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Novel method for converting industrial waste 1,2-dimethylhydrazine into methylhydrazine

A technology of dimethyl hydrazine and industrial waste, applied in the directions of hydrazine preparation, organic chemistry, etc., can solve the problems of waste, environmental pollution and resources, and achieve the effects of low cost, high conversion rate, and avoiding environmental pollution and waste of resources.

Active Publication Date: 2014-11-19
DONGLI NANTONG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention solves the problem that the by-product 1,2-dimethylhydrazine in the industrial waste discharged when synthesizing monomethylhydrazine with hydrochloric acid methanol hydrazine hydrate can be fully utilized, avoiding the environmental pollution caused by such dangerous compounds and the Waste of resources, in order to better realize the problem of turning waste into treasure for industrial waste liquid, an industrial waste containing by-product 1,2-dimethylhydrazine in the production process of monomethylhydrazine was invented by using an oxidant A New Method and Separation Technique for Oxidative Reconversion to Monomethylhydrazine

Method used

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  • Novel method for converting industrial waste 1,2-dimethylhydrazine into methylhydrazine

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Add respectively 265g (22.7%) of waste liquid and 324g (2mol) of ferric trichloride containing 1mol1,2-dimethylhydrazine in the 2L four-necked round-bottomed flask that thermometer, stirrer and reflux condenser are equipped with and Stir continuously for a period of time, add 2mol of 45% phosphoric acid aqueous solution dropwise under ice-salt water cooling, heat to 5-95°C for 1-16 hours after dropping, add solid calcium oxide when the reaction solution is cooled to about 0-10°C with ice-salt water Adjust the pH value to between 5 and 13, filter the generated inorganic salts by means of suction filtration, wash the filter cake with cold water, combine the filtrate and washing liquid and rectify, collect 95g of components between 101 and 103°C, a The content of hydrazine is 43%, the recovery rate is 88%, and the purity is 98%.

Embodiment 2

[0024] In the 2L four-neck round-bottomed flask that thermometer, stirrer and reflux condenser tube are equipped with, add respectively the waste liquid of 265g (22.7%) containing 1mol1, the copper oxide powder of 2-dimethylhydrazine and 160g (2mol), in Add 2 mol of 95% sulfuric acid dropwise under ice-brine cooling, heat to 5-95°C and control the temperature for 1-16 hours after dropping, add ammonia water to adjust the pH value to 5-13 when the reaction solution is cooled to about 0-10°C with ice-brine In between, filter the generated inorganic salts by means of suction filtration, wash the filter cake with cold water, combine the filtrate and washing liquid and rectify, collect 98g of components between 101 and 103°C, and the content of monomethylhydrazine is 39%. , the recovery rate was 83%, and the purity was 98.5%.

Embodiment 3

[0026] In the 2L four-neck round bottom flask that thermometer, stirrer and reflux condenser are equipped with, add respectively the waste liquid of 265g (22.7%) containing 1mol1,2-dimethylhydrazine and the solid potassium chlorate of 245g (2mol), in ice Add 197g (2mol) of 37% hydrochloric acid dropwise under brine cooling, heat to 5-95°C and control the temperature for 1-16 hours after dropping, add solid potassium hydroxide to adjust the pH when the reaction solution is cooled to about 0-10°C with ice-brine When the value is between 5 and 13, filter the generated inorganic salts by suction filtration, wash the filter cake with cold water, combine the filtrate and washing liquid and rectify, collect 118g of components between 101 and 103°C, monomethylhydrazine The content is 31%, the recovery rate is 83%, and the purity is 98.5%.

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Abstract

The invention discloses a novel method for converting industrial waste 1,2-dimethylhydrazine into methylhydrazine. A by-product 1,2-dimethylhydrazine liquid waste in industrial production of methylhydrazine is directly oxidized by using an oxidant for the first time, and a high-purity methylhydrazine water solution is obtained in rectifying and concentrating manners, so that commercial use of the 1,2-dimethylhydrazine by-product is solved. The method is simple in reaction process, high in conversion rate, and low in cost, the fed oxidant can be recycled after being restored, above all, waste is changed into treasures, the environmental pollution caused by discharged highly toxic industrial waste is prevented, and the safety is improved.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a synthesis route and separation technology for converting industrial waste 1,2-dimethylhydrazine into monomethylhydrazine with an oxidant. Background technique [0002] my country is a big producer of monomethylhydrazine, and its annual output ranks among the top in the world. Monomethylhydrazine is a very valuable compound that is widely used in various industries such as medicine, pesticide, chemical industry, aerospace and missiles. With the large demand of the market, the production of this raw material is also doubled. [0003] Hydrochloric acid methanol hydrazine hydrate method is one of the methods to produce monomethylhydrazine, which is relatively mature and widely used at present. The main process is: using methanol and hydrazine hydrate as raw materials, using hydrochloric acid and methyl chloride as catalysts, and preparing monomethylhydrazine under the pressure of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/14C07C241/02
Inventor 周建乌拉阔夫·巴洛特阿依别克·马力克阿拉法特·阿依别克周俊杰乌拉阔夫·侯赛因
Owner DONGLI NANTONG CHEM
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