# US 5,349,084 A · Process for recovering high-purity organic acid > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,349,084 A - Document ID: US5349084A - Status: Granted - Kind: A - Application number: 07/765,582 - Filed: 1991-09-25 - Granted: 1994-09-20 - Earliest claimed: 1990-09-28 - Assignees: Idemitsu Petrochemical Co., Ltd. - Inventors: Akihiro Shishikura; Hiroshi Kimbara; Katsuhisa Yamaguchi; Kunio Arai - Web page: https://patentgrep.com/patent/US5349084A ## CPC - C07C 51/48: by liquid-liquid treatment - C07C 51/42: Separation; Purification; Stabilisation; Use of additives - C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS ## Abstract The present invention relates to a process for inexpensively and effectively recovering a high-purity organic acid, according to which a crude organic acid is subjected to extraction treatment with an organic solvent to obtain an organic solvent extract containing an organic acid; the organic solvent extract is mixed with a high-pressure gas to precipitate and separate impurities thereby obtaining a solution containing a high-purity organic acid; and the organic acid is separated from the solution to obtain a high-purity organic acid. ## Claims ### Claim 1 A process for recovering a high-purity organic acid, which comprises (a) subjecting a crude organic acid mixture comprising an organic acid, said organic acid comprising a carboxylic acid having 3 to 20 carbon atoms which is a product of a fermentation process, to an extraction treatment with an organic solvent selected from the group consisting of alcohols, ketones and ethers to obtain an organic solvent extract containing the organic acid; (b) mixing the organic solvent extract with a high-pressure gas, said high pressure gas having a pressure not higher than critical pressure, said high pressure gas being selected from the group consisting of CO.sub.2, ethylene, propylene, N.sub.2 O and fluoromethane to precipitate and separate impurities, thereby obtaining a solution containing a high-purity organic acid; and (c) separating the organic acid from the solution. ### Claim 2 (depends on 1) The process according to claim 1, wherein the crude organic acid is at least one member selected from the group consisting of fermented koji or grain obtained by surface-fermentation of starch pulp or molasses in the presence of a microorganism of a known fungus genus; an organic acid aqueous solution obtained by subjecting the above fermented koji or grain to extraction with hot water; and a broth of submerged fermentation obtained by submerged fermentation of starch pulp or molasses in the presence of a microorganism of a known fungus genus. ### Claim 3 (depends on 1) The process according to claim 1, wherein the crude organic acid contains 0.5 to 50% by weight of an organic acid. ### Claim 4 (depends on 1) The process according to claim 1, wherein the carboxylic acid is at least one member selected from the group consisting of citric acid, malic acid and lactic acid. ### Claim 5 (depends on 2) The process according to claim 2, wherein the fermented koji or grain as a crude organic acid is dehydrated to a water content of 3 to 30% by weight before the extraction treatment with an organic solvent. ### Claim 6 (depends on 2) The process according to claim 2, wherein the organic acid aqueous solution or the broth of submerged fermentation as a crude organic acid is dehydrated to a water content of 3 to 30% by weight before the extraction treatment with an organic solvent. ### Claim 7 (depends on 1) The process according to claim 1, wherein the extraction treatment with an organic solvent is carried out at a temperature between 20.degree. C. and 40.degree. C. ### Claim 8 (depends on 5, 6) The process according to claim 5 or 6, wherein the organic solvent is used in an amount which is 2 to 20 times as large as that of a dehydrated organic acid. ### Claim 9 (depends on 1) The process according to claim 1, wherein the impurities formed are separated by filtration after the extraction treatment with an organic solvent. ### Claim 10 (depends on 1) The process according to claim 1, wherein the high-pressure gas to be mixed with the organic solvent extract is a hydrophobic and low-polarity high-pressure gas. ### Claim 11 (depends on 1) The process according to claim 1, wherein the organic solvent extract and the high-pressure gas are mixed at a temperature between 0.degree. C. and 80.degree. C. ### Claim 12 (depends on 1) The process according to claim 1, wherein the organic solvent extract and the high-pressure gas are mixed at a pressure which is between 1 kg/cm.sup.2 G and 150 kg/cm.sup.2 G. ### Claim 13 (depends on 1) The process according to claim 1, wherein the high-pressure gas and the organic solvent extract have a high-pressure gas/organic solvent extract weight ratio of 0.1/1 to 5/1. ### Claim 14 (depends on 1) The process according to claim 1, wherein the organic solvent is at least one alcohol selected from the group consisting of methanol, ethanol, propanol, isopropanol and butanol. ### Claim 15 (depends on 1) The process according to claim 1, wherein the organic solvent is at least one ketone selected from the group consisting of acetone and methylethylketone. ### Claim 16 (depends on 1) The process according to claim 1, wherein the organic solvent is at least one ether selected from the group consisting of diethylether and petroleum ether. ### Claim 17 (depends on 3) The process according to claim 3, wherein the carboxylic acid is selected from the group consisting of citric acid, malic acid and lactic acid; the extraction treatment is carried out at a temperature of 20.degree. C. to 40.degree. C.; the organic solvent extract and the high-pressure gas are mixed at a temperature of 0.degree. C. to 80.degree. C. and at a pressure which is not higher than critical pressure and between 1 kg/cm.sup.2 G and 150 kg/cm.sup.2 G; the high-pressure gas and the organic solvent extract have a high-pressure gas/organic solvent extract weight ratio of 0.1/1 to 5/1; and the organic solvent is in an amount which is 2 to 20 times as large as that of a dehydrated organic acid. ### Claim 18 (depends on 1) The process according to claim 1, wherein the high pressure gas is CO.sub.2 at a pressure of 5 to 70 kg/cm.sup.2 G. ### Claim 19 (depends on 17) The process according to claim 17, wherein the high pressure gas is CO.sub.2 at a pressure of 5 to 70 kg/cm.sup.2 G.