Synthesis method of tert-butylhydrazine

A technology of tert-butylhydrazine and its synthesis method, which is applied in the preparation of hydrazine, etc., can solve the problems of high production cost, many process steps, and high equipment requirements, and achieve the effects of less waste discharge, simple process steps, and low equipment requirements

Inactive Publication Date: 2018-06-22
李亚杉
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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

[0012] Put 555g of tert-butanol, 260.4g of hydrazine hydrate with a content of 96% and 25g of D002 macroporous resin into the reaction kettle, start stirring, seal the reaction kettle, raise the temperature in the kettle to 100°C, keep the temperature for 4 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 400.6 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 D002 macroporous resin into the reaction kettle, start stirring, seal the reaction kettle, raise the temperature in the kettle to 110°C, keep the temperature for 5 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 409.3 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 D002 macroporous resin into the reaction kettle, start stirring, seal the reaction kettle, raise the temperature in the kettle to 120°C, keep the temperature for 6 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 419.8 g of tert-butylhydrazine.

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PUM

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Abstract

The invention provides a synthesis method of tert-butylhydrazine. The method is characterized in that under the protection of inert gas, tertiary butanol and hydrazine hydrate take alkylation reactionat certain temperature under the effect of catalysts to generate tert-butylhydrazine; after the reaction is finished, reaction liquid is rectified to obtain a finished product of the tert-butylhydrazine; the catalyst used for reaction is D002 macropore strong-acidity cation exchange resin. Compared with the prior art, the synthesis method has the advantages that the tert-butylhydrazine is synthesized by using the tertiary butanol and the hydrazine hydrate as raw materials by a one-step method; the process steps are simple; the requirements on equipment are low; the equipment investment is low; the reaction yield is high; the production cost is low; the discharged wastes are few; the synthesis method belongs to 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 李亚杉
Owner 李亚杉
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