibit activity of the TraR protein of Agrobacterium tumefaciens. J. Bacteriol. 1998, 180 (20), 5398-5405.] However, activities were low to modest in these species, except for compound 1, which is a good antagonist in both strains. The general lack of activity in the V. fischeri and A. tumefaciens strains is to be expected considering that the library was designed for the P. aeruginosa LasR protein and reinforces previous work demonstrating that the length of the acyl tail is highly species dependent. [Geske, G. D.; O'Neill, J. C.; Miller, D. M.; Mattmann, M. E.; Blackwell, H. E., Modulation of Bacterial Quorum Sensing: Systematic Evaluation of N-Acylated Homoserine Lactones in Multiple Species and New Insights into Their Mechanism of Action. J. Am. Chem. Soc. 2007, 129, 13613-13625.]
[0172] This set of screening data provides several noteworthy discoveries. First, the thiolactone derivative of the P. aeruginosa natural ligand (1) is highly active in all strains tested—either as an agonist in the strains examining LasR activity [94% agonist in DH5α (pJN105L+pSC11) and 88% agonist in PA01 MW1 (pUM15)] or as an antagonist in the V. fischeri (LuxR; 92% inhibition) and A. tumefaciens (TraR; 65% inhibition) strains. The high degree of activity across these four strains suggests that the sulfur substitution in the lactone ring does not sufficiently alter the binding of 1 from the natural ligand and suggests that the electronics at that position are not critical for binding. Second, the cyclopentyl amine derivative (3) is an agonist in both strains testing for LasR activity and a modest antagonist in the V. fischeri strain. This is remarkable because the cyclopentyl amine head group lacks functionality for hydrogen bond acceptance, which has been proposed as critical for neutral ligand binding based on the LasR crystal structure. This suggests that either the lactone carbonyl's hydrogen bonds are not as crucial as originally thought, or that 3 binds in an alternative manner. Third, compound 2 is of interest for its antagonism capabilities in both strains evaluating the LasI/R system, even though there are no hydrogen bond acceptor substitutions, further questioning the proposed critical nature of the lactone carbonyl. Fourth, compound 14 provides some insight into the differences between the isolated LasI/R system in E. coli and the LasI/R system in the natural P. aeruginosa background. LasR appears to be strongly agonized by 14 in the E. coli strain, while assays using the natural P. aeruginosa background show slight antagonism rather than an agonistic effect. Compound 14 represented an excellent candidate for further testing in additional heterologous strains containing isolated QS subsystems like QscR and RhII/R.
[0173] Additional comparative data for several compounds of FIG. 4 is provided in Table 1
[0000]
TABLE 1
E. coli
DH5α
(pJN105L +
P. aeruginosa
V. fischeri
A. Tumefaciens
pSC11)
PA01 MW1
ESI 114 (Δ-Luxl)
WCF (pCF372)
Compd
Antagonist
Agonist
Antagonist
Agonist
Antagonist
Agonist
Antagonist
Agonist
2
53.7
—
28.7
—
—
—
—
—
3
—
83.5
—
54.2
89.4
—
—
—
7
38.8
—
—
—
—
3.1
—
—
10
—
—
25.5
—
—
3.3
—
—
12
—
—
−6.6
4.0
34.9
3.0
−22.0
—
13
41.0
—
16.8
—
43.8
1.7
—
—
14
−67.7
73.0
37.8
—
14.6
—
—
—
Agonist results are reported as a percent of activation compared to the positive control.
Antagonist results are reported as a percent inhibition compared to a positive control.
Negative values indicate agonist properties detected in an antagonist assay.
Example 2
Focused Libraries-Racemic Thiolactone Library
[0174] Based upon the results of the initial library screen, focused libraries around the most active leads (1, 2, 3, 16 from FIG. 4 ) were developed. In these libraries, the identified head group remained identical while the 3-oxo-C12 acyl tail was replaced with mimics previously shown to be active in AHL libraries. [Geske, G. D.; O'Neill, J. C.; Miller, D. M.; Mattmann, M. E.; Blackwell, H. E., Modulation of Bacterial Quorum Sensing: Systematic Evaluation of N-Acylated Homoserine Lactones in Multiple Species and New Insights into Their Mechanism of Action. J. Am. Chem. Soc. 2007, 129, 13613-13625.]
[0175] The first focused library ( FIG. 6 ) was a racemic homoserine thiolactone library, synthesized from 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDC) couplings between homoserine thiolactone and the appropriate carboxylic acid (Scheme 2).
[0000]
[0176] Scheme 2 provides EDC coupling synthesis to make the racemic thiolactone library illustrated in FIG. 6 .
[0177] This method can be employed for synthesis of various compounds herein by choice of starting materials and routine adaptation of methods disclosed herein or of methods that are well-known in the art. This method can be used for synthesis of compounds, where R is various substituted and unsubstituted heterocyclic rings, in particular, where R is a ring substituted thiolactone group. Appropriate starting materials for making ring-substituted compounds of this inventions are readily available either form commercial sources or by known synthetic methods. Additional references which provide details useful in the synthesis of thiolactones of this invention include among others U.S. Pat. Nos. 3,840,534 and 3,926,965 and Krasncv et al. (1999) Russian J. Org. Chem. 35(4):572-577.
[0178] The racemic thiolactone library was tested in the same LasR reporter strains as the initial library ( FIGS. 7A and 7B ). Differences between the isolated LasR reporter system and LasR reporter system in the natural P. aeruginosa background have been uncovered in this second generation library. All of the library members were active in the heterologous LasI/R system while inactive in the intact P. aeruginosa QS system. One possibility is that library members are regulating multiple competing QS pathways, resulting in net inactivity in the natural background. For this reason it is crucial to examine the LasI/R system in the natural P. aeruginosa background where additional QS subsystems are also present and not simply as an isolated system in the E. coli background. Differences in cell permeability, especially since P. aeruginosa is known to be less permeable than E. coli, could also account for the discrepancy in activity between the two strains.
Example 3
Focused Libraries-Enantiopure Thiolactone Library
[0179] After finding several active compounds in the racemic thiolactone library in the heterologous E. coli LasI/R strain and the V. Fischeri strain, a third generation library was designed containing the enantiopure thiolactone along with additional acyl chain mimics to further explore the structure-activity relationship of the thiolactone head group ( FIG. 8 ). The L enantiomer of the thiolactone was chosen based on previous studies that found the L enantiomer of P. aeruginosa 's natural autoinducer to be active and the D enantiomer to be inactive. [Geske, G. D.; O'Neill, J. C.; Miller, D. M.; Mattmann, M. E.; Blackwell, H. E., Modulation of Bacterial Quorum Sensing: Systematic Evaluation of N-Acylated Homoserine Lactones in Multiple Species and New Insights into Their Mechanism of Action. J. Am. Chem. Soc. 2007, 129, 13613-13625; Glansdorp, F. G.; Thomas, G. L.; Lee, J. K.; Dutton, J. M.; Salmond, G. P. C.; Welch, M.; Spring, D. R., Synthesis and stability of small molecule probes for Pseudomonas aeruginosa quorum sensing modulation. Org. Biomol. Chem. 2004, 2, 3329-3336.]
[0180] FIG. 8 provides structures (with reference numbers) of compounds of the enantiopure thiolactone library synthesized from a combination of Meldrum's acid precursors and EDC couplings.
[0181] The third generation thiolactone compounds were similarly tested in bacterial assays beside the racemic version, if synthesized, to determine the effect of stereochemistry on activity ( FIGS. 9A-9H ). FIGS. 9A-9H provide a comparison between racemic and enantiopure thiolactone analogs. All synthetic ligands were tested at 10 μM using standard methods described in FIGS. 5A and 5B . Compounds 24-30 of the enantiopure library were not compared to a racemic counterpart. If stereochemistry played a large role in binding, the enantiopure compounds were expected to have approximately twice the activity of the racemic compounds when screened at 10 μM total synthetic ligand in each case. In both strains testing for LasR activity, it appeared, however, that stereochemistry was not important for activity of the non-native thiolactones in contrast to the lactones. Without wishing to be bound by any particular theory, we presently believe that binding is likely less specific for the thiolactones compared to the natural lactone ligand, where it is known that the L enantiomer is far more active than the D enantiomer.
[0182] Dose response analysis for the active enantiopure thiolactone compounds was conducted to quantify the activity of the synthetic ligands (Table 2). The activity of the thiolactone head group alone became evident through compound 21E in the heterologous LasR strain, whose AHL analogue was found to have little activity. [Geske, G. D.; O'Neill, J. C.; Miller, D. M.; Mattmann, M. E.; Blackwell, H. E., Modulation of Bacterial Quorum Sensing: Systematic Evaluation of N-Acylated Homoserine Lactones in Multiple Species and New Insights into Their Mechanism of Action. J. Am. Chem. Soc. 2007, 129, 13613-13625.] Based on the results of the enantiopure thiolactone dose response data, it appears that relatively long or electron withdrawing side chains are excellent antagonists of LasR isolated in the E. coli background. However, natural ligand mimics 1E and 25E are strong agonists for the heterologous LasR system. All of the active compounds in PA01 MW1 (PUM15) ( P. aeruginosa natural background) were also active in E. coli DH5α (pJN105L+pSC11). However, a significant number of the compounds active in the E. coli DH5α (pJN105L+pSC11) strain were not active in the P. aeruginosa PA01 MW1 (PUM15) strain. These findings corroborate our hypothesis that when LasR is evaluated in the natural P. aeruginosa background a muted effect is may be seen due to the effects of the other QS systems present in intact P. aeruginosa, such as QscR and the PQS system. A variety of other effects could be contributing to the differences seen between the two strains, including differences in cell permeability.
[0000]
TABLE 2
Table 2. The IC 50 and EC 50 values for the most active enantiopure
thiolactone library members.
DH5α
(pJN105L +
PA01 MW1
ESI 114 (Δ-
pSC11)
(pUM15)
Luxl)
WCF (pCF372
E. Coli
P. aeruginosa
V. fischeri
A. tumefaciens
IC 50
EC 50
IC 50
EC 50
IC 50
EC 50
IC 50
EC 50
Comp. #
(μM)
(μM)
(μM)
(μM)
(μM)
(μM)
(μM)
(μM)
1E
0.092
3.2
0.45
1.8
18E
0.40
0.77
19E
4.1
11
20E
7.2
21E
2.5
22E
1.8
23E
2.9
0.35
24E
0.35
20
25E
1.9
21
26E
0.14
0.13
2.8
27E
0.79
0.31
10
28E
1.1
0.84
30E
0.13
13
3.2
[0183] Activity differences between the two strains evaluating LasR raise questions about the integrity and degradation of the ligands since the incubation time in the assay for the heterologous strain is shorter than for the native P. aeruginosa strain. It is well known that the homoserine lactone ring, used by all of the bacterial species of interest as their autoinducer head group, is prone to hydrolysis at pH 7 and above. [Eberhard, A.; Widrig, C. A.; MaBath, P.; Schineller, J. B., Analogs of the autoinducer of bioluminescence in Vibrio fischeri. Arch. Microbiol. 1986, 146, 35-40; Schaefer, A. L.; Hanzelka, B. L.; Eberhard, A.; Greenberg, E. P., Quorum sensing in Vibrio fischeri: Probing autoinducer-LuxR interactions with autoinducer analogs. J. Bacteriol. 1996, 178, 2897-2901; Byers, J. T.; C., L.; Salmond, G. P. C.; Welch, M., Nonenzymatic turnover of an Erwinia carotovora quorum sensing signaling molecule. J. Bacteriol. 2002, 184, 1163-1171.] Previous literature has indicated that the P. aeruginosa natural autoinducer has a half-life of approximately two days in growth media at 37° C., while shorter chain AHLs degrade in even shorter periods of time. [Glansdorp, F. G.; Thomas, G. L.; Lee, J. K.; Dutton, J. M.; Salmond, G. P. C.; Welch, M.; Spring, D. R., Synthesis and stability of small molecule probes for Pseudomonas aeruginosa quorum sensing modulation. Org. Biomol. Chem. 2004, 2, 3329-3336; Yates, E. A.; Philipp, B.; Buckley, C.; Atkinson, S.; Chhabra, S. R.; Sockett, R. E.; Goldner, M.; Dessaux, Y.; Camara, M.; Smith, H.; Williams, P., N-Acylhomoserine lactones undergo lactonolysis in a pH-, temperature-, and acyl chain length dependent manner during growth of Yersinia pseudotuberculosis and Pseudomonas aeruginosa. Infect. Immun. 2002, 70, 5635-5646]
[0184] Finding QS antagonists and agonists that are more hydrolytically stable are of considerable interest, since molecules that hydrolyze rapidly are not ideal therapeutic agents or biological probes. While many of the compounds synthesized in the initial library are non-hydrolyzable, the thiolactone derivative of the natural ligand (1E) is hydrolyzable. However, the differences in activities between the thiolactone derivatives and the natural lactone derivatives make the thiolactone derivatives both worthwhile to pursue as a target and for further half-life experiments.
[0185] Table 3 provides a summary of data for the antagonism assay for compounds tested having thiolactone head groups against selected bacteria. Compounds exhibiting 50% or higher inhibition in assays with Escherichia coli and Agrobacterium tumefaciens and those exhibiting 20% or higher inhibition with Vibrio fischeri are preferred for applications for disrupting bacterial quorum sensing, particularly in Escherichia coli, Agrobacterium tumefaciens and Vibrio fischeri strains, and for inhibiting and/or disrupting biofilm formation, particularly in Escherichia coli, Agrobacterium tumefaciens and Vibrio fischeri strains.
[0000]
TABLE 3
Antagonism Assay Data Thiolactone Libraries
E. coli
V. fischeri
A. tumefaciens
Comp #
Inhib %
Comp #
Inhib %
Comp #
Inhib %
18
80
1
99
26E
99
27E
78
24E
99
30E
93
18E
68
23
98
1
92
21
65
18
97
27E
78
26E
64
28E
93
1E
51
21E
61
1E
91
19
33
28E
59
18E
91
19E
30
23
56
23E
85
23E
26
22E
54
26E
80
18E
25
20
51
27E
78
21E
13
20E
48
22E
75
23
9
23E
45
20
70
25E
6
29E
17
22
68
21
−22
22
16
30E
62
20E
−24
19E
−3
20E
59
22E
−26
19
−13
25E
57
18
−60
24E
−30
29E
42
29E
−70
1
−40
21
34
28E
−78
1E
−61
19E
30
22
−80
25E
−93
21E
30
24E
−89
30E
−119
19
19
20
−107
[0186] Table 4 provides a summary of data for the agonism assay for compounds tested having thiolactone head groups with certain bacteria. Compounds exhibiting 50% or higher inhibition in assays with Escherichia coli and P. aeruginosa are preferred for applications for activating bacterial quorum sensing, particularly in Escherichia coli, and P. aeruginosa strains and for activating biofilm formation therein.
[0000]
TABLE 4
Agonism Assay Data for Thiolactones
E. coli
P. aeruginosa
Comp #
Act %
Comp#
Act %
1E
102
1E
127
1
94
1
88
26E
85
30E
76
19
82
25E
42
19E
81
29E
22
22E
72
28E
20
23
9
21E
17
18E
8
22
10
27E
8
18
8
30E
6
20
7
22
4
18E
5
25E
4
19
5
29E
4
20E
4
21E
3
19E
3
18
2
22E
3
21
2
23
3
20
1
24E
3
28E
1
21
2
20E
0
23E
1
23E
0
26E
0
24E
0
27E
0
Example 4
Comparison of Functional Half-Lives of Autoinducers
[0187] A biologically based assay was developed to determine the functional half-life of the P. aeruginosa natural ligand, OdDHL, and the corresponding thiolactone analog (1E). This assay does not directly measure hydrolysis, but rather the ability of the degraded ligand to cause a QS response. However, previous experiments have shown that the hydrolysis half-life for the P. aeruginosa natural ligand, OdDHL, is approximately two days, while racemization of the chiral center was found to be less than 5% over the course of a week. [Glansdorp, F. G.; Thomas, G. L.; Lee, J. K.; Dutton, J. M.; Salmond, G. P. C.; Welch, M.; Spring, D. R., Synthesis and stability of small molecule probes for Pseudomonas aeruginosa quorum sensing modulation. Org. Biomol. Chem. 2004, 2, 3329-3336.] This data suggests that most ligand degradation is due to hydrolysis and not epimerization. In these cases the results were determined by NMR experiments conducted in deuterated buffers. Due to problems with the water solubility of OdDHL, a 50% solution of DMSO was used. Unfortunately, the use of high levels of DMSO reduces the biological relevance of the assay because large concentrations of DMSO cannot be tolerated by biological systems. Furthermore, the required concentrations of ligand are lower in a biologically based functional assay than in an NMR experiment because YFP production is much more sensitive than NMR, which requires relatively high concentrations.
