Preparation method of isopropyl hydrazine

A technology of isopropyl hydrazine and isopropyl alcohol, applied in the field of preparation of isopropyl hydrazine, can solve the problems of high cost of raw materials, environmental pollution, long process route, etc., and achieves less waste discharge, less reaction risk, production low cost effect

Inactive Publication Date: 2018-07-17
重庆晶萃化工科技有限公司
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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, complicated process, high cost of raw materials, and a yield of less than 80%. 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] Put 360g of isopropanol, 260.4g of hydrazine hydrate with a concentration of 96% and 25g of D001 macroporous resin into the reactor, start stirring, heat up to 80°C, close the reactor, continue to heat up to 115°C, and keep it warm for 8 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 344.8 g of isopropylhydrazine.

Embodiment 2

[0013] Put 480g of isopropanol, 255.1g of hydrazine hydrate with a concentration of 98% and 38g of D001 macroporous resin into the reaction kettle, start stirring, close the reaction kettle when the temperature rises to 80°C, continue to heat up to 110°C, and keep it 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 a rectification kettle for rectification, and the temperature was collected at 106-108°C to obtain 340.2 g of isopropylhydrazine.

Embodiment 3

[0015] Put 600g of isopropanol, 252.5g of hydrazine hydrate with a concentration of 99% and 50g of D001 macroporous resin into the reactor, start stirring, close the reactor when the temperature is raised to 80°C, continue to heat up to 120°C, and keep it warm for 7 hours After the reaction, the temperature of the reactor was reduced 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 to 108° C. to obtain 350.5 g of isopropylhydrazine.

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PUM

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Abstract

The invention provides a preparation method of isopropyl hydrazine. The method comprises the steps that under the protection of inert gas and under the action of a catalyst, alkylation reaction is conducted on isopropanol and hydrazine hydrate at a certain temperature to generate isopropyl hydrazine; an organic phase containing isopropyl hydrazine is separated from an aqueous phase after the reaction is finished; then the organic phase is rectified to obtain an isopropyl hydrazine finished product, wherein the catalyst used for the reaction is D001 macroporous strong acid cation exchange resin. Compared with the prior art, isopropanol and hydrazine hydrate serve as raw materials, isopropyl hydrazine is prepared through a one-step method, the number of process steps is small, post-treatmentis simple, the reaction risk is low, the yield is high, the production cost is low, little waste is discharged, and the method 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 preparation 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 pr...

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 重庆晶萃化工科技有限公司
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