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公开(公告)号：DE59902731D1
公开(公告)日：2002-10-24
申请号：DE59902731
申请日：1999-11-13
Applicant: BASF AG
Inventor： OOST CARSTEN , STROEZEL MANFRED , ETZRODT HEINZ , WELLER DIETMAR , RHEUDE UDO , KAIBEL GERD , KRUG THOMAS , SPISKE LUISE , JAEDICKE HAGEN
IPC: B01J31/14 , C07B61/00 , C07C45/67 , C07C45/74 , C07C49/203
Abstract: Preparation of unsaturated ketones by reaction of the corresponding alpha , beta -unsaturated alcohol with an alkyl acetoacetate compound in the presence an organo-aluminum catalyst at constant temperature, with separation and continuous removal of CO2 and alcohol formed. Preparation of unsaturated ketones of formula (I) by reaction of the corresponding alpha , beta -unsaturated alcohol of formula (II) with an alkyl acetoacetate compound of formula (III) in the presence of 0.1-5 mole% (based on (III)) of an organo-aluminum catalyst with separation and continuous distillative removal of CO2 and alcohol of formula R3OH formed during reaction, in a reactor containing a fractionation column, where: (A) (II) is added to the reaction mixture together with the organic catalyst without additional solvent and (III) is then added to this mixture; (B) the reaction temperature is kept constant between 175-220 degrees C; (C) the content of (III) is kept at a constant level between 0.1-10 wt.% during the reaction. R1, R3 = 1-4C alkyl; R2 = 4-30C aliphatic, cycloaliphatic or cycloaliphatic-aliphatic; a, b = optional additional bonds.
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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
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.
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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
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.
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公开(公告)号：DE10031119A1
公开(公告)日：2002-01-10
申请号：DE10031119
申请日：2000-06-30
Applicant: BASF AG
Inventor： KAIBEL GERD , STAMMER ACHIM , STROEZEL MANFRED
IPC: B01J19/32
Abstract: In zig-zag sheet metal column packing, a proportion X of the openings has a spacing b which is no greater than 0.4a from a fold edge. The proportion X is at least 60%. Preferred Features: X is at least 80% or 90%. Dimension b is 0.3a or 0.2a at most. The angle of folding is 40-120 degrees , preferably 60-90 degrees . Openings take up 5-40%, preferably 10-20% of the folded area. Openings are rectangular with aspect ratio 5:1 to 1:1, preferably 3:1 to 2:1. The longer side of the opening, is parallel to the folded edges. In a packed column, folded edges of the packing include an angle of 20-70 degrees , preferably 30-45 degrees with the column axis.
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公开(公告)号：DE59704133D1
公开(公告)日：2001-08-30
申请号：DE59704133
申请日：1997-05-02
Applicant: BASF AG
Inventor： RHEUDE UDO , HOERCHER ULRICH , WELLER DIETMAR , STROEZEL MANFRED
IPC: C07B37/10 , C07C20060101 , C07C49/21 , C07C403/14 , C07C403/16
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Patent Agency Ranking
公开(公告)号：DE19936276A1
公开(公告)日：2001-02-08
申请号：DE19936276
申请日：1999-08-02
Applicant: BASF AG
Inventor： BROECKER FRANZ-JOSEF , HAAKE MATHIAS , KAIBEL GERD , ROHRBACHER GERD , SCHWAB EKKEHARD , STROEZEL MANFRED
IPC: B01J23/42 , B01J8/00 , B01J10/00 , B01J19/24 , B01J19/26 , B01J32/00 , B01J35/04 , B01J35/06 , C07B61/00 , C07C5/10 , C07C13/18 , F28D9/04 , B01F13/00
Abstract: The apparatus for carrying out reactions in the gaseous, liquid and solid phases comprises a liquid stream-gas compressor for producing a reaction fluid, a reactor charged with metal braiding coated with catalyst, and a feed line. The apparatus for carrying out reactions in the gaseous, liquid and solid phases comprises a liquid stream-gas compressor (6) for producing a reaction fluid by dispersing a gas phase in a liquid phase; a reactor (1) having an inlet and an outlet and a reaction chamber limited by heat-deviating walls, the reactor being charged with a metal braiding coated with catalyst; and a line (7) feeding the reaction fluid from the compressor to the reactor inlet and is short so that the degree of dispersibility of the fluid does not change during the passage through the line. An Independent claim is also included for a process for carrying out reactions in the gaseous, liquid and solid phases comprising producing a reaction fluid by dispersion of a gaseous phase in a liquid phase; feeding the reaction fluid produced through the reactor; exchanging reaction heat on the walls of the reactor chamber; and separating the reaction fluid into a gas phase and a liquid phase.
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公开(公告)号：AT193462T
公开(公告)日：2000-06-15
申请号：AT97100519
申请日：1997-01-15
Applicant: BASF AG
Inventor： KAIBEL GERD DR , RHEUDE UDO DR , STROEZEL MANFRED , GRAAUW JAN DE PROF DR , OLUJIC ZARKO DR , FREY GUENTHER , JANSEN HELMUT
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公开(公告)号：DE19840747A1
公开(公告)日：2000-03-09
申请号：DE19840747
申请日：1998-09-07
Applicant: BASF AG
Inventor： OOST CARSTEN , STROEZEL MANFRED , ETZRODT HEINZ , WELLER DIETMAR , BOCKSTIEGEL BERNHARD , REIMER KLAUS , KAIBEL GERD , JAEDICKE HAGEN
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 , C07C45/65 , C07C49/255
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.
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公开(公告)号：DE19619557C1
公开(公告)日：1997-11-20
申请号：DE19619557
申请日：1996-05-14
Applicant: BASF AG
Inventor： RHEUDE UDO DR , HOERCHER ULRICH DR , WELLER DIETMAR DR , STROEZEL MANFRED
IPC: C07B37/10 , C07C20060101 , C07C49/21 , C07C403/14 , C07C403/16
Abstract: A process for the continuous production of alpha and/or beta -ionones or homologous compounds by means of concentrated sulphuric acid at temperatures of 20 to 90 DEG C in the presence of organic solvents or diluents with cooling, and the subsequent halting of the reaction by the hydrolysis of the reaction mixtures with water or dilute sulphuric acid, in which the cyclization of the pseudo-ionones and the subsequent hydrolysis of the reaction mixture is performed in a practically adiabatic reaction in one or more successive reaction mixing pump(s) consisting of a rotational symetrical mixing chamber formed by a peripheral wall and two faces and driven mixing rotor of a material unaffected by sulphuric acid, where the mixing chamber has at least one inlet for each component and an outlet for the reaction mixture and annular chanels in fluid communication with each other in the faces, and the heat of reaction of both reactions is partly or fully evacuated with the aid of a downstream heat exchanger.
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100.发明专利
公开(公告)号：CA2203821A1
公开(公告)日：1997-10-30
申请号：CA2203821
申请日：1997-04-25
Applicant: BASF AG
Inventor： KAIBEL GERD , RHEUDE UDO , STROEZEL MANFRED
Abstract: A dividing wall column for separating a mixture into 3 or more fractions by distillation is described, where at least one dividing wall is detachably attached within the dividing wall column.
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