[0188] In this assay, media, ligand, and antibiotics are prepared in Teflon-capped vials and allowed to incubate at 37° C. for predetermined times. P. aeruginosa cells from the strain PA01 MW1 (pUM15) were cultured overnight. These cells were then pelleted and washed with LB containing 50 mM MOPS. After washing, the cells were resuspended in a minimal amount of media containing antibiotics and were added to a 96 well plate containing the media, natural ligand, and antibiotic previously prepared and incubated for specific, predetermined times. At this point, the optical density at 600 nm of the cells was comparable to the optical density after subculturing the cells during a traditional assay. The 96 well plate was incubated for 8 hours and then analyzed for optical density and YFP fluorescence. Bacteria were cultured, pelleted, and washed before addition to the assay plate. A traditional PA01 MW1 assay is completed to analyze for ligand degradation. Fluorescence was normalized to cell density and time points were analyzed as a percentage of the ability of the freshly prepared natural ligand to agonize the P. aeruginosa system. Since we predict that the ligand degradation is a product of hydrolysis, we assumed a pseudo first order rate and plotted the natural log of the agonism as a percent of the fresh natural ligand versus time. The slope of the graph can be used to determine the half-life of the ligand according to the formula t½=ln(2)/slope ( FIGS. 10A and 10B ).
[0189] We found the half-life for the OdDHL natural ligand to be 48.2 hours. This value corresponds closely with the previously found hydrolysis half-life of approximately two days. [Glansdorp, F. G.; Thomas, G. L.; Lee, J. K.; Dutton, J. M.; Salmond, G. P. C.; Welch, M.; Spring, D. R., Synthesis and stability of small molecule probes for Pseudomonas aeruginosa quorum sensing modulation. Org. Biomol. Chem. 2004, 2, 3329-3336.]
[0190] A similar analysis found the half-life of the thiolactone analog of the OdDHL P. aeruginosa natural ligand (1E) to be 82.3 hours. In the case of both the natural ligand and the thiolactone analog, the half-life of the compounds are sufficiently long so that standard in vitro assays on the time scale of 8 hours or less are testing the ligand in its native form. This is important because previous work has shown that the ring open form of the natural ligand is inactive. [Yates, E. A.; Philipp, B.; Buckley, C.; Atkinson, S.; Chhabra, S. R.; Sockett, R. E.; Goldner, M.; Dessaux, Y.; Camara, M.; Smith, H.; Williams, P., N-Acylhomoserine lactones undergo lactonolysis in a pH-, temperature-, and acyl chain length dependent manner during growth of Yersinia pseudotuberculosis and Pseudomonas aeruginosa. Infect. Immun. 2002, 70, 5635-5646; Kapadnis, P. B.; Hall, E.; Ramstedt, M.; Galloway, W. R. J. D.; Welch, M.; Spring, D. R., Towards quorum-quenching catalytic antibodies. Chem. Commun. 2009, (5), 538-540.]
[0191] It is interesting to note that the half-life of 1E is slightly less than double the half-life of OdDHL, the natural ligand. This is particularly intriguing because one would expect the sulfur analog to have a faster hydrolysis rate from an electronics argument. Our current hypothesis is that although compound 1E is able to ring open faster than OdDHL, 1E is also able to recyclize at a faster rate than the natural ligand. Previous analysis of lactone hydrolysis has shown that once ring opened, the lactone does not reclose in appreciable quantities until under pH 2 due to differences in the mechanisms for ring opening and closing. [Yates, E. A.; Philipp, B.; Buckley, C.; Atkinson, S.; Chhabra, S. R.; Sockett, R. E.; Goldner, M.; Dessaux, Y.; Camara, M.; Smith, H.; Williams, P., N-Acylhomoserine lactones undergo lactonolysis in a pH-, temperature-, and acyl chain length dependent manner during growth of Yersinia pseudotuberculosis and Pseudomonas aeruginosa. Infect. Immun. 2002, 70, 5635-5646.} In order for the lactone ring to close, the pH must first approach the pKa of the carboxyl group so that significant amounts of the acid as opposed to the acid salt are present. The differences in ring opening and closing mechanisms may cause the natural ligand to take longer to ring open, but remain ring opened, while the sulfur analog would ring open faster and close back up again so that it would have a longer hydrolysis half-life than the natural ligand. Conversely, the sulfur's increased nucleophilicity may be able to hold the lactone ring together in aqueous solution better than the corresponding oxygen.
Example 5
Focused Libraries-Non-Hydrolyzable Head Groups
[0192] While many of the natural ligands for QS systems contain a lactone ring, it would be advantageous to find QS modulators that are not prone to hydrolysis or degradation. To this end focused libraries based on non-hydrolyzable head groups screened in the initial library were designed, synthesized, and screened. Head groups based upon glycine ethyl ester (16), cyclopentyl amine (3), and aniline (2) were chosen as particularly interesting non-hydrolyzable head groups based on activity in the initial library screens.
[0193] The glycine ethyl ester head group is particularly interesting because the stereochemistry has been removed from the head group. The glycine ethyl ester head group is derived from the lactone ring when a disconnection is made between the carbons 2 and 3 in the lactone ring. (Scheme 3).
[0000]
[0194] While the compounds of this library ( FIG. 11 ) are non-natural analogs of the lactone ring, it is interesting that some activity can be observed. One characteristic of this library is that the compounds appear to be cooperative agonists because many of the library members show heightened activity in antagonistic assays and minimal activity in agonistic assays (FIGS 12 A and 12 B). Compound 34 showed excellent antagonistic activity in V. fischeri. While most library members do not seem to fit as traditional agonists or antagonists, further analysis could yield important information about alternative binding sites or methods, or information about dimerization requirements.
[0195] Cyclopentyl amine and aniline were used to synthesize libraries to explore the activity of ligands with a lack of hydrogen bonding capabilities on the head group ( FIG. 13 (cyclopentyl amine library HG=cyclopentyl), FIG. 14 (analine library, H=phenyl)). Agonism and antagonism assays, performed as described above, are illustrated in FIGS. 15A and 15B , respectively. While these carbocycles were active when appended with the 3-oxo dodecanoyal containing acyl chain, only moderate activities were observed when paired with acyl tail mimics. These studies show that viable agonists and antagonists can be found either by altering the head group of the natural ligand or by creating acyl tail mimics. However, when both the head group and the acyl tail are modified in the same molecule, the molecule doesn't always combine the activities of the two initial modifications. In fact, the dual modifications are frequently deleterious to the activity of the molecule.
[0196] Pursuing QS modulators that are either non-hydrolyzable or hydrolyze slowly allows for new biological probes or therapeutics. It is important for therapeutics to remain biologically active for extended periods of time yet be cleared from the body in a time dependent manner. Compounds like the thiolactone derivatives of this invention may serve as excellent therapeutics because they are active for longer periods of time than the natural lactone analogs, yet do lose activity in a time dependent fashion.
|
Compounds which modulate quorum sensing in quorum sensing bacteria. Compounds of the invention inhibit quorum sensing and/or activate quorum sensing in various bacteria. Compounds that inhibit quorum sensing are particularly useful for inhibition of detrimental bacterial biofilm formation. Compounds that activate quorum sensing are particularly useful for promoting growth and biofilm formation of beneficial bacterial.
| 2
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TECHNICAL FIELD
The present invention generally relates to vehicle brake systems and more particularly relates to a method of operating a brake assistant system.
BACKGROUND OF THE INVENTION
In order to realize a shortest possible stopping distance of automobiles in emergency brake situations, it is necessary to excessively raise the brake pressure with respect to a pedal force initiated by the driver. Since studies have yielded the result that, in emergency brake situations, normal drivers often cannot or only with a delay induce the required pre-pressure, so-called “brake assistant systems” were developed which raise the brake pressure automatically above the level pre-determined by the driver.
In principle, there are three known systems. In a first one, the brake pressure is raised by means of an automatic control of the brake booster. In the second one, the active pressure raise occurs through suitable control of the ABS/ESP hydraulics by means of the electric return pump. Further, there are other known brake assistant systems which all will be further developed. Just for example, it is referred to mechanical or electrical/mechanical brake assistants.
A method to shorten the stopping distance in critical driving situations has been disclosed in the German Patent DE 40 28 290 C1. In the method disclosed in this document, the excess of a first threshold value by the actuation speed of the brake pedal initiated by the driver is the criterion for the release of an automatic brake event, where, immediately after the release of the automatic brake event, such a brake pressure is automatically built up which corresponds to the value of the brake pressure at optimum vehicle deceleration. In order to ensure that the excessively raised brake pressure is reduced when the necessity of an automatic brake event is eliminated, it is verified, according to the teaching of this document, whether the actuation force of the brake pedal is smaller than a pre-set threshold value, i.e. whether the vehicle driver wants to reduce the power of the brake event and thus only a brake event with a lower brake force is necessary.
A mode of operation is provided which provides for the transition from a full pressure build-up of the actual brake assistant to a conventional brake behavior in order to avoid an abrupt termination of the support provided by the brake assistant which, immediately upon termination of the brake assistant, could have the result that a relatively low tandem master cylinder pressure coincides with a relatively high locking pressure.
Therefore, the objective of the present invention consists in avoiding the disadvantages of the prior art and in indicating a method of operating a brake assistant which avoids an abrupt termination of the brake support and which, at the same time, is particularly safe and user-friendly.
This objective is achieved in a method of the kind mentioned above by means of the present invention. Here, excess elevation is not understood as being the, regarding its absolute value, higher wheel cylinder pressure raised by the brake assistant with respect to the tandem master cylinder pressure, but it is rather the relative amount of this excess elevation with respect to the pressure in the tandem master cylinder.
A special advantage of the invention consists in that a once-initiated transition to conventional braking behavior is not being maintained for a longer time period. Otherwise, this would, e.g. while going downhill, result in an undesired and unsafe state of operation.
Preferably, the excess elevation is dependent on the driving situation and/or the input of a vehicle driver my means of the brake pedal. Thus, the brake force support can be tuned to the driving conditions in the best possible way. Also, in this case, a harmonic correlation can be ensured between the driver's directive and the pressure raise.
Preferably, the rate at which the excess elevation is reduced increases with the time duration and/or the intensity of a reduction of pedal force induced by the vehicle driver. A reduction of pedal force indicates a driver's intention that a brake operation is not necessary or not necessary as forceful any more. The input control by the driver can be used in an advantageous way to design the transition of the brake assistant function to the conventional brake operation.
A particularly simple and cost-effective realization of the invention results from using a counting device to recognize whether and/or by what amount the driver reduces the pedal force.
In order to implement the invention, it is preferred if the momentary value of the wheel brake pressure results substantially from a multiplication of a current value of a time-dependent excess elevation function and the current value of the tandem master cylinder pressure.
And the excess elevation function, as a function of time, is monotonously descending.
Preferably, the excess elevation function descends in time segments in which the master cylinder pressure descends. Further, the excess elevation function is constant in time segments in which the tandem master cylinder pressure increases. Thus, every diminution of the induced brake force effects a reduction of the excess elevation, and every other input via the brake pedal affects the wheel brake pressure but not the excess elevation. In this way, the brake assistant support can be diminished unnoticeably for the driver.
According to a preferred enhancement of the invention, a momentary value of the excess elevation function depends on the previous course of the tandem master cylinder pressure. The consideration of the history of the tandem master cylinder pressure is particularly preferred for the estimate of the driving situation and of the driver's intention. Advantageously, the excess elevation function includes a pre-set maximum value. In this way, implausible excess elevations of the wheel brake pressure can be avoided.
The brake assistant system preferably changes over from the third mode of operation to the first mode of operation when the excess elevation function substantially occupies the value “1”. In this case, the driver himself affords the required locking pressure and does not need any further support.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a schematic depiction of the course of the time-dependent tandem master cylinder pressure p TMC (t).
FIG. 2 shows a schematic depiction of a time-dependent excess elevation function K(t) in order to illustrate an embodiment of the present invention.
FIG. 3 shows a schematic depiction of the three modes of operation of the brake assistant system according to the invention and of the transitions between the respective states.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIG. 3 , three kinds or modes of operation of the brake assistant system according to the invention are schematically depicted. From FIG. 3 can be obtained the function of the brake assistant system as an automaton of states. The first state or mode of operation “Passive” means that the brake assistant function is not active. As soon as an emergency braking situation is recognized, the system changes over into the second state or mode of operation “Total Pressure Build-up”. In this state, a total pressure build-up is generated by means of a return pump and suitable control of separating and switch-over valves. From the state “Total Pressure Build-up”, a change can be made as well into the state of passivity into the third mode of operation, the dosage mode if the pedal force is significant reduced which can be detected e.g. through the pressure sensor device arranged in the tandem master cylinder. Higher-ranking criteria for the activation of the state “Dosage” out of the state “Total Pressure Build-up” are the recognition of a driver's intention of a dosed diminution of the brake force. This is sensed in case of a significant diminution of the tandem master cylinder pressure p TMC after reaching the global locking-pressure level. A significant diminution of the tandem master cylinder pressure prior to reaching the global locking-pressure results in the direct transition from the state “Total Pressure Build-up” into the state “Dosage”. In the state “Dosage”, the brake force is modulated in dependence on the pedal force. After termination of the maximum actuation, the pressure build-up is gradually diminished or even increased again, in dependence on the driver's intention sensed by means of the measured tandem master cylinder pressure, in order to achieve in this way a comfortable transition between the maximum support during the emergency brake situation and the conventional brake behavior of the “Passive” mode after termination of the emergency brake support. This state resembles a brake-by-wire mode and can be called modulating.
In FIG. 1 , a possible pressure course p TMC (t) of the tandem master cylinder pressure, substantially after the state “Total Pressure Build-up”, is schematically depicted. The tandem master cylinder pressure p TMC (t) is, due to the actuation of the brake assistant function, significantly smaller than the wheel brake pressure (not depicted). The possible pressure course p TMC (t) schematically depicted in FIG. 1 is the result of an input by the driver by means of actuation of a brake pedal. In FIG. 1 can be seen that the tandem master cylinder pressure p TMC (t) is substantially constant between a point in time t 0 and t 1 . This means that p TMC ′(t)=0 in the interval from t 0 to t 1 . Between the point in time t 1 and a point in time t 2 , the tandem master cylinder pressure decreases continuously. At the point in time t 2 , the tandem master cylinder pressure p TMC (t) reaches a minimum value p TMC (t 2 ). Between the point in time t 2 and a point in time t 3 , the tandem master cylinder pressure p TMC (t) increases continuously. At the point in time t 3 , the master cylinder pressure has a maximum value p TMC t 3 . Between the point in time t 3 and a point in time t 4 , the master cylinder pressure decays continuously. At the point in time t 4 , the tandem master cylinder pressure p TMC (t) has a minimum value p TMC (t 4 ). In this example, the master cylinder pressure rises anew as of the point in time t 4 .
