Phosphoric Or Sulfuric Acid Patents (Class 203/35)
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Patent number: 4435595Abstract: The present invention provides a process for the production of high purity methyl acetate from methanol and glacial acetic acid wherein the acetic acid functions both as a reactant and as an extractive agent. The process comprises countercurrently flowing approximately stoichiometric quantities of acetic acid and methanol through a single reactive distillation column in the presence of an acidic catalyst which is preferably sulfuric acid. The column provides intimate contact between the acetic acid and the methanol and between the acetic acid and the azeotropes (methyl acetate/water and methyl acetate/methanol) which are formed in the column. At preferred catalyst concentrations, the residence time in the column is at least about two hours. The process further comprises continuously removing high purity methyl acetate from the top of the column and continuously removing water from the bottom of the column.Type: GrantFiled: April 26, 1982Date of Patent: March 6, 1984Assignee: Eastman Kodak CompanyInventors: Victor H. Agreda, Lee R. Partin
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Patent number: 4434301Abstract: Crude isophorone is refined by contacting it with aqueous caustic followed by washing and fractional distillation.Type: GrantFiled: August 25, 1982Date of Patent: February 28, 1984Assignee: Union Carbide CorporationInventor: Anthony J. Papa
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Patent number: 4395311Abstract: Crude aminomethanols are converted to salt form by the addition of a strong acid and subsequently distilled under vacuum. The resulting purified aminomethanol is essentially free of unreacted aldehydes and other volatile impurities.Type: GrantFiled: November 30, 1981Date of Patent: July 26, 1983Assignee: The Dow Chemical CompanyInventor: Charles J. McDonald
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Patent number: 4388154Abstract: A process is provided wherein acetaldehyde and methanol are obtained from reaction mixtures which result from the homologization of methanol and which in addition to acetaldehyde essentially contain acetaldehyde dimethylacetal, methanol, methyl acetate and water.Type: GrantFiled: May 1, 1981Date of Patent: June 14, 1983Assignee: BASF AktiengesellschaftInventors: Waldheim Hochstein, Gerd Kaibel, Franz-Josef Mueller, Horst Hartmann
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Patent number: 4383893Abstract: Liquid mixtures containing aliphatic alcohols are separated, by distillation, into a higher-boiling alcohol-containing fraction and a lower-boiling fraction containing the other liquids, by carrying out the fractionation in the presence of water and of an alkanal and, over about 3/4 of the column height, in the presence of a non-volatile or only slightly volatile acid.Type: GrantFiled: April 20, 1981Date of Patent: May 17, 1983Assignee: BASF AktiengesellschaftInventors: Gerd Kaibel, Horst Hartmann, Waldhelm Hochstein, Franz-Josef Mueller
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Patent number: 4350572Abstract: A process for purifying carboxylic acid esters which have been obtained by reacting olefinically unsaturated compounds with carbon monoxide and alkanols and which contain aldehydes or acetals, wherein the said esters are treated with a strongly acidic agent, with or without addition of water.Type: GrantFiled: November 6, 1980Date of Patent: September 21, 1982Assignee: BASF AktiengesellschaftInventors: Rudolf Kummer, Volker Taglieber, Franz-Josef Weis, Heinz-Walter Schneider
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Patent number: 4336109Abstract: Acetone having a markedly low content of aldehydes is recovered from an aqueous rectification residue brought about by rectification of crude acetone carried out after one crude acetone having been alkali-treated or while an alkali or an aqueous solution thereof being added to the crude acetone, by mixing the aqueous rectification residue with an alkali, neutralizing the mixture to a pH of 4 to 9, and then subjecting the resulting mixture to distillation to obtain acetone as a distillate.Type: GrantFiled: May 19, 1980Date of Patent: June 22, 1982Assignee: Sumitomo Chemical Company, LimitedInventors: Hirokazu Hosaka, Kenji Tanimoto, Kunihiko Tanaka, Toshiharu Morita, Katsuyuki Shiota, Yuji Ueda, Seiichi Kai
