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A kind of technology of removing hydrazine hydrochloride in tert-butylhydrazine hydrochloride

A technology of tert-butyl hydrazine and hydrochloride, applied in the field of pesticide intermediates and pesticides, can solve the problems of high solubility of tert-butyl hydrazine hydrochloride, low yield, and insignificant changes in solubility with temperature.

Inactive Publication Date: 2021-01-29
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of technology of removing hydrazine hydrochloride in tert-butylhydrazine hydrochloride
  • A kind of technology of removing hydrazine hydrochloride in tert-butylhydrazine hydrochloride

Examples

Experimental program
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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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Patent Type & Authority Patents(China)
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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