Methylhydrazine continuous flow microchannel alkylation method

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...

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

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