公开(公告)号：DE50012565D1

公开(公告)日：2006-05-24

申请号：DE50012565

申请日：2000-12-08

Applicant: BASF AG

Inventor： REIMER KLAUS ,  KAIBEL GERD DR ,  KAMMEL ULRICH DR ,  BROECKER FRANZ-JOSEF DR ,  ANSMANN ANDREAS DR ,  ETZRODT HEINZ DR ,  STROEZEL MANFRED ,  HAAKE MATHIAS DR ,  LAUPICHLER LOTHAR DR ,  BOCKSTIEGEL BERNHARD DR

IPC: C07C5/09 ,  B01J23/44 ,  B01J23/50 ,  B01J35/04 ,  B01J35/06 ,  B01J37/02 ,  B01J37/08 ,  C07B61/00 ,  C07C29/17 ,  C07C33/02 ,  C07C33/03

Abstract: Production of alkenes by liquid-phase hydrogenation of alkynes containing 10-30 carbon (C) atoms comprises using a monolithic supported palladium catalyst and hydrogen containing 10-2000 ppm carbon monoxide (CO). Production of alkenes by liquid-phase hydrogenation of alkynes containing 10-30 C atoms at 20-250 degrees C and a hydrogen partial pressure of 0.3-200 bar comprises: (a) using a fixed bed of a catalyst prepared by calcining a support material in air, cooling it, impregnating it with a solution containing a palladium salt and optionally other metal ions, drying the product and shaping it into a monolithic catalyst element; and (b) either adding 10-2000 ppm CO to the hydrogen or generating an equivalent amount of CO by adding a CO-releasing compound to the liquid phase.

公开(公告)号：ES2184187T3

公开(公告)日：2003-04-01

申请号：ES98119215

申请日：1998-10-12

Applicant: BASF AG

Inventor： OOST CARSTEN DR ,  STROEZEL MANFRED ,  ETZRODT HEINZ DR ,  BOCKSTIEGEL BERNHARD DR ,  JAEDICKE HAGEN DR ,  WELLER DIETMAR DR

IPC: B01J31/02 ,  B01J31/14 ,  B01J31/22 ,  C07B61/00 ,  C07C45/67 ,  C07C45/68 ,  C07C49/203 ,  C07F5/06

Abstract: Preparation of gamma , delta -unsaturated ketones (I) by modified Carroll reaction is catalysed by a stable liquid aluminum acetoacetate compound or mixture of such compounds. Some such catalyst mixtures are new. Preparation of gamma , delta -unsaturated ketones of formula (I) involves modified Carroll reaction of an allyl alcohol of formula (II) with diketene or an alkyl acetoacetate of formula (III) in presence of an aluminum catalyst. R1 = H or 1-20C, saturated or unsaturated, branched hydrocarbyl; R2 = 1-5C alkyl. The novelty is that the catalyst consists of an aluminum compound (or aluminum compound mixture) which is a stable liquid at room temperature and contains at least one alkyl acetoacetate-forming group and 1 or 2 alkoxy groups or exclusively alkyl acetoacetate forming groups which are esterified sec. butanol or isobutanol or with at least two different alkanols. Independent claims are included for: (1) new mixtures of aluminum tris-acetoacetates of formula (V) which are liquid at room temperature; and (2) the preparation of mixtures as in (1). R3 = 1-5C alkyl, preferably Me or Et; R4 = 3-10C alkyl, preferably CHMe2, CH(Me)Et, CMe3 or CH(Me)-C3H7; R5 = 1-10C alkyl, preferably Me, Et, CHMe2, CH(Me)Et or CH(Me)-C3H7; provided that R3-R5 are not all the same. A further Independent claim relates to the continuous preparation of compounds (V) (or their mixtures), having the narrower proviso that R3-R5 can only be the same if they are -CH(Me)Et or -CH2CHMe2, which are liquid at room temperature. The process involves continuously reacting 1 mole of aluminum alcoholate of formula (VI) with 3-10 moles of (III), or with at least 3 moles of a mixture of 2 or 3 different compounds (III), optionally dissolved in an inert solvent. Reaction is at 100-250 (preferably 150-200) degrees C and 1-100 (preferably 1-10) bars with a dwell time of 5-120 (preferably 15-45) minutes, the pressure and temperature being such that no gas phase is formed in the reaction vessel. R6 = 2-10C alkyl, preferably -CH2CHMe2, -CH(Me)Et or -CH(Me)C3H7; provided that R2 and R6 can only be the same if they are -CH(Me)Et or -CH2CHMe2.

