Metal Or Ammonium Containing Patents (Class 423/305)
  • Patent number: 4044106
    Abstract: Rinse acid collected from an aluminum bright dipping operation is reacted with soda alkalies at 80.degree. C or higher to yield a solution of trisodium phosphate, Na.sub.3 PO.sub.4, sodium aluminate, NaAlO.sub.2, sodium nitrate, NaNO.sub.3, and trace insolubles. The hot solution is quickly filtered to remove all insoluble impurities and then cooled so that the trisodium phosphate crystallizes out which, after filtering, leaves a mother liquor containing some remaining trisodium phosphate and soluble impurities, namely, sodium aluminate and sodium nitrate. The mother liquor is then recycled repeatedly with further batches of rinse acid to maximize the phosphate recovery.
    Type: Grant
    Filed: October 15, 1975
    Date of Patent: August 23, 1977
    Inventor: Albert Yi-Hung Fang
  • Patent number: 4043860
    Abstract: Single crystals of neodymium pentaphosphate greater than one centimeter in size and of high purity and quality are grown from polyphosphoric acid solutions using the combination of a dilute solution, seeding, growth temperatures of 500.degree. to 650.degree. C, and a double crucible configuration.
    Type: Grant
    Filed: January 24, 1977
    Date of Patent: August 23, 1977
    Assignee: The United States of America as represented by the Secretary of the Army
    Inventors: Thomas R. Au Coin, Abraham Schwartz, John G. Gualtieri, Melvin J. Wade
  • Patent number: 4041133
    Abstract: Stable aqueous ammonium phosphate containing a higher proportion of polyphosphates is obtained by reacting phosphoric acid with ammonia in the presence of sulfuric, nitric or hydrochloric acids under conditions sufficient to produce a partially neutralized melt containing polymeric phosphates at a temperature between 400.degree. and about 750.degree. F. by the autogenous heat of neutralization, quenching and further neutralizing the melt.
    Type: Grant
    Filed: August 15, 1975
    Date of Patent: August 9, 1977
    Assignee: Union Oil Company of California
    Inventor: Donald C. Young
  • Patent number: 4029742
    Abstract: An advantageous process of producing Maddrell salt which is substantially free of water-soluble by-products is described. The resulting substantially water-insoluble Maddrell salt is especially useful as polishing and cleaning agent in toothpaste.
    Type: Grant
    Filed: April 6, 1976
    Date of Patent: June 14, 1977
    Assignee: Benckiser-Knapsack GmbH
    Inventors: Klaus Sommer, Hermann Weber
  • Patent number: 4028237
    Abstract: There are disclosed methods for removing fluorine values from fluorine-containing waste waters, in which aluminum ions are added to fluorine-containing waste water to convert fluorine to hydroxyfluoride complexes, adding phosphoric acid or phosphate and calcium compound are added to form fluoride apatite with residual fluorine in the waste water, and the hydroxy-fluoride complex and fluoride apatite are removed from the waste water.
    Type: Grant
    Filed: March 1, 1976
    Date of Patent: June 7, 1977
    Assignee: Hitachi, Ltd.
    Inventors: Shigeoki Nishimura, Toshio Sawa, Kouji Otani, Seiichi Kikkawa
  • Patent number: 4025608
    Abstract: Zirconium phosphate is made by reacting a zirconium salt with phosphoric acid or a phosphate in a liquid medium, the zirconium salt being insoluble in water. A granular product may be obtained having a grain size controlled by that of the salt. The product may be used as an ion-exchange material.
    Type: Grant
    Filed: December 16, 1974
    Date of Patent: May 24, 1977
    Assignee: Magnesium Elektron Limited
    Inventors: David S. Tawil, Michael H. Clubley, Frank Farnworth
  • Patent number: 4024225
    Abstract: Wet-process phosphoric acid is partially purified by extraction with an organic solvent followed by scrubbing with a portion of the aqueous phosphoric acid from a water-stripping unit, then water-stripping and base-stripping. At the water-stripping stage, all the remaining impurities and approximately two-thirds of the P.sub.2 O.sub.5 are transferred from the organic to the aqueous phase, which renders the other one-third P.sub.2 O.sub.5, subsequently recovered by base-stripping, essentially free of impurities. The bulk of the aqueous phosphoric acid from the water-stripping is purified further by precipitating the impurities with an alkali metal hydroxide or carbonate. The precipitate is filtered off and the filtrate used for base-stripping. The resulting aqueous solution from base-stripping is adjusted to a desired alkali metal-to-phosphate ratio and used for manufacture of high purity alkali metal phosphate in general and particularly sodium tripolyphosphate.
