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Industrial production method for toluene sulfonamide

A technology of p-toluenesulfonamide and p-toluenesulfonyl chloride, which is applied in the field of industrial production of p-toluenesulfonamide, can solve the problems of high labor intensity, large amount of ammonia nitrogen, low yield, etc., to reduce labor intensity, reduce COD emissions, reduce Effects of Environmental Pollution

Active Publication Date: 2012-07-18
浙江嘉化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] This reaction process will produce a large amount of ammonia nitrogen waste water, and the yield is low
Intermittent reaction is labor intensive

Method used

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  • Industrial production method for toluene sulfonamide
  • Industrial production method for toluene sulfonamide
  • Industrial production method for toluene sulfonamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The dichloromethane solution of p-toluenesulfonyl chloride is sent from the acid chloride workshop to the intermediate storage tank. Then the dichloromethane solution of p-toluenesulfonyl chloride is injected into the first-level amination still with the speed of 300kg / h by delivery pump, and puts into the first-level amination still with the dichloromethane from head tank at the speed of 450kg / h simultaneously . Through the side outlet of the primary amination kettle, it enters the secondary amination kettle in the form of overflow, and then enters the third-level amination kettle in the form of overflow through the side outlet of the second-level amination kettle, and then enters the fourth-level amination kettle in the same way. grade amination kettle. Then it enters the centrifuge through the lower outlet of the fourth-stage amination kettle. Reactor temperature control is 20~35 ℃.

[0043] Ammonia gas enters from the three-stage amination kettle with a flow rate...

Embodiment 2

[0050] Process is identical with embodiment 1, and each process parameter is:

[0051] The dichloromethane solution of p-toluenesulfonyl chloride is squeezed into the primary amination still with the speed of 560kg / h,

[0052] Dichloromethane is put into the primary amination kettle from the head tank at a speed of 840kg / h,

[0053] The temperature of the amination reaction is controlled at 20-35°C,

[0054] The flow rate of the ammonia entering the three-stage amination kettle is 51kg / h,

[0055] The temperature of the dissolution tank is controlled at 70-80°C,

[0056] The temperature of the decolorization kettle is controlled at 70-80°C,

[0057] The temperature of the crystallization tank is controlled at 5-15°C,

[0058] The washing temperature of the washing tank is 25-40°C.

[0059] After the system operated for 195 hours, 48.882t of p-toluenesulfonamide was obtained, and the output rate was 251kg / h.

Embodiment 3

[0061] Process is identical with embodiment 1, and each process parameter is:

[0062] The dichloromethane solution of p-toluenesulfonyl chloride is injected into the primary amination kettle at a speed of 1000kg / h,

[0063] Dichloromethane is put into the primary amination kettle from the head tank at a speed of 1500kg / h,

[0064] The temperature of the amination reaction is controlled at 20-35°C,

[0065] The flow rate of the ammonia entering the three-stage amination kettle is 90kg / h,

[0066] The temperature of the dissolution tank is controlled at 70-80°C,

[0067] The temperature of the decolorization kettle is controlled at 70-80°C,

[0068] The temperature of the crystallization tank is controlled at 5-15°C,

[0069] The washing temperature of the washing tank is 25-40°C.

[0070] After running the system for 288 hours, 128.921t of p-toluenesulfonamide was obtained, and the output rate was 447kg / h.

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Abstract

The invention discloses an industrial production method for toluene sulfonamide. Continuous amination is performed on paratoluensulfonyl chloride and ammonia gas in methylene dichloride solvent in a countercurrent absorbing way, then active carbon is used for decoloring, and through alcohol recrystallization and drying after water scrubbing, a qualified product can be obtained. Meanwhile, continuous production is achieved, that gas ammonia in tail gas is discharged within controlling index of national standards can be achieved, environment pollutions are reduced, and meanwhile, labor intensity is lowered. Solvent is adopted for replacing water for amination, the side reaction of hydrolyzation is stopped, and COD emission in waste water is lowered greatly while reaction conversion rate is improved.

Description

technical field [0001] The invention relates to an industrial production process of amide, and an industrial production method of p-toluenesulfonamide. Background technique [0002] p-toluenesulfonamide is a very important organic synthetic drug intermediate, commonly used in the synthesis of dozens of drugs such as chloramphenicol, chloramine-T, and thiamphenicol. [0003] The existing mature p-toluenesulfonamide production process is to use a batch reaction kettle, use p-toluenesulfonyl chloride as raw material, mix with 20% ammonia water, add water 2.5 times the mass of p-toluenesulfonyl chloride, heat up to 55 ° C for 2 hours, and then heat up Heat at 65°C for 2 hours, then raise the temperature to 75°C for 2 hours, and finally raise the temperature to 95°C for 1 hour. After the reaction was completed, it was cooled and filtered to obtain a solid crude product. After washing with water, filtering and drying, the product p-toluenesulfonamide is obtained. [0004] The r...

Claims

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Application Information

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IPC IPC(8): C07C311/16C07C303/38C07C303/44
Inventor 王宏亮沈高庆俞兴源汪晓林赵丽丰周航峰屠力冬顾群峰
Owner 浙江嘉化新材料有限公司
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