公开(公告)号：DE59805594D1

公开(公告)日：2002-10-24

申请号：DE59805594

申请日：1998-10-12

Applicant: BASF AG

Inventor： OOST CARSTEN DR ,  STROEZEL MANFRED ,  ETZRODT HEINZ DR ,  BOCKSTIEGEL BERNHARD DR ,  JAEDICKE HAGEN DR ,  WELLER DIETMAR DR ,  LAUPICHLER LOTHAR DR ,  REIMER KLAUS

IPC: B01J31/02 ,  B01J31/14 ,  B01J31/22 ,  C07B61/00 ,  C07C45/67 ,  C07C45/68 ,  C07C49/203 ,  C07F5/06

Abstract: Preparation of gamma , delta -unsaturated ketones (I) by modified Carroll reaction is catalysed by a stable liquid aluminum acetoacetate compound or mixture of such compounds. Some such catalyst mixtures are new. Preparation of gamma , delta -unsaturated ketones of formula (I) involves modified Carroll reaction of an allyl alcohol of formula (II) with diketene or an alkyl acetoacetate of formula (III) in presence of an aluminum catalyst. R1 = H or 1-20C, saturated or unsaturated, branched hydrocarbyl; R2 = 1-5C alkyl. The novelty is that the catalyst consists of an aluminum compound (or aluminum compound mixture) which is a stable liquid at room temperature and contains at least one alkyl acetoacetate-forming group and 1 or 2 alkoxy groups or exclusively alkyl acetoacetate forming groups which are esterified sec. butanol or isobutanol or with at least two different alkanols. Independent claims are included for: (1) new mixtures of aluminum tris-acetoacetates of formula (V) which are liquid at room temperature; and (2) the preparation of mixtures as in (1). R3 = 1-5C alkyl, preferably Me or Et; R4 = 3-10C alkyl, preferably CHMe2, CH(Me)Et, CMe3 or CH(Me)-C3H7; R5 = 1-10C alkyl, preferably Me, Et, CHMe2, CH(Me)Et or CH(Me)-C3H7; provided that R3-R5 are not all the same. A further Independent claim relates to the continuous preparation of compounds (V) (or their mixtures), having the narrower proviso that R3-R5 can only be the same if they are -CH(Me)Et or -CH2CHMe2, which are liquid at room temperature. The process involves continuously reacting 1 mole of aluminum alcoholate of formula (VI) with 3-10 moles of (III), or with at least 3 moles of a mixture of 2 or 3 different compounds (III), optionally dissolved in an inert solvent. Reaction is at 100-250 (preferably 150-200) degrees C and 1-100 (preferably 1-10) bars with a dwell time of 5-120 (preferably 15-45) minutes, the pressure and temperature being such that no gas phase is formed in the reaction vessel. R6 = 2-10C alkyl, preferably -CH2CHMe2, -CH(Me)Et or -CH(Me)C3H7; provided that R2 and R6 can only be the same if they are -CH(Me)Et or -CH2CHMe2.

公开(公告)号：DK0909750T3

公开(公告)日：2002-10-14

申请号：DK98119215

申请日：1998-10-12

Applicant: BASF AG

Inventor： OOST CARSTEN DR ,  STROEZEL MANFRED ,  ETZRODT HEINZ DR ,  BOCKSTIEGEL BERNHARD DR ,  JAEDICKE HAGEN DR ,  WELLER DIETMAR DR ,  LAUPICHLER LOTHAR DR ,  REIMER KLAUS

