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

Inventor： STEIN FRANK ,  KRUG THOMAS ,  NOEBEL THOMAS ,  RUST HARALD

IPC: C07B61/00 ,  C07C29/149 ,  C07C31/20

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.

公开(公告)号：MY116778A

公开(公告)日：2004-03-31

申请号：MYPI9804995

申请日：1998-11-03

Applicant: BASF AG

Inventor： STEIN FRANK ,  FISCHER ROLF HARTMUTH ,  PINKOS ROLF DR

IPC: C07C27/00 ,  C07B61/00 ,  C07C29/149 ,  C07C29/80 ,  C07C31/20 ,  C07C51/367 ,  C07C62/02 ,  C07C67/31 ,  C07C69/675

Abstract: A PROCESS FOR THE PREPARATION OF L, 6-HEXANEDIOL AND 6-HYDROXYCAPROIC ACID OR ESTERS THEREOF BY CATALYTIC HYDROGENATION OF ADIPIC ACID, ADIPIC ACID MONOESTERS OR ADIPIC ACID DIESTERS OR STREAMS OF STARTING MATERIAL WHICH CONTAIN ADIPIC ACID OR ESTERS THEREOF AS ESSENTIAL CONSTITUENTS, IN WHICH THE BOTTOM PRODUCT OBTAINED IN THE DISTILLATION OF THE HYDROGENATION PRODUCT, FOLLOWING REMOVAL OF THE HEXANEDIOL AND HYDROXYCAPROIC ACID OR ESTERS THEREOF, AND ESSENTIALLY COMPRISES OLIGOMERIC ESTERS OF 6-HYDROXYCAPROIC ACID, IS RECYCLED TO THE HYDROGENATION, AND THE RESULTING ''MIXTURE OF STARTING MATERIAL AND RECYCLE STREAM IS REACTED AT FROM 100 TO 300°C, AT FROM 10 TO 300 BAR IN THE LIQUID PHASE AND AT A MOLAR RATIO OF CARBOXYL GROUPS TO BE HYDROGENATED TO HYDROGEN IN THE REACTOR OF FROM 1 : 5 TO 1 : 100 ON HYDROGENATION CATALYSTS IS DESCRIBED.

公开(公告)号：CA2433073A1

公开(公告)日：2002-07-18

申请号：CA2433073

申请日：2002-01-08

Applicant: BASF AG

Inventor： GALL MARTIN ,  RUST HARALD ,  KRUG THOMAS ,  KAIBEL GERD ,  STEIN FRANK

IPC: C07D309/30 ,  B01D3/14 ,  C07C29/80 ,  C07C31/20 ,  C07D315/00

Abstract: The invention relates to a method for the distillative processing of the crude products 1,6-hexandiols (HDO), 1,5-pentandiol (PDO) or caprolactone (CLO) obtained according to the method of German patent application DE-A 196 07 954 in order to obtain the corresponding pure products. The distillative processing proceeds in a separation column (TK) in which a separating wall (T) is arranged in the column longitudinal direction forming an upper common column section (1), a lower common column section (6), a feed part (2, 4) with reinforcement part (2) and drive part (4), and a removal part (3, 5) with output part (3) and reinforcement part (5). The corresponding crude product HDO, PDO or CLO is fed in the center section of the feed part (2, 4), the high- boiling fraction (C) is removed from the column sump, the low-boiling fraction (A) is removed via the column head and the medium-boiling fraction (B) is removed from the center section of the removal part (3, 5). The inventive method can also be carried out in thermally coupled columns.

公开(公告)号：AT192730T

公开(公告)日：2000-05-15

申请号：AT97905123

申请日：1997-02-28

Applicant: BASF AG

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

IPC: C07D313/04 ,  C07C27/12 ,  C07C29/149 ,  C07C29/80 ,  C07C29/88 ,  C07C31/20 ,  C07C31/27 ,  C07C51/31 ,  C07D315/00

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.

公开(公告)号：CA2329040A1

公开(公告)日：1999-11-04

申请号：CA2329040

申请日：1999-04-12

Applicant: BASF AG

Inventor： BREITSCHEIDEL BORIS ,  PINKOS ROLF ,  STEIN FRANK

IPC: B01J23/72 ,  C07B61/00 ,  C07C29/149 ,  C07C31/20

Abstract: The invention relates to a method for producing hexanediol by hydrogenating adipic acid dialkyl esters or mixtures containing adipic acid dialkyl esters as an essential constituent and organic halogen compounds as impurities. According to said method, the adipic acid dialkyl esters or the mixtures containing adipic acid dialkyl esters are guided over copper catalysts at a temperature of 50 to 250 ~C and at a pressure of 1 to 100 bar before hydrogenation in order to remove the organic halogen compounds. Said copper catalysts contain 0.5 to 80 wt. % copper calculated as CuO and have a surface of 5 to 1500 m2/g, 0.05 to 1.5 cm3/g porosity and a copper surface of 0.1 to 20 m2/g.

公开(公告)号：CA2305590A1

公开(公告)日：1999-07-08

申请号：CA2305590

申请日：1998-12-10

Applicant: BASF AG

Inventor： BREITSCHEIDEL BORIS ,  PINKOS ROLF ,  FISCHER ROLF HARTMUTH ,  STEIN FRANK ,  LIANG SHELUE

IPC: C07B61/00 ,  C07C29/149 ,  C07C31/20

Abstract: The invention relates to a method for producing 1,6-hexanediol by hydrogenating adipic acid esters and/or 6-hydroxycarboxylic acid esters in the gaseous phase at an elevated temperature and pressure in the present of chromium-free catalysts. Hydrogenation is carried out a) using catalysts containing copper, manganese and aluminium as essential constituents or in the presence of Raney copper; b) at temperatures of between 150 and 230 ~C and pressures of between 10 and 70 bar; c) at a molar ratio of hyrogen to hydrogenating ester of between 150 to 1 and 300 to 1; and d) at a catalyst load of between 0.01 and 0.3 kg C3-ester per litre of catalyst and hour.

