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Preparation method and application of high-refractive-index modified silane

A high-refractive-index and modified technology, applied in the field of high-refractive-index modified silane and its preparation, can solve the problems of large polymer dispersion, high resin density, high product odor, etc., and achieve mild reaction conditions and high product yield. , the effect of easy industrialization

Active Publication Date: 2018-08-17
SHENZHEN ANPIN SILICONE MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) The introduction of aromatic compounds or condensed ring compounds can increase the refractive index, but the prepared polymer has large dispersion, and there are hard and brittle defects in mechanical properties, and the refractive index can only reach about 1.5
[0005] (2) Introduce halogen elements other than F, but the density of the resin increases, the weather resistance is poor, and it is easy to yellow
[0006] (3) Introduce heavy metal ions such as lead, lanthanum or TiO 2 , PbS, FeS nanoparticles to increase the refractive index, but the resin density is high, the impact resistance is reduced, it is easy to yellow, and the practicability is poor
[0009] However, the existing method of introducing sulfur through sulfur heterocyclic monomers is prepared by Grignard reaction under ultra-low temperature conditions, which has the disadvantages of strong product odor and harsh preparation conditions, which limits the application of such high refractive index silanes and resins to promote

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 76.10 g (0.50 mol) of 2,5-dihydroxy-1,4-dithiane, ViMe 2 SiOEt 143.29g (1.1mol), ethyl acetate 438.78g, ethanol 175.51g, stirred for 40min, dichloroacetic acid 6.60g (0.051mol, PKa=1.48) and 37% concentrated hydrochloric acid 1.76g (0.018mol) were added, Stir for 10min, add 13.86g (0.77mol) of distilled water into the reaction system dropwise in a constant pressure funnel, react at 100°C for 25h, cool down to room temperature, add 7.52g (0.095mol) of ammonium bicarbonate, stir for 45min, use deionized water Wash 2 times with water, separate layers, take the oil layer, filter, rotary evaporate at 60°C, -0.095MPa for 60min, separate and purify by column chromatography (n-hexane / ethyl acetate=15 / 1) to obtain modified silane.

Embodiment 2

[0041] Add 198.30 g (1.00 mol) of 4-(1,3-dithiolane) phenol, (CH 2 =CH-CH 2 ) 2 MeSiOEt 180.2g (1.06mol), cyclohexane 378.50g, methanol 227.10g and stir for 30min, add pyruvic acid 3.78g (0.043mol, PKa=2.39) and mass fraction of 37% concentrated hydrochloric acid 3.78g (0.037mol), stir 20min, add 11.45g (0.64mol) of distilled water into the reaction system dropwise in a constant pressure funnel, react at 105°C for 35h, cool down to room temperature, add 9.50g (0.12mol) of ammonium bicarbonate and stir for 35min, wash with deionized water for 2 Repeat, separate layers, take the oil layer, filter, rotary evaporate at 70°C and -0.095MPa for 30min, separate and purify by column chromatography (petroleum ether / methanol=15 / 1) to obtain modified silane.

Embodiment 3

[0043] Add 136.24 g (1.00 mol) of 1,3-dithiapentane-2-ylmethanol, CH 2 =CH-CH 2 Me 2 SiOEt 156.68g (1.09mol), benzene 732.29g, isopropanol 292.18g and stir for 20min, add 14.65g of dichloroacetic acid (0.114mol, PKa=1.48) and trifluoromethanesulfonic acid 1.46g (0.01mol), stir for 25min, Add 15.70g (0.87mol) of distilled water into the reaction system dropwise in a constant pressure funnel, react at 100°C for 30h, cool down to room temperature, add 12.76g (0.16mol) of ammonium bicarbonate, stir for 60min, and wash twice with deionized water , separate layers, take the oil layer, filter, rotary evaporate at 60°C and -0.095MPa for 90min, separate and purify by column chromatography (petroleum ether / methanol=15 / 1) to obtain modified silane.

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PUM

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Abstract

The invention discloses high-refractive-index modified silane. A preparation method of the high-refractive-index modified silane comprises the following steps: mixing a sulfur-containing heterocyclicmonomer, a silane monomer and an organic solvent, adding an acidic stabilizer and a catalyst, adding water dropwise under stirring, performing heating, performing a reaction, performing cooling, performing a neutralization reaction, performing washing by using water, and performing separation to obtain the high-refractive-index modified silane, wherein the acidic stabilizer is an organic acid withPKa satisfying a relationship of 0<=PKa<=3.0. According to the method provided by the invention, the sulfur-containing heterocyclic modified silane monomer is prepared by an improved process, the sulfur-containing heterocyclic modified silane monomer can be used as an additive or a synthetic raw material of an organic silicone material and as a component of a packaging material, and improves light transmittance of a product; and the product has a high yield and little smell and is beneficial to application.

Description

technical field [0001] The invention belongs to the technical field of organosilicon materials, and relates to a high-refractive-index modified silane and a preparation method and application thereof. technical background [0002] The application fields of optical materials are expanding, and the products are constantly developing towards high refractive index, high light transmittance and high reliability. Silicone materials are widely used in medicine, biology because of their good temperature resistance, mechanical properties and non-toxic environmental protection. , communications and other optical material preparation fields have been widely used. At present, silicone materials used in optical lenses, optical fiber materials and other fields require a higher refractive index, even as high as 1.7 or more, and have good mechanical properties. [0003] The prior art methods for improving the refractive index of silicone materials are mainly to introduce high refractive in...

Claims

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Application Information

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IPC IPC(8): C07F7/18C07F7/08C07F7/12C08G77/28C08G77/06
CPCC07F7/0812C07F7/127C07F7/1892C08G77/06C08G77/28
Inventor 刘珠丁小卫祝琳
Owner SHENZHEN ANPIN SILICONE MATERIAL
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