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Clean production method of p-anisidine

A technology of p-aminoanisole and p-nitroanisole, which is applied in the field of clean production of p-aminoanisole, can solve the problems of increased methanol distillation volume, increased energy consumption, and high energy consumption, and achieves simple operation, Reduce high salt and high COD wastewater, high yield and high purity effect

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

[0005] Although this method can significantly reduce the TOC of wastewater, it still has the following disadvantages: 1. The low TOC wastewater produced by it contains a large amount of sodium chloride, which needs to be evaporated and crystallized to obtain industrial grade sodium chloride, and the energy consumption is relatively high; 2. A large amount of resin is used in the treatment process, which leads to high cost; 3. In both reaction processes, methanol needs to be distilled once, resulting in an increase in the amount of methanol distillation and a corresponding increase in energy consumption

Method used

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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 to carry out contact reaction. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 6 hours, wherein the purity of p-nitroanisole is 97.2%.

[0023] Then the reaction product is filtered to obtain p-nitroanisole solution and filter cake. The filter cake is washed with methanol and dried to obtain sodium chloride, the content of which is more than 99%, reaching the industrial product standard. The resulting p-nitroanisole solution was distilled to remove about 300 g of methanol, then the material was...

Embodiment 2

[0026] 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 to carry out contact reaction. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 6 hours, wherein the purity of p-nitroanisole is 97.5%.

[0027] Then the reaction product is filtered to obtain p-nitroanisole solution and filter cake. The filter cake is washed with methanol and dried to obtain sodium chloride, the content of which is more than 99%, reaching the industrial product standard. The obtained p-nitroanisole solution was distilled to distill out about 400g of methanol, then the material ...

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Abstract

The invention discloses a clean production method of p-anisidine. The clean production method comprises the following steps of (1) enabling nitrochlorobenzene, sodium hydroxide and methanol to be subjected to an etherification reaction so as to obtain etherification reaction liquid; (2) directly filtering the etherification reaction liquid obtained in the step (1) to obtain a filtrate and filter cakes, washing the filter cakes with the methanol, drying the washed filter cakes to obtain industrial-grade sodium chloride, and distilling the filtrate so as to obtain p-nitroanisole concentration liquid; and (3) under the condition that a hydrogenation catalyst exists, enabling the p-nitroanisole concentration liquid obtained in the step (2) to be subjected to a hydrogenation reduction reaction in the hydrogen atmosphere, and after the reaction is completed, performing after-treatment so as to obtain the p-anisidine. According to the clean production method, after the etherification reaction is finished, direction filtration is performed so that the sodium chloride is removed, then concentration treatment is performed on the etherification reaction liquid, the hydrogenation reaction is directly performed, the operation is simple and convenient, and the yield and the purity of the obtained product are high.

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-aminoanisole. 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. In the dye industry, blue salt VB, bay red base GP, naphthol AS-SG, AS-RL, vat red are mainly synthesized, and p-aminoanisole can be used to synthesize 2-amino-4-acetamidoanisole. The compound is an important raw material for disperse dyes, and can be used to synthesize a series of disperse dyes, such as C.I. disperse blue 79, 226, 301, disperse violet 58, disperse navy blue S-2GL, etc.; it is mainly used in the synthesis of adipine and primaquine in the pharmaceutical i...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C217/84
CPCC07C201/12C07C213/02C07C217/84C07C205/37
Inventor 阮光栋章文刚高立江陆皝明
Owner ZHEJIANG RUNTU INST
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