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Methylhydrazine continuous flow microchannel alkylation method

A technology of methylhydrazine and alkylation, which is applied in the field of methylhydrazine preparation, can solve the problems of small scale, difficulty in adapting to the violent reaction environment of methylhydrazine, and difficulty in large-scale industrial production, so as to reduce the generation of by-products and ensure safety High performance, reduce the effect of side effects

Pending Publication Date: 2022-03-04
DONGLI NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the prior art, there are no process reports or literature records of using continuous flow reaction to synthesize methylhydrazine. Because traditional microchannel reactors are usually small in scale, it is difficult to realize large-scale industrial production, and it is also difficult to adapt to methylhydrazine. Due to the severe reaction environment in the production process, it is necessary to propose a microchannel reaction method suitable for the modern production process of methylhydrazine according to the reaction process and process characteristics

Method used

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  • Methylhydrazine continuous flow microchannel alkylation method
  • Methylhydrazine continuous flow microchannel alkylation method
  • Methylhydrazine continuous flow microchannel alkylation method

Examples

Experimental program
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Effect test

Embodiment 1

[0050] (1) Hydrazine hydrochloride is mixed with water to prepare an aqueous solution of hydrazine hydrochloride so that the mass percentage concentration of hydrazine hydrochloride is 75%, and methyl alcohol is mixed with a concentration of 30% aqueous hydrochloric acid to prepare methanolic hydrochloride solution so that the concentration of hydrochloric acid is 3%. ;

[0051] (2) send the hydrochloric acid methanol solution into the microchannel of the microchannel reactor with a pump earlier, fill up the microchannel, then use the pump to send the hydrazine hydrochloride aqueous solution into the microchannel, so that the hydrazine hydrochloride and methyl alcohol are continuously reacted in the microchannel, Wherein, the reaction temperature is 110°C, the reaction pressure is 0.4MPa, the residence time is 15min, the mass ratio of hydrazine hydrochloride and methanol is controlled to be 1:1.05, and the aqueous solution of hydrazine hydrochloride is controlled to be sent int...

Embodiment 2

[0058] (1) Hydrazine hydrochloride is mixed with water to prepare an aqueous solution of hydrazine hydrochloride so that the mass percentage concentration of hydrazine hydrochloride is 85%, and methyl alcohol is mixed with a concentration of 30% aqueous hydrochloric acid to prepare methanolic hydrochloride solution so that the concentration of hydrochloric acid is 3%. ;

[0059] (2) send the hydrochloric acid methanol solution into the microchannel of the microchannel reactor with a pump earlier, fill up the microchannel, then use the pump to send the hydrazine hydrochloride aqueous solution into the microchannel, so that the hydrazine hydrochloride and methyl alcohol are continuously reacted in the microchannel, Wherein, the reaction temperature is 120°C, the reaction pressure is 0.3MPa, the residence time is 10min, the mass ratio of hydrazine hydrochloride and methanol is controlled to be 1:1.15, and the aqueous solution of hydrazine hydrochloride is sent into the microchanne...

Embodiment 3

[0066] (1) Hydrazine hydrochloride is mixed with water to prepare an aqueous solution of hydrazine hydrochloride so that the mass percent concentration of hydrazine hydrochloride is 80%, and methyl alcohol is mixed with a concentration of 30% aqueous hydrochloric acid to prepare a methanolic hydrochloride solution so that the concentration of hydrochloric acid is 3%. ;

[0067] (2) send the hydrochloric acid methanol solution into the microchannel of the microchannel reactor with a pump earlier, fill up the microchannel, then use the pump to send the hydrazine hydrochloride aqueous solution into the microchannel, so that the hydrazine hydrochloride and methyl alcohol are continuously reacted in the microchannel, Wherein, the reaction temperature is 115°C, the reaction pressure is 0.35MPa, and the residence time is 12.5min. The mass ratio of hydrazine hydrochloride and methanol is controlled to be 1:1.1, and the aqueous solution of hydrazine hydrochloride is controlled to be sen...

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Abstract

The invention belongs to the technical field of methylhydrazine preparation, and particularly relates to a methylhydrazine continuous flow microchannel alkylation method which comprises the following steps: (1) preparing a hydrazine hydrochloride aqueous solution from hydrazine hydrochloride and water, and preparing a hydrochloric acid methanol solution from methanol and a hydrochloric acid aqueous solution; (2) respectively feeding a hydrazine hydrochloride aqueous solution and a hydrochloric acid methanol solution into the micro-channel by using a pump, and continuously reacting hydrazine hydrochloride and methanol in the micro-channel; (3) collecting the generated mixed solution, and performing atmospheric distillation to recover the methanol mixed solution; (4) carrying out reduced pressure distillation to remove residual methanol and water; (5) controlling the temperature to be 70-80 DEG C, adding hydrazine hydrate to perform dissociation, and dissociating methyl hydrazine; (6) carrying out reduced pressure distillation, and collecting a methylhydrazine crude product; and (7) carrying out normal-pressure rectification, and collecting azeotrope of methylhydrazine and water to obtain a methylhydrazine aqueous solution. According to the method, the hydrazine hydrochloride and the methanol are subjected to the continuous alkylation reaction in the microreactor to prepare the methylhydrazine, so that the selectivity is high, the reaction condition is mild, the energy consumption is low, and the safety is high.

Description

technical field [0001] The application belongs to the technical field of methylhydrazine preparation, in particular to a continuous-flow microchannel alkylation method for methylhydrazine. Background technique [0002] Methylhydrazine, also known as monomethylhydrazine, is an important chemical product with a structural formula of CH 3 NHNH 2 . Methylhydrazine can spontaneously ignite in contact with a strong oxidant, and it is very easy to burn and explode when exposed to open flames and high heat. It is often combined with dinitrogen tetroxide and other oxidants to form a bicomponent liquid propellant, which is used in the monitoring systems of space shuttles, spacecraft and satellites. It has been widely used in the synthesis of pharmaceuticals, pesticides and other fine chemical products over the years. [0003] The alkylation reaction link in the existing methylhydrazine synthesis process is a high-risk process, the reaction process is violent and difficult to contro...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/14B01J19/00
CPCC07C241/02B01J19/0093C07C243/14
Inventor 沈建祥陆立新吴雪峰李鑫鑫陆凌军石玉晶
Owner DONGLI NANTONG CHEM
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