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A kind of 3,3'-diaminodiphenyl sulfone continuous synthesis method

A technology of diaminodiphenylsulfone and dinitrodiphenylsulfone, which is applied in the field of fine chemicals, can solve the problems of not meeting the requirements of aviation composite materials, unfavorable large-scale production, and low yield, and achieves easy washing, filtration and product separation , improve production capacity and equipment utilization, and overcome the effect of excessive iron ions

Active Publication Date: 2021-05-14
HEBEI JIANXIN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the disadvantage is that this method will produce a large amount of iron sludge that is difficult to handle, and the yield is not high, and it is easy to introduce iron ions, which cannot meet the requirements of aviation composite materials. In addition, batch production is not conducive to large-scale production Manufactured and meets modern safety standards

Method used

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  • A kind of 3,3'-diaminodiphenyl sulfone continuous synthesis method
  • A kind of 3,3'-diaminodiphenyl sulfone continuous synthesis method
  • A kind of 3,3'-diaminodiphenyl sulfone continuous synthesis method

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Effect test

Embodiment 1

[0030] Preparation of sodium disulfide reducing solution:

[0031] first to 5m 3 Add 3.4m 3of water, start stirring, and 1300kg of sodium sulfide (mass content is 60%) is added in batches in the first raw material preparation still, and then in the first raw material preparation still, add the solid sulfur of 310kg, in order to prevent the reaction system from generating The highly toxic hydrogen sulfide gas overflows and hurts employees. The system uses the induced draft fan to maintain a slight negative pressure in the first raw material preparation kettle, and at the same time the gas discharged by the induced draft fan is absorbed by spraying sodium hydroxide solution. The tail gas produced by the reaction is absorbed by the lye. The first raw material preparation kettle is slowly heated to 90°C, after the sodium sulfide and sulfur are completely dissolved, continue to keep warm for 1 hour, then cool the reaction system to 75°C, filter through the filter 2 while it is ho...

Embodiment 2

[0039] Preparation of sodium disulfide reducing solution:

[0040] first to 5m 3 Add 3.4m 3 of water, start stirring, and 1300kg of sodium sulfide (mass content is 60%) is added in batches in the first raw material preparation still, then in the first raw material preparation still, add the solid sulfur of 330kg, in order to prevent the reaction system from generating The highly toxic hydrogen sulfide gas overflows and hurts employees. The system uses the induced draft fan to maintain a slight negative pressure in the first raw material preparation kettle, and at the same time the gas discharged by the induced draft fan is absorbed by spraying sodium hydroxide solution. The tail gas produced by the reaction is absorbed by the lye. The first raw material preparation kettle is heated slowly to 95°C. After the sodium sulfide and sulfur are completely dissolved, continue to keep warm for 1.5 hours. Then, after the reaction system cools down to 75°C, it is filtered through the fi...

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Abstract

A 3,3'-diaminodiphenylsulfone continuous synthesis method comprises the following steps: a, preparation of sodium disulfide reducing solution; b, preparation of 3,3'-dinitrodiphenylsulfone dispersed turbid solution; c , pre-reduction reaction: the prepared sodium disulfide reducing solution and 3,3'-dinitrodiphenyl sulfone dispersed turbid solution are added to the reduction reaction kettle in a certain proportion, stirred and reacted for a certain period of time at a certain temperature; d, continuously Material and output: the prepared sodium disulfide reducing solution and 3,3′-dinitrodiphenyl sulfone dispersed turbid solution are continuously fed into the reduction reactor at a certain mass flow rate through a metering pump, and the reaction temperature is kept constant , the product enters the solid-liquid separator from the overflow port at the upper end of the side wall of the reduction reactor, and is separated to obtain 3,3'-diaminodiphenylsulfone product. The invention realizes the industrialized continuous reduction of 3,3'-dinitrodiphenylsulfone to prepare 3,3'-diaminodiphenylsulfone, and has simple operation, low cost, high product yield and less impurities.

Description

technical field [0001] The invention relates to a continuous synthesis method of 3,3'-diaminodiphenylsulfone, which belongs to the technical field of fine chemicals. Background technique [0002] 3,3'-diaminodiphenyl sulfone is an important monomer for the synthesis of polysulfone fiber and aerospace composite materials. Aramid sulfone fiber is formed by condensation of 3,3′-diaminodiphenylsulfone, 4,4′-diaminodiphenylsulfone and terephthaloyl chloride at low temperature. Aramid sulfone fiber is mainly used for protective clothing and insulation Materials and other aspects, such as space suits, special military uniforms, fire suits and other high temperature resistant products. In terms of insulation, it is mainly used for motor insulation and transformer insulation. Among them, insulating paper (H, F) grades is a main application aspect of polysulfone fiber materials. In addition, polysulfone fibers can also be made into honeycomb structure materials for aircraft interlaye...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/36C07C315/04C07C315/06
CPCC07C315/04C07C315/06C07C317/36
Inventor 刘佳伟朱秀全王成鹏李天天李书宇
Owner HEBEI JIANXIN CHEM IND CO LTD
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