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Method for preparing 2-amino-4-nitrophenol through liquid catalytic hydrogenation

A nitrophenol, liquid-phase catalysis technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problem of reducing production safety and cleanliness, increasing equipment investment and energy consumption, and increasing processing Process and other issues, to achieve important economic value and environmental significance, reduce equipment investment and energy consumption, reduce the effect of cost of use

Inactive Publication Date: 2016-05-11
SHENYANG RES INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] In the above-mentioned published patents, the preparation of 2-amino-4-nitrophenol by catalytic hydrogenation has largely solved the problem of serious environmental pollution caused by the original alkali sulfide reduction process, whether using Raney nickel as a catalyst or using When palladium carbon is used as a catalyst, alcohols need to be added as solvents. However, the use of alcohol solvents increases the post-treatment process of product separation and solvent recovery, resulting in increased equipment investment and energy consumption, especially for low-boiling, volatile alcohols. Solvents also greatly reduce the safety and cleanliness of production

Method used

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Embodiment 1

[0033] The quality of palladium in the palladium charcoal catalyst of the present embodiment is 5% of the quality of the activated carbon carrier, and the quality of the transition metal is 0.1% of the quality of the activated carbon carrier; the activated carbon carrier is an activated carbon carrier treated with sulfide; the transition metal is iron ;

[0034] The preparation method of described palladium carbon catalyst comprises the following steps:

[0035] Step 1. Dissolve 0.1g of sodium sulfide in water to form an aqueous solution of sodium sulfide with a mass concentration of 0.1%, and then prepare a solution with a particle size of 300 mesh and a specific surface area of ​​950m 2 / g of coconut shell charcoal soaked in sodium sulfide solution, stirred at 50°C for 3 hours, filtered and dried to obtain activated carbon carrier;

[0036] Step 2, the activated carbon carrier described in 24.0g step 1 is 10% Na with 300mL mass concentration 2 CO 3 The aqueous solution is...

Embodiment 2

[0041] This embodiment is the same as Embodiment 1, except that the transition metal is cobalt, nickel, copper, zinc, chromium or cerium.

Embodiment 3

[0043]In a stainless steel high-pressure reactor with a volume of 500mL, add 300.0g of industrial grade 2,4-dinitrophenolate aqueous solution and 0.225g of 5% Pd / C catalyst with a mass concentration of 15.0%, close the reactor, and replace the nitrogen in the reactor with nitrogen. Air three times, then replace nitrogen with hydrogen three times and maintain the hydrogen pressure in the reactor, raise the temperature to 80°C, the reaction pressure is 1.0MPa, start stirring, the stirring rate is 800 rpm, constant temperature reaction 3.0h. Cool down to room temperature, stop stirring, evacuate the hydrogen in the kettle, open the kettle, take out the reaction solution, filter to separate the catalyst and the filtrate, adjust the pH value of the filtrate to 4.8 with dilute hydrochloric acid, and precipitate yellow crystals as 2-amino-4-nitrate Base phenol product, the purity of 2-amino-4-nitrophenol analyzed by liquid chromatography is 99.6%, and the yield is 96.5%.

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Abstract

The invention relates to a method for preparing 2-amino-4-nitrophenol, in particular to a method for preparing 2-amino-4-nitrophenol through liquid catalytic hydrogenation. 2,4-dinitrochlorobenzene is hydrolyzed to obtain industrial 2,4-dinitrochlorobenzene serving as a raw material, and 5 percent of Pd / C is used as a catalyst, so that the 2-amino-4-nitrophenol is prepared by performing catalytic hydrogenation on a liquid phase system. Compared with original sodium sulfide reduction, the liquid catalytic hydrogenation process disclosed by the invention has the advantages of low pollution, high yield and high quality; meanwhile, the catalytic hydrogenation system takes water serving as a solvent to replace an alcohol solvent which is low in boiling point and easy to volatilize, so that the problem of solvent recycling in the catalytic hydrogenation process is solved, and the safety of production is improved.

Description

technical field [0001] The invention relates to a method for preparing 2-amino-4-nitrophenol, in particular to a method for preparing 2-amino-4-nitrophenol by liquid-phase catalytic hydrogenation. Background technique [0002] 2-Amino-4-nitrophenol is an important dye and pharmaceutical intermediate, mainly used in acid mordant brown RH; neutral black BL, BRL, BGL, etc. [0003] The preparation methods of 2-amino-4-nitrophenol mainly include electrochemical reduction, chemical reduction and catalytic hydrogenation reduction. Due to the constraints of electrode materials, electrolytic equipment, cost and other factors, the electrochemical reduction method has been stuck in the research stage, and the product yield is only 53%, which cannot be industrialized. [0004] In industry, the traditional preparation process of 2-amino-4-nitrophenol is obtained by partially reducing 2,4-dinitrophenol with alkali sulfide under alkaline conditions. U.S. Patent US2464194 reports a metho...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C215/76
Inventor 尹荃闫海生任树杰喻滔李丽龚亚军刘冰曲旭坡陈二中
Owner SHENYANG RES INST OF CHEM IND
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