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Method used for removing hydrazine hydrochloride in tert-butylhydrazine hydrochloride

A technology of tert-butylhydrazine and hydrochloride, which is applied in the field of pesticide intermediates and pesticides, can solve the problems of increasing the difficulty of purification of downstream products, high solubility of tert-butylhydrazine hydrochloride, and low yield

Inactive Publication Date: 2019-01-11
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The presence of hydrazine hydrochloride leads to waste of raw materials in the production of downstream products; introduces new impurities in downstream products; increases the difficulty of purification of downstream products
[0004] Due to the high solubility of tert-butylhydrazine hydrochloride in water, and the solubility does not change significantly with temperature, the conventional recrystallization method is used for purification, and the yield is low

Method used

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  • Method used for removing hydrazine hydrochloride in tert-butylhydrazine hydrochloride
  • Method used for removing hydrazine hydrochloride in tert-butylhydrazine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 100mL flask equipped with a stirring device and a reflux device, add 20mL of absolute ethanol, 6.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride, stir in a water bath at 60°C to dissolve, cool to room temperature, and add bicarbonate Ammonium 0.90g, reacted at room temperature for 2 hours, filtered after the reaction, and washed the filter cake with a small amount of ethanol. The filtrate was recovered and applied once, and the operation method was the same as above. The filter cake was dried to obtain a total of 10.48 g of white powder. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride was 91.86%, and the yield was 89.78%.

Embodiment 2

[0022] In a 100mL flask equipped with a stirring device and a reflux device, add 20mL of 98% (v / v) ethanol, 8.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride, stir in a water bath at 70°C to dissolve, and cool to At room temperature, add 1.60 g of ammonium bicarbonate, react at room temperature for 1 hour, filter after the reaction, and wash the filter cake with a small amount of ethanol. The filtrate was recovered and applied mechanically twice, and the operation method was the same as above. The filter cake was dried to obtain a total of 19.80 g of white powder. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride was 90.72%, and the yield was 92.32%.

Embodiment 3

[0024] In a 100mL flask equipped with a stirring device and a reflux device, add 20mL of 95% (v / v) ethanol, 10.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride, stir in a water bath at 80°C to dissolve, and cool to At room temperature, add 2.00 g of ammonium bicarbonate, react at room temperature for 1 hour, filter after the reaction, and wash the filter cake with a small amount of ethanol. The filtrate was recovered and applied mechanically 3 times, and the operation method was the same as above. The filter cake was dried to obtain a total of 33.56 g of white powder. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride was 89.14%, and the yield was 93.89%.

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Abstract

The invention belongs to the field of pesticide intermediate, and discloses a method used for removing hydrazine hydrochloride in tert-butylhydrazine hydrochloride. The method comprises following steps: ethanol, and tert-butylhydrazine hydrochloride are introduced into a reaction container provided with a stirring device and a backflow device, 60 to 80 DEG C water bath stirring is carried out fordissolving, an obtained product is cooled to room temperature, ammonium bicarbonate is added, reaction is carried out for 1 to 3 at room temperature, after reaction, filtering is carried out, an obtained filter cake is washed with a small amount of ethanol and is dried, and an obtained filtrate is recycled for 1 to 3 times. The method is simple in operation, is capable of removing all hydrazine hydrochloride in tert-butylhydrazine hydrochloride; generation of waste gas, waste water, and solid waste in production process is little, it is beneficial for environment protection, and is suitable for industrialized production.

Description

technical field [0001] The invention belongs to the field of pesticides and pesticide intermediates. Background technique [0002] Tert-Butylhydrazine Hydrochloride (Tert-Butylhydrazine Hydrochloride), also known as Tert-Butylhydrazine Hydrochloride, is an important pesticide intermediate. It is an important raw material for the synthesis of insecticides such as hydrazine, tebufenozide, chlorfenozide, methoxyfenozide, cyclofenozide and pyridaben. [0003] At present, the purity of tert-butylhydrazine hydrochloride obtained in industrial production is about 90%. The main impurity is hydrazine hydrochloride. The existence of hydrazine hydrochloride causes waste of raw materials in the production of downstream products; introduces new impurities in downstream products; increases the difficulty of purification of downstream products. [0004] Since the solubility of tert-butylhydrazine hydrochloride in water is relatively large, and the solubility does not change significantl...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/14
CPCC07C241/02C07C243/14
Inventor 刘立业赵文卓史晋宜丁元生
Owner JILIN INST OF CHEM TECH
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