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Process for preparing phenetidine and amino phenol by using mixture of nitrophenetol and nitrophenol as raw materials

A technology of nitrophenetole and aminophenetole, which is applied in the field of preparation of aminophenetole and aniline, can solve the problems of high energy consumption in the production process, increased pre-treatment costs, and a large amount of process wastewater, and achieves low equipment corrosion and saves Effects of pretreatment steps and process safety

Active Publication Date: 2008-11-19
江苏仁欣化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, p-aminophenethyl ether, o-aminophenethyl ether and aniline are independent preparation processes and separation and refining processes. This traditional preparation process has the following disadvantages: since a single component is used as a raw material during preparation, the mixture raw materials need to be pre-prepared. In order to obtain the required single-component raw material, the pretreatment requires a lot of equipment and unit operations in the preparation process, which inevitably has the disadvantages of high energy consumption and high cost in the production process, and a large amount of process wastewater will be generated during the pretreatment process, causing serious Environmental pollution and loss of materials, such as the treatment of these waste water will greatly increase the cost
This process of using a single nitrophenetole as a raw material to prepare aminophenetole puts forward the following requirements for raw materials in the preparation process, which will inevitably lead to higher requirements for etherification reaction or pretreatment, thereby increasing the cost of pretreatment defect

Method used

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  • Process for preparing phenetidine and amino phenol by using mixture of nitrophenetol and nitrophenol as raw materials
  • Process for preparing phenetidine and amino phenol by using mixture of nitrophenetol and nitrophenol as raw materials
  • Process for preparing phenetidine and amino phenol by using mixture of nitrophenetol and nitrophenol as raw materials

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The main process equipment is: stirred tank reactor, blade filter device, solvent recovery device, continuous rectification tower.

[0030] A kind of technology that prepares aminophenetole and aniline with nitrophenetole and nitrochlorobenzene mixture as raw material, described process step is as follows:

[0031] (1) Catalytic hydrogenation and catalytic dechlorination reaction: In a stirred tank reactor for catalytic hydrogenation and catalytic dechlorination reduction, ethanol is used as a solvent, and a mixture of nitrophenethyl ether and nitrochlorobenzene is used as a raw material, and the raw material nitro The consumption ratio of phenetole and nitrochlorobenzene mixture and ethanol is 1g: 0.5ml, and described nitrophenetole is p-nitrophenetole and o-nitrophenetole, and described nitrochlorobenzene is o-nitro Chlorobenzene, m-nitrochlorobenzene and p-nitrochlorobenzene, the percentage by weight of various ingredients in the raw material mixture is 95.0% for nit...

Embodiment 2

[0036] The main process equipment is: stirred tank reactor, blade filter device, solvent recovery device, batch rectification tower.

[0037] A kind of technology that prepares aminophenetole and aniline with nitrophenetole and nitrochlorobenzene mixture as raw material, described process step is as follows:

[0038] (1) Catalytic hydrogenation and catalytic dechlorination reaction: In a stirred tank reactor for catalytic hydrogenation and catalytic dechlorination reduction, ethanol is used as a solvent, and a mixture of nitrophenethyl ether and nitrochlorobenzene is used as a raw material, and the raw material nitro The consumption ratio of phenetole and nitrochlorobenzene mixture and ethanol is 1g: 3ml, and described nitrophenetole is p-nitrophenetole and o-nitrophenetole, and described nitrochlorobenzene is o-nitrochloride Benzene and m-nitrochlorobenzene and p-nitrochlorobenzene, the percentage by weight of various components in the raw material mixture is 98.5% for nitrop...

Embodiment 3

[0043] The main process equipment is: stirred tank reactor, blade filter device, solvent recovery device, continuous rectification tower.

[0044] A kind of technology that prepares aminophenetole and aniline with nitrophenetole and nitrochlorobenzene mixture as raw material, described process step is as follows:

[0045] (1) Catalytic hydrogenation and catalytic dechlorination reaction: In a stirred tank reactor for catalytic hydrogenation and catalytic dechlorination reduction, ethanol is used as a solvent, and a mixture of nitrophenethyl ether and nitrochlorobenzene is used as a raw material, and the raw material nitro The consumption ratio of phenetole and nitrochlorobenzene mixture and ethanol is 1g: 3ml, and described nitrophenetole is p-nitrophenetole and o-nitrophenetole, and described nitrochlorobenzene is o-nitrochloride Benzene, m-nitrochlorobenzene and p-nitrochlorobenzene, the percentage by weight of various components in the raw material mixture is 96.0% for nitr...

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Abstract

The invention relates to a process for preparing phenetidine and aniline by taking a mixture of nitrophenetol and nitrochlorobenzene as a raw material. The process comprises the following steps that: (1) a step of the catalytic hydrogenation reaction and the catalytic dechlorination reaction, during which, ethanol is taken as a solvent, the mixture of the nitrophenetol and the nitrochlorobenzene is taken as the raw material, catalyst is added, hydrogen is aerated; (2) a step of the solid-liquid separation, during which, solid and liquid in the material obtained from the step (1) after the catalytic hydrogenation reaction and the catalytic dechlorination reaction are separated, a liquid phase comprises phenetidine, aniline, ethanol, hydrochloride and water and is utilized in the next step; (3) a step of the liquid-liquid separation, during which, the oil phase-water phase liquid-liquid separation is performed in the material obtained in the step (2), the phenetidine and aniline in the oil phase is utilized in the next step; (4) a step of distillation separation, during which, the distillation separation is performed in the oil phase to produce the products of para aminophenyl ethyl ether, o-phenetidineand aniline. The process for preparing the aminoanisole and the aniline has the advantages that: (1) the cost is low, the preliminary treatment step is saved, and the process is simple; (2) the process is clean, the energy consumption is low, and the 'three wastes' are little; (3) the purity of the product is high.

Description

technical field [0001] The invention relates to a process for preparing aminophenetole and aniline by using a mixture of nitrophenetole and nitrochlorobenzene as raw materials, and belongs to the technical field of fine chemicals. Background technique [0002] P-aminophenetole, o-aminophenetole and aniline are important organic intermediates. At present, it is mainly used for the preparation of ethyl vanillin. In addition, it is also used in the preparation of azo dyes, ice dyes, etc. p-Aminophenetole and o-Aminophenetole are widely used and are in great demand at home and abroad. Therefore, more and more attention has been paid to the synthesis of p-Aminophenetole and o-Aminophenetole. The traditional synthetic routes of p-aminophenetole and o-aminophenetole mainly include: (1) taking p-nitrophenol and o-nitrophenol as raw materials respectively, and carrying out ethoxylation reaction with bromoethane under phase transfer catalysis to generate p-nitrophenetole and o-nitr...

Claims

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Application Information

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IPC IPC(8): C07C211/46C07C217/84C07C209/36C07C213/02
Inventor 段玉辉
Owner 江苏仁欣化工股份有限公司
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