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Green synthesis method of p-aminophenetole

A technology for the green synthesis of p-aminophenethyl ether, which is applied in the preparation of aminohydroxyl compounds, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of environmental hazards, affecting product purity, and high yield, so as to improve product purity. , the environment and operators are safe and reliable, and the effect of reducing production costs

Inactive Publication Date: 2020-01-31
JIANGSU FENGHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] But there is following one or more shortcoming in above-mentioned synthesis method: 1, all need to use organic solvent methanol, ethanol as reaction medium, not only cause harm to a certain degree to surrounding environment, personnel; 2, solvents such as methanol and reduction Amino reaction generates amine toluene by-products, which affects product purity; therefore, it is necessary to improve the existing method for synthesizing p-aminophenetole, with less energy consumption and higher yield

Method used

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  • Green synthesis method of p-aminophenetole

Examples

Experimental program
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Effect test

Embodiment 1

[0020] First use nitrogen (<1MPa) to continuously purge the 5000L reduction reactor for 3 times, and discharge the purge gas through the vent pipe. Under the condition of no solvent, add 2000kg of p-nitrophenethyl ether into the reaction kettle, add 2kg of Raney nickel catalyst, use steam to raise the temperature to 80°C, feed hydrogen, and keep the heat and pressure (80~90°C, 1.5~2.5 MPa ) under the condition of hydrogenation reduction reaction for 6 hours. After the reaction, purging with nitrogen (<1MPa) continuously for 3 times, at 65°C, filter under normal pressure to recover the catalyst, and rectify the filtrate for 120 hours under negative pressure to obtain 1600kg of p-aminophenethyl ether, 20kg of o-aminophenethyl ether, Aminophenethyl ether 60kg, the distillation residue is handled by a qualified unit.

Embodiment 2

[0022] First use nitrogen (<1MPa) to continuously purge the 5000L reduction reactor for 3 times, and discharge the purge gas through the vent pipe. Under solvent-free conditions, add 2001kg of p-nitrophenethyl ether into the reaction kettle, add 4kg of Raney nickel catalyst, use steam to raise the temperature to 80°C, pass in hydrogen, and keep the temperature and pressure (80-90°C, 1.5-2.5 MPa ) under the condition of hydrogenation reduction reaction for 6 hours. After the reaction, purging with nitrogen (<1MPa) continuously for 3 times, at 65°C, filter under normal pressure to recover the catalyst, and rectify the filtrate for 120 hours under negative pressure to obtain 1610kg of p-aminophenethyl ether, 20kg of o-aminophenethyl ether, Aminophenetole 50kg, the distillation residue is handled by a qualified unit.

Embodiment 3

[0024] First use nitrogen (<1MPa) to continuously purge the 5000L reduction reactor for 3 times, and discharge the purge gas through the vent pipe. Add 2002kg of p-nitrophenethyl ether into the reaction kettle, add 2.5kg of Raney nickel catalyst, use steam to raise the temperature to 80°C, feed hydrogen, and carry out heating under the conditions of heat preservation and pressure (80-90°C, 1.5-2.5 MPa). The hydrogen reduction reaction was carried out for 6 hours. After the reaction, purging with nitrogen (<1MPa) continuously for 3 times, at 65°C, filter under normal pressure to recover the catalyst, and rectify the filtrate for 120 hours under negative pressure to obtain 1620kg of p-aminophenethyl ether, 20kg of o-aminophenethyl ether, Aminophenetole 40kg, the distillation residue is handled by a qualified unit.

[0025] The whole process of the present invention adopts solvent-free process conditions, which reduces the discharge of organic matter in the traditional productio...

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Abstract

The invention relates to a green synthesis method of p-aminophenetole, and belongs to the field of preparation methods of chemical products. The synthesis method mainly comprises the following steps:adding raw material p-nitrophenetole into a reduction reaction kettle, performing a hydrogenation reduction reaction under the conditions of no solvent and Raney nickel as a catalyst, after the reaction is finished, cooling, filtering at normal pressure to recover the catalyst, and performing negative-pressure rectification on filtrate to obtain p-aminophenetole. The solvent-free technological conditions are adopted in the whole process, and emission of organic matters in a traditional production process is reduced; the problem that solvents such as methanol are subjected to reaction with reduced amino to generate carbaryl by-products is solved, and the product purity is improved; compared with a conventional solvent method, the green synthesis method has the advantages of lower temperature and lower energy consumption, reduces the production cost, and facilitates energy conservation and emission reduction.

Description

technical field [0001] The invention belongs to the field of preparation methods of chemical products, in particular to a green synthesis method of p-aminophenethyl ether. Background technique [0002] p-aminophenethyl ether, colorless oily flammable liquid. Exposure to air and sunlight gradually turns red to brown. Insoluble in water, soluble in ether, ethanol, benzene and chloroform, etc., slightly alkaline, and soluble in inorganic acid solutions. Used in medicine and making dyes. It can be used in the production of rubber antioxidant AW, that is, 6-ethoxy-2,2,4-trimethyl-1,2-dihydroquinoline. It is also used in feed and food to prevent the oxidation and deterioration of fat and protein during storage, and it is also used for the preservation of vitamin A and vitamin E and other medicines. In medicine, it is used in the production of antipyretic and analgesic drug phenacetin, anti-tuberculosis and antiseptic drug Rivanol; it is also used in the preparation of naphthol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C217/84
CPCC07C213/02C07C217/84
Inventor 郑龙生方东张亮李付香
Owner JIANGSU FENGHUA CHEM IND
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