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Preparation method for hexafluoropropylene oxide homopolymers

A technology of hexafluoropropylene oxide and homopolymer, which is applied in the field of preparation of hexafluoropropylene oxide homopolymer, which can solve the problem of inaccurate control of polymerization degree, inability to meet high-performance perfluoropolyether lubricating oil, difficulty in recycling, etc. question

Active Publication Date: 2016-01-27
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Abstract
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Problems solved by technology

In 2009, SergeiV.Kostjuk et al. published an article on the polymerization of hexafluoropropylene oxide on Macromolecules. Different fluorinated solvents were used, and potassium fluoride was used as a catalyst. The degree of polymerization obtained was between 15 and 21. Can not meet the requirements of preparing high-performance perfluoropolyether lubricating oil
Chinese patent CN101775130B uses potassium fluoride as a catalyst and hexafluoropropylene oxide oligomer as an initiator to controllably prepare hexafluoropropylene oxide polymers with a degree of polymerization of 3-50, but the control of the degree of polymerization is still not accurate enough , the need to additionally use prepared oligomers as initiators, and the use of hexafluoropropylene which is difficult to recycle as diluents

Method used

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  • Preparation method for hexafluoropropylene oxide homopolymers
  • Preparation method for hexafluoropropylene oxide homopolymers
  • Preparation method for hexafluoropropylene oxide homopolymers

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preparation example Construction

[0015] According to the preparation method provided by the technical solution of the present invention, in some embodiments, the reaction temperature is lowered each time by 5-10°C.

[0016] In some embodiments, the stirring reaction time is 1-3 hours.

[0017] The solvent of the catalyst potassium fluoride or cesium fluoride, in theory, the polar aprotic solvent can be used as the solvent of the catalyst. In the technical scheme of the present invention, the solvent used as the catalyst is a mixed solution of tetraethylene glycol dimethyl ether and a fluorine-containing solvent. Mixed with fluorine-containing solvent, stirred and filtered at room temperature. The mixture of tetraethylene glycol dimethyl ether and fluorine-containing solvent has the effect of stabilizing fluoride ions in the reaction process, and this effect is well known in the art.

[0018] According to the preparation method provided by the technical solution of the present invention, the cesium fluoride ...

Embodiment 1

[0039] N 2 Under protection, add 7.2 g of strictly dried potassium fluoride into 150 ml of a mixture of tetraethylene glycol dimethyl ether and hexafluoropropylene dimer (volume ratio 1:1), stir at room temperature for 0.5 h, and then filter. Vacuumize the strictly dry 2L reaction kettle to -1 bar, add the filtrate to the reaction kettle, and feed according to the method in Table 1 at 0°C, the feeding rate is: 0.5g / min of hexafluoropropylene oxide, 0.05ml of cesium fluoride saturated solution / min. A total of 480 g of hexafluoropropylene oxide was added, wherein the cesium fluoride saturated solution was a cesium fluoride saturated solution with a volume ratio of tetraethylene glycol dimethyl ether to hexafluoropropylene dimer at room temperature of 1:1. After the feeding is completed, the temperature in the kettle is slowly raised to room temperature (25° C.), and the product hexafluoropropylene oxide homopolymer is obtained by discharging from the bottom of the kettle. Afte...

Embodiment 2

[0044] N 2 Under protection, add 7.2 g of strictly dried potassium fluoride into 150 ml of a mixture of tetraethylene glycol dimethyl ether and hexafluoropropylene dimer (4:1 by volume), stir at room temperature for 0.5 h, and then filter. Vacuumize the strictly dry 2L reaction kettle to -1 bar, add the filtrate to the reaction kettle, and feed according to the method in Table 2 at 0°C. The feeding rate is: hexafluoropropylene oxide 1g / min, cesium fluoride saturated solution 0.1ml / min. A total of 960 g of hexafluoropropylene oxide was added, wherein the cesium fluoride saturated solution was a cesium fluoride saturated solution with a volume ratio of tetraethylene glycol dimethyl ether to hexafluoropropylene dimer at room temperature of 1:1. After the feeding is completed, the temperature in the kettle is slowly raised to room temperature (25° C.), and the product hexafluoropropylene oxide homopolymer is obtained by discharging from the bottom of the kettle. After its methy...

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Abstract

The invention discloses a preparation method for hexafluoropropylene oxide homopolymers. Potassium fluoride is employed as a catalyst to trigger ring-opening polymerisation of hexafluoropropylene oxide, a saturated solution of tetraethylene glycol dimethyl ether and fluorine containing solvent of cesium fluoride is added in batches for multiple times, the reaction temperature is lowered gradually from 0 DEG to -40 DEG C, thus reaction activity of tail end groups of hexafluoropropylene oxide homopolymers is kept, hexafluoropropylene oxide monomers are added continuously on this basis, and through control of addition times of hexafluoropropylene oxide and the cesium fluoride solution, hexafluoropropylene oxide homopolymers with an average polymerization degree of 50 can be synthesized. Through control of addition of monomers, hexafluoropropylene oxide homopolymers with an average polymerization degree of 20-50 can be synthesized selectively, and different industrial production requirements are met.

Description

technical field [0001] The invention relates to the field of fluorine-containing fine chemistry, in particular to a preparation method of a homopolymer of hexafluoropropylene oxide. Background technique [0002] High-polymer hexafluoropropylene oxide homopolymer terminal fluorination can prepare perfluoropolyether lubricating oil, which is liquid at room temperature. The molecular structure of fluoropolyether lubricants is similar to that of hydrocarbon lubricants, except that in perfluoropolyether molecules, fluorine atoms replace hydrogen atoms, and stronger C-F bonds replace C-H bonds, making perfluoropolyether oxidative stability , higher thermal stability, good chemical inertness and insulation. Perfluoropolyether oil with large molecular weight also has low volatility, wide temperature range and excellent viscosity-temperature characteristics, which are widely used in electronics, aerospace, machinery, nuclear industry, military, magnetic media, chemical industry and ...

Claims

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Application Information

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IPC IPC(8): C08G65/24
Inventor 李义涛阳峰冯海兵郑宝液徐俊星刘群方张兵兵陆翠方游孟梦
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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