阅读说明：本技术 一种对乙酰氨基苯磺酰氯的生产工艺 (Production process of p-acetamido-benzenesulfonyl chloride ) 是由 蔡红新 闫玲玲 陈东梅 王书擘 *** 于 2019-10-28 设计创作，主要内容包括：本发明创造涉及一种对乙酰氨基苯磺酰氯的生产工艺,所述生产工艺包括以下步骤：A、以乙酰苯胺为原料,反应溶剂采用氯仿,在反应釜内加入氯磺酸,加入过程中进行雾化处理；B、将步骤A中的混合液搅拌处理,搅拌时间为3-4h；C、对步骤B中的反应液进行加热,加热温度为50-55度,并保持1-1.5h；D、向步骤C中的反应液内加入五氯化磷,保温反应1-2h；E、将步骤D中的溶液进行离心处理,离心完毕后静置3-4h,然后将下层液体导入结晶釜中；F、对步骤E的结晶进行清洗,清洗完毕后进行密封收集；本发明具有环保、制作方便的优点。(The invention relates to a production process of p-acetamido-benzenesulfonyl chloride, which comprises the following steps: A. acetanilide is used as a raw material, chloroform is used as a reaction solvent, chlorosulfonic acid is added into a reaction kettle, and atomization treatment is carried out in the adding process; B. b, stirring the mixed solution obtained in the step A for 3-4 hours; C. heating the reaction solution in the step B at 50-55 ℃ for 1-1.5 h; D. adding phosphorus pentachloride into the reaction liquid in the step C, and reacting for 1-2h under the condition of heat preservation; E. d, centrifuging the solution in the step D, standing for 3-4h after centrifugation is finished, and then introducing the lower-layer liquid into a crystallization kettle; F. e, cleaning the crystals obtained in the step E, and sealing and collecting the crystals after cleaning; the invention has the advantages of environmental protection and convenient manufacture.)

1. A production process of p-acetamido-benzenesulfonyl chloride is characterized by comprising the following steps: the production process comprises the following steps:

A. acetanilide is used as a raw material, chloroform is used as a reaction solvent, chlorosulfonic acid is added into a reaction kettle, and atomization treatment is carried out in the adding process;

B. b, stirring the mixed solution obtained in the step A for 3-4 hours;

C. heating the reaction solution in the step B at 50-55 ℃ for 1-1.5 h;

D. adding phosphorus pentachloride into the reaction liquid in the step C, and reacting for 1-2h under the condition of heat preservation;

E. d, centrifuging the solution in the step D, standing for 3-4h after centrifugation is finished, and then introducing the lower-layer liquid into a crystallization kettle;

F. and E, cleaning the crystals obtained in the step E, and sealing and collecting the crystals after the crystals are cleaned.

2. The process for producing p-acetamidobenzenesulfonyl chloride as claimed in claim 1, wherein: the mass ratio of the acetanilide to the chloroform to the chlorosulfonic acid to the phosphorus pentachloride is 4:2:0.5: 0.4.

3. The process for producing p-acetamidobenzenesulfonyl chloride as claimed in claim 1, wherein: the stirring speed in the step B is 400-600r/min, and the stirring speed in the reaction is gradually reduced.

4. The process for producing p-acetamidobenzenesulfonyl chloride as claimed in claim 1, wherein: the phosphorus pentachloride is used as a chlorinating agent.

5. The process according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: the production process comprises the following steps:

A. acetanilide is used as a raw material, chloroform is used as a reaction solvent, chlorosulfonic acid is added into a reaction kettle, and atomization treatment is carried out in the adding process;

B. b, stirring the mixed solution obtained in the step A for 3 hours;

C. heating the reaction solution in the step B at 50 ℃ for 1 h;

D. adding phosphorus pentachloride into the reaction liquid in the step C, and reacting for 1h under the condition of heat preservation;

E. d, centrifuging the solution in the step D, standing for 3 hours after centrifugation is finished, and then introducing the lower-layer liquid into a crystallization kettle;

F. and E, cleaning the crystals obtained in the step E, and sealing and collecting the crystals after the crystals are cleaned.

6. The process according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: the production process comprises the following steps:

A. acetanilide is used as a raw material, chloroform is used as a reaction solvent, chlorosulfonic acid is added into a reaction kettle, and atomization treatment is carried out in the adding process;

B. b, stirring the mixed solution obtained in the step A for 4 hours;

C. heating the reaction solution in the step B at 55 ℃ for 1.5 h;

D. adding phosphorus pentachloride into the reaction liquid in the step C, and reacting for 2 hours under the condition of heat preservation;

E. d, centrifuging the solution in the step D, standing for 4 hours after centrifugation is finished, and then introducing the lower-layer liquid into a crystallization kettle;

F. and E, cleaning the crystals obtained in the step E, and sealing and collecting the crystals after the crystals are cleaned.

