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One-pot catalytic synthesis method for polycondensation of aromatic polyamide sulfonamide solution

A technology of solution polycondensation of aromatic polyamide sulfonamide, which is applied in the field of one-pot catalytic synthesis of aromatic polyamide sulfonamide solution polycondensation, which can solve the problems of difficulty, low activity, and restrictions on the industrial application of polyamide sulfonamide

Active Publication Date: 2020-12-11
庆阳职业技术学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of solution polymerization is mostly adopted, and the shortcoming of the polyamide sulfonamide polymer synthesized by diamine monomers containing sulfonamide bonds and bisacyl chloride monomers is that the preparation steps of diamine monomers containing sulfonamide bonds are cumbersome and the reaction The conditions are harsh, and at the same time, the diamine monomer containing sulfonamide bonds has low activity, and it is not easy to react with dichloro monomers to synthesize high molecular weight polyamide sulfonamide polymers; while fluorine-containing polyamide sulfonamide requires special reaction conditions and can be operated Poor stability, low molecular weight, low yield, high cost and other defects, which limit the performance and industrial application of polyamide sulfonamide

Method used

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  • One-pot catalytic synthesis method for polycondensation of aromatic polyamide sulfonamide solution
  • One-pot catalytic synthesis method for polycondensation of aromatic polyamide sulfonamide solution
  • One-pot catalytic synthesis method for polycondensation of aromatic polyamide sulfonamide solution

Examples

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Effect test

Embodiment 1

[0043] Example 1 One-pot catalytic synthesis method of aromatic polyamide sulfonamide solution polycondensation:

[0044] Under the protection of normal pressure and sufficient nitrogen, mix the aromatic diamine monomer, composite catalyst, and sulfolane, and stir until fully dissolved to obtain a mixed solution; add dropwise to the mixed solution three times at 0-8°C with an interval of 5 minutes between two times 3-Chlorosulfonylbenzoyl chloride monomer, after reacting for 25min, react at 27°C for 1h, then gradually raise the temperature to 60°C for 24h, until the solution becomes viscous. After the reaction is over, pour the viscous solution into deionized water while it is hot, and a white wire-like substance precipitates out, and then alternately wash it with boiled deionized water and absolute ethanol for 5 times, and the white precipitate is vacuum-dried at 100°C for 24 hours , to obtain the aromatic polyamide sulfonamide polymer with a yield of 93.82%.

[0045] Among ...

Embodiment 2

[0049] Example 2 One-pot catalytic synthesis method of aromatic polyamide sulfonamide solution polycondensation:

[0050] Under normal pressure and sufficient nitrogen protection, mix aromatic diamine monomers, composite catalysts, and N,N-dimethylacetamide, and stir until fully dissolved to obtain a mixed solution; divide in the mixed solution at 0-8°C Add 3-chlorosulfonylbenzoyl chloride monomer dropwise three times at intervals of 5 minutes, react for 45 minutes, then react at 30°C for 1 hour, then gradually raise the temperature to 70°C and react for 20 hours until the solution becomes viscous. After the reaction is over, pour the viscous solution into deionized water while it is hot, and a white wire-like substance precipitates out, and then alternately washes with boiled deionized water and absolute ethanol for 3 times, and the white precipitate is vacuum-dried at 100°C for 24 hours , to obtain the aromatic polyamide sulfonamide polymer with a yield of 88.92%.

[0051] ...

Embodiment 3

[0055] Example 3 One-pot catalytic synthesis method of aromatic polyamide sulfonamide solution polycondensation:

[0056] Under normal pressure and sufficient nitrogen protection, mix aromatic diamine monomers, composite catalysts, and N,N-dimethylformamide, stir until fully dissolved, and obtain a mixed solution; divide in the mixed solution at 0-8°C Add 3-chlorosulfonylbenzoyl chloride monomer dropwise three times at intervals of 5 minutes, react for 30 minutes, then react at 28°C for 1 hour, then gradually raise the temperature to 65°C and react for 22 hours until the solution becomes viscous. After the reaction is over, pour the viscous solution into deionized water while it is still hot, and a white stringy substance precipitates out, and then alternately wash it with boiled deionized water and absolute ethanol for 4 times, and the obtained white precipitate is vacuum-dried at 100°C for 24 hours , to obtain the aromatic polyamide sulfonamide polymer with a yield of 90.04%...

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Abstract

The invention relates to a one-pot catalytic synthesis method for polycondensation of an aromatic polyamide sulfonamide solution, which comprises the steps of under normal pressure and sufficient nitrogen protection, mixing an aromatic diamine monomer, a composite catalyst and a polar aprotic organic solvent, and stirring until the components are fully dissolved to obtain a mixed solution; dropwise adding a 3-chlorosulfonyl benzoyl chloride monomer into the mixed solution for three times at the temperature of 0-8 DEG C at an interval of 5min, reacting for 25-45min, then reacting for 1h at thetemperature of 27-30 DEG C, gradually heating to the temperature of 60-70 DEG C, reacting for 20-24h, alternately washing a product obtained after the reaction with boiled deionized water and absoluteethyl alcohol for 3-5 times in sequence, and drying in vacuum to obtain the aromatic polyamide sulfonamide polymer. The method is simple in process and easy to implement, and the obtained aromatic polyamide sulfonamide polymer has good thermal stability, friction performance and solvent resistance and can be used as a potential membrane material for reverse osmosis, ultrafiltration and the like and a solid lubrication and special engineering material.

Description

technical field [0001] The invention relates to the field of functional polymer materials, in particular to a one-pot catalytic synthesis method of aromatic polyamide sulfonamide solution polycondensation. Background technique [0002] Polyamide (PA), also commonly known as nylon, refers to a class of polymer materials containing amide groups in the repeating unit of the main chain. In 1931, it was developed and industrialized by W.H.Carother of the DuPont Central Research Institute in the United States. At the same time, it applied for the first polyamide patent U.S.Pat.2130948. Polyamide has excellent mechanical properties and electrical properties, as well as wear resistance, solvent resistance, oil resistance, self-lubricating properties and good processing performance. It is currently the preferred engineering material, and therefore many modified functional materials have been derived. Indispensable structural materials for industries such as electrical appliances, ae...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42
CPCC08G69/42
Inventor 刘利剑张绍印吴龑平曹强王程牛梦彪郭娜刘丽
Owner 庆阳职业技术学院
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