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A kind of purification process of tert-butylhydrazine hydrochloride

A technology of tert-butylhydrazine and hydrochloride, applied in the field of pesticide intermediates and pesticides, can solve the problems of waste of raw materials, low yield, high solubility of tert-butylhydrazine hydrochloride, etc.

Inactive Publication Date: 2021-01-15
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 purification process of tert-butylhydrazine hydrochloride
  • A kind of purification process of tert-butylhydrazine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 100mL three-necked flask equipped with a stirring device, add 10.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride and 20mL of absolute ethanol respectively, stir for 30 minutes, cool to 4°C, and add 2.00g of ferric chloride g. React at 4°C for 2 hours, filter immediately after the reaction, wash the filter cake with a small amount of cold ethanol, and dry to obtain 7.15 g of white powder with a yield of 80.01%. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride is 98.06%.

Embodiment 2

[0020] In a 100mL three-necked flask equipped with a stirring device, add 8.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride and 20mL of 90% (v / v) ethanol respectively, stir for 20 minutes, cool to 0°C, add Ferric chloride 0.80g. React at 0°C for 2 hours, filter immediately after the reaction, wash the filter cake with a small amount of cold ethanol, and dry to obtain 5.91 g of white powder with a yield of 82.67%. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride is 98.67%.

Embodiment 3

[0022] In a 100mL three-neck flask equipped with a stirring device, add 6.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride and 20mL of 80% (v / v) ethanol respectively, stir for 10 minutes, cool to 2°C, add Ferric chloride 1.50g. React at 2°C for 3 hours, filter immediately after the reaction, wash the filter cake with a small amount of cold ethanol, and dry to obtain 4.18 g of white powder with a yield of 77.96%. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride is 98.52%.

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Abstract

The invention belongs to the field of pesticides and pesticide intermediates and discloses a process for purifying tert-butylhydrazine hydrochloride. The process disclosed by the invention comprises the following operating steps: respectively adding ethanol and tert-butylhydrazine hydrochloride into a reaction container filled with a stirring device, stirring for 10-30 minutes, cooling to the temperature of 0-4 DEG C, and adding ferric trichloride; reacting at the temperature of 0-4 DEG C for 1-3 hours, immediately filtering after the reaction is ended, washing the filter cake with a small amount of cold ethanol, and drying, namely obtaining the product. The process disclosed by the invention is simple, and the purity of the tert-butylhydrazine hydrochloride is greatly improved. Moreover,less three wastes are produced in the production process, the environmental protection is facilitated, and the process is suitable for industrial 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): C07C243/14C07C241/02
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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