According to the present invention, the excess elevation of the brake force caused by the automatic brake assistant shall be successively diminished. A diminution according to a simple time-dependent function, however, yields the disadvantage that the behavior of the system goes beyond the driver's understanding. This is the case, for instance, when the brake effect fades despite keeping the pedal force constant. According to the invention, the vehicle deceleration or the wheel brake pressure p WHEEL (t), respectively, are controlled dependent on a measured tandem master cylinder pressure p TMC (t) during the dosage phase. A sample course of p TMC (t) was described above in connection with FIG. 1 . A possible functional correlation for controlling the wheel brake pressures p WHEEL (t) is: p WHEEL (t)=K(t)*p TMC (t). This functional correlation is just given as an example and serves in particular also to define the excess elevation function K(t) inasfar as estimated values or currently measured values, respectively, are used. It is noted that, in particular also in the above equation, an offset can be considered, i.e. in particular of the kind=K(t)*. If the value or x, for example, amounts to 6, the third mode of operation can be exited into the passive mode when the tandem master cylinder pressure falls below a minimum pressure of 6 bar. The course of the time-dependent excess elevation function K(t), which can also be called amplification factor, is, according to a variant of the present invention, schematically depicted in FIG. 2 . From FIG. 2 , it can be gathered that K(t) has a monotonously declining course. The value of K(t) ranges between a substantially maximum starting value for the dosage mode which is substantially determined according to the proportion between an estimated locking-pressure level and the current tandem master cylinder. In principle, a maximum value for K(t) is pre-set, e.g. 3.5, in order to avoid implausible wheel brake pressure excess elevations. During the entire dosage mode, the value of K(t) is greater than 1, for otherwise no further brake support is required and the system changes into the passive mode. In the embodiment shown, the course of K(t) is not strictly monotonous, for there are times when K′(t) equals 0. Substantially, the rule is that, in phases in which the tandem master cylinder pressure p TMC (t) is constant or rises, that means in phases in which p TMC ′(t) is greater than or equal to 0, K(t) is constant. Substantially in phases in which p TMC (t) declines, i.e. when p TMC ′(t) is smaller than 0, K(t) declines as well, i.e. K′(t)<0. In FIG. 2 can be seen that, in the interval from t 0 to t 1 , K(t) is substantially constant. In the interval from t 1 to t 2 , K(t) declines substantially monotonously to a value K(t 2 ). In the interval from t 2 to t 3 , K(t) is substantially constant. In the interval from t 3 to t 4 , K(t) declines substantially monotonously. As of the point in time t 4 , K(t) is constant for all t>t 4 . Therefore, the course of K(t) is substantially a sequence of declining plateaus corresponding to the oscillations of the tandem master cylinder pressure p TMC (t). The plateaus themselves are substantially characterized by phases of rising tandem master cylinder pressure p TMC (t). The plateaus, which, with time increasing, have declining values, are connected by monotonously declining line segments which substantially correspond to phases of declining tandem master cylinder pressure p TMC (t). It is noted that, according to the depicted and described embodiment of the invention, the brake assistant support is diminished practically undetectably by the driver. Advantageously, the rate at which the support of the hydraulic brake assistant is diminished, i.e. in particular the derivative K′(t), increases according to its absolute value the longer and the more distinctly the driver diminishes the pedal force. This means graphically, particularly in the embodiment, that, if the interval, e.g. between t 1 and t 2 increased, i.e. if the driver diminished the pedal force over a longer time interval, the inclination of K(t) would increase. Accordingly, the same is true if the diminution of pedal force, i.e., for instance, the value of p TMC (t 2 ) minus p TMC (t 3 ) increased.
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In a method of operating a brake assistant system which includes a first mode of operation in which the brake assistant system is not operated, a second mode of operation in which, after recognition of an emergency brake situation, a pressure build-up of wheel brakes is generated, and a third mode of operation which is provided for the transition from the second into the first mode of operation, wherein in the third mode of operation the wheel brake pressure (p WHEEL ) is excessively elevated compared to the tandem master cylinder pressure (p TMC ) in a controlled way, a particularly safe and user-friendly termination of the brake assistant system results from diminishing the amount of the excess elevation over the course of time.
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BACKGROUND OF THE INVENTION
The condensation of 1,4-dihalobutene-2 such as 1,4-dichlorobutene-2, with lower alkyl malonic esters such as dimethyl malonate is widely used in industry to prepare various vinylcyclopropane derivatives such as dimethyl 2-vinylcyclopropane-1,1-dicarboxylate which has utility in a wide variety of industrial applications.
The starting material for this condensation, 1,4-dichlorobutene-2 as a commercial product, is usually composed of three isomeric dichlorobutenes, trans-1,4-dichlorobutene-2, cis-1,4-dichlorobutene-2 and 3,4-dichlorobutene-1. Trans-1,4-dichlorobutene-2 is the preferred starting material as the stereochemistry of the intermediate (I) is such that the desired dimethyl 2-vinylcyclopropane-1,1-dicarboxylate is the exclusive product. This is illustrated in Mechanism I below: ##STR1##
Cis-1,4-dichlorobutene-2 gives two products, dimethyl 2-vinylcyclopropane-1,1-dicarboxylate and dimethyl cyclopent-3-ene-1,1-dicarboxylate in nearly equal amounts as shown in Mechanism II below. ##STR2##
It is nearly impossible to separate dimethyl cyclopent-3-ene-1,1-dicarboxylate from the desired dimethyl 2-vinylcyclopropane-1,1-dicarboxylate by any reasonable means. In the described condensation reaction the third isomer, 3,4-dichlorobutene-1 gives only useless elimination products.
Fractional distillation of the three dichlorobutene isomers can readily be accomplished, but this is an expensive process and leads to the additional difficulty and cost of disposing of 3,4-dichlorobutene-1 and cis-1,4-dichlorobutene-2.
Efforts have been made in terms of isomerizing cis-1,4-dichlorobutene-2 to trans-1,4-dichlorobutene-2, but these methods have met with only moderate success.
Heterogeneous iron, tin and copper compounds as well as onium salts have been reported in the literature as dichlorobutene isomerization catalysts. A typical process employing a copper catalyst is disclosed in U.S. Pat. No. 2,911,450. However, such processes are not completely satisfactory as they either have proven to be ineffective in some instances or have given equilibrium mixtures of all three dichlorobutenes.
The use of thiols as cis-to-trans-olefin isomerization catalysts has also been reported in the literature. See, W. G. Niehaus, Jr., Bioorg. Chem., 3(3), 302-10 (1974) and C. Walling, et al., J. Amer. Chem. Soc., 81, 1144-8(1959) as has hydrogen bromide-catalyzed isomerization. See N. P. Neureiter, et al., J. Amer. Chem. Soc., 82, 5354-8 (1960). However, the thiol-catalyzed and hydrogen bromide-catalyzed isomerization of olefins typically leads to an equilibrium mixture of approximately 80% trans- and 20% cis-olefin. This appears to be true regardless of whether the starting olefin is cis or trans. See C. Walling, et al. Ibid.
It would be highly desirable, therefore, if an improved process could be developed which would permit an efficient cis-to-trans isomerization of 1,4-dichlorobutene-2 so that a high trans (>90%) mixture could be obtained from the usual commercial mixture of 1,4-dichlorobutene-2, which normally has a trans/cis ratio of 77/23, or from other mixtures having even lower trans content without any of the attendant disadvantages of the prior art.
It would also be highly desirable to provide a product with a high content of trans-1,4-dichlorobutene-1 and being substantially free from the other two isomers, cis-1,4-dichlorobutene-2 and 3,4-dichlorobutene-2, which in the described condensation reaction with malonic esters either give approximately equal amounts of the desired dimethyl 2-vinylcyclopropane-1,1-dicarboxylate and the unwanted dimethyl cyclopent-3-ene-1,1-dicarboxylate or in the case of the isomeric 3,4-dichlorobutene-1 only useless elimination products.
BRIEF SUMMARY OF THE INVENTION
We have now discovered that it is possible to produce an efficient cis-to-trans isomerization of 1,4-dichlorobutene-2 so as to provide a high trans content greater than 90% which is eminently suitable for condensation with malonic esters to provide excellent yields of dimethyl 2-vinylcyclopropane-1,1-dicarboxylate with greater than 95% purity and with substantial elimination of 3,4-dichlorobutene-1.
DETAILED DESCRIPTION OF THE INVENTION
The present invention is based upon the discovery that mixtures of cis-and-trans-1,4-dichlorobutene-2 can be rapidly isomerized to mixtures containing very high levels of trans-1,4-dichlorobutene-2 under very mild conditions. The isomerization is accomplished under the catalytic influence of thiols or anhydrous hydrogen bromide or hydrogen chloride with ultraviolet light and/or chemical initiators so that an 80/20 trans/cis mixture is isomerized to a 95/5 trans/cis mixture in as little as ten minutes.
The temperature of the reaction is not critical and may conveniently be from room temperature up to 80° C. or higher depending upon the catalyst employed for the isomerization.
Likewise, the amount of catalyst is not critical and may conveniently be from 0.5 mole % based on the weight of the dichlorobutene to about 20 mole % and preferably from 5 mole % to 10 mole %.
The time of the reaction is likewise not critical and depends to some extent upon the catalyst employed for the isomerization. Thus with the thiol catalyzed isomerization the time may range from 30 minutes to an hour or more at reaction temperatures of from 70° C. to 90° C. whereas with the anhydrous hydrogen bromide or chloride catalyzed isomerization the time is frequently from twenty to thirty minutes or so at temperatures preferably at about room temperature.
With both the thiol catalyzed and hydrogen bromide or chloride catalyzed isomerizations, ratios better than 93/7 trans/cis- dichlorobutene-2 have consistently been obtained with 95-97% recovery of the dichlorobutene-2.
Typical throls useful in the described isomerization reaction are 2-mercaptoethanol, thiophenol, thiolacetic acid, methanethiol, thioglycolic acid, mercaptosuccinic acid, etc.
In the thiol catalyzed isomerization of the dihalobutenes as well as in the anhydrous hydrogen bromide or chloride isomerization reaction it is necessary to employ an initiator for the reaction. Typical chemical initiators may be, for example, 2,2'-azobisisobutyronitrile (AIBN), benzoyl peroxide, t-butyl peroxide, etc.
The amount of chemical initiator employed in the reaction is not critical but must be present in sufficient amount to initiate the reaction. Typically from about 0.1 mole % to about 5 mole % based on the weight of the dichlorobutene has been found to be effective.
As indicated above, 2-mercaptoethanol as the catalyst and 2,2'-azobisisobutyronitrile (AIBN) as the initiator are preferred and have been found to be highly useful in the isomerization of dichlorobutene as they consistently provide ratios greater than 93/7 or higher trans/cis-dichlorobutene with 95-97% recovery of the dichlorobutenes.
Hydrogen bromide with either AIBN or ultraviolet light has also been found to be effective in producing remarkably high trans/cis (95/5) ratios of dichlorobutene at room temperature.
Hydrogen bromide is the preferred catalyst in the described reaction and has been found to be equally effective with either AIBN or ultraviolet light initiation. However, 2-mercaptoethanol with ultraviolet light and hydrogen chloride with ultraviolet light showed marginal activity and hydrogen iodide and I 2 showed no catalytic activity with either AIBN or ultraviolet light.
While the present invention has been described hereinabove and in the examples which follow as being particularly applicable to 1,4-dichlorobutene-2 and 1,4-dibromobutene-2, it is to be understood that the isomerization reaction described is applicable to a wide variety of 1,4-dihalobutenes-2 including the following which are exemplary only and it is to be understood that the present invention is not limited thereto:
1,4-dichloro-2-methylbutene-2; 1,4-dibromo-2-methylbutene-2;
1,4-dichloro-2,3-dimethylbutene-2; 1,4-dibromo-2,3-dimethylbutene-2;
1,4-dichloropentene-2; 1,4-dibromopentene-2;
1,4-dichloro-4-methylpentene-2;
1,4-dibromo-4-methylpentene-2;
As indicated above, 1,4-Dichloro- and 1,4-dibromobutene-2 are particularly useful for the present process in view of their commercial availability, reactivity and ability to yield highly useful vinylcyclopropane derivatives.
The invention will be described in greater detail in conjunction with the following specific examples in which the parts are by weight unless otherwise specified.
EXAMPLE 1
Isomerization of Dichlorobutene with 2-Mercaptoethanol and 2,2'-Azobisisobutyronitrile (AIBN)
To 10 mL of 1,4-dichlorobutene-2 was added 0.5 mL of 2-mercaptoethanol (7.5 mole % based on 1,4-dichlorobutene-2) and 0.15 g of AIBN (0.97 mole %). The reaction was then stirred at 80° C. with the following results:
______________________________________ 0 minutes 80.5/19.2 trans/cis15 minutes 88.9/8.5 trans/cis30 minutes 91.0/6.7 trans/cis______________________________________
EXAMPLE 2
Isomerization of Dichlorobutene with HBr and UV Light
Approximately 100 mL of 1,4-dichlorobutene-2 was saturated with anhydrous HBr by subsurface introduction through a fritted glass gas dispersion tube. HBr addition was terminated when persistent fumes were visible above the liquid surface. The mixture was then stirred at ambient temperature while being irradiated with a Pen-Ray* lamp with the following results:
______________________________________0 minutes 76.6/22.9 trans/cis5 minutes 90.9/5.4 trans/cis10 minutes 90.4/5.1 trans/cis______________________________________
EXAMPLE 3
Following the procedure of Examples 1 and 2, the isomerization of 1,4-dichlorobutene was carried out with the results as shown in Table 1 below.
TABLE 1__________________________________________________________________________Isomerization of DichlorobutenesCat. Init. Rxn. Product distribution.sup.4Catal..sup.1Level.sup.2 Init..sup.1 Level.sup.2 Temp. Time.sup.3 t-1,4 c-1,4 other.sup.5__________________________________________________________________________2-ME 7.5 none -- .sup. 80° C. 0 78.8 21.2.sup.6 -- 180 81.8 18.2.sup.6 --2-ME 7.5 AIBN 0.96 80° 0 80.5 19.2 0.3 30 91.0 6.7 2.32-ME 0.5 AIBN 0.5 90° 0 76.7 22.4 0.9 60 80.1 19.1 0.82-ME 7.5 UV -- 80° 0 78.2 21.8.sup.6 -- 180 86.8 13.2.sup.6 --HBr -- AIBN 2.0 58° 0 73.6 21.3 5.1 10 90.0 7.0 3.0HBr -- UV -- 25° 0 76.6 22.9 0.5 10 90.4 5.1 4.5HBr -- UV -- 40° 0 6.8 91.3 1.9 5 89.7 6.0 4.2HCl -- AIBN 2.0 80° 0 75.0 22.1 2.9 10 75.1 21.9 3.0HCl -- UV -- 70° 0 79.4 19.0 1.6 20 82.7 15.1 2.2__________________________________________________________________________ .sup.1 2ME = 2mercaptoethanol; AIBN = 2,2azobisisobutyronitrile; UV = 253.7 nm ultraviolet light. .sup.2 Mole percent based on dichlorobutene. .sup.3 Reaction time in minutes .sup.4 Area percent by packed column GC analysis; t1,4 = trans1,4-dichlorobutene-2; c1,4 = cis1,4-dichlorobutene-2. .sup.5 Unidentified, but probably 3,4dichlorobutene-1. .sup.6 Product distributions for these two reactions are trans/cis ratios
EXAMPLE 4
Following the procedure of Examples 1 and 2, the isomerization of 1,4-dibromobutene-2 was carried out. Under the influence of the catalyst/initiator combinations of 2-mercaptoethanol/AIBN, 2-ME/UV light, and HBr/UV light, trans/cis-1,4-dibromobutene-2 product ratios ranging from 71/29 to 87/13 with 78-90% recovery of 1,4-dibromobutene-2 were obtained. The results are shown in Table 2 below.
TABLE 2__________________________________________________________________________Isomerization of DibromobutenesCat. Init. Rxn. Product distribution.sup.4Catal..sup.1Level.sup.2 Init..sup.1 Level.sup.2 Temp. Time.sup.3 t-1,4 c-1,4 other.sup.5__________________________________________________________________________2-ME 7.5 AIBN 0.96 80° 0 17.3 74.9 4.2 30 75.1 12.7 11.32-ME 7.5 AIBN 0.96 80° 0 18.2 74.6 2.8 30 77.4 12.8 9.8HBr -- AIBN 2.0 60° 0 13.4 83.2 3.4 10 18.2 77.2 4.7HBr -- AIBN 2.0 60° 0 44.9 36.6 17.6 20 65.3 18.6 16.1HBr -- UV -- 28° 0 27.0 58.3 14.7 15 65.1 13.1 21.8__________________________________________________________________________ .sup.1 2ME = 2mercaptoethanol; AIBN = 2,2azobisisobutyronitrile; UV = 253.7 nm. ultraviolet light .sup.2 Mole percent based on dibromobutene .sup.3 Reaction time in minutes .sup.4 Area percent by packed column GC analysis; t1,4 = trans1,4-dibromobutene-2; c1,4 = cis1,4-dibromobutene-2 .sup.5 Unidentified, but probably 3,4dibromobutene-1
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This invention relates to an efficient cis-to-trans isomerization of 1,4-dihalobutene-2 by means of a thiol or hydrogen bromide or hydrogen chloride catalyzed reaction.
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RELATED APPLICATIONS
The present application is based on, and claims priority from, Japanese Application Number 2008-001916, filed Jan. 9, 2008, the disclosure of which is hereby incorporated by reference herein in its entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a motor drive apparatus equipped with a dynamic braking circuit fault detection capability, and more particularly to a motor drive apparatus having a capability to detect faults in a dynamic braking circuit (such as a contact welding defect or an electrically inoperable contact, breakage of a resistor, disconnection of a connecting cable, etc.).
