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Method for synthesizing benzenesulfonyl hydrazide

A finished product of benzenesulfonyl hydrazide, the technology of benzenesulfonyl hydrazide, which is applied in the preparation of sulfonic acid amide, organic chemistry, etc., can solve the problems of high production cost, pollution and high treatment cost, and achieves less waste discharge and high reaction yield , The effect of low production cost

Inactive Publication Date: 2017-07-07
重庆丽澄环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The shortcoming that prior art exists is: (1) used benzene to make solvent in the reaction, and benzene is a kind of volatile, the toxic substance that can cause poisonous effect to human body, and a small amount of escaping and volatilization of benzene in use process all can be harmful to Damage and pollution to human health and the environment; (2) A large amount of organic salt-containing wastewater will be produced in the production process, which is difficult to treat, has high treatment costs, and will pollute the environment; (3) The current synthetic The methods all use expensive hydrazine hydrate as raw material, the yield is about 85%, and the production cost is relatively high

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  • Method for synthesizing benzenesulfonyl hydrazide

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Embodiment 1

[0013] 157g of benzenesulfonamide, 185g of butanazine and 200ml of water are placed in a four-necked flask with stirring, a thermometer and a rectifying column, and a conduit is connected to the upper part of the receiver of the rectifying column so as to absorb ammonia; Heating to 90-100°C, when the gas generated by the reaction enters the rectification column, extract methyl ethyl ketone and recover ammonia gas at the column top temperature of 75-80°C; take a sample for analysis after reacting for 8-12 hours, when the reaction liquid When the content of benzenesulfonamide drops to 2%, stop heating and end the reaction. After the flask is cooled to normal temperature, take out the material in the flask, centrifugally filter, wash the filter cake with water and dry at 60-80°C to obtain benzenesulfonamide Hydrazine 161.2g.

Embodiment 2

[0015] 157g of benzenesulfonamide, 224g of butanazine and 250ml of water are placed in a four-necked flask with stirring, a thermometer and a rectifying column, and a conduit is connected to the receiver top of the rectifying column so as to absorb ammonia; Heating to 90-100°C, when the gas generated by the reaction enters the rectification column, extract methyl ethyl ketone and recover ammonia gas at the column top temperature of 75-80°C; take a sample for analysis after reacting for 8-12 hours, when the reaction liquid When the content of benzenesulfonamide drops to 2%, stop heating and end the reaction. After the flask is cooled to normal temperature, take out the material in the flask, centrifugally filter, wash the filter cake with water and dry at 60-80°C to obtain benzenesulfonamide Hydrazine 163.5g.

Embodiment 3

[0017] Benzenesulfonamide 157g, butanazine 260g and water 300ml are placed in the four-neck flask with stirring, thermometer and rectifying column, and a conduit is connected to the receiver top of the rectifying column so as to absorb ammonia; Heating to 90-100°C, when the gas generated by the reaction enters the rectification column, extract methyl ethyl ketone and recover ammonia gas at the column top temperature of 75-80°C; take a sample for analysis after reacting for 8-12 hours, when the reaction liquid When the content of benzenesulfonamide drops to 2%, stop heating and end the reaction. After the flask is cooled to normal temperature, take out the material in the flask, centrifugally filter, wash the filter cake with water and dry at 60-80°C to obtain benzenesulfonamide Hydrazine 165.1g.

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Abstract

The invention discloses a method for synthesizing benzenesulfonyl hydrazide. According to the method, benzene sulfonamide, methyl ethyl ketazine and water serve as raw materials to react at a certain temperature, and the benzenesulfonyl hydrazide is synthesized. In the reaction process, generated ammonia and butanone are recovered, after the reaction is finished, precipitated solid matter is centrifuged and filtered, and a filter cake is subjected to washing and drying to obtain a finished benzenesulfonyl hydrazide product. The method is simple in process, high in reaction yield, simple in product postprocessing and high in purity, and has few impurities; recovered by-products, namely the ammonia and the butanone, can be reused for synthesis of methyl ethyl ketazine, and the production cost is low; benzene is not used as a solvent, so that no organic salt-containing wastewater is generated, few wastes are discharged, and the method is an environment-friendly production technology.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of benzenesulfonyl hydrazide. Background technique [0002] Benzenesulfonylhydrazide, white to light yellow crystalline solid, melting range is 101-103°C, soluble in aqueous solution of inorganic acid and alkali, insoluble in water and organic solvents. Benzenesulfonyl hydrazide is widely used as a blowing agent in the manufacture of foam plastics and foam rubber. [0003] At present, the synthesis method of benzenesulfonyl hydrazide is mainly prepared by reacting benzenesulfonyl chloride and hydrazine hydrate. The process steps are as follows: dissolve benzenesulfonyl chloride in benzene according to the proportion, and send the prepared solution to the overhead tank for standby. Add hydrazine hydrate with a concentration of 40% and an appropriate amount of caustic soda into the stirred reactor, and dissolve it into a uniform solution u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/36C07C311/49
CPCC07C303/36C07C311/49
Inventor 张晓玲
Owner 重庆丽澄环保科技有限公司