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Preparation method and application of addition-type nano-zirconium-titanium composite sol/organosilicon hybrid resin

A technology of hybrid resin and composite sol, which is applied in the direction of coating, etc., can solve the problems of reducing material transparency, uneven dispersion, large internal stress, etc., and achieve the effects of UV aging resistance, mild reaction conditions, and good heat resistance

Active Publication Date: 2018-10-23
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Epoxy resins generally have the advantages of excellent adhesion, sealing, electrical insulation and corrosion resistance, but there are also disadvantages that cannot be ignored: such as low refractive index, easy to turn yellow after being heated or absorbing ultraviolet rays, internal high stress
However, its preparation process is complex and not suitable for large-scale production, and the direct addition of nanoparticles to the organic system will lead to uneven dispersion and easy agglomeration, resulting in light scattering and reducing the transparency of the material.
[0006] To sum up, there are still problems in the preparation of LED packaging materials, such as difficult reaction control, residual impurities, complex preparation process, system compatibility, and environmental pollution.

Method used

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  • Preparation method and application of addition-type nano-zirconium-titanium composite sol/organosilicon hybrid resin
  • Preparation method and application of addition-type nano-zirconium-titanium composite sol/organosilicon hybrid resin
  • Preparation method and application of addition-type nano-zirconium-titanium composite sol/organosilicon hybrid resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] In this example, see figure 1 with figure 2 , a preparation method of addition-type nano-zirconium-titanium composite sol / organosilicon hybrid resin, comprising the steps of:

[0052] ①Preparation of vinyl silicone resin: Add 35.0g of vinyltrimethoxysilane to a three-necked flask, heat up to 60°C under stirring, slowly add 9.2g of triethylmethoxysilane, continue to stir for 15min, then heat up to 80°C , then slowly add 20.6g triphenylmethoxysiloxane, then add 27.8g n-butanol, 5.4g deionized water and 2g dilute hydrochloric acid mixture, stir for 8 hours, cool to room temperature, use filtration technology to remove silicone resin Impurities in the product, after the reaction is completed, the solid impurities in the product are removed by filtration to obtain a colorless and transparent vinyl silicone resin for subsequent use;

[0053] ②Preparation of nano-zirconia-coated titania core / shell structure composite sol: Pour 25.5g tetrabutyl titanate into a flat-bottomed ...

Embodiment 2

[0058] This embodiment is basically the same as Embodiment 1, especially in that:

[0059] In this embodiment, a method for preparing addition-type nano-zirconium-titanium composite sol / organosilicon hybrid resin includes the following steps:

[0060] 1. Preparation of vinyl silicone resin: this step is the same as that of Example 1;

[0061] ②Preparation of nano-zirconia-coated titania core / shell structure composite sol: this step is the same as that in Example 1;

[0062] ③ Preparation of modified hybrid resin base glue: this step is the same as that of Example 1;

[0063] ④ Preparation of addition-type hybrid resin: Add 63.0 g of the modified hybrid resin base glue prepared in step ③ and 0.15 g of Kasrtdet catalyst (Pt~2%) into a flat-bottomed flask, mix and stir for 15 minutes, and mix well Then add 42.0g of methyl phenyl hydrogen-containing resin, the mass fraction of active hydrogen in the methyl phenyl hydrogen-containing resin is 0.5%, the refractive index at 25°C is...

Embodiment 3

[0066] This embodiment is basically the same as the previous embodiment, and the special features are:

[0067] In this embodiment, a method for preparing addition-type nano-zirconium-titanium composite sol / organosilicon hybrid resin includes the following steps:

[0068] ① Preparation of vinyl silicone resin: Add 32.0g methylvinyldimethoxysilane, 24.4g diphenyldimethoxysiloxane and 7.2g methyltrimethoxysiloxane in a three-necked flask, Heat up to 70°C under stirring, then add a mixture of 30.0g isopropanol, 5.4g deionized water and 1.0 acetic acid, continue mechanical stirring for 10 hours, cool to room temperature, use filtration technology to remove impurities in the silicone resin, and use The solid impurities in the product are removed by filtration to obtain a colorless and transparent vinyl silicone resin for subsequent use;

[0069] ②Preparation of nano-zirconia-coated titanium oxide core / shell structure composite sol: Pour 26.8g tetraisopropyl titanate into a flat-bo...

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Abstract

The invention discloses a preparation method and an application of addition type nano zirconium-titanium composite sol / silicone hybrid resin. The preparation method comprises steps as follows: vinyl siloxane, phenyl siloxane and alkyl siloxane are subjected to hydrolytic polycondensation for 2-12 h under the acidic condition, and transparent vinyl silicone resin is prepared; titanate is hydrolyzed under the acidic condition firstly, zirconate monomers are added for cohydrolysis, and nano-zirconia coated titanium oxide core / shell structured composite sol with adjustable refractive index is prepared; the vinyl silicone resin and the composite sol in certain proportion have a hybridization reaction, and the nano zirconium-titanium composite sol / vinyl silicone hybrid resin is obtained after suction of a solvent. The addition type nano zirconium-titanium composite sol / silicone hybrid resin has high refractive index, high transmittance, low water absorbability, anti-ultraviolet ageing performance, low internal stress and good heat resistance; the preparation method has the advantages of low raw material cost, simple process, safety and environment protection and is expected to be applied to the fields of LED package and optical materials.

Description

technical field [0001] The invention relates to a preparation method and application of a composite resin, in particular to a preparation method and application of an addition-type organic silicon composite resin, which is applied in the technical field of functional materials. Background technique [0002] Light-emitting diodes (LEDs) are another new generation of lighting sources after incandescent lamps and fluorescent lamps. The LED packaging material not only has the function of sealing and protecting the chip, reducing the junction temperature and heat dissipation of the chip, but also has the function of preventing the LED from being affected by the humidity and temperature of the surrounding environment, and reducing the difference in refractive index between the chip and the air, thereby improving the effective output of light. . Therefore, for LED packaging materials, good transmittance, high refractive index, heat resistance, UV aging resistance, low stress and l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08K9/10C08K3/22C08L83/07C08L83/05C09D183/07C09D183/05
Inventor 施利毅杭建忠钟敏花孙小英金鹿江陈伟
Owner SHANGHAI UNIV