Methyl phenyl vinyl borosilicate resin and preparation method and application thereof

A technology of methylphenylvinyl boron and silicone resin, which is applied in the direction of electrical components, circuits, semiconductor devices, etc., can solve the problems that the reliability of epoxy resin packaging materials, UV resistance and thermal aging performance cannot meet the requirements of packaging materials, and achieve Conducive to safe production, less investment in equipment, and reduced procedures

Inactive Publication Date: 2015-05-20
项炯华 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Epoxy resin packaging materials are far from meeting the requirements of packaging materials in terms of reliability, UV and heat aging resistance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: Preparation of methylphenylvinyl borosilicate resin

[0026] The molar ratio of monophenyltrimethoxysilane, methylphenyldimethoxysilane, tetramethyldivinyldisiloxane, boric acid and methylvinyldimethoxysilane is 0.214:0.135:0.009:0.081 : 0.093 for hydrolysis and polycondensation reaction, nitrogen protection 15% trifluoromethanesulfonic acid 50mL, hydrolysis reaction solvent is methyl isobutyl ketone 110mL, hydrolysis temperature is set at 50 ℃, reaction for 8h, cooling after hydrolysis, and separating the water layer , the methyl isobutyl ketone layer was washed with water for 3-4 times to neutrality, and after the methyl isobutyl ketone was recovered by distillation under reduced pressure, the low boilers were removed at 165°C and the pressure -0.095Mpa to obtain methyl phenyl ethylene based borosilicate resin.

[0027] Ph / R=0.48, R / Si=1.6, B / Si=0.18, Vi / Si=0.24 (atomic ratio), and the refractive index measured by Abbe refractometer is 1.52. The obtai...

Embodiment 2

[0028] Embodiment 2: Preparation of methylphenylvinyl borosilicate resin

[0029] The molar ratio of monophenyltrimethoxysilane, diphenyldimethoxysilane, tetramethyldivinyldisiloxane, boric acid, dimethyldiethoxysilane and vinyltrimethoxysilane is 0.214: 0.066: 0.043: 0.065: 0.012: 0.020 Carry out hydrolysis polycondensation reaction, nitrogen protection, 18% hydrochloric acid 50mL, hydrolysis reaction solvent is 100mL xylene, hydrolysis temperature is set at 60°C, react for 4h, cool after hydrolysis, and separate the water layer , Wash the xylene layer with water for 3-4 times to neutrality. After recovering the xylene by distillation under reduced pressure, remove low boilers at 155°C and pressure -0.095Mpa to obtain methylphenylvinyl borosilicate resin.

[0030] Ph / R=0.53, R / Si=1.6, B / Si=0.16, Vi / Si=0.27 (atomic ratio), and the refractive index measured by Abbe refractometer is 1.53. The obtained methylphenylvinyl borosilicate resin will not turn black and carbonized whe...

Embodiment 3

[0031] Embodiment 3: Preparation of methylphenylvinyl borosilicate resin

[0032]The molar ratio of monophenyltrimethoxysilane, methylphenyldimethoxysilane, tetramethyldivinyldisiloxane, boric acid, methylvinyldimethoxysilane and vinyltrimethoxysilane is 0.241: 0.135: 0.009: 0.081: 0.093: 0.020 for hydrolysis polycondensation reaction, nitrogen protection, 16% sulfuric acid 50mL, hydrolysis reaction solvent is toluene 110mL, hydrolysis temperature is set at 50 ℃, reaction 6h, cooling after hydrolysis, and separating water The toluene layer was washed with water for 3-4 times to neutrality. After the toluene was recovered by distillation, the low boilers were removed at 165°C and the pressure -0.095Mpa to obtain methylphenyl vinyl borosilicate resin.

[0033] Ph / R=0.49, R / Si=1.5, B / Si=0.16, Vi / Si=0.26 (atomic ratio), the refractive index measured by Abbe refractometer is 1.52. The obtained methylphenylvinyl borosilicate resin will not turn black and carbonized when placed at...

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Abstract

The invention discloses methyl phenyl vinyl borosilicate resin and a preparation method and application thereof. the preparation method of the methyl phenyl vinyl borosilicate resin comprises the following steps: dissolving raw materials (including trifunctional alkoxy silane, bifunctional alkoxy silane, boric acid or boron halide, a double-end capping agent or unifunctional alkoxy silane) into a solvent according to a certain ratio; under the action of strong acid, introducing nitrogen gas for protection and carrying out hydrolytic polycondensation for 4-8h; then washing with water and separating liquid; recycling the solvent under reduced pressure; and finally removing low-boiling-point substances in vacuum at a temperature of 145-175 DEG C under a pressure of lower than -0.095MPa to obtain the methyl phenyl vinyl borosilicate resin. The prepared methyl phenyl vinyl borosilicate resin has the advantages of high light transmittance, no yellowing, strong caking property, good high-temperature resistance and high tensile strength and can be applied to the field of LED packaging material.

Description

technical field [0001] The invention relates to the field of resin synthesis, in particular to a methylphenylvinyl borosilicate resin, a preparation method and an application thereof. Background technique [0002] Existing LED packaging technologies generally use high-transparency resins such as epoxy resins and silicone rubber-based resins as packaging materials. With the continuous improvement of LED brightness and power, higher requirements are put forward for the performance of LED packaging materials, such as high refractive index, high light transmittance, high thermal conductivity, UV resistance and heat aging resistance, low thermal expansion coefficient, low ion content and stress etc. Epoxy resin packaging materials are far from meeting the requirements of packaging materials in terms of reliability, UV resistance and heat aging performance. Silicone packaging materials have good transparency, high and low temperature resistance, and weather resistance, and are c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/56C08G77/20C08G77/06C08L83/14H01L33/56
Inventor 项炯华罗正鸿
Owner 项炯华
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