Synthetic method for isopropyl hydrazine

A technology of isopropyl hydrazine and a synthesis method, applied in the synthesis field of isopropyl hydrazine, can solve the problems of high production cost, long process route, complicated process, etc., and achieves low reaction risk, less waste discharge and production cost. low effect

Inactive Publication Date: 2018-05-04
重庆锦杉科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis method has a long process route, high risk of hydrogenation process, high process conditions, complex process, yield less than 80%, and high production cost; in addition, because the by-product sodium carbonate contains a large amount of organic impurities, recycling and The cost of environmental protection treatment is relatively high, and it is easy to cause environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] With 450g of isopropanol, 260.4g of hydrazine hydrate and ZnO / Al with a content of 96% 2 o 3 Put 38g of the composite catalyst into the reactor, start stirring, close the reactor when the temperature rises to 80°C, continue to heat up to 120°C, and keep it warm for 7 hours. After the reaction, reduce the temperature of the reactor to 80°C, and then put The upper organic phase was transferred to a rectification kettle for rectification, and fractions with a temperature of 106-108°C were collected to obtain 344.2 g of isopropylhydrazine.

Embodiment 2

[0013] With 525g of isopropanol, 255.1g of hydrazine hydrate and ZnO / Al with a content of 98% 2 o 3 Put 25g of the composite catalyst into the reactor, start stirring, close the reactor when the temperature rises to 80°C, continue to heat up to 110°C, keep the temperature for 6 hours, after the reaction, lower the temperature of the reactor to 80°C, and then put the The upper organic phase was transferred to a rectification kettle for rectification, and fractions with a temperature of 106-108°C were collected to obtain 339.8 g of isopropylhydrazine.

Embodiment 3

[0015] With isopropanol 600g, content is the hydrazine hydrate 252.5g of 99% and ZnO / Al 2 o 3 Put 50g of the composite catalyst into the reactor, start stirring, close the reactor when the temperature rises to 80°C, continue to heat up to 130°C, keep the temperature for 8 hours, after the reaction, reduce the temperature of the reactor to 80°C, and then put the The upper organic phase was transferred to a rectification kettle for rectification, and fractions with a temperature of 106-108°C were collected to obtain 352.1 g of isopropylhydrazine.

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PUM

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Abstract

The invention provides a synthetic method for isopropyl hydrazine. The method comprises the step: under the protection of inert gases, carrying out an alkylation reaction on isopropanol and hydrazinehydrate under the effect of a catalyst at a certain temperature, to generate the isopropyl hydrazine. After the reaction ends, an organic phase of isopropyl hydrazine is separated with a water phase,and then the organic phase is rectified to obtain an isopropyl hydrazine finished product, and the catalyst used for the reaction is a ZnO / Al3O3 compound catalyst. Compared with the prior art, the isopropyl hydrazine is synthesized in a one-step method by taking isopropanol and hydrazine hydrate as raw materials, and the method is few in reaction steps, simple in post-treatment, little in reactiondangerousness, high in yield, low in production cost and little in waste emission and is an environment-friendly production technology.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of isopropylhydrazine. Background technique [0002] Isopropylhydrazine is a widely used pharmaceutical intermediate and organic synthesis intermediate with excellent biological and chemical activity. Isopropylhydrazine itself is also a commonly used anti-tuberculosis drug and antidepressant, and it is also the starting material of the highly effective insecticide Mileol. [0003] According to literature reports, isopropylhydrazine can be prepared by reacting isopropane bromide with a large amount of excess hydrazine hydrate, and after treatment, use a large amount of continuous extraction with ether. However, due to the high solubility of the product in hydrazine hydrate, the extraction is difficult, the post-treatment time is long, and the yield is low, it is not suitable for large-scale production. And another kind of method for prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/14C07C241/02
CPCC07C241/02C07C243/14
Inventor 不公告发明人
Owner 重庆锦杉科技有限公司
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