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A kind of method utilizing meta-position oil to prepare m-chloroaniline

A technology for chloroaniline and chloronitrobenzene, which is applied in the field of preparing m-chloroaniline by using meta oil, can solve the problems of low product yield, polluted environment, easy dechlorination by hydrogenation reduction, etc., and achieves high economic benefit and high output , low cost effect

Active Publication Date: 2021-05-14
AZUREWAVE TEHNOLOGIES INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The iron powder reduction method produces a large amount of iron sludge, which seriously pollutes the environment; the alkali sulfide reduction method has the characteristics of complex reduction route, low product yield, and large amount of waste liquid; the electrochemical reduction method consumes too much energy; the catalytic hydrogenation method has a reaction route , low energy consumption, and environmental friendliness. However, during the catalytic hydrogenation of m-nitrochlorobenzene, the meta-activation of the nitro group can also increase the side reaction of C-CL bond hydrogenolysis and dechlorination to generate aniline, thereby Reduced yield of main product
At the same time, the hydrogen chloride generated by dechlorination will also cause corrosion to equipment
[0005] To sum up, at present, the existing technology has problems such as high cost of raw material m-nitrochlorobenzene, environmental pollution caused by reduction of auxiliary raw material iron powder, high cost of sodium sulfide reduction, easy dechlorination by hydrogenation reduction, corrosion of equipment, etc.

Method used

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Comparison scheme
Effect test

Embodiment

[0029] A method utilizing meta-position oil to prepare m-chloroaniline, comprising the following steps:

[0030] (1) Batching reaction: add the meta-position oil into the methoxylation reaction kettle, measure methanol from the methanol metering tank in a closed state, and then put in the catalyst ammonium chloride, stir at a speed of 60r / min, and heat the reaction kettle at the same time Temperature to 58-63°C, adjust the pressure of the reactor to 0-0.2MPa, and finally add sodium hydroxide to the reactor, keep the temperature constant, take a sample for detection after 5 hours of reaction; among them, meta oil: methanol: sodium hydroxide : The mass ratio of ammonium chloride = 1: 0.30: 0.32: 0.045, when the content of p-nitrochlorobenzene ≤ 0.1% and the content of o-nitrochlorobenzene ≤ 2%, the methanol is recovered and then transferred to the next washing process ;

[0031] (2) Washing: The material obtained by the reaction in step (1) is transported to the workshop storag...

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Abstract

The invention relates to a method for preparing m-chloroaniline by using meta-position oil, which belongs to the technical field of preparing m-chloroaniline, and specifically includes the steps of batching reaction, water washing, drying, three-stage vacuum distillation, crystallization, reduction, redistillation and the like. The present invention uses waste meta-oil produced by p- and o-nitrogen and industrial waste liquid sodium hydrosulfide as raw materials, utilizes methoxylation, crystallization and reduction to prepare m-chloroaniline, and generates by-products o-aminoanisole and p- Anisole, thereby realizing low cost, high output, compared with existing production technology, has obvious cost advantage, has higher economic benefit.

Description

technical field [0001] The invention belongs to the technical field of preparation of m-chloroaniline, and in particular relates to a method for preparing m-chloroaniline by utilizing meta-position oil. Background technique [0002] m-Chloroaniline, colorless liquid to light amber liquid, poisonous, is an important fine chemical intermediate, mainly used as an intermediate of azo dyes and pigments, drugs, insecticides, and pesticide chemicals. [0003] Meta-oil, mainly composed of m-, o-, and p-chloronitrobenzene, is a general term for the two products of p-nitrate and ortho-nitrate in the production process of p-o-nitrate, as well as the waste liquid rich in m-nitrochlorobenzene and high boiling point organic matter. [0004] Most of the existing methods for preparing m-chloroaniline are to reduce the nitro group of m-nitrochlorobenzene to obtain m-chloroaniline. The traditional nitro reduction methods mainly include iron powder reduction method, alkali sulfide reduction m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/36C07C211/52C07C201/16C07C205/12C07C213/02C07C217/84
CPCC07C201/12C07C201/16C07C209/365C07C213/02C07C211/52C07C205/12C07C217/84C07C205/37
Inventor 郝宗贤解凤贤张其忠欧加思柏阳
Owner AZUREWAVE TEHNOLOGIES INC
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