Utilizing Phosphoric Acid Or Its Anhydride As Reactant Patents (Class 423/309)
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Patent number: 5443808Abstract: The invention relates to a method for producing alkali metal phosphate, in particular monopotassium phosphate or its aqueous solution, by reacting fertilizer-grade phosphoric acid with alkali metal chloride at 350.degree. . . . 700.degree. C. to produce alkali metal metaphosphate, hydrolyzing thus obtained solid reaction product, removing the insoluble residue containing impurities from the hydrolysis solution in order to achieve a pure solution of alkali metal phosphate, and if further desired, crystallizing and separating the alkali metal phosphate from said aqueous solution.Type: GrantFiled: December 12, 1994Date of Patent: August 22, 1995Assignee: Kemira OyInventors: Stig-Goran A. Weckman, Robert Perander, Sakari Riihmaki
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Patent number: 5427755Abstract: In the process for the preparation of dicalcium phosphate dihydrate, which has a good compatibility with fluorine and stability to hydrolysis and causes the minimum possible after-thickening when used in tooth-pastes, by reaction of calcium carbonate suspended in water with an aqueous solution of orthophosphoric acid, precipitation of dimagnesium phosphate trihydrate, as a stabilizer, by reaction of aqueous solutions of a magnesium salt and of orthophosphoric acid in the presence of a basic compound and final filtration, drying and grinding of the precipitate, 0.2 to 0.8% by weight of polyphosphoric acid, calculated with respect to the dicalcium phosphate dihydrate precipitated in the reaction mixture, is added to the reaction mixture as a further stabilizer.Type: GrantFiled: February 17, 1994Date of Patent: June 27, 1995Assignee: Hoechst AktiengesellschaftInventors: Franz-Josef Dany, Gerhard Kalteyer, Gerhard Nolte, Hedwig Prell
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Patent number: 5427756Abstract: In the process for the preparation of dicalcium phosphate dihydrate, which has a good compatibility with fluorine and stability to hydrolysis and causes the minimum possible after-thickening when used in toothpastes, by reaction of calcium carbonate suspended in water with an aqueous solution of orthophosphoric acid, precipitation of dimagnesium phosphate trihydrate, as a stabilizer, by reaction of aqueous solutions of a magnesium salt and of orthophosphoric acid in the presence of a basic compound and subsequent addition of tetrasodium pyrophosphate to the reaction mixture as a further stabilizer and final filtration, drying and grinding of the precipitate, 0.2 to 0.6% by weight of tetrasodium pyrophosphate, calculated with respect to the dicalcium phosphate dihydrate precipitated in the reaction mixture, is added to the aqueous reaction mixture.Type: GrantFiled: February 7, 1994Date of Patent: June 27, 1995Assignee: Hoechst AktiengesellschaftInventors: Franz-Josef Dany, Gerhard Kalteyer, Gerhard Nolte, Hedwig Prell, Hermann Schrodter
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Patent number: 5405436Abstract: A process for the preparation of a hydroxyapatite, which is suitable as a tooth-cleaning substance, by precipitation from aqueous phosphoric acid and calcium hydroxide solution, in which a calcium-doped phosphoric acid solution is fed to an intensive mixer with a suspension of calcium hydroxide/oxide in a molar ratio of Ca:P=1.667 corresponding to the hydroxyapatite of and reacted there at precipitation temperatures of 60.degree.-100.degree. C., preferably 80.degree.-90.degree. C. and a pH of 4-8, preferably of 6.5-7.5. Also disclosed in a tooth-cleaning substance containing the hydroxyapatite.Type: GrantFiled: September 27, 1993Date of Patent: April 11, 1995Assignee: BK Ladenburg GmbH Gesellschaft fur Chemische ErzeugnissesInventors: Alexander Maurer, Gudrun Raab, Guenter Raab, Reinhold Schmitt, Detlev Schober, Richard Taenzler
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Patent number: 5378258Abstract: A method and an installation for producing granulated triple superphosphate wherein a premixer for phosphate and a phosphoric acid solution includes unclogging means comprising in combination a flexible axial sleeve of non-vulcanized elastomer for injecting phosphate together with at least one sprayer for spraying the phosphoric acid solution and acting level with the free bottom end of the sleeve. The invention is applicable to the chemical industry.Type: GrantFiled: July 9, 1992Date of Patent: January 3, 1995Assignee: Maroc- ChimieInventor: El Hadi Kendili
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Patent number: 5338524Abstract: The present invention provides a process and apparatus for the production of coarse-grained dicalcium phosphate anhydride, at least 95% of which consists of particles with a grain diameter of >45 .mu.m, wherein, at a temperature of 60.degree. to 100.degree. C., a highly reactive calcium component, for example freshly slaked milk of lime or an aqueous slurry or suspension of calcium hydroxide and/or calcium carbonate, is introduced directly into the stirrer zones of a vessel containing aqueous phosphoric acid and having one or more turbulent stirrer zones. An equivalent amount of aqueous phosphoric acid is introduced into another zone of the vessel, the speed of introduction being so regulated that a pH value of 3.0 to 4.5 is obtained in the stirrer zone and the whole batch or a continuously or semi-continuously removed part thereof is cooled to 40.degree. to 60.degree. C. The removed part then is mixed with an additional calcium component, for example milk of lime, to obtain a pH value of from 5.5 to 6.Type: GrantFiled: December 23, 1992Date of Patent: August 16, 1994Assignee: BK Ladenburg GmbHInventors: Alexander Maurer, Guenter Raab, Gudrun Raab, Hans-Georg Steinert, Richard Taenzler
