PROCESS FOR PREPARING 1,6 HEXANEDIOL AND CAPROLACTONE

    公开(公告)号:CA2248004C

    公开(公告)日:2006-04-11

    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 .epsilo n.- 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 carboxyli c 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 par t 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 fro m (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 heat ed to temperatures above 200 .degree.C at reduced pressure, thereby causing cyclization of 6-hydroxy caproic acid ester to form caprolacton, and pure e-caprolacton is recovered from the cyclization product by distillation.

    METHOD FOR THE PRODUCTION OF CYCLOHEXANOL FROM BENZOLE

    公开(公告)号:PL374274A1

    公开(公告)日:2005-10-03

    申请号:PL37427403

    申请日:2003-02-28

    Applicant: BASF AG

    Abstract: A process for preparing cyclohexanol from benzene by: a) preparing cyclohexene by hydrogenating benzene in the presence of a catalyst, and b) preparing cyclohexanol by hydrating the cyclohexene in the presence of a catalyst, comprises: carrying out steps a) and b) in a reaction facility which has a bottom region at the lower end, a top region at the upper end, and a reaction zone between the top region and the bottom region which contains the catalyst according to steps a) and b), evaporating a portion of the benzene using the heat of reaction in the reaction zone, condensing it in the top region and returning it to the reaction zone, and withdrawing a reaction mixture containing cyclohexanol in the bottom region.

    73.
    发明专利
    未知

    公开(公告)号:MX226058B

    公开(公告)日:2005-02-03

    申请号:MXPA02006394

    申请日:2000-12-21

    Applicant: BASF AG

    Abstract: A process is disclosed for the purification, by distillation, of trimethylolpropane originating from the hydrogenation of 2,2-dimethylolbutanal, said process including the following steps:(a) reaction of n-butyraldehyde with formaldehyde in the presence of catalytic amounts of a tertiary amine, and hydrogenation of the resulting mixture to give a mixture containing trimethylolpropane;(b) separation of water, methanol, trialkylamine and/or trialkylammonium formate by distillation;(c) heating of the residue obtained in (b) under reduced pressure to a temperature at which TMP is volatile and compounds boiling above TMP are cleaved, in order to separate off, by distillation, TMP and compounds more volatile than TMP;(d) distillation of the distillate obtained in (c) in order to separate off the more volatile compounds and recover pure TMP; and(e) optional distillation of the TMP obtained in (d) in order to recover TMP with a low APHA color index.A process is also disclosed in which trialkylammonium formate is distilled under mild conditions from crude mixtures of polyhydric alcohols, predominantly trimethylolpropane.

    75.
    发明专利
    未知

    公开(公告)号:DE50005700D1

    公开(公告)日:2004-04-22

    申请号:DE50005700

    申请日:2000-06-21

    Applicant: BASF AG

    Abstract: A process for preparing 1,6-hexanediol from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol after water extraction of the reaction mixture followed by extraction with aqueous sodium hydroxide solution, by esterification of the acids and hydrogenation comprisesa) liberating the carboxylic acids from the alkaline extract by addition of a mineral acid,b) fractionating the organic phase comprising carboxylic acids to give a distillate comprising the low molecular weight monocarboxylic acids and a residue comprising adipic acid and 6-hydroxycaproic acid,c) reacting the monocarboxylic an dicarboxylic acids present in the aqueous dicarboxylic acid mixture with a low molecular weight alcohol to give the corresponding carboxylic esters,d) freeing the esterification mixture obtained of excess alcohol and low boilers in a first distillation step,e) fractionating the bottom product in a second distillation step to give an ester fraction essentially free of 1,4-cyclohexanediols and a fraction comprising at least the major part of the 1,4-cyclohexanediols,f) catalytically hydrogenating the ester fraction which is essentially free of 1,4-cyclohexanediols andg) isolating 1,6-hexanediol from the hydrogenation product in a manner known per se in a final distillation step.

    77.
    发明专利
    未知

    公开(公告)号:DE10209701A1

    公开(公告)日:2003-09-18

    申请号:DE10209701

    申请日:2002-03-06

    Applicant: BASF AG

    Abstract: A process for preparing cyclohexanol from benzene by: a) preparing cyclohexene by hydrogenating benzene in the presence of a catalyst, and b) preparing cyclohexanol by hydrating the cyclohexene in the presence of a catalyst, comprises: carrying out steps a) and b) in a reaction facility which has a bottom region at the lower end, a top region at the upper end, and a reaction zone between the top region and the bottom region which contains the catalyst according to steps a) and b), evaporating a portion of the benzene using the heat of reaction in the reaction zone, condensing it in the top region and returning it to the reaction zone, and withdrawing a reaction mixture containing cyclohexanol in the bottom region.

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