2. Description of the Related Art
FIG. 7 is a block diagram showing the configuration of a motor drive apparatus according to the prior art.
In the motor drive apparatus 101 shown in FIG. 7 , a DC power supply 102 converts AC power, supplied from an AC power supply not shown, into DC power. The DC power from the DC power supply 102 is supplied to a synchronous motor 104 (hereinafter referred to as the motor) via a power transistor unit 103 comprising power transistors A to F. When the power to the motor 104 is cut off while the motor 104 is running, a dynamic braking circuit 105 actuates switches S 1 and S 2 , i.e., relay contacts, so that the power is dissipated through resistors Ru, Rv, and Rw in the dynamic braking circuit 105 .
A motor drive control circuit 110 outputs a dynamic braking circuit control signal SIG 1 , in response to which a fault detection circuit 111 generates a power transistor control signal SIG 2 for controlling the driving/stopping of the motor 104 , i.e., a power transistor ON/OFF signal, and supplies it to the power transistors A to F in the power transistor unit 103 . A current detector 106 detects current flowing from the power transistor unit 103 to the motor 104 .
The fault detection circuit 111 receives the dynamic braking circuit control signal SIG 1 from the motor drive control circuit 110 and a contact state signal SIG 70 from the dynamic braking circuit 105 , i.e., an ON/OFF signal indicating the operation ON/OFF state of the motor 104 in accordance with the ON/OFF state of the switches S 1 and S 2 , and detects from these signals a fault occurring in the dynamic braking circuit 105 (such as a contact welding defect or an electrically inoperable contact, breakage of a resistor, or disconnection of a connecting cable). To check the operation of the dynamic braking circuit 105 at the time of control of the motor 104 , it is common to use the contact state signal SIG 70 that indicates the contact state of the switches S 1 and S 2 as hardware provided in the dynamic braking circuit 105 .
Methods that do not use such a contact state signal are also known; as one such method, there is disclosed, for example, in Patent Publication No. 1, a method that checks the operation/non-operation of the dynamic braking circuit by lowering the DC voltage when starting the motor operation.
[Patent Publication No. 1] Japanese Patent No. 3383965 (refer to [CLAIM 1] in Patent Claims, paragraphs [0003] to [0006] in Patent Specification, and FIGS. 1 and 2)
The method that requires the addition of a hardware contact signal involves the problem that the apparatus cost increases. On the other hand, the method of Patent Publication No. 1 that does not use such a contact signal requires the addition of a control circuit in order to perform control to obtain a low supply voltage necessary for fault detection, and this also involves the problem that the apparatus cost increases.
SUMMARY OF THE INVENTION
The present invention has been devised to solve the problem that the cost increases due to the addition of two extra hardware pieces, i.e., the contact signal and the control circuit, and it is an object of the present invention to provide a motor drive apparatus equipped with a dynamic braking circuit fault detection capability to detect faults in a dynamic braking circuit without requiring the addition of such two extra hardware pieces.
It is another object of the invention to enable the operation of the dynamic braking to be checked in a short time while the motor is in a stopped condition.
A motor drive apparatus that accomplishes the above objects has a dynamic braking circuit for producing a deceleration torque utilizing a braking force caused by a synchronous motor acting as a generator when the synchronous motor is deenergized, and is equipped with a dynamic braking circuit fault detection capability, comprising: a DC power supply which is obtained by rectifying input AC power; voltage application means for applying a voltage to a winding of the synchronous motor and to the dynamic braking circuit for a predetermined length of time by switching a power transistor connected to the DC power supply; current detection means for detecting the value of a current flowing from the power transistor; and fault checking means for checking the dynamic braking circuit for the presence or absence of a fault, based on the current value detected by the current detection means and on a predefined threshold value.
In the motor drive apparatus, the predetermined length of time during which the voltage is applied from the DC power supply is chosen so that a transient current that flows through the motor winding after the power transistor is turned on does not exceed a current that flows through a dynamic braking resistor.
In the motor drive apparatus, the predetermined length of time during which the voltage is applied from the DC power supply is set longer than a current detection delay time that occurs when the current detection means detects the current.
In the motor drive apparatus equipped, the threshold value is changed according to the resistance value of the dynamic braking circuit or to the inductance of the synchronous motor.
In the motor drive apparatus, an overcurrent detection circuit incorporated in a motor drive control circuit is used as the current detection means, and the threshold value is set so as to serve as an overcurrent detection level when checking the dynamic braking circuit for a fault.
According to the invention, the operation of the dynamic braking can be checked in a short time while the motor is in a stopped condition.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram schematically showing the configuration of a motor drive apparatus according to a first embodiment of the present invention.
FIG. 2 is a flowchart illustrating a fault detection process for a dynamic braking circuit in the motor drive apparatus shown in FIG. 1 .
FIGS. 3A to 3C are time charts showing a first specific example of the pattern of a dynamic braking circuit control signal and the resulting current (when there is no current detection delay) in the motor drive apparatus shown in FIG. 1 : FIG. 3A shows a power transistor ON/OFF signal output from a fault detection circuit, FIG. 3B shows the waveform of the current when the dynamic braking circuit is not connected, and FIG. 3C shows the waveform of the current when the dynamic braking circuit is connected.
FIGS. 4A to 4C are time charts showing a second specific example of the pattern of the dynamic braking circuit control signal and the resulting current (when there is current detection delay) in the motor drive apparatus shown in FIG. 1 : FIG. 4A shows the power transistor ON/OFF signal output from the fault detection circuit, FIG. 4B shows the waveform of the current when the dynamic braking circuit is not connected, and FIG. 4C shows the waveform of the current when the dynamic braking circuit is connected.
FIG. 5 is a block diagram schematically showing the configuration of a motor drive apparatus according to a second embodiment of the present invention.
FIG. 6 is a flowchart illustrating a fault detection process for a dynamic braking circuit in the motor drive apparatus shown in FIG. 5 .
FIG. 7 is a block diagram showing the configuration of a motor drive apparatus according to the prior art.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The embodiments of the present invention will be described below with reference to the accompanying drawings.
FIG. 1 is a block diagram schematically showing the configuration of a motor drive apparatus according to a first embodiment of the present invention.
In the motor drive apparatus 1 generally shown in FIG. 1 , a DC power supply 2 converts AC power, supplied from an AC power supply 200 , into DC power. The DC power from the DC power supply 2 is supplied to a synchronous motor (hereinafter referred to as the motor) 4 via a power transistor unit 3 comprising power transistors A to F. When the power to the motor 4 is cut off while the motor 4 is running, a dynamic braking circuit 5 actuates switches S 1 and S 2 , i.e., relay contacts, so that the power is dissipated through resistors Ru, Rv, and Rw in the dynamic braking circuit 5 .
A motor drive control circuit 10 outputs a dynamic braking circuit control signal SIG 1 , in response to which a fault detection circuit 11 generates a power transistor control signal SIG 2 for controlling the driving/stopping of the motor 4 and supplies it to the power transistors A to F in the power transistor unit 3 . A current detector 6 detects current flowing from the power transistor unit 3 to the motor 4 , converts the current value from analog to digital, and supplies the resulting current signal SIG 10 to the fault detection circuit 11 .
The fault detection circuit 11 receives the dynamic braking circuit control signal SIG 1 from the motor drive control circuit 10 and the current signal SIG 10 from the current detector 6 , and detects from these signals a fault occurring in the dynamic braking circuit 5 (such as a contact welding defect or an electrically inoperable contact, breakage of a resistor, or disconnection of a connecting cable).
FIG. 2 is a flowchart illustrating a fault detection process for the dynamic braking circuit in the motor drive apparatus 1 shown in FIG. 1 . The process is executed by the fault detection circuit 11 comprising a conventional computer, that is, a CPU, an input/output interface, a RAM, a ROM, a disk, etc.
In step 201 , the power transistor control signal SIG 2 for checking purposes is applied to the power transistors A to F for a predetermined length of time Δt. The predetermined length of time Δt during which the voltage is applied from the DC power supply 2 to the dynamic braking circuit 5 is chosen so that the transient current that flows through the motor windings after the power transistors are turned on does not exceed the current that flows through the dynamic braking resistors.
In step 202 , the current that is output from the power transistors A to F is detected by the current detector 6 , and the analog-to-digital converted current signal SIG 10 (current value I) is received.
In step 203 , the dynamic braking circuit 5 checks whether the dynamic braking circuit control signal SIG 1 output from the motor drive control circuit 10 is indicating a connect command or not; if the result of the check is YES, the process proceeds to step 214 , but if the result of the check is NO, the process proceeds to step 204 .
In step 204 , the current value I received in step 202 is compared with a threshold value TH, and if I <TH, the process proceeds to step 205 , but if I≧TH, the routine is terminated. The threshold value TH may be changed according to the resistance values Ru, Rv, and Rw of the dynamic braking circuit 5 or the inductances Lu, Lv, and Lw of the motor. Further, an overcurrent detection circuit (not shown) incorporated in the motor drive control circuit 10 may be used as the current detector 6 , and the threshold value may be set so as to serve as an overcurrent detection level when checking the dynamic braking unit 5 for faults.
In step 205 , it is determined that the dynamic braking circuit 5 is faulty, and a message “DYNAMIC BRAKING CIRCUIT TO BE DISCONNECTED IS FAULTY” is produced using a display or a printer not shown in FIG. 1 .
In step 214 , the current value I received in step 202 is compared with the threshold value TH, and if I>TH, the process proceeds to step 215 , but if I≦TH, the routine is terminated.
In step 215 , it is determined that the dynamic braking circuit 5 is faulty, and a message “DYNAMIC BRAKING CIRCUIT TO BE CONNECTED IS FAULTY” is produced using a display or a printer not shown in FIG. 1 .
FIGS. 3A to 3C are time charts showing a first specific example of the pattern of the dynamic braking circuit control signal and the resulting current (when there is no current detection delay) in the motor drive apparatus shown in FIG. 1 : FIG. 3A shows the power transistor ON/OFF signal output from the fault detection circuit, FIG. 3B shows the waveform of the current when the dynamic braking circuit is not connected, and FIG. 3C shows the waveform of the current when the dynamic braking circuit is connected. In FIGS. 3A to 3C , the abscissa represents the time, the ordinate in FIG. 3A represents the ON/OFF state, and the ordinate in FIGS. 3B and 3C represents the waveform of the current.
Usually, when the power to the motor 4 is cut off while the motor 4 is running, the dynamic braking circuit 5 is connected to the motor power line, and the energy from the motor 4 is dissipated through the resistors Ru, Rv, and Rw in the dynamic braking circuit 5 , thereby reducing the stopping distance of the motor.
On the other hand, when driving the motor 4 , the dynamic braking circuit 5 is disconnected from the power transistor unit 3 which is a motor drive circuit, and only the motor 5 is connected to the motor driving power transistor unit 3 .
If the contacts for connecting the dynamic braking circuit 5 to the motor power line remain closed due to welding defects, and the dynamic braking circuit 5 is not disconnected from the motor power line when driving the motor 4 , the currents Iu, Iv, and Iw for driving the motor 4 flow into the dynamic braking circuit 5 , resulting in an inability to perform desired current control or in overheating the resistors in the dynamic braking circuit 5 or generating an overcurrent alarm.
The motor drive apparatus 1 provided by the present invention is equipped with a capability to apply a dynamic braking checking control signal SIG 2 before driving the motor 4 and thereby verify that the dynamic braking circuit 5 is disconnected or connected properly.
More specifically, the DC power supply 2 for driving the motor 4 is obtained by rectifying the input AC power, and the voltage from the DC power supply 2 is applied via the power transistors A to F to the motor windings Lu, Lv, and Lw for a suitable length of time for the respective phases U, V, and W of the motor 4 , and the currents Iu, Iv, and Iw flowing from the power transistors A to F to the resistors ru, rv, and rw of the respective windings of the motor 4 are detected by the current detector 6 to check the dynamic braking circuit 5 for any fault.
When voltage Vdc is applied from the DC power supply 2 to the power transistors A to F and to the dynamic braking circuit 5 and the motor 4 , the current I (Iu, Iv, Iw) that flows from the power transistors A to F after time t has elapsed from the application of the voltage is expressed by the following equation.
I=Vdc/r{ 1−exp(− r/L*t )}+ Vdc/R (Equation 1)
where
r: Motor winding resistance
L: Motor inductance
R: Dynamic braking circuit resistance
As far as the transient period immediately after switching is concerned, it may be assumed that r/L*t<<1, and therefore Equation 1 can be approximated by Equation 2 shown below.
I≈Vdc/L*t+Vdc/R (Equation 2)
The first term Vdc/L*t represents the current I (Iu, Iv, Iw) that flows into the windings Lu, Lv, and Lw of the motor 4 , and the second term Vdc/R represents the current I (Iu, Iv, Iw) that flows into the dynamic braking circuit 5 . The first characteristic here is that the current I (Iu, Iv, Iw) that flows when the dynamic braking circuit 5 is disconnected is different by an amount equal to Vdc/R from that when the dynamic braking circuit 5 is connected.
FIGS. 4A to 4C are time charts showing a second specific example of the pattern of the dynamic braking circuit control signal and the resulting current (when there is current detection delay) in the motor drive apparatus shown in FIG. 1 : FIG. 4A shows the power transistor ON/OFF signal output from the fault detection circuit, FIG. 4B shows the waveform of the current when the dynamic braking circuit is not connected, and FIG. 4C shows the waveform of the current when the dynamic braking circuit is connected. In parts FIGS. 4A to 4C , the abscissa represents the time, the ordinate in FIG. 4A represents the ON/OFF state, and the ordinate in FIGS. 4B and 4C represents the waveform of the current.
The current I (the first term) (Iu, Iv, Iw) that flows into the windings Lu, Lv, and Lw of the motor 4 has a large inductive component, and hence the second characteristic that it takes time to rise after the power transistors A to F are turned on.
The predetermined length of time Δt during which the voltage is applied from the DC power supply 2 is set longer than the current detection delay time δthat occurs when the current detector 5 detects the current.
From the first and second characteristics, when the current I (Iu, Iv, Iw) flowing from the power transistors A to F is detected immediately after (Δt seconds after) switching the power transistors A to F, if, despite the presence of a command for connecting the dynamic braking circuit 5 to the windings Lu, Lv, and Lw of the motor 4 , the current I (Iu, Iv, Iw) flowing from the power transistors A to F is smaller than a threshold value which is set as a current value smaller than Vdc/R but larger than Vdc/L*Δt, it is determined that a fault has occurred such as an electrically inoperable contact in the switches S 1 and S 2 functioning as relay contacts for connecting the dynamic braking circuit 5 , breakage of a resistor in the dynamic braking circuit 5 , or disconnection of a connecting cable to the motor power line.
On the other hand, if, despite the presence of a command for disconnecting the dynamic braking circuit 5 from the windings Lu, Lv, and Lw of the motor 4 , the current I (Iu, Iv, Iw) flowing from the power transistors A to F is larger than the threshold value, it is determined that a fault has occurred such that the contacts for connecting the dynamic braking circuit 5 remain closed due to welding defects.
An overcurrent detection circuit (not shown) originally provided in the motor drive control circuit 10 may be used to detect the current value.
When an overcurrent detection circuit 57 such as shown in FIG. 5 described below is used, it is also possible to use the threshold value by switching between the threshold value for checking the dynamic braking circuit 5 (the overcurrent detection level) and the normal (motor driving) overcurrent detection level.
FIG. 5 is a block diagram schematically showing the configuration of a motor drive apparatus according to a second embodiment of the present invention.
In the motor drive apparatus 15 generally shown in FIG. 5 , the DC power output from a DC power supply 52 is supplied to a motor 54 via a power transistor unit 53 comprising power transistors A to F. When the power to the synchronous motor (hereinafter referred to as the motor) 54 is cut off while the motor 54 is running, a dynamic braking circuit 55 actuates switches S 1 and S 2 , i.e., relay contacts, so that the power is dissipated through resistors Ru, Rv, and Rw in the dynamic braking circuit 55 .
A motor drive control circuit 60 outputs a dynamic braking circuit control signal SIG 1 , in response to which a fault detection circuit 61 generates a power transistor control signal SIG 2 for controlling the driving/stopping of the motor 4 and supplies it to the power transistors A to F in the power transistor unit 53 . A current detector 56 detects current flowing from the power transistor unit 53 to the motor 54 . An overcurrent detection circuit 57 compares the current value, detected and analog-to-digital converted by the current detector 56 , with the overcurrent threshold value supplied to the overcurrent detection circuit 57 , and supplies the resulting overcurrent state signal SIG 50 to the fault detection circuit 61 .
