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Preparation method of aromatic hydrocarbon sulfonyl chloride derivative

A technology of aromatic hydrocarbon sulfonyl chloride derivatives and aromatic hydrocarbons, which is applied in the field of preparation of aromatic hydrocarbon sulfonyl chloride derivatives, can solve the problems of inability to directly recycle, excessive demand for chlorosulfonic acid, and high energy consumption, so as to improve utilization value and reduce energy consumption , the effect of high yield

Active Publication Date: 2013-09-18
TAIZHOU QIANJIN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The disadvantages of this method: the one is that hydrogen chloride gas is generated in the reaction process, and it is easy to generate sulfone by-products, and the chlorosulfonic acid needs to be excessive; Contains hydrochloric acid and sulfuric acid at the same time, cannot be recycled directly

Method used

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  • Preparation method of aromatic hydrocarbon sulfonyl chloride derivative
  • Preparation method of aromatic hydrocarbon sulfonyl chloride derivative
  • Preparation method of aromatic hydrocarbon sulfonyl chloride derivative

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Add 466g (4mol) of chlorosulfonic acid in a 1000ml flask, feed 40g (0.5mol) of sulfur trioxide gas to make a chlorosulfonic acid solution of sulfur trioxide, then slowly add 123g (1mol) of nitrobenzene , be warming up to 120°C and keep warm until the reaction ends, then cool to 25°C, control the temperature below 40°C, slowly add 448g of 40% by weight dilute sulfuric acid dropwise in the above-mentioned reaction solution, the hydrogen chloride gas generated passes into water, passes through water Can be used as by-product hydrochloric acid recovery after absorbing, finally add the dichloromethane of 12 times of nitrobenzene weight, leave standstill layering after stirring for 1 hour, lower layer is 70% by weight sulfuric acid (hydrochloric acid content is lower than 0.45% by weight), can be used as by-product The product was recovered, and the upper layer was distilled to remove the solvent to obtain 218g of m-nitrobenzenesulfonyl chloride, the content was 99.57%, and th...

Embodiment 2

[0038] Add 291.3g (2.5mol) of chlorosulfonic acid in a 1000ml flask, feed 120g (1.5mol) of sulfur trioxide gas to make a chlorosulfonic acid solution of sulfur trioxide, then slowly add 123g (1mol) of nitric acid Base benzene, heat up to 130°C and keep warm until the reaction is over, then cool to 25°C, control the temperature below 40°C, slowly add 438g of 60% dilute sulfuric acid dropwise to the above reaction solution, the hydrogen chloride gas generated is passed into water, After the water is absorbed, it can be recovered as by-product hydrochloric acid. Finally, ethylene dichloride with 8 times the weight of nitrobenzene is added, and after stirring for 1 hour, it is allowed to stand for stratification. The lower floor is 80% by weight sulfuric acid (hydrochloric acid content is lower than 0.18% by weight), Recovered as a by-product, the upper layer was distilled to remove the solvent to obtain 217g of m-nitrobenzenesulfonyl chloride, the content was 99.05%, and the yield...

Embodiment 3

[0040] Add 349.5g (3mol) of chlorosulfonic acid in a 1000ml flask, feed 80g (1mol) of sulfur trioxide gas to make a chlorosulfonic acid solution of sulfur trioxide, then slowly add 123g (1mol) of nitrobenzene , be warming up to 130°C and keep warm until the reaction ends, then cool to 25°C, control the temperature below 40°C, slowly add 402g of 50% by weight dilute sulfuric acid dropwise in the above-mentioned reaction solution, the hydrogen chloride gas generated is passed into water, passed through water Can be used as by-product hydrochloric acid recovery after absorbing, finally add the carbon tetrachloride of 10 times of nitrobenzene weight, leave standstill layering after stirring for 1 hour, lower layer is 75% by weight sulfuric acid (hydrochloric acid content is lower than 0.40% by weight), can be used as The by-products were recovered, and the upper layer was distilled to remove the solvent to obtain 217g of m-nitrobenzenesulfonyl chloride, the content was 99.00%, and ...

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Abstract

The invention discloses a preparation method of an aromatic hydrocarbon sulfonyl chloride derivative. The preparation method comprises the following steps of: (1) introducing sulfur trioxide gas into chlorosulfonic acid to prepare a chlorosulfonic acid solution of the sulfur trioxide, slowly adding an aromatic hydrocarbon, heating to 50-140 DEG C, performing heat preservation till the end of reaction, and then cooling to 25-35 DEG C; (2) controlling the temperature to be lower than 40 DEG C, and slowly dripping dilute sulfuric acid into the reaction solution, wherein generated hydrogen chloride gas can be recovered as a byproduct, namely hydrochloric acid after being absorbed by water; and (3) adding a solvent, stirring for 0.5-1h, and then standing for lamination, wherein the lower layer is sulfuric acid and can be recovered as a byproduct, and the upper layer can obtain a product, namely the aromatic hydrocarbon sulfonyl chloride derivative after removal of the solvent by distillation. The preparation method disclosed by the invention has the advantages of steady reaction, high yield, no generation of the hydrogen chloride gas during the reaction process, low energy consumption during the post-treatment process and high utilization value of the recovered sulfuric acid.

Description

technical field [0001] The invention belongs to the technical field of manufacturing dye chemical intermediates, and relates to a preparation method of aromatic hydrocarbon sulfonyl chloride derivatives. Background technique [0002] The common preparation method of aromatic hydrocarbon sulfonyl chloride derivatives is to carry out chlorosulfonation of aromatic hydrocarbons with excess chlorosulfonic acid, then dilute the reaction solution with a large amount of ice, and then filter the aromatic hydrocarbon sulfonyl chloride derivatives after precipitation. The reaction formula is as follows: [0003] Main response: [0004] [0005] side effects: [0006] [0007] Post-processing: [0008] Excess ClSO 3 H+H 2 O(ice)→HCl+H 2 SO 4 [0009] The disadvantages of this method: the one is that hydrogen chloride gas is generated in the reaction process, and it is easy to generate sulfone by-products, and the chlorosulfonic acid needs to be excessive; It also contains ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/86C07C309/88C07C303/08C01B17/90C01B7/01
Inventor 王云德余英洲袁慎峰谭英宇
Owner TAIZHOU QIANJIN CHEM CO LTD
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