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Patent number: 4330374Abstract: Relatively dry hydrogen iodide can be recovered from a mixture of HI, I.sub.2 and H.sub.2 O. After the composition of the mixture is adjusted so that the amounts of H.sub.2 O and I.sub.2 do not exceed certain maximum limits, subjection of the mixture to superatmospheric pressure in an amount equal to about the vapor pressure of HI at the temperature in question causes distinct liquid phases to appear. One of the liquid phases contains HI and not more than about 1 weight percent water. Often the adjustment in the composition will include the step of vaporization, and the distinct layers appear following the increase in pressure of the vapor mixture. Adjustment in the composition may also include the addition of an extraction agent, such as H.sub.3 PO.sub.4, and even though the adjusted composition mixture contains a significant amount of such an agent, the creation of the distinct liquid phases is not adversely affected.Type: GrantFiled: September 7, 1979Date of Patent: May 18, 1982Assignee: General Atomic CompanyInventors: Dennis R. O'Keefe, Kenneth H. McCorkle, Jr., Johannes D. de Graaf
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Patent number: 4306943Abstract: Crude liquid polyether-polyols containing an alkaline catalyst are purified by the steps of:neutralizing said crude liquid polyether-polyol with a mineral acid having a dissociation constant of greater than 10.sup.-3 at 25.degree. C.distilling off water from said liquid, and filtering the same. The improvement resides in the step of adding a hydrate of a metal salt of said mineral acid to the liquid polyether-polyol at a stage before the distillation step for promoting the crystal growth of a salt formed from said alkaline catalyst by the neutralization.Type: GrantFiled: March 12, 1981Date of Patent: December 22, 1981Assignee: Dai-Ichi Kogyo Seiyaku Co., Ltd.Inventors: Shigeo Mori, Takeshi Fujita
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Patent number: 4298622Abstract: Wheat germ oil is treated by degumming with phosphoric acid and water, bleaching with activated clay and distilled in a centrifugal molecular still at 140.degree.-200.degree. C. at pressures below 50 milli-torr. The free fatty acids which are removed by the distillation step may be recovered as valuable by-products. The phospholipids removed in the degumming step may be recovered as valuable by-products. A vitamin E concentrate may be prepared by further distilling the purified wheat germ oil at 220.degree.-300.degree. C. at pressures below 25 milli-torr.Type: GrantFiled: April 3, 1979Date of Patent: November 3, 1981Assignee: Vitamins, Inc.Inventors: Laxman Singh, Wayne K. Rice
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Patent number: 4268361Abstract: Formation of butadiene-1,3 polymer during the extractive distillation of a C-4 hydrocarbon mixture to separate and purify butadiene-1,3 using a solvent composition in which an alkoxynitrile is present in a proportion of 50-99 percent by weight, is decreased through inclusion in the solvent of a synergistic combination of 2,4-dinitrophenol and phosphoric acid, each in a proportion of 0.05 to 0.5 percent by weight.Type: GrantFiled: May 19, 1980Date of Patent: May 19, 1981Assignee: The B. F. Goodrich CompanyInventor: Pradeep V. Patel
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Patent number: 4264501Abstract: A process is described for the recovery of 2-pyrrolidone monomer from polypyrrolidone waste material by heating the latter in the presence of a small amount of strong acid, and distilling off the said monomer.Type: GrantFiled: May 4, 1978Date of Patent: April 28, 1981Assignee: Stamicarbon, B.V.Inventors: Edmond H. J. P. Bour, Sijbrandus E. Schaafsma, Jean M. M. Warnier
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Patent number: 4248673Abstract: A process for obtaining colorless and stable isophorone is characterized by distilling a raw synthesis mixture to remove alkaline agents, acetone, and a major portion of the water which is present, thermally treating the distilled mixture with an acidic ion-exchanging resin, neutralizing the effluent following said thermal treatment with an excess of an alkaline agent, adding water in a volume sufficient to dissolve any salts which may have formed, then again, neutralizing the now alkaline mixture wherein the pH of the resultant mixture is between 6.5 and 7, washing the mixture in water by decantation, and distilling the mixture under reduced pressure.Type: GrantFiled: January 30, 1979Date of Patent: February 3, 1981Assignee: Produits Chimiques Ugine KuhlmannInventors: Bernard Cheminal, Paul Kiener
