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Preparation method of N-methyl-4-methoxyaniline

A technology of methoxyaniline and methyl, which is applied in the field of preparing N-methyl-4-methoxyaniline, can solve problems such as difficult industrial production, unfavorable environmental protection treatment, catalyst poisoning, etc., and achieve good product quality and improved The utilization rate of raw materials and the effect of reducing environmental pressure

Active Publication Date: 2016-09-07
JIANGSU ZHONGDAN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has high requirements on raw materials, catalysts and reaction equipment, and it is difficult to realize industrial production: first, in the reaction process of aniline and methanol, the catalyst is poisoned due to the influence of trace elements in the raw materials; secondly, the catalyst In the process of carrying out the reaction, its activity itself will become worse and worse, which requires continuous improvement of the reaction temperature. Even so, in the later stage of the reaction, the content of the second-protected impurities in the obtained product is getting higher and higher, and the catalyst needs to be carried out. Activation treatment; in addition, because the catalyst used is a composite solid catalyst, the solid catalyst is difficult to handle, which brings great disadvantages to environmental protection treatment

Method used

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  • Preparation method of N-methyl-4-methoxyaniline
  • Preparation method of N-methyl-4-methoxyaniline
  • Preparation method of N-methyl-4-methoxyaniline

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Embodiment 1

[0034] The concrete steps of the method for described preparation N-methyl-4-methoxyaniline are:

[0035] (1) Synthesis of N-methyl-4-methoxyaniline

[0036] a. Put 100kg of p-aminoanisole, 500Kg (5w / w) of N, N-dimethylformamide, 26.8kg (1.1eq) of paraformaldehyde and 15kg of Raney nickel into the autoclave. Nitrogen was replaced 3 times, and then replaced with hydrogen 3 times. After the replacement, the system began to gradually heat up to 60 ° C, and hydrogen gas was started to control the reaction temperature at 60 ° C. The reaction pressure was controlled at 1.5 Mpa, and the reaction time was 8 hours until the system pressure no longer change.

[0037] b. When the reaction pressure is basically unchanged, close the hydrogen valve, and continue the reaction at this temperature and pressure for 1 hour. If the pressure remains unchanged, take a sample of the reaction solution and calibrate N-methyl-4-methoxy Aniline content, when the main content reaches more than 70%, it ...

Embodiment 2

[0048] The concrete steps of the method for described preparation N-methyl-4-methoxyaniline are:

[0049] (1) Synthesis of N-methyl-4-methoxyaniline

[0050] a. Put 100kg of p-aminoanisole, 200Kg (2w / w) of N, N-dimethylformamide, 17.07kg (0.7eq) of paraformaldehyde and 10kg of catalyst Raney nickel into the reaction kettle. Nitrogen was replaced 3 times, and then replaced with hydrogen 3 times. After the replacement, the system began to heat up gradually, and hydrogen gas was started. The reaction temperature was controlled at 80°C, the reaction pressure was controlled at 1.0Mpa, and the reaction time was controlled for 8h until the system pressure did not change any more. until.

[0051] b. When the reaction pressure is basically unchanged, close the hydrogen valve, and continue the reaction at this temperature and pressure for 1 hour. If the pressure remains unchanged, take a sample of the reaction solution and calibrate N-methyl-4-methoxy Aniline content, when the main co...

Embodiment 3

[0056] The concrete steps of the method for described preparation N-methyl-4-methoxyaniline are:

[0057] 1) Synthesis of N-methyl-4-methoxyaniline

[0058] a. Put 100kg of p-aminoanisole, 400Kg (4w / w) of N, N-dimethylformamide, 21.9kg (0.9eq) of paraformaldehyde and 2kg of catalyst Raney nickel into the reaction kettle. Nitrogen was replaced 3 times, and then replaced with hydrogen 3 times. After the replacement, the system began to gradually heat up, and hydrogen was started. The reaction temperature was controlled at 120°C, the reaction pressure was controlled at 0.6Mpa, and the reaction time was controlled for 8 hours until the system pressure did not change any more. until.

[0059] b. When the reaction pressure is basically unchanged, close the hydrogen valve, and continue the reaction at this temperature and pressure for 1 hour. If the pressure remains unchanged, take a sample of the reaction solution and calibrate N-methyl-4-methoxy Aniline content, when the main con...

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Abstract

The invention relates to a method for preparing N-methyl-4-methoxyaniline, and relates to the field of petroleum additive and chemical pharmaceutical intermediates. According to the invention, the preparation of N-methyl-4-methoxyaniline is divided into two steps which are N-methyl-4-methoxyaniline synthesis and N-methyl-4-methoxyaniline rectification. According to the method, N-methyl-4-methoxyaniline is synthesized through catalytic hydrogenation under a condition with a solvent. During an N-methyl-4-methoxyaniline conversion synthesis process, the hydrogenation reaction is carried out with a catalyst, such that the process has the advantages of mild reaction, short time, low temperature, simple operation and the like. During the rectification process, first the organic solvent is removed, then rectification is carried out, such that a qualified N-methyl-4-methoxyaniline standard product can be obtained.

Description

technical field [0001] The invention belongs to the field of petroleum additives and chemical and pharmaceutical intermediates, and in particular relates to a method for preparing N-methyl-4-methoxyaniline. Background technique [0002] N-methyl-4-methoxyaniline is currently the most effective, economical and practical petroleum additive. It has the characteristics of high anti-oxidation efficiency, high safety performance, convenient use, clean and environmental protection, and is suitable for gasoline and diesel oil. , it is an efficient antiknock agent. [0003] Low cost at present, is applicable to the method for industrialized preparation N-methyl-4-methoxyaniline, also does not report, only has similar synthetic method, as Russian patent (RU 2270187, RU 2205067, Ru 2205067) has similar structure Synthesis method, this patent uses aniline and methanol as raw materials, and after loading a copper-containing composite catalyst in a solid-bed reactor, the synthesis is car...

Claims

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Application Information

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IPC IPC(8): C07C217/84C07C213/00
CPCC07C213/00C07C217/84
Inventor 唐静王春民沙燕红任云华张家庆
Owner JIANGSU ZHONGDAN CHEM TECH
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