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Patent number: 5336264Abstract: Setting times of calcium phosphate cement compositions are enhanced by the addition of phosphate or carbonate lubricant compositions. Methods for preparing the cement compositions are provided.Type: GrantFiled: July 23, 1992Date of Patent: August 9, 1994Assignee: Norian CorporationInventors: Brent R. Constanz, Mark T. Fulmer, Bryan M. Barr
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Patent number: 5227147Abstract: An apatite whisker has a mean aspect ratio (length along c-axis/length along a-axis) of not less than 10.0 and contains a carbonic acid group of not less than 0.01 wt. % based on total weight of the whisker. A method for preparing an apatite whisker involves precipitating and growing an apatite from a liquid containing phosphoric acid and calcium to have a mean aspect ratio (length along c-axis/length along a-axis) of not less than 10.0.Type: GrantFiled: November 19, 1991Date of Patent: July 13, 1993Assignees: Mitsubishi Materials Corp., Masahiro YoshimuraInventors: Masahiro Yoshimura, Koji Ioku, Kengo Okamoto, Hiroyasu Takeuchi
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Patent number: 5200187Abstract: A class of new oxide structures containing octahedral molybdenum and tetrahedral phosphorous has been generated using hydrothermal, techniques. These materials are produced by the reaction of a molybdenum oxide source with phosphate and any one, or combination of organic cation/alkali-metal cation/organic amine as a templating/mineralizing agent. A reducing agent is necessary to convert the Mo(VI) to a lower valent form and can be either added to the reaction mixture or is provided in the form of one of the reactants.Type: GrantFiled: September 18, 1991Date of Patent: April 6, 1993Assignee: Exxon Research and Engineering CompanyInventors: Robert C. Haushalter, Linda A. Mundi
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Patent number: 5180564Abstract: A process for the production of an aqueous suspension of hydroxylapatite from calcium hydroxide or calcium oxide, and phosphoric acid in which, while stirring, phosphoric acid is slowly added to an aqueous solution or suspension of the calcium compound up to a calcium/phosphorus mole ratio of 10:6, wherein the course of the reaction and the achievement of the end point of the reaction is determined by the conductivity of the solution or suspension. The process results in the production of essentially pure hydroxylapatite, which is useful as, for example, a teeth cleaning agent, a bone-replacement, or as a carrier material for pharmaceutical compositions.Type: GrantFiled: November 22, 1991Date of Patent: January 19, 1993Assignee: BK Ladenburg GmbHInventors: Friedrich Wahl, Andrea Maurer-Rothmann, Karl Merkenich
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Patent number: 5178845Abstract: Novel compositions are provided for the production of hydroxyapatite, where a dry mixture is provided which combines a calcium source and an acidic phosphate source, particularly monocalcium phosphate monohydrate or orthophosphoric acid crystals. These two are combined, optionally with other ingredients, with mechanical mixing, resulting in partial reaction or intimate combination to produce a product which requires less water for formation of a desired viscosity, has enhanced mechanical properties and is physiologically acceptable.Type: GrantFiled: July 2, 1991Date of Patent: January 12, 1993Assignee: Norian CorporationInventors: Brent R. Constantz, Bryan Barr, Kevin McVicker
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Patent number: 5158756Abstract: Porous particles of a calcium phosphate compound having a Ca/P ratio of 1.5 to 1.80, which contain open pores having an average pore size of 100 to 4000 .ANG. and are in the form of spherical particles having an average particle size of 1 to 40 .mu.m, and a process for their production. 90% of the total pore volume of the particles is occupied by pores having a pore size that is 0.5 to 2 times larger than the average pore size of the open pores and the total volume is at least 0.5 ml/g of the particles. The porous calcium phosphate particles are particularly useful as packings for liquid chromatography.Type: GrantFiled: June 25, 1990Date of Patent: October 27, 1992Assignee: Asahi Kogaku Kogyo Kabushiki KaishaInventors: Tetsuro Ogawa, Akihiko Yokoo, Kazuhiro Naganuma, Satoshi Fujinuma, Katsumi Kawamura