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Patent number: 4236973Abstract: Organic material having a normal boiling point in excess of 200.degree. C. and a relative volatility with respect to water of at least one is removed from water contaminated therewith. The process comprises passing a current of vapor, sufficient to vaporize at least a portion of the organic material, through a moving stream of the contaminated water. In a preferred embodiment, the process comprises adjusting the pH of the contaminated water to a level sufficient to prevent substantial dissociation of the organic material. The contaminated water is then countercurrently contacted with a sufficient vapor flow to vaporize at least a portion of the organic material. The resulting organic material-containing vapor can be recovered, and the organic material removed. Illustrative of the process is the removal by air stripping of pentachlorophenol from waste water contaminated with about 250 parts per billion thereof.Type: GrantFiled: May 14, 1979Date of Patent: December 2, 1980Assignee: The Dow Chemical CompanyInventor: Lanny A. Robbins
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Patent number: 4191615Abstract: In order to prevent corrosion of the apparatus in extraction and extractive distillation processes where N-substituted morpholine is employed as the selective solvent an additive is added to the solvent which additive consists of (a) phosphoric acid, (b) a salt thereof, (c) a vanadium compound, (d) a molybdenum compound or (e) a mixture of two or more of these compounds, the addition being effected in an amount of about 0.005 to 0.02% by weight of the morpholine solvent.Type: GrantFiled: December 23, 1977Date of Patent: March 4, 1980Assignee: Krupp-Koppers GmbHInventors: Martin Schulze, Gerhard Preusser
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Patent number: 4167525Abstract: An aromatic acyl chloride is obtained with industrial advantages by reacting an aromatic carboxylic acid, phosphorus trichloride and chlorine, treating the reaction mixture comprising by-produced phosphorus pentachloride with at least one treating agent selected from water and phosphorus compounds to convert the phosphorus pentachloride into phosphorus oxychloride, and then subjecting the resulting reaction mixture to distillation to obtain the desired aromatic acyl chloride.Type: GrantFiled: July 10, 1978Date of Patent: September 11, 1979Assignee: Sumitomo Chemical Company, LimitedInventors: Yushin Kataoka, Shojiro Itoh, Masahiro Niwano
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Patent number: 4158611Abstract: Crude phenol is recovered from CHP reaction products by continuously feeding to a main column separating in its uppermost section phenol from crude acetone, this fraction being removed overhead, and in the lower section crude phenol from higher boilers, including acetophenone and carbinol, the crude phenol being removed as a sidestream fraction from the main column at a point in the column above the feed-point wherein the total concentration of acetophenone plus carbinol is less than 1,000 ppm and the higher boiling compounds being removed as a base fraction.Type: GrantFiled: December 15, 1977Date of Patent: June 19, 1979Assignee: BP Chemicals LimitedInventor: Maurice D. Cooke
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Patent number: 4154658Abstract: The formaldehyde hydrazone of UDMH can be removed from an aqueous solution f UDMH by codistillation with a hydrocarbon or other solvent which is inert to both acidic or basis mediums. The solvent can then be recovered from the hydrazone solution by washing with an acid solution and the solvent can be reused.Type: GrantFiled: July 3, 1978Date of Patent: May 15, 1979Assignee: The United States of America as represented by the Secretary of the NavyInventor: George W. Nauflett
