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    PRODUCTION OF SOLID BY PRECIPITATION
    1.
    发明专利
    PRODUCTION OF SOLID BY PRECIPITATION 失效

    公开(公告)号：JPH11128732A

    公开(公告)日：1999-05-18

    申请号：JP24057698

    申请日：1998-08-26

    Applicant: BASF AG

    Inventor： HORN HANS CHRISTOPH DR ,  KUMBERGER OTTO DR ,  MILIES MARCO DR ,  NETH NORBERT DR ,  WOLFGANG JUERGEN ,  RIEKER CHRISTOPHER WILLIAM DR ,  SPRAGUE MICHAEL JOLYON DR ,  STROEZEL MANFRED

    IPC: B01J19/18 ,  B01F5/00 ,  B01F5/06 ,  B01F7/00 ,  B01F7/22 ,  B01F15/02 ,  B01F15/06 ,  B01J14/00 ,  B01J19/00 ,  C01G1/00

    Abstract: PROBLEM TO BE SOLVED: To produce a high quality solid by precipitation by supplying a plurality of starting materials to a mixing chamber of a mixing apparatus comprising stirring blades through inlets formed in the circumferential wall of the chamber and discharging the resultant mixture containing the solid produced by mixing out of an outlet formed in the circumferential wall of the mixing chamber. SOLUTION: In the case of production of a solid such as carbonates, hydroxycarbonates, hydroxides to be used as precursors of catalysts or the simple substances, a plurality of starting substances are supplied to a mixing apparatus 3 through conduits 1, 2 especially in a manner that the resultant slurry comes to the center of impellers and at the same time sodium carbonate and a metal salt solution are added form side faces. Then, precipitation reaction is caused in the mixing apparatus 3 and the obtained mixture is supplied to a degassing tank 5 provided with a stirring apparatus 6 through a conduit 4. A partial flow of the product is turned back to the mixing apparatus 3 through a conduit 7 by a pump 8 and at that time, the temperature of the mixing apparatus 3 is adjusted to be at the demanded temperature by a heat exchanger 9.

    PRODUCTION OF GAMMA, DELTA-UNSATURATED KETONE
    2.
    发明专利
    PRODUCTION OF GAMMA, DELTA-UNSATURATED KETONE 失效

    公开(公告)号：JPH10147548A

    公开(公告)日：1998-06-02

    申请号：JP31011997

    申请日：1997-11-12

    Applicant: BASF AG

    Inventor： ETZRODT HEINZ DR ,  STROEZEL MANFRED ,  WELLER DIETMAR DR ,  JAEDICKE HAGEN DR

    IPC: C07C45/69 ,  C07C45/67 ,  C07C45/71 ,  C07C45/76 ,  C07C49/203

    Abstract: PROBLEM TO BE SOLVED: To obtain the subject compound useful as an intermediate product for the production of perfumes, vitamin A, etc., by Carrol reaction in a specific solvent. SOLUTION: This γ,δ-unsaturated ketone, e.g. 2-methyl-2-hepten-6-one is obtained by using a cyclic carbonate of formula I (R -R are each H, methyl, etc.; R is H, isopropyl, etc.), e.g. ethylene carbonate, etc., a γ-lactone of formula II, e.g. γ-butyrolactone, etc., as a solvent, and reacting vinycarbinol or propargyl alcohol with an acetoacetic alkyl ester or diketene, then in the presence of an aluminum catalyst and at 120-220 deg.C, by thermal rearrangement reaction of the resultant acetoacetate to the aimed γ,δ-unsaturated ketone.

    DISTILLATION COLUMN FOR SEPARATING MIXTURE OF LIQUIDS INTO A PLURALITY OF PURE FRACTIONS
    3.
    发明专利
    DISTILLATION COLUMN FOR SEPARATING MIXTURE OF LIQUIDS INTO A PLURALITY OF PURE FRACTIONS 失效

