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Preparation method of double-terminated polysulfone

A technology of double end-capping polymerization and end-capping agent, applied in the field of polymer materials, can solve the problems of flammability and explosion, easy to depolymerize, and difficult to remove end-capping agent.

Active Publication Date: 2021-09-14
FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the relatively backward domestic technical level, the appearance of polysulfone resin is poor, the light transmittance is low, the yellowness is high, and the crystallinity is high. In most cases, it is unacceptable in the actual application process. This problem has become Limits its development in color and appearance sensitive applications
Different end groups of resins have different heat resistance, for example, the heat resistance of phenolic hydroxyl end groups is lower than that of chlorine end groups, and phenolic hydroxyl groups are prone to oxidation under high temperature and aerobic conditions, resulting in yellowing of the resin and a decrease in color grade
[0003] Therefore, using an end-capping agent has become an effective method to solve this problem. Most of the existing patents use methyl chloride as an end-capping agent. Explosive, toxic gas, more dangerous
Some patents use asymmetric aromatic ketone derivatives as end-capping agents, although it has a more obvious effect on controlling molecular weight, but this end-capping agent is difficult to remove, which affects the performance of polysulfone
There are also patents using monochlorosulfone as the end-capping agent for polysulfone polymerization. Although monochlorosulfone has a faster reaction speed, monochlorosulfone is not easy to obtain and prone to depolymerization, which affects the later processing and use of polymers.

Method used

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  • Preparation method of double-terminated polysulfone
  • Preparation method of double-terminated polysulfone
  • Preparation method of double-terminated polysulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] With condensing, N 2 4.34Kg bisphenol A, 5.74Kg 4,4'-dichlorodiphenylsulfone and 2.90Kg Kg 2 CO 3 Add 47L of N,N-dimethylacetamide, gradually raise the temperature from room temperature to 120°C, add p-hydroxyacetophenone according to the water content in the reaction system, test the water content of the reaction system in the first 1h to 1.0235%, the reaction process Add 6.09g of p-hydroxyacetophenone, 2-3h test reaction system water content is 0.44568%, need to add 3.43g of p-hydroxyacetophenone, 3-4h test reaction system water content is 0.29324%, need to add p-hydroxyacetate Acetophenone 0.90 g. At the same time, during the reaction process, the effluent was produced at a rate of 5 L / h for 4 hours (the water content in the final produced solution was less than 0.5%), and the temperature was continued to rise to 160°C for 6 hours, and then the concentration of 1.8mol / 5 L of N,N-dimethylacetamide solution of p-aminophenol (completely added in half an hour). Add ...

Embodiment 2

[0040] With condensing, N 2 4.34Kg bisphenol A, 5.74Kg 4,4'-dichlorodiphenylsulfone and 2.90Kg Kg 2 CO 3 Add 47L of N,N-dimethylacetamide, gradually raise the temperature from room temperature to 120°C, add p-nitrophenol according to the water content in the reaction system, test the water content of the reaction system in the first 1h to 1.13400%, during the reaction process Add 5.55g of p-nitrophenol, 2-3h test reaction system water content 0.53251%, need to add 3.64g p-nitrophenol, 3-4h test reaction system water content is 0.30511%, need to add p-nitrophenol 1.38 g. At the same time, during the reaction process, the effluent was produced at a rate of 5 L / h for 4 hours (the water content in the final produced solution was less than 0.5%), and the temperature was continued to rise to 160°C for 6 hours, and then the concentration of 1.8mol / 5L of N,N-dimethylacetamide solution of L-p-aminophenol (completely added in half an hour). Add 15L of N,N-dimethylacetamide to dilut...

Embodiment 3

[0042] With condensing, N 2 4.34Kg bisphenol A, 5.74Kg 4,4'-dichlorodiphenylsulfone and 2.90Kg Kg 2 CO 3 Add 47L of N,N-dimethylacetamide, gradually raise the temperature from room temperature to 120°C, add p-hydroxybenzenesulfonic acid according to the water content in the reaction system, test the water content of the reaction system in the first 1h to 1.03460%, the reaction process Add 7.70g of p-hydroxybenzenesulfonic acid, 2-3h test reaction system water content is 0.48921%, need to add 4.14g p-hydroxybenzenesulfonic acid, 3-4h test reaction system water content is 0.28911%, need to add p-hydroxybenzenesulfonic acid Benzenesulfonic acid 1.52g. At the same time, during the reaction process, the effluent was produced at a rate of 5 L / h for 4 hours (the water content in the final produced solution was less than 0.5%), and the temperature was continued to rise to 160°C for 6 hours, and then the concentration of 1.8mol / L N-(4-hydroxyphenyl)acetamide in N,N-dimethylacetamid...

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Abstract

The invention belongs to the technical field of high polymer materials, and particularly relates to a preparation method of double-terminated polysulfone, thepreparation method comprises the following steps: taking bisphenol A and 4, 4 '-dichlorodiphenyl sulfone as reaction monomers, adding an end-capping reagent A with activity lower than that of the bisphenol A, a salt-forming agent and a solvent for reaction until the molecular weight reaches the target molecular weight, adding an end-capping reagent B with activity higher than that of the bisphenol A for continuous reaction, and after the reaction is finished, carrying out post-treatment to obtain the double-terminated polysulfone. The end-capping reagent A with activity lower than that of bisphenol A is added in the early stage of the reaction to reduce the low molecular weight polymer part in the final product so that the mechanical property, heat resistance, thermal stability and other properties of the product are improved. When the reaction is about to be finished, the end-capping reagent B with higher activity than bisphenol A is added so that the molecular weight is controlled through rapid end capping, the performance of products in different batches can be more stable, and the method is more suitable for the field of preparation of hollow fiber membranes.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of double-terminated polysulfone. Background technique [0002] Polysulfone resin is a thermoplastic engineering plastic that appeared after the mid-1960s. It is a non-crystalline polymer compound containing sulfone groups and aromatic nuclei in the main molecular chain. Polysulfone generally includes three types of bisphenol A polysulfone, polyphenylsulfone and polyethersulfone. Bisphenol A polysulfone and polyethersulfone in polysulfone are widely used because of their good thermal stability and dimensional stability, hydrolysis resistance, radiation resistance, and flame resistance. However, due to the relatively backward domestic technical level, the appearance of polysulfone resin is poor, the light transmittance is low, the yellowness is high, and the crystallinity is high. In most cases, it is unacceptable in the actual applicati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/23
CPCC08G75/23
Inventor 史碧波王敏廖广明
Owner FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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