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Patent number: 4113848Abstract: Copper is processed via solutions of copper salts, both cupric and cuprous, in acidified aqueous solutions containing organic nitriles. Methods of producting solutions of cuprous salts include reduction of cupric salts and oxidation of copper and copper sulphides. Solutions of cuprous salts are thermally or electrochemically disproportionated to produce copper and solutions of cupric salts.Type: GrantFiled: May 14, 1976Date of Patent: September 12, 1978Assignee: Anumin Pty. LimitedInventors: Alan James Parker, Winfield Earle Waghorne, Dion Ewing Giles, John Howard Sharp, Robert Alexander, David Michael Muir
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Patent number: 4050994Abstract: A two-stage evaporative method for recovering polymerizable 2-pyrrolidone from alkaline aqueous solutions such as those obtained by washing the catalyst from an incompletely reacted polypyrrolidone polymerizate, includes the steps of neutralizing the base with mineral acid, removing most of the water in an initial reduced pressure evaporation and recovering the pyrrolidone from a salt/pyrrolidone slurry by vaporization under reduced pressure.Type: GrantFiled: November 26, 1976Date of Patent: September 27, 1977Assignee: Chevron Research CompanyInventor: Byron E. Anshus
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Patent number: 4033829Abstract: Styrene is inhibited against polymerization during the distillation thereof by incorporating therein, in an amount sufficient to inhibit polymerization thereof, the dinitrophenol solution recovered from styrene still residues or tars resulting from the distillation of styrene in the presence of dinitrophenol. The recovered dinitrophenol solution is a more effective polymerization inhibitor than dinitrophenol per se.Type: GrantFiled: December 15, 1975Date of Patent: July 5, 1977Assignee: Monsanto CompanyInventors: Thomas D. Higgins, Jr., Raymond A. Newsom
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Patent number: 4002539Abstract: A process for isolating carboxylic acids from residues of the oxo reaction which are obtained as residues, on hydroformylation of ethylene or propylene, optionally after removing a part of the aldehydes produced, subsequent hydrogenation, treatment with aqueous alkali metal hydroxide solutions and subsequent distillation, wherein the residues are acidified with strong mineral acids to a pH of from 2-4, the acidified mixture not containing more than 5 parts by weight of water per part by weight of the carboxylic acids contained in the mixture, the organic phase is then separated off and the carboxylic acids are isolated therefrom by distillation at pressures below 150 mbar. The carboxylic acids obtained can be used as solvents or for the manufacture of esters.Type: GrantFiled: September 23, 1974Date of Patent: January 11, 1977Assignee: BASF AktiengesellschaftInventors: Max Strohmeyer, Werner Hagen, Heinz Hohenschutz
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Patent number: 3966890Abstract: Methods of reducing aqueous solutions of cupric sulfate to cuprous solutions by using organic nitrile compositions are disclosed. The particular nitrile used is acetonitrile and the reductant is sulphur dioxide. The method has application commercially to leaching ores containing oxidised copper to obtain cuprous ion solutions. Such solutions can be treated by electrochemical or thermal disproportionation methods to obtain very pure copper.Type: GrantFiled: December 17, 1974Date of Patent: June 29, 1976Assignee: Anumin Pty. LimitedInventors: Alan James Parker, Winfield Earle Waghorne, Dion Ewing Giles, John Howard Sharp, Robert Alexander, David Michael Muir
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Patent number: 3961028Abstract: Method of preparing cuprous sulfate and bisulfate solutions from materials containing copper and impurities by a leaching process are disclosed. The leaching composition contains sulfuric acid, cupric ions, water and an organic nitrile. The leaching composition may be used with copper sulfide ores in particulate form. The cuprous solutions resulting from the leaching can be treated by disproportionation methods to recover pure copper.Type: GrantFiled: December 17, 1974Date of Patent: June 1, 1976Assignee: Anumin Pty. LimitedInventors: Alan James Parker, Winfield Earle Waghorne, Dion Ewing Giles, John Howard Sharp, Robert Alexander, David Michael Muir