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Patent number: 5145520Abstract: An excellent bioactive cement is provided which can chemically and firmly bond to teeth or bones of living bodies, adapt the shape of defected portions of bones or teeth of living bodies, harden quickly, and exhibit high initial strength, without forming inflammation to the surrounding tissue of living bodies. The bioactive cement is composed of glass powder comprising Ca as a main constituent, and an aqueous solution of ammonium phosphate as a hardening liquid for the glass powder, and is economical and stable without loosing the fixation between the artificial biomaterial and the bones or teeth of living bodies nor degradation thereof in the living bodies during a long period of use in the living bodies.Type: GrantFiled: August 22, 1990Date of Patent: September 8, 1992Assignee: Kyoto UniversityInventors: Tadashi Kokubo, Takao Yamamuro, Satoshi Yoshihara
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Patent number: 5128169Abstract: A method for forming a hydroxyapatite coating film on a substrate which comprises coating a dispersion of flocculated colloids of hydroxyapatite on a substrate and drying. The coating method of this invention does not require heating of the coated substrate to high temperature and hence can also be applied to a substrate which is easily deteriorated with heat. The coated substrate of this invention has excellent strength and adhesion force and is useful in a variety of fields, particularly as an implant and as a material, adsorbing and separating agent.Type: GrantFiled: January 2, 1991Date of Patent: July 7, 1992Assignee: Sumitomo Chemical Company, LimitedInventors: Kenji Saita, Shinji Fujiwara
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Patent number: 5124137Abstract: Alkali metal phosphate solutions having a fluorine content of less than 20 ppm, based on P.sub.2 O.sub.5, are prepared by first digesting crude phosphate using sulfuric acid, and separating the calcium sulfate from the crude phosphoric acid. An alkali metal compound is then added to the crude phosphoric acid, and the precipitated solid is filtered off. The prepurified crude phosphoric acid is neutralized to a pH of at least 7, and the solid produced during this operation is separated off. The resultant alkali metal phosphate solutions having a P.sub.2 O.sub.5 content of from 10 to 30% by weight are adjusted to a pH of between 4.8 and 6.0 using phosphoric acid. The solutions are heated to from 60.degree. to 120.degree. C., and from 1 to 6% by weight, based on the weight of the solution, of an alkaline earth metal oxygen compound are added to the alkali metal phosphate solutions with stirring.Type: GrantFiled: March 28, 1991Date of Patent: June 23, 1992Assignee: Hoechst AktiengesellschaftInventors: Gunther Schimmel, Thomas Staffel, Reinhard Gradl
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Patent number: 5114460Abstract: Potassium phosphate useful as a low-chloride content fertilizer is prepared by reacting phosphoric acid, commercial or technical grade, with fertilizer-grade potassium chloride (Muriate of Potash, 60-63% K.sub.2 O) at a reaction temperature of about 130.degree. C. and a mole ratio of phosphorus to potassium of at least about 1.3:1. The vaporization of hydrogen chloride from the reaction mixture is effected by a novel technique combining air followed by steam stripping. The reaction product is used to produce various types as well as grades of fertilizers. The procedure may be used to form sodium phosphate in analogous manner from sodium chloride, which then may be converted to trisodium phosphate or sodium tripolyphosphate. The potassium phosphate may be converted to potassium pyrophosphate by neutralization with potassium hydroxide followed by calcination.Type: GrantFiled: August 16, 1991Date of Patent: May 19, 1992Assignee: Alpine Plant Foods limitedInventors: Kim D. Nguyen, Donald R. Spink
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Patent number: 5108728Abstract: A process is disclosed for the production of granulated dicalcium phosphate dihydrate from fine-grained, powered dicalcium phosphate dihydrate, wherein 80 t0 95% of dicalcium phosphate dihydrate with a grain size of less than 120 .mu.m and 20 to 5% of calcium hydroxide with a grain size of less than 120 .mu.m are dry mixed and continuously sprayed and granulated in a fluidized bed with 20 to 50% of water, relative to the amount of solids, in which is contained an amount of phosphoric acid sufficient for the neutralization of the calcium hydroxide. The granulate obtained is dried at a temperature of 150.degree. to 200.degree. C., and the portions of coarse and fine grained material are optionally sieved off.Type: GrantFiled: March 1, 1991Date of Patent: April 28, 1992Assignee: BK Ladenburg GmbHInventors: Karl-Martin Rau, Karl Merkenich, Erwin Stoffel
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Patent number: 5085845Abstract: A process for preparing a crystalline layered hydrogenphosphate in a shortened period of time in high efficiency, which comprises reacting a tetravalent metal compound with phosphoric acid or its salt at an elevated temperature with introducing steam into the reaction system. Crystalline layered cerium(IV) bis(hydrogen-phosphate), particularly cerium(IV) bis(hydrogen-phosphate) dihydrate prepared by the above process, has an excellent ability of selectively adsorbing cesium ion, and is useful as a cesium ion adsorbent.Type: GrantFiled: October 25, 1990Date of Patent: February 4, 1992Assignee: Tayca CorporationInventors: Shiunkichi Ueda, Tomoe Suita, Masahiko Murakami, Mitsutomo Tsuhako
