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Preparation method for continuously preparing tert-butylhydrazine hydrochloride

A technology of tert-butylhydrazine and hydrochloride, which is applied in the field of preparation of tert-butylhydrazine hydrochloride, can solve the problems of high VOC emissions, insufficient material contact, low production efficiency, etc., and achieve less discharge of three wastes, production The effect of short cycle time and high degree of automation

Pending Publication Date: 2020-12-04
SHANGHAI NO 4 REAGENT & H V CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method yield is low, and the main reason is that tert-butanol and hydrazine hydrate hydrochloride are not fully contacted in the tank reactor, and hydrochloric acid is too acidic to cause dehydration reaction of tert-butanol to produce olefinic by-products. Emitted into the air in the form of VOC during the reflux reaction
There are disadvantages such as low raw material utilization rate, low product yield, and high VOC emissions. At the same time, the production efficiency of the tank reaction is low and the production cost is high.

Method used

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  • Preparation method for continuously preparing tert-butylhydrazine hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Present embodiment provides a kind of method utilizing microchannel reactor to continuously synthesize tert-butylhydrazine hydrochloride, concrete implementation is as follows:

[0027] Mass concentration 50% hydrazine hydrate solution is pumped into the first reaction zone of microchannel reactor with 15ml / min flow rate, simultaneously, the hydrochloric acid of mass concentration 20% is pumped into the first reaction zone of microchannel reactor with 3.7ml / min flow rate, the first The temperature of the reaction zone was set at 45°C, and the residence time of the hydrazine hydrate solution and the hydrochloric acid solution was 5.0s.

[0028] The hydrazine hydrochloride solution obtained in the first reaction zone is pumped into the microchannel reactor mixing zone with a flow rate of 15ml / min; tert-butyl alcohol is mixed with 75% aqueous solution, with 18ml / min; the flow rate is pumped into the microchannel reactor mixing zone, and the mixing zone is stably set. Set a...

Embodiment 2

[0031] Mass concentration 70% hydrazine hydrate solution is pumped into the first reaction zone of microchannel reactor with 10ml / min flow rate, simultaneously, the hydrochloric acid of mass concentration 30% is pumped into the first reaction zone of microchannel reactor with 2.0ml / min flow rate, the first The temperature of the reaction zone was set at 50°C, and the residence time of the hydrazine hydrate solution and the hydrochloric acid solution was 4.0s.

[0032] The hydrazine hydrochloride solution obtained in the first reaction zone is pumped into the microchannel reactor mixing zone with a flow rate of 11ml / min; tert-butyl alcohol is mixed with 60% aqueous solution, with 24ml / min; the flow rate is pumped into the microchannel reactor mixing zone, and the mixing zone is stably set. Set at 55°C, the residence time is 6s. The mixed solution after mixing enters the second reaction zone of the microchannel reactor at a flow rate of 17.5 ml / min, and the temperature of the se...

Embodiment 3

[0035] Mass concentration 80% hydrazine hydrate solution is pumped into the first reaction zone of microchannel reactor with 10ml / min flow rate, simultaneously, the hydrochloric acid of mass concentration 30% is pumped into the first reaction zone of microchannel reactor with 1.4ml / min flow rate, the first The temperature of the reaction zone was set at 45°C, and the residence time of the hydrazine hydrate solution and the hydrochloric acid solution was 5.0s.

[0036] The hydrazine hydrochloride solution obtained in the first reaction zone is pumped into the microchannel reactor mixing zone at a flow rate of 11ml / min; tert-butanol is formulated into an 80% aqueous solution at 15.5ml / min; the flow rate is pumped into the microchannel reactor mixing zone, and the mixing zone is stable Set to 60°C and dwell time to 5s. The mixed solution after mixing enters the second reaction zone of the microchannel reactor at a flow rate of 26.5 ml / min, and the temperature of the second reacti...

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Abstract

The invention discloses a method for continuously preparing tert-butylhydrazine hydrochloride by using a micro-channel reactor. The method comprises the steps of 1, carrying out primary reaction mixing on hydrazine hydrate with the mass concentration of 40-80% and hydrochloric acid with the concentration of 25-36% in the micro-channel reactor to obtain a hydrazine hydrochloride solution; 2, mixingthe hydrazine hydrochloride solution with a tert-butyl alcohol solution in the micro-channel reactor for later use; and 3, carrying out a secondary reaction on the material mixed in the step 2 to obtain a product aqueous solution, continuously concentrating the product aqueous solution to achieve a certain concentration, carrying out cooling crystallization, filtering, and drying to obtain the tert-butylhydrazine hydrochloride. According to the method, the reaction rate and the raw material utilization rate are increased, the side reaction for producing the olefin compounds through tert-butylalcohol dehydration is avoided, the reaction is easy to control, the production period is short, emission of three wastes is little, the total yield can reach 85% or above, and the automation degreeof the reaction process is high.

Description

technical field [0001] The invention relates to a method for preparing tert-butylhydrazine hydrochloride, in particular to a method for continuously preparing tert-butylhydrazine hydrochloride using a microchannel reactor. Background technique [0002] Tert-butylhydrazine hydrochloride is an important pesticide intermediate, which can be used to synthesize benzoylhydrazine insecticides, dihydrazide insecticides, tebufenozide (tebufenozide), chlorantranilis Halofenozide, methoxyfenozide, and chromafenozide, and the acaricide pyridaben. At the same time, it can also be used as a raw material for synthetic medicine and materials. [0003] In the prior art, tert-butylhydrazine hydrochloride is generally produced by kettle-type batch-type preparation method, hydrazine hydrate is acidified with hydrochloric acid, then reacted with tert-butanol at high temperature, concentrated and recrystallized to obtain tert-butylhydrazine hydrochloride Salt. But this method yield is low, and...

Claims

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Application Information

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IPC IPC(8): C07C243/14C07C241/02B01J19/00
CPCC07C241/02B01J19/0093C01B21/16C07C243/14
Inventor 张传好殷俊周媛媛
Owner SHANGHAI NO 4 REAGENT & H V CHEM
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