The fault detection circuit 61 receives the dynamic braking circuit control signal SIG 1 from the motor drive control circuit 60 and the overcurrent state signal SIG 50 from the overcurrent detection circuit 57 , and detects from these signals a fault occurring in the dynamic braking circuit 55 (such as a contact welding defect or an electrically inoperable contact, breakage of a resistor, or disconnection of a connecting cable).
FIG. 6 is a flowchart illustrating a fault detection process for the dynamic braking circuit in the motor drive apparatus shown in FIG. 5 . The process is executed by the fault detection circuit 61 comprising a conventional computer, that is, a CPU, an input/output interface, a RAM, a ROM, a disk, etc.
In step 601 , the overcurrent detection threshold value is changed from the normal control threshold value THNM to the dynamic braking fault detection threshold value THTM.
In step 602 , the power transistor control signal SIG 2 for checking purposes is applied to the power transistors A to F for a predetermined length of time Δt. The predetermined length of time Δt is set sufficiently longer than the current detection delay time δ(Δt>>δ).
In step 603 , the current that is output from the power transistors A to F is detected and analog-to-digital converted by the current detector 56 , and the overcurrent state signal SIG 50 output from the overcurrent detection circuit 57 in response to the analog-to-digital converted current value I is received. The overcurrent detecting circuit 57 compares the current value I with the test mode threshold value THTM and, if I <THTM, it is determined that the current is not an overcurrent, and a level “0” is output; on the other hand, if I≧THTM, it is determined that the current is an overcurrent, and a level “1” is output.
In step 604 , the dynamic braking circuit 55 checks whether the dynamic braking circuit control signal SIG 1 output from the motor drive control circuit 60 is indicating a connect command; if the result of the check is YES, the process proceeds to step 615 , but if the result of the check is NO, the process proceeds to step 605 .
In step 605 , if the overcurrent state signal SIG 50 received in step 603 is at level “0,” the process proceeds to step 607 , but if it is at level “1,” the process proceeds to step 606 .
In step 606 , it is determined that the dynamic braking circuit 55 is faulty, and a message “DYNAMIC BRAKING CIRCUIT TO BE DISCONNECTED IS FAULTY” is produced using a display or a printer not shown in FIG. 5 .
In step 607 , the overcurrent detection threshold value is changed from the dynamic braking fault detection threshold value THTM to the normal control threshold value THNM, and then the routine is terminated.
In step 615 , if the overcurrent state signal SIG 10 received in step 603 is at level “0,” the process proceeds to step 616 , but if it is at level “1,” the process proceeds to step 607 .
In step 616 , it is determined that the dynamic braking circuit 55 is faulty, and a message “DYNAMIC BRAKING CIRCUIT TO BE CONNECTED IS FAULTY” is produced using a display or a printer not shown in FIG. 5 .
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A motor drive includes a dynamic braking circuit for producing a deceleration torque utilizing a braking force caused by a synchronous motor acting as a generator when the synchronous motor is deenergized. The motor drive apparatus is equipped with a dynamic braking circuit fault detection capability, a DC power supply which is obtained by rectifying input AC power, voltage application function for applying a voltage to the windings of the synchronous motor and to the dynamic braking circuit for a predetermined length of time by switching power transistors connected to the DC power supply, current detection unit for detecting the value of a current flowing from the power transistors, and fault checking unit for checking the dynamic braking circuit for the presence or absence of a fault, based on the current value detected by the current detection unit and on a predefined threshold value.
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BACKGROUND OF THE INVENTION
The present invention relates to coffee brewing and in particular to efficiently manufacturing a filter paper cup.
Various methods of brewing coffee are known. A popular method is using a single serving pod or filter paper cup in a brewing machine designed to accept the corresponding pod or filter paper cup. Pods are generally disk like with a diameter much greater than the depth of the pod, where as a filter paper cup may have similar diameter and depth. Machines are know for efficiently manufacturing pods and described in U.S. Pat. No. 5,012,629 issued May 7, 1991, U.S. Pat. No. 5,649,412 issued Jul. 22, 1997, and U.S. Pat. No. 7,377,089 issued May 27, 2008. While these patents disclose useful methods to manufacture a typical coffee pod, they reply on methods for forming a brewing material receptacle from strips of flat filter paper material which is only suitable for a shallow receptacle because the filter paper cannot stretch to accommodate forming adjacent pods from a common strip of filter paper. Forming such shallow receptacles require minimum stretching or deformation of the filter paper to form adjacent pods. If these machines are merely scaled for a deeper receptacle, the filter paper would be unacceptably deformed or tear in the process. The '629, 412, and 089 patents are incorporated herein in their entirely by reference.
BRIEF SUMMARY OF THE INVENTION
The present invention addresses the above and other needs by providing a filter paper cup manufacturing machine which produces filter paper cups containing a brewing material. The filter paper cups have similar depth and diameter. The machine exercises ordered steps of first cutting a receptacle portion and then forming a recess in the receptacle portion for receiving the brewing material. Performing the cutting step first facilitates forming the recess because surrounding filter paper which would resist forming the recess has been eliminated.
In accordance with another aspect of the invention, there is provided a filter paper cup manufacturing machine comprising a number of sequentially arranged stations. The stations include a roll of first filter paper and a roller guiding the filter paper onto the belt; a cutting station used to perform a circular cut in the filter paper for forming each individual filter paper cup; a stamping station pressing a center portion of the cut filter paper into a corresponding recess in the belt to form a paper recess; a filling station to fill the paper recess in the filter paper with brewing material; a tamping station to tamp the brewing material residing in the paper recess; a vacuum station to remove excess brewing material from a rim of the receptacle portion; a roll of second filter paper and a second roller guiding the second filter paper over the receptacle portion; a seal station bonds the second filter paper to the receptacle portion; and a second cutting station cuts through the second filter paper to compete the filter paper cup.
In accordance with another aspect of the invention, there is provided a method for manufacturing filter paper cups. The method includes the steps of: cutting a separate receptacle portion for forming each individual filter paper cup, forming the receptacle portion; heating or dampening the formed receptacle portion to retain shape; filling the receptacle portion with brewing material; tamping the brewing material; vacuuming excess brewing material; fixing a cover portion over the receptacle portion; and cutting the completed pod.
In accordance with another aspect of the invention, there is provided method for manufacturing a filter paper cup packaging. The method includes: cutting separate attached receptacle portion and cover portion for forming each individual filter paper cup packaging; forming recesses in the receptacle portions; and heating or dampening the formed receptacle portions to retain shape.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
The above and other aspects, features and advantages of the present invention will be more apparent from the following more particular description thereof, presented in conjunction with the following drawings wherein:
FIG. 1 is a filter paper cup manufacturing machine according to the present invention.
FIG. 2 shown a cover portion and receptacle portion of a filter paper cup according to the present invention.
FIG. 3 is a plate element according to the present invention of a segmented belt.
FIG. 3A is a cross-sectional view of the plate according to the present invention taken along line 3 A- 3 A of FIG. 3 .
FIG. 4 is a vacuum table element of the filter paper cup manufacturing machine according to the present invention.
FIG. 5 is a cross-sectional view of the vacuum table element of the filter paper cup manufacturing machine according to the present invention taken along line 5 - 5 of FIG. 4 .
FIG. 6 is a method according to the present invention.
FIG. 7 shows a turret type filter paper cup manufacturing machine according to the present invention.
FIG. 8 shows a turret having arms of the turret type filter paper cup manufacturing machine according to the present invention.
FIG. 9 shows a turret having a rotating table of the turret type filter paper cup manufacturing machine according to the present invention.
FIG. 10 shows a filter paper cup packaging manufacturing machine according to the present invention.
FIG. 11A shows a perspective view of an empty filter paper cup packaging according to the present invention.
FIG. 11B shows a side view of the empty filter paper cup packaging according to the present invention.
FIG. 12 is a method for manufacturing a filter paper cup packaging according to the present invention.
Corresponding reference characters indicate corresponding components throughout the several views of the drawings.
DETAILED DESCRIPTION OF THE INVENTION
The following description is of the best mode presently contemplated for carrying out the invention. This description is not to be taken in a limiting sense, but is made merely for the purpose of describing one or more preferred embodiments of the invention. The scope of the invention should be determined with reference to the claims.
A filter paper cup manufacturing machine 10 according to the present invention is shown in FIG. 1 . The filter paper cup manufacturing machine 10 includes a belt 16 running around two rollers 18 a and 18 b . The belt 16 includes belt recesses 18 used for forming and holding filter paper cup receptacle portions during the manufacturing of filter paper cups 40 . A vacuum table 20 resides under the higher path of the belt 16 to hold first filter paper material 12 a and the lower portions 40 b (see FIG. 2 ) as they are formed and filled with brewing material.
A series of ordered stations process filter paper to manufacture the completed filter paper cups 40 . The stations comprise: a roll of first filter paper 12 a and a roller 14 a guiding the filter paper 12 a onto the belt 16 ; a cutting station 22 used to perform a circular cut in the filter paper 12 a to create separate pieces of filter paper for forming each individual filter paper cup; a stamping station 24 pressing a center portion of the cut filter paper into a corresponding recess 18 in the belt 16 to form a paper recess 39 and using heat or dampening to retain the shape of the recess 39 ; a filling station 26 to fill the paper recess 39 in the filter paper 12 a with brewing material; a tamping station 28 to tamp the brewing material residing in the paper recess 39 ; a vacuum station 30 to remove excess brewing material from a rim 41 of the receptacle portion 40 a ; a roll of second filter paper 12 b and a second roller 14 b guiding the second filter paper 12 b over the receptacle portion 40 a ; a seal station 32 bonds the second filter paper to the receptacle portion 40 a ; and a second cutting station 34 cuts through the second filter paper 12 b to compete the filter paper cup 40 .
The stations of the filter paper cup manufacturing machine 10 are similar to stations of U.S. Pat. No. 5,649,412 (incorporated by reference above), but significantly, the first station is the cutting station 22 which cuts substantially all of the perimeter of the receptacle portion 40 a from the first filter paper 12 a and the receptacle portion 40 a is held against the belt 16 for subsequent stations by vacuum provided by the vacuum table 20 . While it is preferred to cut the receptacle portion 40 a entirely away from the first filter paper 12 a to allow for forming the recess 39 in the receptacle portion 40 a , a small attachment between the receptacle portion 40 a and the filter paper 12 a to, for example, help control the position of the receptacle portion 40 a during processing at subsequent stations.
While the stations 22 , 24 , 26 , 28 , 30 , 32 , and 34 are shown as separate spaced apart stations, the some or all of the stations 22 , 24 , 26 , 28 , 30 , 32 , and 34 may be combined in a single station which performs that processing of the separate stations 22 , 24 , 26 , 28 , 30 , 32 , and 34 in the same order as the spaced apart stations. For example, a single station may include a cutter to first cut the receptacle portion 40 a from the filter paper 12 a , and then a stamp to form the recess 39 in the receptacle portion 40 a . Other stations may be similarly combined. Further, when accepting filter paper from rolls, precut filter paper may be fed and positioned onto the belt 16 . Importantly, any filter paper cup manufacturing machine 10 forming a recess 39 in a pre-cut receptacle portion 40 b is intended to come within the scope of the present invention.
The receptacle portion 40 a and cover portion 40 b of the filter paper cups 40 are shown in FIG. 2 . The receptacle portion 40 a include a rim 41 and recess 39 . Forming the recess 39 in the receptacle portion 40 a of the filter paper cup 40 preferably includes using heat and/or moisture to form permanent folds (or pleats) 45 in the sides 43 and rim 41 of the receptacle portion 40 a to add strength and rigidity to the receptacle portion 40 a so that the receptacle portion 40 a retains its shape after forming, and preferably, adhesive is present in the filter paper 12 a or is applied to the rim 41 and/or the sides 43 to retain the pleats and add strength and rigidity to the filter paper cup 40 . Preferably, the receptacle portion 40 a is constructed from heat sealable filter paper having a heat reacting film on at least one side, which film causes the pleats to adhere to adjacent pleats when heat is applied following forming. The pleats 45 in the rim 41 are generally continuations of the pleats in the sides 43 . The receptacle portion 40 a may alternatively be corrugated to retain shape. The receptacle portion 40 a thus has structure for maintaining a substantially (i.e., within the ability of the paper to maintain a shape) frusto-conical or cylindrical shape unlike known coffee pods with have no structure for maintaining shape and are pillow-like with diameter much greater than depth. U.S. patent application Ser. No. 11/392,893 filed Mar. 28, 2006 filed by the present inventor, discloses a similar filter paper cup forming a coffee pod. The '893 application is herein incorporated by reference in its entirely.
The belt 16 may be a continuous belt or a segmented (e.g. tractor tread like) belt (or continuous chain) configured to receive plates 16 a , allowing substitution of plates having various recess 18 sizes. A perspective view of the plate 16 a is shown in FIG. 3 and a cross-sectional view of the plate 16 a taken along line 3 A- 3 A of FIG. 3 is shown in FIG. 3A . Each plate includes at least one recess 18 for forming and processing one or more receptacle portions 40 a . A vacuum source is provided along the edge or bottom of the plates 16 a to retain the filter paper on the plates 16 a during processing and to remove the vacuum when the filter paper cups 40 are complete. At completion, the vacuum source may be replace by a pressure source to facilitate the finished filter paper cup 40 exit from the recess in the plate. The plates 16 a are preferably coated with a low friction material (for example Teflon®).
The plate 16 a includes the belt recesses 18 for receiving and shaping the receptacle portion 40 a . The plate 16 a preferably includes perforations 17 or other means allowing vacuum to communicate with the filter paper 12 a for retain the position of the filter paper while forming the receptacle portion 40 a , and a vacuum port 19 in communication with a vacuum source. An example of such a segmented belt is discloses in U.S. Pat. No. 5,649,412 incorporated by reference above.
An example of one vacuum source for a continuous belt 16 is the vacuum table 20 according to the present invention shown in FIG. 4 and a cross-sectional view of the vacuum table 20 taken along line 5 - 5 of FIG. 4 is shown in FIG. 5 . The vacuum table includes gaps 21 allowing belt recesses 16 on the bottom of the continuous belt 16 to enter and leave the vacuum table 20 . Gates 21 a are formed from a flexible or deformable material at each end of the gaps 21 to limit the loss of vacuum during operation of the filter paper cup manufacturing machine 10 . The gates 21 a bend or deform when the belt recesses 16 enter or exit the vacuum table 20 . Other types of gates may be used, for example, brushes reaching upward or inward and a filter paper cup manufacturing machine 10 having a vacuum table including any form of gate to limit the loss of vacuum is intended to come within the scope of the present invention.
A method according to the present invention is shown in FIG. 6 . The method includes the steps of: cutting a separate receptacle portion for forming each individual filter paper cup at step 100 , forming the receptacle portion at step 102 ; heating or dampening the formed receptacle portion to retain shape at step 104 ; filling the receptacle portion with brewing material at step 106 ; tamping the brewing material at step 108 ; vacuuming excess brewing material at step 110 ; fixing a cover portion over the receptacle portion at step 112 ; and cutting the completed pod at step 114 . The heating or dampening the formed receptacle portion to retain shape at step 104 is preferably heating heat sealable filter paper having a heat reacting film on at least one side to retain shape of the receptacle portion.
A turret type filter paper cup manufacturing machine 50 according to the present invention is shown in FIG. 7 . The turret type filter paper cup manufacturing machine 50 includes a rotating center 50 and arms 52 rotating under the stations 22 , 24 , 26 , 28 , 30 , 32 , and 34 of FIG. 1 . Each arm 52 may includes a vacuum source to retain the receptacle portion 40 a position. After the cutting station 43 , the arm may be rotated and the vacuum removed to allow the completed filter paper cup 40 to drop from the arm.
A turret having the arms 52 of the turret type filter paper cup manufacturing machine 50 is shown in FIG. 8 and a turret having a rotating table of the turret type filter paper cup manufacturing machine 50 is shown in FIG. 9 . The turret includes receptacles 65 which are rotated under the stations 22 - 34 f for forming the filter paper cups 40 . Both the arms 52 and the table 54 may include the vacuum source for holding the filter paper during processing.
In an alternative embodiment, the horizontally turret is replaced by a vertical carrousel. The stations are positioned around the carrousel to process the filter paper to manufacture the filter paper cup. In still another embodiment, the filter paper is held fixed while the stations are moved linearly, in a horizontal circular motion (e.g., like the horizontal turret), or along a vertical arc (e.g., as along a vertical arc). When the filter paper cup is completed, the filter paper is advanced.
