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Preparation and solidification methods for carborane-liquid fluorine polymer

A curing method and liquid fluorine technology are applied in the field of preparation and curing of carborane-liquid fluoropolymers, which can solve problems such as low mechanical properties, and achieve the effects of low cost and simple and easy process.

Inactive Publication Date: 2013-07-03
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, its chemical properties, especially heat resistance and chemical resistance, are the same as solid fluoroelastomers, but its mechanical properties are lower than traditional fluoroelastomers

Method used

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  • Preparation and solidification methods for carborane-liquid fluorine polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 6.27g carboxyl-terminated liquid fluoropolymer (vinylidene fluoride-hexafluoropropylene copolymer, carboxyl mass percentage content is 1.23%, number average molecular weight Mn=6.2×10 3 , weight average molecular weight Mw=11.7×10 3 ) was dissolved in 50g of tetrahydrofuran and added to a 250mL four-neck flask, followed by adding 1,7-dimethylolcarborane (0.20 g), dicyclohexylcarbodiimide (DCC, 0.5559 g), 4-bis Aminopyridine (DMAP, 0.0229 g), p-toluenesulfonic acid (TsOH, 0.0203 g), at 25 o The reaction was stirred at C for 24h. There will be white suspended matter in the system. Filter the product system to remove the white solid substance. The filtrate is separated by column chromatography and washed with petroleum ether: ethyl acetate (10:1). After 500ml of the eluent, The substance adsorbed on the silica gel was rinsed with tetrahydrofuran until the yellow color faded, the eluent was collected, the solvent was rotated, and the product was vacuum-dried at 60°C for 2...

Embodiment 2

[0023] 6.27g of carboxyl-terminated liquid fluoropolymer (vinylidene fluoride-tetrafluoroethylene-hexafluoropropylene copolymer, carboxyl mass percentage content is 2.21%, number average molecular weight Mn=2.2×10 3 , weight average molecular weight Mw=3.6×10 3 ) was dissolved in 50g of tetrahydrofuran and added to a 250mL four-neck flask, followed by adding 1,7-dimethylolcarborane (0.42 g), dicyclohexylcarbodiimide (DCC, 1.1670 g), 4-bis Dimethinopyridine (DMAP, 0.0480 g), p-toluenesulfonic acid (TsOH, 0.0426 g), at 25 oThe reaction was stirred at C for 24h. There will be white suspended matter in the system, filter the product system, remove the white solid substance, and the filtrate is separated by column chromatography, rinsed with petroleum ether: ethyl acetate eluent, after 500ml of eluent, washed with tetrahydrofuran and adsorbed on The substances on the silica gel were collected until the yellow color faded, and the eluent was collected, and the solvent was evaporat...

Embodiment 3

[0025] 6g of carboxyl-terminated liquid fluoropolymer (vinylidene fluoride-hexafluoropropylene copolymer, carboxyl content 2.14%, number average molecular weight Mn=3×10 3 , weight average molecular weight Mw=6×10 3 , the following examples all use this material, and will not be repeated) dissolved in 50g of tetrahydrofuran, added to a 250mL four-necked flask, and sequentially added 1,7-dimethylolcarborane (0.38 g), DCC (0.94 g ), DMAP (0.0229 g), TsOH (0.0203 g), at 25 o The reaction was stirred at C for 8h. The aftertreatment of the reaction system and the purification of the crude product are the same as in Example 1.

[0026] A yellow viscous liquid was obtained with a yield of 68%. The GPC characterization results of the product showed that its number average molecular weight was 4.6×10 3 , weight average molecular weight Mw=8.7×10 3 . infrared and 1 H NMR all showed that the product was a carborane-liquid fluoropolymer. The detailed results are as follows: FTIR, ...

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Abstract

The invention discloses preparation and solidification methods for a carborane-liquid fluorine polymer. The preparation method takes a carboran diols and carboxyl-terminated liquid fluorine polymer as a raw material, prepares the carborane-liquid fluorine polymer through steglich reaction, and has the characteristics of simple and easy process, little side reaction and the like. The carborane-liquid fluorine polymer prepared by the preparation method has the characteristics of excellent heat resistance, chemical resistance, mechanical properties and the like. The invention further discloses a solidification method for the carborane-liquid fluorine polymer. The carborane-liquid fluorine polymer is solidified through reaction with an organic compound containing more than two isocyanate groups. The solidification product has the characteristics of excellent heat resistance, resistance to aviation kerosene, resistance to cyclohexane, resistance to hydrochloric acid, alkaline resistance, mechanical properties and the like. The carborane-liquid fluorine polymer can be used for preparing sealing agents, adhesives and coatings, which can be used in harsh working environments.

Description

technical field [0001] The invention relates to a preparation and curing method of carborane-liquid fluoropolymer. Background technique [0002] Liquid fluoroelastomers, compared with traditional fluoroelastomers, have lower molecular weight and better processability. Moreover, its chemical properties, especially heat resistance and chemical resistance, are the same as those of solid fluoroelastomers, but its mechanical properties are lower than those of traditional fluoroelastomers. [0003] Carborane is composed of two BH units in the icosahedral borane structure surrounded by two equally charged CH + Formed by replacing the unit, carborane has three configurations: cage, nest and network. The cage is closed, and the nest and network are open. Among them, the number of carborane in the cage is the largest. most stable. Among them, among numerous carborane molecules, dicarbo-closed-dodecaborane (C 2 B 10 h l2 ), especially eye-catching, it is one of the most important...

Claims

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Application Information

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IPC IPC(8): C08F214/22C08F8/42C08G18/62
Inventor 齐士成李娟吕亚非王金达李永平李赟张孝阿江盛玲员荣平
Owner BEIJING UNIV OF CHEM TECH
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