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A kind of hyperbranched polysulfone with controllable degree of branching and preparation method thereof

A technology of hyperbranched polymerization and degree of branching, applied in the field of polymer materials, can solve the problems of complex synthesis of polyhydric phenol monomers, low resin molecular weight, reduced melt viscosity, etc., and achieves superior product performance, simple synthesis method, and melt The effect of viscosity reduction

Active Publication Date: 2022-04-22
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 improved, but the synthesis of the polyhydric phenol monomer is relatively complicated and the cost is high, and the obtained The molecular weight of the resin is also low, the application is limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 50g polysulfone (molecular weight M W =4×10 4 ) and 625mL of dichloromethane, stirred until the polysulfone was completely dissolved, added 150mL of 1,4-dichloromethoxybutane and 7.5mL of anhydrous tin tetrachloride, and reacted at 50°C for 5h. Use ethanol as a precipitating agent to precipitate the product, then repeatedly wash with ethanol and water, and dry at 40°C to obtain chloromethylated polysulfone. The chlorine content is 2mmol / g as measured by the oxygen nitrogen combustion-Volhard method.

[0037] Place a four-necked flask with a water separator, 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 sequence, raise the temperature to 80°C and stir for 3h , then raise the temperature to 110°C to reflux the toluene, collect the generated moisture with a water separator while stirring, and evaporate the toluene when the collected moisture reaches the theoretic...

Embodiment 2

[0039] The preparation process of chloromethylated polysulfone refers to Example 1, and the reaction is carried out at 50° C. for 4 hours to obtain 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 of o-xylene, 25.03g of bisphenol S and 13.82g of potassium carbonate powder in sequence, raise the temperature to 110°C and stir for 4h , and then raised the temperature to 150°C to evaporate part of the o-xylene, and finally raised the temperature to 180°C to completely evaporate the o-xylene, stopped heating and purged with nitrogen, and cooled the system to 160°C. Weigh 28.72g of 4,4'-dichlorodiphenyl sulfone and dissolve it in 139.32g of N,N-dimethylformamide, mix 4,4'-dichlorodiphenyl sulfone / N,N-di Methylformamide solution and 0.46g KF were sequentially added into the system, purged with nitrogen, and the temperature was rapidly raised to 140°C, and...

Embodiment 3

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

[0043] Put 1.5L of ethylbenzene, 200.24g of bisphenol F and 115.02g of solid potassium hydroxide into a reaction kettle with temperature control, stirring and reflux water separation device at one time, raise the temperature to 100°C and react for 4 hours, so that the system is fully salted , then raise the temperature to 140°C to reflux the ethylbenzene, collect the generated water with a water separator while stirring, and evaporate the entrainer ethylbenzene to dryness when the collected water reaches the theoretical value. Heating was stopped and nitrogen was purged, and the system was cooled to 120°C. Weigh 287.16g of 4,4'-dichlorodiphenyl sulfone and dissolve it in 3.73Kg dimethyl sulfoxide, mix 4,4'-dichlorodiphenyl sulfone / dimethyl sulfoxide solution with...

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Abstract

The invention discloses a hyperbranched polysulfone with a controllable degree of branching and a preparation method thereof. The method comprises the following steps: 1) generating bisphenol in a water-insoluble hydrocarbon solvent with an organic bisphenol compound and a salt-forming agent salt; 2) adding the solution of 4,4'-dichlorodiphenyl sulfone / aprotic polar solvent into the bisphenoxide system, and polycondensation reaction occurs under the catalysis of polycondensation catalyst to generate linear polysulfone; 3 ) adding a solution of chloromethylated polysulfone / aprotic polar solvent into the system to react to generate hyperbranched polysulfone; 4) precipitating the product in a precipitating agent, and obtaining hyperbranched polysulfone powder through a post-treatment process. Compared with the traditional method for preparing hyperbranched polysulfone, the present invention does not need to use expensive multifunctional monomers, which greatly saves costs; the molecular weight distribution of the obtained product is narrow, and no gelation phenomenon occurs, and it can also be obtained by selecting different chloroforms. The degree of branching is controlled by polysulfone with the degree of radicalization, which 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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Patent Type & Authority Patents(China)
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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