Hydrogen Containing Patents (Class 423/307)
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Patent number: 4450147Abstract: The disclosure relates to a process for making alkali metal hypophosphite solutions by reacting yellow phosphorus with an aqueous solution of an alkali metal hydroxide and/or carbonate. The disclosure provides more particularly for an aqueous hydrogen peroxide solution to be added to the mixture obtained by reacting the phosphorus with the alkali metal compound solution specified.Type: GrantFiled: February 8, 1983Date of Patent: May 22, 1984Assignee: Hoechst AktiengesellschaftInventors: Georg Elsner, Hermann Hack
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Patent number: 4400365Abstract: Aluminum zinc phosphate hydrates or basic aluminum zinc phosphate hydrates are manufactured by reacting 1 mole of aluminum hydrogen phosphate with from 2.4 to 4 moles of zinc oxide, if necessary with the addition of up to 0.4 moles of alkali aluminate or the equivalent quantity of alkali hydroxide. A 50% by weight acidic aluminum hydrogen phosphate solution is preferably used for the reaction which is carried out at an elevated temperature in the range from 30.degree. to 80.degree. C. The aluminum zinc phosphate hydrates produced by the method are useful anti-corrosion pigments for use in paints.Type: GrantFiled: December 1, 1981Date of Patent: August 23, 1983Assignees: Goslarer Farbenwerke, Dr. Hans Heubach GmbH & Co. KGInventors: Wigo Haacke, Gerhard Adrian, Manfred Gawol, Rainer Henbach, 37
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Patent number: 4386059Abstract: A substantially pure composition of matter and process for making the same which comprises a zinc hydroxy phosphite complex represented by the theoretical structural formula [2Zn(OH).sub.2. ZnHPO.sub.3 ].XZnO wherein X is a number from 0 to 17 and wherein the structure has infrared absorption frequencies at 3506; 3472; 3282; 3163; 2401; 2361; 1079; 947; 867; and 796 cm.sup.-1, .+-.4.0 cm.sup.-1, and X-ray diffraction d(A) spacings at 9.04; 5.94; 4.44; 3.58; 3.44; 3.38; 2.75; 2.70; and 1.67; .+-.0.02A.Type: GrantFiled: May 7, 1982Date of Patent: May 31, 1983Assignee: NL Industries, Inc.Inventors: William W. Reichert, Charles A. Cody, Carle H. Youngken
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Patent number: 4385041Abstract: The invention relates to a process for making aqueous alkali metal phosphate solutions by subjecting aqueous alkali metal phosphite solutions to catalytic oxidation with oxygen or air. More particularly, oxygen or air in stoichiometric excess proportions is introduced into the aqueous alkali metal phosphite solution at about 30.degree. to 110.degree. C., at a pH-value of 0 to about 8, and in the presence of SiO.sub.2 or aluminum silicate containing at most 10 weight % Al.sub.2 O.sub.3, for as long as necessary to achieve conversion of the alkali metal phosphite to alkai metal phosphate. After completion of the oxidation, the aqueous solution is separated from the catalyst.Type: GrantFiled: November 30, 1981Date of Patent: May 24, 1983Assignee: Hoechst AktiengesellschaftInventors: Klaus Jodden, Gero Heymer
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Patent number: 4380531Abstract: An improved process is provided for preparing highly purified phosphorus acid from industrial waste materials which are produced as by-products from the manufacture of sodium hypophosphite. Such industrial waste materials contain substantial quantities of calcium phosphite, and appreciable quantities of various metals such as iron, magnesium, aluminum and arsenic. The process of the present invention comprises, in a preferred embodiment thereof, reacting a slurry of said waste materials with sodium carbonate to produce calcium carbonate as a precipitate and a solution of sodium phosphite. The sodium phosphite solution is then passed through a cation ion exchange resin in the hydrogen form to produce a highly purified phosphorus acid product having significantly reduced quantities of metallic impurities.Type: GrantFiled: October 21, 1981Date of Patent: April 19, 1983Assignee: Occidental Chemical CorporationInventors: Joseph S. Wisnouskas, Roland Ho