IPC: B01J31/02 ,  B01J31/14 ,  B01J31/22 ,  C07B61/00 ,  C07C45/67 ,  C07C45/68 ,  C07C49/203 ,  C07F5/06

Abstract: Preparation of gamma , delta -unsaturated ketones (I) by modified Carroll reaction is catalysed by a stable liquid aluminum acetoacetate compound or mixture of such compounds. Some such catalyst mixtures are new. Preparation of gamma , delta -unsaturated ketones of formula (I) involves modified Carroll reaction of an allyl alcohol of formula (II) with diketene or an alkyl acetoacetate of formula (III) in presence of an aluminum catalyst. R1 = H or 1-20C, saturated or unsaturated, branched hydrocarbyl; R2 = 1-5C alkyl. The novelty is that the catalyst consists of an aluminum compound (or aluminum compound mixture) which is a stable liquid at room temperature and contains at least one alkyl acetoacetate-forming group and 1 or 2 alkoxy groups or exclusively alkyl acetoacetate forming groups which are esterified sec. butanol or isobutanol or with at least two different alkanols. Independent claims are included for: (1) new mixtures of aluminum tris-acetoacetates of formula (V) which are liquid at room temperature; and (2) the preparation of mixtures as in (1). R3 = 1-5C alkyl, preferably Me or Et; R4 = 3-10C alkyl, preferably CHMe2, CH(Me)Et, CMe3 or CH(Me)-C3H7; R5 = 1-10C alkyl, preferably Me, Et, CHMe2, CH(Me)Et or CH(Me)-C3H7; provided that R3-R5 are not all the same. A further Independent claim relates to the continuous preparation of compounds (V) (or their mixtures), having the narrower proviso that R3-R5 can only be the same if they are -CH(Me)Et or -CH2CHMe2, which are liquid at room temperature. The process involves continuously reacting 1 mole of aluminum alcoholate of formula (VI) with 3-10 moles of (III), or with at least 3 moles of a mixture of 2 or 3 different compounds (III), optionally dissolved in an inert solvent. Reaction is at 100-250 (preferably 150-200) degrees C and 1-100 (preferably 1-10) bars with a dwell time of 5-120 (preferably 15-45) minutes, the pressure and temperature being such that no gas phase is formed in the reaction vessel. R6 = 2-10C alkyl, preferably -CH2CHMe2, -CH(Me)Et or -CH(Me)C3H7; provided that R2 and R6 can only be the same if they are -CH(Me)Et or -CH2CHMe2.

公开(公告)号：DE3908768A1

公开(公告)日：1990-09-20

申请号：DE3908768

申请日：1989-03-17

Applicant: BASF AG

Inventor： HOERCHER ULRICH DR ,  JESSEL BARBARA DR ,  BOCKSTIEGEL BERNHARD DR ,  GRAFEN PAUL DR ,  LAAS HARALD DR

IPC: B01J27/122 ,  C07B61/00 ,  C07C46/08 ,  C07C50/02

Abstract: Process wherein trimethylphenol is oxidised with oxygen or an oxygen-containing gas in the presence of a catalyst which contains a copper(II) halide in a two-phase reaction medium consisting of water and an aliphatic alcohol at high temperature, characterised in that the reaction is performed in a mixture of water and a saturated aliphatic alcohol with 12 to 18 C-atoms and a flash point above 120 DEG C, such as 1-dodecanol, 1-tetradecanol, 1-hexadecanol or 1-octadecanol, especially 1-dodecanol, and at temperatures between 60 and 100 DEG C. … Particularly good yields of TMBQ are obtained when the reaction is performed in the presence of a copper(II) halide, such as CuCl2 or CuBr2, and an alkaline earth metal halide, especially CaCl2 or MgCl2, or an alkali metal halide, especially LiCl and NaCl, as catalyst system.

公开(公告)号：ES2240322T3

公开(公告)日：2005-10-16

申请号：ES01130402

申请日：1996-06-29

Applicant: BASF AG

Inventor： HARTMANN HORST ,  BURST WOLFRAM ,  KAISER WULF DR ,  LAAS HARALD DR ,  GRAFEN PAUL DR ,  BOCKSTIEGEL BERNHARD DR

IPC: B01D3/00 ,  B01D3/10 ,  B01D3/14 ,  B01D3/16 ,  B01D3/26 ,  B01D3/32 ,  B01J19/32 ,  C07C17/38 ,  C07D311/72

Abstract: Procedimiento para la obtención de acetato de vitamina-E puro o de tocoferoles puros a partir de mezclas mediante rectificación en una columna con intercambio de materia, que contiene empaquetaduras de tela metálica con estructura ordenada, a una presión en la cabeza desde 0, 2 hasta 2 mbares, en el que a) se lleva a cabo la distribución del líquido con distribuidores en forma de canales con un número igual o mayor que 500 puntos de goteo por m2, b) disponiéndose los canales del distribuidor de líquidos girados con un ángulo de aproximadamente 90º alrededor del eje de la columna con respecto a las capas de tejido de los elementos de empaquetadura, que se encuentran directamente por debajo de estos distribuidores, c) encontrándose por debajo del distribuidor de los líquidos, 2 o varios elementos de empaquetadura con una altura de, tan solo, 20 hasta 100 mm, cuyas capas de tejido están giradas entre sí, respectivamente, 90º alrededor del eje de la columna, d) estando configurada la columna detal manera que, durante la rectificación no tenga lugar prácticamente un intercambio de calor a través de la pared de la columna, e) la columna está configurada de tal manera que pueda trabajarse prácticamente bajo exclusión del aire y f) la pérdida de presión por etapa de separación se reduce mediante un ajuste disminuido de la carga de líquido de tal manera, que las temperaturas, que se presentan en la cola se reduzcan por debajo del intervalo de descomposición del acetato de vitamina-E.

