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Hybrid organic silicon resin with framework structure containing Zr or containing Zr and Ti simultaneously and preparation method of organic silicon resin

A skeleton structure, silicone technology, applied in the field of silicone resin and its preparation, can solve the problems of large ternary sulfur ring tension, long polymerization induction period, unsuitable for packaging, etc., and achieve superior weather resistance and high and low temperature resistance, The synthetic method is simple and easy, and the effect of being easy to industrialized production

Inactive Publication Date: 2016-03-16
YANTAI DEBANG ADVANCED SILICON MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the refractive index of silicone materials for LED packaging with high refractive index can reach between 1.50 and 1.55, which has a certain gap with the chip refractive index (2~4). If the refractive index difference is too large, total reflection will occur, and the light will be reflected back Therefore, it is necessary to increase the refractive index of the packaging material, which can reduce the occurrence of total reflection, thereby improving the light extraction efficiency
[0004] There are many ways to increase the refractive index of polymers, usually by introducing atoms or groups with high molar refractive index (such as sulfur atoms, halogens, fused ring structures, etc.) Inorganic nanoparticles (TiO 2 , ZrO 2 , ZnS, etc.), but most methods are not suitable for packaging LED
The specific performance is as follows: (1) Among the ethylenic optical resins of sulfur-containing resins, vinyl monomers have poor activity and a long polymerization induction period; episulfide compounds have poor stability due to the large tension of the three-membered sulfur ring, and are difficult to Storage; (2) The transparency of polyimide and optical resin containing fluorene structure is not ideal, and the processing temperature is very high; (3) The weather resistance of halogen-containing resin is poor, it is easily affected by light and heat and changes color, and it violates the requirements of environmental protection ; (4) Inorganic nanoparticle composite optical resin has stability and transparency problems, it is often used as a thin film coating, and it is difficult to form a bulk material

Method used

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  • Hybrid organic silicon resin with framework structure containing Zr or containing Zr and Ti simultaneously and preparation method of organic silicon resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 25.2g of vinyl MT silicone resin (number average molecular weight 830), 200g of toluene, 0.1g of concentrated sulfuric acid and 8.0g of water into a three-necked flask, slowly add 84.11g of zirconium n-butoxide dropwise. The dehydration condensation reaction was carried out for 6 hours. After the reaction, wash with water to remove the catalyst in the system, dry and filter the organic phase washed to neutrality, and then remove the solvent and small molecular substances by vacuum rotary evaporation to obtain 45.8 g of transparent titanium-containing silicone resin with a refractive index of 1.67 / 25°C.

Embodiment 2

[0026] Put 50.0g of MQ silicone resin containing Si-H groups (number average molecular weight is 1308), 34.6g of zirconium isopropoxide and 120g of toluene into a three-necked flask, slowly add a mixture of 0.2g of potassium hydroxide and 4.5g of water, dropwise After the addition was completed, the dehydration condensation reaction was carried out at 110° C. for 5 hours. After the reaction, wash with water to remove the catalyst in the system, dry and filter the washed neutral organic phase, and then vacuum rotary evaporation to remove the solvent and small molecular substances to obtain 59.2 g of transparent titanium-containing silicone resin, the resin refractive index is 1.56 / 25°C.

Embodiment 3

[0028] Put 25.0g of vinylphenyl-containing MDT silicone resin (the number average molecular weight is 560), 112.74g of zirconium tert-butoxide and 180g of toluene into a three-necked flask, slowly add a mixture of 0.3g of potassium hydroxide and 10.6g of water, drop After the addition was completed, the dehydration condensation reaction was carried out at 110° C. for 8 hours. After the reaction, wash with water to remove the catalyst in the system, dry and filter the organic phase washed to neutrality, and then remove the solvent and small molecular substances by vacuum rotary evaporation to obtain a transparent titanium-containing silicone resin. 56.6g, the resin refractive index is 1.72 / 25°C.

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Abstract

The invention relates to hybrid organic silicon resin with a framework structure containing Zr or containing Zr and Ti simultaneously and a preparation method of the organic silicon resin. The structure of the resin contains Si-O-Si, Si-O-Zr and Zr-O-Zr structural units, or is likely to contain Si-O-Ti, Ti-O-Ti and Ti-O-Zr structural units simultaneously. According to the preparation method of the resin, the hydrolytic condensation process of organic Zr or combined hydrolytic condensation of organic Zr and titanate is realized in an organic silicon resin solution with the low molecular weight, and the resin is prepared. The synthetic method is simple and easy to implement, and industrial production is facilitated. Zr is introduced, or Ti links are introduced simultaneously, so that the refraction index and the high-temperature resistance of the hybrid resin can be significantly improved. The organic silicon resin with the low molecular weight in raw materials is converted, and olefinic bonds or -Si-H active groups are easily introduced into the hybrid resin structure, so that the hybrid organic silicon resin can have the addition curing reaction.

Description

technical field [0001] The invention relates to a silicone resin whose skeleton structure contains zirconium or simultaneously contains titanium hybridization and a preparation method thereof, belonging to the technical field of organic-inorganic hybrid materials. The zirconium (and titanium) link introduced in the resin can significantly improve the resin's refractive index, weather resistance and high and low temperature resistance; the low molecular weight silicone resin unit can easily introduce dilute bonds or -Si-H in the resin structure as a reaction raw material Active groups enable zirconium (and titanium) hybrid silicone resins to undergo addition curing, and can be used as LED silicone packaging materials, high-temperature resistant coatings, etc. Background technique [0002] Semiconductor lighting based on LED technology has the characteristics of high efficiency, energy saving, environmental protection, long life, and easy maintenance, and is known as a new lig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/00C08G79/14
Inventor 姜云陈维
Owner YANTAI DEBANG ADVANCED SILICON MATERIALS
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