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Method for preparing ethyl hydrazine through continuous flow of microreactor

A micro-reactor, micro-channel reactor technology, applied in chemical instruments and methods, hydrazine preparation, chemical/physical/physical-chemical reactors, etc., can solve the problems of difficult separation, inability to obtain pure ethyl hydrazine, etc. Generation of side reactions, high safety, mild reaction conditions

Active Publication Date: 2022-03-18
DONGLI NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are many methods for preparing ethylhydrazine. Among them, the use of diethyl sulfate for alkylation is a relatively low-cost preparation method for ethylhydrazine, but it is easy to produce diethylhydrazine as a by-product, and it is not easy to separate, resulting in Ethylhydrazine with higher purity cannot be obtained

Method used

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  • Method for preparing ethyl hydrazine through continuous flow of microreactor
  • Method for preparing ethyl hydrazine through continuous flow of microreactor
  • Method for preparing ethyl hydrazine through continuous flow of microreactor

Examples

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Effect test

Embodiment 1

[0045] (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 75%, and ethanol is mixed with 30% aqueous hydrochloric acid to prepare ethanol hydrochloride so that the concentration of hydrochloric acid is 1%. ;

[0046] (2) send the ethanol hydrochloride solution into the microchannel of the microchannel reactor with a pump earlier, fill the microchannel, then use the pump to send the hydrazine hydrochloride aqueous solution into the microchannel, so that the hydrazine hydrochloride and ethanol are continuously reacted in the microchannel, Wherein, the reaction temperature is 102°C, the reaction pressure is 0.25MPa, the residence time is 70s, the molar ratio of ethanol and hydrazine hydrochloride is controlled to be 1.5:1, and the hydrazine hydrochloride aqueous solution is controlled to be sent into the microchannel under the condition of 50-60°C, so that th...

Embodiment 2

[0053] (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 85%, and ethanol is mixed with 30% hydrochloric acid aqueous solution to prepare a hydrochloric acid ethanol solution so that the concentration of hydrochloric acid is 1%. ;

[0054] (2) send the ethanol hydrochloride solution into the microchannel of the microchannel reactor with a pump earlier, fill the microchannel, then use the pump to send the hydrazine hydrochloride aqueous solution into the microchannel, so that the hydrazine hydrochloride and ethanol are continuously reacted in the microchannel, Wherein, the reaction temperature is 105°C, the reaction pressure is 0.2MPa, the residence time is 60s, the molar ratio of ethanol and hydrazine hydrochloride is controlled to be 1.55:1, and the hydrazine hydrochloride aqueous solution is controlled to be sent into the microchannel at 50-60°C to make...

Embodiment 3

[0061] (1) Hydrazine hydrochloride is mixed with water, and the aqueous solution of hydrazine hydrochloride is prepared, so that the mass percentage concentration of hydrazine hydrochloride is 80%, and ethanol is mixed with the aqueous hydrochloric acid solution of 30% with concentration, and the hydrochloric acid ethanol solution is prepared, so that the mass percentage concentration of hydrochloric acid is 1%;

[0062] (2) send the ethanol hydrochloride solution into the microchannel of the microchannel reactor with a pump earlier, fill the microchannel, then use the pump to send the hydrazine hydrochloride aqueous solution into the microchannel, so that the hydrazine hydrochloride and ethanol are continuously reacted in the microchannel, Wherein the reaction temperature is 103°C, the reaction pressure is 0.2MPa, the residence time is 65s, the molar ratio of ethanol and hydrazine hydrochloride is controlled to be 1.5:1, and the hydrazine hydrochloride aqueous solution is cont...

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Abstract

The invention belongs to the technical field of ethyl hydrazine preparation, and particularly relates to a method for preparing ethyl hydrazine through continuous flow of a microreactor, which comprises the following steps: (1) mixing hydrazine hydrochloride with water to obtain a hydrazine hydrochloride aqueous solution, and mixing ethanol with a hydrochloric acid aqueous solution to obtain a hydrochloric acid ethanol solution; (2) respectively feeding the hydrochloric acid ethanol solution and the hydrazine hydrochloride aqueous solution into the microchannel by using a pump, and enabling the hydrazine hydrochloride and ethanol to continuously react in the microchannel; (3) collecting the generated mixed solution, and distilling at normal pressure to recover the ethanol mixed solution; (4) carrying out reduced pressure distillation to remove residual ethanol and water; (5) controlling the temperature to be 60-70 DEG C, adding liquid caustic soda in a flowing manner for dissociation, and dissociating ethyl hydrazine; and (6) carrying out atmospheric distillation, and respectively collecting diethyl hydrazine, ethyl hydrazine and hydrazine hydrate at corresponding temperatures. According to the method, hydrazine hydrochloride and ethyl alcohol continuously react in the microreactor to obtain ethyl hydrazine hydrochloride, then the ethyl hydrazine hydrochloride is dissociated with liquid caustic soda, and finally ethyl hydrazine is collected through atmospheric distillation, so that the method can effectively improve the reaction selectivity and reduce by-products.

Description

technical field [0001] The application belongs to the technical field of preparation of ethyl hydrazine, and in particular relates to a method for preparing ethyl hydrazine in a microreactor continuous flow. Background technique [0002] Ethylhydrazine can be used in the manufacture of pesticides and drugs, and is also an important intermediate in organic synthesis. At present, there are many methods for preparing ethylhydrazine. Among them, the use of diethyl sulfate for alkylation is a relatively low-cost preparation method for ethylhydrazine, but it is easy to produce diethylhydrazine as a by-product, and it is not easy to separate, resulting in Ethylhydrazine with higher purity cannot be obtained. [0003] Microreactor is a new type of continuous flow reaction equipment, which has the following advantages: (1) High mass transfer efficiency: it can be fully mixed in milliseconds to microseconds, shorten the reaction time, reduce the volume of equipment, and improve produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/02C07C243/14B01J19/00
CPCC07C241/02B01J19/0093C07C243/14
Inventor 吴雪峰沈建祥陆立新王全徐林圣亚苏
Owner DONGLI NANTONG CHEM
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