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Patent number: 4374816Abstract: A process for producing hypophosphorous acid (H.sub.3 PO.sub.2) by reacting, in the absence of a catalyst and under an acidic condition, phosphine with an aqueous solution of hydrogen peroxide to produce an acid solution. The acid solution is then contacted with an non-transition metal hydroxide, oxide or carbonate, e.g. sodium hydroxide, to produce a product composition containing a hypophosphite, e.g. sodium hypophosphite (NaH.sub.2 PO.sub.2.H.sub.2 O). The process of this invention finds particular utility in processes of the type wherein phosphorus is reacted with an aqueous non-transition metal hydroxide composition, e.g. an aqueous suspension of a sodium hydroxide and calcium hydroxide, to produce a hypophosphite and byproduct phosphine. The process of this invention converts a substantial portion of the byproduct phosphine to hypophosphite.Type: GrantFiled: November 17, 1980Date of Patent: February 22, 1983Assignee: Stauffer Chemical CompanyInventors: Gregory G. Arzoumanidis, Kirk V. Darragh
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Patent number: 4346065Abstract: The invention relates to a process for making a finely dispersed, sparingly soluble salt of an oxyacid of phosphorus, having a maximum particle size of 20 .mu.m, by reacting a compound of a divalent metal with the oxyacid of phosphorus or an alkali metal or ammonium salt thereof. More particularly, finely dispersed salt consisting to an extent of at least 90% of particles with a size between 0.05 and 7 .mu.m is made. To this end, an at least 5% by weight aqueous solution or suspension of a compound of a divalent metal selected from the group Mg, Ca, Sr, Ba, Mn, Zn, Cu, Cd, Pb, Sn, Co and Ni is reacted, while maintaining a pH range of between 3 and 9 and while stirring, with an at least 2 mol % solution of at least one trivalent metal selected from the group Al, Fe and Cr in the oxyacid of phosphorus and, optionally, with an aqueous solution of an alkali metal or ammonium salt of the oxyacid of phosphorus, and the precipitated salt is separated off and dried.Type: GrantFiled: January 2, 1981Date of Patent: August 24, 1982Assignee: Hoechst AktiengesellschaftInventors: Alexander Maurer, Renate Adrian, Gero Heymer
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Patent number: 4320094Abstract: Alloy scrap containing refractory metals such as chromium, molybdenum, tungsten, vanadium, niobium and tantalum and base metals such as nickel, cobalt, copper and iron are treated to partition the refractory metal values from the base metal values without an energy intensive remelting step. The scrap in finely divided form is calcined in the presence of an oxygen containing gas and a member of a certain group of alkali metal salts at a temperature in the range of 800.degree. C. to 1150.degree. C. for 1/4 hour to four hours. This treatment converts the refractory metals to alkali metal molybdates, tungstates, chromates, vanadates, niobates and tantalates and the base metals to oxides. The calcined product may then be water leached to produce a substantially base metal-free liquor rich in refractory metal values. Both the refractory and the base metal values may be subsequently recovered by conventional hydrometallurgical techniques.Type: GrantFiled: April 15, 1980Date of Patent: March 16, 1982Assignee: Cabot CorporationInventors: Jameel Menashi, Alkis S. Rappas, Donald A. Douglas
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Patent number: 4294808Abstract: The invention relates to a process for making phosphorus-containing anticorrosive pigments having a size of at most 20 microns by reacting one or more compounds of magnesium, calcium, strontium, barium, zinc, aluminum, iron, chromium or manganese with an oxygen acid of phosphorus or its alkali metal or ammonium salts at temperatures within the range 10.degree. to 100.degree. C. More particularly pigments consisting to an extent of at least 90% of particles with a size between 0.05 and 8 microns are produced by introducing an aqueous suspension or solution of the reactants into a dispersing means rotating at a speed of 3000 to 10,000 rpm, reacting the reactants by intimately mixing them, and separating and drying precipitated pigment.Type: GrantFiled: September 17, 1979Date of Patent: October 13, 1981Assignee: Hoechst AktiengesellschaftInventors: Horst-Dieter Wasel-Nielen, Renate Adrian, Herbert Panter, Gero Heymer, Alexander Maurer, Raban von Schenck
