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Method for preparing 3,3-diaminodiphenyl sulphone

A technology of diaminodiphenylsulfone and dinitrodiphenylsulfone, which is applied in 3 fields, can solve the problems of high impurity content, low purity, and low product yield, so as to improve utilization rate, increase selectivity, and reduce cost Effect

Active Publication Date: 2008-08-27
HEBEI JIANXIN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The 3,3-diaminodiphenylsulfone prepared by the current preparation method of 3,3-diaminodiphenylsulfone not only contains high amount of impurities, but also has low purity, and the reaction is not complete in the preparation process, and the product yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 280g of water, 89.8g of iron powder, and 20g of hydrochloric acid into a 1000ml reaction vessel, then raise the temperature to 90°C, then add 300g of sulfolane, and then slowly add 125g of 3,3-dinitrodiphenylsulfone to react for 2 to 3 hours. Then add sodium hydroxide to make the solution alkaline, PH = 9-10, precipitate the iron sludge, filter to remove the iron sludge, and obtain a light yellow filtrate, add activated carbon, decolorize at 80 ° C ~ 100 ° C, filter the activated carbon After separation, the reaction solution was cooled to 20°C to crystallize, suction filtered, and dried to obtain 73 g of white crystal 3,3-diaminodiphenylsulfone with a yield of 73%.

Embodiment 2

[0022] Add 300g of water, 134.4g of iron powder and 25g of hydrochloric acid into a 1000ml reaction vessel, then raise the temperature to 90°C, then add 300g of sulfolane, then slowly add 125g of 3,3-dinitrodiphenylsulfone to react for 2 to 3 hours , then add sodium hydroxide to make the solution alkaline, PH = 9-10, precipitate the iron sludge, remove the iron sludge by filtration, and obtain a light yellow filtrate, add activated carbon, decolorize at 80 ° C ~ 100 ° C, filter Activated carbon was separated, and the reaction solution was cooled to 20°C to crystallize, suction filtered, and dried to obtain 81 g of white crystal 3,3-diaminodiphenylsulfone with a yield of 81%.

Embodiment 3

[0024] Add 300g of water, 120g of iron powder, and 25g of hydrochloric acid into a 1000ml reaction vessel, then raise the temperature to 90°C, then add 300g of sulfolane, and then slowly add 125g of 3,3-dinitrodiphenylsulfone to react for 2 to 3 hours. Then add sodium hydroxide to make the solution alkaline PH = 9~10, precipitate the iron sludge, remove the iron sludge by filtration, and obtain a light yellow filtrate, add activated carbon to decolorize at 80°C~100°C, filter to separate the activated carbon, and react The solution was cooled to 20°C to crystallize, suction filtered, and dried to obtain 77 g of white crystal 3,3-diaminodiphenylsulfone with a yield of 77%.

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PUM

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Abstract

The invention relates to a preparation method of 3, 3-diaminodiphenylsulfone, which comprises adding iron powder with solvent in weak acid property, to reduce 3, 3-dinitrodiphenylsulfone into 3, 3-diaminodiphenylsulfone. The inventive method is beneficial for reaction and the reaction is complete, the invention processes purification after the reaction to obtain high-purity white crystal, the mother liquor is deposited, depressurized and distilled to recover solvent for reuse. In the reaction, sulfolane solvent can be added into the reaction to shorten the reaction time to 2-6h, thereby improving reaction selectivity, and sulfolane can be circulated in the preparation while the loss is 5%, to improve solvent utilization and reduce cost.

Description

technical field [0001] The invention relates to a preparation method of 3,3-diaminodiphenyl sulfone. Background technique [0002] 3,3-Diaminodiphenyl sulfone is an important monomer for the synthesis of polysulfonamide fiber. Polysulfonamide fiber (Polysulfonamide fiber) is referred to as polysulfonamide fiber (PSA). SO 2-) aromatic polyamide fibers, which are polycondensed from 4, 4' diaminodiphenyl sulfone, 3, 3' diamino diphenyl sulfone and terephthaloyl chloride low-temperature solution, formed by wet spinning, high temperature Made by drawing. The fiber is light beige and lustrous, the fiber strength is 3.0-4.5g / d, the elongation is 20-25%, the initial modulus is 760kg / mm2, and the specific gravity is 1.416g / cm3. The para-position has a meta-position structure, and the macromolecule is connected with a sulfone group, so it has heat resistance and flame resistance. After heating in hot air at 300°C for 100 hours, the loss of strength is less than 5%, and it also has g...

Claims

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Application Information

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IPC IPC(8): C07C317/36C07C315/04
Inventor 齐树栋朱守琛朱秀全
Owner HEBEI JIANXIN CHEM IND CO LTD
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