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Preparation and application of vinylphenyl polysiloxane resin containing epoxy groups in side groups

A technology of polysiloxane resin and vinyl phenyl, which is applied in the field of polymer material synthesis and preparation, can solve the problems of addition-type silicone resin mechanical properties and other performance effects, corrosiveness of raw materials, complex preparation process, etc., and achieve improvement The effect of low bond strength, complementary properties, and simple post-processing process

Inactive Publication Date: 2017-10-10
三友(天津)高分子技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

While this method is a convenient and effective way to improve poor adhesion, adhesion promoters can negatively affect the mechanical and other properties of addition-type silicones
Third, introducing reactive active groups (such as alkoxy groups, epoxy groups, acrylic groups) into polysiloxane molecular chains to obtain addition-type silicone resins with self-adhesive capabilities, but the preparation process of this method Relatively complex, so the application is greatly limited
[0004] Usually, vinyl-terminated methylphenyl silicone resins for addition reactions are prepared by cohydrolysis and cocondensation of chlorosilanes, but this method is more dangerous in post-processing, which is caused by the raw materials themselves. caused by corrosion

Method used

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  • Preparation and application of vinylphenyl polysiloxane resin containing epoxy groups in side groups
  • Preparation and application of vinylphenyl polysiloxane resin containing epoxy groups in side groups

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation of the vinyl phenyl polysiloxane resin that side group contains epoxy group:

[0027] Add 236.34 grams of γ-glycidyl etheroxypropyltrimethoxysilane, 41.39 grams of γ-(methacryloyloxy)propyltrimethoxysilane and 288.41 grams of diphenylsilanediol into the three-necked flask, and then add 28.31 201x4 grams of anion exchange resin (the amount of anion exchange resin added is 5% of the total mass of the monomer), protected by nitrogen gas, the temperature of the water bath was raised to 70°C, the condensation reaction was carried out for 8 hours, and then the low pressure was removed at 100°C / 0.096MPa Boiler, remove the anion exchange resin by filtration to obtain vinyl phenyl polysiloxane resin with epoxy group in the side group. γ-glycidyl etheroxypropyltrimethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane and diphenylsilanediol are represented by a, b and c in sequence, a:b:c Molar ratio=3:0.5:4, the sum of the contents of γ-glycidyl etheroxypropyl ...

Embodiment 2

[0031] The preparation of the vinyl phenyl polysiloxane resin that side group contains epoxy group:

[0032] Add 144.23g of 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, 145.21g of methacryloxypropyltriethoxysilane and 216.30g of diphenylsilanediol into the three ports Into the flask, add 40.46g of anion exchange resin 201x7 (the amount of anion exchange resin added is 8% of the total mass of the monomer), protect it with nitrogen, raise the temperature of the water bath to 50°C, and perform condensation reaction for 12 hours, then at 100°C / 0.096 MPa reduced pressure to remove low boilers, filter to remove anion exchange resin, to obtain vinyl phenyl polysiloxane resin with epoxy group in side group. 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, methacryloxypropyltriethoxysilane and diphenylsilanediol are represented by a, b and c in sequence , the molar ratio of a:b:c=2:2:4, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane and methacryloxypropyltriethoxy The sum of the silane cont...

Embodiment 3

[0034] The preparation of the vinyl phenyl polysiloxane resin that side group contains epoxy group:

[0035] Add 34.80g of 3-glycidyloxypropyltriethoxysilane, 175.74g of 3-(acryloyloxy)propyltrimethoxysilane and 216.31g of diphenylsilanediol into the three-necked flask, then add 21.34g of anion exchange resin 205x7 and 21.35g of anion exchange resin D280 (the amount of anion exchange resin added is 10% of the total mass of the monomer), nitrogen protection, the temperature of the water bath is raised to 25 ° C, condensation reaction for 15 hours, and then at 100 ° C / 0.096MPa to remove low boilers under reduced pressure, filter to remove anion exchange resin, and obtain vinyl phenyl polysiloxane resin with epoxy groups in side groups. 3-glycidyloxypropyltriethoxysilane, 3-(acryloyloxy)propyltrimethoxysilane and diphenylsilanediol are represented by a, b and c in sequence, a:b:c Molar ratio = 0.5:3:4, the sum of the contents of 3-glycidyloxypropyltriethoxysilane and 3-(acryloy...

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Abstract

The invention discloses preparation and application of vinylphenyl polysiloxane resin containing epoxy groups in side groups. A trialkoxysilane compound containing epoxy groups, a trialkoxysilane compound containing alkenyl groups as well as diphenyl silanediol are subjected to a condensation reaction at 25-70 DEG C for 8-15 h innitrogen atmosphere under catalysis of anion exchange resin, then a product is subjected to reduced-pressure processing at 100 DEG C and 0.096 MPa, low-boiling-point substances are removed, the anion exchange resin is removed by filtering, and the vinylphenyl polysiloxane resin containing the epoxy groups in the side groups is obtained. The reaction process is easy to control, the preparation is economical, environment-friendly and more suitable for large-scale volume production, and the product contains no inorganic ions and has excellent insulating property. With adoption of the anion exchange resin as a catalyst, a postprocessing process is simple, the anion exchange resin can be recycled, so that the cost is reduced, benefits are provided for environmental protection, the combination property of the vinylphenyl polysiloxane resin is excellent, and the vinylphenyl polysiloxane resin can be applied to the field of high-power LED packaging, fills up the market gap and has huge market potential.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis and preparation, and in particular relates to the preparation and application of a vinylphenyl polysiloxane resin with epoxy groups in side groups. It is used in the packaging field of high-refractive, high-adhesive, high-power light-emitting diodes. Background technique [0002] Among the components of the LED, the LED packaging material plays an important role in obtaining high light efficiency, and the light efficiency of the LED can be further improved by increasing the refractive index of the packaging material. Addition-type silicone resin has become an ideal choice for LED packaging materials because of its excellent thermal properties, good water resistance, oxygen resistance, UV resistance, weather resistance and non-toxicity. However, addition silicones have relatively poor adhesion to substrates due to their extremely low surface free energy and lack of reactive surf...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/14C08G77/08C08L83/06C08L83/07C08L83/05H01L33/56
CPCC08G77/08C08G77/14C08G77/20C08G77/80C08L83/06C08L2201/08C08L2201/10C08L2203/206C08L2205/02H01L33/56C08L83/04
Inventor 赵苗李建武吴子刚吴玉昆段亚冲高之香李士学刘佳
Owner 三友(天津)高分子技术有限公司
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