    Type: Grant
    Filed: July 28, 1975
    Date of Patent: May 17, 1977
    Assignee: United States Steel Corporation
    Inventor: Peter T. Chiang
  • Patent number: 4021528
    Abstract: Crystalline AlH.sub.3 (PO.sub.4).sub.2.3H.sub.2 O is obtained from an aqueous solution of aluminum phosphate containing a molar ratio of Al.sub.2 O.sub.3 :P.sub.2 O.sub.5 of from 1:2 to 1:6 and an organic solvent that is miscible with water. The product is useful in diminishing the setting time of hydraulic binders.
    Type: Grant
    Filed: January 23, 1975
    Date of Patent: May 3, 1977
    Assignee: Hoechst Aktiengesellschaft
    Inventor: Albert Schlegel
  • Patent number: 4018706
    Abstract: A catalyst for purifying exhaust and waste gases comprisingA. a support substrate comprising 2 to 100% by weight of an oxide complex of titanium and phosphorus containing titanium and phosphrus in such a proportion that the molar ratio of TiO.sub.2 to P.sub.2 O.sub.5 is from 5.0 to 0.5 and 98 to 0% by weight of aluminum oxide, andB. supported on said substrate as a catalytic substance, 2 to 300 parts by weight, calculated as metal oxide per 100 parts by weight of the support substrate (A), of at least one heavy metal selected from the group consisting of Ni, Cu, Cr, Fe, Co, Mn, Bi, V, W, Mo, Sn, Zn, Zr, Pb, Sb, Ti, Ta, Cd and Nb, or 0.01 to 1.0 part by weight, calculated as metal per 100 parts by weight of the support substrate (A), of at least one noble metal selected from the group consisting of Pt, Pd, Rh, Ir, Os and Ru.
    Type: Grant
    Filed: July 20, 1976
    Date of Patent: April 19, 1977
    Assignee: Nippon Shokubai Kagaku Kogyo Co., Ltd.
    Inventors: Akira Inoue, Koshi Horie, Koichi Saito, Yukio Aoki, Tetsuji Ono, Takashi Ohara
  • Patent number: 4017589
    Abstract: Ammonium polyphosphates are prepared by a process which comprises heating melamine orthophosphate prepared from impure wet-process phosphoric acid in a stream of gaseous ammonia at a temperature between 150.degree. C and 210.degree. C to produce a mixture of melamine and relatively pure short-chain ammonium polyphosphates. The solid product is extracted with water to remove the ammonium polyphosphates and free the insoluble, crystalline melamine for recycle. Thus, the only starting materials consumed in the process are phosphoric acid and ammonia.
    Type: Grant
    Filed: March 17, 1976
    Date of Patent: April 12, 1977
    Assignee: Tennessee Valley Authority
    Inventors: John F. McCullough, Richard C. Sheridan
  • Patent number: 4014813
    Abstract: Self-activated ultraviolet-emitting hafnium pyrophosphate phosphors. Up to about 20 mole percent of the hafnium may be substituted with one or more of zirconium, germanium and silicon. The phosphors, which may be excited by ultraviolet radiation, x-rays and electron beams, may be used as energy converters in photodevices. The phosphors may be prepared by heating a mixture of a hafnium compound, a phosphate (no added activator ions) and optionally compounds of one or more of zirconium, germanium and silicon, which are present in proportions up to about 25 mole percent of the hafnium present, at about 1000.degree. to 1300.degree. C in air.
