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    METHOD FOR CONTROLLING A REACTIVE DISTILLATION COLUMN
    1.
    发明公开
    METHOD FOR CONTROLLING A REACTIVE DISTILLATION COLUMN 审中-公开

    公开(公告)号：US20240018078A1

    公开(公告)日：2024-01-18

    申请号：US18039504

    申请日：2021-12-01

    Applicant: BASF SE

    Inventor： Wolf-Steffen WEISSKER ,  Edward RICHMOND

    IPC: C07C31/30 ,  C07C29/70 ,  B01D3/00 ,  B01D3/42

    CPC classification number: C07C31/30 ,  C07C29/705 ,  B01D3/009 ,  B01D3/4277

    Abstract: A method for controlling a reactive distillation column for effecting a transalcoholisation reaction, comprising feeding a metal methoxide into the reactive distillation column via a side feed; feeding a reactant alcohol into a lower part of the reactive distillation column; withdrawing methanol from the top of the reactive distillation column; and withdrawing a solution of a product metal alkoxide in the reactant alcohol from the bottom of the reactive distillation column; wherein the method comprises a process control scheme selected from: Scheme A: establishing a signal S1 which is responsive to a temperature in the rectifying section disposed above the feed of the metal methoxide; and manipulating in response to the signal S1 the feed amount of the reactant alcohol; Scheme B: establishing a signal S1 which is responsive to a temperature in the rectifying section disposed above the feed of the metal methoxide; and manipulating in response to the signal S1 the heat supplied to the bottom of the reactive distillation column. The invention also relates to a method for controlling a reactive distillation column for effecting a transalcoholisation reaction, comprising feeding a metal methoxide into the reactive distillation column via a side feed; feeding a reactant alcohol into a lower part of the reactive distillation column; causing an auxiliary alcohol to be present in the reactive distillation column; and optionally replenishing the auxiliary alcohol via a side feed located above the feed of the reactant alcohol and below the top of the column; withdrawing methanol from the top of the reactive distillation column; and withdrawing a solution of a product metal alkoxide in the reactant alcohol from the bottom of the reactive distillation column; wherein the method comprises a process control scheme selected from: Scheme C: establishing a signal S2 which is responsive to a temperature at a point located between the feed of the metal methoxide and the bottom of the reactive distillation column; and manipulating in response to the signal S2 the feed amount of the reactant alcohol; Scheme D: establishing a signal S2 which is responsive to a temperature at a point located between the feed of the metal methoxide and the bottom of the reactive distillation column; and manipulating in response to the signal S2 the heat supplied to the bottom of the reactive distillation column. The methods of the invention allow for improved controlling of a reactive distillation column for effecting a transalcoholisation reaction.

    METHOD FOR PREPARING 1-HYDROXY-2-METHYL-3-PENTANONE
    2.
    发明申请
    METHOD FOR PREPARING 1-HYDROXY-2-METHYL-3-PENTANONE 审中-公开

    公开(公告)号：US20200010394A1

    公开(公告)日：2020-01-09

    申请号：US16460327

    申请日：2019-07-02

    Applicant: BASF SE

    Inventor： Dagmar Pascale KUNSMANN-KEITEL ,  Georg Heinrich GROSCH ,  Jan-Dirk ARNDT ,  Gauthier Luc Maruice AVERLANT ,  Wolf-Steffen WEISSKER ,  Marcus Georg SCHREMS ,  Dan-Tam Daniel TANG

    IPC: C07C45/64 ,  C07C45/83 ,  C07C49/17

    Abstract: Method for preparing 1-hydroxy-2-methyl-3-pentanone (I) by reacting formaldehyde with diethyl ketone in a reactor in the presence of water and a basic component at a temperature of 50 to 150° C. and a pressure of 0.2 to 10 MPa abs, in which the basic component used is a trialkylamine from the group comprising trimethylamine, N,N-dimethylethylamine, N,N-diethylmethylamine, triethylamine, N,N-dimethyl-n-propylamine, N-ethyl-N-methyl-n-propylamine, N,N-dimethylisopropylamine, N-ethyl-N-methylisopropylamine, N,N-dimethyl-n-butylamine, N,N-dimethylisobutylamine and N,N-dimethyl-sec-butylamine, and from the reaction mixture obtained, trialkylamine as low boiler and a bottom product comprising 1-hydroxy-2-methyl-3-pentanone (I) as high boiler are separated in a distillation apparatus, wherein the distillation apparatus is operated at a top pressure of 0.2 to 1 MPa abs.