A filter paper cup packaging manufacturing machine 60 according to the present invention is shown in FIG. 10 and a perspective view of an empty filter paper cup packaging 40 ′ according to the present invention is shown in FIG. 11A and a side view of an empty filter paper cup packaging 40 ′ according to the present invention is shown in FIG. 11B . The filter paper cup packaging manufacturing machine 60 manufactures empty filter paper cups for use with a brewing material holder as disclosed in U.S. patent application Ser. No. 12,960,496 filed Dec. 4, 2010 by the present inventor. The '496 application is herein incorporated by reference.
The filter paper cup packaging 40 ′ is preferably made from a single piece of filter paper cut from the filter paper 12 a at station 22 ′ with cuts for two or more filter paper cup packagings 40 in a single operation, and the recesses 39 for two or more filter paper cup packagings 40 in a single operation at station 24 ′. Because each cut creates a smaller circular cut attached to a larger circular cut, the filter paper cup packagings 40 are alternated in consecutive cuts to optimize the use of the filter paper 12 a . Just as in manufacturing the filled filter paper cups 40 described above, significantly, the filter paper is first cut, and then the recesses 39 are formed. If the filter paper 12 a was not first cut and then formed, the forming step would tear or otherwise distort the filter paper 12 a.
FIG. 12 is a method for manufacturing a filter paper cup packaging according to the present invention. The method includes: cutting separate attached receptacle portion and cover portion for forming each individual filter paper cup packaging at step 116 ; forming recesses in the receptacle portions at step 118 ; and heating or dampening the formed receptacle portions to retain shape at step 120 . The filter paper is preferably a heat sealable filter paper having a heat reacting film on at least one side to retain shape of the receptacle portion, and the formed recess is heated to retain shape.
While the invention herein disclosed has been described by means of specific embodiments and applications thereof, numerous modifications and variations could be made thereto by those skilled in the art without departing from the scope of the invention set forth in the claims.
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A filter paper cup manufacturing machine produces filter paper cups containing a brewing material. The filter paper cups have similar depth and diameter. The machine exercises ordered steps of first cutting a receptacle portion and then forming a recess in the receptacle portion for receiving the brewing material. Performing the cutting step first facilitates forming the recess because surrounding filter paper which would resist forming the recess has been eliminated.
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REFERENCE TO RELATED APPLICATIONS
This is a continuation patent application claiming priority of U.S. patent application Ser. No. 11/024,356 entitled “Tactical Duostock”, filed Dec. 28, 2004, now U.S. Pat. No. 7,104,001 which is a continuation patent application claiming priority to U.S. Pat. No. 6,925,743, issued Aug. 9, 2005 (Ser. No. 10/288,999, filed Nov. 6, 2002), the description of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention.
This invention relates to stocks for firearms. More particularly, it relates to the butt stock of firearms used for tactical or combat situations.
2. Prior Art.
Most modern firearms have a stock which is designed for shooting the firearm in a classical shooting position. In the classical shooting position, the butt stock is placed in the shoulder pocket of the shooter. The shooter's shoulders and feet are at approximately a 30° angle to the direction of the firearm and the shooter's head is lowered and forward such that his cheek is firmly on the top of the butt stock and the shooter's dominant eye is aligned with the firearm's sights.
Use of the classical shooting position while in a tactical or close quarter battle (CQB) situation exposes the shooter to additional risk. In a tactical situation, a shooter typically wears body armor which protects the front and back of the torso of the shooter. However, it does not protect the arms of the shooter and, as such, if the shooter is confronting a threat in the classical shooting position the firearm will typically be pointed towards the threat, the shooter will be standing at a 30° angle to the direction of the firearm, and as such a 60° angle to the threat. This exposes the opening in the body armor where the non-dominant arm goes through the body armor. Upper torso wounds from small arms fire in combat can enter through this opening.
Due to this draw back in the classical shooting position, the tactical shooting position is preferred in a CQB situation. In the tactical shooting position, the shooter stands so that his shoulders and feet are perpendicular to the direction of the firearm. The bottom corner of the butt stock is placed against the shooter's dominant side, upper chest at the mid-clavicular line, while the shooter's head is upright and looking forward. The firearm is carried in the ready position until a threat is confronted. In the ready position, the firearm is pointed downward at a 45° angle towards the ground. Once a threat is confronted, the firearm is raised and pointed toward the threat, and the shooter's shoulders and feet are maintained at a perpendicular orientation to the direction of the firearm. With the firearm in the tactical shooting position, the top of the butt stock is against the shooter's dominant side cheek and the shooter's dominant eye is in line with the sights. The tactical shooting position provides the shooter with an optimal amount of protection from the body armor. It also provides the shooter with a better vision for additional threats coming from the non-dominant side of the shooter.
The problem with using the tactical shooting position with the firearm stocks on the market today is that the only point of contact between the firearm and the shooter's torso is the lower corner of the butt stock. This decreases the stability of the firearm and shooter. Another drawback is that this small pointed area of the firearm is placed directly upon the clavicle of the shooter; therefore, any recoil from the firearm is forced into a very small area on the shooter. This increases the discomfort and stiffness of the shooter resulting from this recoil.
Many sporting firearms such as shotguns have a stock where the butt stock is offset at an angle from the barrel. This helps lower the butt plate of the stock so that when shooting in a classical shooting position the butt plate reaches down to the shoulder pocket of the shooter while the sights remain in front of the shooter's dominant eye. Use of an offset angle is helpful when shooting in the classical or tactical shooting position. However, if the shooter must move to a prone shooting position, the use of a stock with a large offset angle causes the shooter to have to raise their head to a higher level in order to place their dominant eye in line with the sights of the firearm. In a CQG situation, this exposes the shooter to additional risk due to the fact that his head is raised.
There are numerous patents for firearm stocks with an adjustable butt stock which allows the shooter to adjust the offset angle. These patents include U.S. Pat. No. 146,651 entitled “Stocks for Fire-Arms” issued to A. R. Byrkit on Jan. 20, 1874; U.S. Pat. No. 843,227 entitled “Jointed Gun Stock” issued to Homer W. Munson on Feb. 5, 1907; U.S. Pat. No. 855,229 entitled “Gun Stock” issued to Patrick H. Clarisey on May 28, 1907; U.S. Pat. No. 1,088,362 entitled “Adjustable Butt Plate for Gun Stocks” issued to John W. Perkins on Feb. 24, 1914; U.S. Pat. No. 1,582,395 entitled “Butt Cap for Guns, Especially for Short Rifles” issued to Rudolf Haemmerli on Apr. 27, 1926; U.S. Pat. No. 1,651,299 entitled “Adjustable Gun Stock” issued to Roy V. Stansel on Nov. 29, 1927; U.S. Pat. No. 5,010,676 entitled “Hand Guard for Firearms,” issued to Paul Kennedy on Apr. 30, 1991; and U.S. Pat. No. 5,779,098 entitled “Recoil Absorber and Redirector Mechanism for Gun Stock” issued to Jay. P. Griggs on Nov. 9, 1999. However, these devices require that the shooter adjust the stock to one setting for a classical or tactical shooting position. They must then readjust the stock again for a prone shooting position. In a combat situation, the shooter must rapidly move from one firing position to another. This may entail changing from a tactical shooting position to prone shooting position or vice versa. As such, the shooter does not have time when changing firing positions to adjust or readjust a stock in order to obtain optimum performance from the firearm.
U.S. Pat. No. 694,904 (the '904 patent) entitled “Sighting Device for Firearms” issued to William Youlten on Mar. 4, 1902, discloses an adaptor which can be attached to the butt stock of a rifle. This adaptor allows the shooter to operate the firearm from a trench without exposing his head above ground level. The device disclosed in the '904 patent places the firearm above the shooter's head while in use. This differs greatly from the present invention which allows the shooter to shoot from either a classical position, a tactical shooting position or a prone position. The device disclosed in the '904 patent is only useful for firing from a trench and cannot be used for shooting from a classical, tactical or prone shooting position.
U.S. Pat. No. 5,010,676 to Kennedy claims a hand guard or forestock for a firearm. FIG. 1 of Kennedy discloses an AR-15 or M-16. The butt stock of this firearm has a butt plate which appears to have a first and a second surface. The angle between the first and the second surface of the butt plate in Kennedy is nearly straight. The angle between these two surfaces in Kennedy is approximately 170 degrees. The butt plate of the present application has an angle between these two surfaces of less than 155 degrees.
When shooting in the tactical position, the second surface of the butt plate is placed upon the upper chest at the mid-clavicular line of the user. This region of the human body is typically at a 28 degree to 44 degree angle to the vertical. In order for the butt stock to comfortably fit to the user while shooting in a tactical position, the angle of the second surface must be approximately complimentary to the angle of the user's upper chest at the mid-clavicular line, i.e., the angle between the first and second surfaces of the butt plate plus the angle of the upper chest at the mid-clavicular line of the user must add up to approximately 180 degrees. This is necessary so that the second surface of the butt plate can fit comfortably against the upper chest at the mid-clavicular line of the user while the barrel of the firearm is at approximately a 90 degree direction to the first section and a 90 degree angle to the vertical.
When applying the device shown in Kennedy, it suffers from the same shortcomings as that of the other prior art. If the firearm in Kennedy is used in the same manner as the present invention to shoot from a tactical shooting position, the second surface of the butt plate would be resting on the upper chest at the mid-clavicular line of the user. As previously mentioned, this upper chest at the mid-clavicular line is typically from 28 degrees to 44 degrees off of the vertical. With the second surface of the Kennedy device flatly against the upper chest at the mid-clavicular line of the user, the barrel of the firearm would be 18 degrees to 34 degrees above the horizontal. When considering that threats are typically engaged within a 5 to 10 meter range when in a tactical situation such as a SWAT team clearing a house, this would lead to the user shooting well over the head of the threat.
The other option for using the firearm disclosed in Kennedy to shoot from a tactical position would be to have the barrel of the gun approximately on the horizontal. However, this would lead to the same problem as the other prior art. The second surface of the butt plate is not complimentary to the typical range of angles of the mid-clavicle region of a user of approximately 28 to 44 degrees. This in turn causes the user to have to place the bottom corner of the butt stock against the upper chest at the mid-clavicular line, thus causing the recoil from the firearm to go into a very small area of the upper chest at the mid-clavicular line of the user just under that corner of the butt stock. The net result would be little or no improvement over the other prior art of having a single surface butt plate.
As can be seen by the geometric analysis above of using the Kennedy device while shooting from a tactical shooting position, the device does not provide any of the benefits of the present invention. As such, the present invention is not merely a discovery of the optimum or workable ranges and would therefore not be obvious to one skilled in the art.
This is further underscored by the fact that Kennedy does not have any discussion of the design of the butt stock or how it could be used in a manner which would provide the same benefits as the present invention. When Kennedy is reviewed in its entirety, it teaches away from the present invention by requiring the user shooting from a tactical position to either shoot over the head of the threat or shoot with the bottom corner digging into the user's upper chest at the mid-clavicular line.
SUMMARY OF THE INVENTION
Due to the shortcomings of the prior art, it is an objective of the present invention to provide an improved firearm butt stock which can readily be used in a classic shooting position, a tactical shooting position, and a prone shooting position without readjustment of the stock.
Another objective of the present invention is to provide an improved firearm butt stock which has a butt plate with two or more surfaces where one surface is used for shooting from the classical shooting position or the prone position and another one of the surfaces is tailored to provide a more comfortable and stable use of the tactical shooting position.
It is a further objective of the present invention to provide an improved firearm butt stock which has a butt plate with two or more surfaces and that one of those surfaces is adjustable to provide a custom fit of the firearm stock when firing from the tactical shooting position.
Yet another objective of the present invention is to provide a collapsible stock with a butt plate with two or more surfaces. One of those surfaces is used for shooting from the classical shooting position or the prone position and another one of these surfaces of the tactical shooting position. Other objectives, advantages and features of the present invention will be apparent to those skilled in the art following a review of the specifications, drawings and claims of this patent.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 : A side view of a shooter using the classic shooting position.
FIG. 2 : A top view of a shooter using the classic shooting position.
FIG. 3 : A side view of a shooter using the tactical shooting position.
FIG. 4 : A top view of a shooter using the tactical shooting position.
FIG. 5 : A side view of a typical shotgun.
FIG. 6 : A side view of a typical rifle.
FIG. 7 : A side view of a typical rifle equipped with one embodiment of the present invention.
FIG. 8 : A side view of one embodiment of the present invention.
FIG. 9 : A side view of a shooter with a rifle equipped with one embodiment of the present invention in the tactical shooting position.
FIG. 10 : A side view of a shooter with a rifle equipped with one embodiment of the present invention in the prone shooting position.
FIG. 11 : A side view of one embodiment of the present invention.
FIG. 12 : A side view of a rifle equipped with one embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a side view of a shooter 20 holding a firearm 22 in a classical shooting position. FIG. 2 is a top view of a shooter 20 holding a firearm 22 in a classical shooting position. In the classical shooting position, the shoulders 24 and feet 26 of the shooter 20 are at approximately 30 degrees angle to the direction of the firearm 22 . The butt stock 28 of the firearm 22 is held firmly against the shoulder pocket 30 of the shooter 20 . The head 32 of the shooter 20 is leaned forward so that the cheek 34 of the shooter 20 is firmly against the top of the butt stock 28 of the firearm 22 , thus forming a cheek weld between the cheek 34 and the butt stock 28 of the assault right 22 . The dominant eye 36 of the shooter 20 is in line with the sights 38 .
The classical shooting position provides a stable platform from which to shoot. It is well suited for hunting, target shooting and other non-tactical situations; however, it is not the preferred shooting position for tactical or close quarters battle (CQB) situations. The body armor 40 typically used in tactical situations protects the front and back of the shooter's torso 43 . However, the body armor 40 does not protect the dominant or non-dominant arm 44 or 46 of the shooter 22 . This means that if the shooter 20 uses the classic shooting position in a tactical situation, the shooter is increasing his risk of bodily injury by exposing to the threat the unprotected area where the shooter's 20 non-dominant arm 46 attaches to the shooter's20 torso 42 .
The classical shooting position also has the shortcoming in a tactical situation of limited visibility towards the shooter's 20 non-dominant side. While shooting in the classical shooting position the shooter's 20 non-dominant eye 48 typically is closed, also the shooter's torso 42 is turned away from the shooter's non-dominant side. Both of these factors make it difficult for the shooter 20 to detect and confront a threat coming from the shooter's20 non-dominant side.
FIG. 3 shows a side view of a shooter 20 firing a firearm 22 from a tactical shooting position. FIG. 4 shows a top view of a shooter 20 shooting a firearm 22 from the tactical shooting position. The firearm 22 is held in the ready position shown in dash lines in FIG. 3 until a threat is confronted. In the ready position, the firearm 22 is held at a 45 degree angle pointing toward the ground. The butt stock 28 of the firearm 22 is held against the mid-clavicular line 50 . Once the threat is confronted, the firearm 22 is rotated to a position perpendicular to the body of the shooter 20 . The firearm 22 is rotated about the point of contact between the butt stock 28 and the mid-clavicular line 50 of the shooter 20 . The shoulder 24 and feet 26 of the shooter 20 are perpendicular to the firearm 22 . The head 32 of the shooter 20 is in an upright and forward facing position. A cheek weld is established by having the top of the butt stock 28 firmly against the cheek 34 of the shooter 20 . The dominant eye 36 of the shooter 20 is in line with the sights 38 of the firearm 22 .
As best seen in FIG. 3 , the mid-clavicular line 50 of the chest of the shooter 20 is at an angle. Therefore, when the tactical shooting position is used with a firearm 22 with a prior art butt stock 28 , only the lower rear corner of the butt stock 28 is resting against the shooter's 200 mid-clavicle 50 . When the firearm 22 is fired, this small area of contact must absorb all of the recoil generated by the firearm 22 .
It is also important to note the angle of the mid-clavicular line 50 of the chest can vary greatly from individual to individual. This variation and angle is largely due to differences in the development of the pectoralis muscles in the chest of the individual. This angle can typically range from 28° to 44°. The shooter 20 must use this small area of the mid-clavicular line 50 of the chest to steady the firearm 22 .
Many firearms such as the shotgun 52 shown in FIG. 5 have a stock where the butt stock 54 has an offset angle 56 . This helps raise the sights 58 such that when the firearm is shouldered the sight 58 are in front of the shooter's 20 dominate eye 36 while allowing the rear surface of the butt stock or butt plate 60 to be low enough to engage the shoulder of the shooter.