    Type: Grant
    Filed: January 13, 1975
    Date of Patent: March 29, 1977
    Assignee: RCA Corporation
    Inventor: Igal Shidlovsky
  • Patent number: 4011300
    Abstract: Phosphoric acids having H.sub.2 0/P.sub.2 O.sub.5 mole ratios of about 4.5 or less are converted to aqueous solutions of ammonium polyphosphates of which at least about 40 percent of the P.sub.2 O.sub.5 is present as acyclic polyphosphates. The reaction is conducted at 500.degree. to about 750.degree. F. sufficient to increase the polymeric P.sub.2 O.sub.5 content at least 10 percent by reacting a highly dispersed, unconfined acid spray with substantially anhydrous ammonia. High conversions to polymeric species are obtained while minimizing both reactor fouling when using impure wet-process acids, and corrosion occurring with either wet-process or "white" acids.
    Type: Grant
    Filed: June 27, 1975
    Date of Patent: March 8, 1977
    Assignee: Union Oil Company of California
    Inventors: Bruce A. Harbolt, Donald C. Young
  • Patent number: 4008307
    Abstract: A process for the production of monobasic potassium phosphate from wet process phosphoric acid and potassium sulfate by ion exchange. The application of the process is the production of monobasic potassium phosphate by ion exchange from wet phosphoric acid produced by the reaction of sulfuric acid on apatite rock and by-product potassium sulfate from processes for the recovery of aluminum from alunite.
    Type: Grant
    Filed: June 2, 1975
    Date of Patent: February 15, 1977
    Assignees: Southwire Company, National Steel Corporation, Earth Sciences, Inc.
    Inventors: Kent W. Loest, Vernon R. Ewing
  • Patent number: 4005172
    Abstract: Complex phosphates of aluminum containing a halogen and chemically-bound molecule of a hydroxy compound, namely, water. A typical example is a complex phosphate having the empirical formulate AlPClH.sub.11 O.sub.9. They are most conveniently prepared by the reaction of an aluminum halide with water and orthophosphoric acid, under relatively cool conditions. The compounds are generally soluble in water and polar organic solvents. They decompose at low temperatures to give aluminum orthophosphate, thereby providing a method for producing aluminum phosphate in many forms, for example, fibers, coatings, binders and fine particles, from a solution in water or organic solvents.
    Type: Grant
    Filed: October 21, 1974
    Date of Patent: January 25, 1977
    Assignee: Imperial Chemical Industries Limited
    Inventors: James Derek Birchall, John Edward Cassidy
  • Patent number: 4002725
    Abstract: Acicula of rare earth pentaphosphates, of a diameter and length ideal for waveguiding laser-type applications, are grown by controlling the rate of metaphosphoric acid conversion by introducing water vapor into an inert gas atmosphere continuously flowed through the reaction zone. The required amount of water vapor in the reaction zone has to be within the range between approximately 14 grams per cubic meter and 290 grams per cubic meter of the flowing atmosphere. This control is implemented by bubbling the inert gas atmosphere through a water bath at temperatures between 15.degree. and 80.degree. C. It is believed that the control of the water vapor eliminates problems of supersaturation in the forming of pentaphosphoric crystals in the growth solution and thereby promotes their natural tendency to form purely chainlike polymer structures.
    Type: Grant
    Filed: July 9, 1975
    Date of Patent: January 11, 1977
    Assignee: Bell Telephone Laboratories, Incorporated
    Inventors: Paul Michael Bridenbaugh, Paul Foo-Hung Liao, Bruce Cedric Tofield, Heinz Paul Weber
  • Patent number: 3998668
    Abstract: A solid source consisting essentially of high purity aluminum metaphosphate, Al(PO.sub.3).sub.3 is used for introducing elemental phosphorus into P-type silicon chips or wafers of semi-conductor grade. The aluminum metaphosphate functions as a source for the controlled release of P.sub.2 O.sub.5 vapors which are directed to the desired face of the silicon wafer. The reverse side of the silicon wafer receives little or no phosphorus and consequently retains its character as P-type silicon.
    Type: Grant
    Filed: March 18, 1976
    Date of Patent: December 21, 1976
    Assignee: Owens-Illinois, Inc.
    Inventors: Jack M. Florence, William E. Smith
  • Patent number: 3996332
    Abstract: Synthetic rutile is produced from a titaniferous slag derived from ilmenite. Ilmenite concentrates are reduction smelted to remove iron as a high grade pig iron byproduct and to enrich the remaining slag phase in titanium. Oxidation of the slag and aging at high temperature in the presence of a titanium pyrophosphate flux converts the titanium bearing phases to discrete rutile crystals and a phosphate glass phase containing most of the associated impurities. Rutile is separated from the glassy matrix by attrition scrubbing aged, ground slag in dilute mineral acid solutions.
