Synthetic method for tert-butylhydrazine

A technology of tert-butyl hydrazine and a synthesis method, which is applied in directions such as hydrazine preparation, can solve the problems of high equipment requirements, many process steps, and high production costs, and achieves the effects of low equipment requirements, simple process steps, and less waste discharge.

Inactive Publication Date: 2018-06-22
重庆丽澄环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming that prior art synthetic tert-butylhydrazine exists is as follows: 1, the used hydrochloric acid of synthetic method has strong corrosiveness, higher to equipment requirement, and equipment investment is bigger; 2, alkaline hydrolysis process can produce a large amount of saline organic waste water, this Due to the high salt content of wastewater, environmental protection treatment is difficult and expensive, and it is easy to cause environmental pollution; 3. There are many process steps and low yield (the total yield is about 80% based on hydrazine hydrate), and the production cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] 260.4 g of hydrazine hydrate and ZnO / Al with 555 g of tert-butanol and a content of 96% 2 o 3 Put 50g of the composite catalyst into the reaction kettle, start stirring, seal the reaction kettle, raise the temperature in the kettle to 100°C, and keep it warm for 4 hours. After the reaction, transfer the reaction solution into the rectification kettle, heat and distill, and collect The fraction at °C yielded 401.5 g of tert-butylhydrazine.

Embodiment 2

[0013] With 648g of tert-butanol, 255.1g of hydrazine hydrate and ZnO / Al with a content of 98% 2 o 3 Put 63g of composite catalyst into the reaction kettle, start stirring, seal the reaction kettle, raise the temperature inside the kettle to 110°C, keep it warm for 5 hours, transfer the reaction liquid into the rectification kettle after the reaction, heat and distill, and collect The fraction at °C yielded 409.9 g of tert-butylhydrazine.

Embodiment 3

[0015] 740g of tert-butanol, 252.5g of hydrazine hydrate and ZnO / Al with a content of 99% 2 o 3 Put 75g of the composite catalyst into the reaction kettle, start stirring, seal the reaction kettle, raise the temperature inside the kettle to 120°C, keep it warm for 6 hours, transfer the reaction solution into the rectification kettle after the reaction, heat and distill, and collect The fraction at °C yielded 420.7 g of tert-butylhydrazine.

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PUM

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Abstract

The invention provides a synthetic method for tert-butylhydrazine. The method comprises the following steps: subjecting tert-butyl alcohol and hydrazine hydrate to an alkylation reaction under the protection of inert gas and the action of a catalyst at a certain temperature so as to generate the tert-butylhydrazine, and after completion of the reaction, rectifying a reaction solution so as to obtain a finished tert-butylhydrazine product, wherein the catalyst used in the reaction is a ZnO/Al2O3 composite catalyst. Compared with the prior art, the synthetic method synthesizes the tert-butylhydrazine with the tert-butyl alcohol and the hydrazine hydrate as raw materials through a one-step process, has the advantages of simple process steps, low requirements on equipment, small equipment investment, high reaction yield, low production cost and less waste discharge, and is a green and environment-friendly production process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of tert-butylhydrazine. Background technique [0002] Tert-butylhydrazine, also known as tert-butylhydrazine, is an important intermediate in organic synthesis, which can be used to synthesize benzoylhydrazine insecticides, and bishydrazide insecticides, tebufenozide and chlorantraniliprole. Hydrazine, methoxyfenozide and cyclofenozide, and the acaricide pyridaben, etc. [0003] At present, the method for synthesizing tert-butylhydrazine in the prior art mainly uses tert-butyl alcohol, hydrazine hydrate and hydrochloric acid as raw materials to prepare tert-butylhydrazine hydrochloride earlier, then carry out alkaline hydrolysis, and tert-butylhydrazine hydrochloride and hydrogen Sodium oxide reacts to obtain tert-butylhydrazine aqueous solution, and then obtains tert-butylhydrazine through distillation. The shortcoming that prior art s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/02C07C243/14
CPCC07C241/02C07C243/14
Inventor 不公告发明人
Owner 重庆丽澄环保科技有限公司
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