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High refractive resin containing silicon and preparation method of resin

A technology of resin and hydroxy silicone oil, which is applied in the field of silicon-containing high-refractive resin and its preparation, can solve problems such as poor performance, wear resistance, solvent resistance and poor moisture absorption resistance, and achieve good bonding performance and heat resistance. The effect of high refractive index

Inactive Publication Date: 2014-04-09
SHENZHEN POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When this kind of material is used as a base material to make optical devices, it generally has shortcomings such as wear resistance, solvent resistance, and poor moisture absorption resistance. application value, and the coating film used with it should also have a high refractive index.
However, at present, there are few researches on coating films or adhesive resins with special functions such as high refraction.

Method used

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  • High refractive resin containing silicon and preparation method of resin
  • High refractive resin containing silicon and preparation method of resin
  • High refractive resin containing silicon and preparation method of resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In the first step, add 3mol of epichlorohydrin into a 1000mL three-necked flask, stir and heat to 65°C, then add 0.6mol of 1,8-octanedithiol, then add about 300mL of 20% NaOH solution, and stir for 1h , cooled to room temperature, added 5 times the volume of diethyl ether and 5 times the volume of distilled water, separated the organic layer, washed to neutrality, dried with anhydrous magnesium sulfate, filtered, and the solvent was removed under reduced pressure to obtain sulfur-containing epoxy; Add 0.4mol of the sulfur-containing epoxy synthesized above into a 500mL three-necked flask, stir and heat to 120°C, then add 0.5% of the catalyst triethylbenzyl ammonium chloride and 1.0% of the polymerization inhibitor p-hydroxybenzyl ether; then add 0.8mol of acrylic acid, and continue to react for 3.5h to obtain sulfur-containing epoxy acrylate ①; in the second step, add 2.0mol of toluene diisocyanate (TDI) into a 1000mL three-necked flask, heat to 65°C, and Add 0.8% of bu...

Embodiment 2

[0028]In the first step, add 2 mol of epichlorohydrin into a 1000 mL three-necked flask, stir and heat to 75°C, then add 0.3 mol of 2,4-dimercaptopyrimidine, then add about 200 mL of 20% NaOH solution, and stir for 1 h. Cool to room temperature, add 3 times the volume of diethyl ether and 4 times the volume of distilled water, separate the organic layer, wash with water until neutral, dry with anhydrous magnesium sulfate, filter, and remove the solvent under reduced pressure to obtain sulfur-containing epoxy; Weigh 0.2 Add the sulfur-containing epoxy synthesized above into a 250mL three-necked flask, stir and heat to 110°C, then add 1.0% of the catalyst tris(acetylacetonate) complex cobalt (Ⅲ) and 0.8% of the polymerization inhibitor p-hydroxybenzene Methyl ether; add the methacrylic acid of 0.4mol again, continue reaction 4.5h, obtain sulfur-containing epoxy acrylate 1.; second step, in the there-necked flask of 500mL, add the diphenylmethane diisocyanate (MDI) of 1.0mol, Hea...

Embodiment 3

[0030] In the first step, add 3mol of epichlorohydrin into a 1000mL three-necked flask, stir and heat to 50°C, then add 0.3mol of 3,6-dioxo-1,8-octanedithiol, and then add about 300mL of 20 %NaOH solution, stirred and reacted for 2h, cooled to room temperature, added 2 times the volume of diethyl ether and 2 times the volume of distilled water, separated the organic layer, washed with water until neutral, dried with anhydrous magnesium sulfate, filtered, and the solvent was removed under reduced pressure to obtain Sulfur-containing epoxy; Weigh 0.2mol of the above-synthesized sulfur-containing epoxy into a 250mL three-necked flask, stir and heat to 100°C, then add 0.8% catalyst N,N-dimethylbenzylamine and 0.5% Inhibitor p-hydroxyanisole; add 0.4mol of methacrylic acid and continue to react for 5h to obtain sulfur-containing epoxy acrylate ①; in the second step, add 1.0mol of hexamethylene in a 500mL three-necked flask Diisocyanate (HDI), heated to 70°C, dibutyltin dilaurate is...

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Abstract

The invention discloses a high refractive resin containing silicon and a preparation method of the resin. The high refractive dual curing resin containing silicon comprises a sulfur epoxy acrylate chain segment and a silicon urethane acrylate chain segment. The preparation method comprises the following steps: firstly, reacting ethanedithiol with epichlorohydrin to generate epoxy sulfur, and then reacting epoxy sulfur with crylic acid to generate sulfur epoxy acrylate double ester or sulfur epoxy acrylic acid ester; grafting a silicon urethane acrylate prepolymer with an NCO functional group at the side chain, wherein the obtained resin comprises two structures: one structure contains three acrylate double bonds and can be solidified by ultraviolet light free radicals, and the other structure contains two acrylate double bonds (solidified by ultraviolet light free radicals) and an epoxy group (solidified by ultraviolet light cations or hotly cured), and can be dually solidified by ultraviolet light. The resin has high refractive index, and good adhesive performance and heat resistance after being cured, and can be used in ultraviolet-curable adhesives and coatings.

Description

technical field [0001] The invention belongs to the technical field of organic polymer synthesis, and in particular relates to a silicon-containing high-refractive resin and a preparation method thereof. Background technique [0002] Optical materials are generally divided into two categories: inorganic optical materials and organic polymer optical materials. Polymer optical materials have the advantages of light weight, impact resistance, easy processing and molding, and excellent optical properties, which greatly broaden the application level of optical materials. It has a wide range of application prospects. At present, polymer optical materials are gradually replacing inorganic optical materials in many fields. [0003] Compared with inorganic optical materials, polymer optical materials are limited by the chemical structure of the polymer itself, with low refractive index, low hardness, poor heat resistance, weather resistance, abrasion resistance, solvent resistance, ...

Claims

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Application Information

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IPC IPC(8): C08G18/67C08G18/61C08G18/58C08G59/17
CPCC08G18/12C08G18/61C08G18/672C08G18/585C08G18/65
Inventor 刘红波林峰肖望东张武英徐玲
Owner SHENZHEN POLYTECHNIC
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