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Polysulfone and preparation method thereof

A technology of polysulfone and dichlorodiphenyl sulfone, which is applied in sustainable manufacturing/processing, climate sustainability, chemical industry, etc., can solve the problems of unsuitable material environmental protection requirements, catalytic effect, low catalytic efficiency, etc. , to achieve the effects of excellent appearance, improved catalytic efficiency, and easy control of molecular weight

Active Publication Date: 2021-02-26
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalytic efficiency of the onium salt catalyst is low, and a large amount of catalyst needs to be added to the system to achieve the catalytic effect. It is easy to decompose under high temperature and alkaline conditions, resulting in various side reactions
U.S. Patent US5235019 uses a crown ether catalyst to prepare polysulfone. Although it has achieved certain results, the reaction time is long and the catalytic efficiency is not high. Moreover, this type of catalyst is expensive and highly toxic. Obviously, it is not suitable for the environmental protection of materials in today's society. Require
Calixarene catalysts, as the third-generation supramolecular hosts after crown ethers and cyclodextrins, can complex ionic guests and have high catalytic activity, but their conformation is unstable and prone to inversion, which has a positive effect on the catalytic effect. certain influence

Method used

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  • Polysulfone and preparation method thereof
  • Polysulfone and preparation method thereof
  • Polysulfone and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 57mmol sodium hydroxide / 12mL water, 20mmol polyethylene glycol-4 / 20mL tetrahydrofuran successively into a 100mL four-necked flask with an ice-salt bath, stir for 1.5h, slowly drop 37mmol4-methylbenzenesulfonyl chloride / 20mL tetrahydrofuran Into the system (about 2h), react below 5°C for 2.5h. Pour the reaction solution into ice water, add a few drops of 1M dilute hydrochloric acid, extract with dichloromethane, wash the organic phase with water and saturated brine, and dry over anhydrous magnesium sulfate. Filter and remove the organic solvent to obtain tetraethylene glycol di-p-toluenesulfonate.

[0039]Under the protection of nitrogen, 300 mL of acetonitrile, 6.75 mmol of p-tert-butylcalix[4]arene, 7.64 mmol of tetraethylene glycol di-p-toluenesulfonate and 7.64 mmol of potassium carbonate were successively added into a three-necked flask, and the reaction was stirred and refluxed at 80°C for 24 hours. Filtration, the filtrate was evaporated to remove the solvent...

Embodiment 2

[0042] Refer to Example 1 for the preparation process of the catalyst p-tert-butylcalix[4]-1,3-crown-5.

[0043] In a four-necked reaction flask with oil bath heating, stirrer, water separator and condenser, add 0.1 mol bisphenol S, 0.1 mol sodium carbonate, 0.098 mol 4,4'-dichlorobis Phenyl sulfone, 0.455g p-tert-butylcalix[4]-1,3-crown-5, 409.68g N,N-dimethylformamide, stir with nitrogen for 0.5h, and raise the temperature of the oil bath to 170 °C (system temperature 153 °C), 125 g of N,N-dimethylformamide was distilled off, and the reaction was continued for 3 h to obtain a yellow viscous polysulfone solution. Methyl chloride gas (gas flow rate: 1 L / min) was introduced into the system for capping, while the temperature of the oil bath was lowered to 150° C., and the reaction was stirred for 10 min. Dilute the reaction solution to 10% solid content, filter to remove salt, and precipitate in methanol to obtain a white flocculent solid, which is boiled in water for many time...

Embodiment 3

[0045] Refer to Example 1 for the preparation process of the catalyst p-tert-butylcalix[4]-1,3-crown-5.

[0046] 1mol bisphenol A, 2mol potassium carbonate, 0.95mol 4,4'-dichlorodiphenyl sulfone, 42.04g p-tert-butylcalix[4]-1,3-crown-5, 0.98kg sulfolane, one-time Put it into a reaction kettle equipped with temperature control, stirring and reflux water separation device, purge with nitrogen for 0.5h, raise the temperature of the reaction kettle to 300°C (system temperature 285°C), evaporate 120g of sulfolane, and continue the reaction for 10h to obtain a yellow viscous Condensed polysulfone solution. Methyl chloride gas was introduced into the system (gas flow rate 1 L / min) for capping, while the temperature of the oil bath was lowered to 150° C., and the reaction was stirred for 100 minh. Dilute the reaction solution to 10% solid content, filter to remove salt, and precipitate in ethanol to obtain a white flocculent solid, which is boiled in water for many times, filtered, a...

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Abstract

The invention discloses polysulfone and a preparation method thereof. The method comprises the following steps that 1, adding an organic bisphenol compound, 4, 4'-dichlorodiphenyl sulfone, a salt-forming agent, a catalyst and an aprotic polar solvent into a reaction container, increasing the temperature to the boiling point of the aprotic polar solvent, and removing part of the solvent through evaporation; 2) keeping the temperature, and reacting for a certain time to obtain a viscous polysulfone solution; 3) introducing an end-capping reagent into the system for end capping; and 4) separatingout the product in a precipitation agent, and carrying out a post-treatment process to obtain polysulfone powder. The polysulfone is prepared by adopting a one-step method, a water-insoluble hydrocarbon solvent is not needed, the operation is simple, the post-treatment difficulty and the production cost are reduced, meanwhile, calixarene crown ether is adopted as a catalyst, the reaction activityis improved, the reaction time is shortened, and the obtained product is high in molecular weight and narrow in molecular weight distribution.

Description

technical field [0001] The invention relates to a polysulfone and a preparation method thereof, in particular to a method for efficiently catalyzing the preparation of polysulfone and the polysulfone obtained thereby, belonging 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) and so on. Polysulfone resin has excellent properties, such as excellent mechanical properties, high temperature resistance, chemical corrosion resistance, aging resistance and so on. These characteristics make this type of material widely used in many fields such as aerospace, national defense, electrical and electronic, medical, nuclear power, oil well, ship, magnetic wire, military industry, automobile manufacturing industry and food processing. [0003] The preparation method of polysulfone is mainly divided into ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/23
CPCC08G75/23Y02P20/10
Inventor 邹敏张鑫陈海波
Owner WANHUA CHEM GRP CO LTD
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