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Ternary copolymerization perfluoropolyether and preparation method thereof

A technology for ternary copolymerization of perfluoropolyether and perfluoropolyether, which is applied in the field of polymer material synthesis, can solve problems such as difficulty in meeting usage requirements, and achieve the effects of increasing viscosity index, low cost and lowering pour point

Pending Publication Date: 2022-04-26
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The relatively small viscosity index and high pour point make it difficult for K-type perfluoropolyether to meet the requirements of wide temperature range and extreme conditions when it is used as lubricating oil.

Method used

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  • Ternary copolymerization perfluoropolyether and preparation method thereof
  • Ternary copolymerization perfluoropolyether and preparation method thereof
  • Ternary copolymerization perfluoropolyether and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The preparation method steps of the ternary copolymerized perfluoropolyether of this embodiment are as follows:

[0027] (1) Add 1.52g (0.01mol) of CsF and 4.45g (0.02mol) of tetraethylene glycol dimethyl ether to the dry low-temperature pressure-resistant polymerization reactor respectively, and then start stirring and low-temperature circulating bath; After reaching -35°C, first add 100.51g (0.67mol) of pure hexafluoropropylene into the reactor, and then add pure hexafluoropropylene oxide, tetrafluoroethylene oxide and perfluorooxetane respectively Monomer, wherein the molar ratio of the three monomers is 1:50:30, the total molar weight is 0.61mol, and the total mass is 83g. After the feeding is completed, the reaction is continued for 16h; after the reaction is completed, the reaction system is slowly raised to room temperature, and passed The catalyst in the reaction solution is removed by centrifugation, and the solvent and diluent in the reaction solution are remo...

Embodiment 2

[0034] The preparation method steps of the ternary copolymerized perfluoropolyether of this embodiment are as follows:

[0035] (1) Add 0.42g (0.01mol) of newly prepared NaF and 4.45g (0.02mol) of tetraethylene glycol dimethyl ether to the dry low-temperature pressure-resistant polymerization reactor, and then start stirring and low-temperature circulating bath; the reaction system After the temperature dropped to -31°C, add 5.62g (0.03mol) of pure 1,1,2-trifluorotrichloroethane to the reaction kettle, and then add pure hexafluoropropylene oxide, tetrafluorocyclo Oxyethane and perfluorooxetane monomers, wherein the molar ratio of the three monomers is 13:25:28, the total molar mass is 0.27mol, and the total mass is 40g, and the reaction is continued for 12h after the feeding is completed; the reaction is completed , the reaction system is slowly raised to room temperature, and the catalyst in the reaction solution is removed by centrifugation, and the solvent and diluent in th...

Embodiment 3

[0042] The preparation method steps of the ternary copolymerized perfluoropolyether of this embodiment are as follows:

[0043](1) Add 1.52g (0.01mol) of newly prepared CsF and 2.68g (0.02mol) of diethylene glycol dimethyl ether to the dry low-temperature pressure-resistant polymerization reactor, and then start stirring and low-temperature circulating bath; the reaction system After the temperature drops to -30°C, add 28.11g (0.15mol) of pure 1,1,2-trifluorotrichloroethane to the reaction kettle, and then add pure hexafluoropropylene oxide, tetrafluorocyclo Oxyethane and perfluorooxetane monomers, wherein the molar ratio of the three monomers is 30:1:16, the total molar mass is 0.30mol, and the total mass is 50g. After the feeding is completed, the reaction is continued for 15h; the reaction is completed , the reaction system is slowly raised to room temperature, and the catalyst in the reaction solution is removed by centrifugation, and the solvent and diluent in the reactio...

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Abstract

The invention discloses ternary copolymerized perfluoropolyether and a preparation method thereof. The ternary copolymerized perfluoropolyether disclosed by the invention is prepared by carrying out copolymerization on hexafluoropropylene oxide, tetrafluoroethylene oxide and perfluorooxetane. The preparation method disclosed by the invention comprises the following steps: respectively adding a certain amount of hexafluoropropylene oxide, tetrafluoroethylene oxide and perfluorooxetane monomers into a low-temperature pressure-resistant polymerization reaction kettle filled with a catalyst and a solvent, and reacting at low temperature; after the reaction is finished, slowly heating the reaction liquid to room temperature, centrifuging to remove the catalyst, and carrying out reduced pressure distillation to remove the solvent; and performing stabilizing treatment on the synthesized polymer in a reaction kettle resistant to corrosion of hydrogen fluoride and fluorine gas by using F2 to obtain the ternary copolymerized perfluoropolyether. Compared with existing K-type perfluoropolyether, the ternary copolymerized perfluoropolyether provided by the invention is higher in specific viscosity index, lower in pour point and better in comprehensive performance.

Description

technical field [0001] The invention relates to the technical field of polymer material synthesis, in particular to a ternary copolymerized perfluoropolyether of hexafluoropropylene oxide, tetrafluoroethylene oxide and perfluorooxetane and a preparation method thereof. Background technique [0002] Perfluoropolyether is a colorless and transparent polymer material. Compared with ordinary polyether, there are only three elements of C, F, and O in the perfluoropolyether molecule. The fluorine atom with the largest electronegativity makes the attraction between molecules smaller, and the surface tension of the molecule is also smaller. At the same time The C-F bond in the molecule has a strong shielding effect on the C-C and C-O bonds, making it have excellent heat resistance, oxidation resistance, corrosion resistance, radiation resistance and non-combustibility, and is widely used in aerospace, electronics, chemical industry and machinery, etc. field lubricants. [0003] At...

Claims

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Application Information

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IPC IPC(8): C08G65/22
CPCC08G65/226
Inventor 涂东怀吕剑谷玉杰马辉肖啸田松赵锋伟王博
Owner XIAN MODERN CHEM RES INST