    公开(公告)号：JPH0780201A

    公开(公告)日：1995-03-28

    申请号：JP19702394

    申请日：1994-08-22

    Applicant: BASF AG

    Inventor： KAIBEL GERD ,  STROEZEL MANFRED ,  PFEFFINGER JOACHIM

    IPC: B01D3/14 ,  B01D3/32

    Abstract: PURPOSE: To prevent heat flow passing through a separation device and to improve the separation efficiency of a distillation column by providing a gas chamber between two walls of the separation device, which functions in the longitudinal direction at the central zone of the distillation column and setting the space between the both walls to a specified value. CONSTITUTION: The distillation column 1 is divided by a separation device 5 into a feeding part 2 and a withdrawing part 3, which separation device 5 functions in the longitudinal direction at the central zone of the distillation column 1. The separation device 5 is constituted of two walls 4 and has a gas chamber between the walls. The distance between the walls is 1 to 50 mm. An inert gas is charged from an inert gas inlet 6 provided at the upper terminal part of the gas chamber and is introduced into a distillation chamber from an inert gas outlet 7 provided at the lower terminal part. A mixture of plural substances A, B, C is fed into a feeding part 2 and the substances are separated according to the order of the volatility of each substance into each pure fraction. The fraction A having high volatility and the fraction C having low volatility are withdrawn from the distillation column 1 as a overhead product and a bottom product, respectively. The fraction B having intermediate volatility is withdrawn from the side part of the distillation column as a side distillate product.

    PRODUCTION OF HIGHER UNSATURATED KETONE
    5.
    发明专利
    PRODUCTION OF HIGHER UNSATURATED KETONE 失效

    公开(公告)号：JP2000178221A

    公开(公告)日：2000-06-27

    申请号：JP32563599

    申请日：1999-11-16

    Applicant: BASF AG

    Inventor： OOST CARSTEN ,  STROEZEL MANFRED ,  ETZRODT HEINZ ,  DIETMAR WELLER ,  RHEUDE UDO ,  KAIBEL GERD ,  KRUG THOMAS ,  SPISKE LUISE ,  HAGEN IEEDIKKE

    IPC: B01J31/14 ,  C07B61/00 ,  C07C45/67 ,  C07C45/74 ,  C07C49/203

    Abstract: PROBLEM TO BE SOLVED: To produce the subject compound useful as an intermediate capable of producing isophytol of a precursor of an essential vitamin E in higher selectivity and higher space time yield by reacting a corresponding α,β-unsaturated alcohol with an alkyl acetoacetate by Carroll reaction. SOLUTION: (A) A corresponding α,β-unsaturated alcohol of formula II is reacted with (B) an alkyl acetoacetate of formula II (R3 is a 1-4C alkyl) in the presence of (C) 0.1-5 mol% organoaluminum compound as a catalyst in a reactor with a fractionating column while eliminating and continuously removing an alcohol of the formula R3-OH and produced carbon dioxide by distillation, and while introducing the components A and C to the reactor, further a calculated amount of the component B thereto preferably at 175-220 deg.C reaction temperature to provide the objective unsaturated ketone of formula I [a dotted line represents an additional C-C bond; R1 is a 1-4C alkyl; R2 is a 4-30C (un)saturated aliphatic or the like].

    METHOD TO REACT GRIGNARD COMPOUND WITH CARBONYL COMPOUND AND TO HYDROLIZE PRODUCT THEREAFTER
    6.
    发明专利
    METHOD TO REACT GRIGNARD COMPOUND WITH CARBONYL COMPOUND AND TO HYDROLIZE PRODUCT THEREAFTER 失效

    公开(公告)号：JPH10130179A

    公开(公告)日：1998-05-19

    申请号：JP28952597

    申请日：1997-10-22

    Applicant: BASF AG

    Inventor： STROEZEL MANFRED ,  RHEUDE UDO DR ,  RAHN RALF-THOMAS DR ,  KAIBEL GERD DR

    IPC: C07B49/00 ,  C07C29/124 ,  C07C29/40 ,  C07C31/00 ,  C07C33/02

    Abstract: PROBLEM TO BE SOLVED: To provide an improved method that enables to carry out, addition reaction between a Grignard compound and a carbonyl compound and the subsequent hydrolysis, without any trouble with respect to the plant-operation. SOLUTION: This method removes almost all the heat that is generated during exothermic reaction(s) of (a) an addition reaction between a halogenated organomagnesium compound shown by the formula RMgX (R is a 1-6C alkyl, 2-6C alkenyl, 2-6C alkynyl, or an aryl; X is Cl, Br, or I) and a carbonyl compound and/or (b) a hydrolysis of the resulting addition product, by carrying out at least one of these reactions in a solvent or a mixture of solvents and evaporating the solvent or the mixture of solvents.

