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Method for preparing meta (beta-hydroxyethyl sulfuryl) nitrobenzene by catalytic hydrogenation

A hydroxyethyl sulfone group, catalytic hydrogenation technology, applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve the problems of large pollution and low yield in the reduction process, and achieve stable yield and environmental protection. The effect of low pollution and low cost

Inactive Publication Date: 2009-07-15
TIANJIN DEK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved in the present invention is that the reduction process of m-(β-hydroxyethyl sulfone) nitrobenzene has large pollution and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0027] a. Add m-(β-hydroxyethyl sulfone) nitrobenzene 170Kg in the autoclave, and add 340Kg of water, fully stir.

[0028] b. Add 3.4Kg Raney nickel catalyst.

[0029] c. Slowly raise the temperature to 100-105° C., pass hydrogen gas until the pressure in the kettle is 30-35 atmospheres, and keep the temperature for 4 hours.

[0030] Sampling and analysis yielded 134Kg of 100% m-(β-hydroxyethylsulfone) aniline, with a yield of 91.2%.

example 2

[0032] a. Add m-(β-hydroxyethyl sulfone) nitrobenzene 170Kg in the autoclave, and add 510Kg of water, fully stir.

[0033] b. Add 5.1Kg Raney nickel catalyst.

[0034] c. Slowly raise the temperature to 100-105° C., pass hydrogen gas until the pressure in the kettle is 30-35 atmospheres, and keep the temperature for 5 hours.

[0035] Sampling and analysis yielded 138Kg of 100% m-(β-hydroxyethylsulfone)aniline, with a yield of 93.9%.

example 3

[0037] a. Add m-(β-hydroxyethyl sulfone) nitrobenzene 170Kg in the autoclave, and add 680Kg of water, fully stir.

[0038] b. Add 6.8Kg Raney nickel catalyst.

[0039] c. Slowly raise the temperature to 100-105° C., pass hydrogen gas until the pressure in the kettle is 30-35 atmospheres, and keep the temperature for 6 hours.

[0040] Sampling and analysis yielded 135 Kg of 100% m-(β-hydroxyethylsulfone) aniline, with a yield of 91.9%.

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PUM

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Abstract

The invention provides a method for a special hydrogenation catalyst, ensuring yield of reduction products to achieve more than 90% and effectively reducing cost and environmental pollution. Catalytic hydrogenation of m (beta-hydroxyethyl sulfonyl)-nitrobenzene of the invention adopts water as solvent and uses raney nickel in catalytic reduction reaction, therefore, the cost is low and the environmental pollution is little.

Description

technical field [0001] The invention relates to a preparation method of a dye intermediate, in particular to a method for preparing m-(β-hydroxyethylsulfone) aniline by catalytic hydrogenation reduction of m-(β-hydroxyethylsulfone) nitrobenzene method. Background technique [0002] m-(β-hydroxyethyl sulfone) nitrobenzene is an important dye intermediate, which has a wide range of market applications. Ethylsulfone base) aniline, but its process pollution is large, and waste water and waste residue are not easy to handle. China has ordered to limit the production of this method, and the cost is high. At present, the general nitro catalytic hydrogenation reduction reaction uses the solvent method, that is, the material to be reduced is mixed with a solvent with good compatibility with it, and then put into an autoclave, adding a catalyst, and proceeding at a certain pressure and a certain temperature Catalytic hydrogenation reduction. The use of organic solvents leads to lo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/36C07C315/04
Inventor 张玉卿曹世川
Owner TIANJIN DEK CHEM