公开(公告)号：DE59002140D1

公开(公告)日：1993-09-09

申请号：DE59002140

申请日：1990-03-14

Applicant: BASF AG

Inventor： HOERCHER ULRICH DR ,  JESSEL BARBARA DR ,  BOCKSTIEGEL BERNHARD DR ,  GRAFEN PAUL DR ,  LAAS HARALD DR

IPC: B01J27/122 ,  C07B61/00 ,  C07C46/08 ,  C07C50/02

Abstract: Process wherein trimethylphenol is oxidised with oxygen or an oxygen-containing gas in the presence of a catalyst which contains a copper(II) halide in a two-phase reaction medium consisting of water and an aliphatic alcohol at high temperature, characterised in that the reaction is performed in a mixture of water and a saturated aliphatic alcohol with 12 to 18 C-atoms and a flash point above 120 DEG C, such as 1-dodecanol, 1-tetradecanol, 1-hexadecanol or 1-octadecanol, especially 1-dodecanol, and at temperatures between 60 and 100 DEG C. … Particularly good yields of TMBQ are obtained when the reaction is performed in the presence of a copper(II) halide, such as CuCl2 or CuBr2, and an alkaline earth metal halide, especially CaCl2 or MgCl2, or an alkali metal halide, especially LiCl and NaCl, as catalyst system.

公开(公告)号：DE4029198A1

公开(公告)日：1992-03-19

申请号：DE4029198

申请日：1990-09-14

Applicant: BASF AG

Inventor： BOCKSTIEGEL BERNHARD DR ,  HOERCHER ULRICH DR ,  LAAS HARALD DR ,  JESSEL BARBARA DR ,  GRAFEN PAUL DR

IPC: C07C46/08 ,  C07C50/02

公开(公告)号：AT233723T

公开(公告)日：2003-03-15

申请号：AT00111532

申请日：2000-05-30

Applicant: BASF AG

Inventor： KLATT MARTIN JOCHEN DR ,  MUELLER THOMAS DR ,  BOCKSTIEGEL BERNHARD DR

IPC: B01J31/18 ,  B01J31/22 ,  C07B61/00 ,  C07C45/34 ,  C07C45/86 ,  C07C49/403 ,  C07C49/603

公开(公告)号：DK0983988T3

公开(公告)日：2002-03-25

申请号：DK99117101

申请日：1999-08-31

Applicant: BASF AG

Inventor： OOST CARSTEN DR ,  STROEZEL MANFRED ,  ETZRODT HEINZ DR ,  WELLER DIETMAR DR ,  BOCKSTIEGEL BERNHARD DR ,  REIMER KLAUS ,  KAIBEL GERD DR ,  JAEDICKE HAGEN DR

IPC: B01J31/14 ,  B01D3/00 ,  B01D3/14 ,  B01D3/32 ,  B01J10/00 ,  B01J19/24 ,  C07B61/00 ,  C07C45/67 ,  C07C45/68 ,  C07C45/82 ,  C07C49/203 ,  C07C67/54 ,  C07C69/72

Abstract: Continuous production of 5-alken-2-one or 3,5-alkadien-2-one derivatives (I) by reacting a 1-alken-3-ol or 1-alkyn-3-ol derivative (II) with an alkyl acetoacetate (III) in a fractionation column to form an acetoacetate and alcohol involves (i) removing the alcohol and (ii) contacting the acetoacetate with catalyst in the lower part or bottom of the column to form (I). Continuous production of unsaturated ketones of formula (I) by reacting an unsaturated alcohol of formula (II) with an alkyl acetoacetate of formula (III) in the presence of an organoaluminum catalyst is carried out by: (a) reacting (II) with (III) on the plates of a fractionation column to form the acetoacetate of (II) and an alcohol of formula R OH; (b) removing the alcohol in the overhead stream from the column; (c) contacting the acetoacetate of (II) with the catalyst in the lower part or bottom of the column to form (I) and CO2; (d) removing the CO2 in the overhead stream from the column; and (e) withdrawing (I) in the bottoms stream from the column. R = 1-4C alkyl; R = 1-37C (un)saturated aliphatic hydrocarbyl (optionally substituted by methoxy groups), 4-12C cycloalkyl or 5-30C cycloalkylalkyl; and R = 1-5C alkyl.