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Method for synthesizing tert-butylhydrazine

A technology for tert-butyl hydrazine and hydrazine hydrate, which is applied in the field of synthesizing tert-butyl hydrazine, can solve the problems of high equipment requirements, many process steps and high production costs, and achieves low equipment requirements, simple process steps and less waste discharge. Effect

Inactive Publication Date: 2018-05-18
重庆晶萃化工科技有限公司
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  • 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

[0012] Put 555g of tert-butanol, 260.4g of hydrazine hydrate with a content of 96% and 25g of D72 macroporous resin into the reaction kettle, start stirring, close the reaction kettle, raise the temperature in the kettle to 110°C, keep the temperature for 6 hours, and the reaction is over Afterwards, the reaction liquid was transferred to a rectification kettle, heated and distilled, and fractions at 102-104°C were collected to obtain 401.3 g of tert-butylhydrazine.

Embodiment 2

[0014] Put 648g of tert-butanol, 255.1g of hydrazine hydrate with a content of 98% and 50g of D72 macroporous resin into the reaction kettle, start stirring, close the reaction kettle, raise the temperature in the kettle to 115°C, keep the temperature for 7 hours, and the reaction is over Afterwards, the reaction solution was transferred to a rectification kettle, heated and distilled, and the fraction at 102-104°C was collected to obtain 408.8 g of tert-butylhydrazine.

Embodiment 3

[0016] Put 740g of tert-butanol, 252.5g of hydrazine hydrate with a content of 99% and 75g of D72 macroporous resin into the reaction kettle, start stirring, seal the reaction kettle, raise the temperature in the kettle to 120°C, keep it warm for 8 hours, and the reaction is over Afterwards, the reaction solution was transferred to a rectification kettle, heated and distilled, and fractions at 102-104°C were collected to obtain 419.5 g of tert-butylhydrazine.

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Abstract

The invention provides a method for synthesizing tert-butylhydrazine. According to the method, an alkylation reaction is carried out on tertiary butanol and hydrazine hydrate under the effect of a catalyst at a certain temperature under the protection of inert gases to generate tert-butylhydrazine, a reaction solution is refined after the reaction is finished so as to obtain a tert-butylhydrazinefinished product, and the catalyst used for the reaction is D72 porous strong acidity cation exchange resin. Compared with the prior art, the tert-butylhydrazine is synthesized from tertiary butanol and hydrazine hydrate as raw materials in a one-step method, and the method is simple in processing steps, not high in equipment requirement, low in equipment investment, high in production yield, lowin production cost and little in waste emission and is a green and environmentally-friendly production technology.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing 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 a...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/14
CPCC07C241/02C07C243/14
Inventor 不公告发明人
Owner 重庆晶萃化工科技有限公司
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