Preparation process of 2-amino-4-acetyl aminoanisole

A technology of acetamidoanisole and preparation process, which is applied in the field of preparation technology of 2-amino-4-acetamidoanisole, can solve the problems of complex process, many side reactions, and high product impurity content, and achieves process safety , the effect of no three waste discharge, short process flow

Active Publication Date: 2014-01-22
SHANGHAI ZONGXING CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 2-Amino-4-acetylaminoanisole is used as a disperse dark blue H-GL intermediate. At present, there are not many domestic manufacturers and the output is very small. In the past, Zhejiang Huangyan United Chemical Plant and Jiaojiang Chemical No. 4 Plant had small-scale production facilities , it may be due to the process, and the three wastes, it is no longer produced
[0019] Both of the above two methods have the problems of complicated process, long process, a large amount of three wastes generated in the production process, many side reactions, and high impurity content in the product

Method used

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  • Preparation process of 2-amino-4-acetyl aminoanisole

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Embodiment Construction

[0050] A kind of preparation technology of 2-amino-4-acetamidoanisole,

[0051] Add accurately measured methanol, 2,4-dinitroanisole, and catalyst into the hydrogenation tank, and carry out hydrogenation reaction after low-pressure nitrogen replacement. When the system no longer absorbs hydrogen, cool down, filter and recover the catalyst, and then acylate In the still, add acetic anhydride to carry out acylation reaction. The temperature is controlled at 5°C. After the acylation reaction is completed, methanol is recovered through a methanol rectification tower, and the material is sent to a vacuum distillation kettle to recover acetic acid. The material in the kettle is cooled and crystallized to obtain 2-amino-4-acetamidoanisole product.

[0052] The ratio of 2,4-dinitroanisole, acetic anhydride and catalyst is 1100:590:5. The catalyst referred to is Raney nickel.

[0053] The invention can provide an output of 6,000 tons per year. The total industrial output value of thi...

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Abstract

The invention discloses a preparation process of 2-amino-4-acetyl aminoanisole. The preparation process comprises the following steps of (1) taking methanol as a solvent and 2,4-dimitroanisole as a raw material, introducing hydrogen to perform catalytic hydrogenation reduction reaction in the presence of a catalyst; (2) performing solid-liquid separation, and recovering the catalyst; (3) adding acetic anhydride to perform acetylation reaction; (4) recovering methanol which is recycled as a solvent for follow-up hydrogenation reduction; (5) performing reduced pressure distillation to recover acetic acid; (6) performing cooling crystallization to obtain a 2-amino-4-acetyl aminoanisole product.

Description

technical field [0001] The invention relates to the field of preparation of chemicals, in particular to a preparation process of 2-amino-4-acetamidoanisole. Background technique [0002] At present, the types of disperse dyes produced in my country are relatively complete, including high-energy type, medium-energy type, fast dyeing type, etc., with more than 150 varieties, and almost all large-tonnage varieties produced abroad are produced in my country. At present, there are 7 companies with an annual output exceeding 10,000 tons, namely, disperse dark blue H-GL, disperse blue EX-SF300%, disperse ruby ​​S-2GFL, disperse yellow brown S-2RFL, disperse red 3B / FB, disperse blue 2BLN and Disperse black EX-SF300%. Even so, many dyes are subject to the production of intermediates. For example, disperse dark blue H-GL is subject to the production of raw material 2-amino-4-acetamidoanisole, which leads to high production costs and affects the competitiveness of products in the inte...

Claims

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Application Information

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IPC IPC(8): C07C233/43C07C231/02
CPCY02P20/584
Inventor 祝梓琦
Owner SHANGHAI ZONGXING CHEM TECH CO LTD
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