Technical Field

The invention belongs to the technical field of chemical industry, and particularly relates to a production process of p-acetamido benzene sulfonyl chloride.

Background

P-acetamidobenzenesulfonyl chloride is an intermediate for preparing sulfanilamide bactericidal and mildew-inhibiting medicines such as sulfadiazine, sulfisoxazole, sulfpyrazole, sulfadimidine and the like, is also used for synthesizing dyes, and is widely applied to the fields of medicines, coatings, plastics, pesticides and the like; currently, the production of p-acetamidobenzenesulfonyl chloride mostly adopts the traditional process of chlorosulfonation of p-acetanilide by using excessive chlorosulfonic acid. Chlorosulfonation in the existing synthesis process is an equilibrium reaction, and large excess chlorosulfonic acid must be used to participate in the reaction in order to improve the yield. A large amount of hydrogen chloride gas is generated in the synthesis process, so that not only is serious acidic wastewater pollution caused, but also the forward progress of the reaction is influenced, and the purity of the product is reduced, and aiming at the defects, the development of an environment-friendly and convenient-to-manufacture production process of p-acetamidobenzenesulfonyl chloride is necessary; therefore, the development of the environment-friendly and convenient production process of the p-acetaminophenylsulfonyl chloride is of great significance.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a production process of p-acetamido-benzenesulfonyl chloride, which is environment-friendly and convenient to prepare.

The purpose of the invention is realized as follows: a production process of p-acetamido-benzenesulfonyl chloride comprises the following steps:

A. acetanilide is used as a raw material, chloroform is used as a reaction solvent, chlorosulfonic acid is added into a reaction kettle, and atomization treatment is carried out in the adding process;

B. b, stirring the mixed solution obtained in the step A for 3-4 hours;

C. heating the reaction solution in the step B at 50-55 ℃ for 1-1.5 h;

D. adding phosphorus pentachloride into the reaction liquid in the step C, and reacting for 1-2h under the condition of heat preservation;

E. d, centrifuging the solution in the step D, standing for 3-4h after centrifugation is finished, and then introducing the lower-layer liquid into a crystallization kettle;

F. and E, cleaning the crystals obtained in the step E, and sealing and collecting the crystals after the crystals are cleaned.

The mass ratio of the acetanilide to the chloroform to the chlorosulfonic acid to the phosphorus pentachloride is 4:2:0.5: 0.4.

The stirring speed in the step B is 400-600r/min, and the stirring speed in the reaction is gradually reduced.

The phosphorus pentachloride is used as a chlorinating agent.

The production process comprises the following steps:

A. acetanilide is used as a raw material, chloroform is used as a reaction solvent, chlorosulfonic acid is added into a reaction kettle, and atomization treatment is carried out in the adding process;

B. b, stirring the mixed solution obtained in the step A for 3 hours;

C. heating the reaction solution in the step B at 50 ℃ for 1 h;

D. adding phosphorus pentachloride into the reaction liquid in the step C, and reacting for 1h under the condition of heat preservation;

E. d, centrifuging the solution in the step D, standing for 3 hours after centrifugation is finished, and then introducing the lower-layer liquid into a crystallization kettle;

F. and E, cleaning the crystals obtained in the step E, and sealing and collecting the crystals after the crystals are cleaned.

The production process comprises the following steps:

A. acetanilide is used as a raw material, chloroform is used as a reaction solvent, chlorosulfonic acid is added into a reaction kettle, and atomization treatment is carried out in the adding process;

B. b, stirring the mixed solution obtained in the step A for 4 hours;

C. heating the reaction solution in the step B at 55 ℃ for 1.5 h;

D. adding phosphorus pentachloride into the reaction liquid in the step C, and reacting for 2 hours under the condition of heat preservation;

E. d, centrifuging the solution in the step D, standing for 4 hours after centrifugation is finished, and then introducing the lower-layer liquid into a crystallization kettle;

F. and E, cleaning the crystals obtained in the step E, and sealing and collecting the crystals after the crystals are cleaned.

The invention has the beneficial effects that: the invention has the advantages that the product yield is obviously improved, the solvent can be recycled, the ecological environment is protected, and other beneficial effects are detailed in specific embodiments.

Detailed Description

The technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein are for the purpose of describing particular embodiments only and are not intended to be limiting of the invention, and terms such as "and/or" as used herein include any and all combinations of one or more of the associated listed items; in addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.