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Method for treating organic waste acids in p-acetamidobenzene sulfonyl chloride synthesis

A technique for treating acetaminobenzenesulfonyl chloride and its treatment method, which is applied in the field of synthesis of acetaminobenzenesulfonyl chloride, and can solve the problems of difficult utilization of organic waste acids, high production and environmental protection treatment costs, and low yield of acetaminobenzenesulfonyl chloride.

Active Publication Date: 2020-07-10
湖南吴赣药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] But product paracetamol sulfonyl chloride, part unreacted acetanilide raw material and reaction intermediate paracetamol sulfonic acid can be dissolved in the dilute sulfuric acid, thereby cause the yield of paracetamol sulfonyl chloride to be low; And produce A large amount of organic waste acid is difficult to use and can only be treated as organic waste acid. The traditional technical route for organic waste acid treatment is acid-base neutralization to produce miscellaneous salts, but the amount of miscellaneous salts is too large, resulting in high production and environmental protection treatment costs.

Method used

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  • Method for treating organic waste acids in p-acetamidobenzene sulfonyl chloride synthesis

Examples

Experimental program
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Effect test

Embodiment 1

[0019] The present embodiment provides a kind of processing method of organic waste acid in the synthesis of acetaminobenzenesulfonyl chloride, and it comprises the following steps:

[0020] (a) Pump organic waste sulfuric acid (the organic waste sulfuric acid is tested, and the percentage of organic matter is 4.3%, the same below) is pumped into the macroporous resin bed, and organic matter is adsorbed at 20°C and a pressure of 1barg Retention, the hydraulic retention time is 15min; after testing, the organic waste sulfuric acid (defined as sulfuric acid solution) after being absorbed by the macroporous resin bed, the concentration of organic matter in the organic waste sulfuric acid is 0.12% (the organic matter adsorption removal rate is 97.2%);

[0021] (b) After the aforementioned sulfuric acid solution is pumped into the mixer and fully mixed with the oxidant (the amount of hydrogen peroxide added is 5% of the mass of the sulfuric acid solution, calculated as 27.5%wt), it ...

Embodiment 2

[0027] This example provides a treatment method for organic waste acid in the synthesis of acetaminobenzenesulfonyl chloride, which is basically the same as that in Example 1, except that in step (a), the parameters in the macroporous resin bed are controlled as The temperature is 0°C, 5 barg and the hydraulic retention time is 20 min; the yield of p-acetamidobenzenesulfonyl chloride is finally synthesized up to 96.5%.

Embodiment 3

[0029] This example provides a treatment method for organic waste acid in the synthesis of acetaminobenzenesulfonyl chloride, which is basically the same as that in Example 1, except that in step (a), the parameters in the macroporous resin bed are controlled as The temperature is 60°C, the normal pressure and the hydraulic retention time are 5 minutes; the yield of the final synthesis of acetaminobenzenesulfonyl chloride reaches 96.1%.

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Abstract

The invention discloses a method for treating organic waste acids in p-acetamidobenzene sulfonyl chloride synthesis, and the method comprises the following steps: (a) pumping the organic waste sulfuric acids into a macroporous resin bed, and carrying out organic matter adsorption interception to obtain a sulfuric acid solution; (b) mixing the sulfuric acid solution with an oxidant, introducing themixture into an oxidation reactor, carrying out oxygenolysis, and decolorizing to obtain purified sulfuric acid, wherein the oxidant is hydrogen peroxide or ozone, and the mass ratio of the oxidant to the sulfuric acid solution is (0.02-0.15): 1; (c) carrying out backwashing desorption on organic matters adsorbed by the resin in the macroporous resin bed by using a backwashing solvent to obtain an eluent; and (d) introducing the eluent into an evaporator to evaporate and recover the solvent, treating the obtained product by a dryer, and recycling. The obtained product is directly used for sulfonation reaction and is used for sale or downstream sections.

Description

technical field [0001] The invention belongs to the technical field of acetaminobenzenesulfonyl chloride synthesis, and in particular relates to a method for treating organic waste acid in the synthesis of acetaminobenzenesulfonyl chloride. Background technique [0002] At present, the synthesis of acetaminobenzenesulfonyl chloride mainly adopts chlorosulfonic acid as the sulfonating reagent to carry out chlorosulfonation reaction with acetanilide, and then removes excess chlorosulfonic acid through hydrolysis, thereby obtaining dilute sulfuric acid solution of acetaminobenzenesulfonyl chloride , separated by filtration to obtain p-acetamidobenzenesulfonyl chloride and organic waste sulfuric acid. [0003] But product paracetamol sulfonyl chloride, part unreacted acetanilide raw material and reaction intermediate paracetamol sulfonic acid can be dissolved in the dilute sulfuric acid, thereby cause the yield of paracetamol sulfonyl chloride to be low; And produce A large amo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/90C07C309/88C07C303/02
CPCC01B17/905C07C303/02C07C309/88
Inventor 刘永超钱炜雯韩菊泉吴景渊
Owner 湖南吴赣药业有限公司
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