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Patent number: 5082566Abstract: A calcium-phosphate type hydroxyapatite for chromatographic separation is in the form of spherulites having a mean particle diameter of 0.5 to 50 .mu.m, preferably 1 to 10 .mu.m. The spherulites are each an aggregate mainly of acicular crystallites belonging to a series of hexagonal systems and having unit lattice constants of 9.58.+-.0.08 .ANG. for the a axis and 7.00.+-.0.05 .ANG. for the c axis. The hydroxyapatite is produced by granulating a calcium-phosphate type hydroxyapatite in the form of a gel and then firing the granular apatite at 400.degree. to 700.degree. C., preferably at 500.degree. to 600.degree. C. The firing is performed by heating the granules in the presence of oxygen or air for a given period of time.Type: GrantFiled: September 12, 1988Date of Patent: January 21, 1992Assignees: Toa Nenryo Kogyo Kabushiki Kaisha, Asahi Kogaku Kogyo Kabushiki KaishaInventors: Nobuaki Tagaya, Hideyuki Kuwahara, Takao Hashimoto, Noriko Komatsu, Keiko Fukamachi, Tsugio Maeshima, Toshihiro Ishikawa, Tetsuro Ogawa
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Patent number: 5075087Abstract: A phosphate-containing synthetic hydrotalcite of the following empirical formula:xMgO.Al.sub.2 O.sub.3.yPO.sub.4.zH.sub.2 Owherein, x, y and z are integers indicating the number of moles present of MgO, PO.sub.4 and H.sub.2 O, respectively. The phosphate-containing hydrotalcite being prepared by the addition of sufficient phosphoric acid to the reaction mixture to liberate carbon dioxide. The phosphate-containing hydrotalcite improves the flame retardant characteristics by providing char promotion to the system.Type: GrantFiled: October 5, 1989Date of Patent: December 24, 1991Assignee: J. M. Huber CorporationInventors: John A. Kosin, Barry W. Preston, David N. Wallace
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Patent number: 5072031Abstract: Layered divalent metal pentavalent metallate, M(HAO.sub.4).sub.x (RAO.sub.3).sub.y (Z).sub.z wherein M is divalent metal, A is a pentavalent metal, e.g. phosphorus, R is a substituent group other than H or OH, e.g., phenyl, covalently bonded to A, x+y=1, y is greater than 0, z ranges from 0 to 2, inclusive, and Z is an intercalated moiety is prepared by contacting a source of divalent metal with a substituted phosphonic acid-type compound under hydrothermal conditions.Type: GrantFiled: July 9, 1990Date of Patent: December 10, 1991Assignee: Mobil Oil Corp.Inventor: Stuart D. Hellring
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Patent number: 5055124Abstract: Potassium phosphate useful as a low-chloride content fertilizer is prepared by reacting phosphoric acid, commercial or technical grade, with fertilizer-grade potassium chloride (Muriate of Potash, 60-63% K.sub.2 O) at a reaction temperature of about 130.degree. to about 200.degree. C. and a mole ratio of phosphorus to potassium of at least about 1.3:1. The vaporization of hydrogen chloride from the reaction mixture is effected by a novel technique combining air followed by steam stripping. The reaction product is used to produce various types as well as grades of fertilizers.Type: GrantFiled: October 31, 1989Date of Patent: October 8, 1991Assignee: Alpine Plant Foods LimitedInventors: Kim D. Nguyen, Donald R. Spink
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Patent number: 5053212Abstract: Novel compositions are provided for the production of hydroxyapatite, where a dry mixture is provided which combines a calcium source and an acidic phosphate source, particularly monocalcium phosphate monohydrate or orthophosphoric acid crystals. These two are combined, optionally with other ingredients, with mechanical mixing, resulting in partial reaction or intimate combination to produce a product which requires less water for formation of a desired viscosity, has enhanced mechanical properties and is physilogically acceptable.Type: GrantFiled: July 27, 1990Date of Patent: October 1, 1991Assignee: Norian CorporationInventors: Brent R. Constantz, Bryan Barr, Kevin McVicker
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Patent number: 5047031Abstract: Calcium phosphate minerals are formed by using phosphoric acid substantially free of uncombined water in conjunction with a calcium source, normally as any combination of carbonate, phosphate and hydroxide, and, as required, any additional base to neutralize the phosphoric acid. Protein may be optionally added. The resulting product is readily formed and then sets to a hard, stable, workable shaped object.Type: GrantFiled: May 30, 1989Date of Patent: September 10, 1991Assignee: Norian CorporationInventor: Brent R. Constantz
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Patent number: 5024825Abstract: For the preparation of dicalcium phosphate dihydrate stabilized with dimagnesium phosphate trihydrate and sodium pyrophosphate, an aqueous suspension of calcium carbonate is introduced into a reactor and recirculated by pumping through a high-speed mixer at 3,500 to 8,000 rpm which is in flow connection with the lower and upper portion of the reactor. Into the mixer an amount of phosphoric acid is introduced which is at least sufficient for the quantitative formation of dicalcium phosphate dihydrate and then an oxygen-containing magnesium compound is introduced into the reactor. Finally, lime milk is metered into the reactor up to a maximum pH of 6.9, before the sodium pyrophosphate is added to the reactor. The resulting suspension which has a stabilized dicalcium phosphate dihydrate content of 20 to 33% by weight is spray-dried.Type: GrantFiled: May 10, 1990Date of Patent: June 18, 1991Assignee: Hoechst AktiegesellschaftInventors: Horst Buhl, Josef Holz, Franz-Josef Dany
