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Continuous production method and device of 4-chlorophenylhydrazine hydrochloride

A technology of chlorophenylhydrazine hydrochloride and chloroaniline hydrochloride is applied in the field of continuous production method and device of p-chlorophenylhydrazine hydrochloride, and can solve the problems affecting product purity and yield, uneven mixing of materials, heavy weight, etc. The problem of slow decomposition of nitrogen salts can improve the continuity of production, improve production efficiency, and reduce high-salt wastewater.

Active Publication Date: 2018-01-12
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yet simple still reaction has obvious defect: (1) the reaction time of diazotization reaction is longer, and production efficiency is low; (2) mechanical agitation causes material to mix inhomogeneously, and local heat release is too much and easily causes safety accident; ( 3) The diazonium salt decomposes slowly, and then produces a series of by-products, which ultimately affects the purity and yield of the product

Method used

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  • Continuous production method and device of 4-chlorophenylhydrazine hydrochloride

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Embodiment 1

[0024] A continuous production method of p-chlorophenylhydrazine hydrochloride, comprising the following steps:

[0025] (1) prepare p-chloroaniline hydrochloride hydrochloride solution in the first batching still 1: p-chloroaniline 127.5kg, 37% hydrochloric acid 246.6kg and water 200kg; Prepare sodium nitrite solution in the second batching still 2: nitrous acid Sodium 69kg and water 140kg; P-chloroaniline hydrochloride solution and sodium nitrite solution are pumped in mixer 6 by metering pump 5, obtain mixed solution, adjust the feed ratio that mixed solution enters tubular reactor 7, parachlorine The molar ratio of aniline to sodium nitrite is 1:1.02, and the reaction temperature is 10° C. to prepare the diazonium salt intermediate;

[0026] (2) respectively drop into sodium sulfite 157.5kg and water 350kg and Raney's nickel catalyst 0.5kg in 2 reduction reactors 8 in advance, continue to pass into sulfur dioxide gas to reduction reactor 8, will the diazo that step (1) mak...

Embodiment 2

[0029] A continuous production method of p-chlorophenylhydrazine hydrochloride, comprising the following steps:

[0030] (1) prepare p-chloroaniline hydrochloride hydrochloride solution in the first batching still 1: p-chloroaniline 127.5kg, 37% hydrochloric acid 246.6kg and water 200kg; Prepare sodium nitrite solution in the second batching still 2: nitrous acid Sodium 69kg and water 140kg; P-chloroaniline hydrochloride solution and sodium nitrite solution are pumped in mixer 6 by metering pump 5, obtain mixed solution, adjust the feed ratio that mixed solution enters tubular reactor 7, parachlorine The molar ratio of aniline to sodium nitrite is 1:1.02, and the reaction temperature is 15° C. to prepare the diazonium salt intermediate;

[0031] (2) respectively drop into sodium sulfite 157.5kg and water 350kg and Raney's nickel catalyst 0.5kg in 2 reduction reactors 8 in advance, continue to pass into sulfur dioxide gas to reduction reactor 8, will the diazo that step (1) mak...

Embodiment 3

[0034] A continuous production method of p-chlorophenylhydrazine hydrochloride, comprising the following steps:

[0035] (1) prepare p-chloroaniline hydrochloride hydrochloride solution in the first batching kettle: p-chloroaniline 127.5kg, 37% hydrochloric acid 246.6kg and water 200kg; prepare sodium nitrite solution in the second batching kettle: sodium nitrite 69kg and water 140kg; p-Chloroaniline hydrochloride solution and sodium nitrite solution are pumped into the mixer to obtain a mixed solution, adjust the feed ratio of the mixed solution into the tubular reactor, the mol ratio of p-chloroaniline and sodium nitrite The ratio is 1:1.12, the reaction temperature is 10°C, and the diazonium salt intermediate is obtained;

[0036] (2) respectively drop into sodium sulfite 157.5kg and water 350kg and Raney's nickel catalyst 0.5kg in 2 reduction reactors 8 in advance, continue to pass into sulfur dioxide gas to reduction reactor 8, will the diazo that step (1) makes The salt...

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Abstract

The invention relates to the field of organic synthesis and in particular relates to a continuous production method and device of 4-chlorophenylhydrazine hydrochloride. A continuous production mannercombining tubular reaction and kettle type reaction is adopted; diazotization reaction is carried out in a tubular reactor and raw materials are uniformly mixed; the reaction is stably carried out, the safety of the reaction is improved, side reaction is reduced and the purity and the yield of a final product are improved; reduction reaction and acidification reaction are carried out in a reduction reaction kettle so that the production continuity is improved, the total reaction time is reduced, the production efficiency is improved, the energy consumption is saved and the production cost is reduced; the yield of the prepared 4-chlorophenylhydrazine hydrochloride is greater than 90 percent and the purity is greater than 96 percent; the continuous production method and device meet industrial requirements and are suitable for industrial continuous production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a continuous production method of p-chlorophenylhydrazine hydrochloride and a device thereof. Background technique [0002] p-Chlorophenylhydrazine hydrochloride is a widely used organic synthesis intermediate, which can be used in the synthesis of dyes, medicines and other chemicals. Its molecular formula is C 6 h 8 Cl 2 N 2 , the molecular weight is 179, the appearance is white or light red powder, and the melting point is 210-218 ℃. The main applications of p-chlorophenylhydrazine hydrochloride in chemical synthesis are: (1) for central nervous system drug thieno[2,3',2,3]thiopyran[4,5,c]-pyrazoline -Synthesis of 3(4H)-ketone, blocking the ascending activation system of the brainstem reticular structure; (2) for the synthesis of anxiolytics benzothiophene [5,4-c] pyrazoline; (3) with Used in the synthesis of salicylic acid anti-inflammatory drugs; (4) for the synthesis of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/02C07C243/22C07C245/20B01J19/00
Inventor 刘善和赵维德史玉龙杨继华史清平汪中伟吴德清
Owner ANHUI COSTAR BIOCHEM CO LTD
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