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Preparation method of vinyl-terminated liquid fluoroelastomer supportive of room-temperature quick curing

A fast-curing, vinyl-terminated technology, applied in the field of preparation of vinyl-terminated liquid fluoroelastomers, can solve the problems of affecting service life, prone to degradation, long curing time, etc., and achieves good chemical resistance performance and simple preparation process. Easy to operate, fast curing reaction effect

Active Publication Date: 2016-11-16
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above two preparation methods are simple and easy to operate, with few side reactions, high yield and low cost, they also have disadvantages: the obtained carboxyl-terminated liquid fluoroelastomer is prone to degradation at high temperature, which affects the service life, and the curing temperature is relatively low. Higher and longer curing time; the obtained hydroxyl-terminated liquid fluoroelastomer not only has a relatively high curing temperature and a long curing time, but also has very few curing agents to choose from

Method used

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  • Preparation method of vinyl-terminated liquid fluoroelastomer supportive of room-temperature quick curing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 6g of carboxyl-terminated liquid fluoroelastomer (vinylidene fluoride-tetrafluoroethylene-hexafluoropropylene copolymer, carboxyl mass percentage content is 2.2%, number average molecular weight is 4000, weight average molecular weight is 5286) is dissolved with 70ml of acetone, Put it into a reaction glass container, add 0.852g of glycidyl acrylate and 0.8ml of trimethylamine, and simultaneously add 0.03g of hydroquinone (to inhibit cross-linking reaction), and then react at 95°C for 12 hours. After the reaction was finished, 0.5 ml of hydrochloric acid was added to the reaction system to neutralize trimethylamine. Then directly dry under reduced pressure to obtain vinyl-terminated liquid fluoroelastomer. The yield of the obtained product is 85%, the number average molecular weight of the product is 4355g / mol, the molecular weight distribution is 1.88, and the carboxyl conversion rate is between 84% and 93%. The infrared spectrum shows that the product is at 1770cm -...

Embodiment 2

[0020] Dissolve 12g of carboxyl-terminated liquid fluoroelastomer (vinylidene fluoride-hexafluoropropylene copolymer, carboxyl mass percentage content is 1.8%, number-average molecular weight is 4800, weight-average molecular weight is 5900) with 100ml of toluene, add to the reaction glass In the container, add 2.05g allyl glycidyl ether and 0.8ml trimethylamine, and add 0.06g hydroquinone (to inhibit cross-linking reaction) at the same time, and then react at 80°C for 18 hours. After the reaction was finished, 0.5 ml of hydrochloric acid was added to the reaction system to neutralize trimethylamine. Then directly dry under reduced pressure to obtain vinyl-terminated liquid fluoroelastomer. The yield of the obtained product is 78%, the number average molecular weight of the product is 4210g / mol, the molecular weight distribution is 1.68, and the carboxyl conversion rate is between 75% and 86%. The infrared spectrum shows that the product is at 1770cm -1 The characteristic pe...

Embodiment 3-6

[0022] The specific implementation methods are listed in the table below:

[0023]

[0024] Note: The carboxyl-terminated liquid fluoroelastomer used in Example 3 is vinylidene fluoride-tetrafluoroethylene-hexafluoropropylene terpolymer; the carboxyl-terminated liquid fluoroelastomer used in Example 4 is vinylidene fluoride-trifluorochloro Ethylene copolymer; The carboxyl-terminated liquid fluoroelastomer used in Example 5 is vinylidene fluoride-perfluoroethyl vinyl ether copolymer; The carboxyl-terminated liquid fluoroelastomer used in Example 6 is vinylidene fluoride-hexafluoro Propylene copolymer.

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Abstract

The invention discloses a preparation method of vinyl-terminated liquid fluoroelastomer supportive of room-temperature quick curing. The preparation method includes: dissolving carboxyl-terminated liquid fluoroelastomer into an organic solvent; adding an epoxy group-vinyl compound into a system; in the presence of an alkaline catalyst, stirring for reaction for 4-20 h in nitrogen atmosphere, wherein reaction temperature is controlled to 50-120 DEG C, and reaction pressure is pressure generated by the system itself. Terminated vinyl of the vinyl-terminated liquid fluoroelastomer has quite high reaction activity, curing reaction speed is high, quick curing can be realized at room temperature, and curing agent options are diverse. Curing points are positioned at two ends of a liquid polymer, so that tensile strength and elongation rate of a curing product can realize optimal balance. The curing product has high resistance to chemical media and can be used in harsh environment. The preparation method is simple and easy to implement, free of danger, low in cost and high in yield.

Description

technical field [0001] The invention relates to a preparation method of a vinyl-terminated liquid fluoroelastomer capable of rapid curing at room temperature. Background technique [0002] Traditional fluororubber is generally in solid form, and is prepared into the required structure by molding or extrusion. However, due to the limitation of mold size and shape, traditional solid fluororubber cannot meet all application requirements, and its processing performance is poor. Liquid fluoroelastomer has excellent heat resistance, oxidation resistance and chemical resistance, and can be cured into any desired shape according to needs, especially suitable for bonding, surface protection and pore sealing under harsh conditions. aviation sealing materials. [0003] 200910236784.7, an invention patent application titled "Preparation method of carboxyl-terminated liquid fluoropolymer", discloses a preparation method of liquid fluoroelastomer. Dissolve the solid fluoroelastomer in a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/22C08F8/14C08L27/16
CPCC08F8/14C08L27/16C08L2201/08C08F214/22
Inventor 张孝阿武建华王亚琴杨晓雪江盛玲吕亚非
Owner BEIJING UNIV OF CHEM TECH
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