    PROCESS FOR THE PREPARATION OF C3-5 SATURATED ALIPHATIC CARBOXYLIC ACIDS
    3.
    发明申请
    PROCESS FOR THE PREPARATION OF C3-5 SATURATED ALIPHATIC CARBOXYLIC ACIDS 有权

    公开(公告)号：US20230047974A1

    公开(公告)日：2023-02-16

    申请号：US17791542

    申请日：2020-12-29

    Applicant: BASF SE

    Inventor： Joaquim Henrique TELES ,  Jessica Nadine HAMANN ,  Jonathan Thomas LEFEBVRE ,  Wolf-Steffen WEISSKER ,  Shelue LIANG

    IPC: C07C51/235 ,  C07C51/44

    Abstract: A process for the preparation of a saturated aliphatic carboxylic acid with 3 to 5 carbon atoms by oxidation of the corresponding aldehyde with oxygen in which (a) the corresponding aldehyde is converted with oxygen at a temperature of 40 to 150° C. and an oxygen partial pressure of 0.001 to 1 MPa to obtain a mixture containing the saturated aliphatic carboxylic acid and ≤2 mol-% of the corresponding aldehyde with respect to the saturated aliphatic carboxylic acid, (b) the mixture obtained in step (a) is thermally treated in the liquid phase at a temperature of 80 to 250° C. and a pressure of 0.1 to 2 MPa abs for 0.25 to 100 hours, and (c) the mixture obtained in step (b) is distilled in a distillation apparatus to obtain a distillate containing ≥90 wt.-% of the saturated aliphatic carboxylic acid and having an active oxygen content of 0 to 25 wt.-ppm based on the distillate.

    PROCESS FOR PREPARING METAL ALKOXIDES BY TRANSALCOHOLISATION
    4.
    发明公开
    PROCESS FOR PREPARING METAL ALKOXIDES BY TRANSALCOHOLISATION 审中-公开

    公开(公告)号：US20240002319A1

    公开(公告)日：2024-01-04

    申请号：US18039503

    申请日：2021-12-01

    Applicant: BASF SE

    Inventor： Wolf-Steffen WEISSKER ,  Edward RICHMOND

    IPC: C07C29/70 ,  C07C29/80

    CPC classification number: C07C29/705 ,  C07C29/80

    Abstract: A process for preparing metal alkoxides by transalcoholisation, comprising: feeding a lower metal alkoxide and a higher alcohol into a reactive distillation column; removing a solution of a higher metal alkoxide in the higher alcohol from the bottom of the column or from a recycle stream taken from the bottom of the column; and removing a gaseous lower alcohol from the top of the column, at least partially condensing the gaseous lower alcohol, and recirculating a part of the condensate to the top of the column; wherein an auxiliary alcohol is provided in the reactive distillation column, the boiling point of the auxiliary alcohol being between the boiling point of the lower alcohol and the boiling point of the higher alcohol at the pressure prevailing in the reactive distillation column. The process allows for high conversion of a lower metal alkoxide to a higher metal alkoxide while limiting the formation of solid deposits in the column, while having low energy requirements.

    CATALYTIC PROCESS FOR PREPARING AN a,ß-ETHYLENICALLY UNSATURATED CARBOXYLIC ACID SALT
    8.
    发明申请
    CATALYTIC PROCESS FOR PREPARING AN a,ß-ETHYLENICALLY UNSATURATED CARBOXYLIC ACID SALT 有权

    公开(公告)号：US20230138524A1

    公开(公告)日：2023-05-04

    申请号：US17911666

    申请日：2021-03-17

    Applicant: BASF SE

    Inventor： Nuria HUGET SUBIELA ,  Wolf-Steffen WEISSKER

    IPC: C07C51/15 ,  B01J31/24

    Abstract: A catalytic process for preparing an α,β-ethylenically unsaturated carboxylic acid salt, comprising a) contacting an alkene and carbon dioxide with a carboxylation catalyst, an organic solvent, and an alkoxide having a secondary or tertiary carbon atom directly bound to an [O−] group, to obtain a crude reaction product comprising the α,β-ethylenically unsaturated carboxylic acid salt and an alcohol by-product which is the conjugate acid of the alkoxide, b) allowing the α,β-ethylenically unsaturated carboxylic acid salt to precipitate out from the crude reaction product; and c) subjecting at least part of the crude reaction product to a mechanical separation step while maintaining the alcohol by-product in liquid form to obtain a solid phase comprising the α,β-ethylenically unsaturated carboxylic acid salt and a liquid phase comprising the carboxylation catalyst, the organic solvent and the alcohol by-product. The process allows for easy separation of the α,β-ethylenically unsaturated carboxylic acid salt by a mechanical separation operation.

    METHOD FOR PRODUCING METAL ALCOHOLATES
    9.
    发明申请
    METHOD FOR PRODUCING METAL ALCOHOLATES 有权

    公开(公告)号：US20230054206A1

    公开(公告)日：2023-02-23

    申请号：US17785674

    申请日：2020-12-16

    Applicant: BASF SE

    Inventor： Wolf-Steffen WEISSKER ,  Nuria HUGUET SUBIELA

    IPC: C07C29/70

    Abstract: Process for preparing metal alkoxides by means of transalcoholization, wherein a lower metal alkoxide is fed via a side feed into a reactive distillation column comprising a rectifying section situated above the feed and a stripping section situated below the feed; a higher alcohol is fed into the stripping section, the bottom and/or a bottoms circuit of the column; a solution of a higher metal alkoxide in the higher alcohol is taken off at the bottom of the column and/or from the bottoms circuit; and a vapor comprising lower alcohol is taken off at the top of the column, the vapor is at least partially condensed and a substream of the condensate is recycled to the top of the column as reflux. The process enables the preparation of metal alkoxides with a reduced energy requirement.

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