FIG. 6 shows a firearm 22 typically known as the M16 or AR15. This is the same firearm seen in FIGS. 1 through 4 . It should be noted that the butt stock 28 of the firearm 22 does not have a stock offset angle such as the shotgun 52 shown in FIG. 5 , rather the butt stock 28 of the firearm 22 extends directly back from the receiver 62 .
FIG. 7 shows a firearm 22 equipped with one embodiment of the present invention, an improved butt stock, the tactical duo stock 66 . FIG. 8 is a side view of the embodiment of duo stock 66 which is shown attached to the firearm 22 in FIG. 7 . FIG. 9 shows a shooter 20 holding a firearm 22 in the tactical shooting position. The firearm 22 is equipped with the same embodiment of the tactical duo stock 66 as shown in FIGS. 7 and 8 . The forward end 68 of the duo stock 66 is constructed to attach to the firearm 22 . It will be apparent to those skilled in the art that the forward end 68 of the duo stock 66 can be adapted to many different forms in order to attach various different rifles, shotguns, and other firearms. The duo stock 66 also has a butt plate 70 . The back end 70 is made up of an upper section 72 and a lower section 74 . The butt plate 70 could be comprised of a separate plate attached to the rear of the duo stock 66 or it could be the rear surface of the duo stock 66 without any separate pieces being attached to the duo stock 66 .
The butt plate angle 76 and the offset angle 78 are shown in FIG. 8 . The preferred butt plate angle is 145°, however, this angle could vary from 135° to 155°. Likewise, the preferred offset angle 78 for the duo stock 66 is 35°, however, this could vary from a range of 25° to 45°.
While in the tactical shooting position as shown in FIG. 9 , the lower section 74 of the butt plate 70 rests against the mid-clavicular line 50 of the shooter 20 . Because the surface of the lower section 74 is generally parallel with the mid-clavicular line 50 of the shooter 20 , any force from the recoil of the firearm 22 is spread across the area directly underneath the lower section 74 . This is an improvement over the prior art butt stock 28 , as shown in FIGS. 1-4 and 6 . When that butt stock 28 is used in the tactical shooting position, the force from the recoil of the firearm 22 is directed through the lower corner of the butt stock 28 and against a much smaller area of the mid-clavicular line 50 of the shooter 20 . This increased area of impact created by use of the tactical duostock 66 helps soften the impact of the recoil allowing for faster follow up shots as well as reduced soreness and stiffness of the shooter 20 .
This increased area of contact between the firearm 22 and the shooter 20 , due to the use of the duostock 66 also provides a more stable shooting platform. This in turn increases the comfort, speed, and accuracy of the shooter 20 's performance.
FIG. 10 shows a shooter 20 holding a firearm 22 in a prone position. The firearm 22 is equipped with a tactical duostock 66 . In the prone position, the upper section 72 of the duostock 66 rests against the shoulder of the shooter 20 as with any conventional stock.
FIG. 11 shows a second embodiment of the tactical duostock 66 . In the second embodiment, the duostock 66 has an adjustable lower section 74 . The lower section 74 is pivotally attached to the upper section 72 and/or the body 80 of the duo stock. As shown in FIG. 11 , there is a hinge 82 which creates the pivotal attachment for the lower section 74 . With the adjustable lower section 74 , the butt plate angle 76 can be adjusted to fit the angle of the mid-clavicular line 50 of the individual shooter 20 . This means a better fit for the shooter 20 while using the duostock 66 in a tactical shooting position.
Once the butt plate angle 76 has been adjusted to fit the individual shooter 20 , it can be used like the other embodiments of the duostock 66 , allowing the shooter 20 to move from a prone or classical shooting position to a tactical shooting position, or vice versa, without readjusting the butt plate angle 76 .
The adjustable lower section 74 has a plate 86 which is attached to it. The plate 86 runs alongside the body 80 . There is a slot 88 in the plate 88 through which the lock 84 passes. The adjustable lower section 74 is held in place relative to the upper section 72 and the body 80 by the lock 84 holding the plate 86 in place. The embodiment shown in FIG. 11 uses a cammed lock. However, those skilled in the art could adapt the present invention to use any of a number of locks known in the art.
FIG. 12 shows a firearm 22 equipped with a collapsible stock well known in the art. The collapsible stock is equipped with the duostock 66 . The butt plate 70 of the collapsible stock has the upper section 72 and a lower section 74 at an angle to the upper section 72 . The present invention works the same with the collapsible stock as it does with the other embodiments of the invention. It should be noted that the embodiment of the present invention shown in FIG. 12 could be adapted to incorporate the adjustable butt plate feature shown in FIG. 11 .
The foregoing specifications and drawings are only illustrative of the preferred embodiments of the present invention. They should not be interpreted as limiting the scope of the attached claims. Those skilled in the arts will be able to come up with equivalent embodiments of the present invention without departing from the spirit and scope thereof.
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A butt stock for a tactical weapon, rifle, shotgun or other firearm. The butt stock has a butt plate with two or more surfaces. One of those surfaces is generally perpendicular to the direction of the firearm. The other surface is angled to provide a more stable shooting platform for the firearm as well as more comfortable use of the firearm in a tactical shooting position.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of Ser. No. 12/346,256, filed Dec. 30, 2008, now U.S. Pat. No. 8,621,708, issued Jan. 7, 2014, which is a divisional application of Ser. No. 11/276,167, filed Feb. 16, 2006, now U.S. Pat. No. 7,784,148, which claims the benefit of U.S. Provisional Patent Application No. 60/593,829, filed Feb. 17, 2005, and U.S. Provisional Patent Application No. 60/743,153, filed Jan. 20, 2006, all of which are incorporated herein by reference in their entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a surface cleaning apparatus that fluid cleaning system to deliver heated cleaning fluid to a surface to be cleaned. In one of its aspects, the invention relates to a surface cleaning apparatus that has an inline heater to heat cleaning fluid.
2. Description of the Related Art
Extractors are well-known devices for deep cleaning carpets and other fabric surfaces, such as upholstery. Most carpet extractors comprise a fluid delivery system and a fluid recovery system. The fluid delivery system typically includes one or more fluid supply tanks for storing a supply of cleaning fluid, a fluid distributor for applying the cleaning fluid to the surface to be cleaned, and a fluid supply conduit for delivering the cleaning fluid from the fluid supply tank to the fluid distributor. The fluid recovery system usually comprises a recovery tank, a nozzle adjacent the surface to be cleaned and in fluid communication with the recovery tank through a working air conduit, and a source of suction in fluid communication with the working air conduit to draw the cleaning fluid from the surface to be cleaned and through the nozzle and the working air conduit to the recovery tank. An example of an extractor is disclosed in commonly assigned U.S. Pat. No. 6,131,237 to Kasper et al., which is incorporated herein by reference in its entirety. The Kasper et al. '237 includes an aluminum body that includes a cover made of aluminum and further includes a fluid inlet fitting and a fluid outlet fitting connected to the metal body for circulating fluid through the metal body. Corrosion may be a problem resulting from casting the fluid inlet and fluid outlet fittings into the metal heater block. This problem might be overcome the use screw-in fittings with an O-ring rather than casting the fittings into the block. This solution may reduce the corrosion problem but may also add significant cost in that the block is required to be tapped and a hand assembly is required for threading the fittings into the tapped holes. Further, the metal cover may have to be Teflon coated to avoid corrosion problems.
The U.S. Patent Application Publication No. 2004/0197095 to Thweatt, Jr. discloses a heater for fluids including a housing made of non-metallic material and having an internal cavity and an inlet and an outlet in fluid communication with the internal cavity. The heater housing is made of a polymeric material. A heating element is suspended within the cavity for heating fluid flowing therethrough. Further, the heating element comprises a U-shaped portion and electrical connectors at opposite ends of the heating element which extend through the housing. Thweatt, Jr. '095 has fluid inlet and outlet fittings mounted to the heating element in an end wall of the plastic housing. The heating element may melt the walls of the plastic housing when the housing is dry, regardless of the existence of a thermal cutoff control.
SUMMARY OF THE INVENTION
A surface cleaning apparatus according to the invention comprises a housing, a fluid delivery system mounted to the housing and including a fluid supply chamber for holding a supply of cleaning fluid, a fluid dispenser for applying cleaning fluid from the fluid supply chamber to the surface to be cleaned, and a fluid supply conduit between the fluid supply chamber and the fluid dispenser. The apparatus further comprises a fluid recovery system mounted to the housing and including a suction nozzle and a vacuum source in fluid communication with the suction nozzle to draw dispensed fluid from the surface to be cleaned through the suction nozzle.
According to one embodiment of the invention, the apparatus further comprises an in-line fluid heater comprising a metal body with an embedded heating element and a polymeric cover with a fluid inlet fitting and a fluid outlet fitting connected in-line with the fluid supply conduit.
In another embodiment of the invention, the fluid inlet and outlet fittings of the heater are integrally molded with the cover.
In yet another embodiment of the invention, the metal body of the heater forms a fluid channel having an open upper end, and the cover closes the open upper end of the fluid channel to form a closed fluid channel in the fluid heater.
According to yet another embodiment of the invention, the heater cover is secured to the body of the heater with mechanical fasteners and a gasket located between the cover and the body.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a rear, left perspective view of an extractor according to the invention with a handle assembly pivotally mounted to a foot assembly.
FIG. 2 is a schematic view of a fluid delivery system for the extractor of FIG. 1 .
FIG. 3 is a top view of a heater for use with the fluid delivery system of FIG. 2 .
FIG. 4 is a sectional view taken along line 4 - 4 of FIG. 3 .
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings and particularly to FIG. 1 , an upright extractor 10 according to the invention comprises a housing having a foot assembly 12 for movement across a surface to be cleaned and a handle assembly 14 pivotally mounted to a rearward portion of the foot assembly 12 for directing the foot assembly 12 across the surface to be cleaned. The extractor 10 includes a fluid delivery system for storing cleaning fluid and delivering the cleaning fluid to the surface to be cleaned and a fluid recovery system for removing the spent cleaning fluid and dirt from the surface to be cleaned and storing the spent cleaning fluid and dirt. The components of the fluid delivery system and the fluid recovery system are supported by at least one of the foot assembly 12 and the handle assembly 14 . Details of the extractor 10 are more fully described in parent U.S. Patent Application Publication No. 2009/0101187, filed Dec. 30, 2008, entitled “Surface Cleaning Apparatus with Cleaning Fluid Supply”, which is incorporated herein by reference in its entirety.
The foot assembly 12 comprises a base assembly 20 that supports a recovery tank assembly 22 at a forward portion thereof and a solution supply tank assembly 24 at a rearward portion thereof. Further, a nozzle assembly 340 is removably mounted to a forward portion of the base assembly 20 .
Referring to FIGS. 1 and 2 , the extractor 10 comprises the fluid recovery system for removing the spent cleaning fluid and dirt from the surface to be cleaned and storing the spent cleaning fluid and dirt. The nozzle assembly 340 forms a portion of the fluid flow path, the opening of which is positioned adjacent a surface to be cleaned. When the nozzle assembly 340 and the recovery tank assembly 22 are mounted to the base assembly 20 , a continuous working air path is formed through the nozzle assembly 340 and the recovery tank assembly 22 . A vacuum is drawn on the recovery tank assembly 22 and nozzle assembly 340 by a motor and fan assembly 228 to draw spend cleaning fluid from the surface to be cleaned.
The solution supply tank assembly 24 is removably mounted to the base assembly 20 . The solution supply tank assembly 24 comprises a solution supply tank housing 150 that defines a solution supply chamber (not shown). The solution supply tank housing has outlet 156 in a bottom wall thereof. The outlet 156 receives a valve mechanism 158 for controlling flow of fluid from the solution supply chamber 152 . Spray tips 218 are in fluid communication with solution supply chamber 152 so that the fluid can be supplied from the spray tips 218 to the surface to be cleaned.
As mentioned above, the extractor 10 comprises the fluid delivery system for storing the cleaning fluid and delivering the cleaning fluid to the surface to be cleaned. For visual clarity, the various electrical and fluid connections within the fluid delivery system are not shown in the drawings described above but are depicted schematically in FIG. 2 . Referring now to FIG. 2 , the fluid delivery system comprises a bladder 44 for storing a first cleaning fluid and the solution supply tank housing 150 of the solution supply tank assembly 24 for storing a second cleaning fluid. The first and second cleaning fluids are dispensed from the bladder 44 and the solution supply tank housing 150 through respective valve mechanisms 48 , 158 , which are received by respective valve seats (not shown) when the recovery tank assembly 22 and the solution supply tank assembly 24 , respectively, are mounted to the base assembly 20 . The first cleaning fluid flows from the bladder 44 and through a heater 680 , which heats the first cleaning fluid when the heater 680 is activated through a heater switch 388 , to a mixing manifold 510 . The mixing manifold 510 forms a conduit for the first cleaning fluid between a first fluid inlet 510 A and an outlet 510 B and also includes two second cleaning fluid inlets 510 C, 510 D. The second cleaning fluid inlets 510 C, 510 D fluidly communicate with the conduit for the first cleaning fluid in a mixing chamber 510 E. The heater 680 can heat fluids and is preferably an in-line heater. Exemplary valve mechanisms and heaters are disclosed in U.S. Pat. No. 6,131,237 and U.S. patent application Ser. No. 60/521,693, which are incorporated herein by reference in their entirety.
In operation, when a user depresses a fluid trigger 460 on the handle assembly 14 , a trigger switch 462 opens a spray tip valve 224 to deliver cleaning fluid to the spray tips 218 for dispensation onto the surface to be cleaned.
The heater 680 for heating the cleaning fluid is illustrated in FIGS. 3 and 4 . The heater 680 is similar to the heater disclosed in the aforementioned and incorporated U.S. Pat. No. 6,131,237 in that the heater 680 comprises a metallic body 682 , such as an aluminum body, that forms a serpentine fluid channel 684 with an open upper end and houses a heating element 686 . The heater 680 further comprises a polymeric cover 688 mounted to the body 682 by mechanical fasteners 690 , such as screws, with a gasket 692 therebetween. The cover 688 comprises a fluid inlet port 694 and a fluid outlet port 696 , which are preferably integrally molded with the cover 688 . When the cover 688 is mounted to the body 682 , the cover 688 closes the open upper end of the fluid channel 684 , and the fluid inlet port 694 and the fluid outlet port 696 provide an inlet and an outlet, respectively, to the fluid channel 684 . During operation, the cleaning fluid flows through the fluid inlet port 694 into the fluid channel 684 and exits the fluid channel 684 through the fluid outlet port 696 . As the cleaning fluid flows through the fluid channel 684 , heat from the heating element 686 conducts through the body 682 and to the cleaning fluid to thereby heat the cleaning fluid.
The hybrid heater 680 according to the invention uses a metal block (body 682 ) with an embedded heating element 686 for efficient heat transfer but eliminates a metal cover and integrally forms the inlet and outlet ports 694 , 696 with the plastic cover 688 . Thus, the invention avoids the corrosion problems of the prior art while maintaining the heat transfer properties of the prior art and eliminates expensive machining operations, hand assembly and Teflon coating of the cover. The metal body 682 with the embedded heating element 686 stores heat energy and gives a thermal sensor the time to react. Thus, the invention involves the combination of a plastic cover that mounts the inlet and outlet ports 694 , 696 , preferably by integral molding.
The various features of the extractor 10 described here are not limited for use in an upright extractor. Rather, the features can be employed for any suitable surface cleaning apparatus, including, but not limited to, hand-held extractors, canister extractors, upright and canister vacuum cleaners, shampooing machines, mops, bare floor cleaners, and the like.
While the invention has been specifically described in connection with certain specific embodiments thereof, it is to be understood that this is by way of illustration and not of limitation. Reasonable variation and modification are possible within the scope of the forgoing description and drawings without departing from the spirit of the invention which is defined in the appended claims.
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A surface cleaning apparatus comprises a fluid delivery system including a supply of cleaning fluid stored in a fluid supply chamber and a fluid recovery system for drawing dirty cleaning fluid using suction from the surface to be cleaned. The apparatus has an inline fluid heater having a metal body with an embedded heating element and a polymeric cover provided with a fluid inlet fitting and a fluid outlet fitting. The fluid inlet and fluid outlet fittings are preferably integrally molded with the polymeric cover.
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CROSS-REFERENCES TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application Ser. No. 61/277,246 filed on Sep. 23, 2009 which is incorporated herein by reference in its entirety for all that is taught and disclosed therein.