    Type: Grant
    Filed: December 2, 1975
    Date of Patent: December 7, 1976
    Assignee: The United States of America as represented by the Secretary of the Interior
    Inventors: Gerald W. Elger, Donald E. Kirby
  • Patent number: 3993734
    Abstract: A process for the manufacture of alkali metal polyphosphates having a predetermined crystalline form, in which a mixture of alkali metal orthophosphates having a molar ratio of alkali metal oxide to phosphoric anhydride between 1 and 2 is first granulated, the resulting granules are dried and then are subjected to thermal treatment in the presence of aqueous vapor.
    Type: Grant
    Filed: June 30, 1975
    Date of Patent: November 23, 1976
    Assignee: Rhone-Progil
    Inventors: Jean-Michel Verdier, Jacques Becuwe, Jacques Chastel
  • Patent number: 3981970
    Abstract: Method for production of a zeolitic material represented by the formula:R.sub.x H.sub.5.sub.-x (Al.sub.y Fe.sub.1.sub.-y).sub.4 (P.sub.l As.sub.1.sub.-l).sub.3 O.sub.16.zH.sub.2 Owherein R represents Na or K, x, y, z and l are numerical values of O.ltoreq.x.ltoreq.5, O.ltoreq.y.ltoreq.1, Z.ltoreq.9 and O.ltoreq.l.ltoreq.1, respectively; which comprises preparing an aqueous solution by dissolving (1) at least one source of aluminum and iron, (2) at least one source of phosphorus and arsenic and (3) at least one source of sodium and potassium in water in the ranges expressed in terms of the molar ratios of their oxides of3.5.ltoreq.(Al, Fe).sub. 2 O.sub.3 /(P, As).sub. 2 O.sub.5 .ltoreq.4.5and(K, Na).sub.2 O/(Al, Fe) .sub.2 O.sub.3 >0.12adjusting the pH of the solution to within the range of the cross-hatched area in FIGS. 1 to 4 and heating the solution at 150 to 250.degree.C in a closed vessel to crystallize the zeolitic material and recovering the objective zeolitic material.
    Type: Grant
    Filed: July 16, 1971
    Date of Patent: September 21, 1976
    Assignee: Takeda Chemical Industries, Ltd.
    Inventors: Takeo Wada, Kazuo Okada
  • Patent number: 3978195
    Abstract: Production of substantially water-insoluble linear ammonium polyphosphates of the general formula (NH.sub.4 PO.sub.3).sub.n, in which n is a number between 10 and 1000. To this end, substantially equimolecular proportions of ammonium orthophosphate and phosphorus pentoxide are reacted by heating them to temperatures within the range 170.degree. and 350.degree.C in the presence of gaseous ammonia. The reaction is effected while continuously and simultaneously mixing, kneading and comminuting the reaction material in a reactor. The reactor is closed, provided with means for the supply of solid feed material, a gas inlet and a gas outlet, a discharge opening for the removal of final product, and with mixing, kneading and comminuting implements which are rotatably secured to the inside of the reactor.
    Type: Grant
    Filed: June 3, 1974
    Date of Patent: August 31, 1976
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Hermann Schrodter, Hans-Werner Stephan, Gero Heymer
  • Patent number: 3976752
    Abstract: A continuous process for preparing crystalline, water-insoluble ammonium polyphosphates of controlled pH utilizing a continuous reaction arena, is disclosed.
    Type: Grant
    Filed: November 18, 1974
    Date of Patent: August 24, 1976
    Assignee: American Cyanamid Company
    Inventors: Hans A. Corver, Allan J. Robertson
  • Patent number: 3975308
    Abstract: A method for the preparation of pyrophosphates such as SiP.sub.2 O.sub.7 is disclosed, whereby the undesired formation of by-products such as Si.sub.2 P.sub.2 O.sub.9 is minimized. Such pyrophosphates are particularly suitable for the formation of solid semi-conductor diffusion sources, wherein the presence of by-product is seriously detrimental.