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Patent number: 4971778Abstract: For working up concentrated, preferably partially condensed phosphoric acid which is contaminated with organic components, the phosphoric acid is first thoroughly mixed with fine-grained sand in a weight ratio of (0.5 to 1.5):1. Then, to neutralize the mixture, a basic, oxygen-containing calcium compound is added, while the thorough mixing is continued, until a 10% aqueous suspension of the mixture to which the calcium compound has been added has a pH between 5 and 11. Finally, the mixture which contains the calcium compound is commminuted after cooling.Type: GrantFiled: April 12, 1990Date of Patent: November 20, 1990Assignee: Hoechst AGInventors: Gerhard Bettermann, Gunther Schimmel, Jens Tiedemann
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Patent number: 4962228Abstract: Layered divalent metal pentavalent metallate, M(HAO.sub.4).sub.x (RAO.sub.3).sub.y (Z).sub.z wherein M is divalent metal, A is a pentavalent metal, e.g. phosphorus, R is a substituent group other than H or OH, e.g., phenyl, covalently bonded to A, x+y=1, y is greater than O, z ranges from 0 to 2, inclusive, and Z is an intercalated moiety is prepared by contacting a source of divalent metal with a substituted phosphonic acid-type compound under hydrothermal conditions.Type: GrantFiled: December 29, 1987Date of Patent: October 9, 1990Assignee: Mobil Oil CorporationInventor: Stuart D. Hellring
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Patent number: 4904459Abstract: A process is provided for working up dusts which have been precipitated electrostatically from the gas mixture composed essentially of carbon monoxide and phosphorus vapor produced in the electrothermal production of yellow phosphorus, which process comprises converting the dusts into a calcinate at 300.degree. to 800.degree. C. under oxidizing conditions in a first step, leaching the calcinate with phosphoric acid in a second step, adjusting the pH of the solution in phosphoric acid to 0 to 1.5 with sodium hydroxide solution in a third step, precipitating the sulfides of lead, copper and cadmium from the partially neutralized solution in phosphoric acid by adding sulfide and filtering them off in a fourth step, adjusting the pH of the filtered, partially neutralized solution in phosphoric acid to about 1.5 to 5.Type: GrantFiled: July 26, 1989Date of Patent: February 27, 1990Assignee: Hoechst AktiengesellschaftInventors: Friedrich Kolkmann, Gunther Schimmel, Johannes Scheffer
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Patent number: 4897250Abstract: A process for producing a calcium phosphate comprising the steps of (a) dissolving at least one member selected from the group consisting of calcium hydroxide and calcium oxide in water with at least one member selected from the group consisting of a sugar, a sugar alcohol, and a polyhydric alcohol; (b) and adding phosphoric acid to the solution obtained to precipitate a calcium phosphate.Type: GrantFiled: January 25, 1989Date of Patent: January 30, 1990Assignee: Asahi Kogaku Kabushiki KaishaInventor: Masaya Sumita
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Patent number: 4889725Abstract: A means for promoting the neutralization reaction between particulate calcium carbonate and ionized phosphate by adding a material formed by the reaction of particulate calcium carbonate and dilute hydrofluoric acid. The products of this invention are useful in lowering serum phosphate levels in patients undergoing renal dialysis, and are also useful as antacids. These products are also useful in the treatment of water and waste water to lower phosphate content.Type: GrantFiled: April 17, 1987Date of Patent: December 26, 1989Inventor: Preston L. Veltman
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Patent number: 4885148Abstract: Relatively pure monopotassium phosphate is produced from wet process phosphoric acid in a process wherein the phosphoric acid is mixed with potassium chloride and recycled components from downstream product and by-product recovery steps and heated to permit hydrogen and chloride to evolve from the melt as gases and wherein the melt is subsequently treated so as to remove impurities so that the monopotassium phosphate may be recovered as a relatively pure crystalline product with low chloride content.Type: GrantFiled: September 6, 1988Date of Patent: December 5, 1989Assignee: Phosphate Engineering & Construction Co., Inc.Inventors: William R. Erickson, Donald B. Stain, James D. Wilson