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Patent number: 4278647Abstract: The invention relates to a process for making aqueous phosphorous acid solutions by admixing an aqueous sodium phosphite solution with hydrochloric acid. More specifically, phosphorous acid solutions substantially free from sodium in hydrochloric acid are produced by introducing hydrogen chloride, into the sodium phosphite solution until the latter is saturated therewith and separating precipitating sodium chloride from the resulting phosphorous acid solution in hydrochloric acid.Type: GrantFiled: July 25, 1979Date of Patent: July 14, 1981Assignee: Hoechst AktiengesellschaftInventors: Klaus Jodden, Hans-Werner Stephan, Gero Heymer
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Patent number: 4276273Abstract: Stable aqueous solutions of sodium polyphosphate useful in granulating dry solid cleaning composition components are formed by direct reaction of polyphosphoric acid with sodium carbonate generally at a temperature of about 50.degree. C. The reactants are used in an Na:P ratio of 1.2:1 to 1.5:1, and the product solution contains about 32 to about 37% w/w P.sub.2 O.sub.5 of which a high proportion is present as polyphosphate and has a pH of about 5 to about 6.5.Type: GrantFiled: August 11, 1980Date of Patent: June 30, 1981Assignee: ERCO Industries LimitedInventor: James D. McGilvery
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Patent number: 4268404Abstract: The invention relates to a long chain ammonium polyphosphate and its use as an effective additive in lubricants and/or coolants for metal working under extremely high pressures and temperatures. The polyphosphate chain preferably contains 50 to 1000 phosphorus atoms. Up to 20% of the ammonium groups are replaceable by hydrogen. The additive is preferably added to the lubricant/coolant in a proportion of 0.1 to 30 weight %.Type: GrantFiled: November 13, 1979Date of Patent: May 19, 1981Assignee: Hoechst AktiengesellschaftInventors: Michael Ahlgrim, Gerhard Mietens, Franz-Josef Dany, Joachim Kandler
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Patent number: 4265866Abstract: A process for producing hypophosphorous acid (H.sub.3 PO.sub.2) by reacting, in the absence of a catalyst and under an acidic condition, phosphine with an aqueous solution of hydrogen peroxide to produce an acid solution. The acid solution is then contacted with an non-transition metal hydroxide, oxide or carbonate, e.g. sodium hydroxide, to produce a product composition containing a hypophosphite, e.g. sodium hypophosphite (NaH.sub.2 PO.sub.2.H.sub.2 O). The process of this invention finds particular utility in processes of the type wherein phosphorus is reacted with an aqueous non-transition metal hydroxide composition, e.g. an aqueous suspension of a sodium hydroxide and calcium hydroxide, to produce a hypophosphite and byproduct phosphine. The process of this invention converts a substantial portion of the byproduct phosphine to hypophosphite.Type: GrantFiled: May 3, 1979Date of Patent: May 5, 1981Assignee: Stauffer Chemical CompanyInventors: Gregory G. Arzoumanidis, Kirk V. Darragh
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Patent number: 4258022Abstract: The invention relates to the continuous production of phosphine. To this end, elemental phosphorus is reacted with an aqueous alkali metal hydroxide solution and at least one alcohol, the reactants being used in admixture with 0.01 to 2 weight % of a surfactant, the percentage being based on the alcohol.Type: GrantFiled: September 12, 1979Date of Patent: March 24, 1981Assignee: Hoechst AktiengesellschaftInventors: Georg Elsner, Werner Klose, Christian May, Gero Heymer
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Patent number: 4196136Abstract: Salts and acids containing a triheteropolyanion in which one addenda atom of a heterododecatungstate or heterododecamolybdate is replaced by one tin atom or by two germanium atoms, in which the tin atom or the germanium atoms are bonded to a ligated transition metal, have outstanding utility as catalysts for the oligomerization of terephthalic acid with ethylene glycol, and for the isomerization of 1-butene, and for the dehydration of 2-butanol and subsequent isomerization of the 1-butene formed.Type: GrantFiled: November 6, 1978Date of Patent: April 1, 1980Assignee: E. I. Du Pont de Nemours and CompanyInventor: Walter H. Knoth, Jr.
