Method for preparing 2-amino-4-chlorodiphenyl oxide

A technology of chlorodiphenyl ether and amino, which is applied in the field of preparing 2-amino-4-chlorodiphenyl ether by reducing 2-nitro-4 chlorodiphenyl ether with hydrazine hydrate, which can solve the problem of high equipment requirements and harsh hydrogenation conditions , unfavorable industrial promotion and other issues, to achieve the effect of increasing reaction yield, improving conversion rate, and simple reaction equipment

Active Publication Date: 2016-12-07
ZHEJIANG RUNTU INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) Iron powder reduction method, the biggest disadvantage of this method is that it needs to use a large amount of iron powder, resulting in a large amount of iron sludge, serious pollution, and very unfriendly to the environment
[0007] (2) Catalytic hydrogenation method, this method is friendly to the environment and has no pollution to the three wastes. However, due to harsh hydrogenation conditions and high risk, the requirements for equipment are very high, and the one-time investment is large, which is not conducive to industrial promotion.

Method used

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  • Method for preparing 2-amino-4-chlorodiphenyl oxide

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Experimental program
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Effect test

Embodiment 1

[0028] In the reaction flask, add 2-nitro-4-chlorodiphenyl ether 30g, industrial alcohol 90mL, ferric chloride hexahydrate 5g, activated carbon 5g, stir and use 7g liquid caustic soda (mass percentage concentration is 30% sodium hydroxide aqueous solution ) adjust the pH value to 7.3, heat up to 80-90°C, slowly add 13g of hydrazine hydrate with a mass percentage concentration of 85% to the system under reflux, drop it in about 2 hours, continue to reflux for 3 hours, filter while it is hot, and recover the filtrate by distillation After alcohol, add water and stir for 30 minutes, stand still and separate liquid to obtain 24.85g of light brown oily product, 2-amino-4-chlorodiphenyl ether has a purity of 99.04%, a content of 98.65%, and a product yield of 92.82%.

Embodiment 2

[0030] In the reaction flask, add 2-nitro-4-chlorodiphenyl ether 30g, denatured alcohol 90mL, ferric chloride hexahydrate 5g, gac 5g, stir and adjust the pH value to 9.5 with 9g liquid caustic soda (30%), heat up to 80-90°C, slowly add 13g of hydrazine hydrate with a concentration of 85% to the system under reflux, and drop it in about 2 hours. Continue to reflux for 3 hours and then filter while it is hot. The liquid obtained 21.88g of a dark brown product, the purity of 2-amino-4-chlorodiphenyl ether was 94.74%, the content was 91.55%, and the product yield was 75.85%.

Embodiment 3

[0032] In the reaction flask, add 2-nitro-4-chlorodiphenyl ether 30g, technical alcohol 90mL, ferric chloride hexahydrate 5g, gac 5g, stir and adjust the pH value to 7.5 with 7g liquid caustic soda (30%), be warming up to 80-90°C, slowly add 12g of hydrazine hydrate with a concentration of 85% to the system under reflux, and drop it in about 2 hours. After continuing to reflux for 3 hours, filter while it is hot. After the filtrate is distilled to recover alcohol, add water and stir for 30 minutes. The liquid obtained 22.80 g of light brown product, the purity of 2-amino-4-chlorodiphenyl ether was 98.76%, the content was 95.77%, and the product yield was 82.27%.

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Abstract

The invention discloses a method for preparing 2-amino-4-chlorodiphenyl oxide. The method comprises the following steps: dispersing 2-amino-4-chlorodiphenyl oxide, ferric chloride hexahydrate and active carbon in ethanol, then adding alkali for adjusting the pH value to 7-9, under heating condition, dropping hydrazine hydrate for performing a reduction reaction, after the reaction is complete, and processing the material to obtain 2-amino-4-chlorodiphenyl oxide. The preparation method has the advantages of mild reaction condition, easy control, and simple reaction equipment, a catalyst and a solvent are repeatedly used, and the 2-amino-4-chlorodiphenyl oxide is friendly to environment, has the advantages of stable product quality, good purity, and high yield, and is in favor of realizing large-scale production.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for preparing 2-amino-4-chlorodiphenyl ether by reducing 2-nitro-4-chlorodiphenyl ether with hydrazine hydrate. Background technique [0002] 2-Amino-4-chlorodiphenyl ether (CAS: 93-67-4, 5-Chloro-2-phenoxyaniline, molecular weight: 219.67), the structural formula is as follows: [0003] [0004] 2-amino-4-chlorodiphenyl ether is an important acid dye intermediate, mainly used in the production of acid red 249, acid red 149, acid blue 128, etc. [0005] At present, 2-amino-4-chlorodiphenyl ether is generally prepared by reducing 2-nitro-4-chlorodiphenyl ether, and there are mainly the following two methods: [0006] (1) Iron powder reduction method. The biggest disadvantage of this method is that it needs to use a large amount of iron powder, which produces a large amount of iron sludge, which causes serious pollution and is very unfriendly to the environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/06C07C215/76
CPCY02P20/584C07C213/06C07C215/76
Inventor 顾高炜邬伟国赵国生任闻飞
Owner ZHEJIANG RUNTU INST
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