公开(公告)号：CA2311589A1

公开(公告)日：1999-06-24

申请号：CA2311589

申请日：1998-12-04

Applicant: BASF AG

Inventor： DOSTALEK ROMAN ,  FISCHER ROLF HARTMUTH ,  STEIN FRANK ,  KRUG THOMAS ,  PINKOS ROLF ,  PAUL AXEL

IPC: C07B61/00 ,  C07C29/149 ,  C07C29/17 ,  C07C31/13 ,  C07C31/20 ,  C07C31/27

Abstract: The invention relates to a method for catalytically hydrogenating carboxylic acids or the anhydrides or esters thereof into alcohol on heterogeneous catalysts containing hydrogenating elements of groups 6, 7, 8, 9, 10 and 11 and optionally groups 2, 14 and 15 of the periodic table of elements or consisting thereof, in a liquid phase at temperatures of 100-300 ~C and at pressures of 10-300 bars, whereby 1-3,000 ppm of a basic alkali or earthalkaline compound in relation to the liquid hydrogenating feed and selected from a group consisting of hydroxides, carbonates, carboxylates and alcoholates is added to the hydrogenating reaction mixture.

公开(公告)号：CA2273265A1

公开(公告)日：1998-06-11

申请号：CA2273265

申请日：1997-11-18

Applicant: BASF AG

Inventor： HESSE MICHAEL ,  PLITZKO KLAUS-DIETER ,  FISCHER ROLF ,  MUELLER ULRICH ,  STEIN FRANK ,  BECKER RAINER ,  SIGWART CHRISTOPH ,  ELLER KARSTEN

IPC: B01J23/24 ,  C08G65/10 ,  C08G65/20 ,  C08G65/26 ,  C08G65/28

Abstract: Polytetrahydrofuran, tetrahydrofuran copolymers, diesters or monoesters of these polymers are prepared by polymerizing tetrahydrofuran in the presence of at least one telogen and/or comonomer on a heterogeneous carrier catalyst which contains on an oxidic carrier material as active mass a catalytically active amount of at least one oxygenous molybdenum and/or tungsten compound and, when the precursor compounds of the active mass have been applied to the carrier material precursor, has been calcined at temperatures of between 500 ~C and 1000 ~C. The catalyst used contains a promotor which comprises at least one element or a compound of an element of the 2nd, 3rd including the lanthanides, 5th, 6th, 7th, 8th or 14th group of the periodic system of elements.

公开(公告)号：AU4556497A

公开(公告)日：1998-05-05

申请号：AU4556497

申请日：1997-09-23

Applicant: BASF AG

Inventor： SIGWART CHRISTOPH ,  ELLER KARSTEN ,  BECKER RAINER ,  PLITZKO KLAUS-DIETER ,  FISCHER ROLF ,  STEIN FRANK ,  MULLER ULRICH ,  HESSE MICHAEL

IPC: C08G65/10 ,  B01J23/24 ,  C08G18/48 ,  C08G65/20 ,  C08G65/28

Abstract: PCT No. PCT/EP97/05204 Sec. 371 Date Apr. 1, 1999 Sec. 102(e) Date Apr. 1, 1999 PCT Filed Sep. 23, 1997 PCT Pub. No. WO98/15589 PCT Pub. Date Apr. 16, 1998Polytetrahydrofuran, copolymers of tetrahydrofuran and 2-butyne-1,4-diol, diesters of these polymers with C2-C20-monocarboxylic acids or monoesters of these polymers with C1-C10-monocarboxylic acids are prepared by polymerization of tetrahydrofuran in the presence of one of the telogens water, 1,4-butanediol, 2-butyne-1,4-diol, polytetrahydrofuran having a molecular weight of from 200 to 700 Dalton, a C1-C10-monocarboxylic acid or an anhydride of a C2-C20-monocarboxylic acid or a mixture of these telogens over a heterogeneous supported catalyst which comprises a catalytically active amount of an oxygen-containing molybdenum and/or tungsten compound on an oxidic support material and which has been calcined at from 5OO DEG C. to 1OOO DEG C. after application of the precursor compounds of the oxygen-containing molybdenum and/or tungsten compounds onto the support material precursor, wherein the catalyst is activated by treatment with a reducing agent before it is used as a polymerization catalyst.

公开(公告)号：CA2247991A1

公开(公告)日：1997-09-04

申请号：CA2247991

申请日：1997-02-28

Applicant: BASF AG

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

IPC: C07C29/149 ,  C07C31/20

Abstract: The invention relates to a process for the preparation of 1,6 hexane diol 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 byproduct of the oxidation of cyclohexane into cyclohexanone/ cyclohexanol by water extraction of the reaction mixture. Said process involves esterification of the acids and hydrogenation. According to this process (a) the monocarboxylic acids and the dicarboxylic acids contained in the aqueous dicarboxylic acid mixture are reacted with a low-molecular alcohol to form the corresponding carboxylic acid esters; (b) the excess alcohol and low-boiling agents of the resultant esterification mixture are released in a first distillation stage; (c) separating into an 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) the ester fraction substantially free of 1,4 cyclohexane diols is catalytically hydrogenated; and (e) in a pure distillation stage 1,6 hexane diol is extracted from the hydrogenated discharge in a known manner.