    Type: Grant
    Filed: February 7, 1975
    Date of Patent: August 17, 1976
    Assignee: The Carborundum Company
    Inventors: Thomas A. Myles, Curtis E. Zimmer
  • Patent number: 3969483
    Abstract: Particulate carbonaceous matter in ammonium polyphosphate liquid made from impure wet-process phosphoric acid is removed by intimately mixing the liquid with a combination of selected organic flocculating agents and then transferring the mixture to a separation vessel where the particulate carbonaceous matter floats rapidly to the surface. Clarified liquid that contains essentially no particulate carbonaceous matter is withdrawn from the bottom of the separation vessel. The particulate carbonaceous matter and a minor portion of the input ammonium polyphosphate liquid are withdrawn from the top of the separation vessel and processed into fluid or solid fertilizers.
    Type: Grant
    Filed: June 5, 1975
    Date of Patent: July 13, 1976
    Assignees: Tennessee Valley Authority, Akzona Incorporated
    Inventors: John M. Stinson, Horace C. Mann, Jr., Dale H. Johnson
  • Patent number: 3965248
    Abstract: Aqueous AlF.sub.3 enriched crystallization mother liquors contaminated with P.sub.2 O.sub.5 values and having less than 5% free acidity are treated with a material which provides bismuth ions in the mother liquor in amounts small enough to insure that the Bi/PO.sub.4 mole ratio remains below about 1.05. Under these conditions, the bismuth and P.sub.2 O.sub.5 react essentially quantitatively to form a BiPO.sub.4 precipitate by which the P.sub.2 O.sub.5 can be separated from the mother liquor. Bismuth can be regenerated from the BiPO.sub.4 and recycled for further use in the process.The invention finds utility in the preparation of AlF.sub.3 by the reaction of an aluminum ore and P.sub.2 O.sub.5 contaminated HF or H.sub.2 SiF.sub.6 such as that available as a by-product of wet process phosphoric acid manufacture. The AlF.sub.3 reaction product is recovered by a crystallization step which, because it is normally only about 70 to 90% efficient, produces a mother liquor containing substantial amounts of AlF.sub.3.
    Type: Grant
    Filed: August 12, 1974
    Date of Patent: June 22, 1976
    Assignee: Freeport Minerals Company
    Inventors: Tadeusz K. Wiewiorowski, Michael O. Nutt
  • Patent number: 3957955
    Abstract: A solution of sodium ammonium phosphate is prepared by reacting monoammonium phosphate with sodium carbonate in a vertical column having vapor-liquid contact means at a temperature in the range of 150.degree.F. up to the boiling point.
    Type: Grant
    Filed: December 30, 1974
    Date of Patent: May 18, 1976
    Assignee: Olin Corporation
    Inventor: Bernard H. Nicolaisen
  • Patent number: 3956462
    Abstract: Waste material consisting substantially of contaminated phosphorous acid is utilized. To this end, the phosphorous acid is introduced, with agitation into a liquid phase. Liquid phase and phosphorous acid are maintained in a ratio by volume between 1:1 and 10:1. The liquid phase is placed in a reactor, maintained between 250.degree. and 400.degree.C and selected from a phosphoric acid of the general formula H.sub.n.sub.+2 P.sub.n O.sub.3n.sub.+1, in which n substantially stands for a number between 1 and 5. Resulting hydrogen phosphide is removed. In the event of continuous operation, newly formed liquid phase is removed from the reactor, at the same rate as it is being formed.
    Type: Grant
    Filed: March 18, 1974
    Date of Patent: May 11, 1976
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Gero Heymer, Wolfgang Scheibitz, Hasso Spott
  • Patent number: 3949058
    Abstract: There is disclosed a method and apparatus for the production of ammonium polyphosphate solutions of high concentrations from phosphoric acid and ammonia. The process is ideally suited for the production of such solutions from wet-process phosphoric acid which has a P.sub.2 O.sub.5 content of from 56 to about 70 weight percent, impurity-free basis, and which, preferably, contains from 5 to about 50 percent of its phosphorus present as polyphosphoric acid. The method comprises introducing the phosphoric acid into a reactor bearing a Teflon liner and reacting it therein with vapors of ammonia while controlling the amount of ammonia from 0.2 to about 0.3 pound ammonia per pound of P.sub.2 O.sub.5 in the feed acid, sufficient to achieve a peak reaction temperature in the reactor between about 525.degree. and 775.degree.F., the absolute value of which is dependent on the bulk water content of the feed acid.
