公开(公告)号：US20220388949A1

公开(公告)日：2022-12-08

申请号：US17775966

申请日：2020-11-13

Applicant: BASF SE

Inventor： Stefan BLEI ,  Friedemann GAITZSCH ,  Christian SCHUETZ ,  Indre THIEL ,  Petra DECKERT ,  Jun GAO ,  Jessica Nadine HAMANN ,  Andreas MELZER

IPC: C07C315/06

Abstract: The invention relates to a process for working up water containing 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone as impurities, comprising: (a) mixing the water containing 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone as impurities with an organic solvent in which 4,4′-dichlorodiphenyl sulfoxide and/or 4,4′-dichlorodiphenyl sulfone have a solubility of at least 0.5 wt % based on the amount of 4,4′-dichlorodiphenyl sulfoxide and/or 4, 4′-dichlorodiphenyl sulfone and organic solvent at 20° C., which forms a two-phase system with water and which can be stripped from water with a stripping gas and subsequently separating the obtained mixture into an aqueous phase and an organic phase, and (b) stripping the organic solvent from the aqueous phase with a stripping gas.

公开(公告)号：US20220324795A1

公开(公告)日：2022-10-13

申请号：US17635142

申请日：2020-08-20

Applicant: BASF SE

Inventor： Jessica Nadine HAMANN ,  Stefan BLEI ,  Oliver BEY

IPC: C07C315/02 ,  C07C317/14

Abstract: The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone comprising reacting a solution comprising 4,4′-dichlorodiphenyl sulfoxide and at least one linear C6-C10 carboxylic acid as solvent with an oxidizing agent to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone, wherein the concentration of water in the reaction mixture is kept below 5 wt %, the process comprising: (a) adding 0.9 to 1.05 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide uniformly distributed to the solution at a temperature in the range from 80 to 105° C. over a period from 1.5 to 5 h in a first step to obtain the reaction mixture; (b) agitating the reaction mixture after completion of the first step at the temperature of the first step for 5 to 30 min without adding oxidizing agent; (c) adding 0.05 to 0.2 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide to the reaction mixture at a temperature in the range from 80 to 105° C. over a period of less than 40 min in a second step; (d) agitating the reaction mixture after completion of the second step at the temperature of the second step for 10 to 30 min without adding oxidizing agent, (e) heating the reaction mixture to a temperature in the range from 95 to 110° C. and hold this temperature for 10 to 90 min to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone.

公开(公告)号：US20220267261A1

公开(公告)日：2022-08-25

申请号：US17635580

申请日：2020-08-20

Applicant: BASF SE

Inventor： Jun GAO ,  Frauke THRUN ,  Indre THIEL ,  Jessica Nadine HAMANN ,  Christian SCHUETZ ,  Stefan BLEI

IPC: C07C315/02 ,  C07C315/06

Abstract: The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone, comprising: (I) reacting thionyl chloride, chlorobenzene and aluminum chloride forming an intermediate reaction product and hydrogen chloride; (II) mixing aqueous hydrochloric acid and the intermediate reaction product to obtain an organic phase comprising 4,4′-dichlorodiphenyl sulfoxide and an aqueous phase; (III) cooling the organic phase to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfoxide to obtain a suspension; (IV) solid-liquid-separation of the suspension to obtain crystallized 4,4′-dichlorodiphenyl sulfoxide, and mother liquor; (V) washing the crystallized 4,4′-dichlorodiphenyl sulfoxide with a carboxylic acid to obtain carboxylic acid-wet 4,4′-dichlorodiphenyl sulfoxide; (VI) reacting the washed 4,4′-dichlorodiphenyl sulfoxide and an oxidizing agent in a carboxylic acid as solvent to obtain a reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid; (VII) separating the reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid into a residual moisture comprising 4,4′-dichlorodiphenyl sulfone as crude product and a liquid phase comprising carboxylic acid.

公开(公告)号：US20220135523A1

公开(公告)日：2022-05-05

申请号：US17429200

申请日：2020-02-06

Applicant: BASF SE

Inventor： Indre THIEL ,  Christian SCHUETZ ,  Andreas MELZER ,  Stefan BLEI

IPC: C07C315/06

Abstract: The invention relates to a process for purifying 4,4′-dichlorodiphenyl sulfoxide comprising: (a) providing a suspension comprising particulate 4,4′-dichlorodiphenyl sulfoxide in monochlorobenzene, (b) solid-liquid separation of the suspension to obtain residual moisture containing 4,4′-dichlorodiphenyl sulfoxide, (c) washing residual moisture containing 4,4′-dichlorodiphenyl sulfoxide with monochlorobenzene, (d) optionally repeating steps (a) to (c).

公开(公告)号：US20220135522A1

公开(公告)日：2022-05-05

申请号：US17429028

申请日：2020-02-06

Applicant: BASF SE

Inventor： Lukas METZGER ,  Christian SCHUETZ ,  Indre THIEL ,  Stefan BLEI

IPC: C07C315/06

Abstract: The invention relates to a process for obtaining 4,4′-dichlorodiphenyl sulfoxide from a liquid mixture comprising dichlorodiphenyl sulfoxide and a solvent, comprising: (a) cooling the liquid mixture to a temperature below the saturation point of 4,4′-dichlorodiphenyl sulfoxide in the solvent to obtain a suspension comprising crystallized 4,4′-dichlorodiphenyl sulfoxide, (b) solid-liquid-separation of the suspension to obtain a residual moisture containing solid 4,4′-dichlorodiphenyl sulfoxide as a product and mother liquor, (c) concentrating the mother liquor, (d) recycling at least a part of the concentrated mother liquor into the cooling step (a).

公开(公告)号：US20220135521A1

公开(公告)日：2022-05-05

申请号：US17429035

申请日：2020-02-06

Applicant: BASF SE

Inventor： Indre THIEL ,  Oliver BEY ,  Christian SCHUETZ ,  Stefan BLEI

IPC: C07C315/02 ,  C07C315/06

Abstract: The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfoxide comprising: (a) reacting thionyl chloride, chlorobenzene and aluminum chloride in a molar ratio of thionyl chloride:chlorobenzene:aluminum chloride of 1:(6 to 9):(1 to 1.5) at a temperature in the range from 0 to below 20° C., forming an intermediate reaction product and hydrogen chloride, (b) mixing aqueous hydrochloric acid and the intermediate reaction product at a temperature in the range from 70 to 110° C. to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfoxide, (c) separating the crude reaction product into an organic phase comprising the 4,4′-dichlorodiphenyl sulfoxide and an aqueous phase, (d) washing the organic phase with an extraction liquid.

公开(公告)号：US20220127221A1

公开(公告)日：2022-04-28

申请号：US17429043

申请日：2020-02-04

Applicant: BASF SE

Inventor： Indre THIEL ,  Christian SCHUETZ ,  Stefan BLEI ,  Jun GAO ,  Lukas METZGER

IPC: C07C315/06

Abstract: The invention relates to a crystal (C) consisting of at least 95% by weight of 4,4′-dichlorodiphenylsulfoxide, 0 to 2% by weight of impurities and 0 to 3% by weight of an organic solvent (os). Moreover, the present invention relates to a crystal composition (CC) comprising crystals (C) and a process for the production of the crystal composition (CC) and the crystal (C).