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Patent number: 4880610Abstract: Calcium phosphate minerals are formed by using highly concentrated phosphoric acid in conjunction with a calcium source, normaly as carbonate or a combination of carbonate and hydroxide, optimally in conjunction with calcium phosphate crystals and additional base to neutralize the phosphoric acid. Protein may be optionally added. The resulting product is readily formed and then sets to a hard, stable, workable shaped object.Type: GrantFiled: April 20, 1988Date of Patent: November 14, 1989Assignee: Norian CorporationInventor: Brent R. Constantz
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Patent number: 4853200Abstract: Unmilled commercially available granular "natural" soda ash is reacted with orthophosphoric acid to produce a highly concentrated slurry at a molar Na:P ratio of about 1.5 in a continuous process. Problems associated with incomplete reaction are solved and the slurry can be dried to the double salt Na.sub.3 H.sub.3 (PO.sub.4).sub.2 or reacted with aqueous sodium hydroxide to produce a superior precursor for manufacturing sodium tripolyphosphate.Type: GrantFiled: March 21, 1988Date of Patent: August 1, 1989Assignee: Monsanto CompanyInventors: N. Earl Stahlheber, John E. Lyon
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Patent number: 4849193Abstract: This invention relates to the manufacture of hydroxylapatite in a through-solution process wherein monobasic calcium phosphate is reacted with a calcium hydroxide solution. In a preferred embodiment, an acidic premix is formed by reacting phosphoric acid and calcium hydroxide with high shear agitation in a first stage, and thereafter reacting the acidic premix with a saturated solution of calcium hydroxide also under high shear agitation in a second stage. The second stage reaction is carried out in an alkaline solution by carefully metering the acid premix into the calcium hydroxide solution whereby the pH of the solution is maintained above 11 until the reaction is near completion. It is particularly preferred to use a stoichiometric portion of calcium hydroxide in carrying out the reactions. After the hydroxylapatite precipitate is recovered, it may be sintered at a temperature between about 700.degree. C. and 1100.degree. C. for about 5 to 30 minutes to form a crystalline hydroxylapatite.Type: GrantFiled: May 2, 1988Date of Patent: July 18, 1989Assignee: United States Gypsum CompanyInventors: Jay W. Palmer, Terry L. Rosenstiel
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Patent number: 4846853Abstract: Layered divalent metal hydrogen phosphate, MHPO.sub.4.nH.sub.2 O wherein M is a Group IIA or Group IIB element and n ranges from about 0 to 2, is prepared by hydrothermal treatment of an aqueous mixture containing a source of metal oxide, a source of phosphorus oxide and a source of hydrogen atoms, said aqueous mixture having an initial pH ranging between about 3 and 10.Type: GrantFiled: March 9, 1987Date of Patent: July 11, 1989Assignee: Mobil Oil CorporationInventors: Clarence D. Chang, Stuart D. Hellring
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Patent number: 4836995Abstract: The present invention relates to a process for the manufacture of monopotassium phosphate using solvent extraction technique. According to the invention, the reaction occurs between phosphoric acid and potassium chloride at a temperature between 0 and 100 degrees C. in the presence of an organic solvent comprising a long chain primary amine having between 6 to 28 carbon atoms. The lower phase containing monopotassium phosphate and dipotassium phosphate is acidulated with a solution of phosphoric acid to a pH in the range of between 2 to 6, whereby crystallized monopotassium phosphate is obtained and separated. The upper phase which contains the organic solvent, aminehydrochloric acid as well as most of the impurities originally present in the starting reagents, is treated with a base at a temperature in the range of 20 to 100 degrees C. whereby the amine is regenerated and recycled to the process. Typical examples of suitable bases are calcium oxide, calcium carbonate or mixtures thereof.Type: GrantFiled: November 23, 1988Date of Patent: June 6, 1989Assignee: Haifa Chemicals Ltd.Inventors: Shalom Manor, Grigori Pipko, Adrian Langham, Nitza Friedman, Amalia Steiner
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Patent number: 4836994Abstract: The present invention relates to a process for preparing a calcium-phosphorus-apatite, essentially characterized by admixing a single solvent of water or an organic solvent compatible with water or a mixed solvent of water with an organic solvent compatible with water with calcium and phosphorus compounds soluble in said single or mixed solvent to prepare a raw material solution, and atomizing the raw material solution into a flame or a heating zone for effecting a thermal decomposition reaction thereof to form a calcium-phosphorus-apatite; a calcium-phosphorus-apatite obtained by the process and having novel characteristics; and the use of the calcium-phosphorus-apatite as a chromatographic packing material.Type: GrantFiled: September 11, 1987Date of Patent: June 6, 1989Assignee: Kanto Kagaku Kabushiki KaishaInventors: Senya Inoue, Akira Ono