    Type: Grant
    Filed: December 20, 1973
    Date of Patent: April 6, 1976
    Assignee: Union Oil Company of California
    Inventors: Donald C. Young, Bruce A. Harbolt
  • Patent number: 3947548
    Abstract: A single crystal of gallium phosphide including 0.5 atomic ratio or less of indium is grown from a melt consisting of indium, gallium and phosphorous with an atomic ratio of gallium to phosphorous equal to at least 2.0.
    Type: Grant
    Filed: August 28, 1973
    Date of Patent: March 30, 1976
    Assignee: Semiconductor Research Foundation
    Inventors: Jun-Ichi Nishizawa, Ken Suto, Yasuo Okuno
  • Patent number: 3938982
    Abstract: Improved stable suspension liquid fertilizers based on ammonia and phosphoric acid obtained by the wet method, and combining both a high content of fertilizing elements and a long storage life are prepared by ammoniating the phosphoric acid with gaseous ammonia in two steps at a temperature of from 90.degree.C to 120.degree.C until a pH of between 6 and 8 is attained, rapidly cooling the resulting ammonium phosphate suspension to a temperature of from 0.degree.C to 35.degree.C, and during the cooling adding a suspending agent to the suspension while maintaining the suspension under stirring.
    Type: Grant
    Filed: July 27, 1973
    Date of Patent: February 17, 1976
    Assignee: Montecatini Edison S.p.A.
    Inventors: Alessandro Frangioni, Giovanni Venturino, Giorgio Morandi, Adriano Del Vesco
  • Patent number: 3939254
    Abstract: Aqueous monoammonium phosphate is reacted at elevated temperature with sodium carbonate in a vertical column having vapor-liquid contact means to produce an aqueous solution of sodium ammonium phosphate having a reduced carbon dioxide content. The sodium ammonium phosphate solution is treated in a second such column at elevated temperature and pressure to produce ammonia and an ammonia-free solution of alkali metal orthophosphate having a desired alkali metal to phosphorus molar ratio.
    Type: Grant
    Filed: December 30, 1974
    Date of Patent: February 17, 1976
    Assignee: Olin Corporation
    Inventor: Bernard H. Nicolaisen
  • Patent number: 3936304
    Abstract: When titanium phosphate is used as a white pigment to an article of which surface comprises polyolefin composition, the article is remarkably whitened.
    Type: Grant
    Filed: October 12, 1973
    Date of Patent: February 3, 1976
    Inventors: Tsuneo Kasugai, Nobuhiko Minagawa, Yasushi Hamada, Yujiro Sugahara, Hiroyuki Naito
  • Patent number: 3935297
    Abstract: A process of carbo-chlorination of AlPO.sub.4 wherein AlPO.sub.4 or AlPO.sub.4 -containing material is introduced into a reactor along with chlorinating agents and a source of carbon. The reactor is heated to approximately 600.degree. to 1200.degree.C and forms aluminum chlorides, phosphorous oxides, phosphorous chlorides, phosphorous oxychlorides and carbon oxides. These reaction products are then separated into three fractions by condensation, the first fraction being P.sub.2 O.sub.5, the second fraction being AlCl.sub.3 and AlCl.sub.3 .POCl.sub.3 and the third fraction being remaining gasses, namely PCl.sub.3, PCl.sub.5, P.sub.2 O.sub.3, CO and CO.sub.2. The second fraction is reacted in a further reactor to give AlCl.sub.3 and P.sub.2 O.sub.3 which are separated by distillation. The phosphorous chlorides from the third fraction are oxidized, along with the P.sub.2 O.sub.3 of the second fraction, to form P.sub.2 O.sub.5.
    Type: Grant
    Filed: December 19, 1973
    Date of Patent: January 27, 1976
    Assignee: Toth Aluminum Corporation
    Inventors: Alfred Lippman, Charles Toth, Roger Frank Sebenik