Hyperbranched polysulfone with controllable branching degree and preparation method thereof

A technology of hyperbranched polymerization and degree of branching, which is applied in the field of polymer materials, can solve the problems of complex synthesis of polyphenol monomers, low resin molecular weight, and reduced melt viscosity, and achieve superior product performance, simple synthesis method, and melt Effect of Viscosity Reduction

Active Publication Date: 2020-07-14
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent document CN105330837 synthesized a star-shaped polysulfone resin by adopting aromatic polyphenol monomer, the melt viscosity of the material is greatly reduced, and the processability is

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0035] Example 1:

[0036] Add 50g polysulfone (molecular weight M W = 4×10 4 ) And 625 mL of dichloromethane, stir until the polysulfone is completely dissolved, add 150 mL of 1,4-dichloromethoxybutane and 7.5 mL of anhydrous tin tetrachloride, and react at 50°C for 5 hours. The product is precipitated with ethanol as a precipitating agent, and then repeatedly boiled and washed with ethanol and water, and dried at 40°C to obtain chloromethylated polysulfone. After oxygen-nitrogen combustion-Folhard method, the chlorine content is 2mmol / g.

[0037] Place a four-necked flask with water trap, condenser and mechanical stirring in an oil bath reactor, add 300mL of toluene, 45.66g of bisphenol A and 16g of solid sodium hydroxide to the flask in turn, and stir at 80℃ for 3h , Then heat to 110°C to reflux the toluene, collect the generated water with a water separator while stirring, and when the collected water reaches the theoretical value, distill off the toluene. The heating was sto...

Example Embodiment

[0038] Example 2:

[0039] For the preparation process of chloromethylated polysulfone, refer to Example 1. The reaction was carried out at 50° C. for 4 hours to obtain a chloromethylated polysulfone with a chlorine content of 1 mmol / g.

[0040] In a four-necked reaction flask with oil bath heating, stirrer, water separator and condenser, add 200mL o-xylene, 25.03g bisphenol S and 13.82g potassium carbonate powder in sequence, and heat up to 110℃ and stir for 4h , Then heat up to 150°C to evaporate part of the o-xylene, and finally heat up to 180°C to completely evaporate the o-xylene, stop heating and purge with nitrogen, and cool the system to 160°C. Weigh 28.72g 4,4'-dichlorodiphenylsulfone and dissolve it in 139.32g N,N-dimethylformamide, and mix 4,4'-dichlorodiphenylsulfone / N,N-diphenylsulfone Methylformamide solution and 0.46g KF were sequentially added to the system, purged with nitrogen, and the temperature was rapidly raised to 140°C, and reacted for 3 hours to obtain a v...

Example Embodiment

[0041] Example 3:

[0042] For the preparation process of chloromethylated polysulfone, refer to Example 1. The reaction was carried out at 50°C for 6.5 hours to obtain a chloromethylated polysulfone with a chlorine content of 3 mmol / g.

[0043] Put 1.5L ethylbenzene, 200.24g bisphenol F and 115.02g solid potassium hydroxide into a reactor equipped with temperature control, stirring and reflux water separator at one time, and heat up to 100℃ to react for 4 hours to make the system fully salt. Then the temperature is raised to 140°C to make the ethylbenzene reflux, and the generated water is collected with a water separator while stirring. When the collected water reaches the theoretical value, the azeotropic agent ethylbenzene is evaporated. The heating was stopped and purged with nitrogen, and the system was cooled to 120°C. Weigh 287.16g 4,4'-dichlorodiphenyl sulfone and dissolve it in 3.73Kg dimethyl sulfoxide, add 4,4'-dichlorodiphenyl sulfone / dimethyl sulfoxide solution and 0...

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Abstract

The invention discloses hyperbranched polysulfone with controllable branching degree and a preparation method thereof. The method comprises the following steps: 1) generating bisphenol salt from an organic bisphenol compound and a salt-forming agent in a non-water-soluble hydrocarbon solvent; 2) adding a solution of 4, 4'-dichlorodiphenyl sulfone/aprotic polar solvent into a bisphenol salt system,and carrying out condensation polymerization under the catalytic action of a condensation polymerization catalyst to generate linear polysulfone; 3) adding a chloromethylated polysulfone/aprotic polar solvent solution into the system, and reacting to generate hyperbranched polysulfone; and 4) separating out the product in a precipitation agent, and carrying out a post-treatment process to obtainhyperbranched polysulfone powder. Compared with a traditional method for preparing hyperbranched polysulfone, the method has the advantages that expensive polyfunctional monomers do not need to be adopted, so that the cost is greatly reduced; the molecular weight distribution of the obtained product is narrow, the gelation phenomenon is avoided, the branching degree can be controlled by selectingpolysulfones with different chloromethylation degrees, and the method is simple and easy to operate.

Description

technical field [0001] The invention relates to a preparation method of polysulfone, in particular to a hyperbranched polysulfone and a preparation method thereof, and belongs to the field of polymer materials. Background technique [0002] Polysulfone is an important thermoplastic special engineering plastic, mainly including polyethersulfone (PES), bisphenol A polysulfone (PSU), polyphenylene sulfone (PPSU), etc., among which bisphenol A polysulfone is the most widely used The broadest and most productive one. The rigid benzene ring structure, flexible ether group, and the large conjugated system formed by the sulfone group and the entire structural unit endow polysulfone with excellent properties, such as excellent mechanical properties, high temperature resistance, chemical corrosion resistance, and aging resistance. These characteristics make this type of material widely used in many fields such as aerospace, national defense, electrical and electronic, medical, nuclea...

Claims

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Application Information

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IPC IPC(8): C08G81/00C08G75/23C08G75/20
CPCC08G81/00C08G75/23C08G75/20
Inventor 邹敏张鑫陈海波
Owner WANHUA CHEM GRP CO LTD
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