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Patent number: 4828823Abstract: The monofluorophosphate compatibility of dicalcium phosphate dihydrate can be improved in processes in which a slaked lime slurry is reacted with phosphoric acid to form a monocalcium phosphate solution to which is added magnesium oxide, additional lime slurry and pyrophosphoric acid with later removal of the dicalcium phosphate dihydrate. The improvement involved adding the magnesium oxide at 0.3%-2% and adding 0.1%--less than 0.5% of trimagnesium phosphate to the recovered dicalcium phosphate dihydrate.Type: GrantFiled: April 7, 1986Date of Patent: May 9, 1989Assignee: Stauffer Chemical CompanyInventor: Rosa Li
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Patent number: 4794171Abstract: A calcium-phosphate type hydroxyapatite which belongs to a series of hexagonal systems has unit lattice constants of 9.58.+-.0.08 .ANG. for the a axis and 7.00.+-.0.05 .ANG. for the c axis. Its Ca/P ratio is in the range of 1.50 to 1.90. It is for use as a column packing material for chromatographic separation of biopolymers. The hydroxyapatite is produced by firing it in the form of a gel or powder at a temperature of 400.degree. to 700.degree. C. As a gel the hydroxyapatite takes the form of a suspension or slurry. A powder is prepared by removing moisture from the hydroxyapatite in the gel form and then drying. Either gel or powder is fired by heating in the presence of oxygen or air at 500.degree. to 600.degree.0 C.Type: GrantFiled: September 22, 1986Date of Patent: December 27, 1988Assignee: Toa Nenryo Kogyo Kabushiki KaishaInventors: Nobuaki Tagaya, Hideyuki Kuwahara, Takao Hashimoto, Noriko Komatsu, Keiko Fukamachi, Tsugio Maeshima
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Patent number: 4781905Abstract: A process is developed for producing phosphoric acid and phosphates from wet-process phosphoric acid. The crude acid is extracted with a waterimmiscible solvent mixture consisting of mixed trialkyl phosphine oxide and a diluent, wherein about 2/3 P.sub.2 O.sub.5 in the crude acid is extracted into solvent mixture and the balance remains in the raffinate. Pure phosphoric acid or phosphates are produced by stripping the loaded solvent with appropriate aqueous phase and secondary calcium phosphate fertilizer is obtained by neutralizing the raffinate with calcium carbonate.Type: GrantFiled: May 30, 1986Date of Patent: November 1, 1988Inventors: Jiang Yu-Ming, Su Yuan-Fu
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Patent number: 4781904Abstract: A calcium-phosphate type hydroxyapatite for chromatographic separation is in the form of spherulites having a mean particle diameter of 0.5 to 50 .mu.m, preferably 1 to 10 .mu.m. The spherulites are each an aggregate mainly of acicular crystallites belonging to a series of hexagonal systems and having unit lattice constants of 9.58.+-.0.08 .ANG. for the a axis and 7.00.+-.0.05 .ANG. for the c axis. The hydroxyapatite is produced by granulating a calcium-phosphate type hydroxyapatite in the form of a gel and then firing the granular apatite at 400.degree. to 700.degree. C., preferably at 500.degree. to 600.degree. C. The firing is performed by heating the granules in the presence of oxygen or air for a given period of time.Type: GrantFiled: September 22, 1986Date of Patent: November 1, 1988Assignees: Tao Nenryo Kogyo Kabushiki Kaisha, Asahi Kogaku Kogyo Kabushiki KaishaInventors: Nobuaki Tagaya, Hideyuki Kuwahara, Takao Hashimoto, Noriko Komatsu, Keiko Fukamachi, Tsugio Maeshima, Toshihiro Ishikawa, Tetsuro Ogawa
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Patent number: 4759920Abstract: The present invention relates to a process for the manufacture of disodium phosphate of a high purity without utilizing organic solvents. According to the process, monosodium sulfate is reacted, at a temperature, in the range of 40 to 100 degrees C. with a phosphate constituent selected from phosphate rock, dicalcium phosphate or mixtures thereof, in the presence of phosphoric acid. The common metal impurities, organic matter and fluorides present in the starting phosphate rock are substantially complete eliminated with the solid gypsum or dicalcium phosphate resulted thereto. After separating said solid, the filtrate is treated in two neutralization stages: first by a calcium constituent selected from calcium carbonate, calcium hydroxide or mixtures thereof and separating the formed dicalcium phosphate, followed by a second neutralization with an alkali sodium constituent selected from sodium hydroxide, sodium carbonate and sodium bicarbonate or mixtures thereof at a pH in the range of 8.0 to 9.5.Type: GrantFiled: June 6, 1986Date of Patent: July 26, 1988Assignee: Negev Phosphates Ltd.Inventors: Alexander Iosef, Menachem Bar-On
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Patent number: 4755367Abstract: A process for the preparation of coarse-particle dicalcium phosphate dihydrate having a virtually spherical crystal shape and a particle size range between about 63 and 450 .mu.m, preferably between about 90 and 300 .mu.m, by reacting pure aqueous phosphoric acid with aqueous suspensions of precipitated chalks, wherein an amount of suspension corresponding to the reaction product formed is removed continuously or semicontinuously and the dicalcium phosphate dihydrate is separated off, washed and dried. Also disclosed is coarse-particle dicalcium phosphate dihydrate produced by the above process.Type: GrantFiled: April 21, 1986Date of Patent: July 5, 1988Assignee: Benckiser-Knapsack GmbHInventors: Gerold Brachtel, Guenter Raab, Detlev Schober