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Patent number: 4088738Abstract: A method of making phosphoric acid and gypsum through a precipitated phosphate intermediary which comprises mixing a precipitated dicalcium phosphate with a highly dispersed reaction admixture of sulfuric acid and phosphoric acid, at a temperature between about 25.degree. and 80.degree. C; and withdrawing and separating phosphoric acid containing up to about 45% or more P.sub.2 O.sub.5 and gypsum containing generally less than 0.25% P.sub.2 O.sub.5. The resultant gypsum is highly filterable and very low in occluded phosphate value. Preferably, the process involves first obtaining a weak phosphoric acid solution from and by leaching as-mined phosphate mineral containing material to obtain the precipitated dicalcium phosphate; and then converting the precipitated phosphate by the process to the strong phosphoric acid solution.Type: GrantFiled: April 8, 1976Date of Patent: May 9, 1978Assignee: United States Gypsum CompanyInventor: Douglas O. Hauge
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Patent number: 4046858Abstract: A new synthesis is disclosed which produces synthetic crystalline hydroxyapatite. The process comprises reacting anhydrous trisodium phosphate wih calcium chloride in a formamide/water solution. Good yields of hydroxyapatite are obtained quickly, simply, and at low temperatures.Type: GrantFiled: July 24, 1974Date of Patent: September 6, 1977Inventors: John J. Barsa, Edward T. Farris, Richard J. Lagow
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Patent number: 3981970Abstract: 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: GrantFiled: July 16, 1971Date of Patent: September 21, 1976Assignee: Takeda Chemical Industries, Ltd.Inventors: Takeo Wada, Kazuo Okada
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Patent number: 3965245Abstract: A selected ammonium phosphate is reacted at elevated temperature and pressure with sodium hydroxide in a vertical column having vapor-liquid contact means to produce an alkali metal orthophosphate having a low alkali metal/P molar ratio which is substantially free of ammonia. Ammonia is taken overhead.Type: GrantFiled: December 30, 1974Date of Patent: June 22, 1976Assignee: Olin CorporationInventor: Bernard H. Nicolaisen
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Patent number: 3956462Abstract: 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: GrantFiled: March 18, 1974Date of Patent: May 11, 1976Assignee: Hoechst AktiengesellschaftInventors: Gero Heymer, Wolfgang Scheibitz, Hasso Spott
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Patent number: 3947332Abstract: Heteropoly acids of tungsten and molybdenum, such as tungstosilicic acid and molybdosilicic acid, are produced by first preparing an aqueous solution of an alkali metal tungstate or molybdate and an alkali metal salt of the hetero atom, and then removing the alkali metal cations from the solution by means of a cation exchange membrane under the influence of an applied electrical potential, whereby the reactive tungstate or molybdate and hetero species anions react to form the desired heteropoly acid.Type: GrantFiled: June 7, 1974Date of Patent: March 30, 1976Assignee: GTE Sylvania IncorporatedInventors: Clarence D. Vanderpool, James C. Patton, Jr., Tai K. Kim, Martin B. MacInnis
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Patent number: T962001Abstract: dicalcium phosphate is prepared from phosphate rock by a process which comprises reacting phosphate rock with sulfur dioxide and an organic carbonyl compound for 0.5 to 10 hours while maintaining the temperature of the reaction mixture below 50.degree. C. The reaction yields a mixture of gangue, solid calcium .alpha.-hydroxy sulfonate and soluble dicalcium phosphate. The solids are separated from the liquid and P.sub.2 O.sub.5 values adhering to the solid are washed free with a mixture of carbonyl, water, and sulfur dioxide. The wash effluent is recycled to the process and both carbonyl and some sulfur dioxide are recovered from the filter cake by heating it. The offgas from the heated filter cake is recycled to the process and the dry filter cake, now largely calcium sulfite hemihydrate, is discarded.Dicalcium phosphate is precipitated from the reaction mixture filtrate in high yield by partially distilling sulfur dioxide from the filtrate.Type: GrantFiled: October 6, 1976Date of Patent: September 6, 1977Assignee: Tennessee Valley AuthorityInventors: John F. McCullough, John F. Phillips, Jr., Leslie R. Tate