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Method for preparing magnesium sulfate from byproduct sulfuric acid of benzene sulfone chloride

A technology of benzenesulfonyl chloride and magnesium sulfate, applied in the preparation of sulfonic acid, magnesium sulfate, chemical instruments and methods, etc., can solve problems such as trouble, waste, instability, etc., and achieve the effect of accelerating the replacement reaction

Pending Publication Date: 2020-11-24
江苏康祥实业集团有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Benzenesulfonyl chloride, benzenesulfonylchloride, molecular formula C6H5ClO2S, molecular weight 176.62, colorless transparent oily liquid, mainly used in organic synthesis, preparation of sulfonamides and identification of various amines, unstable, exposed to the air, will absorb a lot in the air Water in the air, and gradually hydrolyzes, and pH value is reduced, and the hydrogen chloride that volatilizes can form white smog, has very strong irritant, and benzenesulfonyl chloride can generate by-product sulfuric acid in the process of preparation, but in existing technology It will be very troublesome to separate sulfuric acid, and the generated sulfuric acid cannot be used, which is very wasteful

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment one: a kind of method that benzenesulfonyl chloride by-product sulfuric acid prepares magnesium sulfate, comprises the steps:

[0021] (1) Sulfonation reaction: take chlorosulfonic acid and pure benzene as raw materials, the mol ratio of chlorosulfonic acid and pure benzene is 3:1, first chlorosulfonic acid is added in the reactor, then the reactor is heated, heated The temperature is 20°C, and the reaction kettle is started. After the start-up, under the stirring state with a stirring rate of 100r / min, pure benzene is added dropwise through a constant pressure dropping funnel, and the dropping rate is 1ml / min. After the dropping is completed, let it react for 2h The hydrogen chloride gas produced last, then the hydrogen chloride gas is made mass concentration through condensation, secondary falling film absorption and is 38% hydrochloric acid solution, after obtaining the solution, add the sulfonation auxiliary agent of 10g in the inside of the solution, the ...

Embodiment 2

[0025] Embodiment two: a kind of method that benzenesulfonyl chloride by-product sulfuric acid prepares magnesium sulfate, comprises the steps:

[0026] (1) Sulfonation reaction: take chlorosulfonic acid and pure benzene as raw materials, the mol ratio of chlorosulfonic acid and pure benzene is 3:1, first chlorosulfonic acid is added in the reactor, then the reactor is heated, heated The temperature is 30°C, and the reaction kettle is started. After the start-up, under the stirring state with a stirring rate of 150r / min, pure benzene is added dropwise using a constant pressure dropping funnel, and the dropping rate is 1.5ml / min. After the dropping is completed, make it react The hydrogen chloride gas produced after 3h, then the hydrogen chloride gas is condensed and absorbed by the secondary falling film to make a mass concentration of 45% hydrochloric acid solution, and after obtaining the solution, add 15g of sulfonation additive in the solution, the sulfonation additive Amm...

Embodiment 3

[0030] Embodiment three: a kind of method that benzenesulfonyl chloride by-product sulfuric acid prepares magnesium sulfate, comprises the steps:

[0031] (1) Sulfonation reaction: take chlorosulfonic acid and pure benzene as raw materials, the mol ratio of chlorosulfonic acid and pure benzene is 3:1, first chlorosulfonic acid is added in the reactor, then the reactor is heated, heated The temperature is 20°C, and the reaction kettle is started. After the start-up, under the stirring state with a stirring rate of 150r / min, pure benzene is added dropwise using a constant pressure dropping funnel, and the dropping rate is 1ml / min. After the dropping is completed, let it react for 2h The hydrogen chloride gas produced last, then the hydrogen chloride gas is made mass concentration through condensation, secondary falling film absorption and is 44% hydrochloric acid solution, after obtaining the solution, add the sulfonation auxiliary agent of 15g in the inside of the solution, the ...

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PUM

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Abstract

The invention discloses a method for preparing magnesium sulfate from byproduct sulfuric acid of benzene sulfone chloride. The method comprises the following steps: (1) sulfonation reaction: chlorosulfonic acid and pure benzene are taken as raw materials; firstly, the chlorosulfonic acid is added into a reaction kettle; then, the reaction kettle is heated, and the reaction kettle is started; afterstarting, under the stirring state that the stirring rate is 100-150r / min, the pure benzene is dropwise added by employing a constant-pressure dropping funnel; and after being dropwise added, the pure benzene and the chlorosulfonic acid react for 2-3h to produce hydrogen chloride gas; then the produced hydrogen chloride gas is condensed and is absorbed by a secondary falling film to prepare a hydrochloric acid solution with mass concentration of 38%-45%; after the solution is obtained, 10-15g of sulfonation additive is added into the solution; then the reaction kettle is restarted for reaction; and after the reaction ends, cooling, hydrolyzing, crystallization, suction filtration, water washing and drying are performed to obtain the benzene sulfone chloride and by-products thereof; the sulfuric acid can be separated very conveniently, and the magnesium sulfate can be quickly prepared by using the sulfuric acid.

Description

technical field [0001] The invention relates to the technical field of magnesium sulfate production, in particular to a method for preparing magnesium sulfate by-product sulfuric acid from benzenesulfonyl chloride. Background technique [0002] Benzenesulfonyl chloride, benzenesulfonylchloride, molecular formula C6H5ClO2S, molecular weight 176.62, colorless transparent oily liquid, mainly used in organic synthesis, preparation of sulfonamides and identification of various amines, unstable, exposed to the air, will absorb a lot in the air Water in the air, and gradually hydrolyzes, and pH value is reduced, and the hydrogen chloride that volatilizes can form white smog, has very strong irritant, and benzenesulfonyl chloride can generate by-product sulfuric acid in the process of preparation, but in existing technology It will be very troublesome to separate sulfuric acid, and the generated sulfuric acid cannot be used, which is very wasteful. Contents of the invention [00...

Claims

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Application Information

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IPC IPC(8): C01F5/40C01B17/74C07C303/02
CPCC01F5/40C01B17/74C07C303/02C07C309/86
Inventor 朱雪松张福祥刘仕通马龙于海洋
Owner 江苏康祥实业集团有限公司