    PRODUCTION OF UNSATURATED KETONE
    8.
    发明专利
    PRODUCTION OF UNSATURATED KETONE 失效

    公开(公告)号：JP2000159721A

    公开(公告)日：2000-06-13

    申请号：JP33329199

    申请日：1999-11-24

    Applicant: BASF AG

    Inventor： OOST CARSTEN ,  STROEZEL MANFRED ,  ETZRODT HEINZ ,  DIETMAR WELLER ,  KAIBEL GERD DR ,  HAGEN IEEDIKKE

    IPC: B01J31/12 ,  B01J19/18 ,  C07B61/00 ,  C07C45/67 ,  C07C45/68 ,  C07C45/70 ,  C07C49/203

    Abstract: PROBLEM TO BE SOLVED: To obtain an unsaturated ketone in a high yield by subjecting a specific α,β-unsaturated alcohol and an alkyl acetoacetate to a Carol reaction in the presence of an organic aluminum compound in the absence of a solvent at a specific reaction temperature. SOLUTION: This method for producing an unsaturated ketone of formula III (the dotted line is an additional C-C bond; R1 is a 1-2C alkyl; R2 is a 1-4C alkyl) comprises reacting (A) an α,β-unsaturated alcohol of formula I with (B) an alkyl acetoacetate of formula II in the presence of (C) an organic aluminum compound in a reactor system having a rectifier connected thereto, while continuously removing an alcohol of the formula: R3OH released from the alkyl acetoacetate during the release reaction and during the Carol reaction. In the reaction, the component A has a boiling point of

    CONTINUOUS PRODUCTION OF UNSATURATED KETONE
    9.
    发明专利
    CONTINUOUS PRODUCTION OF UNSATURATED KETONE 失效

    公开(公告)号：JP2000086566A

    公开(公告)日：2000-03-28

    申请号：JP25309699

    申请日：1999-09-07

    Applicant: BASF AG

    Inventor： OOST CARSTEN ,  STROEZEL MANFRED ,  ETZRODT HEINZ ,  DIETMAR WELLER ,  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: PROBLEM TO BE SOLVED: To continuously produce an unsaturated ketone in high yield for a short time in a single reactor without using a medium-boiling material by reacting an unsaturated alcohol with an alkyl acetoacetate in the presence of an organic aluminum compound. SOLUTION: The purpose of this invention is achieved by reacting an unsaturated alcohol of formula I [R1 is a 1-4C alkyl; R2 is a (methoxy-substituted) (1-37C) aliphatic hydrocarbon group or the like] with an alkyl acetoacetate of formula II (R3 is a 1-5C alkyl) on the internal structure of a rectifier to form an acetoacetate of an unsaturated alcohol, by separating an alcohol of the formula R3-OH from the overhead flow of the rectifier, and (A) by making the resultant acetoacetate of an alcohol of formula I rearrange into an unsaturated ketone of formula III in the presence of an organic aluminum compound (pref. an aluminum trialkoxide) in the lower part of the rectifier and/or (B) by feeding carbon dioxide formed each time at the bottom of the rectifier to the overhead flow through the rectifier and by separating an unsaturated ketone of formula III from the rectifier through the bottom.

    PRODUCTION OF 2,5,6-TRIMETHYL-2-CYCLOHEXEN-1-ONE
    10.
    发明专利
    PRODUCTION OF 2,5,6-TRIMETHYL-2-CYCLOHEXEN-1-ONE 失效

    公开(公告)号：JPH11292819A

    公开(公告)日：1999-10-26

    申请号：JP6492199

    申请日：1999-03-11

    Applicant: BASF AG

    Inventor： RUFF DETLEF DR ,  BURST WOLFRAM ,  KAISER WULF DR ,  STROEZEL MANFRED

    IPC: C07C45/72 ,  C07C45/74 ,  C07C49/603

    Abstract: PROBLEM TO BE SOLVED: To provide a method for producing 2,5,6-trimethyl-2-cyclohexen-1-one in industrial scale, good yield and good space time yield. SOLUTION: This method for producing 2,5,6-trimethyl-2-cyclohexen-1-on comprises simultaneously pumping 1 mol crotonaldehyde or 1 mol compound which is converted under the reaction conditions into crotonaldehyde, about 5-30 mol diethyl ketone and the aqueous solution or suspension of a strong base in the presence of a base agent at elevated temperature, through separate lines or at least partly in the form of a suitable mixture, continuously into a pressure vessel, which is heated where appropriate and which ensures vigorous mixing, in such a way that the reaction temperature is 150-350 deg.C and the average residence time in the pressure vessel is about 0.1 second to 20 min.

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