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Clean production method of paranitroanisole

A p-nitroanisole and clean production technology, 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, environmental pollution, etc., and achieve improvement Yield, the effect of achieving zero emissions

Active Publication Date: 2016-03-16
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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  • Clean production method of paranitroanisole

Examples

Experimental program
Comparison scheme
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 paranitroanisole. The method comprises the step that sodium hydroxide, para-nitrochlorobenzene and methanol react to produce the paranitroanisole, and the reaction refers to that a sodium hydroxide methanol solution is added to a para-nitrochlorobenzene methanol solution in batches under gradient temperature rise. Besides, the clean production method further comprises the step of treatment of a reaction product mixture: the reaction product mixture is distilled, water is added to a reaction kettle after distillation for washing, standing and layering, and the paranitroanisole is obtained from an organic phase. With the adoption of the method, on the premises that side products are turned into wealth and TOC in wastewater is treated to be lower than 20, the yield of the paranitroanisole can be significantly increased and can be higher than 96% particularly.

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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IPC IPC(8): C07C201/12C07C205/37
Inventor 章文刚高立江任闻飞
Owner ZHEJIANG RUNTU INST
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