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    12.
    发明专利
    未知

    公开(公告)号：DE19641707A1

    公开(公告)日：1998-04-16

    申请号：DE19641707

    申请日：1996-10-10

    Applicant: BASF AG

    Inventor： BECKER RAINER DR ,  BROECKER FRANZ JOSEF DR ,  KAIBEL GERD DR ,  PINKOS ROLF DR ,  WULFF-DOERING JOACHIM DR

    IPC: B01J25/02 ,  B01J8/02 ,  B01J8/06 ,  B01J10/00 ,  B01J19/00 ,  B01J19/24 ,  B01J19/26 ,  C07B61/00 ,  C07C29/17 ,  C07C31/20

    Abstract: The invention concerns a process for preparing 1,4-butanediol by continuous catalytic hydrogenation of 1,4-butinediol in that 1,4-butinediol is reacted with hydrogen in the liquid continuous phase in the presence of a heterogeneous hydrogenation catalyst at temperatures of between 20 and 300 DEG C, a pressure of between 1 and 200 bar and values of the liquid-side mass transfer coefficients kLa, relative to the volume, of between 0.1 s and 1s , a) with a catalyst suspended in the reaction medium, wherein, when a packed bubble column is used, it is operated in the upwards mode and at a ratio of the amount of gas leaving the reaction vessel to the amount fed thereto of between 0.99:1 and 0.4:1, or b) is guided upwards in parallel flow through a fixed bed reactor operated in the circulating gas mode, the ratio between the amount of gas fed to the reaction vessel and the amount of gas leaving the latter being maintained between 0.99:1 and 0.4:1.

    Economical production of pure 1,6-hexane-diol from by-product of oxidation of cyclohexane
    13.
    发明专利
    Economical production of pure 1,6-hexane-diol from by-product of oxidation of cyclohexane 未知

    公开(公告)号：DE19607955A1

    公开(公告)日：1997-09-04

    申请号：DE19607955

    申请日：1996-03-01

    Applicant: BASF AG

    Inventor： BAUR KARL GERHARD DR ,  FISCHER ROLF DR ,  PINKOS ROLF DR ,  STEIN FRANK DR ,  RUST HARALD

    IPC: C07C29/149 ,  C07C31/20 ,  B01J23/89 ,  C07C29/74

    Abstract: A process for the production of 1,6-hexanediol (I) from a carboxylic acid mixture (II) of adipic acid, 6-hydroxycaproic acid and small amounts of cyclohexan-1,4-diol(s) is obtained as by-product of the oxidation of cyclohexane to cyclohexanone/cyclohexanol with (gas containing) oxygen by extraction of the reaction mixture with water. The process involves esterification of the acids and hydrogenation. First, (a) the mono- and dicarboxylic acids in the aqueous (II) are esterified with a low molecular alcohol. This is followed by 2 distillation stages, in which (b) excess alcohol and low-boiling compounds are removed and (c) the sump is separated into an ester fraction free from cyclohexan-1,4-diol(s) and a fraction of (mainly) cyclohexan-1,4-diol(s). Then (d) the ester fraction is hydrogenated catalytically and (e) pure (I) is recovered from the hydrogenation product by distillation.

    Economical production of pure 1,6-hexane-diol and epsilon-capro-lactone from by-product of oxidation of cyclohexane
    14.
    发明专利
    Economical production of pure 1,6-hexane-diol and epsilon-capro-lactone from by-product of oxidation of cyclohexane 未知

