Tech. of preparing 2-amino-4-acetamido methyl-phenoxide

A technology of acetamidoanisole and amino group, applied in the field of preparing 2-amino-4-acetamidoanisole, can solve the problems of serious environmental pollution and high process cost, achieve high product purity, improve operating environment and reduce losses Effect

Inactive Publication Date: 2008-02-13
CHANGZHOU JIASEN CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This production process mainly has the following disadvantages: the total yield of the above-mentioned acylation, nitration and reduction three-step reaction is only about 76%, and the production of raw material p-aminoanisole adopts traditional nitration process, alkali sulfide reduction and iron powder Reduction will produce a large number of three wastes that are difficult to deal with. Its main three wastes are acidic wastewater, washing water, reduced iron sludge, washing water, alkali sulfide reduction wastewater in p-aminoanisole and phenolic wastewater in etherification
Therefore, the production of 2-amino-4-acetylaminoanisole has always been a difficult problem in the dye industry. This process has high cost and serious environmental pollution.

Method used

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  • Tech. of preparing 2-amino-4-acetamido methyl-phenoxide
  • Tech. of preparing 2-amino-4-acetamido methyl-phenoxide
  • Tech. of preparing 2-amino-4-acetamido methyl-phenoxide

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Embodiment 1

[0032] A kind of technique for preparing 2-amino-4-acetamidoanisole, described process step is as follows:

[0033] (1). Catalytic hydrogenation reduction reaction, using methanol as a solvent, add 2-4 dinitroanisole to the catalytic hydrogenation reduction reactor tank reactor with Raney-Ni as a catalyst, the amount of catalyst is nitro 2.0% of the material, the catalyst particle size is 5.0mm, and then hydrogen is introduced into the stirred tank reactor. The reactor is equipped with a supporting controller, which can display or control the reaction temperature, pressure and stirring speed. For the hydrogen reduction reaction, the temperature is controlled at 120°C, the reaction time is 4 hours, and the operating pressure is 4MPa. During the reaction, the temperature should be controlled to prevent the occurrence of overheating.

[0034] (2). Solid-liquid separation. After the catalytic hydrogenation reduction reaction is completed, solid-liquid separation is carried out aft...

Embodiment 2

[0040] A kind of technique for preparing 2-amino-4-acetamidoanisole, described process step is as follows:

[0041](1). Catalytic hydrogenation reduction reaction, using methanol as a solvent, add 2-4 dinitroanisole to the catalytic hydrogenation reduction reactor tank reactor with Raney-Ni as a catalyst, the amount of catalyst is nitro 4.8% of the material, the catalyst particle size is 9.5mm, and then hydrogen is introduced into the stirred tank reactor. The reactor is equipped with a matching controller, which can display or control the reaction temperature, pressure and stirring speed. For the hydrogen reduction reaction, the temperature is controlled at 180°C during the reaction, the reaction time is 1h, and the operating pressure is 6MPa. During the reaction, the temperature must be controlled to prevent the occurrence of overheating.

[0042] (2). Solid-liquid separation. After the catalytic hydrogenation reduction reaction is completed, solid-liquid separation is carri...

Embodiment 3

[0048] A kind of technique for preparing 2-amino-4-acetamidoanisole, described process step is as follows:

[0049] (1). Catalytic hydrogenation reduction reaction, using methanol as a solvent, add 2-4 dinitroanisole to the catalytic hydrogenation reduction reactor tank reactor with Raney-Ni as a catalyst, the amount of catalyst is nitro 0.5% of the material, the catalyst particle size is 1.0mm, and then hydrogen is introduced into the stirred tank reactor. The reactor is equipped with a supporting controller, which can display or control the reaction temperature, pressure and stirring speed. For the hydrogen reduction reaction, the temperature is controlled at 140°C, the reaction time is 9 hours, and the operating pressure is 2.4MPa. During the reaction, the temperature must be controlled to prevent the occurrence of overheating.

[0050] (2). Solid-liquid separation. After the catalytic hydrogenation reduction reaction is completed, solid-liquid separation is carried out aft...

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Abstract

A process for preparing 2-amino-4-acetamino phenylmether includes such steps as catalytic hydroreducing reaction between methanol, 2,4-dinitro phenylmether and catalyst, solid-liquid separation, recovering catalyst, adding acid binding agent and the methanol solution of acetic anhydride, acelating reaction, cooling while crystallizing, filtering to obtain filtered cake recrystallizing in methanol, and separation.

Description

technical field [0001] The invention relates to a process for preparing 2-amino-4-acetamidoanisole, which belongs to the technical field of fine chemicals. Background technique [0002] 2-Amino-4-acetylaminoanisole, its English name is 4-Acetamino-2-aminoanisol, its molecular formula is C 9 h 12 N 2 o 2 Its molecular weight is 180.21, and its chemical molecular structure formula is: [0003] [0004] 2-Amino-4-acetamidoanisole is a white solid crystal with a melting point of 116°C to 118°C. It is an important intermediate for the production of dark varieties of disperse dyes (blue). Disperse dyes are the largest of the seven categories of dyes, with an annual output of 300,000 tons of finished products worldwide, while dark varieties account for 70% of the first class of dyes, and 90% of the coupling components in disperse dyes use aniline, 2-amino-4- Acetaminoanisole and m-acetamidoaniline are raw materials, wherein 2-amino-4-acetamidoanisole accounts for more than ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/07C07C231/02
Inventor 许文林段玉辉刘学谦
Owner CHANGZHOU JIASEN CHEM
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