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Method for producing m-acetamino-N,N-diethyl aniline

A technology of acetaminoaniline and its production method, which is applied in the field of chemical synthesis of dye intermediates, can solve the problems of large energy consumption, increased product cost, and difficulty in reusing by-products, etc., and achieve the effect of reducing costs

Active Publication Date: 2010-06-09
ZHEJIANG RUNTU
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Problems solved by technology

[0007] In the prior art, a large amount of sodium bromide and sodium chloride by-products will be produced after the ethylation reaction, not only the by-products are difficult to reuse, but also the separation and treatment of sodium bromide and sodium chloride, as well as corresponding environmental protection measures It will consume a lot of energy and increase the total cost of the product

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  • Method for producing m-acetamino-N,N-diethyl aniline
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  • Method for producing m-acetamino-N,N-diethyl aniline

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Embodiment Construction

[0038] In 3 parts by weight of water, add 10 parts by weight of m-phenylenediamine, 17 parts by weight of 48% hydrobromic acid, then add 8.5 parts by weight of glacial acetic acid, add, and react at 90°C for 20 hours, (sampling detection, liquid phase Chromatographic detection of m-phenylenediamine peak ≤ 1.5% is qualified), cooling to 80°C, adding 4 parts by weight of water, cooling to 40°C, standing for 10 hours, filtering to obtain the acylate, and filtering the mother liquor for reuse as the next batch of acylation.

[0039] When filtering the mother liquor for reuse, you can add about 30 parts by weight of the mother liquor to the reactor, heat up, and distill out 10 parts by weight of water (which contains about 20% acetic acid, and the acetic acid that is steamed is purified in the acylation and salt-forming reaction through rectification. Apply mechanically), then add 10 parts by weight of m-phenylenediamine, 16 parts by weight of 48% hydrobromic acid, and 8.5 parts by ...

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Abstract

The invention discloses a method for producing m-acetamino-N,N-diethyl aniline, which comprises the following steps: (1) mixing m-phenylenediamine, glacial acetic acid and hydrobromic acid to perform an acylation reaction to obtain an acetylated compound; (2) performing ethylation of the acetylated compound and bromoethane, and after the reaction is finished, diluting and filtering the reaction system, and eluting the product filtered out to obtain m-acetamino-N,N-diethyl aniline; (3) concentrating mother solution produced by filtration and elution in the step (2); and (4) dripping sulfuric acid and ethanol into the mother solution to perform an reaction to obtain bromoethane and collecting the bromoethane for use in the ethylation in the step (2). The production method of the invention has the advantages that: the active ingredients in waste water produced in production are fully used; the recycling of the waste water reduces cost; and clean production is realized.

Description

technical field [0001] The invention relates to a production method of N,N-diethyl-m-acetamidoaniline, which belongs to the field of chemical synthesis of dye intermediates. Background technique [0002] N, N-diethyl-m-acetamidoaniline is an important chemical raw material and intermediate, widely used in the production of fine chemicals such as dyes. [0003] The most commonly used synthetic method at present is: take m-phenylenediamine as main raw material, generate m-aminoacetanilide (acylate) after carrying out acylation with acetic anhydride and hydrogen chloride, and salt-forming reaction, and the reaction formula is as follows: [0004] [0005] The acylate reacts with ethyl bromide to obtain N,N-diethyl-m-acetamidoaniline. The reaction formula is as follows: [0006] [0007] In the prior art, a large amount of sodium bromide and sodium chloride by-products will be produced after the ethylation reaction, not only the by-products are difficult to reuse, but als...

Claims

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Application Information

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IPC IPC(8): C07C233/43C07C231/12C01D5/00
Inventor 赵国生方标陈田木唐勇何江伟杜维扬
Owner ZHEJIANG RUNTU
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