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Patent number: 4721615Abstract: Novel processes are provided for producing anhydrous dicalcium phosphate (DCPA) and the gamma and beta forms of calcium pyrophosphate (CPP) from the reaction of phosphoric acid and lime. Dentifrice compositions containing the resultant phosphates are also disclosed.Type: GrantFiled: June 6, 1986Date of Patent: January 26, 1988Assignee: Monsanto CompanyInventors: Edward J. Griffith, William C. McDaniel
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Patent number: 4717556Abstract: A microfine .beta.-tricalcium phosphate powder is produced by mixing hydrogen calcium phosphate powder, calcium carbonate powder, and water in amounts calculated to give a slurry having a solids concentration in the range of 5 to 15% by weight and a CA:P atomic ratio in the range of 1:1.4.about.1.6 and subjecting the slurry to attrition.Type: GrantFiled: October 8, 1986Date of Patent: January 5, 1988Assignees: Agency of Industrial Science & Technology, Ministry of International Trade & IndustryInventors: Sukezo Kawamura, Motohiro Toriyama
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Patent number: 4711769Abstract: The present invention relates to a process for preparing a calcium-phosphorus-apatite, essentially characterized by admixing a single solvent of water or an organic solvent compatible with water or a mixed solvent of water with an organic solvent compatible with water with calcium and phosphorus compounds soluble in said single or mixed solvent to prepare a raw material solution, and atomizing the raw material solution into a flame or a heating zone for effecting a thermal decomposition reaction thereof to form a calcium-phosphorus-apatite; a calcium-phosphorus-apatite obtained by the process and having novel characteristics; and the use of the calcium-phosphorus-apatite as a chromatographic packing material.Type: GrantFiled: July 30, 1986Date of Patent: December 8, 1987Assignee: Kanto Kagaku Kabushiki KaishaInventors: Senya Inoue, Akira Ono
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Patent number: 4701314Abstract: The process for producing microsized amorphous particles of a metal phosphate incorporates the steps offorming a solution of a metal alkoxide in an organic solvent,forming an aqueous phosphoric acid solution,introducing the alkoxide and the phosphoric acid solutions into a reactor vessel wherein the solutions are immiscible and forming two separate liquid phases with an interface,applying agitation to at least the region of the interface to promote a reaction between the metal alkoxide and said phosphoric acid at the interface,collecting the reaction product, andfiring it in an oxygen containing environment at a temperature sufficiently high to drive off the organic residue.Type: GrantFiled: October 29, 1986Date of Patent: October 20, 1987Assignee: International Business Machines CorporationInventor: Lawrence D. David
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Patent number: 4686094Abstract: Pyrophoric elemental phosphorus-containing material, e.g., solid waste containing high levels of elemental phosphorus (P.sub.4), is treated by contact with an oxygen-containing gas, such as air, to reduce the amount of elemental phosphorus contained therein while it is otherwise protected from contact with oxygen in the air by being blanketed by a non-flammable fluid (e.g., while under an aqueous protective layer). This renders the material less pyrophoric and also enables the recovery of phosphorus values therefrom, e.g., in the form of a weak phosphoric acid solution. This treatment, for example, mobilizes highly pyrophoric solid waste into a more flowable sludge or mud form while rendering it substantially more non-pyrophoric.Type: GrantFiled: August 8, 1986Date of Patent: August 11, 1987Assignee: Stauffer Chemical CompanyInventors: Auston K. Roberts, William E. Trainer, Steve Nakamura, Leon C. Duffin, David L. Biederman
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Patent number: 4686105Abstract: The present invention relates to a granular product comprising a reaction product between magnesium oxide and phosphoric acid; this product exhibiting high solubility in neutral citrate solubility tests and the weight ratio of magnesium to phoshorous being smaller than 1.8:1.Type: GrantFiled: March 5, 1985Date of Patent: August 11, 1987Assignee: Boliden AktiebolagInventors: Sven-Eric Dahlgren, Douglas S. Ekman, Claes E. Ericsson
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Patent number: 4678650Abstract: An aqueous alkali phosphate solution is made. An organic phase is countercurrently mixed with an aqueous phase, the two phases being used in a volume ratio larger than 1:1 and formed aqueous alkali phosphate solution is separated from the remaining organic phase. The two phases are mixed and reacted in a reaction zone comprised of a mixing and separating zone. The organic phase is continuously dispersed in the aqueous phase. A volume excess of aqueous phase is maintained in the mixing zone and the two phases are used in an overall quantity sufficient to provide a volume ratio of organic to aqueous phase of 4:6 to 2:8.Type: GrantFiled: March 22, 1985Date of Patent: July 7, 1987Assignee: Hoechst AktiengesellschaftInventors: Reinhard Gradl, Gero Heymer