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Method for synthesizing isopropyl hydrazine

A technology of isopropyl hydrazine and hydrazine hydrate, applied in the field of synthesizing isopropyl hydrazine, can solve the problems of high production cost, environmental pollution, long process route and the like, and achieves less waste discharge, less reaction risk and low production cost Effect

Inactive Publication Date: 2018-06-22
张晓玲
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  • Claims
  • Application Information

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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
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Effect test

Embodiment 1

[0011] Put 450g of isopropanol, 260.4g of hydrazine hydrate with a content of 96% and 38g of sodium hexametaphosphate into the reaction kettle, start stirring, close the reaction kettle when heating to 80°C, continue to heat up to 120°C, and keep warm for 7 hours After the reaction, the temperature of the reactor was lowered to 80°C, and then the upper organic phase in the reactor was transferred to a rectification kettle for rectification, and the temperature was collected at 106-108°C to obtain 345.7 g of isopropylhydrazine.

Embodiment 2

[0013] Put 525g of isopropanol, 255.1g of hydrazine hydrate with a content of 98% and 25g of sodium hexametaphosphate into the reaction kettle, start stirring, close the reaction kettle when heating to 80°C, continue to heat up to 110°C, and keep warm for 6 hours After the reaction, the temperature of the reactor was lowered to 80°C, and then the upper organic phase in the reactor was transferred to the rectification kettle for rectification, and the temperature was collected at 106-108°C to obtain 339.3 g of isopropylhydrazine.

Embodiment 3

[0015] Put 600g of isopropanol, 252.5g of hydrazine hydrate with a content of 99% and 50g of sodium hexametaphosphate into the reaction kettle, start stirring, close the reaction kettle when heating to 80°C, continue to heat up to 130°C, and keep warm for 5 hours After the reaction, the temperature of the reactor was lowered to 80°C, and then the upper organic phase in the reactor was transferred to the rectification kettle for rectification, and the temperature was collected at 106-108°C to obtain 351.5 g of isopropylhydrazine.

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Abstract

The invention provides a method for synthesizing isopropyl hydrazine. According to the method for synthesizing isopropyl hydrazine, an alkylation reaction is performed on isopropanol and hydrazine hydrate under protection of inert gas under the action of a catalyst at a certain temperature so as to generate isopropyl hydrazine, an organic phase which contains isopropyl hydrazine is separated froman aqueous phase after the reaction is completed, and then the organic phase is rectified so as to obtain the finished product isopropyl hydrazine, wherein the adopted reaction catalyst is sodium hexametaphosphate. Compared with the prior art, the method adopts isopropanol and hydrazine hydrate as raw materials to synthesize isopropyl hydrazine in one step, the method has few reaction steps, simple post-treatment, small reaction risks, high yield, low production cost and little waste emission, and the method 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 method for synthesizing 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 ...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/14
CPCC07C241/02C07C243/14
Inventor 张晓玲
Owner 张晓玲
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