    公开(公告)号：DE19607954A1

    公开(公告)日：1997-09-04

    申请号：DE19607954

    申请日：1996-03-01

    Applicant: BASF AG

    Inventor： BAUR KARL GERHARD DR ,  FISCHER ROLF DR ,  PINKOS ROLF DR ,  STEIN FRANK DR ,  RUST HARALD

    IPC: C07C29/149 ,  C07C29/80 ,  C07C29/88 ,  C07C51/31 ,  C07D315/00 ,  C07D313/04 ,  C07D307/33 ,  C07D309/30

    Abstract: A process for the production of 1,6-hexandiol (I) and iota -caprolactone (II) from a carboxylic acid mixture (III) of adipic acid, 6-hydroxycaproic acid and small amounts of cyclohexan-1,4-diol(s) is obtained as by-product of the oxidation of cyclohexane to cyclohexanone/cyclohexanol with (gas containing) oxygen by extraction of the reaction mixture with water. The process involves esterification, hydrogenation of a side stream to (I) and cyclisation of 6-hydroxycaproic ester to (II) by the following stages. First, (a) the mono- and dicarboxylic acids in the aqueous (III) are esterified with a low molecular alcohol. This is followed by 3 distillation stages, in which (b) excess alcohol and low-boiling compounds are removed, (c) the sump is separated into an ester fraction free from cyclohexan-1,4-diol(s) and a fraction of (mainly) cyclohexan-1,4-diol(s), and (d) a stream of (mainly) 6-hydroxycaproic ester is separated from the ester fraction. Then (e) the remaining ester fraction from (d) is hydrogenated catalytically and (I) is recovered from the hydrogenation product by distillation and (f) the 6-hydroxycaproic ester stream is heated to > 200 deg C at low pressure to cyclise the ester to (II), and pure (II) is recovered from the cyclisation product by distillation.

    Process for the preparation of butenediol monocarboxylates
    16.
    发明专利
    Process for the preparation of butenediol monocarboxylates 未知

    公开(公告)号：DE4429690A1

    公开(公告)日：1995-03-02

    申请号：DE4429690

    申请日：1994-08-22

    Applicant: BASF AG

    Inventor： PINKOS ROLF DR ,  FISCHER ROLF DR

    IPC: C07C67/26 ,  C07C69/12 ,  C07C69/16

    Abstract: Process for the preparation of butenediol monocarboxylates of the formulae I and II in which R and R are identical or different and represent hydrogen or a C1- to C5-alkyl group and in which R represents an aliphatic, cycloaliphatic, araliphatic or aromatic C1- to C15- radical, by reacting vinyl oxiranes of the formula III in which R and R are identical or different and represent hydrogen or a C1- to C5-alkyl group, with aliphatic, aromatic, cycloaliphatic or araliphatic carboxylic acids R COOH, in which R has the abovementioned meaning, in the presence of water.

    Butene-diol(s) and butene-diol ether(s) prepn. - by reacting vinyl oxirane(s) with water or 1-10C alcohol(s) in absence of catalyst
    18.
    发明专利
    Butene-diol(s) and butene-diol ether(s) prepn. - by reacting vinyl oxirane(s) with water or 1-10C alcohol(s) in absence of catalyst 未知

    公开(公告)号：DE4342030A1

    公开(公告)日：1994-06-16

    申请号：DE4342030

    申请日：1993-12-09

    Applicant: BASF AG

    Inventor： PINKOS ROLF DR ,  FISCHER ROLF DR

    IPC: C07C29/10 ,  C07C29/56 ,  C07C41/03 ,  C07C43/178 ,  C07C29/128 ,  C07C33/035 ,  C07C41/02

    Abstract: Prepn. of butenediols and butenediol ethers of formula (I) and formula R3O-CH-C(R1)=C(R2)-CH2-OR4 (II) comprises reaction of vinyl-oxiranes of formula (III) with water and/or 1-10C alcohols at 0-250 deg.C in the absence of catalyst. R1, R2 = H or 1-5C alkyl, R3 = R4 = H or one of these gps. = H and the other = 1-10C alkyl or hydroxyalkyl. USE/ADVANTAGE - 2-Butene-1,4-diol is useful for the prodn. of butane-1,4-diol and 1-butene-3,4-diol is useful as an intermediate in the prodn. of vitamin A, the diol ethers are useful as crosslinkable diols for the prodn. of polyurethanes and polyesters. This process gives (I) and (II) in high yield and with high selectivity (such that the yield of the vitamin precursor (I) far exceeds that of (II)) and without the high cost involved in sepn. of catalyst (contrast prior-art processes). (I) and (II) are easily sepd. by fractional distn.

    19.
    发明专利
    未知

    公开(公告)号：DE4205471A1

    公开(公告)日：1993-08-26

    申请号：DE4205471

    申请日：1992-02-22

    Applicant: BASF AG

    Inventor： GOSCH HANS-JUERGEN DR ,  RUST HARALD ,  FISCHER ROLF DR ,  HECHLER CLAUS DR ,  PINKOS ROLF DR

    IPC: C07C29/80 ,  C07C29/82 ,  C07C31/20

    Abstract: A process for isolating 1,4-butanediol from mixtures obtained by catalytic hydrogenation of maleic acid esters, fumaric acid esters and/or succinic acid esters, which in addition to 1,4-butanediol contain tetrahydrofuran, water, C1-C4-alcohols, succinic acid diesters, hydroxybutyric acid esters, succinic acid alkyl hydroxyalkyl esters, gamma-butyrolactone and butyric acid esters.

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