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Preparation method and solidification method of silicyl-terminated liquid fluorine polymer

A silyl-terminated, liquid fluorine technology, which is applied in the preparation and curing of silyl-terminated liquid fluoropolymers, can solve problems that affect the service life of the product and cannot meet the requirements of curing and use, and achieve good chemical resistance and low cost. Inexpensive, simple and easy-to-operate effect

Inactive Publication Date: 2013-07-10
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the carboxyl-terminated fluoroelastomer will degrade at high temperature, which will affect the service life of the product
Moreover, the curing of carboxyl polymer needs to be carried out at a certain temperature, which cannot meet the requirements of curing at room temperature.

Method used

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  • Preparation method and solidification method of silicyl-terminated liquid fluorine polymer
  • Preparation method and solidification method of silicyl-terminated liquid fluorine polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 8g of carboxyl-terminated liquid fluoropolymer (vinylidene fluoride-hexafluoropropylene copolymer, carboxyl mass percentage content 2.14%, number average molecular weight Mn=6.2×10 3 , weight average molecular weight Mw=11.7×10 3 , the following examples are not described, all of this substance) was dissolved in 50g of tetrahydrofuran, added to a 250mL four-neck flask, and pentafluorophenol (PFP, 0.81 g, 4.37 mmol), dicyclohexylcarbodiimide (DCC , 1.12 g, 5.47 mmol), 4-dimethylaminopyridine (DMAP, 0.026 g, 0.21 mmol), p-toluenesulfonic acid (TsOH, 0.041 g, 0.21 mmol), 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 matter, drop the filtrate into petroleum ether, and purify the product. The solvent was evaporated by rotary evaporation, and the product was dried under vacuum at 60° C. for 24 h. 7.03 g of a yellow viscous liquid were obtained. Infrared analysis showed...

Embodiment 2

[0022] 8g of carboxyl-terminated liquid fluoropolymer (vinylidene fluoride-tetrafluoroethylene-hexafluoropropylene copolymer, the mass percentage of carboxyl group is 2.21%, the number average molecular weight Mn=2.2×10 3 , weight average molecular weight Mw=3.6×10 3 ) was dissolved in 50g tetrahydrofuran / dichloromethane mixed solution, added to a 250mL four-necked flask, and pentafluorophenol (PFP, 0.81 g, 4.37 mmol), dicyclohexylcarbodiimide (DCC, 1.12 g, 5.47 mmol), 4-dimethylaminopyridine (DMAP, 0.026 g, 0.21 mmol), p-toluenesulfonic acid (TsOH, 0.041 g, 0.21 mmol), at 25 o The reaction was stirred at C for 8h. There will be white suspended matter in the system, filter the product system to remove the white solid matter, drop the filtrate into petroleum ether, and purify the product. The solvent was evaporated by rotary evaporation, and the product was dried under vacuum at 60° C. for 24 h. 7.46 g of a yellow viscous liquid were obtained. Infrared analysis showed that ...

Embodiment 3~6

[0025] The specific implementation method is the same as in Example 1, except that the molecular weight of the raw material changes, and the specific changes are as shown in the table, and the obtained results are also listed in the table. where: M n and M w / M n is the number-average molecular weight of the polymer tested by GPC; the conversion rate of the intermediate product is calculated by dividing the carboxyl content of the product after the reaction by the carboxyl content in the raw material.

[0026]

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Abstract

The invention discloses a preparation method of a silicyl-terminated liquid fluorine polymer. The silicyl-terminated liquid fluorine polymer is synthesized by a two-step method. The method comprises the following steps: (1) preparing a pentafluorophenol ester-terminated liquid fluorine polymer via a Steglich reaction by taking a carboxyl-terminated liquid fluorine elastomer and pentafluorophenol as raw materials; and (2) carrying out substitution reaction on the pentafluorophenol ester-terminated liquid fluorine polymer and silane, thereby preparing the silicyl-terminated liquid fluorine polymer. The humid solidification of the silicyl-terminated liquid fluorine polymer can be carried out at the room temperature, wherein the Tg of a solidified film is decreased along with the increasing of the relative molecular mass of the silicyl-terminated liquid fluorine polymer before being solidified. The solidified film has good resistance to acid, aviation kerosene, nonpolar solvents and other chemicals. The resisting performance of the solidified film with high molecular weight to the aviation kerosene, cyclohexane and hydrochloric acid is superior to that of the solidified film with low molecular weight. The method is simple and low in cost. The yield of the silicyl-terminated liquid fluorine polymer reaches more than 85%; and the strict pollution control measures are not required. The silicyl-terminated liquid fluorine polymer can be served as a raw material for preparing a sealant, an adhesive, a coating material and the like.

Description

technical field [0001] The invention relates to a preparation method and a curing method of a silyl-terminated liquid fluoropolymer. Background technique [0002] Liquid fluoropolymer has excellent heat resistance, oxidation resistance and chemical resistance, and can be cured into any desired shape at a lower temperature as required, especially suitable for bonding, surface protection and pore sealing under harsh conditions , It is an ideal sealing material, adhesive and coating for the aviation industry. [0003] At present, the existing liquid fluoroelastomers are mainly carboxyl-terminated liquid fluoroelastomers. However, the carboxyl-terminated fluoroelastomer will degrade at high temperature, which will affect the service life of the product. Moreover, the curing of the carboxyl polymer needs to be carried out at a certain temperature, which cannot meet the requirements of curing at room temperature. Therefore, it is particularly important to modify fluoroelastomer...

Claims

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Application Information

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IPC IPC(8): C08F214/22C08F214/18C08F8/42C08J3/24
Inventor 齐士成李娟吕亚非张孝阿王金达李永平李赟江盛玲员荣平
Owner BEIJING UNIV OF CHEM TECH
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