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Transparent photocurable high-refractive-index sulfydryl silicone oil and preparation method thereof

A high-refractive-index, light-curing technology, applied in the field of polymer materials, can solve problems such as long thermal curing time, time-consuming and energy-consuming refractive index, and low

Active Publication Date: 2021-08-03
HUIZHOU QIANGDA ELECTRONICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of the present invention is to provide a fast-curable high-refractive index mercapto silicone oil and its preparation method to overcome the defects of long thermal curing time, time-consuming and energy-consuming and generally low refractive index of organosilicon polymers in the prior art

Method used

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  • Transparent photocurable high-refractive-index sulfydryl silicone oil and preparation method thereof
  • Transparent photocurable high-refractive-index sulfydryl silicone oil and preparation method thereof
  • Transparent photocurable high-refractive-index sulfydryl silicone oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Unsaturated symmetrical episulfide silane monomer C 5 H 10 SiS 2 The preparation process of (theoretical value: C 37.04%, H 6.17%), Found: C 37.28%, H 6.42%, 10.04g, 95.63wt.%, the structural formula is as follows:

[0080]

[0081] Methylvinyldimethoxyalkane (13.20 g, 0.1 mol), HSCH 2 CH 2 SH (4.70 g, 0.05 mol), toluene (452.00 g) and p-toluenesulfonic acid (0.11 g) in N 2 Under protected conditions, at 80 °C, mechanically stirred for 48 h, and then added HSCH 2 CH 2 SH (4.70g, 0.05mol) and p-toluenesulfonic acid (0.11g), and then mechanically stirred at 100 ° C for 36h, brought to room temperature, with NaHCO 3 The saturated aqueous solution was washed twice with water, and the oil layer was taken and washed with anhydrous CaCl. 2 After drying, rotary evaporation, and vacuum concentration, unsaturated symmetric episulfide silane monomer C can be obtained 5 H 10 SiS 2 .

[0082] The mercaptomethylmethyldimethoxysilane (16.72 g, 0.11 mol), unsaturated symmet...

Embodiment 2

[0088] Unsaturated symmetrical episulfide silane monomer C 9 H 10 SiS 2 The preparation process of (theoretical value: C 51.43%, H 4.76%), Found: C 51.83%, H 4.42%, 22.95g, 93.47wt.%, the structural formula is as follows:

[0089]

[0090] Methylvinyldiethoxyalkane (16.00g, 0.1mol), (8.50 g, 0.06 mol), ethyl acetate (612.50 g) and p-toluenesulfonic acid (0.196 g) under N 2 Under the protection conditions, at 100 ℃, mechanical stirring for 36h, and then add (8.50g, 0.06mol) and p-toluenesulfonic acid (0.196g), and then at 80 ° C, mechanically stirred for 42 h, brought to room temperature, with NaHCO 3 The saturated aqueous solution was washed twice with water, and the oil layer was taken and washed with anhydrous MgSO. 4 After drying, rotary evaporation, and vacuum concentration, unsaturated symmetric episulfide silane monomer C can be obtained 9 H 10 SiS 2

[0091] The mercaptopropylmethyldimethoxysilane (63.12g, 0.35mol), unsaturated symmetrical episulfide silan...

Embodiment 3

[0097] Unsaturated symmetrical episulfide silane monomer C 13 H 12 SiS 2 The preparation process of (theoretical value: C 60.00%, H 4.62%), Found: C 59.83%, H 4.86%, 24.33g, 95.08wt.%, the structural formula is as follows:

[0098]

[0099] Methylvinyldiethoxyalkane (16.03g, 0.10mol), (9.62g, 0.05mol), diethyl ether (768.00g) and trifluoromethanesulfonic acid (0.26g) under N 2 Under protected conditions, mechanically stirred at 90 °C for 40 h, and then added (9.62g, 0.05mol) and trifluoromethanesulfonic acid (0.26g), and then mechanically stirred at 90°C for 36h, cooled to room temperature, and washed with NaHCO 3 The saturated aqueous solution was washed twice with water, and the oil layer was taken and washed with anhydrous Na 2 SO 4 After drying, rotary evaporation, and vacuum concentration, unsaturated symmetrical episulfide silane C can be obtained 13 H 12 SiS 2 .

[0100] The mercaptopropylmethyldiethoxysilane (45.84g, 0.22mol), unsaturated symmetrical epi...

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Abstract

The invention discloses transparent photocurable high-refractive-index sulfydryl silicone oil and a preparation method thereof. The structural formula of the transparent photocurable high-refractive-index sulfydryl silicone oil is (R1R2R3SiO1 / 2)a(R4R5SiO)b(R6CH3SiO)c(R7CH3SiO)d, R1, R2 and R3 are the same or different hydrogen groups, monovalent alkyl without aliphatic unsaturated bonds or unsaturated alkyl with 2-10 carbon atoms; R4 and R5 are monovalent hydrocarbon groups or aromatic hydrocarbon groups which do not contain aliphatic unsaturated bonds and at least contain one aromatic hydrocarbon group; the structure of R6 is -(CH2)eS-CH2CH2R0, e is a positive integer from 1 to 3, R0 is a symmetric epithio heterocyclic silicon group and has n sulfur atoms, and n is an integer multiple of 2; and the structure of R7 is -(CH2)fSH, and f is a positive integer from 1 to 3. The prepared high-refractive-index sulfydryl silicone oil is transparent, capable of being rapidly cured, high in refractive index, stable at room temperature, good in storage stability and low in odor. In addition, a one-pot two-step method is adopted, the preparation process is simple and convenient, the production efficiency is high, the cost is low, no harsh reaction conditions exist, and industrial production is easy to achieve.

Description

technical field [0001] The invention relates to polymer materials, in particular to a transparent photocurable high refractive index mercapto silicone oil and a preparation method thereof. Background technique [0002] At present, the vulcanization molding process of silicone polymers mainly adopts room temperature and high temperature vulcanization molding process, which often requires long-term room temperature or high temperature thermal curing and post-curing before safe use, which cannot realize continuous operation and production, which is time-consuming; high-temperature vulcanization The process often needs to be carried out at 150-180 °C, which is not conducive to co-molding with heat-sensitive components. The molding time is long, the application occasions are limited, and the energy consumption is serious. In addition, regardless of room temperature vulcanization silicone rubber or high temperature vulcanization silicone rubber, the vulcanization process lacks spa...

Claims

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Application Information

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IPC IPC(8): C08G77/28C08G77/06
CPCC08G77/28C08G77/06
Inventor 刘珠肖定书熊前程申玉求李险峰
Owner HUIZHOU QIANGDA ELECTRONICS