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Method for separating and purifying byproduct isopropyl hydrazine produced in preparation of hydrazine hydrate from ketazine

A technology of ketazine hydrazine hydrate and isopropylhydrazine, which is applied in the field of separation and purification of by-products of ketazine hydrazine hydrate, can solve the problems of cumbersome operation process, many steps in the preparation method, and high parameter requirements, so as to improve economic benefits, effect of problem solving

Pending Publication Date: 2019-12-31
YIBIN HAIFENG HERUI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common isopropylhydrazine preparation method has: (1) bromoisopropane reacts with a large amount of excess hydrazine hydrate, then continuously extracts with a large amount of ether, and then separates to obtain isopropylhydrazine; (2) ethyl carbazate and Acetone reaction, and then obtained by hydrogenation and ester removal of the protective group; (3) the synthesis method of isopropylhydrazine mentioned in patent CN105017064 A, first hydrazine hydrate and hydrochloric acid generate hydrazine hydrochloride, and hydrazine hydrochloride reacts with isopropanol Generate isopropylhydrazine hydrochloride, then use excessive hydrazine hydrate to free to obtain isopropylhydrazine and hydrazine hydrochloride, separate to obtain isopropylhydrazine, and hydrazine hydrochloride returns to the previous step; the preparation method of isopropylhydrazine has many steps and is easy to operate. The process is cumbersome and requires high parameters

Method used

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  • Method for separating and purifying byproduct isopropyl hydrazine produced in preparation of hydrazine hydrate from ketazine

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Add 500 kg of a solution containing 10.30% isopropylhydrazine into the distillation still, heat to carry out distillation, control the temperature of the still still at 100-105°C, control the distillation temperature at 95-98°C, and the concentration of isopropylhydrazine after distillation is 78.25% , standing for stratification, standing for 0.5h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 300kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 49.95kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 95.52%, and the calculated yield was 92.64%.

Embodiment 2

[0031]Add 500 kg of a solution containing 10.05% isopropylhydrazine into the still, heat to carry out distillation, control the temperature of the still still at 100-108°C, control the distillation temperature at 95-100°C, and the concentration of isopropylhydrazine after distillation is 80.5% , standing for stratification, standing for 1h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 350kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 46.96kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 98.84%, and the calculated yield was 94.55%.

Embodiment 3

[0033] Add 500 kg of a solution containing 11.3% isopropylhydrazine into the distillation still, heat to carry out distillation, control the temperature of the still still at 101-108°C, control the distillation temperature at 95-100°C, and the concentration of isopropylhydrazine after distillation is 81.62% , standing for stratification, standing for 0.5h, there is an obvious phase interface, the stratification is over, add the oil phase to the extraction kettle, add 300kg ether for extraction three times each time, combine the extracts into the distillation kettle, distill out the ether, and collect at 750mmHg 53.0kg of isopropylhydrazine was obtained from the fraction at 106-108°C, the content of which was analyzed to be 98.50%, and the calculated yield was 92.39%.

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Abstract

The invention discloses a method for separating and purifying the byproduct isopropyl hydrazine produced in the preparation of hydrazine hydrate from ketazine. The method comprises the following steps: distilling the byproduct, namely isopropyl hydrazine waste liquid separated in the production process of hydrazine hydrate via a ketazine method, controlling the temperature of a distillation kettleto be 100-108 DEG C and a distillation temperature to be 95-100 DEG C, and distilling off low-boiling-point substances to obtain a concentrated isopropyl hydrazine solution at the bottom of the kettle; subjecting the kettle-bottom isopropyl hydrazine solution obtained after distillation to standing and layering, removing a water phase, then extracting an oil phase containing isopropyl hydrazine,distilling an extract, controlling a distillation temperature to be 106-108 DEG C after an extracting agent is distilled out, and collecting a fraction to obtain isopropyl hydrazine. According to themethod, the byproduct isopropyl hydrazine waste liquid containing isopropyl produced in the preparation of hydrazine hydrate from ketazine is separated and purified through the four steps consisting of distillation, standing and layering, extraction and distillation, so the low-value isopropyl hydrazine organic waste liquid is converted into high-quality medical raw materials and intermediates, and thus, problems in treatment of the organic waste liquid produced in the preparation of hydrazine hydrate from ketazine are solved.

Description

technical field [0001] The invention relates to a method for separating and purifying a by-product of ketazine hydrazine hydrate, in particular to a method for separating and purifying isopropylhydrazine, a by-product of ketazine hydrazine hydrate. Background technique [0002] Hydrazine hydrate, also known as: hydrazine hydrate, chemical formula is N 2 h 4 ·H 2 O, a strong reducing agent, is an important chemical raw material, and is also a raw material for medicine, pesticides, dyes, foaming agents, developers, and antioxidants; it is used for deoxidizing boiler water, producing high-purity metals, and synthesizing and reducing organic compounds. , separation of rare elements, and also used in the manufacture of rocket fuel and explosives. With the advancement of technology and the development of society, the application fields of hydrazine hydrate are constantly expanding in recent years. The production methods of hydrazine hydrate mainly include Raschig method, urea m...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/14
CPCC07C241/02
Inventor 陈尚思周明柴进祥舒帮会罗浩
Owner YIBIN HAIFENG HERUI
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