Method for preparing aminodiphenyl ether by p-nitrchlorobenzene serving as raw material

A technology of p-nitrochlorobenzene and aminophenyl ether, which is applied in the field of preparation of p-aminophenyl ether, can solve problems such as equipment corrosion, difficult recovery of reaction heat, and difficulty in product separation, and achieves fewer by-products, simple operation, and high purity Effect

Active Publication Date: 2018-04-17
JIANGSU ZHONGDAN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has disadvantages such as huge equipment, difficult recovery of reaction heat, large consumption of iron powder, serious environmental pollutio

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1) Etherification reaction: Add 500kg of methanol to the reaction kettle, add 500kg of p-nitrochlorobenzene and 0.5kg of hexadecyldimethylbenzyl ammonium chloride catalyst, start stirring and heat to 55 ° C, and then add to the reaction 100kg of sodium hydroxide solution and 0.05kg of hydrogen peroxide were added dropwise, and the reaction was detected by a high-efficiency gas chromatograph to finally obtain the etherified product p-nitroanisole;

[0041] 2) cooling the etherified product in step 1) to room temperature, separating the oil and water phases, removing the organic phase and washing with water, and distilling the washed organic phase under reduced pressure to obtain etherified oil;

[0042] 3) Catalytic hydrogenation reaction: add 500kg methanol, the etherified oil obtained in step 2), and 10kg Raney nickel into the autoclave, heat and stir after replacing the hydrogen, the heating temperature is 80°C, and use a high-efficiency gas chromatograph to detect the...

Embodiment 2

[0046] 1) Etherification reaction: Add 500kg of ethanol to the reaction kettle, add 500kg of p-nitrochlorobenzene and 7.5kg of cetyldimethylbenzyl ammonium chloride catalyst, start stirring and heat to 65 ° C, and then add to the reaction 110kg of sodium hydroxide solution and 0.5kg of hydrogen peroxide were added dropwise, and the reaction was detected by a high-efficiency gas chromatograph to finally obtain the etherified product p-nitrophenetole;

[0047] 2) cooling the etherified product in step 1) to room temperature, separating the oil and water phases, removing the organic phase and washing with water, and distilling the washed organic phase under reduced pressure to obtain etherified oil;

[0048] 3) Catalytic hydrogenation reaction: add 500kg of methanol, the etherified oil obtained in step 2) and 12kg of Raney nickel to the autoclave, heat and stir after replacing the hydrogen, the heating temperature is 100°C, and use a high-efficiency gas chromatograph to detect the...

Embodiment 3

[0052] 1) Etherification reaction: Add 500kg of methanol into the reaction kettle, add 500kg of p-nitrochlorobenzene and 2.5kg of cetyldimethylbenzyl ammonium chloride catalyst, start stirring and heat to 60 ° C, and then add to the reaction 100kg of sodium hydroxide solution and 0.2kg of hydrogen peroxide were added dropwise, and the reaction was detected by a high-efficiency gas chromatograph to finally obtain the etherified product p-nitroanisole;

[0053] 2) cooling the etherified product in step 1) to room temperature, separating the oil and water phases, removing the organic phase and washing with water, and distilling the washed organic phase under reduced pressure to obtain etherified oil;

[0054] 3) Catalytic hydrogenation reaction: add 500kg of toluene, the etherified oil obtained in step 2), and 10kg of Raney nickel into the autoclave, heat and stir after replacing the hydrogen, the heating temperature is 90°C, and use a high-efficiency gas chromatograph to detect t...

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Abstract

The invention relates to a preparation method of aminodiphenyl ether, in particular to a method for preparing aminodiphenyl ether by p-nitrchlorobenzene serving as a raw material. The method includesthe steps: etherification reaction; oil-water phase separation of etherification products; catalytic hydrogenation reaction; filtering; rectification and the like. The method for preparing the aminodiphenyl ether by the p-nitrchlorobenzene serving as the raw material is clean, environmentally friendly, simple to operate, low in energy consumption and pollution-free in environment, and the aminodiphenyl ether prepared by the method is high in yield and purity. According to the method for preparing the aminodiphenyl ether by the p-nitrchlorobenzene serving as the raw material, phase transfer catalysts are less in dosage, and fewer by-products are generated in the reaction process.

Description

technical field [0001] The invention relates to a preparation method of p-aminophenyl ether, in particular to a method for preparing p-aminophenyl ether by using p-nitrochlorobenzene as a raw material. Background technique [0002] p-Aminoanisole is a traditional dye and pharmaceutical intermediate. In the dye industry, it can produce ice dyes, disperse dyes, vat dyes, reactive dyes and various chromophores, naphthols, etc.; it is mainly used in the pharmaceutical industry Synthesize traditional medicines such as adipine and indomethacin. p-Aminophenetole is an important intermediate of dyes, medicines, pesticides, food additives and rubber additives. P-aminophenethyl ether is also widely used in medicine, and can be used to produce phenacetin, celiprolol, Anboxi, mesalazine and rivanol, etc. [0003] The synthetic method of p-aminophenyl ether produced and researched at home and abroad mainly contains following 3 kinds at present: 1) nitrobenzene method, and nitrobenzene ...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C201/16C07C205/37C07C213/02C07C213/10C07C217/84
CPCY02P20/584C07C201/12C07C201/16C07C213/02C07C213/10C07C205/37C07C217/84
Inventor 褚伟华顾杰任云华叶娟
Owner JIANGSU ZHONGDAN CHEM TECH
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