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High refractive index titanium hybrid silicon resin and preparation method thereof

A technology of titanium hybrid silicon and high refractive index, which is applied in the field of new high refractive index titanium hybrid silicone resin and its preparation, can solve problems such as high shrinkage rate and defects in cured products, and achieve high reaction temperature and high refractive index. , the effect of increasing the refractive index

Inactive Publication Date: 2013-08-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The double bonds in the hybrid resin can be cured by hydrosilylation, and no low-molecular substances are released during the reaction, which overcomes the shortcomings of high shrinkage rate of condensation-type cured silicone resin and defects in the cured product.

Method used

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  • High refractive index titanium hybrid silicon resin and preparation method thereof
  • High refractive index titanium hybrid silicon resin and preparation method thereof
  • High refractive index titanium hybrid silicon resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put a 50mL three-necked bottle with a condensing device into an 80°C oil bath, then add 2.965g of vinyltrimethoxysilane, 2.5g of xylene, and 23mg of barium hydroxide monohydrate (Ba(OH) 2 ·H 2 O) and 1.895g tetraisopropyl titanate, after stirring evenly, add diphenylsilanediol in batches (approximately every 5-10min, a total of 8.652g), after all diphenylsilanediol is added , the reaction continued for 6h, and the whole reaction was carried out under nitrogen atmosphere. In the later stage of the reaction, use a water separator to separate out the small molecule alcohol compounds produced in the system. After the reaction, the hybrid resin is cooled to room temperature, and the resin is filtered with a micron-scale oily filter membrane to remove solid impurities and residual catalysts in the system. Due to the high viscosity of the resin, it needs to be diluted with a solvent (acetone, chloroform or toluene, etc.) . Finally, at 85°C, the vacuum degree is -0.09Mpa~-0....

Embodiment 2

[0029] Put a 50mL three-necked bottle with a condensing device into an oil bath at 80°C, then add 1.4825g of vinyltrimethoxysilane, 4g of xylene, and 18mg of barium hydroxide monohydrate (Ba(OH) 2 ·H 2 O) and 2.842g tetraisopropyl titanate, after stirring evenly, add diphenylsilanediol in batches (approximately every 5-10min, a total of 6.489g), after all diphenylsilanediol is added , the reaction was continued for 8h, and the whole reaction was carried out in a nitrogen atmosphere. In the later stage of the reaction, use a water separator to separate out the small molecule alcohol compounds produced in the system. After the reaction, the hybrid resin is cooled to room temperature, and the resin is filtered with a micron-scale oily filter membrane to remove solid impurities and residual catalysts in the system. Due to the high viscosity of the resin, it needs to be diluted with a solvent (acetone, chloroform or toluene, etc.) . Finally, at 85°C, the vacuum degree is -0.09Mp...

Embodiment 3

[0031] Put a 50mL three-neck bottle with a condensing device into an 80°C oil bath, then add 1.1117g of vinyltrimethoxysilane, 4g of xylene, and 26mg of barium hydroxide monohydrate (Ba(OH) 2 ·H 2 O) and 6.395g tetraisopropyl titanate, after stirring evenly, add diphenylsilanediol in batches (approximately every 5-10min, a total of 9.7338g), after all diphenylsilanediol is added , the reaction continued for 10 h, and the whole reaction was carried out in a nitrogen atmosphere. In the later stage of the reaction, use a water separator to separate out the small molecule alcohol compounds produced in the system. After the reaction, the hybrid resin is cooled to room temperature, and the resin is filtered with a micron-scale oily filter membrane to remove solid impurities and residual catalysts in the system. Due to the high viscosity of the resin, it needs to be diluted with a solvent (acetone, chloroform or toluene, etc.) . Finally, at 85°C, the vacuum degree is -0.09Mpa~-0.1...

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Abstract

The invention relates to a high refractive index titanium hybrid silicon resin and a preparation method thereof, and belongs to the technical field of organic-inorganic hybridization. The preparation method comprises: placing a titanate monomer, a trifunctional alkoxy silane monomer and a solvent into a reactor, then adding dihydroxydiphenylsilane in batch, and carrying out copolycondensation for 2-12 h at a temperature of 60-110 DEG C under an alkaline catalyst effect to prepare a series of transparent and highly-viscous hybrid silicon resins with an adjustable refractive index, wherein the resins concurrently contain a Si-O-Si structure unit and a Ti-O-Si structure unit. The preparation method has advantages of simple process, mild reaction conditions, good repeatability, good controllability and the like. The hybrid resin has characteristics of high refractive index, excellent weathering resistance, excellent high temperature resistance and excellent low temperature resistance, wherein the double bond in the resin can be subjected to addition curing, small molecule substances are not generated during the curing process, and defects of high condensation type curing shrinkage rate, sand holes in the cured material, and the like are improved.

Description

technical field [0001] The invention belongs to the technical research field of organic-inorganic hybrid materials, and in particular relates to a novel high-refractive-index titanium hybrid silicone resin and a preparation method thereof. Compared with traditional silicone resin, the introduction of titanium element and phenyl group can significantly improve the resin's refractive index, weather resistance and high and low temperature resistance performance, and it is expected to be used as a substrate for LED silicone packaging materials, high temperature resistant coatings and composite materials resin. Background technique [0002] Light Emitting Diode (LED for short) is a semiconductor solid light source packaged with polymer materials (epoxy resin, silicone material), with long life, energy saving, environmental protection (no heat radiation and mercury and other toxic substances pollution ) and other advantages, it is known as a new light source in the 21st century. ...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06
Inventor 张军营展喜兵程珏史翎林欣张晓丰
Owner BEIJING UNIV OF CHEM TECH
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