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A kind of cleaner production method of p-nitroanisole

A technology for p-nitroanisole and cleaner production, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large amount of by-products, large amount of waste water, and many by-products of hydrolysis, etc. Achieve the effect of improving yield and achieving zero emissions

Active Publication Date: 2018-01-12
ZHEJIANG RUNTU INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has low reaction yield, large amount of by-products, and no effective measures are taken to treat the high-salt and high chemical oxygen demand (COD) wastewater generated in the production process, causing serious pollution to the environment
Although there are a large number of literature reports at present, the synthesis of p-nitroanisole by phase transfer catalyst method is used to overcome the harsh reaction conditions of the existing process, many hydrolysis by-products, and large amounts of waste water. However, this method is not yet mature and cannot be carried out. large-scale industrial production

Method used

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  • A kind of cleaner production method of p-nitroanisole

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Add 204.4g of p-nitrochlorobenzene and 200g of methanol into a 1000mL autoclave, close the autoclave, slowly raise the temperature until the p-nitrochlorobenzene is basically dissolved, start stirring and continue to heat up to 80°C, and then start to oxidize 460mL of hydrogen Sodium methanol solution (the content of sodium hydroxide is 125g / L) is added in batches to p-nitrochlorinated benzyl alcohol solution for contact reaction, the dropping process is controlled as follows: add 150mL dropwise for about 1 hour; then continue to heat up to 85°C About 230 mL was added dropwise in about 2 hours; then the temperature was raised to 90-95°C, and the remaining sodium hydroxide methanol solution was added dropwise in about 1 hour. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 6 hours.

[0023] Then the obtained reaction product mixture is distilled to obtain gaseous methanol and a distillation substrate,...

Embodiment 2

[0027] Add 204.4g of p-nitrochlorobenzene and 115g of methanol into a 1000mL autoclave, close the autoclave, slowly raise the temperature until the p-nitrochlorobenzene is basically dissolved, start stirring and continue to heat up to 80°C, and then start to oxidize 430mL of hydrogen Sodium methanol solution (the content of sodium hydroxide is 155g / L) is added in batches to p-nitrochlorinated benzyl alcohol solution for contact reaction. The dropping process is controlled as follows: add 150mL dropwise for about 1 hour; then continue to heat up to 85°C Add 200 mL dropwise in about 2 hours; then raise the temperature to 90-95°C, and add the remaining methanolic sodium hydroxide solution dropwise in about 1 hour. Finally, continue to raise the temperature to 100-105° C. and keep it warm for the reaction, and reach the end of the reaction in about 4.5 hours.

[0028] Then the obtained reaction product mixture is distilled to obtain gaseous methanol and distillation bottoms, where...

Embodiment 3

[0032] Add 204.4g of p-nitrochlorobenzene and 150g of methanol into a 1000mL autoclave, close the autoclave, slowly raise the temperature until the p-nitrochlorobenzene is basically dissolved, start stirring and continue to heat up to 80°C, and then start to oxidize 440mL of hydrogen Sodium methanol solution (the content of sodium hydroxide is 140g / L) is added in batches to p-nitrochlorinated benzyl alcohol solution for contact reaction, the dropping process is controlled as follows: add 150mL dropwise for about 1 hour; then continue to heat up to 85°C Add 200 mL dropwise in about 2 hours; then raise the temperature to 90-95°C, and add the remaining methanolic sodium hydroxide solution dropwise in about 1 hour. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 5 hours.

[0033] Then the obtained reaction product mixture is distilled to obtain gaseous methanol and distillation bottoms, wherein, the gaseous met...

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Abstract

The invention provides a clean production method of p-nitroanisole, which comprises the step of reacting sodium hydroxide, p-nitrochlorinated benzene and methanol to obtain p-nitroanisole, and the reaction is carried out under gradient temperature rise The sodium hydroxide methanol solution was added in batches to the p-nitrochlorinated benzyl alcohol solution for reaction. In addition, the clean production method also includes the step of processing the reaction product mixture, including: distilling the reaction product mixture, adding water to the reactor for washing, standing, and layering after the distillation, and obtaining p-nitrobenzene from the organic phase. methyl ether. The method of the present invention can significantly improve the yield of p-nitroanisole under the premise of ensuring that the by-products are turned from waste to treasure, and the TOC of the waste water is treated below 20. Specifically, the yield of p-nitroanisole The rate can reach more than 96%.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a clean production method of p-nitroanisole. Background technique [0002] p-nitroanisole, also known as p-nitroanisole, is an important raw material for the synthesis of p-aminoanisole, which is an important intermediate for the synthesis of dyes. When used as dyes and pharmaceutical intermediates, it is mainly used to produce dyes such as p-aminoanisole, blue salt VB, maroon base GP, and naphthol AS. [0003] At present, the existing method for preparing p-nitroanisole is mainly to react p-nitrochlorobenzene, methanol, and solid sodium hydroxide in an autoclave at one time. However, this method has low reaction yield, large amount of by-products, and no effective measures are taken to treat the high-salt and high chemical oxygen demand (COD) wastewater generated in the production process, causing serious pollution to the environment. Although there...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/12C07C205/37
Inventor 章文刚高立江任闻飞
Owner ZHEJIANG RUNTU INST
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