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    9 views7 pages

    BASF Acid Formic

    Uploaded by

    alfin

    Copyright:

    © All Rights Reserved
    Download as PDF or read online from Scribd
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    US006713649BL a2) United States Patent (0) Patent No: US 6,713,649 BL Hladiy et al. (45) Date of Patent: Mar. 30, 2004 (54) METHOD FOR PRODUCTION OF FORMIC 4326073 A 4082. Wolf th ACID 4561390 A © 41996 Dizckelmann ea... S89526 (15) lnventors: Serhly Hla, Borystav (UA); FOREIGN PATENT DOCUMENTS Myktiylo Starchevskyy, Borylav i” vive nem (UA); Yuriy Pazderskyy, Boryslav (WA); Yaroslav Lastovyak, Deobobyeh «ed py examinee (UA) (73) Assignee: BASF Aktiengesellschatft, Primary Examiner—Sbailendra Kumat Ludwigshafen (DE) Assistant Examiner—Karl Pulte, (74) Attorney, Agent, or Firm—Keil & Weinkaut (4) Notice: Subject to any disclaimer the term of his " patent is extended or adjusted under 35. (57) ABSTRACT US.C. 154(0) by 46 days. aes The invention relates to a process for the preparation of 1) Appl. No: 10/129,511 formic acid, comprising the following steps: PCT Filed = 4) hydrolysis of methyl formate to give a mixture of water, oD eat A) formic acid, methanol and excess methyl formate; (86) PCT No. PCT/EPOI/11046 +) removal of the methanol and excess methyl formate from the mixture of water, formic acid, methanol and $371 (XA), ; ; © dae: May 6, 2002 excess methyl formate by distillation (0 give aqueous formic acid (81) PCT Pub, Nos WOOU3HS4S «) extraction of the aqueous formic acid with at last one , = formic acd ester give a mixture of said at last one cena ame formic acid ester and formic acids (30) Foreign Application Priority Data 4) separation of said at least one formic acid ester and necatiooniany featsatnaat formic acid by distillation, (51) Int. C1? COTE §3/02; CO7B 53/00 ‘The process according tothe invention enables gentle prepa (2) U 362/609; 562/606 ration of formie acid. Only very slight decomposition of (58) Field of Search 362/606, 609; formic acid occurs, and the formic acid exhibits only a slight 3/84 corrosion action under the reaction conditions according to the invention. (56) References Cited S. PATENT DOCUMENTS 2,160,004 A 5/1939 Eversole 8Ck ms, 1 Drawing Sheet 4 7 3 2 | 1 6 5 L__] U.S. Patent Mar. 30, 2004 US 6,713,649 B1 US 6,713,649 BL 1 METHOD FOR PRODUCTION OF FORMIC ‘ACID BACKGROUND ‘The present invention relates to a process for the prepa- ration of formic acid. More recent processes for the preparation of formic acid ‘on an industrial scale start from methyl formate, which is ‘easily accessible by earbonylation of methanol. The methyl formate is subsequently hydrolyzed, with the formic acid acting as catalyst, Since both the bydrolysis and the re-esterification are catalyzed, an. equilibrium becomes ‘established in which all four components, methyl formate, ‘water, formic acid and methanol, are present in high pro- portions, ‘This results in problems in performing the reaction. It is not possible to shift the equilibrium by removing the desired process products by distillation since the methyl formate (boiling point 32° C.) has a significantly lower boiling point than methanol (boiling point 65° C.) and formie acid (boiling point 101° C.). It would therefore be favorable to shift the equilibrium to the formic acid side by means of an excess of water. Further problems oceur in working up the aqueous formic acid. Formic acid and water form an azeotrope which ‘contains 77.5% by weight of HCOOH and boils at 107.1° C. at 101.3 kPa. The aqueous formic acid formed on hydrolysis ‘of methyl formate has an acid content of from about 20 t0 60% by weight. Pure or more highly concentrated formic acid therefore cannot easily be recovered from these dilute aqueous formic acid solutions by distil US. Pat. No, 2,160,064 proposes separ by distillation at various pressures, To this end, the dilute acid is frst separated at relatively high pressure into water as the top product and a formic acid-rich azeotrope as the bottom product. This azeotrope is subsequently distilled again ina second column operated at relatively low pressure ‘This gives formic acid as the top product and an azeotrope having a lower acid content than that from the first dist lation step as the bottom product. The azeotrope from the second step is fed back into the first step. In a practical implementation, the distillation is carried ‘out at a pressure of from approximately 202.6 t0 303.9 KPa ‘This causes the composition of the azeotrope to sift toward a higher acid content, Theoretically, the azeotrope should ‘contain from approximately 84 to 85% by weight of formic acid at 253.2 kPa, When the distillation is carried out in practice, the formic acid content in the still of the first

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