Phosphoric Or Sulfuric Acid Patents (Class 203/35)
  • Patent number: 4435595
    Abstract: 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: Grant
    Filed: April 26, 1982
    Date of Patent: March 6, 1984
    Assignee: Eastman Kodak Company
    Inventors: Victor H. Agreda, Lee R. Partin
  • Patent number: 4434301
    Abstract: Crude isophorone is refined by contacting it with aqueous caustic followed by washing and fractional distillation.
    Type: Grant
    Filed: August 25, 1982
    Date of Patent: February 28, 1984
    Assignee: Union Carbide Corporation
    Inventor: Anthony J. Papa
  • Patent number: 4395311
    Abstract: 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: Grant
    Filed: November 30, 1981
    Date of Patent: July 26, 1983
    Assignee: The Dow Chemical Company
    Inventor: Charles J. McDonald
  • Patent number: 4388154
    Abstract: 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: Grant
    Filed: May 1, 1981
    Date of Patent: June 14, 1983
    Assignee: BASF Aktiengesellschaft
    Inventors: Waldheim Hochstein, Gerd Kaibel, Franz-Josef Mueller, Horst Hartmann
  • Patent number: 4383893
    Abstract: 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: Grant
    Filed: April 20, 1981
    Date of Patent: May 17, 1983
    Assignee: BASF Aktiengesellschaft
    Inventors: Gerd Kaibel, Horst Hartmann, Waldhelm Hochstein, Franz-Josef Mueller
  • Patent number: 4350572
    Abstract: 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: Grant
    Filed: November 6, 1980
    Date of Patent: September 21, 1982
    Assignee: BASF Aktiengesellschaft
    Inventors: Rudolf Kummer, Volker Taglieber, Franz-Josef Weis, Heinz-Walter Schneider
  • Patent number: 4336109
    Abstract: 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: Grant
    Filed: May 19, 1980
    Date of Patent: June 22, 1982
    Assignee: Sumitomo Chemical Company, Limited
    Inventors: Hirokazu Hosaka, Kenji Tanimoto, Kunihiko Tanaka, Toshiharu Morita, Katsuyuki Shiota, Yuji Ueda, Seiichi Kai
  • Patent number: 4330374
    Abstract: 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: Grant
    Filed: September 7, 1979
    Date of Patent: May 18, 1982
    Assignee: General Atomic Company
    Inventors: Dennis R. O'Keefe, Kenneth H. McCorkle, Jr., Johannes D. de Graaf
  • Patent number: 4306943
    Abstract: 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: Grant
    Filed: March 12, 1981
    Date of Patent: December 22, 1981
    Assignee: Dai-Ichi Kogyo Seiyaku Co., Ltd.
    Inventors: Shigeo Mori, Takeshi Fujita
  • Patent number: 4298622
    Abstract: 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: Grant
    Filed: April 3, 1979
    Date of Patent: November 3, 1981
    Assignee: Vitamins, Inc.
    Inventors: Laxman Singh, Wayne K. Rice
  • Patent number: 4268361
    Abstract: 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: Grant
    Filed: May 19, 1980
    Date of Patent: May 19, 1981
    Assignee: The B. F. Goodrich Company
    Inventor: Pradeep V. Patel
  • Patent number: 4264501
    Abstract: 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: Grant
    Filed: May 4, 1978
    Date of Patent: April 28, 1981
    Assignee: Stamicarbon, B.V.
    Inventors: Edmond H. J. P. Bour, Sijbrandus E. Schaafsma, Jean M. M. Warnier
  • Patent number: 4248673
    Abstract: 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: Grant
    Filed: January 30, 1979
    Date of Patent: February 3, 1981
    Assignee: Produits Chimiques Ugine Kuhlmann
    Inventors: Bernard Cheminal, Paul Kiener
  • Patent number: 4236973
    Abstract: 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: Grant
    Filed: May 14, 1979
    Date of Patent: December 2, 1980
    Assignee: The Dow Chemical Company
    Inventor: Lanny A. Robbins
  • Patent number: 4191615
    Abstract: 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: Grant
    Filed: December 23, 1977
    Date of Patent: March 4, 1980
    Assignee: Krupp-Koppers GmbH
    Inventors: Martin Schulze, Gerhard Preusser
  • Patent number: 4167525
    Abstract: 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: Grant
    Filed: July 10, 1978
    Date of Patent: September 11, 1979
    Assignee: Sumitomo Chemical Company, Limited
    Inventors: Yushin Kataoka, Shojiro Itoh, Masahiro Niwano
  • Patent number: 4158611
    Abstract: 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: Grant
    Filed: December 15, 1977
    Date of Patent: June 19, 1979
    Assignee: BP Chemicals Limited
    Inventor: Maurice D. Cooke
  • Patent number: 4154658
    Abstract: 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: Grant
    Filed: July 3, 1978
    Date of Patent: May 15, 1979
    Assignee: The United States of America as represented by the Secretary of the Navy
    Inventor: George W. Nauflett
  • Patent number: 4113848
    Abstract: 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: Grant
    Filed: May 14, 1976
    Date of Patent: September 12, 1978
    Assignee: Anumin Pty. Limited
    Inventors: Alan James Parker, Winfield Earle Waghorne, Dion Ewing Giles, John Howard Sharp, Robert Alexander, David Michael Muir
  • Patent number: 4050994
    Abstract: 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: Grant
    Filed: November 26, 1976
    Date of Patent: September 27, 1977
    Assignee: Chevron Research Company
    Inventor: Byron E. Anshus
  • Patent number: 4033829
    Abstract: 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: Grant
    Filed: December 15, 1975
    Date of Patent: July 5, 1977
    Assignee: Monsanto Company
    Inventors: Thomas D. Higgins, Jr., Raymond A. Newsom
  • Patent number: 4002539
    Abstract: 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: Grant
    Filed: September 23, 1974
    Date of Patent: January 11, 1977
    Assignee: BASF Aktiengesellschaft
    Inventors: Max Strohmeyer, Werner Hagen, Heinz Hohenschutz
  • Patent number: 3966890
    Abstract: 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: Grant
    Filed: December 17, 1974
    Date of Patent: June 29, 1976
    Assignee: Anumin Pty. Limited
    Inventors: Alan James Parker, Winfield Earle Waghorne, Dion Ewing Giles, John Howard Sharp, Robert Alexander, David Michael Muir
  • Patent number: 3961028
    Abstract: 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: Grant
    Filed: December 17, 1974
    Date of Patent: June 1, 1976
    Assignee: Anumin Pty. Limited
    Inventors: Alan James Parker, Winfield Earle Waghorne, Dion Ewing Giles, John Howard Sharp, Robert Alexander, David Michael Muir