PROCESS FOR PREPARING 1,6 HEXANEDIOL AND CAPROLACTON

    公开(公告)号:CA2248004A1

    公开(公告)日:1997-09-04

    申请号:CA2248004

    申请日:1997-02-28

    Applicant: BASF AG

    Abstract: The invention relates to a process for preparing 1,6 hexane diol and .epsilon.caprolacton from a carboxylic acid mixture containing adipic acid, 6-hydroxy caproic acid and, in small quantities, 1,4 cyclohexane diols. Said mixture is obtained as a by-product of the oxidation of cyclohexane into cyclohexanone/ cyclohexanol with oxygen or gases containing oxygen, by water extraction of the reaction mixture. Said process involves esterification and hydrogenation of a partial stream into hexane diol and cyclization of 6-hydroxy caproic acid esters into caprolacton. According to this process: (a) the monocarboxylic acids and the dicarboxylic acids contained in the aqueous reaction mixture are reacted with a low-molecular alcohol to form the corresponding carboxylic acid esters; (b) the excess alcohol, water and low-boiling agents of the resultant esterification mixture are released in a first distillation stage; (c) separating into a ester fraction substantially free of 1,4 cyclohexane diols, and a fraction containing at least the greater part of the 1,4 cyclohexane diols is carried out from the bottom product in a second distillation stage; (d) at least part of a stream substantially containing 6-hydroxy caproic acid ester is separated from the ester fraction in a third distillation stage; (e) the ester fraction from (d), from which 6-hydroxy caproic acid ester was at least partially removed, is hydrogenated catalytically and 1,6 hexane diol is extracted by distilling the hydrogenated product in a known manner; and (f) the stream substantially containing 6-hydroxy caproic acid ester is heated to temperatures above 200 ~C at reduced pressure, thereby causing cyclization of 6-hydroxy caproic acid ester to form caprolacton, and pure .epsilon.caprolacton is recovered from the cyclization product by distillation.

    PROCESS FOR PREPARING 1, 6 HEXANE DIOL WITH A LEVEL OF PURITY OVER 99%

    公开(公告)号:MY117553A

    公开(公告)日:2004-07-31

    申请号:MYPI9700831

    申请日:1997-03-01

    Applicant: BASF AG

    Abstract: 1,6-HEXANEDIOL IS PREPARED FROM A CARBOXYLIC ACID MIXTURE COMPRISING ADIPIC ACID, 6-HYDROXYCAPROIC ACID AND SMALL AMOUNTS OF 1,4- CYCLOHEXANEDIOLS WHICH IS OBTAINED AS A BY-PRODUCT IN THE OXIDATION OF CYCLOHEXANE TO CYCLOHEXANONE/CYCLOHEXANOL BY WATER EXTRACTION OF THE REACTION MIXTURE, BY ESTERIFICATION OF THE ACIDS AND HYDROGENATION WHEREIN A) THE MONOCARBOXYLIC AND DICARBOXYLIC ACIDS PRESENT IN THE AQUEOUS DICARBOXYLIC ACID MIXTURE ARE REACTED WITH A LOW MOLECULAR WEIGHT ALCOHOL TO GIVE THE CORRESPONDING CARBOXYLIC ESTERS, B) THE RESULTING ESTERIFICATION MIXTURE IS FREED OF EXCESS ALCOHOL AND LOW BOILERS IN A FIRST DISTILLATION STAGE, C) THE BOTTOMS ARE FRACTIONATED IN A SECOND DISTILLATION STAGE TO GIVE AN ESTER FRACTION ESSENTIALLY FREE OF 1,4-CYCLOHEXANEDIOSL AND A FRACTION COMPRISING AT LEAST THE MAJOR PART OF THE 1,4-CYCLOHEXANEDIOLS, D) THE ESTER FRACTION ESSENTIALLY FREE OF 1,4-CYCLOHEXANEDIOLS IS CATALYTICALLY HYDROGENATED AND E) IN A PURE DISTILLATION STAGE, 1,6-HEXANEDIOL IS ISOLATED FROM THE HYDROGENATION PRODUCT IN A MANNER KNOWN PER SE. 3

    26.
    发明专利
    未知

    公开(公告)号:PT883591E

    公开(公告)日:2000-10-31

    申请号:PT97905123

    申请日:1997-02-28

    Applicant: BASF AG

    Abstract: PCT No. PCT/EP97/00990 Sec. 371 Date Aug. 28, 1998 Sec. 102(e) Date Aug. 28, 1998 PCT Filed Feb. 28, 1997 PCT Pub. No. WO97/31883 PCT Pub. Date Sep. 4, 19971,6-hexanediol and epsilon -caprolactone are prepared from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as a by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol using oxygen or oxygen-containing gases by water extraction of the reaction mixture, by esterifying and hydrogenating a substream to give hexanediol and cyclizing 6-hydroxycaproic esters to give caprolactone.

    27.
    发明专利
    未知

    公开(公告)号:ES2147435T3

    公开(公告)日:2000-09-01

    申请号:ES97905123

    申请日:1997-02-28

    Applicant: BASF AG

    Abstract: PCT No. PCT/EP97/00990 Sec. 371 Date Aug. 28, 1998 Sec. 102(e) Date Aug. 28, 1998 PCT Filed Feb. 28, 1997 PCT Pub. No. WO97/31883 PCT Pub. Date Sep. 4, 19971,6-hexanediol and epsilon -caprolactone are prepared from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as a by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol using oxygen or oxygen-containing gases by water extraction of the reaction mixture, by esterifying and hydrogenating a substream to give hexanediol and cyclizing 6-hydroxycaproic esters to give caprolactone.

    Recovery of Iodine
    30.
    发明专利

    公开(公告)号:GB1164691A

    公开(公告)日:1969-09-17

    申请号:GB92867

    申请日:1967-01-06

    Applicant: BASF AG

    Abstract: 1,164,691. Methacrylates. BADISCHE ANILIN- & SODA-FABRIK A.G. 6 Jan., 1967 [8 Jan., 1966], No. 928/67. Heading C2C. [Also in Division C1] In a process for the preparation of methacrylates by the oxidative dehydrogenation of an isobutyrate ester in the presence of an iodine catalyst the iodine is recovered by oxidizing at 700‹ to 1000‹ C., the organic phase of the reaction mixture containing iodine which is obtained by fractional distillation, scrubbing the flue gas with aqueous potassium iodide and extracting the resulting solution with isobutyrate ester. The iodine in the aqueous phase may also be recovered as above or by conventional methods. The solution of iodine in isobutyrate may be recycled to the oxidative dehydrogenation process.

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