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Method for preparing m-chloroaniline by using meta-position oil

A technology of chloroaniline and chloronitrobenzene, which is applied in the field of using meta-oil to prepare m-chloroaniline, which can solve the problems of low product yield, environmental pollution, easy dechlorination by hydrogenation reduction, etc., and achieve high economic benefits and high output , low-cost effect

Active Publication Date: 2017-06-23
ANHUI HAIHUA CHEM
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  • Abstract
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  • Claims
  • Application Information

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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 the high cost of raw material m-nitrochlorobenzene, the environmental pollution caused by the reduction of auxiliary raw material iron powder, the high cost of sodium sulfide reduction, the easy dechlorination of hydrogenation reduction, and the corrosion of equipment.

Method used

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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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PUM

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Abstract

The invention relates to a method for preparing m-chloroaniline by using meta-position oil and belongs to the technical field of preparation of m-chloroaniline. The method specifically comprises the steps of carrying out an ingredient reaction, carrying out water washing, carrying out drying, carrying out third-stage vacuum distillation, carrying out crystallization, carrying out reduction and carrying out re-distillation. According to the method, m-chloroaniline is prepared from waste, i.e., meta-position oil of production of p-nitrophenol and o-nitrophenol and industrial waste liquid, i.e., sodium hydrosulfide, which serve as raw materials, by using methoxylation, crystallization and reduction, and byproducts, i.e., o-aminoanisole and p-aminoanisole are produced, so that low cost and high yield are achieved, and the method has an obvious cost advantage and higher economic benefit compared with the existing production technologies.

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, toxic, is an important fine chemical intermediate, mainly used as an intermediate of azo dyes and pigments, drugs, insecticides, and pesticide chemicals. [0003] Meta-position oil, the main components are m-, o-, and p-chloronitrobenzene. It is a general term for the two products of p-nitrate and o-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. Traditional nitro reduction methods mainly include iron powder reduction method, alkali sulfide reduct...

Claims

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Application Information

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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 ANHUI HAIHUA CHEM
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