BACKGROUND
Technical Field
This disclosure relates to a multi-function tool, and more particularly, a multi-function tool for driving fasteners such as bolts and nuts, and any type of machine or wood screw and the like. The multi-function tool includes an extendible and a retractable shaft that can be extended in an offset position with respect to the handle as well as a retracted position in a centerline position with respect to the handle.
When inserting or removing a fastener with a hand tool into or out from a work piece, a workman's efficiency is limited by the ability of the tool to translate mechanical force exerted by his hand to the fastener through rotary movement. For example, a tool, such as a conventional screwdriver or wrench having a fixed handle mounted to a straight shaft, imposes a physical limitation on the workman, allowing him to utilize only the torque which he can exert through his hand by the twisting of his wrist. Additionally, because the wrist cannot rotate completely about a circle, to complete a full cycle of rotation with a conventional hand tool, the workman must periodically release his grip on the handle of the tool, rotate his hand back to a starting position and re-grip the tool handle to continue applying force. A tool utilizing an offset shaft from the handle that rotates freely within the handle, commonly called a twirly or a whirlybird, allows the workman to continuously grip the tool and move the handle of the tool in a continuous circle as the tip acts against the fastener. Unfortunately, when a shaft is offset and rotates freely off of the centerline axis, it restricts the amount of force or torque that can be exerted, thus failing to generate an equivalent force of a standard centerline screwdriver or wrench. Attempts have been made to provide rotary tools permitting better translation of the workman's exertions. However, none of the rotary tools currently known allow the workman to change positions of the shaft in relation to the centerline axis of the handle and an offset position with a motion completed with the same hand, either the right hand or the left hand.
SUMMARY
This Summary is provided to introduce in a simplified form a selection of concepts 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 to limit the scope of the claimed subject matter.
This disclosure is directed in one embodiment to a multi-function tool having the ability to offset the shaft connected to a handle and rotate freely in either a clockwise or counterclockwise direction. The shaft of the tool can retract or extend into and out of a handle by means of a movable button or lever. The movable button or lever allows the shaft to extend from one end of the handle and become offset from a centerline position of the handle, and to retract back inside the end of the handle to realign the shaft with the centerline of the handle. The movable button or lever may be activated manually or spring loaded in an otherwise automatic or semi-automatic mechanical operation. In the retracted position in the handle, a ratchet mechanism or a gearbox can restrict shaft rotation in either a clockwise or counterclockwise direction, or allow free rotation in either direction.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
FIG. 1A shows a perspective view of an embodiment of the multi-function tool.
FIG. 1B shows a top view of an embodiment of the multi-function tool.
FIG. 1C shows a side view of an embodiment of the multi-function tool.
FIG. 1D shows an end view of an embodiment of the multi-function tool.
FIG. 2 shows an exploded view of an embodiment of the multi-function tool.
FIG. 3A shows a partial view of the head end of the multi-function tool in a retracted position in an embodiment of the invention.
FIG. 3B shows a partial view of the head end of the multi-function tool in an extended and offset position in an embodiment of the invention.
FIG. 4 shows a detailed view of the movable arms assembly in an embodiment of the invention.
FIG. 5A shows several screwdriver bits utilized in an embodiment of the invention.
FIG. 5B shows several hollow nut driver bits utilized in an embodiment of the invention.
DETAILED DESCRIPTION
Referring now to the Figures, like reference numerals and names refer to structurally and/or functionally similar elements thereof, and if objects depicted in the figures that are covered by another object, as well as the tag line for the element number thereto, may be shown in dashed lines. FIGS. 1A , 1 B, 1 C, and 10 show a perspective view, a top view, a side view, and an end view respectively, and FIG. 2 shows an exploded view, of an embodiment of the multi-function tool. Referring now to FIGS. 1A-1D , and FIG. 2 , Multi-Function Tool 100 has a Top Housing 1 and a Bottom Housing 2 . When assembled together, Top Housing 1 and a Bottom Housing 2 have a shaped handle and belly that fit the form of either hand, feels comfortable, and is easy to grip with a mass of the handle that fits the palm of either hand. Pointer Finger Choil 3 and Middle Finger Choil 4 enhance a grip position for applying maximum torque. Storage Door 5 is hinged on one end and has a bendable clip on the other end that locks in place in the base of Top Housing 1 and a Bottom Housing 2 . Storage Area 6 is formed by Top Housing 1 , Bottom Housing 2 , and Storage Door 5 . Within Storage Area 6 standard Screwdriver Bits 47 (see FIG. 5A ) and Hollow Nut Driver Bits 48 (see FIG. 5B ) may be stored that fit into to Hex Holder Tip 22 . Screwdriver Bits 47 may be different types, such as flat head or Phillips head, and may be various sizes. Hollow Nut Driver Bits 48 may also be of different types and sizes. Multi-Function Tool 100 may be built in different sizes to accommodate various sizes of bits.
Top Slide Shaft 7 and Bottom Slide Shaft 8 mate together and are secured through Slide Barrel 9 with C-Clip 10 at their ends. Slide Button 11 abuts Ring 12 of Slide Barrel 9 . Pawl 13 , Spur Barrel 14 , Ratchet Rings 15 (which mate together to form a unitary ratchet ring), Washer 16 , Tab 17 , and Ratchet Spring 43 form a standard ratchet mechanism familiar in the art. Pawl 13 has two teeth that face in opposite directions. These teeth engage the spurs on Spur Barrel 14 . Tab 17 is contained inside Ratchet Rings 15 with Ratchet Spring 43 that pushes Tab 17 down against Pawl 13 . When Ratchet Rings 15 are in a middle position, Tab 17 pushes down against the middle of Pawl 13 so that both teeth engage the spurs on Spur Barrel 14 , locking it into place. When Ratchet Rings 15 are rotated to either side, Tab 17 pushes on the edge of Pawl 13 so that only one tooth engages Spur Barrel 14 . This allows Spur Barrel 14 to rotate in one direction but not the other, which enables the ratchet feature in the two directions indicated by Arrow 19 .
Thumb Nubs 18 on Ratchet Rings 15 allow the workman to change the clockwise or counter clockwise direction of the shaft spin without changing the workman's grip on the handle. While the workman grasps Multi-Function Tool 100 with his hand, with the pointer and middle fingers engaged with Pointer Finger Choil 3 and Middle Finger Choil 4 , the workman, with using only the thumb of the hand grasping Multi-Function Tool 100 , can engage Thumb Nubs 18 with the thumb and rotate Ratchet Rings 15 in the transverse direction to Centerline 44 shown by Arrow 19 . In the same fashion, the workman with using only the thumb of the hand grasping Multi-Function Tool 100 can move Slide Button 11 in the parallel direction to Centerline 44 shown by Arrow 20 . In FIGS. 1A-1D , Multi-Function Tool 100 is shown in a partially extended position but not offset. FIG. 3A shows Multi-Function Tool 100 in the retracted position. FIG. 3B shows Multi-Function Tool 100 in the extended and offset position. In FIG. 1B , Slide Button 11 as shown would represent Multi-Function Tool 100 in the retracted position as shown in FIG. 3A . When Slide Button 11 is pushed forward to the Slide Button Phantom Position 11 ′ shown in FIG. 1B , Multi-Function Tool 100 would be in the extended and offset position as shown in FIG. 3B . In FIGS. 3A and 3B , Covers 24 are not shown.
Collar 21 provides an opening that allows Movable Arms Assembly 23 which are attached to Hex Holder Tip 22 to extend out from Top Housing 1 and Bottom Housing 2 to the extended and offset position shown in FIG. 3B . A pair of Covers 24 are secured to Movable Arms Assembly 23 by their pins that pass through Holes 46 . The shape and curvature of Covers 24 help assist the smooth extension and retraction of Movable Arms Assembly 23 in and out from Collar 21 .
FIG. 4 shows a detailed view of Movable Arms Assembly 23 . Referring now to FIG. 4 , in one embodiment, each arm of Movable Arms Assembly 23 is comprised of a number of individual layers: Outer Layers 25 , Intermediate Layers 26 , and Inner Layer 27 . Each assembled arm is a mirror image of the other. As can be seen in FIG. 4 , a Channel 28 is formed by the individual layers which accommodates Eyelet 29 and Eyelet 30 when Movable Arms Assembly 23 is in the extended and offset position as shown in FIG. 3B . In another embodiment, each arm of Movable Arms Assembly 23 is machined from a solid part. Regarding the various parts that make up Multi-Function Tool 100 , one skilled in the art will recognize that the parts may be made of combinations of one or more of injection molded plastic, injection molded nylon, machined metals, die cast aluminum and aluminum alloys, stamped steel, forged and drilled carbon steel with nickel coating, extruded steel, and the like. One material may be substituted for another depending upon specific design criteria and the intended use or application.
Referring back to FIG. 2 , Shaft Pins 31 secure one end of Movable Arms Assembly 23 to Top Slide Shaft 7 and Bottom Slide Shaft 8 through Holes 32 . Tip Pins 33 secure the other end of Movable Arms Assembly 23 to Hex Holder Tip 22 through Holes 34 . Center Pins 35 fit in Holes 36 and are flush with the outer surfaces of Outer Layers 25 . Shaft Pins 31 and Tip Pins 33 extend from the outer surfaces of Outer Layers 25 and are slightly smaller in diameter than Holes 32 and Holes 34 allowing Movable Arms Assembly 23 to rotate freely about Shaft Pins 31 and Tip Pins 33 with respect to Top Slide Shaft 7 and Bottom Slide Shaft 8 and Hex Holder Tip 22 .
Tail Spring Pin 37 fits in Holes 38 of Top Slide Shaft 7 and Bottom Slide Shaft 8 . One end of Tail Spring 39 wraps around Tail Spring Pin 37 , and the other end of Tail Spring 39 is secured to Eyelet 30 . Head Spring Pin 40 fits in Holes 41 of Hex Holder Tip 22 . One end of Head Spring 42 wraps around Head Spring Pin 40 , and the other end of Head Spring 42 is secured to Eyelet 29 . Due to the offset nature of the attachment of Tail Spring 39 and Head Spring 42 , to Top Slide Shaft 7 /Bottom Slide Shaft 8 and Hex Holder Tip 22 , tension is applied to each member of Movable Arms Assembly 23 . As Slide Button 11 is engaged by the workman's thumb and is slid in a forward direction indicated by Arrow 20 , Movable Arms Assembly 23 begins to extend from the retracted position shown in FIG. 3A towards the extended and offset position shown in FIG. 3B . Once the tips of Top Slide Shaft 7 /Bottom Slide Shaft 8 extend far enough out from Collar 21 , the tension provided by Tail Spring 39 and Head Spring 42 cause Movable Arms Assembly 23 top snap from a straight position to the extended and offset position shown in FIG. 3B , rotating freely about Shaft Pins 31 and Tip Pins 33 . When the workman slides Slide Button 11 in a backward direction indicated by Arrow 20 , Movable Arms Assembly 23 will return to the retracted position shown in FIG. 3A . One skilled in the art will recognize that leaf springs may be substituted for Tail Spring Pin 37 and Head Spring Pin 40 . Other mechanisms for biasing Movable Arms Assembly 23 with respect to Top Slide Shaft 7 /Bottom Slide Shaft 8 and Hex Holder Tip 22 are within the scope of this disclosure. In other embodiments of the invention, Movable Arms Assembly 23 may consist of a single arm with a single spring.
The manner of utilizing Multi-Function Tool 100 in one embodiment can be described as follows. A workman desires to remove a Phillips head screw from a work piece. The workman places a Phillips head screwdriver bit in Hex Holder Tip 22 . The workman grasps Multi-Function Tool 100 with one hand and slides Slide Button 11 with the workman's thumb to place Multi-Function Tool 100 in the retracted position as shown in FIG. 3A (if not already in the retracted position). The workman next manipulates Thumb Nubs 18 with the workman's thumb to move Ratchet Rings 15 into the middle position (if not already in the middle position), which locks the ratchet mechanism from turning. The workman then engages the screwdriver bit with the screw and then turns Multi-Function Tool 100 with his hand in a counterclockwise direction, allowing the workman to exert the torque needed to break the screw loose from the work piece.
The workman next manipulates Slide Button 11 with his thumb in a forward direction indicated by Arrow 20 to move Movable Arms Assembly 23 to the extended and offset position shown in FIG. 3B . In the extended and offset position, Pawl 13 becomes disengaged from the spurs of Spur Barrel 14 , which now allows Top Slide Shaft 7 /Bottom Slide Shaft 8 , Movable Arms Assembly 23 , and Hex Holder Tip 22 to freely rotate clockwise or counterclockwise in the directions indicated by Arrow 19 with respect to Offset Centerline 45 . Thus, Multi-Function Tool 100 now behaves like an offset screwdriver commonly called a twirly or a whirlybird. Offset screwdrivers work like a single bike pedal. Turning the whirlybirds handle like a pedal will turn the tip and the screw. The workman may now rapidly move the handle portion of Multi-Function Tool 100 in a counterclockwise direction, rotating about Offset Centerline 45 , to speedily remove the screw from the work piece. In one embodiment of the invention, Centerline 44 and Offset Centerline 45 are parallel to each other. After the screw is engaged with the Phillips head screwdriver bit, all of the above steps beyond that point are accomplished with either the right hand alone or the left hand alone and without removing the screwdriver bit from the screw.
The manner of utilizing Multi-Function Tool 100 in another embodiment can be described as follows. A workman desires to drive a hex head bolt into a work piece. The workman places a hollow nut driver bit of the desired size in Hex Holder Tip 22 . The workman grasps Multi-Function Tool 100 with one hand and slides Slide Button 11 with the workman's thumb to place Multi-Function Tool 100 in the retracted position as shown in FIG. 3A (if not already in the retracted position). The workman next manipulates Thumb Nubs 18 with the workman's thumb to move Ratchet Rings 15 into the middle position (if not already in the middle position), which locks the ratchet mechanism from turning. The workman then turns Multi-Function Tool 100 with his hand in a clockwise direction, allowing the workman to exert the torque needed to begin driving the bolt into the work piece. The workman next manipulates Slide Button 11 with his thumb in a forward direction indicated by Arrow 20 to move Movable Arms Assembly 23 to the extended and offset position shown in FIG. 3B . In the extended and offset position, Pawl 13 becomes disengaged from the spurs of Spur Barrel 14 , which now allows Top Slide Shaft 7 /Bottom Slide Shaft 8 , Movable Arms Assembly 23 , and Hex Holder Tip 22 to freely rotate clockwise or counterclockwise in the directions indicated by Arrow 19 with respect to Centerline 44 . Thus, Multi-Function Tool 100 now behaves like an offset screwdriver commonly called a twirly or a whirlybird. The workman may now rapidly move the handle portion Multi-Function Tool 100 in a clockwise direction about Offset Centerline 45 to speedily drive the bolt into the work piece. Once snug, the workman can manipulate Slide Button 11 in a backwards direction to move Movable Arms Assembly 23 into the retracted position. The workman then manipulates Thumb Nubs 18 to lock the ratchet mechanism to provide torque in the clockwise direction, and allow free turning in the counterclockwise direction. The workman may now rotate Multi-Function Tool 100 with his hand in a clockwise rotating manner to fully tighten the bolt into the work piece. After the bolt is engaged with the hollow nut driver bit, all of the steps beyond this point are accomplished with one hand and without removing the hollow nut driver bit from the bolt.
Although the subject matter has been described in language specific to structural features and/or methodological acts, it is to be understood that the subject matter defined in the appended claims is not necessarily limited to the specific features or acts described above. Rather, the specific features and acts described above are disclosed as example forms of implementing the claims. It will be understood by those skilled in the art that many changes in construction and widely differing embodiments and applications will suggest themselves without departing from the scope of the disclosed subject matter.
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A multi-function tool includes an extendible and retractable portion that becomes offset from a centerline position of the handle when in the offset position. A locking mechanism allows the workman to offset the shaft from a centerline position of the handle, or retract the shaft back into the handle into a centerline position. While the shaft is in the extended and offset position, the shaft rotates freely in either a clockwise or counterclockwise direction. When the shaft is retracted in the straight centerline position, a ratchet mechanism or gear box restricts shaft rotation in either a clockwise or counterclockwise direction, or allows rotation in either direction. The shaft can be extended and offset by means of a spring or other device that allows the locking mechanism to offset automatically or semi-automatically when the locking mechanism is activated. The shaft allows the workman to interchange bits or sockets for multiple applications.
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